final report group 6.pdf

Preliminary Design of Vanillin Production Plant From Black Liquor

i

Table of Content

Table of Content ...................................................................................................... i

CHAPTER 1 ........................................................................................................... 1

INTRODUCTION .................................................................................................. 1

1.1 Plant Development Background .............................................................. 1

1.2 Plant Development Goal ......................................................................... 7

1.3 Plant Development Analysis ................................................................... 8

1.3.1 Raw Material Analysis ...................................................................... 8

1.3.2 Location Analysis ........................................................................... 12

1.3.3 Market & Capacity Analysis .......................................................... 16

CHAPTER 2 ......................................................................................................... 23

PROCESS DESIGN .............................................................................................. 23

2.1 Process Technology Selection ................................................................ 23

2.2 Process Description ................................................................................ 26

2.2.1 Type Of Process .............................................................................. 26

2.2.2 BFD and Description ...................................................................... 30

2.2.3 PFD and Description ....................................................................... 32

CHAPTER 3 ......................................................................................................... 36

MASS AND ENERGY BALANCE ..................................................................... 36

3.1 Mass Balance .......................................................................................... 36

3.1.1 Overall Mass Balance ..................................................................... 36

3.1.2 Mass Balance Process Units ........................................................... 37

3.2 Energy Balance ...................................................................................... 40

CHAPTER 4 ......................................................................................................... 45

UTILITIES ............................................................................................................ 45

4.1 Water Utility ........................................................................................... 45

4.1.1 Water Utility Classification ............................................................ 45

4.2 Electric Utility ........................................................................................ 46

4.3 Steam Utility .......................................................................................... 48

BAB 5 ................................................................................................................... 49


ii

SIZING ................................................................................................................. 49

5.1 Vessel .......................................................................................................... 49

5.1.1 Black Liquor Storage Tank (S-101) ................................................ 49

5.1.2 Acidification Tank (V-101) ............................................................ 50

5.1.3 Acidification Tank (V-102) ............................................................ 51

5.1.4 Blending Tank (V-103) ................................................................... 53

5.1.5 Lignin Slurry Storage (S-102)......................................................... 54

5.1.6 Waste Storage (S-103) .................................................................... 55

5.1.7 H2SO4 Storage (S-104) ................................................................... 56

5.1.8 NaOH Storage (S-105) .................................................................... 57

5.2 Filtration ................................................................................................. 58

5.2.1 Plate and Frame Filter (PF-101)...................................................... 58

5.2.2 Plate and Frame Filter (PF-102)...................................................... 59

5.3 Pump ....................................................................................................... 60

5.3.1 Black Liquor Pump (P-101) ............................................................ 60

5.3.2 Black Liquor Acidification pump (P-102) ...................................... 60

5.3.3 Lignin Acidification Pump (P-103) ................................................ 61

5.3.4 Lignin Solution Pump (P-104) ........................................................ 62

5.3.5 Lignin Solution Pump (P-105) ........................................................ 63

5.3.6 Vanillin Slurry Pump (P-106) ......................................................... 63

5.3.7 Vanillin Solution Pump (P-107) ..................................................... 64

5.3.8 Water Pump (P-109) ....................................................................... 65

5.4 Conveyor ................................................................................................ 66

5.5 Bubble Column Reactor .............................................................................. 67

5.6 Ultrafiltration ............................................................................................... 68

5.7 Spray Dryer ................................................................................................. 69

5.8 Heat Exchanger .......................................................................................... 70

5.8.1 Heat Exchanger HE-101 ....................................................................... 70

5.8.2 Heat Exchanger HE-102 ....................................................................... 70

CHAPTER 6 ......................................................................................................... 71

PROCESS CONTROL ......................................................................................... 71

6.1 Process Control Instrumentation ............................................................ 71


iii

6.2 Process Control on Raw Material Storage Tank .................................... 71

6.3 Process Control on Heat Exchanger ....................................................... 72

6.4 Process Control on Reboiler ................................................................... 72

6.5 Process Control on Black Liquor Treatment Vessel .............................. 72

6.6 Process Control on Acidification Vessel and Lignin Solution Vessel ... 73

6.7 Process Control on Oxidation Reactor ................................................... 74

6.8 Process Control on Spray Dryer ............................................................. 76

CHAPTER 7 ......................................................................................................... 82

PLANT LAYOUT AND PIPING DESIGN ......................................................... 82

CHAPTER 8 ......................................................................................................... 86

HEALTH, SAFETY, AND ENVIRONMENT MANAGEMENT ....................... 86

8. 1 Health Aspects ........................................................................................ 87

8. 2 Safety Aspects ........................................................................................ 87

8.2.1 Hazard Identification and Risk Assessment (HIRA) ...................... 87

8.2.3 Hazard Operability Study (HAZOP) of Vanillin Plant....................... 94

8. 3. Environmental Aspects .......................................................................... 99

8. 3. 1. Liquid Waste ...................................................................................... 99

8. 3. 2. Solid Waste ........................................................................................ 99

8. 3. 3. Waste Gas .......................................................................................... 99

8. 4. Risk Management ................................................................................... 99

8.4.1. Personal Protection Equipment.......................................................... 100

8.4.2. Fire extinguisher ................................................................................ 105

8.4.3. MSDS (Material Safety Data Sheet).................................................. 107

8.5. Quality Control in Vanillin Plant ............................................................. 107

CHAPTER 9 ....................................................................................................... 108

ECONOMIC ANALYSIS .................................................................................. 108

9.1 Plant Cost Estimation ................................................................................ 108

9.2 Annual Operating Costs ....................................................................... 113

9.2.1 Raw Material Costs ....................................................................... 113

9.2.2 Operating Labor Costs ................................................................ 115

9.2.3 Utilities Costs ................................................................................ 116

9.2.4 Total Direct Costs ......................................................................... 117


iv

9.2.5 Total Fixed Costs .......................................................................... 117

9.2.6 Plant Overhead .............................................................................. 117

9.2.7 Total Manufacturing Cost ............................................................. 117

9.2.8 Expenses Cost ............................................................................... 118

9.2.9 Total Operating Cost ..................................................................... 118

9.3 Equity ................................................................................................... 119

9.4 Investment feasibility Analysis ............................................................ 120

9.5.1 Cash Flow ..................................................................................... 120

9.5.2 IRR ................................................................................................ 122

9.5.3 Net Present Value (NPV).................................................................... 124

9.5.4 Pay Back Period .................................................................................. 125

9.5.5Break Event Point (BEP) ..................................................................... 125

9.5.6 Sensitivity Analysis ............................................................................ 126

APPENDIX ......................................................................................................... 129

1. Vessel ....................................................................................................... 129

1.1 Black Liquor Storage Tank (S-101) ................................................. 129

1.2 Acidification Tank (V-101) ............................................................. 130

1.3 Acidification Tank (V-102) .............................................................. 132

1.4 Blending Tank ( V-103).................................................................... 133

1.5 Lignin Slurry Storage (S-102) .......................................................... 135

1.6 Waste Storage (S-103) ...................................................................... 137

1.7 H2SO4 Storage (S-104)..................................................................... 138

1.8 NaOH Storage (S-105) ..................................................................... 140

2. Plate and Frame Filter .............................................................................. 141

2.1 Plate and Frame Filter (PF-101) ....................................................... 141

2.2 Plate and Frame Filter (PF-102) ....................................................... 143

3 Pump ........................................................................................................ 144

3.1 Black Liquor Pump (P-101)&(P-102) .............................................. 144

3.2 Black Liquor Acidification Pump (P-102) ....................................... 146

3.3 Lignin Acidification Pump (P-103) .................................................. 148

3.4 Lignin Solution Pump (P-104) ......................................................... 150

3.5 Lignin Solution Pump (P-105) ......................................................... 152


v

3.6 Vanillin Slurry Pump (P-106) ........................................................... 154

3.7 Vanillin Solution Pump (P-107) ....................................................... 156

3.8 Water Pump (P-108) ......................................................................... 158

4 Bubble Column Reactor ........................................................................... 161

5 Ultrafiltrasi ............................................................................................... 163

6 Spray Dryer .............................................................................................. 165

7. Material Safety Data Sheet (MSDS) ........................................................ 171

REFERENCE ...................................................................................................... 174


1

CHAPTER 1

INTRODUCTION

1.1 Plant Development Background

Vanillin (4-hydroxy-3-methoxybenzaldehyde) is the major flavor

constituent of vanilla. This organic compound possesses the aldehydic, etheric and

phenolic functional groups, and its molecular formula is C8H8O3 corresponding to a

molecular weight of 152.15 (Washburn, 2003). The chemical structure and geometry

of vanillin are presented in Figure 1.1. Some relevant physical properties of vanillin

are shown in Table 1.1.

Figure 1.1. Chemical structure (a) and geometry (b) of vanillin molecule.

Vanillin occurs widely in nature, especially in the cured beans of the tropical

Vanilla orchids. It is the major component among about 200 other flavor compounds

found in these beans (Walton et al., 2003). Isolated vanillin occurs in the form of

white needle-like crystalline powder with a pleasant aromatic vanilla odor and an

intensively sweet taste, which are the main reasons for its widespread demand.

Table 1.1. Physical properties of vanillin.


2

Vanillin has a wide range of applications in food industry as a flavor agent

and in perfumery as an additive. Other applications are as chemical precursor in

the pharmaceutical industry, ripening agent, antifoaming agent in lubrication oils,

brightener in zinc coating baths, vulcanization inhibitor, and starting material for

insecticides and herbicides (Mathias, 1993; Villar et al., 1997).

There are around 150 varieties of vanilla, but only two of them are grown

commercially – Bourbon and Tahitian vanilla (McGregor, 2005). Vanilla has it

origins on Mesoamerican Mexico, with this country dominating the world

production until the late 19th century. Since then, the focus of development was

shifted to the former French colonies, in particular Madagascar, Comoros,

Reunion and Tahiti. Nowadays, vanilla is grown on numerous countries, with data

from 2005 indicating that Madagascar was the largest producer, accounted for

around 60% of the world production, followed by Indonesia and China, with 23%

and 10%, respectively. Looking at the last 20 years, the vanilla production has

oscillated between 1200 and 4000 tonnes, with a world consumption varying from

1800 to 3000 tonnes (McGregor, 2005).

The natural vanilla market is characterized by very volatile prices.

Normally the price pattern of vanilla is made up of high peaks and prolonged

periods of relatively low prices. These prices have been particularly sensitive to

events affecting a single country – Madagascar. From 1989 to 1995, the vanilla

market was regulated by the Univanille cartel, an alliance of vanilla exporters.

The major buyers and producers, principally Madagascar, met annually to

determine demand and export pricing. In Figure 1.2 is schematically shown the

evolution on the market prices of natural vanilla, since the early 1990’s to the first

half of 2005.


3

Figure 1.2. Evolution of natural vanilla prices since the early 1990’s to 2005 (Jaeger (2005)

Vanilla does not consist of vanillin alone, but contain several tens of

aromatic compounds. For example, the vanilla world trade in 2001 (2300 tonnes)

represents less than 50 tonnes of natural vanillin (Loeillet, 2003), which only

constitutes a yield around 2%. Historically, the production of vanillin was its

direct extraction from vanilla beans. However, according to the constantly

increasing markets, new chemicals routes were developed. Synthetic vanillin

became widely used and competition of markets is longstanding and turns more

fierce when prices of natural vanilla rockets.

Vanillin was first produced by Haarmann and Reimer in the late 1800’s,

using guaiacol from phenol. This was the main route for more than 40 years, until

it was discovered that vanillin could be produced from lignin present in the waste

liquor of pulp and paper industry. The commercial production of vanillin from

lignin started in 1937. This process become the dominant one for many years,

with 80% supply ratio of the synthetic vanillin market (Triumph Venture Capital,

2004). However, in the 1980’s some changes in the processes of pulp and paper


4

industry led to a decrease in the available raw material required by the vanillin

plants. The traditional calcium sulphite pulping process produced huge amounts

of disposable effluents, that combined with the growing public awareness on

environmental issues were leading to unsustainable waste treatment costs. These

mills started to close, or were converted to new technology that allowed the

recycling of the waste liquors for chemical recovery and thus making these by-

products streams not available for vanillin production. Since 1993, only

Borregaard was producing vanillin from lignin. Nowadays the synthesis of

vanillin from guaiacol accounts for 85% of the world supply, with the remaining

15% being produced from lignin (Triumph Venture Capital, 2004b).

Commercial users can choose between natural vanilla (very expensive and

used only in niche markets), synthetic vanillin and artificial vanilla flavor (ethyl

vanillin). Synthetic vanillin is a cost effective alternative to vanilla and is

increasingly substituting the natural product. It not only substitutes vanilla, but

also supplements adulterated vanillin extracts. Global demand for synthetic

vanillin currently is around 16000 tonnes per year. But guaiacol is petroleum

derivatives and it has been limited. Natural "vanilla extract" is a mixture of

several hundred different compounds in addition to vanillin. Artificialvanilla

flavoring is a solution of pure vanillin, usually of synthetic origin. Because of the

scarcity and expense ofnatural vanilla extract, there has long been interest in the

synthetic preparation of its predominant component. The first commercial

synthesis of vanillin start with the more readily available natural compound

eugenol today, artificial vanillin is made from either guaiacol or from lignin, a

constituent of wood which is a byproduct of the pulp industry, Lignin based

artificial vanilla flavoring is alleged to have a richer flavor profile than oil based

flavoring; the difference is due to the presence of acetovanillone in the lignin-

derived product.

Rhodia SA dominates the world vanillin market using the catechol-

guaiacol process. Rhodia entered the USA vanillin market in 1986 with the

purchase of the Monsanto plant. This plant was subsequently closed down in

1991. In November 1993, Rhodia purchased the ITT Rayonier vanillin business

and immediately closed the plant. After that, their main target has been China.


5

Borregaard (Norway), the second largest vanillin producer, is the only remaining

producer of lignin. The company also has guaiacol vanillin and ethyl vanillin

production capacity as it acquired Eurovanillin in 1995 (Triumph Venture Capital,

2004). Borregaard mainly supplies the European market and its lignin vanillin

production is almost exclusively for large costumers under long-term contracts.

Lignin based vanillin is in high demand in certain market sectors,

particularly the perfume industry, European chocolate manufacturers, and the

Japanese market, and as such tends to command a price premium. The price of

lignin vanillin is consistently maintained at about $1.00 to $2.00 per kg above that

of guaiacol based vanillin (Triumph Venture Capital, 2004b). The ethyl vanillin

price follows the same basic trend as the vanillin price. It is maintained at about

twice that of vanillin, but as it has about three times the flavour intensity of

vanillin there is a cost saving associated with substituting vanillin with ethyl

vanillin.

The main source of pure lignin is the pulp and paper industry, where

nowadays the Kraft process prevails with approximately 80% of the world

chemical pulp production (Ullmann’s Encyclopedia, 2003). A by-product stream

of this process, known as black liquor, contains typically 30 to 34% of lignin in

dry solid weight basis. This stream is burned to provide energy for mill

operations, and to facilitate the recovery of pulping chemicals. Due to the

complex energetic integration of the Kraft process, an expansion in the production

of pulp implies a revamp in the burners. An alternative plant design to the burners

revamp will be a utilization of the increased amount of black liquor in the

production of high-added value products and the elimination of a production

bottleneck at the recovery boiler (Axelsson et al., 2006). In this work, the focus is

on the production of synthetic vanillin from lignin obtained from black liquor.

A flow sheet of a process to produce synthetic vanillin from lignin in a

pulp and paper industrial unit is proposed in Figure 1.2. A portion of the by-

product stream, black liquor, is processed to extract lignin. This extraction can be

done by the traditional acidification/precipitation followed by separation, or using

an improved method similar to one developed by a Swedish group and known as

LignoBoost (Öhman et al., 2006). After obtaining purified lignin, the subsequent


6

process is based on three main steps studied in LSRE. The first step consists on

the alkaline lignin oxidation in a bubble column reactor, which is the main subject

of this thesis. Then, the mixture obtained in the reaction passes through a

membrane ultrafiltration process where the bigger molecules of degraded lignin

are retained. Sodium vanillate (salt of vanillin) and other low molecular weight

species goes to the permeate stream (Zabkova, 2006). Finally, the permeate

containing smaller molecules and excess NaOH flows through a packed bed on

acid resin in H+ form, in order to convert the sodium vanillate into vanillin

(Zabkova et al., 2007). This ion exchange step is accompanied by neutralization

reaction resulting in a lower pH for the product exit stream.

In order to have a reference point for the results to achieve, it is important

to refer a study developed in South Africa that revealed a benchmark final vanillin

concentration was 4.2 g/l, for a production process based on Kraft black liquors

(Triumph Venture Capital, 2004a). A process which final product has a

concentration below this value should not be very competitive in the present

scenario of the synthetic vanillin market.

Figure 1.3. Flow sheet of a process for vanillin production integrated in a pulp and paper mill

(Zabkova, 2006).


7

In the wide scope of the forestry activities the black liquor is obtained as a

by-product of the pulp and paper industry. For this reason, this work deals with

this industry. Pulp and paper industries are unquestionably of great relevance to

the Indonesia economy. In fact Badan Pusat Statistik (BPS) noted that pulp export

from January until September 2011 had increased by 72,37% from 1,05 juta tonne

to 1,81 million tonne. Indonesia take 9th

place in the world in pulp production.

The total of pulp industry is 13 units, where 6 units is in Sumatera. The

production capacity is for about 6,5 million tonne pulp per year.

Black liquor is the main raw material for vanillin making from lignin.

Black liquor is obtained from one of the biggest pulp and paper industry in

Indonesia that loctaing in Riau, PT Riau Andalan Pulp & Paper. The available

side product capacity of pulp is 4.920.000 m3/year. Because of the large side

production of black liquor, PT Riau Andalan concern to process the black liquor

beside to use it as fuel. Therefore, PT Riau Andalan Pulp & Paper decide to make

Vanillin Plant based on lignin that use black liquor as the raw material. By see the

ability of black liquor production and the excellence compared to China in

product shipping cost, the vanillin product from this plant can compete with

competitive price with good margin profit. Beside to fulfill the needs of vanillin

demand in Indonesia, the development of this plant will also create new job

opportunity, expand the vanillin export, and give contribution for local

communities. This is the first vanillin plant from lignin in Indonesia, it is expected

to increase confidence and independence of this nation to apply knowledge and

technology in real life.

1.2 Plant Development Goal

Market increase, raise in energy prices and high volatility in natural vanilla

prices are a strong driving force to have a deeper understanding of alternative

methods to produce vanillin. Vanillin obtained from lignin can employ a low-

value fuel to produce a high-added value and also represents a “green process”,

since it is biomass-based.

The guaiacol process to produce vanillin employs benzene obtained from a

non-renewable source (petroleum). Within this context, the objective of this plant

is to design the plant of vanillin production from lignin and its implementation in


8

Indonesia. The source of lignin should be black liquor from pulp and paper

industries using the Kraft process. In this work it was used lignin from softwood

Pinus spp., kindly supplied by PT Riau Andalan Pulp and Paper. The target of

vanillin production per day is 4500 kg or 1750 ton per year.

Needs of vanillin in Indonesia until this plant design was done is still filled

with synthetic vanillin imported from China. This vanillin factory has a useful life

20 years. We assume that vanillin needs always grow every years according to

projections import data we have collected. Until 2022 the vanillin needs of

Indonesia is still below 1750 ton / year. That’s way until that year this plant can

fulfill all of vanillin needs in Indonesia. Otherwise, in 2035 vanillin needs of

Indonesia can reach 12000 ton / year, and we predict that there will be another

vanillin plant from lignin to fulfill needs of vanillin, but with keeping the best

quality of vanillin this plant won’t lose the customer.

1.3 Plant Development Analysis

1.3.1 Raw Material Analysis

Vanillin (4-hydroxy-3-methoxybenzaldehyde) is organoleptically the

characteristic aroma component of the cured vanilla pod, where it contributes to

about 2% (w/w) of the dry matter (Priefert, H., Rabenhorst, J., & Steinbüchel, A.,

2001). It is used in a broad range of flavors for foods, confectionery, and

beverages (approximately 60%), as a fragrance ingredient in perfumes and

cosmetics (approximately 33%), and for pharmaceuticals (approximately 7%).

From the annual consumption of the world flavor market, only about 0.2%

originates from botanical sources (Krings and Berger 1998). There are 2 types of

commercially available vanillin. The first one is a natural vanillin extracted from

the vanillin pods and the second type is a pure vanillin chemically synthesized

from various chemical substrates. The price of the chemically synthesized

“nature-identical” vanillin is very low (about US$15 kg–1), compared to the price

of cured vanilla pods [between US$30 kg–1 and US$120 kg–1 (actual price)],

which usually contain about 2% (w/w) vanillin. The high price of “natural”

vanillin is mainly due to the limited availability of vanilla pods depending on

climate-associated fluctuations of harvest yields, economical and political


9

decisions, and last but not least to the labor-intensive cultivation, pollination,

harvesting and curing of vanilla pods.

