68

CHAPTER 3

EXPERIMENTAL PLAN

3.1 INTRODUCTION

The present chapter describes the experimental plan of the research

work in three divisions as given in Figure 3.1. The first division describes the

application of different chemicals on various wool fibers and Angora rabbit

hair. The physio-chemical, mechanical and morphological properties studied

for the untreated and chemically treated fibers are given in Figure 3.2.

The second division describes the utilization of chemical treated

Angora rabbit hair as given in Figure 3.3. Angora rabbit hair was treated with

the suitable chemical and the treated fibre was used in the production of a

blend yarn. The yarn was converted into union fabric. The union fabric was

then finished with ten finishing formulations and their performance properties

were evaluated. The compatibility of rabbit hair with wool, and cotton fibre

substrates in the production of hygienic textile by the application of natural

ingredients such as aloevera were also studied.

The third division describes the application of a cellulase and a

protease enzyme either separately or successively, followed by treatment with

different finishing chemicals. Then the performance properties of finished and

unfinished woolen material with and without prior enzyme treatment(s) were

evaluated as given in Figure 3.4.

69

Figure 3.1 Flow chart of the experimental plan

To treat the different wool fibers and Angora rabbit hair with

different chemicals and to select a suitable chemical treatment

based on the physiochemical and mechanical properties of

treated fibers.

To develop a union fabric using treated Angora rabbit hair and

viscose rayon followed by finishing with softeners and to

evaluate its performance properties.

To treat the woolen materials using enzymes followed by

finishing with various formulation in order to improve their

aesthetic and functional properties

70

Figure 3.2 Flowchart for chemical treatment on wool fibres and rabbit hair and evaluation of properties

1. Marwari

2. Avikalin

3. Nali

4. Magra

5. Bharat merino

6. Kashmir merino

7. AUS merino

8. RUS merino

9. NZ merino

10. Angora rabbit hair

1. Thioglycollic acid

2. NaHSO3 in water,

3. NaHSO3 in ethanol

4. Morpholine

5. Formic acid

6. Sodium hydroxide

7. Protease enzyme

1. Fibre diameter

2. Fibre length

3. Fibre strength

4. Crimp frequency

5. Moisture regain

6. UB solubility

7. Sulphur content

8. Fibre swelling

9. Keratose content (α, β, γ)

10. Dye uptake

11. Fastness properties

12. Morphological components

Chemical treatments Fibres Properties

71

Error!

Figure 3.3 Flowchart for product development from Angora rabbit

hair

Different chemical treatments on rabbit hair and

evaluation of their properties

Suitable chemical treatment for product

development

Blending treated fibre with viscose rayon fibre in

20:80 ratio and production of blended yarn through

Union fabric produced from blend yarn

Preparatory processing and finishing of union fabric and

evaluation of their performance properties

Evaluation of properties of rabbit hair: viscose rayon

blend yarn

Antimicrobial assessment of natural ingredient treated

rabbit hair substrates

72

Figure 3.4 Flowchart for enzyme treatment(s) and subsequent finishing treatment on wool/cotton union fabric and

their evaluation

Cellulase enzyme

treatment

(Bactosol-CA)

Cellulase enzyme treatment

followed by protease

enzyme treatment

Protease / Lipase enzyme treatment

(Bactosol-WO, Savinase-16.0L Ex,

Papain-URPP and Lipolase-100T)

Wool/Cotton

Union fabric

Treating with different finishing

chemicals both in individual and

combination forms

Evaluation of performance properties of untreated, enzyme treated, enzyme treated and finished,

finished-only wool-cotton union fabrics

No enzyme treatment No finishing

Enzyme(s) treated

Wool/Cotton union fabric

No enzyme treatment

73

3.2 STUDY ON THE EFFECT OF CHEMICAL TREATMENT

ON WOOL FIBRE AND ANGORA RABBIT HAIR

3.2.1 Materials

3.2.1.1 Wool fibres and Angora rabbit hair

The indigenous Indian wools Marwari, Nali and Magra and

crossbred wools like Bharat merino (a crossbred of Merino with Chokla/Nali)

(Parthasarathy et al 1996) and Avikalin (a crossbred of Malpura with

Rambouillet) (Parthasarathy et al 2000) and a speciality hair fibre Angora

Rabbit Hair were procured from Central Sheep and Wool Research Institute

(CSWRI), Rajasthan (India). Other wool fibres were procured from different

organization as follows; Kashmir fine merino wool from Sheep Husbandry

Department, Srinagar, Jammu & Kashmir (India), Australian 64’s Merino

wool from Raymond woolen mills, Mumbai (India), Russian Merino wool

from Moscow Textile Institute, Moscow (Russia) and New Zealand Fine

Merino wool from Wool Research Organization of New Zealand.

The wool fibres were immersed in luke-warm water to remove

suint, rinsed in repeated change of distilled water, dried at 80oC and then

degreased with petroleum ether in Soxhlet extractor. Vegetable matters from

degreased wool were removed manually. The purified fibres were conditioned

at 25oC and 65% relative humidity as per standard condition.

Even though Angora rabbit hair has special characteristics, its

processing is difficult due to lower scale height and absence of inter-fibre

cohesion. Since products of Angora rabbit hair have high demand in elite

group of consumers, this fibre has been taken along with wool fibres in this

work to improve its processing as well as aesthetic value.

74

3.2.1.2.1 Enzyme and reagents

The enzyme used in this study was Bactosol-WO, an alkaline protease

enzyme supplied by Clariant Chemicals (I) Ltd., Mumbai. All other chemicals used

were of analytical grade.

3.2.2 Methods

3.2.2.1 Evaluation of physical properties

The average fibre diameter of the fibres was measured as per

standard ASTM: D2130-90 (2001a). The fibre length of fibre was measured

as per well-established standard IS 1377:1971 (2004a). The fibre strength of

the untreated fibre and chemically treated fibres was measured as per standard

ASTM D 3822-01 (2004a). The crimp of fibre was measured by calculating

the number of waviness per inch as per standard method IS 6124:1971

(2004b). The moisture content of fibre was measured as per standard ASTM

D-1576-90 (2001b).

