dyeing of nylon 6 fibres with calendula officinalis 2

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1 Dyeing of Nylon 6 Fibres with Calendula officinalis & Casuarina cunninghamiana Extracts. R. M. Mohamed Fashion Department, Art & Design Academy, The High Institute of Applied Arts- 6 th October City, Giza Egypt Abstract Extraction and application of natural dyes for dyeing polyamide fibre , i.e. nylon 6 , were studied in details. Two different natural dyes from vegetable sources were selected for this study, namely: Calendula and Casuarina. Optimization of dyeing processes was carried out in detail. The amount of natural dyes that exhausted and fixed on the fibre was found to depend on the application conditions. By lowering the pH level of the dye bath the quantity of absorbed dye was found to increase. The optimum pH levels for attaining maximum colour strengths were at pH = 4 and 3 for Casuarina and Calendula respectively. Addition of electrolyte (NaCl) resulted in some decrease in the colour strength owing to its retarding action on the rate of dye absorption. The rate and degree of dye fixation on the nylon was found to increase greatly by raising dyeing temp. up to boiling. Natural mordant that extracted from Carob ( Ceratonia siliqua) and synthetic mordants were used for post-mordanting the dyed materials since reliable fastness properties were realized.

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Page 1: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

1

Dyeing of Nylon 6 Fibres with Calendula officinalis & Casuarina

cunninghamiana Extracts.

R. M. Mohamed Fashion Department, Art & Design Academy,

The High Institute of Applied Arts- 6th

October City, Giza – Egypt

Abstract

Extraction and application of natural dyes for dyeing polyamide

fibre , i.e. nylon 6 , were studied in details.

Two different natural dyes from vegetable sources were selected for

this study, namely: Calendula and Casuarina.

Optimization of dyeing processes was carried out in detail. The

amount of natural dyes that exhausted and fixed on the fibre was

found to depend on the application conditions. By lowering the pH

level of the dye bath the quantity of absorbed dye was found to

increase. The optimum pH levels for attaining maximum colour

strengths were at pH = 4 and 3 for Casuarina and Calendula

respectively. Addition of electrolyte (NaCl) resulted in some decrease

in the colour strength owing to its retarding action on the rate of dye

absorption. The rate and degree of dye fixation on the nylon was

found to increase greatly by raising dyeing temp. up to boiling.

Natural mordant that extracted from Carob (Ceratonia siliqua)

and synthetic mordants were used for post-mordanting the dyed

materials since reliable fastness properties were realized.

Page 2: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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1. Introduction

Pollution may be considered one of the most important problems in

the recent years. Therefore, a great concern with this problem was

appeared all over the world to find suitable and acceptable solutions

for reducing pollution of environment.

In fact there are three main methods for the reduction of pollution,

these are: elimination, substitution and treatment before release.

One of the most important and effective ways for reducing

pollution is the replacement of polluting materials and chemicals by

eco-friendly natural materials.

For realizing this aim and to prevent or minimize the toxicity and

allergic reaction of synthetic dyes, a new trial for dyeing and

mordanting polyamide fibers with natural dyes and mordants were

made.

Synthetic fibers rarely accept natural dyes; except nylon which can

be dyed but other synthetic fibers based on coal or petroleum do not

usually accept natural dyes.(3)

Some nylon for ladies' underwear is mordanted in chrome and dyed

with logwood chips and fustic.

Samples of nylon yarn were mordanted with Alum, Chrome, Iron

and Tin, then dyed with Golden rod, Weld, Onion skins, Madder,

Cochineal and Elderberry.

Wool and nylon 6 fabrics treated with oxygen, carbon tetra-

fluoride, and ammonia low temperature plasmas are dyed with several

natural dyes, such as cochineal, Chinese cork tree, madder and

gromwell. (19) The dyeing behaviour of natural dyes on nylon 6 fabric

is unaffected by the plasma pretreatment.

Nylon and polyester fibers have been dyed with carotenoid dye

bixin-the colour component of annato.

It is observed that though both the fibers have good affinity for this

dye. The colours obtained on nylon and polyester fibers are

reasonably fast to washing, though not so fast to light.