Vanillin can be produced from phenolic compounds such as phenolic

stibenes, guaiacol, lignin, isoeugenol, eugenol, ferulic acid, vanillic acid, aromatic

amino acid, sugar beet pulp, wheat straw and biomass substances (Vaithanomsat,

P., & Apiwatanapiwat, W. , 2009). The main portion is produced by chemical

synthesis from guaiacol and lignin (Priefert, H., Rabenhorst, J., & Steinbüchel, A.,

2001).

1. Guaiacol

Guaiacol is one of the raw material to produce vanillin which is derived

from petroleum. Rhone-Poulenc is the World’s largest producer of vanillin and

ethyl vanillin with a $60m turnover in these two products. The company has

concentrated on the guaiacol route. Production facilities are situated in Saint Frons

(France), which has been in operation since 1978 and in Baton Rouge, Louisiana

(USA), which was commissioned over a two-year period ending in mid-1992.

Combined capacities for vanillin and ethyl vanillin are estimated to be 3 000t and

5 000t respectively. Ube Industries in Japan also use the guaiacol route to vanillin

and ethyl vanillin. The company recently expanded their 1 000t manufacturing

facility by 400t and are understood to produce more or less equal volumes of both

vanillin and ethyl vanillin.

Chinese producers are thought to produce only vanillin, mostly via the

guaiacol route (total capacity 2 000t). Rhodia acquired in 2000 the existing

business of the Chinese company Xuebao Fine Chemicals Co. Ltd, one of the

most recent vanillin plant at that time. Rhodia shares its experience in vanillin

manufacture about environmental problem, involved higher toxicity of the raw

materials (guaiacol), unfavourable ecobalance (3 to 5 more tars and COD -

Chemical Oxygen Demand, and 5 times more VOC - Volatile Organic

Compounds, 1/3 of which benzene), non compliance with environmental

standards, high health & safety risks and unacceptable standards for a flavor.

Therefore, many manufacturers are trying to produce vanillin with raw materials

that are environmentally friendly and renewable, likes lignin.


10

2. Lignin

The term lignin is derived from the Latin word for wood lignum. Lignin is

a major constituent in structural cell walls of all higher vascular land plants. Its

polyphenolic structure is well known for its role in woody biomass to give

resistance to biological and chemical degradation. Lignin is third component

macromolecule of wood associated kovalen with cellulose and hemicellulose. At

this time and future, the application of lignin has prospect. Lignin commercially

can be used as binder, filler, surfactant, polymer product, disperser and others

chemical raw, especially benzene derivate.

Figure 1.4 Sustainable industrial wood biorefinery operated by Borregaard, Norway (2010).

Lignin is a renewable raw material that could potentially be used as a raw

material in the manufacture of vanillin. This sustainable resource is to be used

within the biobased economy which is expected in the years to come to gradually

take a larger share compared to the fossil-based economy. The biobased economy

is not just the implementation of innovative technologies using renewable

resources, but it will be a real transition with a broad and high impact on society

at different levels (Langeveld and Sanders 2010).

The use of lignin as a raw material has the advantage in terms of

availability of raw material is abundant, especially in Indonesia. Lignin is an

organic compound produced by woody plants and Indonesia are rich of it. One of

lignin source which has abundant availability in Indonesia are oil palm empty fruit

bunches (PEFB). At present and for the future, Indonesia is one of the largest

palm oil producing country in the world that automatically as well as the world's

largest producer of PEFB. However, in the manufacture of vanillin, PEFB


11

ineffective if used as a raw material because of the process is not possible. Initial

pre-treatment to get lignin from PEFB not support passage of vanillin plant. This

is because the process of getting lignin is too complicated and a lot of equipment

needed. Moreover, until now there has been none of plant that utilizes PEFB as

raw materials in Indonesia.

Another alternative that can be used as raw material is black liquor. Black

liquor is the waste produced by the pulp and paper plant. Black liquor availability

is very abundant in Indonesia because Indonesia is one of the largest paper

producers in Southeast Asia. Therefore, black liquor can be used as renewable raw

materials in the vanillin manufacture. PT. Riau Andalan Pulp and Paper is a pulp

and paper plant that produced black liquor in Indonesia. The plant can produce

4.92 million tons of black liquor per year. 10% of black liquor produced by this

plant can support the needs of vanillin for 20 years.

Not only that, the processing of black liquor into lignin is much more economical

compared with the processing of PEFB into lignin.

Based on the explanation above, it was concluded that the raw materials

used to produce lignin vanillin was obtained from black liquor.

Table1.2 Analysis of Selection Raw Material

No Considerations Factor PEFB Black Liquor

1 Raw material

availability

5 4

2 Distance traveled raw

materials

5 5

3 Substances in the

material and the quality

of the products

4 3

4 Materials processing

efficiency

1 4

5 Material prices 4 5


12

1.3.2 Location Analysis

1.3.2.1 Raw Material Availability Aspect

Raw material availability aspect is the most influence aspect to decide the

location of the plant that we want to build. Relating to this aspect, plant

construction must near with the source of raw material to minimize the

transportation cost and also avoid production obstacle due to raw material supply.

Main raw material of vanillin plant is black liquor as waste of pulp and paper

production plant.

In Indonesia, The biggest pulp and paper industry is Riau Andalan Paper

and Pulp (RAPP) with production capacity about two million tonnes a year. As

one of the largest integrated pulp and paper mill in the world, black liquor as the

waste production is so much, around 4.920.000 m3 a year. RAPP locates in

PangkalanKerinci village, Langgam sub-district, Pelalawan Regency, Riau,

Sumatra.

Based on black liquor availability, we choose to build our plant in

Pelalawan Regency, Riau near RAPP plant. Actually, the black liquor of this plant

is used to production methanol as renewable energy and reduced consumption of

fossil fuel for their plant. On the other side, total mass of black liquor that we need

per day is 1000.5 tonnes or just about 0.007% from the total black liquor waste

production per day from RAPP. Therefore, we sure that RAPP will give the black

liquor as our raw material plant.

Figure 1.5, 1.6, and 1.7 show the location of RAPP and also location of

vanillin plant that we want to build in Riau.

1.3.2.2 Utility Needs Availability Aspect

The utility needs for vanillin plant is water, electricity, and fuel. The water

need is obtained PDAM and Kampar Kiri River near the plant. Meanwhile energy

fuel resource is obtained from Pertamina RU II Dumai which is distributed

through piping.Te electricity need is obtained from PLTA.


13

Figure 1.5. Location of raw material avaibility and plant building

Source: BadanKoordinasi Survey danPemetaanNasional, 2002


Source : googlemap.com

Riau Andalan Pulp & Paper

(Sumber Black Liquor)

Vanillin Plant



Vanillin Plant


14


Source : googlemap.com

1.3.2.3 Product Marketting Aspect

Our consumer is food companies especially milk, chocolate, and ice cream

industy. Most of that company locates in Cikarang industrial area.Some of the

biggest company are Unilever, Nestle, Diamond, and Campina.Vanillin product

will be distributed via land and sea transportation.Based on market place above,

vanillin plant in Pekanbaru, Riau is not too strategic because far from food

company target. We need more cost to distribute vanillin product. However, if we

compare with choosing to build vanillin plant near the market target, cost for

distribute vanillin product from Riau to Cikarang is lower than cost for deliver

raw material from riau to Cikarang.

Vanillin Plant




15

1.3.2.4 Transportation Aspect

Transportation in our plant is need to support our process production plant,

mainly for supply the supporting material and distribution the vanillin to the target

marketing. From the figure 1.4.3, we can looked that our plant is near with east

main road Jambi-Riau. Our plant also near with the Kampar Kiri River. For, the

air transport, our plant is near with the Sultan SyarifKasim II Airport in

Pekanbaru. Therefore, from the transportation aspect, our plant location is

strategic.

1.3.2.5 Social and Environment Aspect

1. Geographic Aspect

Pelalawan regency is one of ten regency in Riau Province and

located at 00o46,24’ LU - 00

o24,34 LS dan 101

o 30,37’-103

o21,36’

BT.Pelalawan has area about 13.256,7 km2danborders to the following

area.

a. North : Siak regency

b. South :IndragiriHuluand Indragiri Hilirregency

c. West : Kampar danIndragiriHulurengency

d. East :Karimun, Kepulauan Riau province, Bengkalis regency

Pelalawan regency topography consist of lowland and hill, which

the lowland is about 93% from total area of Pelalawan Regency. Ground

characteristic from certain parts are organic ground and acidic with

brackish ground water. The humidity and temperature quite high. In

general, Pelalawan regency is suitable use for plant construction because

the ground structur is flat, not bumpy, and near with water resource.

2. Social Aspect

The number of residents in regency Pelalawan based on survey in

2009 (BPS, 2009) is 280.197, consist of 145.442 are men (51,54%) and

134.775 are women (48,46%). Majority residents are moslem (257.447

people) and the others are Protestan, Katolik, Hindu, and Budha.

3. Labor Aspect

The occupation of Pelalawan regency residents is quite diverse.

There are businessman, farmer, fisherman, labor, and others. The


16

availability of labor is quite big due to Riau province have many Industry

and residents. Therefore we can quite easily get the labor.

1.3.3 Market & Capacity Analysis

Vanillin is a versatile, well-established aroma chemical used mostly as a

flavourcompound. The total world market is estimated at 10,500 tons per annum.

Themajor applications are in the manufacture of chocolate and ice cream, with

smallerquantities used in baked goods and confectionery. Vanillin can also be

used as a fragrance and fixative in perfumes, cosmetics and other fragrance

mixtures. It is alsoused as a pharmaceutical intermediate.Commercial users can

choose between natural vanilla (very expensive and used onlyin niche markets),

nature-identical vanillin (guaiacol or lignin vanillin), and artificialvanilla flavour

(ethyl vanillin).

Figure 1.8 Vanillin Use for Flavour Market

Source : www.nedlac.org.za/media/5959/industry.pdf

Natural vanilla flavouring, produced from the pod of the vanilla orchid by

extraction of the aroma compounds with ethanol, constitutes less than 5% of the

world market. Natural vanilla contains both vanillin and a range ofother aroma

chemicals, which in total are responsible for the full flavour of true vanilla.

Natural vanilla is considerably more expensive than synthetic vanillin by afactor

of 10.

Synthetic vanillin is produced on a commercial scale using two distinct

technologies.Vanillin produced by the different process routes has different

flavour profiles.Consumer preference ultimately drives demand for the different

vanillin products. Incertain applications, particularly the perfume industry,


17

European chocolate manufacturers, and the Japanese market, lignin vanillin is

preferred over guaiacolvanillin. As is the case with most aroma chemicals used in

the flavour industry,companies are reluctant to change from current suppliers as

the organoleptic profilewill also change.

The world demand for vanillin in its major applications is as follows: The

world demand for vanillin in its major applications is as follows:

Table 1.3 Vanillin World Demand Applications


Vanillin is a mature market, and the market is growing steadily,

anticipated to be 2–3% over the next few years. Flavour and fragrance

applications continue to expandin line with demographics and increases with

disposable income. As a result, thegrowth in consumption of vanillin in flavour

and fragrance products is growing at 4%in developing nations, in comparison to

2% in developed regions.Vanillin for many years was used as an intermediate for

2,3,5-trimethoxybenzaldehyde, which itself is an intermediate for the drug

trimethoprim.This product is now however manufactured almost exclusively in

China using thecheaper gallic acid route. In the 1980’s the use of vanillin as a

pharmaceuticalintermediate in the production of drugs such as L-methyl dopa

declined. It has nowlevelled to approximately 10% of total vanillin demand. In

Europe, the use of vanillinas a pharmaceutical intermediate appears to be captive

to Rhodia. The globaldemand for vanillin is estimated as follows:

http://www.nedlac.org/


18

Tabel 1.4 World Demands for Vanillin


The high cost of production and natural vanillin causes the industries of

vanillin consumer (foods and drinks, pharmaceuticals, and perfumes) in Indonesia

prefer to choose using synthetic vanillin which is imported from other countries.

Based on literature that we have learned, there is several reasons Indonesia has to

import synthetic vanillin. Firstly, in agricultural areas that producing vanilla beans

such as Jawa Tengah, Jawa Timur, Bali, Nusa Tenggara Timur, Sulawesi Utara,

Lampung, and Sumatra are found the pest of vanillin called Busuk Batang Vanili

(BBV). It is the primary diseases and became one of problems in Indonesia’s

vanillin production since 1960 (Soetono 1962; Hadisutrisno et al. 1967; Risfaheri

et al. 1998). BBV has destroyed vanilla plants in production areas so it causes

loosing of billions of rupiahs every years. The loss that caused by BBV in 1991 is

predicted almost Rp 32 billions (Untung, 1992). The damage of vanillin plants

caused by BBV In Bali is almost 80% (Sedhana, 1996). The consequences are the

cost of vanillin natural is so much expensive and not sold in Indonesia’s markets

so the natural vanillin products is exported to many countries. In the other hand,

vanillin needs in Indonesia is fulfilled by synthetic vanillin product import that

much cheaper.

Literally, the good or bad market qualities from vanillin commodities, is

not only determined by the vanilla qualities. There is many things that determine

the vanillin quality markets, they are farmer, collector, wholesaler, processor,

importir and also the marketing models that used in market systems. This case

also causes synthetic vanilin cost that imported by Indonesia is so expensive. Price

of natural vanillin producton the marketis 3-4 times the price of synthetic vanillin. Price


19

of natural vanilla extract U.S.$ 30-60 per gallon, while the priceof synthetic vanillin

U.S.$10-15 pergallon(Schultz, 2005, referenced inMelawati2006).

Synthetic vanillin prodution is predicted about 3000 tonnes per year,

whereas the global market demand of synthetic vanillin reaches 3500 tonnes.

Along with the development of food and drink and pharmaceutical industries, the

demand of synthetic vanillin will always increase with velocity 8-9% per year

with the market target in USA 27 %, Eropa 45 %, Asia 21 % and others 7 %. For

saving the foreign exchange and decreasing the dependence of vanillin import, so

the production of synthetic vanillin with efficien process technology and high

quality product is needed. This indicates that the vanillin market in Indonesia is

big enough.

In the future, we predict that the interest of people in Indonesia for the

products such as ice cream, chocolate and the others semi-luxury foods FMCG

owns like Wall’s, Campina, Diamond, Nestle and others will increase too.

Moreover, today, the cake factories in big cities have increased so big. This case

is supported with three reasons. Firstly, the facts that the economic growth is

stable enough and will increase straightly. It will effect the amounts of middle

class people in Indonesia which has high purchasing power is increased too.

Finally, the semi-luxury food products that contains vanilla will be more

affordable and demand will increase continously. Secondly, the aggresiveness of

large FMCG campanies in Indonesia causes their volume increases continously.

As a result, demand forvanillaas one of theraw materialswould be even greater. The last

reasonis that Indonesiais havingstyle trendsof consumerismwhere the need forfood and

beverageis notanymorelimited tostaplefoods anddrinksbut also thesemi-luxury foods and

drinksthat tendimpulsive. Wetried tomap thelocation ofplant semi-luxuryfood and

beverage productsthat wil be our prospective customers. Someof these companiesare

listed in Table 1.5 below.


20

Table 1.5 FMCG Companies

No Companies Products

1 Wall's

Ice Creams : Magnum, Paddle Pop,

Vienetta, Cornetto, Buavita, etc

2 Campina

Ice Creams: Concerto, Hula-Hula,

Tropicana, Bazooka, etc

3 Diamond Ice Creams

4 PT IndoMeiji Diary Food Ice Creams

5 PT Ceres Chocolates

6 PT Cadbury Indonesia Chocolates

7 PT Nestlé Indonesia

Coffees (Nescafe), Milk (Milo,

Carnation), Candies (FOXS)

Needs of vanillin in Indonesia until this plant design was done is still filled

with synthetic vanillin imported from China. This vanillin factory has a useful life

20 years. We assumed that vanillin neededs always grow every years according to

projections import data we have collected. Thus the amount of vanila needed each

year until 2035 (according to the useful life on the plant) can be calculated.

Table 1.6 Vanillin Needs in Indonesia

Code Commodity 2007 2008 2009 2010 2011 Trend

291241 Vanillin (4-hydroxy-3-

methoxybenzaldehyde)

2,413.8 3,320.5

3,165.4

4,564.1

3,873

13.47


21

Figure 1.9 Curve Vanillin Needs in Indonesia

Prediction and calculation needs vanillin until 2035 are shown in Table 1.7

below.

Table 1.7 Value of Imported Vanillin in 2015-2035

Years

Indonesian

Imported

Vanillin (ton)

Years Indonesian Imported

Vanillin (ton)

2011 288 2023 1868

2012 336 2024 2183

2013 393 2025 2551

2014 459 2026 2981

2015 537 2027 3484

2016 627 2028 4072

2017 733 2029 4759

2018 857 2030 5562

2019 1001 2031 6501

2020 1170 2032 7597

2021 1367 2033 8879

2022 1598 2034 10377

2035 12128

Vanillin factory will be built in 2013-2015 and began operating in 2015.

The factory is designed to meet 53% requirement of vanilla in 2025. Because

production in 2015-2035 produced about 4.5 tons per day. Amount of excess vanillin

y = 4E-133e0.1559x R² = 0.8783 0

1000

2000

3000

4000

5000

6000

2006.5 2007 2007.5 2008 2008.5 2009 2009.5 2010 2010.5 2011 2011.5


22

which we produce will be exported to Australia so the factory will not be lossin the

beginning of the operation. The production capacity of the factory is shown in the table

1.8 below.

Table 1.8 Production Capacity 2015-2035

Years

Demand of

Vanillin in

Indonesia

(ton)

Plant

Production

Capacity (ton)

Excess of

Production (ton)

2013 393 Building Plant

2014 459 Building Plant

2015 537 1350 813

2016 627 1350 723

2017 733 1350 617

2018 857 1350 493

2019 1001 1350 349

2020 1170 1350 180

2021 1367 1350

2022 1598 1350

2023 1868 1350

2024 2183 1350

2025 2551 1350

2026 2981 1350

2027 3484 1350

2028 4072 1350

2029 4759 1350

2030 5562 1350

2031 6501 1350

2032 7597 1350

2033 8879 1350

2034 10377 1350

2035 12128 1350

Thus, the plant design for the production of synthetic vanillin from lignin can

bedone, because the assessment can be realized technically and financially

feasible. Feasibility is a projection that could change if the price of raw material

or product prices fluctuate, so it is recommended to do innovation processes to

reduce production costs and still prioritize the qualities of synthetic vanillin.


23

CHAPTER 2

PROCESS DESIGN

2.1 Process Technology Selection

In the manufacture of vanillin, a process that is needed is a method of

decision LignoBoost. Lignin from black liquor and high temperature oxidation

process in a reactor that will produce vanillin. In addition to the method above

methods, other ways that are often used in the making of the balck liquor lignin,

which Organosolv method using alcohol. Organosolv method is the technology

used to convert biomass into compounds lignosellulosic the compound cellulose,

lignin, and hemicellulose (Mosier et al., 2005). These technologies include

enzymatic fractionating by cellulases and chemical hydrolysis by hot water

treatment, steam explosion, ammonia fiber explosion, dilute or concentrated acid

hydrolysis, alkaline treatment and organosolv processes. While Organosolv

process itself means the use of ethanol in the pre-treatment process in biorefinery

useful to recover the desired multiple lignin products.

While LignoBoost is a method of making lignin extraction from black

liquor using a compact cake or pellets and products can be used for biofuels or

raw material for the chemical industry. LignoBoost works in conjunction with

evaporation. It all starts with being precipitated lignin from the black liquor by

lowering the pH with CO2. The precipitate is then dewatered using a filter press.

LignoBoost then overcomes conventional sodium filtering and separation

problems by redissolving the lignin in spent wash water and acid. The resulting

slurry is dewatered and washed once again, with acidified wash water, to produce

virtually pure lignin cakes. The lignin can be exported or, after the final drying, be

used as fuel in the lime kiln.


24

Figure 2.1 Proses Lignoboost

Table 2.1 Scoring Process of Lignin Production

Parameter

Retention

Time

(30%)

Process

Handling

(10%)

Cost

(40%)

Concentration

Obtained

(20%)

Total

Organosolv

Process 1 1 3 1 1.8

LignoBoost

Process 4 3 1 4 2.7

Retention time is the length of time used in the process of making lignin.

The greater nilainy, means less time spent in the process. Conversely, the more

time spent, indicating the smaller value given. In the references we get, the time

used to process more than one day Organosolv in a single batch. Meanwhile,

LignoBoost Process only requires 4 hours in a single batch.

Handling Process is how easy the process was done. In a reference point

that we get, Organosolv mixing process using the process at every stage of the

process used to be done so that the guard is large enough. Meanwhile, LignoBoost

Process conducted in a reactor so that maintenance is done not so great. Cost is


25

how inexpensive process. Process Organosolv use only simple tools are used so

the cost is not expensive. Otherways, LignoBoost Process using a mixing tank

used so the cost is very expensive. Obtained Concentration is how much product.

With a very high price, LignoBoost Process can use the tank so that the results can

be produced very much.

The next process is the process of making lignin into vanillin. In the

manufacture of vanillin tool used is oxidation reactor. Reactor oxidation can be

used in a continuous or batch mode. Continuous process is usually done to reduce

the area of the plant so that the plant will be used more efficiently. In contrast,

batch processes are used to meet the needs of the production of very large so the

existing plant will be larger wide area.

