AHSANULLAH UNIVERSITY OF SCIENCE AND TECHNOLOGY

Department of Textile Technology

COURSE NO : TEX-400 SESSION : FALL 2010

PROJECT WORK ON THE EFFECTS OF SOAPING AGENT & FIXING AGENT ON THE COLOR FASTNESS TO WASH OF THE REACTIVE DYED COTTON FABRICS

SUPERVISED BY: SUPERVISED BY:

CO-

MOHAMMAD GIAS UDDIN ATIQUZZAMAN

ASST. PROFESSOR PROFESSOR DEPARTMENT OF TEXTILE TECHNOLOGY TEXTILE TECHNOLOGY AUST

A.S.M.
ASST. DEPARTMENT OF AUST

SUBMITTED BY NAME ID

MD. IFTEKHAR HOSSAIN SUSHAMA SAHA SWATI MD. MOSTAFIZUR RAHMAN MD. AKHLAKUR RAHMAN MD. SHOEB HOSSAIN

07.01.06.067 07.01.06.077 07.01.06.084 07.01.06.117 07.01.06.119

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Acknowledgement___________________________
At first we would like to thank the almighty ALLAH for giving us strength to finish this project work successfully. We express our heartiest thanks to our Project Supervisor Assistant Professor Mohammad Gias Uddin for his guidelines, valuable suggestions, encouragement, constructive criticism and for providing all necessary support for completing this project. We also like to thank Project Co-supervisor Mr. A.S.M. ATIQUZZAMAN, Assistant Professor of AUST for his necessary advice and cordial supervision. Finally we thank all of our Respected Teachers of the department of Textile Technology for their insightful information, advice and suggestions.

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Content
Chapter
Chapter 1

Topic Name
Introduction

Page No.

Objective Chapter 2 Literature Review *Cotton *Reactive dyes *Wash off of unfixed Reactive dyes *Cationic fixing of Reactive dyes Chapter3 Materials & Methods *Dyeing *Soaping *Fixing Chapter 4 Chapter 5 Results & Discussion Our Findings

Limitations

Suggested Recipe Chapter 6 Conclusion

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References

CHAPTER 1:

INTRODUCTION
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Reactive

dyes have better property in terms of fastness.

Reactive dyeing of cellulosic substrate takes place under alkaline conditions. But this alkaline condition also facilitates the reaction of reactive group with the dye liquor (water), resulting in deactivation or hydrolysis of the dye. Approximately 3/4th of the dye gets fixed while remaining 1/4th gets hydrolyzed. After dyeing the substrate contains unfixed hydrolyzed dyes and usually some residual active dyes. This hydrolyzed dye adheres onto the substrate and keep on getting removed during washing treatments causing poor wash fastness. So besides taking steps to reduce the hydrolysis as much as possible, this hydrolyzed dye must be removed by rinsing and using an appropriate washing-off agent in order to retain the fastness properties. Effective washing after reactive dyeing is crucially important. The dyeing does not show optimal wet fastness properties until this loose color is removed or rendered insignificant in amount. It is remarkable that, on an average, only about 0.003% dye on weight of substrate will produce a stain equivalent to a grey scale rating of 4. The amount remaining after washing must be sufficiently small to ensure that after migration the fibres on the surface of the material still exhibit acceptable fastness. During washing the rate of diffusion out of the fibre is retarded by the substantivity forces between dye and cellulose
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molecules. The smaller the proportion of unfixed dye and the weaker these substantivity forces, the easier is the removal of the unfixed hydrolyzed dye remaining. Especially when applying reactive dyes in full depths, difficulties may arise in removing the unfixed dyes. In these circumstances it may be found necessary to after-treat the dyeing with a cationic fixing agent. Treatment with a cationic agent is not a substitute here for thorough washing to remove unfixed dye. Formation of the insoluble dyeagent complex on goods that have not been thoroughly washed will lead to unacceptable color fastness to wash and rub.

Objective Of the Project:

The main objects of this experiment can be illustrated as follows: To determine the color fastness to wash of the reactive dyed fabrics using light, medium and deep shades. To determine the effect of different soaping agents on the color fastness to wash after reactive dyeing. To determine the effect of different fixing agents on the color fastness to wash after soaping for reactive dyed fabrics. To investigate the effect of fixing agents over light, medium and deep shades on reactive dyeing.
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To compare the color fastness to wash using different proportion of soaping agents and fixing agents. To compare the color fastness to wash results between two similarly processed dyed fabrics- one of which is first washed followed by fixing and the other is first fixed followed by washing. To set some guidelines for effective washing and fixing for removing unfixed, hydrolyzed reactive dyes from cotton fabric.

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CHAPTER 2:

LITERATURE REVIEW

Cotton
Cotton is a cellulosic fiber, which is actually the most pure natural form of cellulose. It is a soft fibre that grows around the seeds of the cotton plant . The fibre is most often spun into thread and used to make a soft, breathable textile. Cellulose content of the raw cotton fiber ranges from 88 to 96%. Cellulose is a polymer of -D-glucose. The repeating unit of cellulose consist of two -D-glucose molecules linked together at the 1:4 carbon atoms. The cellulose is arranged in a way that gives cotton unique properties of strength, durability, and absorbency. It's also comfortable and retains colors and dyes well. It's strong under water, and it stands well against high temperatures.

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Fig1: Chemical structure of cellulose

Components of Reactive dyes

Simple representation of reactive dye:

Fig. 2: Simple structure of Reactive dye

Where, S is the Solubilizing group

C is the Chromophoric group or the color bearing part

B is the bridging group X is the halogen containing reactive group

Nature of Reactive dyes:

Reactive dyes are anionic soluble dyes. They react with the fibre to form covalent bond. They possess in their dye molecule, a reactive group, either a haloheterocycle or an activated double bond, which in alkaline condition reacts with the hydroxyl groups of the cellulose to form a stable chemical linkage. The molecules of reactive dyes are smaller and their smaller size in accompanied by a correspondingly lower substantivity.