3.2.2.2 Chemical treatments

3.2.2.2.1 Acid, alkali and enzyme treatment

The purified wool fibres and Angora rabbit hair were pretreated

with formic acid (98%, 15 minutes, 25oC), morpholine (10% v/v, 30 minutes,

25oC), sodium hydroxide (1.5% w/v, 15 minutes, 25oC) and Bactosol WO

(4% owm, 45 minutes, 50oC, pH 8.5) separately. Finally the pretreated wool

fibres were thoroughly washed with distilled water to get rid of corresponding

used chemicals.

75

3.2.2.2.2 Reduction treatment

Reduction using thioglycollic acid: Cystine linkages in the wool

were reduced to cysteine in 0.10 M thioglycollic acid (AR) for 16 hours,

followed by subsequent blocking of thiol groups with 0.1 M iodoacetic acid

between pH 8 and 9 for 24 hours to prevent rapid reformation of disulphide

bonds by atmospheric oxidation. Reduced and blocked wool fibres were

subjected for the determination of percentage reduction (Maclaren 1962).

Reduction using sodium bisulphite: Sulphytolysis of wool by

sodium bisulphite (AR) in 50% ethanol-water and 100% aqueous media was

done at pH 5.4 for 2 ½ hours by the procedure of Miro and Hueso, followed

by blocking of thiol / sulfydryl groups by dyeing of reduced wool fibre with

reactive dyes (Miro and Hueso 1968).

3.2.2.3 Dyeing and measurement of dye uptake

The intact and chemically treated (reduced, treated with formic

acid, morpholine, sodium hydroxide and protease enzyme) Angora rabbit hair,

Indian wools and fine wools were dyed with Drimalan Yellow F-3GL (CI

Reactive yellow 69) by the established method of dyeing of wool fibre with

reactive dye (Lewis 1992). A spectronic-20 D spectrophotometer was used to

determine the optical density of the aqueous dye solution at wavelength of

maximum absorption (λmax).

After extraction of dye from dyed wool fibre by treatment with

pyridine-formic acid-water mixture, dye uptake on wools was then measured

spectro-photometrically (Lewis 1977).

76

3.2.2.4 Fastness properties

The washing, light and bleaching fastness of intact, dyed and

chemically treated and dyed wool fibres and Angora rabbit hair were

evaluated as per standard method AATCC 61-1996 (2003a), AATCC 16-1998

(2003b) and AATCC 188-2000 (2003c) respectively.

3.2.2.5 Isolation of morphological components and their dyeability

Morphological components namely cuticle and cortical cells from

each formic acid swollen wool fibres and angora rabbit hair were separated by

ultrasonic disruption followed by the screening technique of Kulkarni and

Bradbury (1971) as in Figure 3.1.

The cuticle and cortical cells were quantitatively estimated,

followed by their dyeing (1% shade) with Drimalan Yellow F-3 GL by the

established procedure (Lewis 1992). The medullary cells from chloroauric

acid (AR) stained wool fibres and Angora rabbit hairs were separated in pure

form by the technique of Bradbury and O’Shea (1969).

3.2.2.6 Preparation of high- and low-sulphur protein fractions

(keratoses)

The keratose fractions from peracetic acid oxidized wool fibres /

rabbit hair were isolated by the established method (Corfield et al 1958).

77

Ultrasonicate 1 g chopped wool fibres in 50 ml formic acid (99%) and pass through Buchner Funnel to remove intact fibre segments

Fibrous residue retained Filtrate centrifuge

Residue Supernatant Dissolved

matter

Wash repeatedly with water and finally with ethanol at centrifuge. Sieve the ethanolic suspension through

125 micron Nytel cloth

Fibrous residue

retained Filtrate – Cortical cells

+Macro fibrils +Cuticle fragments Sieve the ethanolic suspension through 125 micron Nytel cloth

Residue retained

Intact cortical cells Filtrate

Disrupted cortical cells + Macrofibrils + Cuticle fragments

Figure 3.5 Schematic diagram showing separation of morphological

components from wool and rabbit hair

3.2.2.7 Evaluation of chemical properties

3.2.2.7.1 Estimation of urea bisulphite solubility

Urea-bisulphite solubility (UBS) of wool fibre and Angora rabbit

hair was estimated by the method given by Dusenbury (1960).

78

3.2.2.7.2 Estimation of cystine, cysteine and total sulphur content

A known weight of conditioned wool/rabbit hair was hydrolyzed in

5.7 N hydrochloric acid in a sealed glass tube at 105oC for 24 hours. The acid

was then removed in vacuum over caustic soda and the hydrolysate dissolved

in known volume of distilled water. The sulphur containing amino acids

cystine and cysteine from the acid hydrolysate were determined

colourimetrically by the method of Sinohara(1935) as modified by Fletcher

and Robson (1962).

3.2.2.8 Estimation of swelling in formic acid

The swelling of wool fibres and Angora rabbit hair was estimated

by the gravimetric method (Caldwell and Milligan 1970).

3.2.2.9 SEM Study

SEM photograph of untreated and treated Angora rabbit hair were

taken from 30kV scanning electron microscope JEOL (Japan) Model

JSM-6360.

3.3 ANGORA RABBIT HAIR IN VALUE ADDED TEXTILES

3.3.1 Angora rabbit hair /viscose rayon blend yarn

3.3.1.1 Materials

The Angora rabbit hair (14.24 micron and 60 mm length) and staple

viscose rayon fibre (14.0 micron and 51 mm length) were selected for this

study. All other chemical reagents used were of analytical grade.

79

3.3.1.2 Methods

The Angora rabbit hair was treated with sodium hydroxide (Sodium

hydroxide-1.5% (w/v); 15 minutes; 25oC; 1:20 MLR; Sandoclean-PCJ-

0.1gpl), neutralized with 0.25% acetic acid, washed and dried. The sodium

hydroxide treated Angora rabbit hair was hand mixed with staple viscose

rayon fibre in 20:80 ratio. The blended fibre mixture was fed directly into a

carding machine and the machinery setting for carding, drafting and spinning

process were similar to 23’s conventional cotton spinning system.

