synthesis, characterization and application of ...°刷修改版 pp233-244.pdf · the present...

U. Rafique et al. / Journal of Water Sustainability 4 (2012) 233-244 1

* Corresponding to: [email protected]

Synthesis, Characterization and Application of Nanomaterials for

the Removal of Emerging Pollutants from Industrial Waste Water,

Kinetics and Equilibrium Model

Uzaira Rafique1*, Anum Imtiaz

1, Abida K. Khan

2

1Department of Environmental Sciences, Fatima Jinnah Women University, The Mall Rawalpindi, 46000 Pakistan. 2Institute of Information Technology, Abbottabad Campus, KPK

ABSTRACT

Nanotechnology is an emerging science offering promising models of decontamination. The present experimental

design is to synthesize novel nanoparticles of Iron and Nickel oxides to be used as catalysts for in situ removal of

different pollutants discharged from various industries. Particle size of synthesized iron and nickel oxides

nanoparticles was characteristic of ~28-36 nm and ~48-56, respectively done with help of SEM and XRD analysis.

Furthermore, the linkage of metal-oxygen linkage and red shift is confirmed through FTIR and UV-Visible

spectroscopic technique, respectively. Physico-chemical characterization of industrial effluents showed remarkably

higher concentration of nitrates and sulphates. Nitrates and sulphates were abundantly concentrated in leather

industry effluents, designating it most polluted chemical processing industry. These results directed application of

nanoparticles as adsorbents for selected removal of Nitrates and sulphates from wastewater in batch experiments.

Concentration of the pollutants like sulphates and nitrates was reduced to 18 and 54 times, respectively, lower than

the background concentration on application of Ni oxide nanoparticles. Kinetics model revealed pseudo second

order whereas Langmuir and Freundlich equilibrium gave comparable fitness to adsorption data with regression

coefficient of 0.999. The study concludes that nanotechnology provides potential and economically viable solution

for removal of wastewater pollutants through synthesis of metal nano adsorbents.

Keywords: Nanotechnology; synthesis; wastewater treatment; emerging pollutants; adsorption; isotherms and

kinetics

1. INTRODUCTION

Nanotechnology is an emerging science with

wide applications in the remediation of envi-

ronmental pollutants. In recent years, a great

deal of attention has been focused on the syn-

thesis and application of nanostructure mate-

rials as adsorbents or catalysts to remove tox-

ic and harmful substances from water and air.

Resurgence to synthesize and manipulate

nanoparticles finds use in improving air, soil

and water quality in the environment. Reac-

tive nanoparticles have a significant amount

of surfaces and thus attract much interest to be

applied as adsorbents in comparison to ma-

cromolecules. Various nanoparticles have

been applied in removing radionuclides, ad-

sorption of organic dyes, remediation of con-

taminated soils, and magnetic sensing. Metal

oxides play a significant role in many fields of

nanotechnology including nanocatalysis, sens-

ing, supermagnetic properties, nanoenergy

Journal of Water Sustainability, Volume 2, Issue 4, December 2012, 233–244

© University of Technology Sydney & Xi’an University of Architecture and Technology

Presented at the International Conference on the Challenges in Environmental Science and Engineering

(CESE-2012), Melbourne, Australia, 9–13 September 2012.

234 U. Rafique et al. / Journal of Water Sustainability 4 (2012) 233-244

storage and conversion, fuel cells, and elec-

troceramics (Bao et al., 2001; Gao et al., 2001;

Braos-Garcı´a et al., 2003; Liang et al., 2004;

Seto et al., 2005; Tian et al., 2005; Jeon et al,

2005, 2006). The compounds and nanomate-

rials of iron and nickel having low dimensions

have always been the subject of study due to

their diverse applications in the fields of elec-

tronics, catalysis, magnetics etc. (Chen et al,

2009; Dominguez- Crespo, 2009; Libor and

Zhang, 2009; Qiao et al., 2009; Masoud and

Fatemeh, 2009; Kassaee et al; 2011; Somaye

et al., 2011).

Synthesis is an important aspect of nano-

technology. An entirely new set of physical

properties and applications of nanomaterials

depends on the choice of selection procedure.

Remarkable achievements in innovative syn-

thetic routes and growth mechanisms have

been made to obtain desired size crystal, mor-

phology, microstructure and chemical compo-

sition. The sizes of nanoparticles are usually

confined to less than 100 nm and such small

sizes confer unique properties that are fre-

quently different from the properties of bulk

materials (Kannan and Sundaram, 2001;

Zhuang and Wang, 2001), making them ideal

for certain applications.