On nylon, the dye apparently gets absorbed on the positively

charged sites and ionic forces control the adsorption. (9)

Page 3: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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Calendula officinalis (10)

is an annual plant. (4)

The pale green, oval

leaves are slightly indented and the golden to orange-red capetula

have numerous, brightly coloured ray florets (16)

The seed contains (30.6-36.9) % protein and (40.8-45.8) % oil, on a

zero-moisture basis.

Capetula which yield a yellow dye for cloth,(17)

contain the

amorphous calendulin, analogous to bassorin, traces of an essential

oil, musilage, oleanolic acid, a gum, a resin, a saponin, a sterol,

cholesterol, esters of lauric, myristic, palmitic, stearic, pentadecylic

acids, faradiol and arnidiol. (12)

Nineteen carotenoids were identified in extracts of petals of orange

and yellow flowered cultivars of Calendula. (13)

Dry rays florets, which have the highest concentration of active

ingredients, contain stigmasterol, sitosterol, 28- isofucosterol,

campesterol, 24- methylene cholesterol and cholesterol as well as

other more complex materials.

The pigment consists of beta- carotene, lycopene, rubixanthine,

violaxanthin, saponins and phytosterols. (12)

Fresh plant material contains the analgesic salicylic acid (0.34mg /

kg).

Fig. (1): Calendula officinalis.(10)

Page 4: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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Casuarinas cunnighamiana (10)

They mainly distributed in Australia

and New Caledonia.(14)

They are morphologically distinctive with the

foliage consisting of long needle-like articulate photosynthetic

(assimiolatory) branchlets, which have more or less spaced nodes. At

each of these is a whorl of 4-20 leaves reduced to teeth.(5)

Some of 15 species of Casuarina are cultivated in Egypt of which

C. cunninghamiana is one of the most popular especially in the

countryside.(6)

The bark of Casuarina yields (6.7-11.3) % of tannin.(18)

Fig. (2): Casuarina cunnighamiana.(8)

C. cunninghamiana contains flavonoids: (kaempferol, kaempferol

glucoside, quercetin, quercetin glucoside) and phenolic (ellagic

acid).(7)

Page 5: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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The present study is a serious trial to optimize the dyeing of

nylon 6 with these selected vegetable dyes and to determine the

availability of using synthetic and natural mordants to enhance the

dyeing fastness properties.

2. Materials:

2.1 Fabric:

100% nylon 6 woven fabrics (120 g/m2) from Middle East Co.

for Textile Industry, Cairo, Egypt were used throughout the

present work.

2.2 Dyes:

The used natural dyes were extracted from uqhuwan

(Calendula - officinalis) and Casuarina (Casuarina cunnin –

ghamiana).

Plant materials i.e the outer bark of hard and heavy wood of

Casuarina and the yellow orange florets of Calendula were

dried in hot air for three days till the plant materials become

crisp. Then, the plant materials were ground in a laboratory

hammer and mill to pass through a 40 mesh (British Standard

Screen) sieve to be very fine powder. Various extraction

methods were used to get the extract solution from plants.

2.3 Mordants:

2.3.1 Natural mordant:

Carob (Ceratonia siliqua).

2.3.2 Synthetic mordants:

Alum, Magnesium chloride and Tannic acid were used as

mordants. All these mordants were of pure grades.

2.4 Chemicals:

-Formic acid and sodium carbonate of laboratory grade

were used for adjusting the pH of the dye bath.

-Hostapal CV-ET (Hoechst), a nonionic detergent for

soaping bath.

-Powdered active charcoal for decolourization the natural

mordant.

Page 6: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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3-Procedures and Measurements:

3.1 Extraction of Dyes:

Calendula:

By soaking 10 g dry plant material in 50 ml water for 12 hr,

after which the extract was filtered and completed to 100 ml

solution with water.

Casuarina:

By boiling (10 g plant materials for 100 ml water) for one

hr. using 5g/l sodium carbonate. After filtration the extract was

completed to 100 ml with water.

3.2. Extraction of Natural Mordant:

The plant material was soaked in water for 24 hr after which

it was boiled for 30 min. The extract was then, filtered and

decolourized using active charcoal to get transparent and clear

solution.

3.3 Dyeing Process:

The dyeing process was achieved using Electric Thermo

Water Bath.