3.3.1.3 Quality parameters of blend yarn

The blend ratio of the blend yarn was estimated by removing rabbit

hair by treating the yarn with 5% sodium hydroxide (w/w) at 60oC for

15 minutes. The blend ratio was in 19.9: 80.1. The quality parameters of the

blend yarn were evaluated as per the standard methods with and without

sodium hydroxide treated rabbit hair in the yarn. The physical parameters of

the yarn such as count (ASTM 2004b), moisture regain (ASTM 2004c), twist

(ASTM 2004d), single yarn strength (ASTM 2004e), total imperfections and

hairiness index (ASTM 2004f) were evaluated. Absorbency of yarn was

evaluated by calculating time required to immerse a known weight of yarn by

a standard weight in a water column.

3.3.2 Union fabric from rabbit hair /viscose rayon blend yarn

3.3.2.1 Materials

The above said blend yarn (23’s) was taken as weft and grey cotton

yarn (2/40’s) as warp, and woven into a fabric (58 EPI; 60 PPI; 150±5 g/m2)

as plain weave in a power loom.

80

3.3.2.2 Methods

3.3.2.2.1 Preparatory processing of union fabric

The grey fabric was desized with an amylase enzyme (Bactosol-

HTN -1 ml/l, Sandoclean PCJ-0.5gpl; pH 5.5 with acetic acid; 60oC; 1:10

MLR; 45 minutes), mild scoured (Sodium hydroxide-2% (owm); Sandoclean

PCJ-1.0% (owm); 85oC; 1:10 MLR; 60 minutes) and cold bleached

(Hydrogen peroxide-3% (owm); Sodium carbonate-1% (owm); Sandoclean

PCJ-0.5% (owm), pH 8.5; 25oC; 1:10 MLR; 6 Hours) with intermediate

washing and drying. The weight loss in desizing, scouring and bleaching were

1.79%, 1.29% and 0.23% respectively.

3.3.2.2.2 Finishing of union fabric

The bleached fabric was treated with ten finishing formulations as

given in Table 3.1.

For each finishing formulation, Sandoclean PCJ-0.25gpl solution

was added and the pH was adjusted to 5.0±0.2 by adding 0.5 % acetic acid.

The bleached fabric (G0) of 35 cm 35 cm of dimension was impregnated in

the finishing bath for 5 minutes at 25oC and padded with 80±5 % expression

under 1.5 Kg/cm2 using a laboratory padder (RB Engineering Ltd., Gujarat,

India). After padding, the fabric was dried at 100oC in an oven and cured at

150oC for 3 minutes in high temperature steamer (RB Engineering Ltd.,

Gujarat, India), washed with distilled water and dried.

81

Table 3.1 Recipe of finishing treatments for union fabric

S.No. Recipe Abbreviation

1 Grey G

2 Bleached G0

3 Sandosoft-SPG = 30gpl* G1

4 Sandoperm-SE1 = 10gpl G2

5 Ceraperm-TOWI = 30gpl G3

6 Ceraperm-Jet = 30 gpl G4

7 Ceraperm- MW = 30gpl G5

8 Ceraperm-UP = 30gpl G6

9 Sandoperm-RPU = 30 gpl G7

10 Ceraperm-Aqua = 30gpl G8

11 Sandoperm-RPU = 20 gpl Ceraperm-Aqua = 10gpl

G9

12 Sandosoft-SPG = 30 gpl Ceraperm- MW = 15gpl Ceraperm-Aqua = 15gpl

G10

* - needs no curing

3.3.2.2.3 Evaluation of performance properties

The performance properties of finished and unfinished union fabric

such as finish add-on, moisture regain (ASTM 2001b), wicking height

(Harnett et al 1984), wettability (BSI 1990a), bending length (ASTM 2001c),

flexural rigidity, bending modulus (BSI 1990b), dry crease recovery angle

(AATCC 2003d), drape coefficient (BSI 1990c), tearing strength (ASTM

2004g), CIE whiteness index (AATCC 2003e) and area shrinkage (AATCC

2003f) were evaluated.

82

3.3.3 Application of natural antimicrobial ingredients on wool,

rabbit hair and cotton substrates

3.3.3.1 Materials

The materials with the following specification were taken for this

study. 100% semi-bleached cotton fabric (plain weave, 80’s count, 78EPI and

60PPI, 75g/m2), Bharat merino wool fibre (23µ, 75mm length) and Angora

rabbit hair (16µ and 70mm length). The wool and rabbit hair were mild

scoured with 0.5% sodium carbonate and 0.1% non-ionic wetting agent at

50oC for 30 minutes, washed with distilled water and dried at ambient

condition prior to application.

3.3.3.2 Natural antimicrobial ingredients

Chitosan, with a deacetylation of 90% (molecular weight of 65 kilo

dalton) was procured from Central Marine Fisheries Research Institute,

Kochi-682 018 (India). Aloevera (molecular weight of 200 kilo dalton) in gel

form and curcumin (molecular weight of 368.39 gm) in powder form were

procured from IFGTB, Coimbatore, India. All other chemicals mentioned

elsewhere were analytical grade reagents.

3.3.3.3 Methods

3.3.3.3.1 Pretreatment

The semi bleached cotton fabric was subjected to hydrogen

peroxide bleaching as per standard procedure (Trotman 1976). The formic

acid pre-treatment was given to both wool fibre and Angora rabbit hair. The

bath was set with 10% (owf) formic acid (98%) and the material were entered

83

at 25oC and treated separately for 30 minutes with material to liquor ratio as

1:10, then washed with distilled water and dried.

3.3.3.3.2 Antimicrobial treatment

Chitosan was dissolved with 2% acetic acid solution; Aloe vera and

curcumin were dissolved with hot distilled water, and they were filtered

before application. The required quantity of antimicrobial chemical was taken

in a bath with material to liquor ratio of 1:100. The sample was entered into

the bath and the pH was maintained at 5.0±0.2 with acetic acid solution. The

bath temperature was raised to boil and kept at this temperature for 30

minutes. Then, the bath was cooled to 30oC; the sample was taken out and

washed with warm water, rinsed with cold water and dried. The compositions

of natural antimicrobial ingredients taken for the treatment either separately or

combination with each other were as follows.

