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AASCIT Journal of Materials

2015; 1(4): 111-122 Published online November 10 2015 (http://www.aascit.org/journal/materials)

Keywords Acrylamide, Chemical Softening, Citric Acid, Crease Resistant Finish, Ester-Crosslinking, Grafting, Jute- Cotton Union Fabric, Photo-Functionalisation

Received: August 31, 2015 Revised: September 15, 2015 Accepted: September 17, 2015

Effects of Selective Chemical Softening and Different Modes of Citric Acid Treatment on Properties of Jute-Cotton Union Furnishing Fabric

Ashis Kumar Samanta1, Sunanda Mitra Roy

2, Deepali Singhee

3,

Pubalina Samanta3

1Department of Jute and Fibre Technology, Institute of Jute Technology, University of Calcutta, Kolkata, West Bengal, India

2Department of Bachelor of Fashion and Apparel Design, Rani Birla Girls’ College, Affiliated to University of Calcutta, Kolkata, West Bengal, India

3J. D. Birla Institute, Affiliated to Jadavpur University, Kolkata, West Bengal, India

Email address [email protected] (A. K. Samanta), [email protected] (S. M. Roy), [email protected] (D. Singhee), [email protected] (P. Samanta)

Citation Ashis Kumar Samanta, Sunanda Mitra Roy, Deepali Singhee, Pubalina Samanta. Effects of Selective Chemical Softening and Different Modes of Citric Acid Treatment on Properties of Jute-Cotton Union Furnishing Fabric. AASCIT Journal of Materials. Vol. 1, No. 4, 2015, pp. 111-122.

Abstract Bleached jute-cotton (75:25) union fabric have been subjected to treatment with selective chemical softeners such as catasoftener, aminosilicone, poly-oxo-ethylene and their mixtures and the changes in textile related properties of the same have been evaluated and compared. Catasoftener gives appreciable softening action but causes some degree of yellowing. Aminosilicone does not produce appreciable softening action and poly-oxo-ethylene render the fabric a moderate degree of softening action. However, 4% (owf) overall dose of 25:75 mixture of catasoftener and poly-oxo –ethylene emulsion softener gives a synergetic softening action rendering the fabric a much better balance of its textile related properties. Simple citric acid leaching makes jute-cotton union fabric brighter and resilient to some extent. Citric acid treatment in presence of equal amount of Na3PO4 by pad-dry (90°C for 10 min) and cure (140°C for 5min) technique show reasonable improvement in the fabric crease resistant property associated with some loss in tensile strength and increase in fabric stiffness. Among selective single and mixture of chemical softeners applied during citric acid cross-linking, addition of 4% overall dose of 25:75 mixture of aminosilicone and poly-oxo-ethylene render the fabric higher crease recovery with measurable reduction in stiffness having an overall desirable balance in other textile related properties. Also, photo-functional character of citric acid has been utilized by exposure of citric acid treated bleached jute-cotton union fabric to UV-light for grafting of acrylamide on the same rendering the modified fabric desirable soft hydrophilic finish with a better balance in its textile related properties.

1. Introduction

Natural (raw) or conventional H2O2 bleached jute-cotton union fabrics being commercially produced either in handloom sector or in jute-mill sector are gaining popularity in its use as furnishing fabric or other home textiles for its heaviness and unique surface texture. However, its market demand and production volume are still

112 Ashis Kumar Samanta et al.: Effects of Selective Chemical Softening and Different Modes of Citric Acid Treatment on Properties of Jute-Cotton Union Furnishing Fabric

limited due to restricted market growth owing to some of its major and minor drawbacks [1, 2]such as high stiffness (poor drape), high surface roughness and hairs of jute, high fibre shedding from jute component in jute direction, unequal wash shrinkage and unequal dye uptake in two directions, poor crease resistance and poor abrasion resistance etc. citric acid cross linking [3] route may be utilized but this increases the stiffness of the fabric. Hence, suitable chemical softening is highly essential identifying suitable softener for such jute based fabrics. It is expected that the use of jute-cotton union furnishing fabric as home textiles and its demand and acceptability in both domestic and export market of jute products may further be increased, if some of the above said major/ minor drawbacks may be eliminated or partially suppressed/ removed by selective treatments with appropriate finishing chemicals or softeners and/ or other functional property modifiers as per end use requirement. There are many available reports on such work [3-11] for 100% jute fibre/ fabrics but a very few of them are only for jute-cotton union fabric. A few such mention worthy work on jute fabric include studies on crosslinking using citric acid treatment [3], photo-functionalisation of oxalic acid [4] for grafting and softening with mixed enzymes [5, 6] and chemical softeners [6] like catasofteners and aminosilicone. Recently, treatment of jute fibres with mixed enzymes and aminosilicone [7] has been reported from this laboratory to improve spinnability and yarn quality for manufacture of jute yarns. A comprehensive report on diversification of jute decorative fabrics by different chemical finishing treatments are also available in literature [8]. Eco-friendly and energy efficient room temperature bleaching of jute and jute-cotton union fabrics have also been reported [9] recently. Improvement of crease resistancy of jute fabric by cross-linking with citric acid has been reported [3] earlier from this laboratory (but not on jute-cotton union fabric) showing the resultant jute fabric to be somewhat stiffer. Hence, citric acid cross-linked jute or jute-cotton union fabrics need to be softened by suitable chemical softeners either by post treatment or simultaneous treatment during cross-linking, identifying suitable chemical softeners for it. Crease- resistant finishing of jute and jute-cotton union fabrics using DMDHEU and acrylamide formaldehyde (AMF) resin with or without different additives and softeners has also been reported [1, 2, 10, 11] earlier from this laboratory. But considering the today’s need of eco-friendly non-formaldehyde crease resistant finish, it is thought appropriate to study citric acid cross-linking on jute-cotton union fabric with either pre-softening or simultaneous softening with appropriate chemical softeners after identifying suitable softeners for such fabric. Moreover, it is also thought to utilize the photo-functional character of citric acid, as chemical initiator, for chemical modification of jute-cotton union fabric by grafting of acrylamide for imparting a hydrophilic polymeric finish on it to obtain a desirable improvement in some of its textile related properties.