During synthesis of the nanoparticles con-

trol on nucleation and growth and agglomera-

tion stages are the important stages which

need to be controlled appropriately which is

only possible by co-precipitation method. Co-

precipitation method has been adopted to syn-

thesize the metal oxide nanoparticles as it

promise to provide not only smaller size par-

ticles as compare to solvothermal or hydro-

thermal method but also stable particles as

well. Surfactant assisted method leaves the

traces of surfactants on the surface of NPs

causes unavailability of surface to the adsor-

bents due to which the efficiency is reduced

(Bangash and Alam, 2004).

Various preparation techniques, such as

sol-gel pyrolysis method (Sun et al., 2000),

hydrothermal technique (Jing et al., 2006) and

mechanical alloying (Ponder et al., 2000) has

been used to prepare ferrite nanoparticles, but

co-precipitation method is considered to be an

economical way of producing fine particles

(Hu et al., 2004; Ko et al., 2007) .

The present study has two-fold significance.

It offers simple synthesis method for metal

and metal oxide particles and its application

for the removal of pollutants like sulphates

and nitrates from industrial wastewater. Struc-

tural properties of synthesized metal oxides

are also investigated to understand the me-

chanism. Different kinds of adsorbents have

been developed for the treatment of waste wa-

ter (Kannan and Sundaram, 2001). Metal

oxide particles enjoy a unique position having

a significant amount of surfaces, thus, attracts

much interest as potential adsorbents because

of exclusive properties and potential applica-

tion (Sun et al., 2000).

1.1 Objectives

Synthesis of nanoparticles by different me-

thods.

Application of nanoparticles for removal

of emerging pollutants from industrial ef-

fluent or waste water.

Can nanoparticles be used for the selective

removal of pollutants like sulphates and ni-

trates.

Specificity of the nanoparticle with respect

to specific pollutants.

2. MATERIALS AND METHODS

Nanoparticles were synthesized by using two

different methods in order to check which me-

thod gives best yield and particle size of the

adsorbents.

2.1 Synthesis of metal particles

(Solvothermal direct method)

The Ni-bipyridine (sample 1) and Fe-

bipyridine (sample 2) complexes were pre-


pared separately by a direct reaction between

nickel chloride and iron chloride with 4,4-

bipyridine following solvothermal method.

Nickel chloride (0.1 mol) and 4,4-bipyridine

(0.1 mol) were dissolved in 2-propanol (100

ml) separately. Then 4, 4- bipyridine solution

was added drop wise to the metal salt solution.

All chemicals were mixed with vigorous stir-

ring, using a magnetic stir bar and refluxed at

80 0C for 10 hours and then cooled to room

temperature. When the reaction was complete,

greenish precipitates were collected and

washed with dry ether of analytical grade sev-

eral times to remove impurity. The final prod-

uct was dried under vacuum at 60 0C over-

night.Sample (b) was also synthesized in the

same way with white precipitates. The

grinded samples were then placed in argon

fitted carbolite furnace for sintering. The

samples were calcined under inert atmosphere,

and then final product was dried.

2.2 Synthesis of metal oxide particles

(Co-precipitation method)

Particles of Iron and Nickel were synthesized

using co-precipitation method (Patricia et al.,

1999; Chakrabarty et al., 2009). The proce-

dure layout is as follows:

Acidic solution of 4.0mL of FeCl3 and 1.0

mL of FeCl2 (1:2 molar ratio, respectively)

was thoroughly stirred for 10-15min followed

by addition of 1.0M NaOH solution till the

appearance of black precipitate. Strong mag-

net was used to settle the particles at the base

of beaker and supernatant was discarded. Par-

ticles were kept in desiccators. Percentage

yield was calculated to be 80%.

Nickel oxide particles were synthesized by

drop wise addition of aqueous solution of

NaHCO3 (1.5 gm in 10 mL water) to the con-

tinuously stirring aqueous solution of NiCl2

(2.3 gm in 10 mL distilled water). The preci-

pitates obtained were centrifuged, washed re-

peatedly with distilled water and dried in oven

at 100°C. Percentage yield of synthesized Ni

particles is calculated to be 63%.