1. Aloe vera - 5 gpl

2. Curcumin - 5 gpl

3. Chitosan - 3 gpl

4. Curcumin - 5 gpl + Chitosan- 3 gpl

5. Aloe vera - 5 gpl + Curcumin- 5 gpl

6. Aloe vera - 5gpl + Chitosan- 3 gpl

7. Aloe vera - 5gpl + Curcumin- 5 gpl + Chitosan - 3 gpl

3.3.3.3.3 Assessment of antimicrobial activity

The antimicrobial activity of untreated and natural ingredients

treated fibrous substrates was determined as per standard method described by

Quinn (1962). The amount of bacterial and fungal growth in inoculated and

84

incubated samples was determined through serial dilution (10-1, 10-2 and 10-3)

and subsequent inoculation of sterile agar. The numbers of bacterial and

fungal colonies were counted visually using a microscope. The wash fast test

was carried out according to ISO6330-1984E (ISO 2005) with a precision

washer for 5, 10, 15, 20 and 25 washings followed by the assessment of

antimicrobial activity on them.

3.4 EFFECT OF ENZYME TREATMENT FOLLOWED BY

FINISHING TREATMENT ON WOOL/COTTON UNION FABRIC

3.4.1 Materials

3.4.1.1 Wool/cotton union fabric

Central Sheep and Wool Research Institute, India (CSWRI) had

developed wool/cotton union fabrics of different specifications from Bharat

merino woolen yarn as weft and cotton yarn as warp (Anon 2006).

Table 3.2 Specifications of wool/cotton union fabric

S. No.

Study Parameters

1 2 3 4 5

1 Ends per inch 40 28 40 40 40

2 Picks per inch 30 17 16 16 15

3 Weave (twill) 2/2 3/1 2/2 2/2 2/2

4 Weight (g/m2) 350 372 365 363 340

5 Warp count (’s) 2/15 2/10 2/15 2/15 2/15

6 Weft count (Nm) 4.05 2.05 2.75 2.75 2.74 7 Thickness (mm) 1.10 1.63 1.52 1.52 1.50

8 Fibre ratio as wool: cotton (%)

60:40 63:37 65:35 66:34 67:33

85

3.4.1.2 Enzymes The details of different enzymes used for this study were given in

Table 3.3. Based on the composition of wool and cotton in the union fabric

and on enzyme manufacturer’s technical information, the concentration of

cellulase and protease enzyme used for this union fabric was optimized by

taking various trails.

The optimum concentration of Bactosol-CA Liq. (acid stable

cellulase enzyme), Bactosol-WO (alkali stable protease enzyme), Savinase-

16.0LEx (alkali stable protease enzyme), Papain-URPP (neutral protease

enzyme) and Lipolase-100T (lipolytic enzyme) used for this fabric were 1gpl,

4%, 2%, 2% and 3% over the weight of wool portion (oww) respectively.

Table 3.3 Details of enzymes used

S. No

Enzyme EC No Source Declared activity

1 Savinase- 16.0L Ex

E.C.3.4.21.62 Novozymes South

Asia Pvt. Ltd., India 16

KNPU/mg

2 Papain- URPP

E.C.3.4.22.2 Senthil Papain,

Coimbatore, India 3.1 U/mg

3 Lipolase-

100T E.C.3.1.1.3

Zydex Corporation Mumbai, India

100 KLU/mg

4 Bactosol-

CA --

Clariant Chemicals (I) Ltd., Mumbai

--

5 Bactosol-

WO --

Clariant Chemicals (I) Ltd., Mumbai

--

6 Bactosol-

HTN --

Clariant Chemicals (I) Ltd., Mumbai

--

86

3.4.1.3 Finishing chemicals

The finishing chemicals used for this study were supplied by

Clariant Chemicals (India) Ltd., Mumbai, India. They were Nuva-

HPU(Fluorocarbon dispersion), Finish-VLF(modified N-methylol

dihydroxylethylene urea), Ceraperm-MW (modified micro polysiloxane),

Sandosoft-SPG(Cationic softener), Curol-EWL(extender for fluorocarbon),

Ceraperm-UP(modified macro polysiloxane), Sandoperm-SE1(nano

polysiloxane), Sandoperm-RPU (Polyurethane based softener), Ceraperm-

TOWI(nano polysiloxane), Ceraperm–Jet(micro polysiloxane), Sanitized T-

9919(antimicrobial agent), Sandolube-HD(non-ionic softener) and Ceraperm-

Aqua(modified macro polysiloxane). Chitosan (cationic biopolymer) with

90% deacetylation was supplied by Indian Sea Foods, Cochin, India.

Synthappret BAP (50% solids) (Bayer) a bisulphate adducts of polyurethane

was supplied by LANXESS India Pvt. Ltd., Mumbai, and β–cyclodextrin was

supplied by DKSH India Pvt. Ltd, Mumbai. All other chemicals used in the

study were AR grade.

3.4.2 Methods

The effect of prior enzyme treatment and subsequent chemical

finishing treatment on aesthetic properties of wool/cotton union fabric was

studied as study 1,2,3,4 and 5 and each study would differ in application of

enzymes and finishing chemicals (refer Table 4.21). In these studies, the

wool/cotton union fabric was treated with cellulase enzyme and protease

enzyme either separately or successively with intermediate washing and

drying. Then the untreated and enzymes treated fabrics were treated with

different finishing chemicals such as polysiloxane emulsion, cationic softener,

polyurethane softener either in individual form and/or in combination form.