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R = Chromophore

Cell = Cellulose

Classification of Reactive dyes:

1. According to reactivity: Three types which are shown below with required information Reactiv Brand Exhaust ity Dyeing Temp. (C) 1.High Cold 20-40 Alka li Type Wea k React ive group DCT Structure

2.Mediu m

Mediu m

40-60

Mild

MFT

3.Low

Hot

60-80

Stron MCT g

2. According to Reactive dyes mechanism:

The dyes fall essentially into two classes2.1. Nucleophilic substitution reaction:
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Nucleophilic substitution mechanism is based on the presence of halogen substituents in heteroatomic systems. ExampleThe chlorotriazinyl dyes . Dye-X +Cell-OH Dye-O-Cell + HX

Among the principle reactive system of the type are the halogen substituted triazine, pyrimidine, pyrozine, quinoxaline and thiazole group. 2.2. Nucleophilic addition reaction: Those that reacting with cellulose by nucleophilic addition to a carbon-carbon double bond, usually activated by an adjacent electron attracting sulphone group. Example- Vinyl Sulphone dyes Dye-SO2-CH=CH2 + Cell-OH Cell Dye-SO2-CH2-CH2-O-

Recent classification of Reactive dyes:

1. Alkali-controllable reactive dyes: These are characterized by low neutral exhaustion and because of high reactivity, alkali is to be carefully added to achieve level dyeing. Their optimum temperatures of fixation are between 40C and 60C. DCT, dichlorofluoropyrimidine , dichloroquinoxaline or VS reactive systems belong to this group. 2. Salt-controllable reactive dyes: They exhibit high neutral exhaustion and salt addition is to be made very carefully to achieve level dyeing. The dyes in this group show optimal fixation at a temperature between 80C and boil. Low-reactivity systems such as trichloropyrimdine, MCT dyes belong to this group. 3. Temperature- controllable reactive dyes: These dyes are represented by dyes that react with cellulose at temperatures above boil in the absence of alkali, although they can be applied as salt controllable dyes under alkaline conditions between 80c and boil. The dyes are self leveling and no auxiliary products are required to facilitate leveling. Good results can be obtained by controlling the rate of temperature rise. At present only NT dyes belong to this group.

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Basic principle of Reactive Dyeing with Cotton:

Three basic steps are for dyeing of cellulose fibers with reactive dyes are as follows:

Exhaustion of the dye from an aqueous bath containing common salts or Glaubers salt in neutral condition. Dyeing is started in neutral solution so that there is little likelihood of the dye reacting with the cellulose. During this stage of dyeing, some reactive dye will be absorbed by the fibres, the amount depending upon its substantivity. The fixation phase. After the initial exhaustion phase, the pH of the dyebath is increased by complete or gradual addition of the appropriate type and amount of alkali. This causes dissociation of some of the hydroxyl groups in the cellulose and the nucleophilic cellulosate ions begin to react with the dye. The post- dyeing washing. The rinsed dyeing contains dye bonded to the cellulose, absorbed but unreacted dye, as well as hydrolysed dye. There will also be residual alkali and salt. The latter are relatively easy to remove by successive rinsing in cold and then warm water. As much unfixed dye as possible must be washed out of the dyeing.

Problems with reactive dyeing:

1. Hydrolysis of Reactive dyes: The reactive dyes have ability to react with fiber polymer as well as with water molecules. Under alkaline conditions, Reactive dyes react with the terminal hydroxyl group of cellulose. But if the solution of the dye is kept for long time, its concentration drops. Then the dyes react with the hydroxyl group of water. The reaction of dye with water is called Hydrolysis of Reactive dyes. The major problem of hydrolysis results in lower fixation rate (less than 70%) as well as incomplete utilisation of dye. D-SO2-CH=CH2 + H2O D-SO2-CH2-CH2-OH
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Some problems associated with dye hydrolysis

Less color yield

Uneven surface after washing The color become light after washing The staining takes place during the washing with light and bright textile materials.
1. Relatively large amounts of electrolyte are required for exhaust

and pad steam applications.

2. Laborious removal of unreacted and hydrolysed dye is required-

often a longer operation than the dyeing step itself and not always entirely satisfactory.
3. Hydrolysed dye is discharged as colored effluent. 4. Color is not easily removed by effluent treatment processes and

in many cases the dyes are not readily biodegradable. 5. Unhydrolysed, unfixed haloheterocyclic reactive dyes may pose an environmental hazard. To minimize above problems reactive dyes contains more than one reactive systems is introduced in the market which shows higher fixation rate than conventional reactive dyes.

Bi-functional Reactive dyes

Many of the new reactive dyes are bifunctional with identical or different reactive groupings in the dye molecule. Bifunctional dyes carry two reactive groups. They are known for their excellent dyeing efficiency and overall fastness properties. Bifunctional dyes with good dyeing properties are created by the careful selection of the right reactive groups and right chromophores.
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It can easily be assessed that dyes with two identical reactive groups and dyes with two different reactive groups exhibit a higher fixation yield than-dyes with one group. There are two types of bi-functional reactive dyes-

1. Homo bi-functional dyes: Bi-functional dyes with two similar functional groups are known as homo bi-functional group dyes. Example-

Fig. 3: Structure of bi-functional Monochlorotriazine dyes

Here, two MCT reactive groups are present.

2. Hetero bi-functional dyes: The dyes having two different functional groups are known as hetero bi-functional dyes. The dyes were conventional Dichlorotriazine type, with the end condensation of -sulphatoethylsulphone to have different type of reactive group in a single molecule. They offer enhanced reproducibility especially for medium to pale shades. Important types of Bi functional reactive dyes include MFT-VS, MCT-VS etc.

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Why bi-functional reactive dyes:

The main problem with conventional reactive dyes lies in the fact that their dyeing efficiency always stands below 100% because of incomplete fixation on the fibre. Usually the efficiency is not more than 70% even in printing application, the remainder undergoes hydrolysis instead of reaction with the fibre. The removal of 30% or more unfixed dye during soaping is troublesome and time consuming, whereas the application procedures of reactive dyes are quite simple. It would be possible to achieve high fixation by using dyes containing more than one reactive group. A dye molecule with only one reactive group may react either with cellulose or with water; but once it has reacted with the later its reactivity is completely gone it is then incapable of reacting with the former. in case of dye having more than one reactive group, the part of the dye which has reacted with water is still capable of further reaction with cellulose. Although the presence of two or more reactive groups in a dye usually favors high fixation properties only carefully selected dyes of this type are technologically suitable in spite of higher probability of reaction with the fibre, a small amount of dye will always be completely hydrolised and has to be removed by washing off.