Table 2.2 Scoring process in Oxidation Reactor

Parameter

Process

Time

(30%)

Process

Handling

(10%)

Cost

(20%)

Concentration

Obtained

(30%)

Mass

Transfer

(10%)

Total

Batch

System 2 2 2 3 3 2.4

Continous

System 3 3 3 1 1 2.2

According to the tables above our team will choose is a batch process

Because of five parameters. Parameters that we choose is big factor in building a

plant. There are Process time, process handling, cost, consentration obatained, and

mass transfer. If the value of retention time is high, it means retention time of that

process happen in not a long time. Otherwise we if the retention time is low, it

means we need a long time in the process. In a batch system, process time need 12

hours a day. While in Continuous System, it takes time in one process can not be

calculated Because every second of BCR will produce.

If the value of the cost is high, it means the process is cheap and if low, it

means the process is expensive. Batch system is more expensive than continuous

process Because in batch system, the area will be very huge to cover capacity of

the plant. If the value of concentration obtained is high, it means we have a big


26

product in that process, and if low it means the product is small amount. Batch

system will produce until 0871 amounted to 0.7 g / L, while, for the continuous

process is 0.56 until 0.67 g / L. Mass transfer describe the amount of movement of

a substance that will the make the process efficient. High value is big mass

transfer, low mass transfer value is small. Batch system will result in a greater

mass transfer due to the mass of those who dwell in the reactor.

2.2 Process Description

2.2.1 Type Of Process

In vanillin production process, there are two primary stages to

producevanillin from black liquor. Black liquor contains typically 30 to 34% of

lignin in dry solid weight basis. Lignin should be extracted from black liquor with

LignoBosstprocess and continued with conversion of lignin to vanillin.

Figure 2.2 Diagram of vanillin production process

2.2.1.1 Lignin Extraction from Black Liquor

LignoBoost is a complete system that extracts ligninfrom Kraft black

liquor.LignoBoost works in conjunction with evaporation.In the LignoBoost

process, a stream of black liquor is taken from the black liquor evaporation plant

(Fig. 2.2), then lignin is precipitated by acidification (the preferred acid is CO2)

and filtered (“chamber press filter 1”, Fig. 2.2).Instead of washing lignin

immediately after filtration, as in traditional processes, the filter cake is re-

dispersed and acidified (“cake re-slurry”, Fig. 2.2). The resulting slurry is then


27

filtered and washed by means of displacement washing (“chamber press filter 2”,

Fig. 2.2). When the filter cake is re-dispersed in a liquid, at pH level and

temperature values approximately equal to those of the final washing liquor, the

concentration gradients during the washing stage will be low.

The change in the pH level, most of the change in ionic strength and any

change in lignin solubility will then take place in the slurry, and not in the filter

cake or in the filter medium during washing.The filtrate fromchamber press filter

2 (filtration, washingand dewatering stages) should be recycled tothe weak black

liquor. The resulting slurry is once again dewatered and washed, with acidified

wash water, to produce virtually pure lignin cakes.In some cases, thisfiltrate can

be also used for washing theunbleached or oxygen delignified pulp.The

LignoBoost process therefore makesit possible to extract lignin efficiently

fromthe black liquor in kraft mills. The majoradvantages, compared to the

previoustechnology, are the following:the filter area and the volume of

acidicwashing water can be kept at lowervalues, resulting in lower

investmentcosts,the addition of sulfuric acid can be alsokept at a lower level,

resulting in loweroperational costs,the yield of lignin is higher, the lignin has a

lower ash and carbohydrate content, the lignin has a higher content of dry solids.

Figure 2.3General layout of the LignoBoost lignin removal process (post-treatment,

drying and pulverizingare excluded)

2.2.1.2 Lignin Oxidation in Batch Process

Production of vanillin lignin based must be made in alkaline conditions.

Alkaline conditions is made to achieve a very high pH nearing pH 14, in addition


28

to high temperature conditions also are 1500C and 10 bar.The purpose of this

process is to break the bond position of alpha-and beta-carbon of fenilpropane and

breaking bonds in the carbon chain in the phenyl propane propanoid. Lignin

oxidation process in batch mode formed in a jacketed reactor with controlled

temperature and pressure. The reactor is under stirring and oxygen was fed to the

reactor.

LigninLingoboost outcome enter into a reactor that has a temperature

operating conditions of 1500C and pressure of 10 bar.Alkaline conditions created

by inserting NaOH pH 14 into reactor first. Then lignin lignoboost enter to the

input process. After that, the solution oxidaze with O2 gas 50% N2 50%.Lignin

reaction occurred with O2 being described at the beginning of the bond that ties

will occur. NaOH will react also with lignin to form Sodium Vanilate.Sodium

Vanilate is salt vanillin mixed with Na+ ions. In addition it also produced some of

the content of impurity content to be separated. Lignin is not transformed to

Sodium Vanilate 100% m.

2.2.1.3 Membrane Ultrafiltration Separation

In the filtration process, the tool used is membrane ultrafikasi.

Membraneultrafikasi used has a large cut-off membrane of 15 kDa, or about 1.6

nm and the pressure used is 0-4 bar. Vanillin has large molecules 152 Da MW,

making vanillin will pass with the existing pores.

This process begins with the entry of sodium vanilate and other impurities.

This process aims to separate Sodium vanilate with other impurities by using the

principle of molecular size difference. Sodiumvanilate is outflow and by product

is lignin and impurities. Lignin obtained from the by-product will in turn go back

to the oxidation tank to re reacted with O2.

2.2.1.4. Spray Dryer

Spray drying is a method of producing a dry powder from a liquid or

slurry by rapidly drying with a hot gas. This is the preferred method of drying of

many thermally-sensitive materials such as foods and pharmaceuticals. A

consistent particle size distribution is a reason for spray drying some industrial

products such as catalysts. Air is the heated drying medium; however, if the liquid


29

is a flammable solvent such as ethanol or the product is oxygen-sensitive

then nitrogen is used.

All spray dryers use some type of atomizer or spray nozzle to disperse the

liquid or slurry into a controlled drop size spray. The most common of these are

rotary disks and single-fluid high pressure swirl nozzles. Alternatively, for some

applications two-fluid or ultrasonic nozzles are used. Depending on the process

needs, drop sizes from 10 to 500 µm can be achieved with the appropriate

choices. The most common applications are in the 100 to 200 µm diameter range.

The dry powder is often free-flowing

The most common spray dryers are called single effect as there is only one

drying air on the top of the drying. In most cases the air is blown in co-current of

the sprayed liquid. The powders obtained with such type of dryers are fine with a

lot of dusts and a poor flowability. In order to reduce the dusts and increase the

flowability of the powders, there is since over 20 years a new generation of spray

dryers called multiple effect spray dryers. Instead of drying the liquid in one

stage, the drying is done through two steps: one at the top (as per single effect)

and one or an integrated static bed at the bottom of the chamber.

The fine powders generated by the first stage drying can be recycled in

continuous flow either at the top of the chamber (around the sprayed liquid) or at

the bottom inside the integrated fluidized bed. The drying of the powder can be

finalized on an external vibrating fluidized bed. The hot drying gas can be passed

as a co-current or counter-current flow to the atomiser direction. The co-current

flow enables the particles to have a lower residence time within the system and

the particle separator (typically a cyclone device) operates more efficiently. The

counter-current flow method enables a greater residence time of the particles in

the chamber and usually is paired with a fluidized bed system.


30

2.2.2 BFD and Description

Figure 2.4 Block Flow Diagram Vanillin Plant from Lignin

Lignin Extraction

(LignoBoost)Lignin Oxidation Filtration Drying

Black Liquor

NaOH

Vanillin +

OthersVanillin

Solution

Powdered

Vanillin

VANILLIN PLANT FROM LIGNIN

BLOCK FLOW DIAGRAM

Drawn By :

Checked By :

Revised By :

Darwing No. :

Date :

Date :

Without Scale A4

Note :

H2SO4

O2, N2 (50%,50%)

Lignin

CO2

Waste Liquor


31

Two main process in Vanillin Plant from Lignin is lignin extraction from

black liquor and vanillin oxidation from lignin itself. From this BFD the raw

material, which is black liquor is treated with acid. lignin is precipitated by

acidification (the preferred acid is CO2) and filtered. Instead of washing lignin

immediately after filtration, as in traditional processes, the filter cake is re-

dispersed and acidified (using H2SO4). The resulting slurry is then filtered and

washed by means of displacement washing.

After the slurry is filtered, the next process is blending with NaOH to

make a base condition of solution before entering bubble column reactor. In

bubble column reactor there will be oxidation reaction between lignin and oxygen.

It will result the vanillin solution and the other compounds. To get vanillin, this

solution must be separated using ultrafiltration, so the other compounds can be

impeded at filter, and the filtrate contains only vanillin. The vanillin solution from

ultrafiltration must be dried using spray dryer before it will be packed and

distributed.


32

2.2.3 PFD and Description

Black LiquorFrom pulp ind

CO2

H2SO4

P-109

P-107

PF-102

Water

NaOH

O2 and N2

P-104

Others

PowderVanillin

Air

Air

Water

1 2

3

4

6

8

7

9

11

10

13

14

P-101S-101

P-102V-101

F-101

P-103

PF-101

P-110

V-102

P-111 V-103

F-101

H-101

CS-101

H-102

UF-101

SD-101

P-101Black Liquor Pump

S-101BL Storage

P-102BL Pump

V-101BL Solid Treatment Vessel

P-103Slurry Pump

PF-101Plate & Frame Filter

P-104Slurry Pump

V-102Acidification Vessel

P-105Slurry Pump

P-106Slurry Pump

P-107Filtrate Pump


SR-101Crusher

P-108Water Pump

V-103Lignin Solution Vessel

P-109H2SO4 Solution Pump

H-101Heat Exchanger

C-101O2 and N2 Compressor

CS-101Oxidation Reactor

UF-101Membrane Ultrafiltration

F-102Air Blower

H-102Heat Exchanger

SD-101Spray Dryer

N2

Steam

18

27

29

5

P-108

P-106

Water

P-107

21

16

22

23

H-103

B-101

P-111NaOH Pump

H-103Heat Exchanger

B-103Steam Reboiler

19

24

25

26

28

Alkali Sulfat +Liq Acid

Lean Liquor

12


PROCESS FLOW DIAGRAM

Drawn By :

Checked By

Revised By :

Drawing No :

Date :

Date :

Without Scale A4

Notes :

Group 6

P-105

C-101

C-102

15

17

20

30

V-104

Figure 2.5 Process Flow Diagram Vanillin Plant from Lignin


33

The main process of this plant consists of LignoBoost process which is the

lignin separation process from black liquor, and the core of this plant is vanillin

oxidation from lignin extract from LignoBoost process. The LignoBoost process

is started from black liquor solid separation from black liquor in V-101 until the

filtration process of black liquor solid so the lignin is separated from black liquor

solid. Otherwise the vanillin oxidation process is started while solid lignin

resulted by filtration F-102 entering the blending storage V-103 and NaOH is also

added in that storage, oxidation in bubble column reactor, ultrafiltration, until

drying process of vanillin to be vanillin powder in spray dryer.

From the PFD it can be seen that the black liquor from PT Riau Andalan

Pulp and Paper flowing through the pipe and pumped by P-101 pump to the black

liquor storage S-101. And then the black liquor is kept until the batch is started.

The black liquor than is pumped through P-102 pump to be precipitated in black

liquor treatment vessel V-101, CO2 is added to the storage. The slurry from V-101

is pumped to press chamber filter (Plate and frame) PF-101, and water is pumped

by P-108 as washing eluent in filtration. As the result, solid black liquor is

impeded above the filter as a cake. Then cake is brought using conveyor C-101 to

Acidification vessel V-102 to be re-dispersed so the lignin can be extracted. It

needs H2SO4 as an acid liquid at pH 4 to extract that lignin. When the filter cake

is re-dispersed in a liquid, at pH level and temperature values approximately equal

to those of the final washing liquor, the concentration gradients during the

washing stage will be low. The change in the pH level, most of the change in ionic

strength and any change in lignin solubility will then take place in the slurry, and

not in the filter cake or in the filter medium during washing. From V-102 the

extract is pumped by P-107 to press chamber filter (Plate and frame) PF-102, and

water is pumped by P-110 as washing eluent in filtration.

The lignin is in the cake then is brought to blending storage V-103 with

NaOH by conveyor C-102. In blending storage lignin is dissolved in NaOH before

it is added to bubble column reactor. NaOH will give a base condition as the

optimum condition in this reaction. Before entering bubble column reactor, the

lignin solution is pumped by P-105 pump. During the process, the lignin solution

is heated to increase the temperature through the heat exchanger HE-101, the heat


34

exchanger agent is steam from boiler B-101 at 220oC. The output temperature of

lignin slurry is 170oC and then it enter the bubble column reactor CS-101. The

operation condition of bubble column reactor itself is 170oC and 10 bar pressure.

In BCR lignin is reacted with O2 resulting vanillin and other compounds. The

reaction can be explained below.

Lignin oxidation : 0.5 L + 1.56 O2 V + 114 X

Vanillin oxidation : V + O2 D

Stoichiometry 1 Conversion 70%

Lignin Oxidation : 0.5 L + 1.56 O2 --> V + 114 X

Initial (mol) 2350.242 10781.25

Change (mol) -1645.17 -7332.75 4700.483

Remaining

(mol) 705.0725 3448.496 4700.483

Stoichiometry 2

Vanilin Oxidation : V + O2 --> Product

Initial (mol) 4700.483 3448.496

Change (mol) -3290.34 -3290.34 3290.338

Remaining

(mol) 1410.145 158.1582 3290.338

massa 500592.048 gram

0.50059205 ton

500.592048 kg

( )

( )

(

)

(

(

) )

(

)

(

(

) )

Where :

- A is Lignin

- B is Oxygen

- C is Vanillin

- D is Vanillin Acid Product


35

Rate Law :

(

)

(

)

The product from CS-101 is pumped using P-106 through HE-103 to

Ultrafiltration membrane UF-101. The filtrate then pumped to spray dryer SD-101

(80oC). In SD-101 the liquid vanillin is powdered with hot air after passing the

HE-102 at 120oC. Vanillin powder then is brought to packing building to be

packaged. The cake from UF-101 is pumped to waste storage.


36

CHAPTER 3

MASS AND ENERGY BALANCE

3.1 Mass Balance

3.1.1 Overall Mass Balance

Overall mass balance in this system is explained in table 3.1 below :

Table. 3.1 Mass Balance in Entire Process

OVERALL Input (ton) Output (ton)

FEED

Black Liquor 111.17 0

CO2 1.10 0

Water 14.54 22.98

H2SO4 0.88 0

NaOH 6.67 0

O2 0.16 0

N2 0.16 0.16

Waste

Lean liquor - 68.92

Liquid acid - 25.48

Alkali sulfat - 5.29

Filtrate cake - 10.14

Hot air 1.02 2.22

PRODUCT

Vanillin - 0.50

TOTAL 135.70 135.70

While the composition of the black liquor and its content found in Figure 3.2

Table. 3.2 Black Liquor Composition

Black Liquor Composition Total mass (ton)

Lignin (4.5%) 5

Water (8%) 8.89

Lean liquor (87,5%) 97.27


37

3.1.2 Mass Balance Process Units

Primary Process Description and Mass Balance in Every Process Units are

explained in the table below :

Table. 3.3 Mass Balance in Storage

STORAGE Input 1

(ton)

Output 2

(ton)

Lignin Alkali 10.01 10.01

Water 8.89 8.89

Lean liquor 92.27 92.27

TOTAL 111.17 111.17

Table. 3.4 Mass Balance in Acidification Process

ACIDIFICATION I Input 2

(ton)

Input 3

(ton)

Output 4

(ton)

Lignin Alkali 10.01 0 10.01

Water 8.89 0 8.44

Lean Liquor 92.27 0 92.27

CO2 0 1.10 0

Liquid Acid 0 0 1.55

111.17 1.10 112.27

TOTAL 112.27 112.27

Table. 3.5 Mass Balance in Filtration Process

FILTRATION I Input 4

(ton)

Input 5

(ton)

Output 6

(ton)

Output 7

(ton)

Lignin Alkali 10.01 0 10.01 0

Water 8.44 11.12 0 19.56

Lean Liquor 92.27 0 0 68.92

Liquid Acid 1.55 0 0 1.55

lean liquor solid 0 0 23.35 0

112.27 11.12 33.35 90.03

TOTAL 123.38 123.38


38

Table. 3.6 Mass Balance in Acidification Process

ACIDIFICATION II Input6

(ton)

Input 8

(ton)

Output 9

(ton)

Lignin Alkali 10.01 0 0

Lean liquor solid 23.35

0

H2SO4 0 0.88 0

Lignin 0 0 5

Alkali Sulfat 0 0 5.29

Liquid acid 0 0 23.93

33.35 0.88 34.23

TOTAL 34.23 34.23

Table. 3.7 Mass Balance in Filtration Process

FILTRATON II Input 9

(ton)

Input 10

(ton)

Output 11

(ton)

Output 12

(ton)

Lignin 5

5 0

Alkali sulfat 5.29 0 0 5.29

Liquid acid 23.93 0 0 23.93

Water 0 3.42 0 3.42

34.23 3.42 5.00 32.65

TOTAL 37.65 37.65

Table. 3.8 Mass Balance in Blending Process

BLENDING Input 11

(ton)

Input 13

(ton)

Output 14

(ton)

Lignin 5 0 0

NaOH 0 6.67 0

Lignin slurry 0 0 11.67

TOTAL 11.67 11.67


39

Table. 3.9 Mass Balance in Storage Lignin slurry

STORAGE Input 13

(ton)

Input 14

(ton)

Output 15

(ton)

Lignin 5 0 0

NaOH 0 6.67 0


TOTAL 11.67 11.67

Table. 3.10 Mass Balance in Oxidation Process

REACTOR

OXIDATION

Input 15

(ton)

Input 16

(ton)

Output 18

(ton)

Output 19

(ton)

Lignin slurry 11.67 0 0 0

N2 0 0.16 0 0.16

O2 0 0.16 0 0

Alkali Ligin Slurry 0 0 5.36 0

Water 0 0 1.20 0

Vanillin 0 0 0.50 0

Others 0 0 4.78 0

11.67 0.33 11.84 0.16

TOTAL 12.00 12.00

Table. 3.11 Mass Balance in Ultrafiltration Process

ULTRAFILTRATION

Input 18

(ton)

Output 20

(ton)

Output 21

(ton)

Vanillin 0.50 0.50 0

Alkali Lignin Slurry 5.36 0 0

water 1.20 1.20 0

Others 4.78 0 0

Filtrate Cake 0 0 10.14

11.84 1.70 10.14

TOTAL 11.84 11.84


40

Table. 3.12 Mass Balance in Drying Process

DRYING Input 20

(ton)

Input 26

(ton)

Output 28

(ton)

Output 29

(ton)

Vanillin 0.50 0 0 0

water 1.20 0 0 0

Hot Air 0 1.02 2.22 0

Vanillin Powder 0 0 0 0.50

1.70 1.02 2.22 0.50

TOTAL 2.72 2.72

3.2 Energy Balance

Table. 3.3.1 Mass Balance in Storage

STORAGE Input 1 (ton) Output 2(ton) Energy In

(Joule)

Energy Out

(Joule)

Lignin Alkali 10.01 10.01 0 0

Water 8.89 8.89 0 0

Lean liquor 92.27 92.27 0 0

TOTAL 111.17 111.17 0 0

Table. 3.3.2 Mass Balance in Acidification Process

ACIDIFICATION I Input 2 (ton) Input 3

(ton) Output 4 (ton) Energy In (Joule)

Energy Out

(Joule)

Lignin Alkali 10.01 0 10.01 0.00 0.00

Water 8.89 0 8.44 141.31 134.15

Lean Liquor 92.27 0 92.27 0.00 0.00

CO2 0 1.10 0 27.64

Liquid Acid 0 0 1.55

34.79

111.17 1.10 112.27

TOTAL 112.27 112.27 168.94 168.94


41

Table. 3.3.3 Mass Balance in Filtration Process

FILTRATION I Input 4

(ton)

Input 5

(ton)

Output 6

(ton) Output 7 (ton)

Energy In

(Joule)

Energy

Out

(Joule)

Lignin Alkali 10.01 0 10.01 0 0 0

Water 8.44 11.12 0 19.56 0 0

Lean Liquor 92.27 0 0 68.92 0 0

Liquid Acid 1.55 0 0 1.55 0 0

lean liquor solid 0 0 23.35 0 - -

TOTAL 112.27 11.12 33.35 90.03 0 0

TOTAL 123.38 123.38 0 0

Table. 3.3.4 Mass Balance in Acidification Process

ACIDIFICATION II Input6 (ton) Input 8

(ton)

Output 9

(ton)

Energy In

(Joule)

Energy Out

(Joule)

Lignin Alkali 10.01 0 0 49689.61 -

Lean liquor solid 23.35

0 - -

H2SO4 0 0.88 0 138.50 -

Lignin 0 0 5

24844.81

Alkali Sulfat 0 0 5.29

24494.23

Liquid acid 0 0 23.93

489.08

TOTAL 33.35 0.88 34.23 49828.12 49828.12

TOTAL 34.23 34.23 49828.12 49828.12


42

Table. 3.3.5 Mass Balance in Filtration Process

FILTRATON II Input 9

(ton)