Nylon samples were introduced into the dyebath containing 60

ml extract/100 ml water at about 50º C. The temperature was

gradually raised to the boil and dyeing was carried out for 60

min. at liquor ratio 1:100. The pH was adjusted at the required

value by adding dilute solutions of either formic acid or sodium

carbonate. At the end of the dyeing process the dyed samples

were removed, rinsed, soaped and rinsed with hot and cold

water.

3.4 Mordanting Method:

The dyed nylon fabrics were mordanted in aqueous bath

containing the suitable amount of mordant and at liquor ratio

1:100. The mordanting process was started at 50º C and the

temp. was then fixed for another 40 min. Nylon samples were,

then, rinsed and soaped with 2 g/l Hostapal CV-ET for 15 min

at 70º C.

3.5 Determination of Minerals:

Total content of Ca, Cu, Fe, Cr, Sn, Zn, Ni and Co were

determined in the digested solutions of natural mordant using

inductively coupled plasma (400) emission spectrometry

(Perkin elemer Emission Spectrometer). (2)

Page 7: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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3.6 Measurement of Colour Strength:

The colour strength (expressed as K/S) of the dyed nylon

samples was evaluated by reflectance measurements ICS-

TEXICON Computerized Spectrophotometer, Model M 520220

(produced by ICS-TEXICON Limited Co., England)

Colour strength of the dyed samples is expressed as K/S

values. They were calculated from the Kubelka – Munk

equation, K/S = (1-R)2/2R, in which K and S are the absorption

and scattering coefficients, respectively, and R is the reflectance

of the dyed fabrics. (1)

The dyed and mordanted nylon samples were measured at

=400 & 460 for yellow and brown shades resulted of

Calendula and Casuarina dyeings respectively.

3.7 Measurement of Colour Fastness:

Colour fastness to rubbing (1)

, perspiration (1)

and light (1)

were determined according to AATCC test Methods: (8-1972),

(15-1973) and (16A-1971) respectively. Colour fastness to

washing (38)

was determined according to Test 2 of India

Standards (IS) 336/1979

Results & Discussion

Dyeing Polyamide Fabrics with Natural Dyes:

1. Effect of pH of Dyeing on Colour Strength:

Different polyamide samples were dyed in various dyebaths

under constant dyeing conditions i.e. conc. of extract, temp., and time

whereas the pH level was varied from one bath to another. The colour

strengths of the dyed samples were measured and the received data

are plotted in Figure 1.

It is well observed, from Fig.1, that pH of dyeing plays a great

role in determining the amount of colouring matter that may be

absorbed and fixed on nylon fibres. Increasing the acidity of the

dyebath is accompanied with higher dyeability of nylon fabric

towards natural dyes.

Maximum colour yield is realized on polyamide fibres when

dyeing process is carried out at lower pH level (3-3.5) for both of the

used dyes.

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For Calendula the optimum pH value was found to be at pH=3 and for

Casuarina at pH=3.5. The high colour yield is realized when dyeing is

carried out from strong acidic medium which may be attributed to the

electrostatic attraction between the positively charged polyamide

fibres and the anions of the colouring matters. The degree of

protonation of polyamide is well known to increase by lowering the

pH level of the aqueous medium.

Therefore, it may be concluded that the dyeing mechanism with

natural dyes is similar to great extent to its mechanism with acid dyes.

Therefore, the amount of absorbed natural dye will be depended

on the degree of ionization of the fibre or in other words will be

related to the pH of the dyebath.

Action of Electrolytes:

Neutral electrolytes such as common salt (sodium chloride)

play an important role in the dyeing operation especially that of ionic

dyeing system. The role played by electrolytes differs from one

system to another according to the nature of both fibre and dye itself.

Electrolytes are used as exhausting agent in case of dyeing cellulosic

materials with anionic dyes owing to the similarity of charges on both

fibres and dyes. In case of protein fibres and polyamide the

electrolytes are considered as leveling agents owing to the

unsimilarity of charges on both fibres and dyes.

It is well noticed, from Figure 2, that addition of sod. chloride

resulted in some decrease in the colour strength of the two applied

dyes. This result is in good agreement with the effect of pH on the

colour strength of the dyed polyamide samples. So the dyeing process

achieved without any salt addition.