87

3.4.2.1 Study on the effect of cellulase enzyme and protease enzyme

(PE1) treatment followed by finishing treatment on wool/cotton

union fabric

In first chemical finishing study, the wool/cotton union fabric of

above-mentioned specification was taken. It was treated with Bactosol-CA

(Enzyme-1gpl; pH 5.5 with acetic acid; 55oC; 60 minutes; 1:20 MLR;

Sandoclean PCJ-0.1gpl) and Bactosol-WO (Enzyme-4% oww; pH 8.5 with

sodium carbonate; 60 minutes; 50oC; 1:20 MLR; Sandoclean PCJ-0.1gpl)

separately as well as successively with intermediate washing and drying.

Then the untreated and enzyme treated fabrics were treated with finishing

chemicals as per recipe given in Table 3.4.

Table 3.4 Recipe of finishing treatments for study-1

S.No. Recipe Condition Abbreviation 1 Unfinished -- A0

2 Nuva-HPU – 60gpl Curol-CWI – 20 mlpl

Cured at 160oC/ 3 minutes A1

3

Finish-VLF – 60gpl Ceraperm-CW – 10 gpl Sandolube-HD – 30 mlpl MgCl2 – 12 gpl

Cured at 150oC/ 3 minutes A2

4 Ceraperm-MW – 30 gpl Cured at 150oC/ 3 minutes A3

5 Sandosoft-SPG – 30 gpl Dried at 100oC and no curing A4

6 Ceraperm-MW – 20 gpl Sandosoft-SPG – 40 gpl

Cured at 150oC/ 3 minutes A5

7 Ceraperm-Aqua – 30 gpl Cured at 150oC/ 3 minutes A6

8 Chitosan – 1 gpl CH3COOH - 5%

Cured at 130oC/ 5 minutes A7

88

For each finishing formulation, Sandoclean-PCJ - 0.25gpl solution

was added and the pH was adjusted to 5.0±0.2 by adding 0.5 % acetic acid.

The fabric of 35cm x 35cm dimension was taken and impregnated in the

finishing solution for 5 minutes at 25oC and padded with 80±5 % expression

under 1.5 Kg/cm2 using a laboratory padder (RB Engineering Ltd., Gujarat,

India). After padding, the fabric was dried at 100oC in an oven and cured in

high temperature steamer (RB Engineering Ltd., Gujarat, India) as per

conditions mentioned in the Table 3.4, washed with distilled water and dried.

The performance properties of finished and unfinished fabric such

as finish add-on, wicking height, moisture regain, wettability, tearing strength,

area shrinkage, drape coefficient, bending length, flexural rigidity, bending

modulus and dry crease recovery angle with and without prior enzyme

treatment(s) were evaluated.

3.4.2.2 Study on the effect of cellulase enzyme and protease enzyme

(PE2) treatment followed by finishing treatment on wool/cotton

union fabric

In second chemical finishing study, the wool/cotton union fabric of

above mentioned specification was taken. It was treated with Bactosol-CA

(Enzyme-1 gpl; pH 5.5 with acetic acid; 60 minutes; 55oC; 1:20 MLR;

Sandoclean PCJ-0.1gpl) and Savinase-16.0L Ex (Enzyme-2% (oww); pH 8.5

with sodium carbonate; 30 minutes; 50oC; 1:20 MLR; Sandoclean PCJ-

0.1gpl) separately and successively. The untreated and enzyme treated fabrics

were treated with finishing chemical as per recipe given in Table 3.5. The

finishing treatments were similar to treatments described in 3.4.2.1.

89

Table 3.5 Recipe of finishing treatment for study-2

S. No.

Recipe Condition Abbreviation

1 Unfinished -- B0

2 Ceraperm-TOWI - 50 gpl Dried at 100oC and cured at

150oC / 3 minutes

B1

3 Ceraperm-MW – 30 gpl B2

4 Ceraperm-Aqua – 30 gpl B3

5 Sandoperm-RPU- 30 gpl B4

The performance properties such as finish add-on, wicking height,

moisture regain, tear strength, area shrinkage, drape coefficient, bending

length, flexural rigidity, bending modulus and dry crease recovery angle of

finished wool/cotton union fabrics with and without prior enzyme

treatment(s) were evaluated.

3.4.2.3 Study on the effect of two different protease enzyme treatment

followed by finishing treatment on wool/cotton union fabric

In third chemical finishing study, the wool/cotton union of above-

mentioned specification was taken. It was treated with Savinase 16.0L-Ex

(Enzyme-2% (oww); pH 8.5 with sodium carbonate; 30 minutes; 50oC;

1:20 MLR; Sandoclean PCJ-0.1gpl) and Papain-URPP (Enzyme-2%(oww);

sodium bisulphite - 10% (oww); pH 6.5 with sodium carbonate; 30 minutes;

50oC; 1:20 MLR; Sandoclean-PCJ-0.1gpl) separately, followed by

neutralization with 0.25% acetic acid, washed with water and dried.

90

The untreated and protease enzyme treated fabric were treated with

finishing chemical as per recipe given in Table 3.6. The finishing treatments

were similar to treatments described in 3.4.2.1. The performance properties

such as finish add-on, moisture regain, wicking height, wettability, dry crease

recovery angle, tear strength, handle by subjective assessment, primary and

total hand value for winter suiting fabric by Kawabata hand evaluation for

winter suiting fabric, bending length, flexural rigidity and bending modulus of

unfinished and finished wool/cotton union fabrics with and without prior

enzyme treatment were evaluated.

Table 3.6 Recipe of finishing treatment for study-3

S. No

Recipe Condition Abbreviation

1 Unfinished -- C0

2 Sandosoft-SPG = 50gpl Dried at 100oC and no curing

C1

3 Sandoperm-SE1 = 10gpl

Dried at 100oC and cured at 150oC for 3

minutes

C2

4 Ceraperm-TOWI = 50gpl C3

5 Ceraperm- MW = 50gpl C4

6 Ceraperm-UP = 50gpl C5

7 Sandoperm-RPU = 50 gpl C6

8 Ceraperm-Aqua = 50gpl C7

9 Sandoperm-RPU = 35 gpl Ceraperm-Aqua = 15gpl

C8

10 Sandosoft-SPG = 50 gpl Ceraperm- MW = 15gpl Ceraperm-Aqua = 15gpl

C9

91

3.4.2.4 Study on the effect of protease and lipase enzyme treatment

followed by combination finishing treatment on wool/cotton

union fabric

In fourth chemical finishing study, the wool/cotton union fabric of

above mentioned specification was taken. It was treated with Savinase-16.0L

Ex (Enzyme-2 % (oww); pH 8.5 with sodium carbonate; 30 minutes; 50oC;

1:20 MLR; Sandoclean PCJ-0.1gpl) and Lipolase-100 T (Enzyme-3% (oww);

pH 9.5 with sodium carbonate; 60 minutes; 55oC; 1:20 MLR; Sandoclean

PCJ-0.1gpl) separately, neutralized with 0.25% acetic acid, washed with

water and dried.