Aspects of bi-functional vinyl sulphone dyes:

The vinyl sulphone group shows strong polarization caused by the

sulphonyl (SO2) group. DyeSO2CH=CH2 Vinyl sulphone dyestuffs dyes possess vinyl sulphone as the reactive group. In presence of alkali, these dyes chemically react with the hydroxyl group of cellulose and form covalent linkage. These dyes are versatile enough to suit different dyeing methods.
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Results are excellent and shade comes clean and brilliant with no variation in the dyeing and printing. These dyes are the sulphates ester of hydroxyethylsulphonyl dyes which on treatment with mild alkali, generates the vinyl sulphone group, which in turn reacts with ionized cellulose to form the dye fiber bond.

The vinyl sulphone group is not normally present in commercial dyes since it is more convenient to use a less reactive precursor such as the - sulphatoethylsulphonyl group obtained from the corresponding - hydroxyethylsulphonyl compounds. These dyes are marketed in the form of sulphetoethylsulphone dye: DyeSO2CH2-CH2OSO3H
VS bi-functional reactive dye consists of two vinyl sulphone groups

in a dye molecule. Because with two potential vinyl sulphone reactive groups there is an increased probability of reaction with the fibre. An example of it is CI Reactive black 5.

Fig. 4: Structure of CI Reactive black 5

Main features of bi-functional vinyl sulphone dyes:

The stability that is exist in the dye-fiber bond between the vinyl sulphone group and cellulose against acid hydrolysis gives extra
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stability to these dyes in the acidic environment of the industry and makes the dyeing effect more lasting. The portion of bi-functional dyes that doesn't fix during the dyeing process can be removed easily. This is because of the low substantivity of the hydrolysed dye. This reduces the risk of staining of the adjacent whites. Better reproducibility in dyeings. Good all round fastness properties. High exhaustion and high fixation efficiency.

Good leveling properties. Possess excellent brightness and good wet fastness. Suitable for exhaust and different pad dyeing method and discharge printing. They are applicable at 40C and 60C.

Washing off of unfixed reactive dyes:

Removal of hydrolysed and unreacted dye from the goods is a vital step after dyeing. Unlike other dye classes much as 50% ofthe total as cost of a reactive dyeing process must be attributed to the washing off stages to remove unfixed or hydrolysed dye and treatment of the resulting effluent. To achieve superior fastness in washing it is more than important to ensure all hydrolised or unreacted dye to be removed during washing off in reactive dyeing.

Why efficient washing is important:

In general, reactive dyes on cellulosic fibres give dyeings with good to very good fastness to washing and other wet processes. Apparent
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inferior fastness to washing is usually because of incomplete removal of unreacted and hydrolysed dye from the material by washing after dyeing. It is more likely to be a problem for deep dyeings. This hydrolised dye possess some extent of affinity to cotton fibre and loosely held with the fabric which in course of end use cause poor wash and rubbing fastness. To gain satisfactory result in end use this hydrolised dyes should be removed as much as possible. So an effective and efficient wash off is essential after dyeing cotton with reactive dyes.

Role of washing off agents in reactive dyeing:

Washing off agents are necessary to remove the unfixed hydrolyzed dye from the dyed material. Soaping agents disperse hydrolyzed dyestuff and keep them in the water bath, preventing their redeposition on the substrate. The washing-off efficiency of dyes would depend upon the amount of unfixed dye and ease of removal of unfixed dye. The washingoff agent should facilitate the diffusion of unfixed dye molecules from the fiber into the water. It must eliminate the negative effect of hard forming ions on the solubility of unfixed hydrolyzed dye.

Mechanism of Washing-off agents:

Normally, soaping off includes a first rinse step, a soaping step, a second rinse step, and a drying step. Typically, soaps, such as phosphate-based detergents, are added during the soaping step to assist in removal of unreacted reactive dyes. However, the liquid alkalis used during fixing have not been considered for use during soaping since they would not be expected to assist in excess dye
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removal. In addition, if the reaction mixture is too "hot" or alkaline, such as is seen with pure sodium hydroxide, the sensitive-type reactive dyes will hydrolyze with the water in the rinse bath and form a nonreactive pigment that has no effect on the fabric color. Furthermore, phosphate & silicate based soaping agents are not accepted by European countries due to their biodegradability issues.

Before washing

Soaping agent

After washing

Fig. 5: Removal of hydrolysed dye from textile fibre Soaps have been replaced by surfactants. But surfactants lack chelating properties. Thus surfactants have been replaced by polymeric washing-off agents. Together with low foaming surfactants, they exhibit excellent washing-off properties. The dispersing properties in the washing-off agent helps to keep the dyes, particularly, disperse, naphthols in the disperse condition, thus not allowing it to re-deposit on the fabric.

Reasons for poor washing-off:

i) Too high substantivity of dyes. ii) Low diffusion co-efficient dyes. iii) Short liquor ratio of washing bath. iv) High electrolyte concentration. v) Inadequate washing time. vi) Inadequate chemicals.
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Washing of reactive dyed fabrics is more complex. It is very difficult to remove the unreacted/unfixed dye from the fabric due to the presence of electrolytes. Thus it is advisable to rinse cold before treating with washing-off agents.

The factors governing the washing-off process are :

1. Time 2. Temperature 3. Type of washing-off agent 4. Concentration of washing-off agent

Cationic fixing of Reactive dye after washing

After washing a reactive dyed fabric, cationic fixing is carried out to promote its dye fixation as well as to increase its fastness properties in terms of consumers end use.