Polyamides contain a limited number of amino groups at the end

of the polymer chains. These amino groups are the available dye sites

in the fibre through which the dye anions are attracted to form salt

links. Addition of sod. chloride into the dyebath means addition of

sodium and chloride ions. Therefore, as a result of the presence of

more than one kind of anions in the same dyebath a competition for

the positively charged sites in the fibre will be occurred since one

anion (chloride of salt or dye anion) being capable of replacing

another according to the following equation:

Ny-N+H3.Cl

- + D

- Ny-N

+H3.D

- + Cl

-

Page 9: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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This reaction mechanism is reversible and a dynamic

equilibrium is attained. Therefore the final distribution of the dye and

inorganic anions will depend upon their relative concentrations.

Thus by increasing the relative concentration of chloride anions in the

dyebath the reaction mechanism will be shifted towards the

replacement of dye anions by chloride anions.

On the other hand, it may be noted also that the equilibrium

position of the displacement reaction is governed not only by the

relative conc. of the two competing ions but also by their relative

affinities for the fibre.

Effect of Dyeing Temperature:

It is obvious, from Figure 3 that the rate of dyeing increases

gradually by raising the temperature. Maximum dye fixation is

achieved at boiling for both Calendula and Casuarina and the rate of

dyeing depends to great extent on the nature of both dye molecules

and the fibre itself. The rate of dyeing of the colouring matter that

extracted from Calendula is higher than that of Casuarina. The

magnitude of increase in colour strength is found to be greater in case

of Casuarina than that of Calendula under the action of temperature.

By raising the dyeing temp. from 23º C to 40º C the percent

increase in K/S is found to be (88 %) for Calendula while it is reached

to (124 %) for Casuarina. When the temp. is elevated from 80º C to

100º C, the percent increase in K/S is observed to be about (4.8 %)

and (130 %) for Calendula and Casuarina respectively.

It may be suggested that the colouring matters of Casuarina

present in the aqueous medium in aggregated form since they need a

high temp. to diffuse inside the polymer chains of polyamide. One can

notice the great difference in K/S when dyeing is carried out at room

temp. (23º C) and at boiling for the two dyes.

Casuarina is more temp.-dependence for attaining maximum

K/S than Calendula. High temp., on the other hand, open up the fibre

structure and increase the number and volume of voids and thus

accelerates the diffusion of dye molecules inside the fibre. Also, it

was known that raising dyeing temp. increase the kinetic energy of

dye molecules which excited and migrated towards the fabrics to

achieve more penetration more absorption and finally more colour

strengths.

Page 10: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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From the previous results, it seems that dye exists in solution as

an aggregate of various sizes. As small aggregates are removed from

solution by the fiber, the larger aggregates break down to maintain an

overall dynamic equilibrium of dye aggregates. When the solution

temperature increases, the thermal energy coming from outsides

impedes aggregation, and therefore, the increases in the amount of the

non aggregated dye particles in the solution. Hence, the effect of

temperature, and consequently, increase in the kinetic energy of the

molecules tends to break up large aggregates into smaller units. The

increase of dye diffusion coefficients at higher temperatures is first of

all caused by the greater kinetic energy acquired by the dye molecules

and by the increase in the frequency and amplitude of thermal

oscillations in the separate sections of the substance macromolecule

chain, which provokes an increase in the number of the pores in the

fiber structure and in their diameter. Thus, the small dye particles

penetrate into the fiber pores at high temperature; when the dye bath

cools, the pore of the fiber contracts, thus fastly retaining.(15)

Effect of Dyeing Time:

Dyeing of polyamide samples were carried out for (15, 30, 45,

60, and 90) min. under fixed dyeing conditions i.e. 60 % extract,

pH=3, and at boiling. Figure 4 illustrates the effect of dyeing time on

the K/S, from which it can be observed that by lasting time of dyeing

the K/S is increased for both Calendula and Casuarina. Optimum

dyeing time is found to be 60 min. for Calendula and 90 min. for

Casuarina.

The colouring matter of Casuarina need longer dyeing time than

of Calendula, which may be attributed to its greater molecular size as

previously suggested.