2.3 Characterization of adsorbents

The synthesized metal oxides particles were

characterized with the help of FTIR (FTIR

8400, Shimadzu), UV-Visible (UV-1601

Shimadzu) spectrophotometer, SEM (JSM-

6490A JEOL) and XRD (Model, Theta-Theta).

2.4 Batch adsorption

Time-dependent batch experiment was con-

ducted for the study of adsorption of sulphates

and nitrates and other compound using the

synthesized materials. The following general

procedure was used for a batch experiment.

The synthetic solution of sulphate and ni-

trate with known concentration (10 mg/L, 20

mg/L) was prepared at neutral pH. A known

volume (10 mL) each was pipette into the se-

ries of cultural vial to which 1mg of the syn-

thesized materials as adsorbent was added.

Upon completion of the given contact time (in

minutes) between adsorbent and adsorbate,

the solution was filtered. The filtrate was de-

termined with the help of UV spectrophoto-

meter for metal nitrate and sulphate concen-

tration. The standard Turbid-metric (4500-

SO4) and Ultraviolet spectrophotometric

screening (4500-NO3) methods are used for

the sulphates and nitrates analysis (APHA,

2005). Each batch experiment was repeated

with varying pH and induced concentration of

metal salt solution.

2.5 Kinetics studies

In order to study the kinetics of the adsorption

process, first order, pseudo first order, pseudo

second order and intra particle diffusion equa-

tions were applied. The conformity between

experimental data and the model predicted

values is expressed by the correlation coeffi-


cient (R2, values close or equal to 1). A rela-

tively high R2 value indicates that the model

successfully describes the adsorption kinetics

(Fadali et al., 2005).

2.6 Adsorption isotherms

Adsorption equilibrium models of Langmuir

(Langmuir, 1918) and Freundlich (Kalavathy

et al., 2005) were applied to determine the

relationship of sulphate and nitrate adsorption

with different induced concentration. The best

fitting isotherm was evaluated by linear re-

gression, and the parameters (Lalhruaitluanga

et al., 2010) obtained from the intercept and

slope of the linear plots of these models.

3. RESULTS AND DISCUSSION

3.1 Characterization of adsorbents

The synthesized metal oxide particles were

run on FTIR (FTIR 8400, Shimadzu) and UV-

Visible (UV-1601 Shimadzu) spectrophoto-

meter for characterization. FTIR spectrum of

Fe3O4 is represents two absorption bands at

around 592 and 630 cm-1

which is due to the

presence of Fe-O bond of Fe3O4 (Figure 1).

Peaks at 2962 cm-1

attributed to different C-H

band vibrations, peaks appeared at 1261.49

cm-1

is due to C-O stretching showing the ab-

sorption of atmospheric water and CO2. FTIR

of NiO shows the band in 700 to 800 cm-1

range assigned to Ni-O stretching vibrations

mode the broadness of band indicates that

NiO powders are nanoparticles (Korosec et al.,

2003) as shown in the Figure 1.

The broad absorption band centered at 3440

cm−1

is attributable to the band O–H stret-

ching vibrations and the weak band near 1635

cm−1

is assigned to H–O–H bending vibra-

tions mode. The jagged absorption bands in

the region of 1000–1500 cm−1

are assigned to

the O-C=O symmetric and asymmetric stret-

ching vibrations and the C–O stretching vi-

bration, but the intensity of the band has wea-

kened, which indicated that the ultrafine pow-

ers tend to strong physically absorption to

H2O and CO2 (Qiao et al., 2009). FTIR spec-

trum of composite showed both the Fe-O and

Ni-O bands.

Figure 1 FTIR spectrum of Iron oxide Particles


UV-VIS indicates blue shift in the bands

which may be due to the presence of small

sized nanoparticles, moreover according to

Mie theory that absorbance increases in nano-

particles (Somaye et al, 2011). Metal clusters

also show cluster size effects in optical spec-

tra (Pinchuk et al, 2008).

A Scanning Electron Microscope (SEM)

image of catalysts was characterized using

Hitachi SEM SU-1500. The surface morphol-

ogy and geometry of the metal nanoparticles

studied by SEM and the result are presented

here for Ni and Fe particles (Figure 2) The

SEM image depicts the uniformity of the

Nickel NPs with size range 150- 250 nm. The

SEM image of Fe iron particle at low resolu-

tion reveals the dispersion of Fe-particle with

relatively less uniformity and low size range

150-200nm as well.