Why cationic fixing is necessary:

It is possible to eliminate color bleeding and staining of adjacent material when an article is first washed during use by after treating the dyeing with a cationic fixative. This type of product reacts with any residual unfixed anionic dye, forming an organic salt of greatly increased molecular size and of lower water solubility and diffusion rate. Such cationic fixatives lack permanence on repeated washing
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but this is not a problem since the unfixed dye will have gradually been removed by that point. They may, however, reduce the light fastness of the dyeing and are therefore more suitable for treatment of deep shades. Such an after treatment is not a remedy for inefficient washing-off of unfixed dye. If the amount of unfixed dye remaining in the goods is significant there is a risk of the precipitated dyeauxiliar complex rubbing off, particularly on wet abrasion. y

Chemical group:
The earlier day fixing agents are based on alkyl pyridinium halides. Many amines, quarternary ammonium, phosphonium and tertiary sulphonium compound can be used as dye-fixing agent. A number of synthetic resin compounds are also used.

Role of fixing agents:

Most of these are cationic surfactants, which unite with the dye anion producing a new substance of greater molecular complexity and less water-solubility with better wash fastness. The complexes may also be broken down by surface- active anions which compete with the dye anions for the cationic sites of the agent. The agent may thus be removed and wash fastness is lowered down to the original.

The mechanism of cationic dye fixing agent:

The Dye-fixing agents are cationic with long cations and short anions. The hydrolyzed reactive dyes have long anions and short cations. Wherever the unfixed dye is exhausted into the fibres the long anions of the Dyestuff react with the long cations of the Fixing agent and would precipitate inside the fibres getting trapped in situ. Since the complex is insoluble they cannot be removed by washing. Therefore the wash fastness will be improved. The insoluble complex formed outside the fabric in the bath will also
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precipitate and they need to be kept in suspension with suitable dispersing agents during soaping and removed; otherwise rubbing fastness may be affected. This situation would arise if the dyeing parameters were not properly monitored and controlled or by the use of dyestuffs whose exhaustion characteristic is very high and the reactivity (fixation) is relatively very low. The chances are that the exhausted, but unfixed hydrolyzed dyestuff will leach out during washing and hence the need to resort to Dye fixing agents. As reacting with any residual unfixed anionic dye, cationic fixing agent form an organic salt of greatly increased molecular size and of lower molecular size and of lower water solubility and diffusion rate, they may reduce the light fastness of the dyeing and therefore more suitable for treatment of deep shades.

The factors governing the fixing process are:

1. Time 2. Temperature
3. Type of fixing agent 4. Concentration of fixing agent

5. pH of the bath
The quantity of fixing agent depends on- the depth of the shade A small amount of formic or acetic acid is often necessary to

& the concentration of the product.

bring the cationic product in solution.

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CHAPTER 3:

MATERIALS & METHOD

Dyeing
Raw material: We used scoured and bleached single jersy plain knitted cotton fabrics(GSM) are collected from factory.

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Dyes: Remazol Red RGB is used as coloring material which is a homo bi-functional reactive dyes. It consists of two vinyl sulphone group as functional group. Dyeing auxiliaries:
i. ii. iii. iv.

v.

Glauber salt 99%: It is used here as dye exhaustion and leveling chemical. Caustic soda 50%(NaOH): It is used as dye fixing agent in the fibre. Soda ash 98%(NaCO3): It is used as dye fixing agent in the fibre. Sequestering agent (Lufibrol MSD): It reacts with metallic ions (Ca2+, Mg2+, Fe2+ etc)present in the water and makes a complex anion and thus deactivate them. Wetting agent (Keralon OL): It reduces the surface tension between the material and liquid. Thus helps to wet the fabric easily and quickly consequently helps the fabric to absorb chemicals quickly.

Dyeing parameters:
Dye, Remazol Red RGB(owf) Fabric weight (gm) Glauber Salt(g/l) Soda ash(g/l) Caustic soda 50%(ml/l) 1st Alkali addition 2nd Alkali addition Sequestering agent(g/l) Wetting 0.5% X 20 5 0 .75 Soda ash Caustic soda 1 1 1 1 1% X 40 5 0 .9 3% X 60 5 1.5 5% X 80 5 2 8% X 100 5 2

Soda ash+1/3 Caustic soda 2/3 Caustic soda 1 1 1 1 1 1

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agent(g/l) Temperature C Fixing Time, min Liquor Ratio 60 15 1:30 60 15 1:30 60 30 1:30 60 30 1:30 60 30 1:30

Dyeing curve: 2nd Alkali additio 1

60 Dy Fabri 1 Alkali
st

40

25-

20

1C/mi

Bath Drop Salt & Auxiliari

Aftrtreatment
Rinsing: After dyeing every shade we give it a simple rinsing first in flowing water.

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Neutralization (Acid wash): Then we removed the alkalinity i.e; neutralized the dyed fabric by acid wash.

Neutralization parameters: Liquor.. 500 ml Acetic acid 1ml/L Temperature.. Room Temperature Time. 10 min

Rinsing: After neutralization we again rinsed it in fresh water.

Soaping
Soaping is carried out after neutralization and drying of every shade%. For a single shade we have used three different types of soaping agent using two different concentration ( 0.5gm/L& 1gm/L) of each chemicals. Soaping chemicals and their properties: 1.Deckol SN (BASF): Characteristics: Nature : Anionic acrylic copolymer Physical form : Clear, yellowish, viscous liquid. pH : 7.5 Solubility : It can be diluted with water in all proportions. Stability : It is stable to acids, alkalis and electrolytes in all concentrations used in dye liquors. Application: It is a dispersing, sequestering agent and protective colloid in the dyeing of cotton and cotton/synthetic fiber blends with vat, reactive, direct and sulfur dyes.
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It is non-foaming and non-retarding. Prevents impurities in cotton (pectinates, waxes and water-hardening substances) from redepositing on the material and their formation of dye adducts with these impurities. Recommendation of use: Generally 1 g/l conc. soaping for 10 min at 200F results in a bright, clean substrate . 2.Ladipur- RSK (Clariant): Characteristics: Ionic nature Appearance Solubility Application: Sequestrant and protective colloid for use in scouring, dyeing and washing off dyeing and prints. Binds Ca and Mg ions without attacking metal complex dyes. An ecofriendly, non foaming fastness improver to be used in the dyeing, printing and during soaping. : Anionic : Form colorless liquid : Perfectly soluble

3.Easy Soap R (Intersac): Characteristics: Chemical composition: Salified Acrylic Co-Polymer Appearance : Form colorless to straw colored liquid Ionic charge : Cationic Solubility : perfectly soluble Compatibility : Compatible with non-ionic and anionic products Application: Sequestering agent specific for calcium and magnesium

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Soaping agent after dyeing and printing of cellulosics and their blends Recommendation of use: EASYSOAP R can be used in soaping of reactive dyeing or printings, quickly removes the unfixed dye and at the same time avoids the redeposition. Generally 0.3-0.5 gm/L in discontinuous treatments and 1-2 gm/L in continuous ones are needed.