Post Mordanting:

Since the aim of the application of natural dyes for dyeing

polyamide fibres is to minimize the pollution of environment by using

eco-friendly materials therefore mordanting with some harmful and

carcinogenic metal salts such as copper sulphate will be of nonsense.

Therefore, our new trend is to use a mordant that extracted from

suitable plant, such as, Carob and also to use some safety mordants

such as, Alum, Magnesium chloride and Tannic acid. A detailed study

Page 11: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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was carried out in order to determine and optimize the application

conditions of these mordants.

The extraction process of Carob plant was carried out in a

similar manner to that of extracting the colouring matters from plants.

The received extract were decolourized by treatment with active

charcoal.

This extract was subjected to chemical analysis to determine its

content of various metals and their concentrations (Table 1). The

presence of miscellaneous metals in the extract may play a great role

in determining the efficiency of metal complexing reaction with the

colouring matters inside the fibre. The received colour hue as well as

the degree of colour fastness properties will depend to great extent on

the kind and conc. of the metals. All these results were compared with

values resulted from using synthetic mordants.

The quantity of metals containing in the natural mordant may

be criticized bearing in mind the eco-friendly application but in

comparing with the more harmful synthetic mordants such as tin,

copper, chrome…etc., the natural mordant was preferred.

Effect of pH of Mordanting:

Nylon fabrics previously dyed with Calendula and Casuarina

dyes were mordanted at various levels of pH to determine their effect

on the K/S and the results are illustrated in Table 2, from which it may

be concluded that:

1. For Calendula, the optimum pH values at which

maximum dye fixation were attained, were found to be at

pH=(4) in case of using Carob, Alum and Magnesium

chloride and pH=(6) in case of Tannic acid. For

Casuarina, were found to be at pH=(7) in case of using

Carob, Alum, and Tannic acid and pH = (8) in case of

Magnesium chloride.

2. Referring to the dyeing properties of the two applied

natural dyes, it can be noticed that Calendula dye is very

sensitive to the variation of pH value of the dyebath.

Maximum absorption capacity was achieved at pH=3.

Increasing the pH value from 3 to 8 was accompanied

with noticeable decrease in the K/S. This behaviour may

give a good idea about the affinity of the dye toward

Page 12: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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nylon fibres. It may be concluded that the dye of

Calendula has a lower affinity compared with that of

Casuarina. Therefore, during the mordanting process the

pH of the medium will affect the absorption/desorption

equilibrium between the fibre and the treatment bath. In

the case of dye of low affinity the amount of desorbed

dye, i.e. migration of dye from fibre to the bath, will

depend greatly on the pH. Mordanting at pH higher than

7 will accelerate the desorption of the dye as in the case

of Calendula. Therefore, the optimum pH value for

mordanting polyamide fibres dyed with Calendula will be

between pH (4-6) for all of mordants. For fibres dyed

with Casuarina the most suitable pH for mordanting

ranged between pH (7-8).

Effect of Mordanting Temperature:

Post mordanting of dyed nylon samples were carried out, using

a fixed amount of natural mordants, at different degrees of temp. and

the results of K/S are illustrated in table 3.

It may be concluded, from table 3, that the optimum temps. for

mordanting were found to be at R.Tº C using Carob, 60º C with Alum,

80º C with Magnesium chloride and 40º C with Tannic acid for

Calendula and in case of Casuarina dye at 100º C using Carob, 60º C

with Alum, 80º C with Magnesium chloride and 40º C with Tannic

acid.

It was observed that lower mordanting temp.s were the nearest

suitable temp.s to achieve highest values of K/S of nylon fibers dyed

with Calendula mordanted with all mordants except with Magnesium

chloride. 80º C was the optimum which may be refer to the increment

of rate of metal complex reaction [fiber-mordant-dye].

In case of Casuarina, high temp.s of mordanting were preferred

except with Tannic acid, 40º C was the optimum one.

These results are in good agreement with the conclusion about

the affinity of the used natural dyes toward nylon fibre and its relation

to the adsorption / desorption mechanism.

Effect of Mordanting Times:

The rate of mordanting reaction may depend on some various

factors:

1. The rate of absorption of the mordant by the

fiber.

Page 13: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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2. The kind of the mordant itself.