Input 10

(ton)

Output 11

(ton)

Output 12

(ton)

Energy In

(Joule)

Energy Out

(Joule)

Lignin 5

5 0 0 0

Alkali sulfat 5.29 0 0 5.29 0 0

Liquid acid 23.93 0 0 23.93 0 0

Water 0 3.42 0 3.42 0 0

34.23 3.42 5.00 32.65 0 0

TOTAL 37.65 37.65

Table. 3.3.6 Mass Balance in Blending Process

BLENDING Input 11 (ton) Input 13

(ton)

Output 14

(ton)

Energy In

(Joule)

Energy Out

(Joule)

Lignin 5 0 0 0

NaOH 0 6.67 0 0


0

TOTAL 11.67 11.67 0

Table. 3.3.7 Mass Balance in Storage Lignin Slurry

STORAGE Input 11 (ton) Input 13

(ton)

Output 14

(ton)

Energy In

(Joule)

Energy Out

(Joule)

Lignin 5 0 0 0

NaOH 0 6.67 0 0


0

TOTAL 11.67 11.67 0


43

Table. 3.3.8 Mass Balance in Oxidation Process

REACTOR

OXIDATION

Input 15

(ton)

Input 16

(ton)

Output

18 (ton)

Output

19 (ton)

Energy In

(Joule)

Energy Out

(Joule)

Lignin slurry 11.67 0 0 0 57971.22 0

N2 0 0.16 0 0.16 0 0

O2 0 0.16 0 0 0 0

Alkali Ligin

Slurry 0 0 5.36 0

0.00 0

Water 0 0 1.20

Vanillin 0 0 0.50 0 0

Others 0 0 4.78 0 0

Total 11.67 0.33 11.84 0.16 57971.22 2811317971.22

TOTAL 12 12 57971.22 2811317971.22

Q masuk tambahan : 2811260000 J

Table. 3.3.9 Mass Balance in Ultrafiltration Process

ULTRAFILTRATION

Input 18 (ton)

Output 20

(ton)

Output 21

(ton)

Energy In

(Joule)

Energy

Out

(Joule)

Vanillin 0.50 0.50 0 0 0

Water 5.36 0 0 0 0

Alkali Lignin Slurry 1.20 1.20 0 0 0

Others 4.78 0 0 0 0

Filtrate Cake 0 0 10.14 0 0

11.84 1.70 10.14 0 0

TOTAL 11.84 11.84


44

Table. 3.3.10 Mass Balance in Drying Process

DRYING Input 20

(ton)

Input 26

(ton)

Output 28

(ton)

Output 29

(ton)

Energy In

(Joule)

Energy Out

(Joule)

Vanillin 0.50 0 0 0 - 4445.67

Hot Air 1.20 0 0 0 142800

Water 0 1.02 2.22 0 286850.67

Vanillin

Powder

0 0 0 0.50 0.00 0.00

1.70 1.02 2.22 0.50 142800 291296.34

TOTAL 2.72 2.72

Q masuk tambahan dari steam : 148496.34 J

So, Total of the heat steam that we need is = 2811408496.34 = 2811.41 MJ


45

CHAPTER 4

UTILITIES

4.1 Water Utility

Water availability system in this vanillin plant is really needed to support

the whole plant production. The water utility in this plant is needed as processes

water, water for equipment washing, domestic water availability and fire

extinguishing water. The water source design based on the water collection,

processing system efficiency and economical factor. The explanation about this

water utility consist as follows :

4.1.1 Water Utility Classification

4.1.1.1 Process Water

Process water that used in this plant is used to solute NaOH that will enter

oxidation reactor and for washer in filtration. In the whole process for this plant,

water is not too needed because water component in the main raw material (black

liquor) is 26% and the most of others materials is liquid solution. The water

process needs in this plant reach 123,40 m3 per day. The details about the needs of

water describes as follows :

Table 4.1 Total Process Water Needs in Plant

Unit Water (kg)

Filtration 1 11120

Filtration 2 3420

Blending 730

Total 15270

4.1.1.2 Domestic Water

This water is used to fulfill water needs for staff and other employers.

Domestic water include toilet facilities, drinking water, water for watering

gardens and many more. Assuming the total domestic water everyone is 100

litre/day. So, total water for domestic water if there is 100 persons in this plant is

10.000 litre/day.


46

4.1.1.3 Fire Extinguishing Water

Fire Extinguishing Water is used to extinguish fire if one day there is fire.

This water is reserved to be used anytime. The firefighting water used was water with

the low specs, but has under gone treatment first. The amount of water required for fire is

assumed to10,000 kg/day.

4.1.1.4 Total Water Requirements

Total water requirements needed for this plant per day covers the water needed

for process water, cooling water, water heater, boiler feed water, domestic water and fire

water. Total water requirement is shown in the table 5.1 below:

Table 4.2 Total Water Needs in Plant

Using water Total (Kg/day)

Processing Water 15270

Domestic water 10000

Fire Extinguishing Water 1000

Total 26270

4.1.1.5 Water Sources

Water supply to the plant will be taken from PT. Riau Andalan industrial area. PT

Riau Andalan independently manage all water providers to the needs of industries that

exist within the industry. Water supplied by PT Riau Andalan is considered clean enough

and qualify for use as water for industrial plants. So in the factory there is no clean water

management facilities further.

4.2 Electric Utility

As the plant in general, to run the equipment contained in the plant Vanillin,

energy required is not small. Equipment that requires a supply of energy, among others:

Pump

Agitator Mixing Tank

Electricity need for vanillin production in this vanillin plant can be seen in

the following table.


47

Table 4.3 Total Electricity Needs in Plant

Item No. Process unit Kwh/ day Kwh/year

V-101 Agitator CO2 precipitation tank 36.32 10897

V-102 Agitator H2SO4 precipitation tank 1.58 474.83

V-103 Agitator lignin slurry tank 0.09 26.68

P-101 Black liquor pump 19.31 5792.45

P-102 Black liquor pump 258.99 77696.04

P-103 CO2 precipitation pump 56.18 16854.27

P-104 Slurry pump 2.89 865.74

P-105 Slurry pump 0.53 157.70

P-106 Slurry pump 3.86 1157.32

P-107 Slurry pump 0.18 53.46

P-108 Water pump 14.19 258.08

P-109 H2SO4 precipitation pump 0.28 84.69

P-110 Water pump 10.38 3113.53

P-111 NaOH pump 1.78 533.65

C-101 Alkali lignin cake conveyor 7.44 2232

C-102 Black liquor solid conveyor 7.44 2232

C-103 Lignin solid conveyor 5.95 1785

C-104 Vanillin conveyor 5.95 1785

TOTAL 433.34 125999.44


48

Electricity need at vanillin plant is AC (accuired current) power type.

Total electricity needs for processes of this plant is equal to 433.34 kWh/day.

While the need support for lighting and other assumed 30% of the total energy is

130 kWh/day. So the total electricity need of vanillin plant is 125999.44

kWh/year.

Electrical power is largely used for two purposes primary. The first

necessity is requiring electrical power needs the production process. The second

purpose is to use electrical power production support facilities. Electricity used for

support facilities for the needs of lighting and air-conditioning (AC) in the office,

laboratories, workshops, as well as the control room, air supply (tap and clean),

water supply (and the net), and the sewage treatment plant.

4.3 Steam Utility

In this vanillin plant, steam utility is needed for heating the reactor through

the jacket. Reaction temperature needed in that process is 170oC. Based on

calculation, it is obtained that heat needed for reactor is 253.01 MJ per day.

It is assumed that steam needed is provided from diesel as fuels. Assuming

that efficiency from boiler is 40%. So, the diesel as fuels to produce steam in this

vanillin plant is :

m = 303 litre per day


49

BAB 5

SIZING

5.1 Vessel

5.1.1 Black Liquor Storage Tank (S-101)

STORAGE TANK

Identification: Item Black Liquor Storage Tank

Item no. S-101

No. required 3

Function: Storage black liquor to keep it from microorganism and algae

Operation: Discrete

Material

handled: Black Liquor

Composition

(%):

Black Liquor 100

Design data Capacity (kg) 333500

Feed quantity (m3/h) 326.57

Operating temperature (K) 333

Operating pressure (psi) 14.70

Storage Tank Specification

Type

Flat-bottomed cylindrical vessel

Material of construction Stainless steel 316

Diameter (m)

7.16

Height (m)

9.55

Thickness of shell (cm) 2.97

Thickness of Roof (cm) 2.97

Controls: S-101 for controlling Black liquor solution


50

5.1.2 Acidification Tank (V-101)

MIXER TANK

Identification: Item Mixer Tank

Item no. V-101

No. required 5

Function: To precipitation black liquor with CO2

Operation: Discrete

Material handled: Black Liquor slurry

Composition (%):

Black Liquor

Slurry

100




Residence time (h) 1


Mixer Tank Specification

Type

Flat-bottom cylindrical vessel


Diameter(m)

2.90

Height (m)

3.87


Thickness of roof (cm) 2.12

Impeller Design

Type Flow turbine with 4 blades

Diameter (m) 1.16

Agitator space from based (m) 0.55

Blade width (m) 0.15

Impeller speed (rpm) 60

Power (kWh) 0.81

Controls: V-101 for precipitation black liquor slurry


51

5.1.3 Acidification Tank (V-102)

MIXER TANK


Item no. V-102 (A)

No. required 1

Function: Acidification process of black liquor slurry

Operation: Discrete


Composition (%):

Black Liquor

Slurry

100




Residence time (h) 0.5



Type



Diameter(m)

2.30

Height (m)

3.06



Impeller Design


Diameter (m) 0.92




Power (kWh) 0.23



52

MIXER TANK


Item no. V-102 (B)

No. required 1

Function: Acidification process of black liquor slurry

Operation: Discrete


Composition (%):

Black Liquor

Slurry

100







Type



Diameter(m)

2.01

Height (m)

2.68



Impeller Design


Diameter (m) 0.80

Agitator space from based

(m) 0.38



Power (kWh) 0.12



53

5.1.4 Blending Tank (V-103)

MIXER TANK


Item no. V-103

No. required 1

Function: To make lignin slurry

Operation: Discrete

Material handled: Lignin slurry

Composition (%):

Lignin Slurry 100







Type


Material of construction Plate steels SA-283 grade C

Diameter(m)

4.53

Height (m)

6.04



Impeller Design


Diameter (m) 1.81




Power (kWh) 8.8

Controls: V-103 for make lignin slurry


54

5.1.5 Lignin Slurry Storage (S-102)

STORAGE TANK

Identification: Item Lignin Slurry Storage Tank

Item no. S-102

No. required 1

Function: Storage lignin slurry before enter to bubble column reactor

Operation: Discrete

Material handled: Black Liquor

Composition (%):

Lignin Slurry 100






Type



Diameter (m)

1.93

Height (m)

2.58



Controls: S-102 for controlling lignin slurry


55

5.1.6 Waste Storage (S-103)

STORAGE TANK

Identification: Item Waste Storage Tank

Item no. S-103

No. required 2

Function: Waste storage from the process

Operation: Discrete

Material handled: Waste from process

Composition (%):

Waste 100






Type


Material of construction Carbon steel

Diameter (m)

7.07

Height (m)

9.43



Controls: S-103 for controlling waste from process


56

5.1.7 H2SO4 Storage (S-104)

STORAGE TANK

Identification: Item H2SO4 Storage Tank

Item no. S-104

No. required 1

Function: Storage H2SO4 to keep it before enter to process

Operation: Discrete

Material handled: H2SO4

Composition (%):

H2SO4 100

Design data Capacity (kg) 47273.63





Type



Diameter (m)

3.07

Height (m)

4.09



Controls: S-103 for controlling H2SO4 from process


57

5.1.8 NaOH Storage (S-105)

STORAGE TANK

Identification: Item NaOH Storage Tank

Item no. S-105

No. required 1

Function: Storage NaOH to keep it before enter to process

Operation: Discrete

Material handled: NaOH

Composition (%):

NaOH 100






Type



Diameter (m)

5.75

Height (m)

7.67



Controls: S-105 for controlling NaOH


58

5.2 Filtration

5.2.1 Plate and Frame Filter (PF-101)

Lignin Alkali Press Filter

Identification: Item Lignin Press Filter

Item no. PF-101

No. required 4

Function: To get lignin alkali solid and lean liquor solid, separate it

from lean liquor, liquid acid, and water.

Operation: batch


Design data: Operating temperature (K) 303

Operating pressure (Pa) 7 x 105

Type

Vertical Plate

Airblow (VPA)


Effective filtration Area

(m2)

345

Filtration area with safety

factor 20% (m2)

414

Filter chamber size (m)

2.03 x 2.03

Number of chambers 50

L (m) 15.6

W (m) 4.25

H (m) 4.58

Weight empty (ton) 80

Total press filter required (item) 4

Total plates required 200


59

5.2.2 Plate and Frame Filter (PF-102)

Lignin Press Filter

Identification: Item Lignin Press Filter

Item no. PF-102

No. required 1

Function: To get solid lignin and separate it from alkali suphate, liquid

acid, and water.

Operation: batch


Design data: Operating temperature (K) 303

Operating pressure (Pa) 7 x 105

Type

Vertical Plate

Airblow (VPA)



(m2)

40.06


factor 20% (m2)

48.08

Filter chamber size (m)

1.5 x 1.5

Number of chambers 24

L (m) 8.5

W (m) 3.8

H (m) 3.16

Weight empty (ton) 27.5

Total press filter required (item) 1

Total plates required 21


60

5.3 Pump

5.3.1 Black Liquor Pump (P-101)

Function : Pumping black liquor to acidification tank I

Type : Centrifugal pump

Number of Unit : 1 unit

No. Specification

1 Scope Double end-Vertical screw pump

2 Service condition Continuous process

3 Operating condition

Capacity (ton/h) 66.77

Suction pressure (Pa) 100,000

Power (kWh) 0.32

4 Liquid Properties

Liquid to be handled Black liqour

Viscosity (cp) 5.091

Temperature of liquid at inlet

(°C)

60

5 Material Stainles steel

5.3.2 Black Liquor Acidification pump (P-102)

Function : Pumping black liquor slurry from acidification tank to press

filter I

Type : Centrifugal pump


No. Specification

1 Scope Centrifugal pump

2 Service condition Continuous process



61



Power (kWh) 2.36

4 Liquid Properties


Viscosity (cp) 1.70


(°C)

60


5.3.3 Lignin Acidification Pump (P-103)

Function : Pumping sludge from acidification tank to filter press II

Type : Piston pump


No. Specification

1 Scope Screw pump

2 Service condition Batch process




Power (kWh) 2.56

4 Liquid Properties



Temperature of liquid at inlet 60


62

(°C)


5.3.4 Lignin Solution Pump (P-104)

Function : Pumping lignin slurry (lignin+water) from mixing tank to

storage

Type : Screw Pump


No. Specification

1 Scope Screw pump





Power (kWh) 0.07

4 Liquid Properties

Liquid to be handled Lignin Solution



(°C)

60



63

5.3.5 Lignin Solution Pump (P-105)

Function : Pumping lignin slurry (lignin+water) from storage to BCR

Type : Screw Pump


No. Specification

1 Scope Screw pump





Power (kWh) 0.12

4 Liquid Properties

Liquid to be handled Lignin Solution



(°C)

60


5.3.6 Vanillin Slurry Pump (P-106)

Function : Pumping Vanilin solution from BCR to Ultrafikasi

Type : Screw pump


No. Specification

1 Scope Screw pump

2 Service condition Continous process




64


Power (kWh) 0.32

4 Liquid Properties

Liquid to be handled Vanillin Solution

Viscosity (cp) 5.13


(°C)

60


5.3.7 Vanillin Solution Pump (P-107)

Function : Pumping Vanillin Solution to Spray Dryer

Type : Screw pump


No. Specification

1 Scope Screw pump

2 Service condition Continous process




Power (kWh) 0.03

4 Liquid Properties

Liquid to be handled Vanillin Slurry

Viscosity (cp) 1.65


(°C)

60



65

5.3.8 Water Pump (P-109)

Function : Pumping water from the reservoir to filtration Plate and Press

I

Type : Piston Pump


No. Specification

1 Scope Piston Pump





Power (kWh) 0.26

4 Liquid Properties

Liquid to be handled Water

Viscosity (cp) 1.65


(°C)

60

5 Material Carbon steel


66

5.4 Conveyor

Conveyor I and II

Function :To transfer filtrate from filtrasi to acidification II.

Type : horizontal belt conveyor

Material : Stainless steel

Operating Condition : - Temperature (T) = 300 C

- Pressure (P) = 1 atm

Conveyor I and II

Rate of material 6.67 ton/10 min 40.18 ton/h

Looseness factor 52.23 ton/h

Conveyor Capacity 54 ton/h

Spesifikasi

Width of Belt 18.00 inch 0.46 m

Area 0.02 m2

Normal Belt Speed 76.00 m/min 1.27 m/s

Maximum Belt Speed 107.00 m/min 1.78 m/s

Power 2.50 hp 1.86 kW

7.44 kWh/day

2,232.00 kWh/year

Number of Conveyor 2 pieces


67

Conveyor III

Function : Transfer of Cake of Filtration to mixer tank.

Type : horizontal conveyor belt

Material : Stainless steel

Operating conditions : Temperature (T) = 300C

Pressure (P) = 1 atm

5.5 Bubble Column Reactor

Equipment

Code CS-101

Operation Mode Batch

Operation

Temperature 170 oC

Pressure 10 Bar

Volume 25.52 m3

Retention Time 2 hours

Dimension

Height 4.48 M

Diameter 2.69 M

Thickness 6,44 mM

Multiple Ring Sparger

Diameter 3 mM

Number of

Holes 15

Material Stainless Steel 316


68

5.6 Ultrafiltration

Vanillin Solution Ultrafilter

Identification: Item Vanillin solution ultrafilter

Item no. UF-101

No. required 6

Function: Separate vanillin solution from lignin alkali solution after

oxidation

Operation: Continuous

Material handled: Lignin alkali and other by product

Design data: Operating temperature (oK) 353

Operating pressure (Psi) 30

Type

Hollow fiber membrane

Material of construction

Polyvinylidenefluoride

PVDF (for filter

membrane)


(m2)


factor (m2)

Available filter area (m2)

130

Number of fiber in each module 10000

L (m) 2.36

W (m) 0.34

D (m) 0.23

Membrane cut-off rating (kDa) 1

Total equipment required (item) 6


69

5.7 Spray Dryer

SPRAY DRYER

Identification: Item Spray Dryer

Item no. SD-101

No. required 2 (1 active, 1 stand by)

Function: Make vanillin powder from vanillin solution

Operation: Batch

Material handled: Vanillin Solution

Composition (%):

Vanillin solution 100

Design Data: Type Closed spray dryer

Material of construction Stainless steel

Atomizer Centrifugal Disc (Vane)

Volume (m3) 5.52

Height cylindrical (m) 1.47

Column Diameter (m) 2.45

Thickness (m) 0.0025

Volume Cone (m3) 4.05

Cone Angle (o) 20.57

Max Temp Operating (oC) 180

Max Press Operating (psi) 600

Power (hp) 116


70

5.8 Heat Exchanger

5.8.1 Heat Exchanger HE-101

5.8.2 Heat Exchanger HE-102

Tipe Shell and Tube

Jenis Countercurrent Floating Head

Heat transfer area, m2 273.50

Heat transfer coefficient, W/m2 0C 900

Agen pemanas Superheated steam 190oC

Laju alir pemanas, kg/hari 32000

Jumlah tube 218

Shell Side Tube Side

Material SS 304 SS304

Densitas, kg/m3 0.521 1060

Cp, 2.09 2.08

Temperature in, 0C 190 60

Temperature out, 0C 190 170

Tipe Shell and Tube

Jenis Countercurrent Floating Head

Heat transfer area, m2 202

Heat transfer coefficient, W/m2 0C 900

Agen pemanas Superheated steam 190oC

Laju alir pemanas, kg/hari 32000

Jumlah tube 161

Shell Side Tube Side

Material SS 304 SS304

Densitas, kg/m3 0.521 1.02

Cp, 2.09 1.00

Temperature in, 0C 190 25

Temperature out, 0C 190 120


71

CHAPTER 6

PROCESS CONTROL

6.1 Process Control Instrumentation

Process control system is absolutely necessary in a factory to control all

the variables such as temperature, pressure, level, and more so the process runs.

Some process control objective to be achieved are as follows:

a) Avoiding dangerous circumstances that may occur in the operation (safety)

b) Maintaining the quality of the resulting product

c) Keeping the equipment is working in a range of operating conditions

d) Keeping operations and various byproducts produced run in accordance with

environmental standards

e) Monitor and diagnose the operation

F) Keeping operations running optimally so keep the plant gains

At this plant a variety of variables controlled by using a variety of instruments that

are available at the P & ID. Here is an explanation of the control system in the

main equipment.

6.2 Process Control on Raw Material Storage Tank

Black liquor storage tank is connected to the acidification vessel. Yield

products from this vessel will greatly depend on the composition of the input to

the output reactor or storage tank. Flow rate control system of storage tanks

needed for the flow rate from the storage tank maintained.