Soaping parameters: Soaping agent Easy Soap R (Intersac) 0.5g/l Fabric wt, gm Temperature , C Time, min 1g/l X 95 15 Ladipur RSK (Clarient) 0.5g/l 1g/l x 95 15 Deckol SN (BASF) 0.5g/l 1g/l X 95 15

Rinsing: After every soaping the fabric was rinsed with fresh water. Then dried in oven.

Fixing
We carried out fixing after soaping and drying of every shade %. For a single shade we have used three different types of fixing agent using two different concentration ( 0.5% & 1% owf) of each chemicals. Fixing chemicals and their properties: 1.Cyclanon Fix (BASF):
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Characteristics: Ionic Nature : Aqueous solution of a cationic polymer Appearance : Colorless Liquid Compatibility : Good with cationic & nonionic agents. However, it should not be used with anionic products, sulphates etc. Solubility : Readily soluble in water Application: Cyclanon FIX is formaldehyde free after-treatment agent for improving wet fastness properties of reactive and direct dyes. Prevents bleeding & staining. Improves fastness to perspiration and wet fastness properties of printed goods. Affects light fastness of direct & reactive dyes if used in excess proportions. Should not be used on Pale shades of reactive dyes. 2.Optifix-EC (Clariant): Characteristics: Ionic nature : Cationic Polymeric Product Appearance : Form pale yellow, transparent liquid pH value : 4-6 Action: It forms electrostatic bonds between anionic dyes & cationic dye fixing agent leading to complex formation & improvement in dye fixation. Thus it increases wash fastness and prevent migration during drying operations.

This product has no detrimental effects upon shade or light fastness. It does not contribute to the pollution of mill effluents nor does it release formaldehyde odors in the dye house or on the goods. Application:
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Formaldehyde-free fixative for dyeing and prints on cellulosic fibres with direct and reactive dyes by exhaust and continuous methods. 3.HUEFIX R (Intersac): Characteristics: Chemical composition : Polyquaternary ammonium salt Appearance : Straw colored, viscous liquid Ionic charge : Cationic pH : 3.0-7.0 Application: Fixing agent for direct and reactive dyeing and printing Recommendations of use: HUEFIX R : 0.3-0.8% pH : 6-7 Temperature : 35-40C Time : 15-20 min Fixing parameters: Fixing agent (owf) Fabric wt, gm Acetic acid, g/l pH Temperature , C Time, min HUEFIX R (Intersac) 0.5% 1% X 0.5 5-5.5 40 10 Octofix EC(Clarient) 0.5% 1% X 0.5 5-5.5 40 10 Cyclanon FIX (BASF) 0.5% 1% X 0.5 5-5.5 40 10

Drying parameters: Temperature110C Time.. 10 minutes.

Estimation of Color Fastness to Wash

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 Test Method for Color Fastness to Wash: ISO 105-CO6:1994

(Third edition) This test method is more severe and usually used for high quality textiles. There are 16 different washing procedures in ISO-105-CO6 which cover the range for Home and Commercial laundering from mild to swear.

Scope: This method is intended for determining the resistance of the color of textiles of all kinds and all forms to domestic or commercial laundering procedures used for normal household articles. Industrial and hospital articles may be subjected to special laundering procedures which may be more severe in some respects. This method does not reflect the effect of optical brighteners present in commercial washing products.

Principle: A specimen of the textile in contact with specified adjacent fabric is laundered, rinsed and dried. Specimens are laundered under appropriate conditions of temperature, alkalinity, bleaching and abrasive action such that the result is obtained in a conveniently short time. The abrasive action is accompanied by the use of a low liquor ratio and an appropriate number of steel balls. The change in color of the specimen and the staining of the adjacent fabric are assessed by comparison with grey scales.

Test Specimen: We attached specimen of 10cm4cm to a piece of multi-fibre(DW) adjacent fabric also 10cm4cm, by sewing along both the shorter edges, with the multi-fibre adjacent fabric next to the face side of the specimen.
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 Test Condition for ISO 105 C06: Test No. C2S Liquor Volume... 50 ml Detergent (ECE standard) 4 gm/L Sodium Perborate. 1gm/L Sodium Carbonate. 1 gm/L Adjust pH 10.50.1 Available Chlorine.. None Time.. 30 min No. of steel balls.. 25

Test procedures: We prepared the wash liquor by dissolving 4 gm of detergent per litre of water, adjusted the pH as required by the addition of approximately 1 gm of sodium carbonate per litre of solution. As perborate is employed we prepared the washing solution containing perborate at the time of use by heating the liquor to a maximum temperature of 60 C for not more than 30 min. After washing we removed the composite specimen and removed stitch from one side and rinsed twice for 1 min in two separate 100 ml portions of water at room temperature. Then extracted the excess water from the composite specimen. Next dried the specimen in woven drier at a temperature not exceeding 60C. Finally we assessed the change in color of the specimen and the staining of the adjacent fabric using the grey scales. To assess the fastness of textiles two types of grey scales are used:
Grey scale for change in color Page | 2

 Grey scale for color staining

Grey scale for change in color: Grey scale for change in color may either be a 5-step or 9-step scale. It consists of 5/9 pairs of grey colored cards/swatches. The first member of each pair is neutral grey in color and the second member of the illustrating fastness rating 5 is identical with the first member. The second member of the remaining pairs are increasingly lighter in color so that each pair illustrates increasing contrast are perceived color differences which are defined calorimetrically. The amount of contrast between the treated and untreated fabric is related to one of the standard pairs to yield the gray scale rating. On this scale 5 indicates that next to no color was lost and 1 indicates that most color was lost.