3. The chemical structure of the colour species

and their rate of reaction with the mordant to

form the metal complex compounds.

For these reasons the duration of mordanting differs from one

mordant to another.

Therefore the mordanting time of eco-friendly mordants were

studied in order to determine their optimum time.

The dyed polyamide samples were after treated for different

durations using fixed amount of mordants and the mordanting process

was carried out at optimum pH values for Calendula and Casuarina.

Table 4 indicates the results of K/S as a function of mordating

duration.

It may be concluded, from table 4, that the optimum

mordanting time with Alum and Tannic acid mordants reaches about

15 min. and 60 min. respectively for both Calendula and Casuarina

dyes. The most suitable time for mordanting with Carob reaches 15

min. for Calendula and about 90 min. for Casuarina whereas reaches

45 min with Magnesium chloride for Calendula and 90 min. for

Casuarina.

Colour Fastness Properties:

Nylon fabrics dyed with Calendula and Casuarina natural dyes

and mordanted with the different mordants were subjected to fastness

tests to washing, perspiration, rubbing and light.

The results of these tests are tabulated in table 5 from which it

may be concluded that:

1. Light fastness:

Using the grey scale assesses it is evident that the fastness of

nylon fabric dyed with Casuarina is higher than that of Calendula.

It is obvious from the table that the mordanting process either by

metal salts or by natural mordant does not affect the light fastness

since it reaches (2-3) and (3-4) for Calendula and Casuarina

respectively.

Page 14: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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2. Wash Fastness:

Unmordanted nylon fabric exhibits very good to excellent (4-5)

for Calendula dye whereas it exhibits fair (3) in case of Casuarina dye.

Synthetic mordants are found to increase the wash fastness in case

of Casuarina since it reaches (4-5) grade with Alum and (3-4) grade

with Magnesium chloride, Tannic acid and Carob mordants.

3. Perspiration fastness:

The fastness to acid perspiration (alt.) exhibits fair to good (3-4)

for unmordanted nylon fabric in case of Casuarina and from good to

excellent in case of Calendula dyes.

For Casuarina the fastness rating is increased as a result of

mordanting since it reaches (4-5) with synthetic and natural mordants.

The fastness properties to alkaline perspiration are found to

improve the alteration especially in case of Casuarina by mordanting

with (Alum). The rating increased from (3) for the unmordanted dyed

fabric to (4-5) and (3-4) with (Alum) and (Magnesium chloride,

Tannic acid and carob) respectively.

4. Rubbing Fastness:

For Calendula no appreciable alteration was observed as a result

of mordanting either with natural mordant or with metal salts. For

Casuarina appreciable variation in both wet and dry rubbing fastness

was observed in case of using Carob as a natural mordant. The wet

rubbing is increased from (2-3) for the unmordanted dyed fabric to (3-

4) and in dry rubbing increased from (3-4) to (4).

Generally, in many cases; the fastness properties of dyed and

mordanted nylon fabrics were considered better than unmordanted

ones.

From that it can be expected using Calendula and Casuarina as

an eco-friendly alternative dyes for nylon fabrics instead of synthetic

dyes to minimize the disadvantages of using synthetic fabrics but

there were many obstructions such as expensive cost of natural dyes,

difficulty extraction process and the reproducibility problems of the

colour shades …. So, natural dyes with their limited colour shades and

rather poor fastness properties can use temporary as a hobby or as a

handicrafts.

Page 15: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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Conclusion

1-Nylon fabric was successfully dyed with natural dyes, namely:

Calendula and Casuarina, and the dyeing conditions were optimized.

2-The behaviour of natural dyes during the dyeing of nylon fabric was

found to similar to that of acid dyes.

3-The rate of dyeing was found to increase as the temp. Increase till

reached its maximum at boiling for the two applied natural dyes.

4-Temp. break down the aggregate of dyes and increases their

solubility as well as opening up the fibre structure and thus accelerates

the diffusion of dye molecules inside the fibre.

5-The pH of dyeing was found to play a great role since maximum

colour strength was achieved at strong acidic medium which may be

attributed to the high electrostatic attraction between positively

charged basic groups in the nylon fibre and the dye anions.