The control system used to control the flow rate is bypass control system.

The process of controlling the flow rate of the tank using orifice meter as a sensor

to measure the flow rate output before entering the control valve. Flow rate

measurements made of the difference in pressure at P1 and P2.

The output of the orifice meter is then analyzed by the controller based on

set point. Then the controller controls the flow rate of the control valve (open

when the flow rate is too small and close when the flow rate is too large) to adjust

the flow rate to set point.


72

6.3 Process Control on Heat Exchanger

Process control in the heat exchanger also has a similar system of controls

for each heat exchanger. Controlled variable is the temperature of the main

product output heat exchanger. The parameters are controlled steam flow rate or

cooling water into the heat exchanger.

Temperature is one of the important variables to be controlled. Heat

exchangers are the main components that require temperature control. Heat

exchanger serves to exchange heat between the main product with steam / cooling

water. Controlling the temperature of the product is required to be maintained in

accordance with the main design.

The control system used for temperature control are feed back control

system. Process control using a thermocouple as a temperature sensor on the

output of main products in heat exchangers.

The output of the thermocouple is then analyzed by the controller based on

set point. Then the controller controls the flow rate of the flow control valve on

the pipe steam / cooling water before it enters the heat exchanger. Control valve

controlling the flow rate of steam / cooling water to adjust the flow rate of steam /

cooling water with a temperature set point to achieve the appropriate design.

6.4 Process Control on Reboiler

Process control more towards the boiler temperature control in steam

output. Boiler using diesel fuel to vaporize water into steam. Controlled variable

is the temperature of the steam output of the boiler. The parameters were

controlled flow rate of diesel fuel and water into the boiler. And also controlling

the pressure in boiler so it can result the high steam pressure needed.

6.5 Process Control on Black Liquor Treatment Vessel

Process control in black liquor treatment vessel is a control process that

involves more than one variable that needs to be controlled. Variables that are

controlled from the oxidation reactor is the flow rate, height, composition, and

pressure.

Height

The height is a variable that must be maintained during the lignin

separation from black liquor. The height of the fluid is maintained in order


73

not higher than the feed inlet and not too low. Sensors are deployed using

a floating sensor surface fluid in the vessel. The parameters are controlled

liquid flow rate at the outlet.

Pressure

The pressure in the black liquor treatment vessel is kept equal to or

slightly above atmospheric pressure. Excessive pressure can affect the

quality of the product and can also be dangerous when the reactor

exploded due to excess pressure. To prevent excess pressure of the reactor

is equipped with a relief valve to release the pressure in the reactor.

Controlled variable is the pressure inside the reactor. When the pressure

exceeds the set point, then the relief valve on the reactor will open thereby

releasing the pressure in the vessel.

Composition

The composition is a variable that can affect the production yield of the

reactor. The process of composition control over the direction of the

control fluid homogeneity in the vessel. Controlled variable is the

composition of the sample in the vessel. The parameters are speed

controlled agitator. Sensor compositions using gas liquid chromatography

(GLC). When the results of the GLC analysis are deviations from the set

point, the parameters changed by the addition of agitation speed of

stirring.

6.6 Process Control on Acidification Vessel and Lignin Solution Vessel

Process control in acidification and liginin solution vessel is a control

process that involves more than one variable that needs to be controlled. Variables

that are controlled from the oxidation reactor is the flow rate, height, composition,

and pressure.

Height

The height is a variable that must be maintained during the lignin

separation from black liquor. The height of the fluid is maintained in order

not higher than the feed inlet and not too low. Sensors are deployed using

a floating sensor surface fluid in the vessel. The parameters are controlled

liquid flow rate at the outlet.


74

Pressure

The pressure in the acidification vessel is kept equal to or slightly above

atmospheric pressure. Excessive pressure can affect the quality of the

product and can also be dangerous when the vessel exploded due to excess

pressure. To prevent excess pressure of the vessel is equipped with a relief

valve to release the pressure in the vessel. Controlled variable is the

pressure inside the reactor. When the pressure exceeds the set point, then

the relief valve on the reactor will open thereby releasing the pressure in

the vessel.

Composition



control fluid homogeneity in the reactor. Controlled variable is the

composition of the sample in the reactor. The parameters are speed

controlled agitator. Sensor compositions using gas liquid chromatography

(GLC). When the results of the GLC analysis are deviations from the set

point, the parameters changed by the addition of agitation speed of

stirring.

6.7 Process Control on Oxidation Reactor

Process control in the manufacture of vanillin making oxidation reactor is

a control process that involves more than one variable that needs to be controlled.

Variables that are controlled from the oxidation reactor is the input flow rate,

height, composition, pressure and temperature.

Flow rate

The flow rate input is an important variable to be controlled in a reactor.

The flow rate input into the reactor can affect the composition in the

reactor that will also affect the yield of the reactor. In addition flow rate

can also affect the height of the liquid in the reactor. Sensors are used to

measure the flow rate is orificemeter. Flow rate is then controlled by the

controller input based on set point. Control the flow rate by the flow

control valve (FCV).


75

Height

The height is one important variable but often forgotten in BCR tank.

Sensor height is needed in order to know whether the height of the fluid is

sufficiently safe for the agitator to operate. The parameters that are

controlled from the control height is input flow rate into the reactor.

Height sensors are used to using sensors floating in the fluid surface. The

height of the fluid in the reactor is controlled by the controller based on set

point. Control the flow rate by the flow control valve (FCV) on the same

input stream as the flow rate control input.

Composition



control fluid homogeneity in the reactor. Controlled variable is the

composition of the sample in the reactor. The parameter control is speed of

gas O2 through component in BCR. Sensor compositions using gas-liquid

chromatography (GLC). When the results of the GLC analysis are

deviations from the set point, the parameters changed by the addition of

flow rate O2 from gas sparger to BCR.

Pressure

Pressure is an important variable in the reactor. The pressure in the reactor

was kept at pressure of 10 bar above atmospheric pressure, but do not be

too excessive. It is intended that the oxidation of lignin into vanillin could

happen. Pressure changes can occur due to the continuous input reactor

and the reaction in the reactor. Excessive pressure can affect the quality of

the product and can also be dangerous when the reactor exploded because

excess pressure. To prevent excess pressure of the reactor is equipped with

a relief valve to release the pressure in the reactor. Controlled variable is

the pressure inside the reactor. When the pressure exceeds the set point,

then the relief valve on the reactor will open thereby releasing the pressure

in the reactor.


76

Temperature

Temperature is the most variable can change in the reactor. The process of

oxidation reaction produces heat which can change the temperature in the

reactor. The reaction in the reactor must be on guard at 170° C for the

reaction to occur and produce vanillin. To keep the temperature inside the

reactor is used jackets. The temperature sensor used is a thermocouple.

Controlled variable is the temperature in the reactor.

6.8 Process Control on Spray Dryer

Process control in the spray drayer is a control process that involves more

than one variable that needs to be controlled. Variables that are controlled from

the spray dryer is the input flow rate, composition, and pressure.

Flow rate

The flow rate input is an important variable to be controlled in a spray

dryer. The flow rate input can affect timing and composition amount.

Sensors are used to measure the flow rate is orificemeter. Flow rate is then

controlled by the controller input based on set point. Control the flow rate

by the flow control valve (FCV).

Composition

The composition is a variable that can affect the vanillin powder

production of spray dryer. The process of composition control is over the

direction of the contain of vanillin. Controlled variable is the composition

of the sample in the spray dryer. The parameters controlled is rate of

evaporation. Sensor compositions using gas-solid chromatography (GSC).

When the results of the GSC analysis are deviations from the set point, the

parameters changed by the addition of rate of hot air into spray dryer.

Pressure

Pressure is an important variable in the reactor. The pressure in spray

dryer was kept at atmospheric pressure or above atmospheric pressure, but

do not be too excessive. Pressure changes can occur due to the continuous

input to spray dryer. Excessive pressure can affect the quality of the

product and can also be dangerous when the spray dryer exploded because

excess pressure. To prevent excess pressure of the spray dryerr is equipped


77

with a relief valve to release the pressure in the reactor. Controlled

variable is the pressure inside. When the pressure exceeds the set point,

then the relief valve will open thereby releasing the pressure in the spray

dryer.


78

Water

Black Liquor

CO2

P-101

S-101

P-102 P-103

P-108

FT

101FIC

101

LT

101

FT

102

FIC

102

AT

101

AC

101

FT

103FIC

103

PT

101

PIC

101

P-14

FT

104FIC

104

FT

106

FIC

106

V-101

PF-101

To V-102

Lean Liquor

LT

102

S-101BL Storage

P-102BL Pump

V-101BL Solid Treatment

Vessel

F-101CO2 Fan

P-103Slurry Pump

PF-101Plate & Frame

Filter

P-105Water Pump


PIPING AND INSTRUMENTATION DIAGRAM

Drawn By :

Checked By

Revised By :

Drawing No :

Date :

Date :

Without Scale A4

Notes :

Group 6

V-19

Figure 6.1 Piping and Instrumentation Diagram - 1


79

P-107

AT

102

AC

102

PT

102

PIC

102

V-5P-4

FT

105FIC

105

V-102

PF-102

Alkali sulfat

LT

103

From PF-101

H2SO4

P-109

FIC

105

FT

105

NaoH

P-111

FIC

108

FT

108

AC

103

PT

103

PIC

103

AT

103

LT

104

P-104

FT

109

FC

109

V-103

Water

P-106

FIC

107

FT

107

TO V-104

V-102Acidification Vessel

P-105H2SO4 Pump

P-106H2SO4 Pump

P-107Lignin Slurry Pump


P-108Water Pump

V-103Lignin Solution Vessel

P-109Lignin Solution Pump



Drawn By :

Checked By

Revised By :

Drawing No :

Date :

Date :

Without Scale A4

Notes :

Group 6

V-22

V-23



80

From P-109

CS-101

H-101

Air

F-102

O2 & N2B-101

P-112

FIC

115

FT

115

PT

105

PIC

105

FIC

114

FT

114

O2 & N2

TT

102

TIC

102

FT

114

FIC

104

TIC

101

TT

101

H-103

AT

104

AC

104

PT

106

PIC

106

P-106

FT

110

FIC

110

LT

105

H-102

To UF-101

TT

103

To SD-101

TIC

103

Steam

N2

H-101Heat Exchanger

C-101O2 and N2 Compressor

CS-101Oxidation Reactor

F-102Air Blower

H-102Heat Exchanger

P-112Water Pump

H-103Heat Exchanger

B-101Steam Reboiler



Drawn By :

Checked By

Revised By :

Drawing No :

Date :

Date :

Without Scale A4

Notes :

Group 6

FT

110

FIC

110

FT

110a

FIC

110a

P-30

AC

104

V-104P-105

P-33

PT

104

PIC

104

AT

104

LT

106



81

From H-102

PT

111

FIC

111

FT

112

FIC

112

P-111

From H-103

TIC

103

TT

104

Others

Air

Powder Vanillin

AT

105

PT

107

PIC

107

FT

114

FIC

114

AC

105

UF-101Membrane Ultrafiltration

SD-101Spray Dryer

P-111Filtrate Pump



Drawn By :

Checked By

Revised By :

Drawing No :

Date :

Date :

Without Scale A4

Notes :

Group 6

FT

113

FIC

113



82

CHAPTER 7

PLANT LAYOUT AND PIPING DESIGN

Vanillin plant is subsidiary of Riau Andalan Pulp & Paper. The location of our

plant is beside RAPP, in Langgam, Pelalawan Regency, Riau. Our Plant Must near with

RAPP because black liquor as vanillin plant raw material sourced from RAPP byproduct.

RAPP total land area in langgam is 10,100 Ha with the following boundaries area.

North : PT Mitra Unggul Pusaka (rubber)

East : PT Mitra Unggul Pusaka (rubber)

South : PT Siak Raya Timber

West : Rubber plantations

Figure 7.1. Location of vanillin plant building

Vanillin Plant




83

Our vanillin plant is divided into several areas. The first area is the main

area of the factory, which is the production area adjacent to a black liqour storage

tank. Additionally, there are utility area at the back of the factory. For the

purposes of administration and personnel, there is a 3-storey office and other

facilities such as clinics, mosque, cafeteria, and athletic fields. For the power

source, there is an electric generator room adjacent to the living room

maintanance tools and fire safety.

Vanillin plant construction is based on safety considerations, ease of

distribution of raw materials, utilities, land availability, ease of marketing and

transportation of goods. Vanillin plant layout and process equipment layout can be

seen in the following figure.


84

Raw

Material

Storage

Labora-

torium

Control

Room

Product

Storage

70 m

Utility

room

OWNER PROJECT

GROUP 6

PLANT DESIGN

2012

SKALA

1 : 5

Project

MASTER PLANT OF VANILLIN PLANT

PICTURE

DESIGN LAYOUT OF VANILLIN PLANT

PICTURE NO:

PL 001/2012

NO.

Page

Total

Page

1

1

INFORMATION

Room or Area:

- Black Liquor storage tank

- Raw material storage

- Control Room

- Production Process Area

- laboratorium

- Utility Area

- Security Post

- Meeting point

- Fire Safety

- Maintenance Room

- Electric Generator Room

- Vehicle Parking Area

- Main Office

CHEMICAL ENGINEERING

DEPARTMENT

ENGINEERING FACULTY

UNIVERSITAS INDONESIA

155 m

125 m

Process Production Area

Black Liquor

Storage

wastewater

Storage

Security

post

Parking Area

clinic Mosque canteen

Meeting Point

Main

Office

Electric

generator

room

Maintenan-

ce room

Sport

Field

Fire

Station

65 m

50 m

30 m

Main Road Main Road

Truck Parking Area Truck Parking Area

Pedistrian road Pedistrian road

Pedistrian road

Pedistrian road

Figure 7.2. Design Layout of Vanillin Plant


85

7.16 m

2.9 m

4.25 m

15.6

m

15 m1.35 m

2.5 m

2.83 m

3.8 m

8.5 m

8 m1 m

1.86 m

4 m1.5 m

2.5 m

2.34 m

2.36 m

2 m

15 m

15 mRaw

Material

Storage

15 m

10 mLabora-

torium

Control

Room

15 m

10 m Product

Storage

15 m

15 m

30 m

65 m

70 m

15 m

10 mUtility

room

8.7 m

OWNER PROJECT

GROUP 6

PLANT DESIGN

2012

SKALA

1 : 5

Project

MASTER PLANT OF VANILLIN PLANT

PICTURE

DESIGN LAYOUT OF VANILLIN PLANT

EQUIPMENT PROCESS

PICTURE NO:

PL 002/2012

NO.

Page

Total

Page

1

1

INFORMATION

Equipment:

- Raw material storage tank

- Acidification Vessel 1

- Plate & Frame Filtration

- Belt Conveyor

- Elevator

- Acidification Vessel 2

- Solution lignin Vessel

- Heat Exchanger

- Ultrafiltration

- Spray Drying

- Wastewater tank

- Air tank

- Compressor

CHEMICAL ENGINEERING

DEPARTMENT

ENGINEERING FACULTY

UNIVERSITAS INDONESIA

160 m

125 m

Black

Liquor

Storage

Acidification

vessel 1Plate & Frame

filtration

Elevator,

acidification

vessel 2,

plate&frame

filtration

Vessel, storage, Heat

exchanger, reactor,

ultrafiltation, spray

drying

wastewater

Storage

Figure 7.3. Design Layout of Vanillin Plant Equipment Process


86

CHAPTER 8

HEALTH, SAFETY, AND ENVIRONMENT MANAGEMENT

Health, Safety, and Environment Program (HSE) is a standard for

industries in Indonesia in order to protect workers' rights. Safety and good health

can improve safety and morale for employees or labor in general. A sense of

safety and employee morale which is great significance for the improvement of

labor productivity is the key to the success of a company or factory. In order to

implement the good HSE program, in the factory applied some policies regarding

work place safety and health. The purpose of the HSE policy implementation

include :

1. Set a target of increasing annual health and safety and make sure

everything is fulfilled by conducting regular audits

2. Prevent personal injury and health risks for all people who are in the

factory

3. Develop, design, build, set up, operate and maintain the process, plant,

equipment, including disposal in accordance with company guidelines and

regulations on occupational safety and health, and document process

control methods are classified as hazardous

4. Provide and maintain a safe system of work and prepare all necessary

plans to tackle any kind of disturbance or damage

5. Ensure that all employees at the location of the company to realize

responsibility for occupational safety and health

6. Ensures staff provide guidance on occupational safety, health and

environmental issues receive adequate training

7. Involve all employees in the implementation of policies and procedures

using advice and training to facilitate the emergence of a sense of

involvement and responsibility

8. Ensuring and summarizes all the experience of occupational safety and

health hazards that are relevant and disseminate the conclusions for the

business as a whole

9. Reviewing periodically and health policy in line with central policy


87

8. 1 Health Aspects

Health factor is one of the main supporters milling operations. With good

health in the factory, all the factors supporting plant performance, especially the

employees will be more productive at work. To prevent disruption of the

environmental health aspects of plant it is necessary to consider what are the

factors that could potentially endanger the health aspects in plant environments.

Danger to the health aspects can be avoided by analyzing the potential hazards

affecting the environmental health aspects of the plant.

8. 2 Safety Aspects

Safety is a very important factor in a factory. Analysis of the factors of

potential harm occurred in this plant needs to be done so that we get the data and

considerations necessary for handling. Hazard Analysis is an analysis of the

composition of the dangers of a place that has the potential dangers.

Identify Adverse events leading to a hazard material

Mechanism analysis of opportunities possible unexpected events

The estimated magnitude of the dangers that may arise. Hazard analysis can

be divided into two, namely:

1. HIRA (Hazard Identification and Risk Assessment)

2. HAZOP (Hazard and Operability Study)

8.2.1 Hazard Identification and Risk Assessment (HIRA)

HIRA is the identification of risks to an activity. Hazard Identification and

Risk Assessment (Hazard Identification and Risk Assessment), analysis carried

out in daily activities and in the factory. In determining HIRA, there are several

steps that must be done. The stages are as follows:

Sorting activities to be carried out into smaller sub-activities and specific

Identify potential hazards for each sub-activity

Determination of the risks that might occur (hazard effects and the

possibilities)

Determining how to prevent and control the risk of harm

Conclusion potential hazards and risks involved for each activity

Conclusion to overall job

Risk = Hazard x Exchange Rate Possible Dangers


88

o Harmful effects are still composed of HIGH, MEDIUM and LOW

o The possible dangers consist of HIGH, MEDIUM and LOW

Table 8.1 Parameter in Counting Dangers Possibilities

PARAMETER HIGH MEDIUM LOW

Frequency of

harm

Each time the

work was done Once in 10-100

One time during

the job done

Frequency of

adverse

danger

Almost every

time the work is

done

Once in 10-100 Once in 100 or

more

Ability level

executive jobs

Without

experience,

never done

before work

Less experienced

Experienced,

have good

ability and often

do the work

Table 8.2 Parameter in Counting Danger Effects

PARAMETER HIGH MEDIUM LOW

Human

Resources

Death, disability,

body dysfunction,

severe injuries

Medium wounds,

the body can still

work

minor injuries

Asset

Damage to the

equipment,

production halted

The damage

causes decreased

production levels

Little damage,

does not affect

the production

of protection

tool

Protection

Tool

No protective

devices are in an

environment with

the presence of a

flammable

substance

Minimal

protection device

Tools available

with sufficient

protection,

installation of

insulated

Evacuation

time

availability

Less than 1 minute Between 1-30

minutes

More than 30

minutes


89

Table 8.5 Hazard Identification and Risk Assessment (HIRA)

Types of

Activities

Potential

Danger Dangers

Danger

Rate

Effects

Possible

Rate Risks Prevention and Management

Final

Risks

Pre-Operational Stage

Plant

Building

Falling from

Height

Permanent

Injuries Death H L M

Work on construction

activities in accordance with

SOP and using PPE safety

belt

L

Objects falling

from height

Moderate to

severe injuries M L M




helmet

L

Tripped up by

construction

equipment

scattered

Mild to

moderate

injuries

M M M




shoes

L

Installation

Tool

Falling or

pinched tool

Death and

organ

dysfunction

H M M Using PPE and safety belt L

Hit or tripped

work

equipment

Non-

permanent

injuries

M M M Checking the condition of the

tool to be used to start a job L


90

Electrical

installation

Electric shock

Death,

permanent

injury

H L M

Using rubber boots,

gloves and other tools

that are insulators

L

Fall at the

time of

installation of

the high

Death and

organ

dysfunction

H M M Using PPE and safety

belt L

Plant Operation Stage

Charging of

raw

materials in

tanks

Exposure to

chemicals

Irritation

and minor

injuries

L H M

Wearing PPE such as

gloves and masks when

filling the tank of raw

materials

L

Slip away due

to chemicals

Permanent

injuries and

death

H L M

Wearing PPE such as

gloves and masks when

filling the tank of raw

materials

L

The

operation

of the

process

Electric shock

at the pump

Permanent

injuries and

death

H L M

Perform regular checks

and maintenance of the

pump according to SOP

L


91

Exposure to

heat flow and

heat exchange

equipment

boiler

Injuries

caused by

the heat of

the skin

M M M

Workers doing the

work in accordance

with SOP

L

Exposure to

chemicals in a

leaky pipe

Irritation

and injury

by heat on

the skin.