Fig.6: Grey scale for change in color Grey scale for color staining: Grey scale for color staining may be 5 steps or 9 steps scale ranging from 5 to 1. The steps may be 5, 4, 3, 2, & 1 or 5, 4-5, 4, 3-4, 3, 2-3, 2, 1-2 & 1. The first member of each pair is white in color and the second member of the illustrating fastness rating 5 is identical with the first member. The second member of the remaining pairs is increasingly darker in color. So that each pair illustrates increasing contrast perceived color differences which are defined calorimetrically. Here the transference of color from the test specimen to an adjacent specimen is evaluated in a manner very similar to that of color change
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scale. A value of 5 corresponds to virtually no staining, whereas 1 indicates poor color fastness.

Fig.7: Grey scale for color staining

Machines used

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Gyro wash

Oven drier

It is a washing machine specially It is an electric oven used to dry designed for wash fastness test. fabrics.

Manufacturer :
Co. Ltd

James H. Heal &

Origin
England

Manufacturer : Binder
: Halifax,

Origin

: Germany

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CHAPTER 4:

RESULTS & DISCUSSION

ASSESSMENT OF THE RATING FOR COLOR FASTNESS TO WASH

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DYED SAMPLE
SHAD E% COLOU R CHAN GE RATIN G 3 3 3 3 2/3 RATINGS FOR DEGREE OF STAINING DIACETA TE BLEACH ED COTTON 3/4 3/4 3 3 2/3 POLYAMI DE POLYEST ER ACRYLI C WOOL

COTTON FABRIC DYED WITH REMAZOL RGB DYE

0.5% 1% 3% 5% 8%

3 3 3/4 3/4 3/4

4 3/4 3/4 3/4 3/4

4/5 4/5 4/5 4/5 4/5

4/5 4/5 4/5 4/5 4/5

4/5 4/5 4/5 4/5 4/5

For the untreated dyed materials, color fastness to wash in case of color change ratings is 3 (Fair) for 0.5% to 5% shade but for 8% shade, this rating is 2/3 (Poor to Fair), which is lower than other shade%. Again, in case of staining on bleached cotton, the ratings came from 3/4 (For light shade) to 2/3 (For deep shade, 8%). In case of staining on wool, all the ratings are 4/5.

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BASF
POST DYEING PROCES S WASHED SAMPLE SOAPIN G (0.5 g/l) SHADE % COLO UR CHAN GE RATIN G 4/5 4 4 4 4 4 3 3/4 3/4 3/4 4/5 4/5 4 4/5 4 4/5 4/5 4 4/5 4/5 RATINGS FOR DEGREE OF STAINING DIACE TATE 4 3/4 4 4 4 3/4 3 4 4 4 4 4 4 4 4 5 4 4 4/5 4 BLEACH ED COTTON 5 4/5 4/5 4/5 4 5 4/5 5 4/5 4/5 5 4/5 4 4/5 4/5 4/5 5 4/5 4/5 4 POLYAMI DE 4/5 3/4 4/5 5 4 4 3/4 4/5 4/5 4/5 4 4 4/5 4/5 4/5 4/5 4 4 4/5 4/5 POLYEST ER 5 4/5 5 5 4/5 5 4/5 5 5 5 5 5 5 5 5 5 4/5 5 5 5 ACRYL IC 5 4/5 5 5 5 5 4/5 5 5 5 5 5 5 5 5 5 4/5 5 5 5 WOOL

0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8%

5 4/5 5 5 5 5 4/5 5 5 5 5 5 5 5 5 5 4/5 5 5 5

WASHED SAMPLE SOAPIN G (1.0 g/l)

WASHED SAMPLE FIXING (0.5%) AFTER SOAPING (0.5 g/l) WASHED SAMPLE FIXING (1.0%) AFTER SOAPING (1.0 g/l)

ASSESSMENT OF THE RATING FOR COLOR FASTNESS TO WASH

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 Here, we can see in the table that, the color fastness to wash is improved after soaping. When we soaped the dyed samples with 0.5 g/l Dekol SN (BASF), we got better fastness to wash than what we got soaping with 1.0 g/l Dekol SN (BASF). From that we can say that, we got better result using lower amount of soaping agent. Again, we found better results in light shade using 0.5 g/l soaping agent. In case of fixing with 0.5% Cyclanon FIX (BASF) on the soaped samples (0.5g/l Dekol SN), we got better fastness to wash i.e. in 1% and 5% shade, before fixing the fastness rating were 4 & after fixing the fastness rating found 4/5. When we increased the fixing chemicals concentration, fastness also improved. For example, before fixing (Only soaping with 1.0g/l Dekol SN) the fastness rating were 4(0.5% shade), 3(1.0% shade), 3/4(5.0% shade), 3/4(8.0% shade) and after fixing with 1.0% Cyclanon FIX the fastness rating was improved to 4/5(For 0.5%, 1.0%, 5.0% & 8.0% shade).

ASSESSMENT OF THE DEGREE OF STAINING

Here, for light shade(0.5% shade) the fastness rating on the bleached cotton shows 5, where the fastness rating shows 4 for dark shade(8.0%shade). Again for most of the shades and various concentration, the fastness rating shows 4/5.
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ASSESSMENT OF THE DEGREE OF STAINING

Here, the fastness rating on the wool for all of the shades shows 5. Only 1% shade shows exceptional rating-4, when it was soaping (0.5g/l) and fixing (0.5%) with BASF chemicals.