The typical SEM images of iron oxide and

nickel oxide particles (Figure 3) show the non

spherical shape. From the image it is seen that

a large number of particles are present and if

we consider single one then calculated aver-

age size is to be nearly equal 36 and 48nm for

iron and nickel respectively.

However the SEM results (Figure 3a and

3b) showed the particles synthesized by

adopting co-precipitation method show quite

smaller size less than 100 nm (20-39.6 nm for

Fe and 32-56.57 nm for Ni) as compared the

metal particles synthesized by solvothermal

method (Figure 2). Co-precipitation method is

typical used and most preferred method for

the synthesis of spherical smaller size NPs

with high degree of uniformity.

The details XRD patterns of the NiO nano-

particles are shown in Figure 4. All the reflec-

tion peaks with relative intensities of different

planes, indexed in the figure, specify the pres-

ence of NiO. The well crystalline nature of

the prepared sample is easily being observed

with the sharpness and the intensity of the

peaks.

The XRD results (Figure 5) of the iron

oxide nanoparticles indicated all the samples

were in face centered cubic phase and in spin-

al structure according to the standard JCPDF

file (card no-25-1402).

(a) (b)

Figure 2 SEM image of (a) Ni Particles and (b) Fe Particles


(a) (b)

Figure 3 SEM image of (a) Iron oxide particles and (b) Nickel oxide particles

Figure 4 X-ray diffraction pattern of Nickel oxide Particles


20 30 40 50 60 70

0

20

40

60

80

100

120

Inte

nsi

ty (

a.u

)

2 Theta (Degree)

(311)

(220)

(111)

(400)

(422)

(511)

(440)

Figure 5 X-ray diffraction pattern of Iron oxide Particles

3.2 Batch adsorption

The present study is designed to devise a de-

contamination model for the removal of ni-

trates and sulfates using synthesized materials.

For this purpose synthetic batch experiments

were designed separately for each material at

optimum operating conditions described

elsewhere (Imtiaz and Rafique, 2011). Series

of Batch experiments were conducted. The

variables used were (a) adsorbate concentra-

tion of 10 mg/L and 20 mg/L; (b) adsorbent

mass of 1 mg; (c) pH 7 (neutral). However,

the optimum concentration of the adsorbate

was found to be 10 mg/L from adsorption ex-

periments showing optimum removal of sul-

phates and nitrates.

All the plots throughout the manuscript are

constructed on the data at optimum operating

parameters of the experiment. It is concluded

from the experiments that lower concentration

of 10 mg/L of the adsorbate, 1mg of the ad-

sorbent dosage and the neutral pH are the op-

timum conditions for this study (Figure 6

showed the optimum concentration of adsor-

bate).

The results graphically presented in Figure

7 depict the efficiency of particles of nickel

and Iron oxides for the removal of aqueous

pollutants. Nitrates are removed to an opti-

mum percentage of 58% and 67% on iron

oxide and nickel oxide particles, respectively.

The results are comparable to reported in lite-

rature (Li et al., 2008; Kasaee et al., 2011).

The sulfates removal was also attempted

which shows a relatively lower percentage of

removal efficiency. It is interesting to note

that efficiency of both particles in removing

sulfates is comparable in contrast to response

for nitrates. However, on cumulative basis, it

can be deduced from the results that nickel

oxide particles are better candidate for the

removal of both inorganic pollutants.

3.3 Kinetic studies

Different kinetic models including first or-

der, pseudo first order, and pseudo second

order and intra particle diffusion equations

were applied to determine the mechanism in-

volved in adsorption process.


(a) (b)

Figure 6 Removal (in %) of (a) Nitrates and (b) Sulfates by Fe and Ni Metal oxide particles at

optimum concentration (10 mg/L) of adsorbate

(a) (b)

Figure 7 Removal (in %) of (a) Nitrates and (b) Sulfates by different Metal Particles

The sorption kinetics may be described by

a simple first order equation (Khan et al,

2007).

0ClogtCtlog + 2.303

k =

1

The sorption kinetics may also be described

by a pseudo first order equation (Ozacar,

2003). The integral form of the model is

tk

qqq ee303.2

loglog 1

The adsorption kinetics may also be de-

scribed by a pseudo second-order equation

(Ho et al, 2001) the differential equation of

this model is as follows:

tqqkq eet

111

22

The intra-particle diffusion model is ex-

pressed as (Ayres et al., 1994)

taloglogklogR id


3.4 Adsorption isotherm model

Adsorption models of Langmuir and Freun-

dlich were applied to determine the relation-

ship of nitrates and sulfates adsorption with

different induced concentration. The best-

fitting isotherm was evaluated by linear re-

gression, and the parameters obtained from

the intercept and slope of the linear plots of

these models.