M L M

Perform regular checks

on the piping system

and start planning a

better pipeline

L

Bumped by

pipelines &

reactors

Non-

permanent

minor

injuries

M L M

Workers work carefully

and in accordance with

SOP

L

Storage of

raw

materials /

product

Exposure to

chemicals

directly

Irritation

and minor

injuries

L M M

Carry out work in

accordance with the

SOP and training

employees periodically

L

Contamination

in the end

product

storage

Decline in

value and

product

quality

M M M

Implementation and

maintenance work as

per SOP tank

periodically

L


92

Factory Maintenance Stages

Maintenance

Process

Stumble and

fall

Non-

permanent

injuries to

permanent

M M M

Maintenance jobs done

mentati applicable

SOPs

L

Pinched or

scratched

appliance

Non-

permanent

injuries to

permanent

M M M Using PPE and safety

belt Obey SOP jobs L

Exposure to

chemicals

Irritation

and minor

injuries

L M M

Maintenance jobs done

mentati applicable

SOPs

L

Electric shock

on job-related

electrical

installation

Permanent

injuries to

farm

H L M

Perform maintenance

and replacement

electrical equipment

periodically and

perform maintenance

work on a regular basis

L

Treatment

Plant

Facilities

Falling from a

height

Permanent

injuries to

death

H L M

Perform maintenance

work in accordance

with the procedures and

PPE safety belt

L


93

Electric shock

Permanent

injuries to

death

H L M

Perform maintenance

and replacement

electrical equipment

periodically and

perform maintenance

work on a regular basis

L


94

8.2.3 Hazard Operability Study (HAZOP) of Vanillin Plant

Operation

Unit

Equipment

Code Parameter Deviation Causes Effects Prevention Control

Vessel

S-101

S-102

S-103

S-104

S-105

V-101

V-102

V-103

Flow rate

Less

Blocking of raw

material

supplies and not

suitable with the

equipment

capacity

Vessel doesn't

work

efficiently

Ensure that raw material

capacity must suitable

with equipment capacity

Flow

control (FC)

More

Raw material

capacity more

than machine

capacity

Vessel will be

damaged

easily

Installing controller

such as valve at the

input of reactor to adjust

raw material capacity

which entering the

equipments

Agitator

Velocity

Less Power resources

is low

Reaction

doesn't work

perfectly and

too long

Giving extra power such

as electrical power Flow

control (FC)

More

Agitator

velocity isn't

appropriate

Making bubble

in the agitating

process

Determine agitator

velocity value (rpm);

Controlling regularly

Pump

P-101

P-102

P-103

P-104

P-105

Flow rate No Blocking in

pump

Pump heat and

damaged

easily

Pump cleaning and

controlling regularly

Flow

control (FC)


95

P-106

P-107

P-108

P-109

P-110

P-111

Less Blocking or

leaking in pump Low supply

Pump cleaning and

controlling regularly,

installing valve and

flow indicator

More

Overload

stirring

performance

Pump

damaged

easily


Heat

Exchanger

H-101

Flow rate

Less Blocking or

leaking in HE

Supply will be

clogged Controlling regularly

Flow

control (FC)

More Input flow rate

increase

HE will be

damaged

easily


and installing valve in

HE input

Temperature

Less Steam supply

will decrease

Temperature

process will

increase too

long

Increasing steam to HE

Temperature

control (TC)

More Steam supply

will increase

Encrement of

temperature

will be

excessed

Decreasing steam to HE

H-102 Temperature

Less Steam supply

will decrease

Temperature

process will

increase too

long

Increasing steam to HE

Temperature

control (TC)

More Steam supply

will increase

Encrement of

temperature

will be excess

Decreasing steam to HE

HE-103 Flow rate Less Blocking or Supply will be Controlling regularly Flow


96

leaking in HE clogged control (FC)

More Input flow rate

increase

HE will be

damaged

easily


and installing valve in

HE input

Temperature Less Chilling water

supply increase

The

temperature

reduction will

be excess

Decreasing water supply

to HE

Temperature

control (TC)

More Chilling water

supply is less

Temperature

reduction

process will

too long

Increasing water supply

to HE

Boiler B-101 Flow rate

Less

Blocking or

leaking in

Boiler

Heating will

be blocked

Lean liquor flow rate

setting Flow

control (FC)

More

The result of

combustion

increase

Damaged

equipment Installing pressure valve

Bubble

column

reactor

CS-101 Flow rate

Less

Raw material

input is blocked

and unsuitable

with equipment

capacity

Reactor

doesn't work

efficiently

Ensure that raw material



Flow

control (FC)

More

Raw material

capacity more

than machine

capacity

reactor

damaged

easily and

liquid spilled



input of reactor to adjust

raw material capacity

which entering the

equipments


97

Blower F-101 Flow rate

Less Low power

supply

Acidification

process doesn't

work

effectively

Giving extra power such

as electrical power Flow

control (FC)

More

Overload

stirring

performance

Blower/fan

damaged

easily


Plate and

Frame

Filtration

PF-101

PF-102 Flow rate

Less Blocking or

leaking in pump

Supply will be

decreased

Controlling pump and

flow regularly;

Installing flow rate

controller Flow rate

Control

More

Overload

stirring

performance in

pump

Filtration

process will

take time too

long

Controlling pump and

flow regularly;

Installing flow rate

controller

Conveyor

CON-101

CON-102

CON-103

CON-104

Belt Speed

Less Low driving

force

Materials

which will be

streamed from

one place to

another would

pile on

operations

Provide additional

power in the form of

electric power Flow

Control

(FC)

More Incorrectness set

point

Supply

products are

expected to be

the product

will be too big

Determining the value

of a new set point and

controlled on a regular

basis


98

Spray Drying SD-101

Temperature

of the Hot air

Less

Hot air

temperature

which use to

atomized is too

small

vanillin still

contain a

water

Increase temperature of

hot air

Temperature

Control

(TC)

More

Hot air

temperature

which use to

atomized is too

big

Vanillin may

participate

evaporate

Decrease flow rate and

temperature steam

Flow rate

input

Less Input flow rate

is too small

Decreases

debit fluid

Increasing the flow rate

input

Flow rate

Control

(LC) More Input flow rate

is too large

Flooding,

crystalization

cannot

maximum

running

Reducing the flow rate

input

Ultrafiltration UF-101 Flow rate

Less

Blocking of

material

supplies and not

suitable with the

equipment

capacity

Ultrafiltration

doesn't work

efficiently

Ensure that material



Flow

control (FC)

More

Raw material

capacity more

than machine

capacity

Ultrafiltration

will be

damaged

easily



input of ultrafiltration to

adjust raw material

capacity which entering

the equipments

Vanillin Production from Lignin

99

8. 3. Environmental Aspects

An industrial process can have a negative impact on the environment if not handled

properly. The negative impact on the environment can affect the sustainability of

production and the local environment. In this section, we discuss some of the

environmental impacts that may result from the presence of the vanillin plant is that the

manufacturing process produces substances called residual waste. Based on his form, the

waste produced by the plant can be grouped into four types, namely:

8. 3. 1. Liquid Waste

Wastewater produced by this plant are lean liquor that will be recycled by PT Riau

Andalan Pulp and Paper and water which is reused for chilling water in heat exchanger.

8. 3. 2. Solid Waste

No solid waste is removed from the production process of this vanillin plant.

8. 3. 3. Waste Gas

Majority of the waste gas produced is CO2 emissions resulting from the generator.

8. 3. 4. Waste Sound (Noise)

Possible noise pollution generated by tools such as pumps and motors drive stirrer.

Noise can also be caused due to the damage to the mechanical system on the appliance. To

reduce the noise level equipment necessary regular maintenance schedule has been

determined. For workers who are diarea that generate noise should be equipped with ear

protection (ear plugs). Meanwhile, for tools that can generate noise can be added by means

of dampening noise.

Noise standards set by the minister of health is 60-70 dB, while the minister of labor

is a maximum of 85 dB for 8 hours. Expected kenisingan of indigo dye plant is not too

large because the pump used is not too large, as well as other tools.

8. 4. Risk Management

Risk Management aims to solve the problem even prevent accidents. A particular

effort is needed to reduce or eliminate potential risks. Risk is a condition where there is the

possibility of an accident or occupational disease because of the presence of a hazard. The

danger is of a material nature, administration of a tool, how to do a job or work


100

environment that can lead to property damage, occupational disease, or the loss of human

lives. To avoid the danger of necessary control components with potential risks such as

human factors, equipment and materials, as well as the methods and sources of danger.

Risk management system is a management process carried out with the intention of

minimizing the risk or the extent possible to avoid the risk altogether. In a risk management

system, which required the application of the hierarchy of control measures against the risk

of a hazard, with the following steps:

Elimination (eliminate the hazard)

Substitution (use raw materials more secure)

Engineering (redesign existing processes to make it more secure)

Administrative control (changing methods or procedures work in a more secure)

Personal protective equipment (using the appropriate protective equipment to isolate

the body from harm)

To meet risk management will require tools and backup facilities to prevent or

overcome danger danger that occurs in plants. The tools and means necessary including

body protective gear for employees, fire extinguishers, MSDS (Material Safety Data

Sheet), and Account Head Point (local assembled) for all employees if fire occurs.

8.4.1. Personal Protection Equipment

Equipment protection for employees is the main standard for a company to protect

its employees from the threat of disruption to the aspects of safety and health at work.

Based on the major needs in the field of personal protective equipment can be divided into:

a. General

Personal protective equipment as a minimum requirement to enter the plant,

ie safety helmet, googles, and safety shoes.

b. Special


101

PPE is used in accordance with the needs of employees in the workplace

each based on hazard and risk. For example: safety goggles, respirators, ear

protection, gloves, earplugs, etc. Here are some of the personal protective

equipment used in the factory:

a. Protective equipment fall

Fall protective equipment used in the petrochemical industry is the seat belt / safety

belt is one of safety for the protection of workers in performing work activities in high

places where workers are likely to fall. Things that need to be considered for fall

protection equipment, namely:

Safety belt used to be in high places over 4 ft, the rope should be tied firmly on

building / sustaining a capable Defence weight

Ensure seat belt component in a condition to be good

To keep the belt remains in good condition, the equipment belt should be cleaned

with hot water and soap, and stored away from the sun and ultaviolet very strong,

also the chemical that causes the fibers to become brittle and weak belt

Type of fall protection equipment consists of:

Belts or harnesses are equipped components stitching, buckles, D-rings, cuts and

abration

The rope is made up of components rot, proper hook and knots, frayed strands or

broker.

b. Respiratory protection

The usefulness of this protection tool, especially in an emergency, eg labor should

help others who suffer accidents / when must escape a sudden atmospheric air

composition changes such that endanger his soul / when should perform repairs

equipment in where very high levels of contaminants.

Respirator or air purifying respirator which serves to clean the air that has been

contaminated in the form of dust, gases, metal vapors, smoke and fog, and protect the

work force has been a breath of danger, composed of chem respirator (steam and gas


102

contaminants), mech filter respirators (dust, mist, vapor metallic, sour) and cartridge /

canister respirator (mixed gas / vapor with solid particles equipped with a filter).

Breathing apparatus (air supply respirator), which supplies clean air or oxygen to the

wearer. Respirator is not equipped with a filter or cartridge, but supplies the user with

compressed air / air cleaner / from an oxygen tank.

Figure 8.1. Respirator

c. Hand protection tool

To protect from possible dangers that occur, it is expected that workers in work

activities always wore gloves, which must be adjusted to the working conditions and in

the absence of injured / contamination of the hands. Various kinds of gloves according

to the types of hazards that must be prevented:

Asbestos gloves, leather, PVC should be used when heat is caused by the heat

generated in the factory work, eg welding gloves to be used must pass through the

wrist

Rubber gloves, made of synthetic material, vinyl as well as natural, to protect hands

from chemicals caustic acids, alkalis and various types of other solvents

Gloves canvas / leather, wear gloves of canvas or heavy cotton is typically used

when the main danger is very high heat caused by friction

Gloves with chrome leather or PVC material with special design, to reduce the

hazard when in contact with sharp objects


103

Figure 8.2. Gloves

d. The tool foot protector

Safety shoes should protect workers against accidents caused by heavy items falling

to the feet, protruding nails, liquid metal, and so on. The types of tools used: Protective

Footwear, used in good condition should provide some protection against the impact of

falling objects or punctures caused by sharp objects to be secure, end-coated steel in a

protective layer of skin shoes worn feet will not slip or high heels at least 3 / 8 inch, 1-1/2

inch maximum.

Figure 8.3. Safety Shoes

e. Eye protection

Use eye protection of workers flake delicate objects and spray chemicals that can

enter and cause irritation to the eyes or even injure the eyes. This tool can also protect your


104

eyes from impact workers against a hard object. For eye protection, personal protective

equipment supplied googles or safety glasses for workers.

Figure 8.4. Goggles

f. Ear protective devices

Ear protective devices commonly used in the area located the tools that may cause

loud noises such as compressors, pumps, steam generators, conveyors and other tools that

use motors for propulsion. For protection against ear every employee who deals with the

tools required to use earplug process provided by the company.

Figure 8.5. Earplugs

g. Protective equipment head

The tool used in the form of head protection safety helmet. This headwear is a

protective device that is used to protect the head from impact by hard objects while

working in the field.

h. The tool body armor


105

Personal protective equipment such as protective clothing body safe. Clothing was

named coverall which serves to avoid the possibility of a leak or spill liquid products in

bulk, so it can protect the body and to avoid direct contact with the skin of workers. To

clean up the spill using absorbent material must be non-combustible inorganic. In addition,

protective clothing or clothing that workers should not be used that has a crease on the

bottom of his pants.

8.4.2. Fire extinguisher

Determining the type of fire extinguishers are provided to extinguish the fire and

fire prevention and control efforts tailored to the classification of fire, state buildings and

items that exist in the building. Classification of types of fires, as follows:

Types of fire extinguishers, among others:

a. Water type fire extinguishers, consists of two types:

Soda Acid

Water CO2

Fire extinguisher soda acid type is not used anymore because it is dangerous to

humans. Water type fire extinguisher was used to extinguish the fire Class-A and

has the following specifications:

Red tube.

Distance sprays to tubes 9 liters (12-15 kg) is 6 meters.

When usage is 1-2 minutes depending on the size of the tube

b. Fire extinguisher types of dry dust, consisting of three types:

BC-class Dry Dust

Fire Class - B and C

Class ABC dry dust

Fire Class - A, B and C

Dry Dust class D

Fire Class - D fire extinguishers dry dust types have the following specifications:

a. Light blue tube

b. Consists of chemicals such as:


106

o Sodium Bicarbonate (97%)

o Magnesium Stearate (1.5%)

o Magnesium Karbinat (1%)

o Tricalcium phosphate (0.5%)

c. Tube size 1-12 kg

d. Distance 9 liters spray tube is 4-6 meters

e. Long time usage depending on size, to the size of 14-16 kg is 15 seconds

c. Types of fire extinguishers carbon dioxide (CO2)

Extinguisher was used to extinguish the fire Class-B and C and has the

following specifications:

o black tube

o distance 4.5-8 kg spray tube is 2 meters

o spending time is 14 seconds

o gas CO2 in liquid tube.

o the level of development is 450:1

d. The type of fire extinguisher foam (foam), consists of three types:

o Scum Chemistry

o Self-Aspirating

o Non-Aspirating AFFF

The type of fire extinguisher foam or foam used to extinguish the fire classes A and

B. Specifications of this type extinguishers are:

o Creamy white colored tube

o Distance sprays to tubes 9 liters (14-16kg) is 4-5 meters

o The duration is 30 seconds spending

o The level of development is 1:8


107

8.4.3. MSDS (Material Safety Data Sheet)

MSDS are data from material or plant material in the interests of health and safety.

Any material or chemicals present in the plant must have a MSDS which serves as the basis

for the use of (material handling). MSDS data serves to communicate and inform everyone

working with these materials so that they can use the material properly and act

appropriately if there is immediate danger. MSDS of some materials of this plant will be

showed in appendix.

8.5. Quality Control in Vanillin Plant

All the food people eat must be absolutely pure and clean. This is one of the most

important principles of the food industry. One decisive criterion here is that products leave

factory without any metal contaminations and other contaminants. Product manufacturers

and service industries have realized that competition in a global market require a continual

and committed effort towards the improvement of product and service quality.

Quality control process consists of raw materials, process, product and service.

Major factors in process that cause variability in quality of finished product are people,

equipment and methods or technologies employed in the process. Use of proper statistical

process control methods is vital for assurance of the product quality. Statistical quality

control comprises the following procedure:

– Finished product is measured

– Value of quality characteristics is used to provide feedback on how process can be

improved

– Sampling occurs for days or weeks

– Lot is either accepted or rejected based on information from sample

– This procedure provided slow feedback of information.

Recognizing the importance of quality control of food products, Government of

Indonesia has legalized the Act No. 7 of 1996 on food and our plant use it as regulation of

quality control. The Food Act is intended as a legal basis for the regulations, development,

and control on the production activities or process, the circulation, and trade of food. This

Act also provides a reference for various legislative regulations related to food, both

already in existence and to be established.


108

WCfeecontractorycontingencfacilitiesoffsitebuildingssiteTBM

WCTPITCI

CCCCCCC

CCC

CHAPTER 9

ECONOMIC ANALYSIS

This chapter gives the economic analysis of vanillin plant from lignin. The steps to analyze

the plant economic is explained below.

9.1 Plant Cost Estimation

For total Capital Investment estimation of vanillin plant, we use Guthrie method with the

following formula.

1. Total Bare Modul Cost (CTBM)

Total bare module cost can be calculated using the costs of bare module (CBM) from

each equipment manufacturer. Cost of bare module (CBM) for each equipment can be seen

in table 9.1 while total bare module cost (CTBM) can be seen in table 6.2.


109

Table 9.1. Recapitulation CBM value for each equipment

Code Equipment Unit

Amount Cost $

Year

Basis

Cost Index

Year Basis

Cost Index in

2013

Cost in 2013

($) Source

P-101 BLACK LIQUOR PUMP 1 8,565.84 2007 525.4 587.88 9,584.48 sinnot,2009

P-102 BLACK LIQUOR ACIDIFICATION

PUMP 2 8,401.91 2007 525.4 587.88 18,802.11 sinnot,2009

P-103 LIGNIN ACIDIFICATION PUMP 1 8,485.19 2007 525.4 587.88 9,494.24 sinnot,2009

P-104 LIGNIN SOLUTION PUMP 1 7,836.77 2007 525.4 587.88 8,768.70 sinnot,2009

P-105 LIGNIN SOLUTION PUMP 1 8,168.08 2007 525.4 587.88 9,139.42 sinnot,2009

P-106 VANILLIN SOLUTION PUMP 1 7,076.06 2007 525.4 587.88 7,917.54 sinnot,2009

P-107 VANILLIN SLURRY PUMP 1 6,955.41 2007 525.4 587.88 7,782.54 sinnot,2009

P-108 WATER PUMP 2 7,092.47 2007 525.4 587.88 15,871.81 sinnot,2009

P-109 H2SO4 PUMP 1 7,005.95 2007 525.4 587.88 7,839.09 sinnot,2009

P-110 WATER PUMP 1 7,234.38 2007 525.4 587.88 8,094.69 sinnot,2009

P-111 NAOH PUMP 1 7,814.68 2007 525.4 587.88 8,743.99 sinnot,2009

S-101 BLACK LIQUOR STORAGE 3 2,646.54 2004 444.2 587.88 10,507.74 sinnot,2004

V-101 ACIDIFICATION VESSEL 5 885.85 2004 444.2 587.88 5,861.90 sinnot,2004

V-102 ACIDIFICATION VESSEL 2 (A) 1 586.39 2004 444.2 587.88 776.06 sinnot,2004

V-102 ACIDIFICATION VESSEL 2 (B) 1 1,892.34 2004 444.2 587.88 2,504.44 sinnot,2009

V-103 BLENDING VESSEL 1 996.13 2004 444.2 587.88 1,318.34 sinnot,2012

S-102 LIGNIN SLURRY STORAGE 1 93,131.21 2004 444.2 587.88 123,255.24 sinnot,2009

S-103 H2SO4 STORAGE 1 21,853.70 2004 444.2 587.88 28,922.45 sinnot,2012

S-104 NaOH STORAGE 1 10,708.90 2004 444.2 587.88 14,172.78 matche,2007

S-105 WASTE STORAGE 2 112,472.97 2004 444.2 587.88 297,706.49 sinnot,2004

PF-101 PLATE AND FRAME FILTRATION 4 215,362.25 2004 444.2 587.88 1,140,091.49 sinnot,2004

PF-102 PLATE AND FRAME FILTRATION 1 56,454.18 2004 444.2 587.88 74,714.73 sinnot,2004

E-101 HE 1 21,700.00 2007 525.4 615.40 25,417.17 Seider, 2003

E-102 HE 1 21,700.00 2007 525.4 615.40 25,417.17 Seider, 2003

E-103 HE 1 19,000.00 2007 525.4 615.40 22,254.66 Seider,2003

UF-101 ULTRAFILTRATION 2 70,834.40 2000 394.0 615.40 221,276.60 Seider, 2003

SD-101 SPRAY DRYING 1 32,269.54 2000 394.0 615.40 50,402.72 Seider, 2003

B-101 BOILER 1 17,032.24 2000 394.0 615.40 26,603.14 Seider, 2003

CS-101 BUBBLE COLUMN REACTOR 1 49,066.96 2004 444.2 587.88 64,938.06 sinnot, 2004