The untreated and enzyme treated union fabric were treated with

selective six finishing combinations as per recipe given in Table 3.7. The

required finishing chemicals were taken in a bath with 0.25gpl Sandoclean-

PCJ and stirred well to get a homogenous mixture and the pH was adjusted to

5.00.2 by adding 0.5 % acetic acid. The sample was impregnated in the

finishing bath for 5 minutes at 25oC and padded with 80±5 % expression.

After padding, the samples were dried at 100oC in an oven and cured at 150oC

for 3 minutes in high temperature steamer, washed with distilled water and

dried.

The performance properties such as finish add-on, wicking height,

moisture regain, wettability, tear strength, bending length, flexural rigidity,

bending modulus, dry crease recovery angle, handle by subjective assessment

and primary and total hand value for winter suiting fabric by Kawabata hand

evaluation system for winter suiting fabric of finished and unfinished

wool/cotton union fabric with and without prior enzyme treatment were

evaluated.

92

Table 3.7 Recipe of finishing treatment study-4

S. No Recipe Abbreviation

1 Unfinished Unfinished (E0)

2 Sandosoft-SPG = 50gpl Ceraperm-MW = 30gpl Sandoperm-SE1 = 10gpl

S-SPG+C-MW+S-SE1 (E1)

3 Sandosoft-SPG = 50gpl Ceraperm-MW = 30gpl Ceraperm-TOWI =30gpl

S-SPG+C-MW+C-TOWI (E2)

4 Sandosoft-SPG = 50gpl Ceraperm-MW = 30gpl Sandoperm-RPU = 25gpl

S-SPG+C-MW+S-RPU (E3)

5 Sandosoft-SPG = 50gpl Ceraperm-MW = 30gpl Ceraperm-UP = 30gpl

S-SPG+C-MW+C-UP (E4)

6 Sandosoft-SPG = 50gpl Sandoperm-SE1 = 10gpl Ceraperm-UP = 30gpl

S-SPG+S-SE1+C-UP (E5)

7

Sandosoft-SPG = 50gpl Ceraperm-MW = 30gpl Sandoperm-SE1 = 10gpl Ceraperm-UP = 10gpl

S-SPG+C-MW+S-SE1+C-UP (E6)

3.4.2.5 Study on the effect of cellulase and protease enzyme treatment

followed by functional finishing treatment on wool/cotton union

fabric

In fifth chemical finishing study, the wool/cotton union of above

mentioned specifications was taken. It was treated with Bactosol CA

(Enzyme-1 gpl; pH 5.5 with acetic acid; 60 minutes; 55oC; 1:20 MLR;

93

Sandoclean PCJ-0.1gpl) and Savinase-16.0L Ex (Enzyme-2% (oww); pH 8.5

with sodium carbonate; 30 minutes; 50oC; 1:20 MLR; Sandoclean PCJ-

0.1gpl) separately, neutralized, washed and dried. The untreated and enzyme

treated union fabric were treated with selective five finishing combinations as

per recipe given in Table 3.8.

For Synthappret-BAP based finishing, the required amount of

Synthappret-BAP was taken along with S-RPU/ C-MW. It was mixed with

0.25 gpl Sandoclean-PCJ in a bath and stirred well. Then finally the dissolved

sodium bicarbonate solution was added gradually with constant stirring and

the pH was adjusted to 7.8±0.2. The union fabric was immersed in the

finishing solution at 25oC for 5 minutes and padded with 80±5 % expression

under 1.5 Kg/cm2 using a laboratory padder (RB Engineering Ltd., Gujarat,

India). After padding, the fabric was dried at 100oC in an oven and cured at

160oC for 5 minutes in high temperature steamer (RB Engineering Ltd.,

Gujarat, India), conditioned for 48 hours, washed with distilled water and

dried.

For β-cyclodextrin based finishing, the required amount of

β-cyclodextrin was taken and dissolved with gradual addition of 0.5gpl acetic

acid solution and 0.25gpl Sandoclean-PCJ solution in a high speed stirrer and

the pH was adjusted to < 5. After a clear solution was obtained, the other

chemicals such as Finish-VLF / Sanitized T-9919 were added one by one with

constant stirring and finally the dissolved MgCl2 solution was added. The pH

of finishing solution was adjusted to 5.0 with 0.25 gpl acetic acid solution.

The union fabric of 35cmx35cm dimension was taken and immersed in the

finishing solution at 25oC for 5 minutes and padded with 80±5 % expression,

dried at 100oC, cured at 150oC for 5 minutes, washed with distilled water and

dried.

94

Table 3.8 Recipe of chemical treatment for study-5

S. No Recipe Abbreviation 1 Unfinished Unfinished (F0)

2 Synthappret-BAP = 45 gpl NaHCO3 = 4.5 gpl

S-BAP (F1)

3 Synthappret-BAP = 30 gpl Sandoperm-RPU = 30 gpl NaHCO3 = 3 gpl

S-BAP+S-RPU (F2)

4 Synthappret-BAP = 30 gpl Ceraperm-MW = 60 gpl NaHCO3 = 3 gpl

S-BAP+C-MW (F3)

5

-cyclodextrin = 16gpl Finish-VLF = 60 gpl Ceraperm-MW = 30 gpl Ceraperm-UP = 20gpl Sandosoft-SPG = 30 gpl MgCl2 = 6 gpl

F-VLF+-CD (F4)

6

-cyclodextrin = 16gpl Sanitized T-9919 = 4 gpl Finish-VLF = 60 gpl Ceraperm-MW = 30 gpl Ceraperm-UP = 20gpl Sandosoft-SPG = 30 gpl MgCl2 = 6 gpl

F-VLF+-CD+S-9919 (F5)

The performance properties such as finish add-on, moisture regain,

wettability, wicking height, tear strength, bending length, flexural rigidity,

bending modulus, dry crease recovery angle, handle by subjective assessment,

primary and total hand value for winter suiting fabric by Kawabata hand

evaluation system for winter suiting fabric, area shrinkage and antimicrobial

activity of finished and unfinished wool/cotton union fabric with and without

prior enzyme treatment were evaluated.