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ASSESSMENT OF THE RATING FOR COLOR FASTNESS TO WASH

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CLARIANT
POST DYEIN G PROCE SS WASHE D SAMPL E SOAPI NG (0.5 g/l) WASHE D SAMPL E SOAPI NG (1.0 g/l) WASHE D SAMPL E FIXING (0.5%) AFTER SOAPI NG (0.5 g/l) WASHE D SAMPL E FIXING (1.0%) AFTER SOAPI NG (1.0 g/l) SHA DE % COLOU R CHAN GE RATIN GS 3/4 3/4 3/4 4 3 RATINGS FOR DEGREE OF STAINING DIACETA TE 3/4 3 3 3/4 3/4 BLEACH ED COTTON 4/5 4/5 4/5 4 3/4 POLYAMI DE 3/4 3/4 3/4 4 4/5 POLYEST ER 4/5 4/5 4/5 4/5 4/5 ACRYL IC 4/5 4/5 4/5 4/5 4/5 WOO L 5 5 4/5 5 5

0.5% 1% 3% 5% 8%

0.5% 1% 3% 5% 8%

3/4 3 3/4 3/4 3/4

4 3/4 3/4 3 3

4/5 4/5 4/5 4 3/4

4 4 4 4 4

5 4/5 4/5 4/5 4/5

5 4/5 5 4/5 4/5

5 5 5 5 5

0.5% 1% 3% 5% 8%

4 4/5 4 4/5 3/4

3 4 4 3/4 3/4

4/5 4/5 4/5 4/5 4

4 4 4 4 4/5

4/5 4/5 5 4/5 5

5 5 5 5 5

5 5 5 5 5

0.5% 1% 3% 5% 8%

4 4 4 4/5 4

3/4 3/4 3/4 4 3/4

4/5 4/5 4/5 4/5 4/5

4 4 4 4 4

4/5 4/5 4/5 4/5 4/5

5 4/5 4/5 5 5

5 5 5 5 5

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 Here in the table we can see that, when soaping is done with 0.5 g/l Ladipur- RSK the color fastness to wash is improved than that of dyed untreated samples. But when we used 1.0 g/l of RSK, fastness to wash remain unchanged, in some cases it decreased (for 1.0% and 5.0% shades). It means, when we used small quantity of soaping chemicals we got better result. But for 8% shade, rating improved from 3 to 3/4 using 1 g/l Ladipur- RSK. In case of fixing with 0.5% Optifix-EC on the soaped samples (0.5g/l Ladipur- RSK), the rating of color fastness to wash is improved. When we increased the fixing chemicals concentration, fastness also improved. For example, before fixing (Only soaping with 1.0g/l Ladipur- RSK) the fastness rating were 3/4(For 0.5%, 5.0% and 8% shades) and 3(1.0% shade), and after fixing with 1.0% Optifix-EC the fastness rating was improved to 4(For 0.5%, 1.0%, 3.0% & 8.0% shade) and 4/5 (For 5.0% shade).

ASSESSMENT OF THE DEGREE OF STAINING

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Here, for 5% shade the rating shows 4 and for 8% shade it shows 3/4, when they soaped with both 0.5g/l and 1g/l Ladipur- RSK. Again all of the shade shows the rating 4/5, , when soaped with both 0.5g/l and 1g/l Ladipur- RSK.

ASSESSMENT OF THE DEGREE OF STAINING

Here, for all shade% the rating shows 5, when we did both soaping (0.5g/l & 1g/l Ladipur- RSK) and fixing (0.5% & 1% Optifix-EC). But it shows 4/5 when we soaped with 0.5g/l Ladipur- RSK, in terms of 3% shade.

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INTERSAC
POST DYEING PROCES S WASHED SAMPLE SOAPIN G (0.5 g/l) WASHED SAMPLE SOAPIN G (1.0 g/l)
WASHED SAMPLE FIXING (0.5%) AFTER SOAPING (0.5 g/l) WASHED SAMPLE FIXING (1.0%) AFTER SOAPING (1.0 g/l)

SHAD E%

0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8%

COLO UR CHAN GE RATIN G 3/4 3/4 3/4 3 3/4 3 3/4 3 3 2/3 4 3/4 3/4 3/4 4 4 3/4 3/4 4 4

RATINGS FOR DEGREE OF STAINING DIACETA TE 3 3/4 3 3 3/4 3/4 3/4 3 3/4 3/4 3 3/4 3/4 3/4 3/4 3/4 3/4 4 4 3/4 BLEACH ED COTTON 4 4/5 3/4 3/4 3/4 4 4 3/4 3/4 3/4 4/5 4/5 4 4 3/4 4 4 4 4 3/4 POLYAMI DE 3/4 4 4 3/4 4 4 3/4 4 4 4 4 4 4 3/4 4 3/4 3/4 4 4/5 4 POLYEST ER 4/5 4/5 5 4/5 4/5 4/5 4/5 4/5 4/5 4/5 4/5 4/5 5 4/5 4/5 4/5 4/5 4/5 5 4/5 ACRYL IC 4/5 4/5 4/5 4/5 4/5 4/5 5 4/5 4/5 4/5 4/5 4/5 5 4/5 4/5 5 5 5 5 5 WOOL

5 5 5 5 4/5 4/5 5 5 5 5 5 5 5 5 5 5 5 5 5 5

ASSESSMENT OF THE RATING FOR COLOR FASTNESS TO WASH

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Here in the table we can see that, after soaping with 0.5g/l Easy Soap R of Intersac, fastness to wash is improved. But when the concentration is increased, color fastness to wash is decreased compared to previous (0.5g/l). The fixing after soaping improved the color fastness rating. For example, fixing with 0.5% Huefix R of Intersac which was soaped with 0.5g/l Easy Soap R, showed the improvement of color fastness to wash rating from 3/4 to 4(For 0.5% and 8% shades) and 3 to 3/4(5.0% shade). When we increased the amount of Huefix R, the rating of color fastness to wash was improved.

ASSESSMENT OF THE DEGREE OF STAINING

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 Here, the fastness rating on the bleached cotton shows for most of shade is 4. It shows 4/5 rating when we were soaping (1g/l) and then fixing (1%) with Intersac chemicals (for 1% shade). It also shows 3/4 rating for 3%, 5% & 8% shade for using most of these chemical concentration.

The rating for degree of staining on the wool, the fastness rating shows 5 for most of the shades. It shows 4/5 rating also for 0.5%, 1% and 8% shades.