110

Table 9.2. Recapitulation CTBM value

Code Equipment

FOB/unit

ammount

($)

Total

Module

Factor

Bare Modul

Cost ($)

P-101 BLACK LIQUOR PUMP

9,584.48 3.47

33,258.15

P-102

BLACK LIQUOR ACIDIFICATION

PUMP

18,802.11 3.47

65,243.33

P-103 LIGNIN ACIDIFICATION PUMP

9,494.24 3.47

32,945.02

P-104 LIGNIN SOLUTION PUMP

8,768.70 3.47

30,427.41

P-105 LIGNIN SOLUTION PUMP

9,139.42 3.47

31,713.78

P-106 VANILLIN SOLUTION PUMP

7,917.54 3.47

27,473.87

P-107 VANILLIN SLURRY PUMP

7,782.54 3.47

27,005.41

P-108 WATER PUMP

15,871.81 3.47

55,075.17

P-109 H2SO4 PUMP

7,839.09 3.47

27,201.64

P-110 WATER PUMP

8,094.69 3.47

28,088.57

P-111 NAOH PUMP

8,743.99 3.47

30,341.66

S-101 BLACK LIQUOR STORAGE

10,507.74 1.41

14,815.92

V-101 ACIDIFICATION VESSEL

5,861.90 4.2

24,619.97

V-102 ACIDIFICATION VESSEL 2 (A)

776.06 1.5

1,164.08

V-102 ACIDIFICATION VESSEL 2 (B)

2,504.44 1.47

3,681.52

V-103 BLENDING VESSEL

1,318.34 4.2

5,537.01

S-102 LIGNIN SLURRY STORAGE

123,255.24 1.47

181,185.20

S-103 H2SO4 STORAGE

28,922.45 4.2

121,474.31

S-104 NaOH STORAGE

14,172.78 3.37

47,762.27

S-105 WASTE STORAGE

297,706.49 1.5

446,559.73

PF-101 PLATE AND FRAME FILTRATION

1,140,091.49 3.47

3,956,117.46

PF-102 PLATE AND FRAME FILTRATION 3.37


111

74,714.73 251,788.64

E-101 HE

25,417.17 1.5

38,125.75

E-102 HE

25,417.17 2.06

52,359.37

E-103 HE

22,254.66 3.37

74,998.21

UF-101 ULTRAFILTRATION

221,276.60 2.7

597,446.81

SD-101 SPRAY DRYING

50,402.72 2.7

136,087.36

B-101 BOILER

26,603.14 2.24

59,591.04

CS-101 BUBBLE COLUMN REACTOR

64,938.06 1.41

91,562.66

Total Bare Modul Cost ($)

6,493,651.30

- Csite cost calculation

( )

- Cbuilding cost calculation

( )

- Coffsite facilities cost calculation

( )

- Ccontingency cost calculation

- Ccontractor fee cost calculation


112

- CWC cost calculation

( (

)

Therefore total capital investment of vanillin plant can be found with following equation.

(

)

(

)

Table 9.3. Total Cost Investment

Component Value in $

Total Bare Modul Cost (C TBM) ($) 6,493,651.30

Site Development Cost (C site) ($)

1,298,730.26

Building Cost (C building) ($)

1,298,730.26

Offsite Facilities Cost (C offsite facilities) ($)

15,000.00

Contingency ($)

974,047.70

Contractor fee ($)

194,809.54

Working Capital (C WC) ($)

2,182,403.43

Total Cost Investment ($)

14,306,866.92


113

9.2 Annual Operating Costs

Annual operating costs are divided into two types; fixed and variable cost, this cost

will be issued during the plant operating. Some of the assumptions used for calculate the

operating costs are as follows:

1. Plant operating life is 20 years.

2. In 1 year, this plant operated for 300 days, 24 hours.

3. The production capacity is 100% since the plant operated.

4. Depreciation is 9%, inflation is 4%, and interest rate is 10% per year.

Operating costs are calculated by performing the following details:

9.2.1 Raw Material Costs

Raw material used in this plant consists of:

1. Black Liquor Costs

Black liquor is result of the paper mill waste. Black liquor obtained from Riau

Andalan Pulp and Paper mill without charge. It because PT. Riau Andalan Pulp and

Paper is owner of this plant.

Needs for a year : 200,100 tons/year

Raw material cost : $ 0 /tons

Raw material cost per year : 200,100 tons/year X $ 0 /tons

= $ 0 /year

2. Carbon Dioxide

Needs for a year : 1,500.30 m3/ year

Raw material cost : $ 2.04 /m3

Raw material cost per year : 1,500.30 m3/ year X $ 2.04 /m3

= $ 3,055.53 /year

3. Sulfuric Acid

Needs for a year : 2,362.50 tons/ year

Raw material cost : $ 412.83 /tons

Raw material cost per year : 2,362.50 tons/ year X $ 412.83 /tons

= $ 975,315.48 /year

4. Sodium Hydroxide


114

Needs for a year : 450 tons/ year

Raw material cost : $ 1,767.78 /tons

Raw material cost per year : 450 tons/ year X $ 1,767.78 /tons

= $ 795,500.61 /year

5. Water

Needs for a year : 333,166.50 tons/ year

Raw material cost : $ 0.13 /tons

Raw material cost per year : 333,166.50 tons/ year X $ 0.13 /tons

= $ 44,604.48 /year

6. Air (O2 and N2)

Needs for a year : 612 m3/ year

Raw material cost : $ 3.16 /m3

Raw material cost per year : 612 m3/ year X $ 3.16 /m3

= $ 1,935.21 /year

Thus, the total direct material cost is $ 1,820,411.31 per year.

Table 9.4. Raw Material Cost per Year

Materials Amount Unit/batch Needs per

year

Cost in 2012

($)

Cost in

2015 ($)

Raw Material

Cost Per

Year ($)

Water 370.19 ton 333,166.50 0.12 0.13 44,604.48

CO2 1.67 m3 1,500.30 1.90 2.04 3,055.53

H2SO4 50.03 ton 45,022.50 385.14 412.83 975,315.48

NaOH 0.50 ton 450.00 1,649.20 1,767.78 795,500.61

Air (O2 and

N2) 0.68 m3 612.00 2.95 3.16 1,935.21

Total Raw Material Cost Per Year 1,820,411.31


115

9.2.2 Operating Labor Costs

Table 9.5. Indirect Labor costs

Qualification Amount

Cost per

month ($)

Cost per

year ($)

Total cost

per year ($)

Commissioner 1 5000 60000 60000

President Director 1 3500 42000 42000

FINANCIAL

Financial Director 1 2000 24000 24000

Marketing Department Manager 1 1500 18000 18000

Marketing Department Staff 2 900 10800 21600

Financial Department Manager 1 1500 18000 18000

Financial Department Staff 2 900 10800 21600

Budgetary Department Manager 1 1500 18000 18000

Budgetary Department Staff 2 900 10800 21600

HUMAN RESOURCES

Human Resources Director 1 2000 24000 24000

Public Relation Manager 1 1500 18000 18000

Public Relation Staff 2 900 10800 21600

Personnel Manager 1 1500 18000 18000

Personnel Staff 2 900 10800 21600

Education & Training Manager 1 1500 18000 18000

Education & Training Staff 2 900 10800 21600

OPERATIONAL

Operational Director 1 3000 36000 36000

Engineering Manager 1 1800 21600 21600

Processing Manager 1 1800 21600 21600

HSE Manager 1 1800 21600 21600

Research & Development

Manager 1 1800 21600 21600

Research & Development Staff 3 1200 14400 43200

Fixed Cost of Indirect Labour 553,200.00

Variable Cost of Indirect Labour = 20% TIL 110,640.00

Total Indirect Labour 663,840.00


116

Table 9.6. Direct Labor costs

Qualification Amount

Cost per

month ($)

Cost per

year ($)

Total cost

per year ($)

Supervisor 2 1500 450,000.00 900,000.00

Engineering Staff 3 1200 14400 43200

Processing Staff 3 1200 14400 43200

HSE Staff 3 1200 14400 43200

R&D Staff 3 1200 14400 43200

Fixed Cost of Direct Labour 172,800.00

Variable Cost of Direct Labour = 20% TDL 34,560.00

Total Direct Labour 207,360.00

Total Operating Labour (OL) 871,200.00

9.2.3 Utilities Costs

The table below explain the detail of the utilities cost needed per year.

Table 9.7. Total Utilities Cost per Year

Utilities Amount Unit Needs per

year

Cost in

2012 ($)

Cost in

2015 ($)

Utilities

Cost Per

Year ($)

Electricity 126129.44 kwh/year 126129.44 0.08 0.09 54432.38

Domestic Water 10.00 m3/day 3000.00 0.12 0.13 401.64

Fuel for Steam 210.43 L/batch 568161 1.10 1.18 669913.58

Total Utilities Cost Per Year 681131.08


117

9.2.4 Total Direct Costs

Table 9.8. Total Direct Costs per Year

Total Raw Material Costs $ 1820411.31

Total Operating Labour (OL) $ 871200.00

Total Utilities Cost $ 681131.08

Maintanance Cost (10% Fc) $ 1212446.35

Direct Supervisory (20% Operating Labour) $ 174240.00

Operating Supplies (1%Fc) $ 121244.63

Laboratory Charges $ 87120.00

TOTAL DIRECT COST $ 4967793.37

9.2.5 Total Fixed Costs

Table 9.9. Total Fixed Cost

Fixed Cost

Local Taxes 3% Fc $ 363733.90

Insurance 1% Fc $ 121244.63

Total Fixed Cost $ 484978.54

9.2.6 Plant Overhead

( ) ( )

9.2.7 Total Manufacturing Cost

Table 9.10. Total Manufacturing Cost

Total direct cost $ 4967793.37


118

Total Fixed Cost $ 484978.54

Plant Overhead $

Total Manufacturing Cost $ 6281542.17

9.2.8 Expenses Cost

Here, we can know value of TOC, with the estimating that total manufacturing cost is 85%

Total Operating cost. So, the value of TOC is :

We can get the expenses cost.

The details of expenses cost is in table 6.11

Table 9.11. Total Expenses Cost

EXPENSES COST

EXPENSES COST = 15% TOC $

Administrative Cost = 15% OL $ 130680.00

Financial Interest = 5% Fc $ 606223.17

Distribution&Selling + R&D = EC – (AC+FI) $ 371604.27

9.2.9 Total Operating Cost

So, total operating cost of this plant is


119

9.3 Equity

The total investment from this vanillin plant is $ 14306866.92 (according to the

preliminary equation). The initial capital came from the plant 60% equity and 40% of the

bank loan.

Table 9.12. Source investment

Source investment % value Interest / year

Self investment 60% 8584120.15 5 %

Bank Loan 40% 5722746.77 10%

Table 9.13. Bank Source Equity

Year Bank Loan Interest

End Year

Payment Loan remaining

2014 5722747 0 0 0

2015 6295021 629502 0 6924524

2016 6924524 692452 2077357 5539619

2017 5539619 553962 1938867 4154714

2018 4154714 415471 1800376 2769809

2019 2769809 276981 1661886 1384905

2020 1384905 138490 1523395 0

Table 9.14. Self Investment Source Equity

Year

Investment

Loan Interest

End Year

Payment Loan Remaining

2014 8584120 0 0 0

2015 9442532 472127 0 9914659

2016 9914659 495733 2478665 7931727

2017 7931727 396586 2379518 5948795

2018 5948795 297440 2280372 3965864

2019 3965864 198293 2181225 1982932

2020 1982932 99147 2082078 0


120

9.4 Investment feasibility Analysis

To determine a project feasible or not to do, it is necessary a feasibility analysis of

investment. Investment is called feasible if it gives more profit than the expected. Expected

minimum profit are commonly known as the MARR, while profits are calculated on the

investment feasibility analysis are known as the IRR. Some of the usual investment

parameters analyzed are given below.

9.5.1 Cash Flow

Cash flow can indicate fluctuations in income earned over the life of the plant

through net income. The calculation is by subtracting the cash inflow with cash flow out.

Calculations of cash inflow involving revenue after taxes cutting, depreciation, rest value of

equipment called the after-tax cash flow (ATCF). Meanwhile, out cash flow can be an

investment, cost, and loans. Calculations before and after tax cash flow is shown in Table

9.15 and is represented in the cash flow diagram in Figure 9.1


121

Figure 9.1. Cash flow diagram

-15000000.00

-10000000.00

-5000000.00

0.00

5000000.00

10000000.00

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22

After Tax Cash Flow

ATCF Total ATCF Bank ATCF Investor


122

Table 9.15 shows the calculation of cash flow that calculated from the initial

construction plant. In early 2013, the construction of the plant is beganwhich an investment is

for the purchase of the entire instrument. Figure 6.1 shows that the largest investment

incurred in the first year. In 2013, the construction is still going on until the middle of 2014,

so it is still a cash flow investment. In 2015, our factory started operation.

9.5.2 IRR

To find out how IRR can be obtained from the cash flow in table 6.12 above, it can be

calculated that the number of trial IRR values PW = 0,

Table 9.16 IRR Calculation

NPV

PV Bank PV Investor PW

-5334763.94 -7929399.12 -14592249.73

-341252.11 -511878.16 -853130.27

-3605180.83 -5457383.83 -8237587.18

3268169.31 4992616.20 6825122.96

2952272.39 4551412.99 5635018.13

2666450.82 4148485.59 4651632.90

2407854.71 3780528.12 3839150.13

2173905.94 3444523.34 3167951.53

1962271.72 3137716.59 2613544.42

1770840.74 2857592.27 2155674.62

1597701.86 2601852.57 1777593.30

1441124.77 2368398.15 1465450.68

1299542.74 2155310.70 1207794.80

1171536.95 1960837.02 995156.86

1055822.43 1783374.61 819708.42

951235.31 1621458.53 674977.72

856721.38 1473749.51 555615.10

771325.68 1339023.03 457198.91

694183.17 1216159.45 376074.98

624510.20 1104134.97 309223.76

561596.91 1002013.39 254150.51

504800.24 908938.61 208794.37


123

Based on the trial was obtained IRR = 20.35%. Then, to know the NPV value as one

component of determining the feasibility of the realization of the design, PW calculation with

i = MARR = 10%, at which NPV = PW.


124

9.5.3 Net Present Value (NPV)

An investment is feasible to be implemented if the investment has a value

of NPV> 0. This value indicates that the value for money of the plant profit not

lower than the value of the money spent as an investment in the factory default.

Therefore all of the above ATCF then be calculated present value rate of 10%

MARR. Table 6.17 shows the calculation of our plant NPV.

Table 9.17 NPV Calculation

Year NPV

PV bank PV Investor

-1 -5334763.94 -7929399.12

0 -341252.11 -511878.16

1 -3605180.83 -5457383.83

2 3268169.31 4992616.20

3 2952272.39 4551412.99

4 2666450.82 4148485.59

5 2407854.71 3780528.12

6 2173905.94 3444523.34

7 1962271.72 3137716.59

8 1770840.74 2857592.27

9 1597701.86 2601852.57

10 1441124.77 2368398.15

11 1299542.74 2155310.70

12 1171536.95 1960837.02

13 1055822.43 1783374.61

14 951235.31 1621458.53

15 856721.38 1473749.51

16 771325.68 1339023.03


125

17 694183.17 1216159.45

18 624510.20 1104134.97

19 561596.91 1002013.39

20 504800.24 908938.61

Total NPV 5143803.48 18242597.62

NPV total 23386401.11

From the table above we can see that the value of the plant NPV is greater than

zero.

9.5.4 Pay Back Period

The payback period can be determined where the number of cumulative

ATCF to year n is equal to zero. From table 6.15, payback period value is located

between 3 and 4 years because in year 3 the value of cumulative ATCF is

negative and in year 4 the value of cumulative ATCF is positive.

Table 9.18 Pay Back Period Calculation

Year Payback Bank Payback Self

investment

Payback overall

3 -1272777.01 -1909165.51 -3181942.52

4 2631173.64 3946760.46 6577934.10

PBP 3.33 3.33 3.33

From the table above, we using the interpolation, we get the payback period is

3,74 years. This shows that the construction of the plant is feasible to be realized.

9.5.5Break Event Point (BEP)

Break Event Point states where the total sales volume of income exactly

equal to the total cost, so the company does not make a profit nor suffer a loss.

Problems of Break event will appear in the company if it has a Variable Costs

and Fixed Costs. A company with a certain production volume may suffer a loss


126

of income due to sales is only able to cover variable costs and can only cover a

small portion fixed costs.

( ) ( )

( )

Where the variable cost is the total of raw material price, labour price, and plant

overhead. The data is gotten from table 6.15.

So, the BEP of this plant is 495,95 tonnes.

9.5.6 Sensitivity Analysis

Sensitivity for product price

Table 9.19. Sensitivity analysis for product price

Deviasi Price NPV

IRR

(%) PBP (tahun)

-0.20 14.40 -5658627.61 12.30 4.71

-0.10 16.20 8863886.75 16.58 3.86

-0.05 17.10 16125143.93 18.51 3.57

0.00 18.00 23386401.11 20.35 3.33

0.05 18.90 30647658.29 22.11 3.13

0.10 19.80 37908915.46 23.80 2.96

0.20 21.60 52431429.82 27.00 2.69

From the table above, we can see that if the price become cheaper, the

value of NPV, IRR and the payback period become lower. The payback period is

sensitive with deviation -20% or the price of vanillin $ 14.40 because the NPV

become a negative value although the PBP below 5 years and IRR still above 10%

(below MARR).


127

Figure 9.2. Sensitivity analysis for product price

Sensitivity for Raw material price

Table 9.20. Sensitivity analysis for raw material cost effect

Deviasi Raw Material Cost NPV

IRR

(%) PBP (tahun)

0.00 1820411.31 23386401.11 20.35 3.33

0.05 1911431.87 21782327.30 19.94 3.38

0.10 2002452.44 20178253.37 19.51 3.44

0.20 2184493.57 16970105.67 18.66 3.57

0.50 2730616.96 7345662.59 16.03 4.02

From the table above, we can see that if the raw material cost

become higher, the value of NPV and IRR become smaller while payback

period lower. The payback period is sensitive with deviation 50% or raw

material cost $ 2730616.96.

y = 1E+08x + 2E+07 R² = 1

-10000000.00

0.00

10000000.00

20000000.00

30000000.00

40000000.00

50000000.00

60000000.00

-0.30 -0.20 -0.10 0.00 0.10 0.20 0.30

NP

V

PriceDeviation

Product Price Effect

Series1

Linear (Series1)


128

Figure 9.3. Sensitivity analysis for raw material cost effect

y = -3E+07x + 2E+07 R² = 1

0.00

5000000.00

10000000.00

15000000.00

20000000.00

25000000.00

0.00 0.20 0.40 0.60

NP

V

Cost Deviation

Operational Cost Effect

Series1

Linear (Series1)


129

APPENDIX

1. Vessel

1.1 Black Liquor Storage Tank (S-101)

Calculation

Storage tank functioning as a repository of black liquor that will be used

for the production of vanillin. To calculate the dimensions of the tank needs to

know the total volume of the tank. The total volume of the tank is calculation of

tank working volume and tank head space. In the design of storage tanks,

assumptions using are:

- Ratio of height to diameter of the tank is 4:3

- Tank working volume is 0.85 of the total volume of tank

- residence time is 1 hour.

Black liquor flow rate:

Tank working volume :

Diameter and height of the tank:

(

)

(

)

Where; D is diameter of the tank and H is height of the tank. From the

results of calculation and rounding up to 0.1 m, height and diameter of the

tank is obtained respectively 9.55 m and 7.16 m.


130

Thickness of shell tank:

x (CA n)

P (psi) = Poperation (psi) + Pstatis + safety factor

= 14.7 psi + 21.8 psi + 20 psi

= 56.50

S = Allowable stress, for stainless steel 316 = 20000 psi

E = Joint efficiency = 0.85

CA= Corrosion Allowance = 0.001 m/year

n = equipment life = 20 years

( )

Roof thickness of the tank:

1.2 Acidification Tank (V-101)

Calculation

a. Tank Design

Mixer tank functioning as a tank to mix black liquor slurry with H2SO4. To

design mixer tank, the dimensions of the tank needs to know the total volume of

the tank. The total volume of the tank is calculation of tank working volume and

tank head space. In the design of storage tanks, the assumptions used are:







131


(

)

(

)





x (CA n)


= 14.7 psi + 4.78 psi + 20 psi

= 39.48





( )



132

b. Impeller Design

Calculated of impeller design are:

Diameter (Da) = 0.4 x 2.90 m = 1.16 m

Blade width (W) = 0.125 x 1.16 m = 0.15 m

Agitator space from based (E) = 0.167 x 3.29 m = 0.55 m

1.3 Acidification Tank (V-102)

Calculation

a. Tank Design







- residence time is 0.5 hour.