95

3.4.3 Evaluation of performance properties

The finished and unfinished fabrics with and without prior enzyme

treatment(s) were conditioned at 20±2oC, 65±2 % RH, 4 hours before the

evaluation of the performance properties.

3.4.3.1 Finish add-on

The sample was dried in an oven at 105oC until a constant weight

was reached and oven-dried weights determined before and after finishing

treatments and add-on was calculated using the following Equation (3.1).

Finish add-on (%) = [(W2-W1)/W1] 100 (3.1)

where W1 - Weight before finishing (g)

W2 - Weight after finishing (g)

3.4.3.2 Moisture regain

The sample was dried in the oven at 105oC for one hour and

weighed the oven-dry sample first and was placed in a desiccator, which kept

under standard conditions (20±2oC, 65±2 %RH). Weight gain was measured

after a definite time and moisture regain was calculated as per standard

(ASTM 2001b).

3.4.3.3 Wettability

The wettability was measured based on the BS 4554:1970 method

in which a drop of 0.1 ml of de-ionized water was placed on the surface of the

96

sample. The time required (in seconds) for the droplet to penetrate completely

into the fabric was measured by means of a stopwatch.

3.4.3.4 Wickability

A sample strip measuring 10cm 2.5cm (both in warp and weft

direction) was taken and the lower edge of the strip was suspended vertically

with its lower end (6mm) dipping into a beaker containing distilled water. The

height of the distilled water reached after five minutes was noted with respect

to warp and weft directions were measured (Harnett et al 1984).

3.4.3.5 K/S value and CIE whiteness index

A Minolta-3200:D-Spectrophotometer (illuminant D65/10o

observer) was used to determine the K/S and CIE whiteness index value of

the samples. Each fabric was folded twice and the K/S or whiteness was

measured four times at different portions of the fabric surface and the average

value was regarded (AATCC 2003e).

3.4.3.6 Tearing strength

The tearing strength was measured by single rip ballistic test on

Elmendorf tearing tester (Paramount Instruments Pvt. Ltd). The strength was

calculated by the following Equation (3.2) both in warp and weft direction.

Ft = (Rs Cs) / 100 (3.2)

where Rs - Scale reading in gf

Cs - Full scale capacity in gf (or) augmenting weight in gf

97

Ft - Tearing strength in gf

The retention of tearing strength by a treatment was calculated from

Equation (3.3), by measuring the tearing strength of the sample before (Ft1)

and after treatment (Ft2).

Retention of tearing strength (%) = [(Ft1- Ft2)/ Ft1] 100 (3.3)

3.4.3.7 Shrinkage

Relaxation shrinkage, consolidation shrinkage and felting shrinkage

and total shrinkage of the unfinished and finished fabric samples were

determined as the dimensional change of sample (20cm 20cm) as per

method described in standard (AATCC 2003h).

3.4.3.8 Drape coefficient

The sample in circular specimen (30cm diameter) was held

concentrically between two small horizontal discs and was allowed to drape

into folds under its own weight. A light was shone from underneath the

specimen and the shadow that the fabric casts was traced on to an annular

piece of paper, the same size as the unsupported part of the fabric specimen.

To measure the areas involved, the whole paper ring was weighed and then

the shadow part of the ring was cut away and weighed. The paper was

assumed to have uniform mass per unit area so that the measured mass was

proportional to the area.

The fabric was tested in both ways up so that a total of six

measurements were made on the same specimen. The drape coefficient as

98

percentage (DC) of the samples was calculated using the following formula

was measure as per standard BS 5058:1973 using the following

Equation (3.4).

Drape coefficient (%) = Mass of shaded area

100 (3.4) Total mass of paper ring

3.4.3.9 Subjective assessment

Fabric handle was evaluated by subjective assessment only. The

handle characteristics were expressed in terms of “smoothness”, “stiffness”,

“softness” and “roughness”. A panel of 16 judges was asked to rate each

fabric on a scale of 1 (lowest) to 4 (highest). The overall rating for each

characteristic was then calculated by the following Equation (3.5) (Zuchariah

et al 1997).

4

i j

i 1

S nPercentage Handle 100

4n

(3.5)

where n - Total number of judges

Si - Judge’s rating

4 - Highest rating

nj - Number of judges giving rating Si

Statistical analysis were done to establish the variance between the

samples compared with the variance within the samples. The statistical

significance level for the F-value was p<0.001 for all parameters such as

softness, stiffness, roughness and smoothness.

99

3.4.3.10 Bending stiffness

Shirley stiffness tester was used for the measurement of bending

length. The test specimens were each 25 mm wide and 152 mm long; three

were cut parallel to the warp and three parallel to weft so that no two warp

specimen contain the same warp threads and no two weft specimens contain

the same weft threads. The strip of the fabric was mounted on a horizontal

platform in which a way that it overhangs and bends downwards to 41.5o and

bended length (L) was measured from Equation 3.6. Four readings were taken

from each specimen one face up and face down on the first end and then the

same for the second end. The mean bended length for the warp and weft

direction was calculated. From the bended length, the bending length (ASTM

2001c), flexural rigidity and bending modulus (BSI 1990b) were calculated

using the following Equations (3.6), (3.7) and (3.8) respectively as per

standard.