Estimation of maximum adsorption capaci-

ty corresponding to complete monolayer cov-

erage on the nanomaterials was calculated us-

ing the Langmuir isotherm model since the

saturated monolayer isotherm can be ex-

plained by the non-linear equation of Lang-

muir Equation:

max

e

maxe

e

q

C

Lq

1

q

C+

K=

Freundlich isotherm is capable of describ-

ing the adsorption of organic and inorganic

compounds on a wide variety of adsorbents

(Kalavathy et al., 2005). The Freundlich eq-

uation is expressed as:

Clogn

1Klogqlog eFe +=

The adsorption Isotherms and Kinetics is

applied on the present study using Nickel and

Iron particles as adsorbents for the removal of

nitrates and sulphates. The data is

summarized in Table 1. The higher R2 values

reveals that isotherms of Freundlich and

Langmuir are in best agreement (R2

= 0.999

for Nitrates and R2 > 0.96 for Sulphates). The

fitness of both Isotherms is also reported by

(Hosik et al., 2009) for the adsorption of As

(V) onto maghemite nanoparticles. Kinetic

studies also stated that it follows the Pseudo

second order which is supported by (Ho and

Chiang, 2001; Wu et al., 2001; Hossain et al.,

2005).

Table 1 Calculation of Parameters of Nitrates and Sulfates using Fe and Ni Particles

Adsorption

Isotherms

Metal

Particles Nitrates Sulfates

Langmuir NN

KL qm R2 KL qm R

2

0.2315 -0.2715 0.9995 2.3807 -15.046 0.9999

FN 0.3433 -0.7184 0.9994 4.3786 -30.831 0.9666

Freundlich

KF n R2 KF n R

2

NN 1.0963 -0.5212 0.9999 3.8038 -3.8786 1

1.2921 -0.8479 0.9999 5.2062 -5.4411 0.9916

Kinetic Models

1st Order NN

Co K1 R2 Co K1 R

2

0.5559 -0.0044 0.8888 0.9033 -0.0004 0.8602

FN 0.6897 -0.0083 0.7092 0.953 -0.004 0.8962

Pseudo 1st Order NN

K1 qe cal. R2 K1 qe cal. R

2

-2E-07 4.8267 0.8957 -1E-07 4.3222 0.8597

FN -7E-07 4.7626 0.7102 -2E-06x 4.3404 0.8913

Pseudo 2nd

Order NN

K2 qe cal. R2 K2 qe cal. R

2

0.0095 0.1483 0.9998 0.0514 0.4733 0.9999

FN 0.0192 0.1705 0.9993 0.909 0.4081 0.9647

Intra-particle

Diffusion NN

α Kid R2 α Kid R

2

0.0084 1.8149 0.6281 0.0096 1.3075 0.663

FN 0.0305 1.7308 0.7103 0.1392 1.1257 0.6823


CONCLUSIONS

The following conclusions are drawn from the

present study:

The synthesis procedure adopted offer sim-

ple, economical and efficient method for

the preparation of Fe and Ni oxide particles

of reduced size, percentage yield being 80

and 65, respectively.

Co-precipitation method is better than sol-

vothermal method for the synthesis of the

spherical smaller size particle with high de-

gree of uniformity.

Nitrates and Sulfates are efficiently re-

moved by Nickel oxide and iron oxide nano

particles at optimum operating conditions

of pH 7, induced concentration 10 mg/L

and adsorbent mass of 1mg.

Nickel oxide NPs are proved to be better

candidate than Fe-oxide NPs.

FUTURE PROSPECTS

Formation of thin membrane of the nickel

oxide NPs which can be used in filters to

capture inorganic pollutants like nitrates

and sulphates from water.

Ni-oxide nanoparticles can be used in small

sachets or in form of pellets to remove the

toxic pollutants efficiently at low level from

water.

Recyclable/regeneratabe thin films on neu-

tral or active support can be formed for fil-

ters

Ni-oxide nanoparticles can be dispersed ho-

mogeneously on the nano-support to get better

efficiency.

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