(

)

(

)


133





x (CA n)


= 14.7 psi + 7.05 psi + 20 psi

= 41.75





( )


b. Impeller Design


Diameter (Da) = 0.4 x 2.30 m = 0.92 m

Blade width (W) = 0.125 x 0.92 m = 0.12 m


1.4 Blending Tank ( V-103)

Calculation


134

c. Tank Design







- residence time is 10 minute.




(

)

(

)





x (CA n)



135

= 14.7 psi + 4.49 psi + 20 psi

= 39.19





( )


c. Impeller Design


Diameter (Da) = 0.4 x 1.54 m = 0.61 m

Blade width (W) = 0.125 x 0.61 m = 0.08 m


1.5 Lignin Slurry Storage (S-102)

Calculation

Storage tank functioning as a repository of alkali lignin slurry before enter

to bubble column reactor. To calculate the dimensions of the tank needs to know

the total volume of the tank. The total volume of the tank is calculation of tank

working volume and tank head space. In the design of storage tanks, assumptions

using are:






136



(

)

(

)





x (CA n)


= 14.7 psi + 5.65 psi + 20 psi

= 40.35





( )



137

1.6 Waste Storage (S-103)

Calculation

Storage tank functioning as a repository of waste from vanillin production

process. To calculate the dimensions of the tank needs to know the total volume

of the tank. The total volume of the tank is calculation of tank working volume

and tank head space. In the design of storage tanks, assumptions using are:







(

)

(

)






138

x (CA n)


= 14.7 psi + 21.6 psi + 20 psi

= 56.34





( )


1.7 H2SO4 Storage (S-104)

Calculation

Storage tank functioning as a repository of H2SO4 before used in vanillin

production process. To calculate the dimensions of the tank needs to know the

total volume of the tank. The total volume of the tank is calculation of tank


using are:







139


(

)

(

)





x (CA n)


= 14.7 psi + 9.09 psi + 20 psi

= 43.79 psi





( )



140

1.8 NaOH Storage (S-105)

Calculation

Storage tank functioning as a repository of NaOH before used in vanillin

production process. To calculate the dimensions of the tank needs to know the

total volume of the tank. The total volume of the tank is calculation of tank


using are:







(

)

(

)





x (CA n)



141

= 14.7 psi + 19.72 psi + 20 psi

= 54.42 psi





( )


2. Plate and Frame Filter

2.1 Plate and Frame Filter (PF-101)

Sizing Calculation :

1. Component mass and volume

Component input mass

(ton) output

mass (ton)

Density

(ton/m3)

input volume

(m3)/ batch

output volum

(m3)/ batch

Lignin Alkali 2 2 1.3 1.54 1.54

Water 3.91 3.91 1 3.91 3.91

Lean Liquor 18.45 13.78 1 18.45 13.78

Liquid Acid 0.31 0.31 1 0.31 0.31

lean liquor solid 0 4.67 1 0 4.67

Total 24.68 24.68 13.35 24.22 24.22

Total Mass

Filtrate

18.01

Total

VolumFiltrat 18.01

Total Mass

Cake

6.67

2. Filtrate density

( )

( )

3. Cake density


142

( )

( )

4. Thickness of cake (L)

Estimated thickness of cake is = 0.06 m

5. Estimated cake porosity

Cake porosity ( ) of black liquor with pH 9 at 30°C = 0.7

6. Dry solid per unit area ( )

( )

( )

kg/m2

7. Effective filtration area (A)

m2

8. Safety factor = 20%

9. Filtration area (A)

( )

10.In this design, we use press filter with the filter area 2 x 2 m (4 m2) and

have 50 chambers. So, total press filter that we need for this process is:

And total minimum plate required is:


143

2.2 Plate and Frame Filter (PF-102)

Sizing Calculation:

1. Component of lignin Slurry

Component input

mass (ton)

output

mass

(ton)

Density

(ton/m3)

input

volume (m3)/

batch

output

volum (m3)/

batch

Lignin 5 5 1.3 3.85 3.85

alkali sulfate 5.29 5.29 2.66 1.99 1.99

Liquid Acid 23.93 23.93 1 23.93 23.93

water 3.42 3.42 1 3.42 3.42

total 37.64 37.64 33.18 33.18

total mass filtrate

32.64

Volume

filtrate 29.34

total mass cake

2.5

2. Filtrate density

3. Cake density




Cake porosity ( ) of black liquor with pH 3 at 30°C = 0.33


( )

( )

kg/m2


144


m2



( )

10.In this design, we use press filter with the filter area 1.5 x 1.5 m (2.25 m2)

and have 24 chambers. So, total press filter that we need for this process

is:

And total minimum plate required is:

3 Pump

3.1 Black Liquor Pump (P-101)&(P-102)

Operation Condition :

Psuction= 100,000 Pa

Pdischarge= 105,000 Pa

T = 600 C

Mass Rate = 66.77 ton/h

Density = 1818.2kg/m3

Liquid Viskosity = 5.09 cP

Pump design :

( ) ( ) (Timmerhaus, 2004)


145

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification:

Nominal Measure: 6 inch

Schedule number : 40

Inner Diameter (ID) : 6.065in

Outer Diameter (OD) : 6.625 in

Inside sectional area : 28.9 inch2

Velocity,

Reynold Number:

(aliran turbulen)

To get the value of the friction factor, used 6:10 on the book charts Noel de

Nevers (1991), in which the first note ε / D. To pipe the design of this plant, used

types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is

known for stainless steel pipes , value ε = 0,000046 m.

So, value ε/D = 0.0029

From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) =

0,0034

Assumption of friction loss in the pipe is relatively the same.

Friction loss :

Number of

Velocity

Equivalent pipe

diameter

Tank outlet 0.5 25

Tank inlet 1 50


146

Gate valve 0.3 15

4 elbow 9 450

Total 10.8 540

Extra Length of Pipe:

Total Length

Pressure Drop

Pressure Drop = 4381.08 N/m2

Head : 3.87 m

Pressure Differences : 5000 N/m2

Efficiency

Eff = 82.77%

From Energy Balance, So we can get,

W : 43.08 J/kg

Power : 0.32 kWh/operation

3.2 Black Liquor Acidification Pump (P-102)




147


T = 600 C


Density = 1020kg/m3


Pump design :

( ) ( ) (Timmerhaus, 2004)







Velocity,

Reynold Number:

(Turbulen Stream)







0,0034



148

Friction loss :

Number of

Velocity

Equivalent pipe

diameter

Tank outlet 0.5 25

Tank inlet 1 50

Gate valvle 0.3 15

4 elbow 6 300

Total 7.8 390


Total Length

Pressure Drop


Head : 4.58 m

Pressure Differences : 595,000 N/m2

Efficiency

Eff = 82.49%


W : 629.46 J/kg

Power :2.35 kWh/operation

3.3 Lignin Acidification Pump (P-103)




T = 600 C


149




Pump design :

( ) ( ) (Timmerhaus, 2004)







Velocity,

Reynold Number:

(Turbulen Stream)







0,0034


Friction loss :

Number of

Velocity

Equivalent pipe

diameter


150

Tank outlet 0.5 25

Tank inlet 1 50

Gate valvle 0.3 15

4 elbow 9 450

Total 10.8 540


Total Length

Pressure Drop


Head : 3.16 m


Efficiency

Eff = 81.98%


W : 368.26 J/kg


3.4 Lignin Solution Pump (P-104)




T = 600 C




151

Liquid Viskosity = 2.08cP

Pump design :

( ) ( ) (Timmerhaus, 2004)


Nominal Measure: 4inch





Velocity,

Reynold Number:

(Turbulen Stream)







0,0035


Friction loss :

Number of

Velocity

Equivalent pipe

diameter

Tank outlet 0.5 25

Tank inlet 1 50

Gate valvle 0.3 15


152

4 elbow 3 150

Total 4.8 240


Total Length

Pressure Drop


Head : 3.12 m


Efficiency

Eff = 79.83 %


W : 32.32 J/kg


3.5 Lignin Solution Pump (P-105)




T = 600 C





153

Pump design :

( ) ( ) (Timmerhaus, 2004)







Velocity,

Reynold Number:

(Turbulen Stream)







0,0035


Friction loss :

Number of

Velocity

Equivalent pipe

diameter

Tank outlet 0.5 25

Tank inlet 1 50

Gate valvle 0.3 15

4 elbow 3 150

Total 4.8 240


154


Total Length

Pressure Drop


Head : 4.48 m


Efficiency

Eff = 81.32 %


W : 44.53 J/kg


3.6 Vanillin Slurry Pump (P-106)




T = 600 C


Density = 1609kg/m3


Pump design :


155

( ) ( ) (Timmerhaus, 2004)


Nominal Measure: 1.5inch





Velocity,

Reynold Number:

(Turbulen Stream)







0,0055


Friction loss :

Number of

Velocity

Equivalent pipe

diameter

Tank outlet 0.5 25

Tank inlet 1 50

Gate valvle 0.3 15

4 elbow 3 150

Total 4.8 240



156

Total Length

Pressure Drop

Pressure Drop = 52,223 N/m2

Head : 0.34 m


Efficiency

Eff = 79.73 %


W : 94.83 J/kg


3.7 Vanillin Solution Pump (P-107)




T = 600 C




Pump design :

( ) ( ) (Timmerhaus, 2004)


157


Nominal Measure: 1.5 inch





Velocity,

Reynold Number:

(Turbulen Stream)







0,0055


Friction loss :

Number of

Velocity

Equivalent pipe

diameter

Tank outlet 0.5 25

Tank inlet 1 50

Gate valvle 0.3 15

4 elbow 3 150

Total 4.8 240


Total Length


158

Pressure Drop

Pressure Drop = 52,223 N/m2

Head : 0.34 m


Efficiency

Eff = 79.69 %


W : 50.12 J/kg


3.8 Water Pump (P-108)




T = 600 C


Density = 1000kg/m3


Pump design :

( ) ( ) (Timmerhaus, 2004)


Nominal Measure: 1.5 inch



159




Velocity,

Reynold Number:

(Turbulen Stream)







0,005


Friction loss :

Number of

Velocity

Equivalent pipe

diameter

Tank outlet 0.5 25

Tank inlet 1 50

Gate valvle 0.3 15

4 elbow 6 300

Total 7.8 390


Total Length

Pressure Drop


160


Head : 4.58 m


Efficiency

Eff = 76.51 %


W : 639.97 J/kg



Diameter and height of the reactor:

(

)

(

)

Where; D is diameter of the tank and H is height of the tank.From the



Thick walls of the tank:


161

P (psig) = P operation (psia) + Pstatis + safety factor

= 159,7 psia + 14.7 psia + 25 psia

= 199,4 psia

= 184,7 psig

S = Allowable stress, for Stainless Steel 316 = 74500 psig

E = Joint efficiency = 0.8 (Walas, 1988)

R = D/2 = 0,8465 m = 33,32 in

Corrosive factor = 0.15 in

4 Bubble Column Reactor

Stoichiometry 1 Conversion 70%

Lignin Oxidation : 0.5 L + 1.56 O2 --> V + 114 X

Initial (mol) 2350.242 10781.25

Change (mol) -1645.17 -7332.75 4700.483

Remaining

(mol) 705.0725 3448.496 4700.483

Stoichiometry 2

Vanilin Oxidation : V + O2 --> Product

Initial (mol) 4700.483 3448.496

Change (mol) -3290.34 -3290.34 3290.338

Remaining

(mol) 1410.145 158.1582 3290.338

massa 500592.048 gram


162

0.50059205 ton

500.592048 kg

Reactor Volume = 25.51 m3

Reactor functioning as a tank to mix and react lignin slurry with oxygen in

alkaline condition. To design bubble column reactor, the dimensions of the reactor

needs to know the total volume of the reactor. In the design of reactor, the

assumptions used are:

- Ratio of height to diameter of the bubble column reactor is 5:3


Diameter and height of the reactor:

(

)

(

)

Where; D is diameter of the tank and H is height of the tank. From the results of

calculation and rounding up to 0.1 m, height and diameter of the tank is obtained

respectively 4.48 m and 2.69 m.


x (CA n)


163


= 145 psi + 6787 psi + 20 psi

= 174.84





( )


5 Ultrafiltrasi

Sizing Calculation :

Component mass and volume

Component Input mass

(ton)

Output

mass (ton)

Density

(ton/m3)

Input

volume

(m3)/

batch

Output

volume

(m3)/

batch

Vanillin 0.500 0.500 1.05 0.476 0.476

Alkali Lignin Slurry 5.360 0.000 1.22 4.393 0

Water 1.200 1.200 1 1.200 1.200


164

Others 4.780 0.000 1 4.780 0

Filtrate Cake 0.000 10.140 1.3 0 7.800

Total 11.840 11.840 10.849 9.476

total mass filtrate 1.700 volum

filtrat

1.676

Filtrate density

( )

( )

3. Cake density

( )

( )




Cake porosity ( ) of product = 0.2


( )

( )

kg/m2



165

m2



( )

10.In this design, we use hollow fiber ultrafiltration with the filter area 190 m2 and

have 10000 fibers per module. So, filter that we need for this process is:

6 Spray Dryer

Surface moisture is removed in about 5 sec, and most drying is completed in less

than 60 sec. Parallel flow of air and stock is most common. Atomizing nozzles

have openings 0.012-0.15 in. and operate at pressures of 300-4000 psi. Atomizing

spray wheels rotate at speeds to 20,000rpm with peripheral speeds of 250-600

ft/sec. With nozzles, the length to diameter ratio of the dryer is 4-5; with spray

wheels, the ratio is 0.5-1.0. For the final design, the experts say, pilot tests in a

unit of 2 m dia should be made.

Diameter of particle,

= 55,65 μm

T air inlet = 120oC

T air oulet = 110oC

T feed inlet = 80oC

T feed outlet = 90oC


166

Design aspect include : Atomizer : its type & design, flow rate of the heated inlet

air, settling velocity, solid & Gas operating velocity, chamber Diameter, residence

time, design of Conical bottom.

Atomizer : Centrifugal disk atomization is particularly advantageous for

atomizing suspensions and pastes that erode and plug nozzle. Type of Disk

atomizer (Vane, Kesner, Pin) Ref. patent US20040139625. Diameter of the disk

atomizer 5-45 cm. Rotational speed 33.000 rpm, peripheral speed 6000 m/min.

Mean particle size 55 micron.

Feed Rate = 730 kg/hr = 24 lb/min

Peripheral speed is got from Herring and Marshal chart (peripheral speed vs.

mean particle diameter, with feed rate as parameter). On interpolation we get 473

ft/s (v =8952 m/min).

Disk Selection

Disk selected = B-1, with diameter 0,59 ft. Vane height= 0,406 ft, vane length = 1

ft, number of vanes = 60.

Rotational speed (N) =

N = 473 * 60 = 15800 rpm

So, power consumption of atomizer can be calcaulated below

( )


167

Spray Chamber design


168

X1 = 0.015, X2 = 0.003

Y1 = 0.01317 (by psychometric chart at given DB & WB) humidity air

HL1= 112.2 kJ/kg of dry solid, HL2= 121.68 kJ/kg of dry solid

H1= 134.29 kJ/kg dry air

Simultaneously solving mass balance and enthalpy balance eq (1) and (2) we get

Y2= 0.0206

Evaporation rate of water = (0.015-0.003)*1500 kg/hr = 18 kg

Assumed chamber efficiency is 70%, therefore net evaporation rate of water is

18/0.7 =25.71 kg water /hr.

Moisture removed per kg of dry air = (0.0206-0.01317)=0.00743 kg water per kg

of dry air.

Gs = 25.71/0.00743 = 3460 kg/hr.

After this we must calculate humid volume


169

Humid volume inlet (Vin) = 0.283 m3/kg dry air

Humid volume outlet (Vout) = 0.281 m3/ kg dry air

Vavg = (Vin + Vout)/2 = 0.282 m3 / kg dry air

Assume Dp = 100 micron

And then we calculate operating velocity. The operating velocity in the case of

non-dusting spray dryer is taken as two times the settling velocity of the drop.

Settling velocity didapatkan berdasarkan perhitungan adalah sebesar 0.25 m/s.

Stoke’s law is applicable if Re < 2. So we must check the reynold number

So we can get operating velocity, va= 2vs = 2*0.25 = 0.5 m/s

Column Area: ( )

= 3.1 m2


170

Column diameter : √

= 1,974 m, for safety, assuming 15 % safety

factor, Dc = 2.1 m.

Residence time : √

Time required to evaporate moisture from droplet :

Өp = 0.00969 sec, Өp < td, design is acceptable

Chamber is a cylindrical with a conical bottom

Total volume of chamber (Vt) = Gs*Vav*td = 5.2 m3

Minimum height of cylindrical portion (hmin) = vs*Өp = 0.00068 m

Recommended height of cylindrical portion (hcyl) = 0.6 *Dc = 1.47 m

Volume Cone =

= 3.1 m3

Height of cone (hcone) =

m

Cone angle : tan(a/2) = Dc/2hcone

a = 20.57 degree

Thickness of chamber : tmin = (Dc+100)/1000 = 0.11 inch


171

7. Material Safety Data Sheet (MSDS)

1. Black Liquor

Properties Information

Molecular Weight (g/mol) Not available

Melting Point (0C) Not available

Boiling Point (0C) Variable

Form Slurry

Odor rotten egg odor

pH Typical Range 10-12

Color Black liquid

Solubility Soluble in cold and hot water

Flammability

Not flammable, will burn at very

high temperatures

Materials to avoid Aluminum and acids. Contact with

acids and oxidizing agents can

result in release of potentially lethal

concentrations of hydrogen sulfide

(H2S) gas

Corrosivity Corrosive with aluminum

Toxic effect Causes eye and skin irritation and

corrosion; respiratory airways

irritation if ingested in large

amounts : digestive tract irritation

and corrosion,

vomiting, diarrhea, and death

(possible)

Handling Do not contact with eyes, skin,

and clothing. Do not be inhaled

Do not contact with the acid

Storage Keep away from acids and

aluminum

Personal protective equipment Gloves, respirator, eye protection,

goggles and footwear

Spill procedures Open ventilation and insulation use


172

a shovel to dispose of spill

2. H2SO4


Molecular Weight (g/mol) 98

Melting Point (0C) 10.36

Boiling Point (0C) 100

Form Liquid

Odor Odorless

pH Typical Range 2-3

Color Transparent

Solubility Soluble in cold and hot water

Flammability Easy to flammable

Materials to avoid Organic material, metal, acids, and

alkali

Corrosivity Corrosive with aluminum, stainless

steel (304,316), not corrosive with

glass

Toxic effect Causes eye irritation and burn if

contact with skin.


and clothing.

Storage Keep in closed container, cool, and

good ventilated



Spill procedures Spare with soil, sand, and not

flammable material


173

3. NaOH


Molecular Weight (g/mol) 40

Melting Point (0C) 323

Boiling Point (0C) 1388

Form Solid

Odor Odorless

pH 13.5 (Basic)

Color White

Solubility Easily soluble in cold water

Flammability Not flammable

Materials to avoid Aluminum

Corrosivity Very caustic to aluminum and other

metals in presence of moisture.

Toxic effect Causes damage to the following

organs: lungs


and clothing.

Storage Keep in closed container and cool



Spill procedures Insulation use a shovel to dispose of

spill


174

REFERENCE

A, m. Z., silva, e. B., & rodrigues, a. (2007). Recovery of vanillin from

lignin/vanillin mixture by using tubular ceramic ultrafiltration membranes.

Journal of membrane science , 221–237.

Araújo, j. D. (2008). Production of vanillin from lignin present in the kraft black

liquor of the pulp and paper industry. Biological and chemical engineering .

Araújo, j. D., grande, c. A., & rodrigues, a. E. (2010). Vanillin production from

lignin oxidation in a batch reactor. Chemical engineering research and

design , 1024–1032.

Heradewi. (2007). Isolasi lignin dari lindi hitam proses pemasakan organosolv

serat tandan kosong kelapa sawit (tkks). Bogor: institut pertanian bogor.

Jo, j. D., grande, c. A., & rodrigues, a. E. (2009). Structured packed bubble

column reactor for continuous production of vanillin from kraft lignin

oxidation. Journal of catalysis today , s330-335.

Peters, m. S., & timmerhaus, k. D. (1991). Plant design and economics for

chemical engineers. New york: mcgraw-hill.

Priefert, h., rabenhorst, j., & steinbüchel, a. (2001). Biotechnological production

of vanillin. Appl microbiol biotechnol , 56:296–314.

Silvaa, e. B., zabkovaa, m., araújoa, j., c.a. Catetob, c., & barreirob, m. (2009). An

integrated process to produce vanillin and lignin-based polyurethanes from

kraft lignin. Chemical engineering research and design , 1276–1292.

Sinnott, R. K. (2005). Chemical Engineering Design, Vol. 6. Butterworth-

Heinemann: Elsevier.

Tomani, p. (2009). The lignoboost process. Cellulose chemistry and technology .


175

final report group 6.pdf

Documents

process description

mass balance process

plant development analysis

process design

energy balance

overall mass balance

type of process

plant development background