Bending Length (C) = L [cos θ /8tan θ] 1/3 cm (3.6)

where θ - 41.5o

L - Bended length (cm)

Flexural Rigidity (G) = M C3 9.807 10-6 µNm (3.7)

where M - weight of sample in g/m2

C - Bending length in mm

Bending Modulus (q) = [(12 G 103) / (T3)] Nm-2 (3.8)

where G - Flexural Rigidity in µNm

T - Thickness of sample in mm

100

3.4.3.11 Dry crease recovery angle

Dry crease recovery angle was carried by the Shirley crease

recovery tester. A sample of the size 5cm 2.5cm was cut from the both warp

and weft directions. The sample was carefully folded into half, kept between

two glass plates and a 907 g weight was placed on the top. After one minute

the load was removed and the sample was placed on the fabric clamp in the

tester and allowed to recover from creasing. Finally the fabric dry crease

recovery angle was read and recorded (AATCC 2003d).

3.4.3.12 Objective assessment by KES-F

The primary hand value and total hand value (for winter suiting

fabric) of finished and unfinished fabrics with and without prior enzyme

treatment were objectively assessed by Kawabata evaluation system for fabric

(KES-F). It consists of four instruments and they used to evaluate the tensile,

shear, bending, compression and surface properties of fabrics in sixteen

parameters as shown in Table 3.9.

Sample of 20 cm 20 cm dimension in triplicates was taken. The KES-

FB1 instrument was used to measure extensibility at 500 gf/cm (EMT), tensile

energy in deformation (J/m2) (WT), resilience to deformation (RT)-the ratio between

recovering energy and tensile energy and linearity in extension (LT). The KES-FB1

instrument was also used to measure shear stiffness (N/m*degree) (G), hysteresis of

shear stiffness at 0.5o deformation (N/m) (2HG) and hysteresis of shear stiffness at

5o deformation (N/m) (2HG5).

101

Table 3.9 Mechanical and Surface properties from KES-F

Parameters Description Unit

Tensile a

1.LT Linearity of Load/extension curve None

2.WT Tensile energy N/m

3.RT Tensile resilience %

Bending a

4.B Bending rigidity 10-4Nm

5.2HB Hysteresis of bending moment 10-2N

Shearing a

6.G Shear stiffness N/m Deg.

7.2HG Hysteresis of shear force at 0.5o of shear angle N/m

8.2HG5 Hysteresis of shear force at 5o of shear angle N/m

Compression

9.LC Linearity of compression/thickness curve None

10.WC Compressional energy N/m

11.RC Compressional resilience %

Surface a

12.MIU Coefficient of friction None

13.MMD Mean deviation of friction None

14.SMD Geometrical roughness µm

Construction

15.T Fabric thickness mm

16.W Fabric weight/unit area 10 g/m2

a - Average of the values in warp and weft directions is applied

102

The KES-FB2 instrument was used to determine bending rigidity

per unit length (N*m2/m) (B) and hysteresis of bending moment per unit

length (mN*m/m) (2HB). The KES-FB3 instrument was used to determine

thickness T of the fabric subjected to a pressure of 0.5 cN/cm2, deformation

energy (J/m2) (WC) and resilience to compression (RC). This last property

was the ratio between elastic recovery energy and deformation energy. The

ratio between deformation energy (WC) and the deformation energy of a

perfectly elastic body subjected to the same conditions of compressions (LC).

The KES-FB4 instrument was used to determine the surface

characteristics such as mean coefficient of friction (MIU), standard deviation

of MIU (MMD) and the geometrical roughness (SMD) (m).

Except compression property, the other mechanical properties

were evaluated both in warp and weft direction and the final reading would be

the average of warp and weft direction.

The above sixteen parameters obtained from KES-F system

combined with the calculation model developed by Prof. Niwa and Kawabata

to obtain an objective evaluation of the hand of the fabrics as mentioned in

Equation (3.9) (Kawabata 1980, Kawabata and Niwa 1989).

Yk = Co + Cki Xi (3.9)

where Yk = kth hand value such that, k=1 is stiffness (Koshi), k=2

is smoothness (Numerii) and k=3 is fullness

(Fukurami) for winter/autumn suiting fabrics

Co and Ci = Constants calculated by Kawabata for each primary

hand values

103

Xi = deviation of the value from the mean parameter xi

measured from the mean of ni of the universe, express

in the form of a standard deviation i

xi = (Xi – Mi)/ i

Having calculated the primary hand values in terms of smoothness,

stiffness and fullness for winter suiting fabrics, Kawabata et al (1989) then

worked out the equation of total hand value (THV) which units all the

primary hand value into a single value as mentioned in Equation (3.10).

THV = Co + Zk (3.10)

2

k1 k k1 k2 k k2k

k1 k 2

C (Y M ) C (Y M )Z

where Zk - Contribution of the kth primary hand value to total

hand value

Mk1 and k1 - Population means and standard deviation of Yk

M k2 and k2 - Population means and standard deviation of Yk2

Ck1 and Ck2 - Constant coefficients

Co - Constants calculated by Kawabata for each Total

hand values

The total hand value (THV) calculated from primary hand values of

finished and unfinished fabrics with and without prior enzyme(s) treatment is

obtained from equation 3.10 in terms of winter suiting fabric in this work .

104

3.4.3.13 Assessment of antimicrobial activity

To analyze the antimicrobial activity of β-cyclodextrin / Sanitized

T-9919 finished union fabric, the fabrics were subjected to parallel streak

method (AATCC 2003g). The organisms used in both the tests were

Staphylococcus aureus (gram-positive organism) and Escherichia coli (gram-

negative organism). The evaluation of parallel streak method was made on the

basis of a clear zone of interrupted growth underneath and along the sides of

the test sample, which was placed in intimate contact with the bacteria agar

that has been previously streaked with inoculums of test organism. The

average width of zone of inhibition along a streak on either side of the test

specimen was calculated using the following Equation (3.11).

W = (T-D)/2 (3.11)

where W - width of the clear zone of inhibition in mm

T - diameter of test specimen and clear zone in mm and

D - diameter of test specimen in mm.