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COMPARISON OF COLOR FASTNESS RATINGS SOAPING (0.5 g/l) WITH DIFFERENT SOAPING AGENTS
SOAPING SOAPED WITH 0.5 g/l BASF SHADE % 0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8% COLOUR CHANGE RATINGS 4/5 4 4 4 4 3/4 3/4 3/4 4 3 3/4 3/4 3/4 3 3/4 RATINGS FOR DEGREE OF STAINING BLEACHED COTTON 5 4/5 4/5 4/5 4 4/5 4/5 4/5 4 3/4 4 4/5 3/4 3/4 3/4 WOOL 5 4/5 5 5 5 5 5 4/5 5 5 5 5 5 5 4/5

SOAPED WITH 0.5 g/l CLARIANT

SOAPED WITH 0.5 g/l INTERSAC

Here we can see that, when we soaped with 0.5g/l Dekol SN (BASF) we got better result than soaping with 0.5g/l of Ladipur- RSK (Clariant) & Easy Soap R (Intersac).

COMPARISON OF DEGREE OF STAINING

Here, staining on the bleached cotton shows better result when we used the BASF chemical and Intersac shows lowest result.
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COMPARISON OF DEGREE OF STAINING

Here, staining on the wool shows the color fastness rating 5 and 4/5 for all of the chemicals used.

COMPARISON OF COLOR FASTNESS RATINGS

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 Here, when we soaped (1g/l) with Dekol SN (BASF) and Ladipur- RSK

SOAPING (1.0 g/L) WITH DIFFERENT SOAPING AGENTS

SOAPING SOAPED WITH 1.0 g/l BASF SHADE % 0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8% COLOUR CHANGE RATINGS 4 3 3/4 3/4 3/4 3/4 3 3/4 3/4 3/4 3 3/4 3 3 2/3 RATINGS FOR DEGREE OF STAINING BLEACHED COTTON 5 4/5 5 4/5 4/5 4/5 4/5 4/5 4 4/5 4 4 3/4 3/4 3/4 WOOL 4/5 5 5 5 5 5 5 5 5 5 4/5 5 5 5 5

SOAPED WITH 1.0 g/l CLARIANT

SOAPED WITH 1.0 g/l INTERSAC

(Clariant) we got better result compare to Easy Soap R (Intersac).

COMPARISON OF DEGREE OF STAINING

Here, the degree of staining on the bleached cotton shows rating 5 and 4/5 for all shades for Dekol SN and Ladipur- RSK except Easy Soap R (4 & 3/4).

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 Here, the degree of staining on the wool shows rating 5 for all shades except 0.5% shade (4/5) for Dekol SN (BASF) and Easy Soap R (Intersac).

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Comparison: Fixing after Soaping VS Soaping after Fixing

Generally after neutralization soaping is done, and then fixing is carried out, but if fixing is carried out without soaping and then soaping is done, then in this case we found very unsatisfactory results.

FIXING AFTER SOAPING WITH BASF

SOAPINGFIXING
DYED SAMPLES FIRST SOAPING WITH 0.5g/l SOAPING AGENT, THEN FIXING WITH 0.5% FIXING AGENT

SHADE %

COLOR CHANGE RATINGS 4/5 4/5 4 4/5 4 4/5 4/5 4 4/5 4/5

0.5% 1% 3% 5% 8%

RATINGS FOR DEGREE OF STAINING BLEACHED COTTON 5 5 4/5 4 4/5 4/5 4/5 5 4/5 4/5 4 5 5 5 5 5 4/5 5 5 5

DYED SAMPLES FIRST SOAPING WITH 1.0 g/l SOAPING AGENT, THEN FIXING WITH 1.0 % FIXING AGENT

0.5% 1% 3% 5% 8%

SOAPING AFTER FIXING WITH BASF

FIXINGSOAPING
DYED SAMPLES FIRST FIXING WITH 0.5% FIXING AGENT, THEN SOAPING WITH 0.5 g/l SOAPING AGENT DYED SAMPLES FIRST FIXING WITH 1.0% FIXING AGENT, THEN SOAPING WITH 1.0 g/l SOAPING

SHADE %

COLOR CHANGE RATINGS 3 3 3 3/4 3/4 3 3 3/4 3/4 3

0.5% 1% 3% 5% 8% 0.5% 1% 3% 5% 8%

RATINGS FOR DEGREE OF STAINING BLEACHED Wool COTTON 5 5 5 5 3/4 5 3/4 5 3 5 5 4/5 4/5 4 4 5 5 5 5 5 Page | 1

AGENT

CHAPTER 5:

OUR FINDINGS

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Use of soaping agent on the reactive dyed cotton fabrics improved the colour fastness to wash ratings than the colour fastness to wash ratings of the dyed fabrics. We got better colour fastness to wash effects using 0.5g/l soaping agent than what we got soaping with 1.0g/l soaping agent. Use of increased amount of fixing agent increased the colour fastness to wash. The improvement of color fastness to wash was found more in darker shades than lighter shade using soaping & fixing chemicals. BASF soaping & fixing chemicals gave better result than the chemicals of Clariant & Intersac Company.

Over all, the soaping and fixing chemicals of Intersac Company gave comparatively bad results among the three.

Fixing after soaping gave much better wash fastness to color in comparison to soaping after fixing.

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Limitations
The colour change ratings found using of 1 g/l soaping agent was lower than the ratings found using 0.5 g/l soaping agent. This is found for all the three soaping agents. This may need further experiment and then there might be some logic behind this outcome, or the more amount of soaping agent affected the soaping bath conditions.

Suggested Recipe Soaping:

Soaping agent : 0.5 gm/L Temperature Time : 90C : 15 min

Fixing:
Fixing agent Acetic Acid : 0.5% (Owf) : 0.5 g/l (pH-5.5)
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Temperature Time

: 40C : 10 min

CHAPTER 6:

CONCLUSION

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This project work was confined to dyeing with one kind of dyes in five different shades to be washed off and fixed with three pairs of soaping and fixing chemicals of three manufacturers. Investigations with other dyestuffs and many more washing and fixing agents are necessary before making any generalized statements. As washing play key roles in reactive dyeing, detailed knowledge of their chemical composition is also essential to understand and explain all the facts. Similarly chemical constitution of fixer should also be known to comprehend their effects. However It may be suggested that further study be undertaken with other washing off and fixing materials having complete technical data and using testing equipment in proper order.

REFFERENCES

Basic Principle of Textile Coloration by D. Broadbent Dyeing & Chemical Technology of Textile Fibres by E.R. Trotman
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Dictionary of Textile Chemistry http://www.indiantextilejournal.com/reactive dyes past & future

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