6-Eco-friendly natural mordant that extracted from Carob was used

beside the safety metal salts since satisfactory fastness properties were

realized.

References

1) Abdel Keriem, A. A.: Dyeing of Cellulosic Fabrics with Natural Dyes,

M.Sc.D. Thesis, Faculty of Applied Arts, Helwan University, P. (59-

61), 1997.

2) Allen, L. B.; Sitonen, P.H. and Thomposon, H.C.: J. Acric. Food

Chem., Vol. (45), Jan., P. (162-165), 1997.

3) Bliss, A.: A Hand Book of Dyes from Natural Materials, New York,

P. (3-47), 1981.

4) Brickell, C.: Encyclopedia of Plants and Flowers, Dorling Kindersley

Limited, London, P. 252,450, 1989.

5) Duhoux, E., Franche, C. and Bogusz, D.: Biotechnology in

Agriculture and Forestry (Trees IV), Vol. (35), P.76, 1996.

Page 16: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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6) El-Hadidi, M. N. and Boulos, L.: The Street Trees of Egypt, The

American University Press, Cairo, P. 24, 38, 1988.

7) Glasby, J. S.: Dictionary of Plants Containing Secondary Metabolites,

Taylor & Francis Limited, London, P. (59-69), 1991.

8) Griffiths, M.: Index of Garden Plants, First Edition, Timber Press,

Inc., North America, P. (407-1105), 1992.

9) Gulrajani, M. L., Gupta, D. and Maulic, S.R.: Indian Journal of Fiber

& Textile Research, Vol. (24), June, P.131, 1999.

10) Hyam, R. and Pankhurst, R.: Plants and their names, Oxford

University Press, Inc., New York, P.81, 95, 1995.

11) Indian Standards, 336, Test 2 (Washing), 1979.

12) James, A. D.: A Hand Book of Medicinal Herbs, CRC Press, Boca

Raton, P.87,88, 1985.

13) Kishimoto, S., Maoka, T. and Ohmiya, A.: Biosci. Biotechnol.

Biochem., Vol. 69, Nov., P.(2122-2128), 2005

14) Lotschert, W. and Beese, G.: Collins Guide to Tropical plants, P. (80-

225), 1993.

15) Maniruzzaman, M., Akther, M. A., and Rahaman, M. H.: Colourage,

Vol. (53), April, P.73-80, 2006.

16) Nishida, K. and Kobayashi, K.: American Dyestuff Reporter, Vol.

(81), July, P. 44, 45, 1992.

17) Singh, S., Jahan, S. and Gupta, K.C.: Colourage, Vol. (XL), August,

P.33, 1993.

18) Watt, J. M. and Gerdina, M.: Medicinal and Poisonous Plants of

Southern and Eastern Africa, Second Edition, London P.(177, 570-

577), 1962.

19) Wakida,T., Choi, S. and Tokino, S.: Textile Res. J., Vol. (68),

Nov., P.848, 1998.

Page 17: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

17

Dyeing of Nylon 6 Fibers with Natural Dyes

Dyebath pH

0 1 2 3 4 5 6 7

K/S

0

2

4

6

8

10

12

Calendula

Casuarina

Fig 1 : Action of Dyebath pH on the Dyeability of Polyamide Fabrics towards Natural Dyes

temp. 100 oC, time 60 min. L.R. 1:100

Page 18: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

18

NaCl Concn. (g/l)

0 1 2

K/S

0

2

4

6

8

10

12

14 Calendula

Casuarina

Fig. 2 : Influence of Sodium Chloride on the Colour Strength of the Dyed Polyamide Fabrics.

temp. 100 oC, pH=3, time 60 min. L.R. 1:100

Page 19: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

19

Dyeing Temp. (oC)

0 20 40 60 80 100

K/S

0

2

4

6

8

10

12

14

Calendula

Casuarina

Fig. 3: Influence of Dyeing Temp. on the Colour Strength of the Dyed Polyamide Fabrics. pH=3, time 60 min. L.R. 1:100

Page 20: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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Dyeing Time (min.)

0 20 40 60 80 100

K/S

4

6

8

10

12

14

16

18

Calendula

Casuarina

Fig.4 : Effect of Dyeing Time on the Colour Strength of the Dyed Polyamide Fabrics.

temp. 100 oC, pH=3, L.R. 1:100

Page 21: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

21

Mordanting of Nylon 6 Fibers

Table 1: Different Metals and their Conc. in the Aqueous Extract of

Carob Plant

Plants

Metal Exist in the Extract

(ppm)

Cr Zn Ni Fe Co Mg Cu Sn Al Ca

Carob 0.025 0.822 2.042 0.024 0.006 106.5 0.139 0.449 __

220.1

Table 2: Effect of pH of Mordanting on K/S of Nylon Fibre Dyed

with Natural Dyes

pH of

Mordanting

K/S of dyed Nylon

Calendula Casuarina

Carob Alum MgCl Tannic

acid Carob Alum MgCl

Tannic acid

4 15.97 14.60 13.87 12.50 9.12 9.38 9.76 10.37

5 15.23 9.18 11.37 12.80 9.41 9.41 11.11 10.40

6 14.69 2.87 7.03 13.80 10.02 10.55 11.16 10.50

7 12.03 2.50 6.60 10.60 11.23 11.03 11.86 10.80

8 11.67 1.66 5.67 9.01 10.44 9.96 12.61 6.52

Page 22: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

22

Table 3: Effect of Mordanting Temp. on K/S of Nylon Fibre Dyed

with Natural Dyes

Temp.(ºC) of

Mordanting

K/S of dyed Nylon

Calendula Casuarina

Carob Alum MgCl Tannic

acid Carob Alum MgCl

Tannic acid

25 16.98 14.07 13.87 14.50 10.50 7.25 10.66 11.86

40 15.73 14.13 14.65 14.80 10.73 7.29 10.72 13.88

60 15.41 14.42 14.85 13.56 11.04 8.27 12.32 13.54

80 12.93 14.33 15.96 13.50 11.12 7.75 12.89 11.88

100 11.67 14.27 15.00 13.40 11.46 7.38 12.57 10.96

Table 4: Effect of Mordanting Time on K/S of Nylon Fibre Dyed with

Natural Dyes

Time (min.) of

Mordanting

K/S of dyed Nylon

Calendula Casuarina

Carob Alum MgCl Tannic

acid Carob Alum MgCl

Tannic acid

15 14.39 16.50 13.42 13.26 10.90 8.06 11.96 10.54

30 11.94 15.50 14.72 13.35 10.94 8.00 12.35 10.60

45 11.79 15.12 15.07 13.42 11.15 7.55 12.48 11.50

60 11.70 14.27 14.01 13.84 11.20 7.40 12.60 10.90

90 11.45 11.58 13.84 12.18 11.23 7.27 12.64 10.44

Page 23: Dyeing of Nylon 6 Fibres With Calendula Officinalis 2

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Table 5: Colour Fastness of the Dyed Nylon Fabrics

Pla

nt

Mordant

Wash Perspiration

Rubbing Light/5 Acid Alkali

Staining Alt.

Staining Alt.

Staining Alt. Wet Dry

Ny. W. Ny. W. Ny. W.

Cale

nd

ula

Without 5 4-5 4-5 4 4 4-5 4-5 4 4-5 4 4 2-3 Alum 5 4-5 4-5 4-5 4-5 4-5 4-5 4 4 4 4 2-3

MgCl2 5 4-5 4 4-5 4 4 4-5 4-5 4 4 4 2-3

Tannic Acid 5 4-5 4 4-5 4 4 4 4 4 4 4 3

Carob 5 4-5 4 4-5 4-5 4 4 3-4 4 4 4 2-3

Casu

ari

na Without 5 4-5 3 4 4 3-4 5 4-5 3 2-3 3-4 3-4

Alum 5 4-5 4-5 4-5 4-5 4-5 5 3-4 4-5 3 4 3-4 MgCl2 5 4-5 3-4 4 4-5 4-5 5 3-4 3-4 3-4 3-4 3-4

Tannic Acid 5 4-5 3-4 4-5 4-5 4-5 4-5 4 3-4 2 4 3 Carob 5 4-5 3-4 4-5 4-5 4 5 4-5 3-4 2-3 2-3 3-4

Ny. = Nylon W. = Wool Alt. = Alteration