With the above thought in mind, in this present work,

conventionally H2O2 bleached jute-cotton union fabric have been subjected to (a) treatment with selective chemical softeners such as catasoftener, aminosilicone, poly-oxo-ethylene emulsion, and their mixtures in different ratios, to identify the most suitable softener or softener combinations for the said jute-cotton union fabric and (b) citric acid treatment in three different modes with different objectives i. e. (i) simple citric acid treatment for surface cleaning and brightening of the fabric, (ii) citric acid pretreatment followed by UV-light exposure for generation of free radicals by photo-functionalisation followed by subsequent grafting with acrylamide (a vinyl monomer) on the said fabric to improve some of its textile related properties and dyeability and (iii) cross-linking of citric acid on jute-cotton union fabric with and without single and mixtures of suitable chemical softeners for obtaining a desired level of non-formaldehyde crease-resistant finish. Thus, present study on the effects of treatment with different chemical softeners and different modes of treatment with citric acid on textile related properties of jute-cotton union fabric has high importance considering this modifications/ treatments as an endeavour to promote its more and more market acceptability to the consumers.

2. Materials and Methods

2.1. Materials

2.1.1. Jute-Cotton Union Fabric

2% H2O2 bleached, plain-weave raw jute-cotton union fabric (75: 25) having fabric weight 260g/m2, 80ends / dm, 70picks / dm, 42 tex warp (cotton) yarn, 185 tex weft (jute) yarn, and 0. 70mm thickness was used in the present work.

2.1.2. Chemicals and Dyes

Laboratory Reagent (LR) grade citric acid (2-hydroxy-1, 2, 3-propane tri-carboxylic acid), common salt (NaCl), glauber’s salt (Na2SO4, 10 H2O), sodium carbonate (Na2CO3), all supplied by M/s E. Merck India was used. Commercially available textile finish aminosilicone emulsion i. e. amino-modified poly-siloxane emulsion (Silicorel-TTSC with 25% solid content along with 2% zinc-acetate in built catalyst) obtained from M/s Reliance silicones, Mumbai and catasoftener (30% solid content) and poly-oxo-ethylene emulsion softener (20% solid content) obtained from a local supplier were used. An acid dye, Polar Red - 3BN (C. I. Acid Red 131) and a hot brand reactive dye Procion Green HE-4BD (C.I Reactive Green 19.)and a basic dye Auramine-O (CI BasicYellow2) supplied by Modi Dye Chem, Kolkata, were also used in the present work.

2.2. Methods

2.2.1. Conventional Desizing, Scouring and

H2O2 Bleaching

Desizing of jute-cotton union fabric [2, 9] was done employing 20-30 L/L of aqueous solution of 3. 6% HCl (0.

AASCIT Journal of Materials 2015; 1(4): 111-122 113

5% owf) at 60°C for 1h using laboratory jigger keeping MLR 1: 5 (w/w) followed by washing and drying. Desized jute-cotton union fabric [2, 9] was scoured in lab-jigger using 4g/l of soda, 1g/l of non-ionic detergent, using MLR 1: 5 at pH- 8-9, for 1h at 100°C followed by repeated washing and drying in air. Raw (untreated) or suitably desized and scoured jute-cotton union fabric samples were subjected to conventional H2O2 bleaching [2, 10] employing 2% (owf) H2O2, 6% (owf) sodium meta-silicate, 0.7% (owf) NaOH, 0.05% (owf) EDTA, 0.3% (owf) non-ionic wetting agent (lissapol-D) at 85°C for 2 h at pH 10.8-11. 0. In each case, the pH of the bleach bath was maintained by adding small amounts of 1% NaOH drop wise. After bleaching, each fabric sample was washed thoroughly under running water, followed by neutralization with 1.5% acetic acid solution for 15 min before further washing with hot and normal water. Finally, the washed fabric samples were dried in air.

2.2.2. Different Modes of Treatment with

Citric Acid

(i) Simple Citric Acid Treatment

Desized, scoured and 2% H2O2 bleached jute-cotton union fabric was subjected to simple treatment with 2% citric acid solution for 30min at room temperature (30°C). Citric acid treated fabric sample was then neutralized for 15 min with 1% sodium hydroxide solution till it is free from alkali and finally washed with hot water followed by washing with normal running water before squeezing and drying in air.

(ii) Citric Acid Initiated

Photo-Functionalisation and Subsequent

Grafting with Acrylamide

In a separate set of experiment, specific dose of citric acid [using 1% aqueous solution of citric acid with MLR-1: 10 i. e. 10% (owf) application on fabric] treated bleached jute-cotton union fabric was also subjected to photo exposure to UV-light (using Philips-500 watt MBTF lamp) for 15-30 min followed by subsequent treatment with 8% (owf) aqueous solution of acrylamide (a vinyl monomer) by pad-cure (at 70°C for 30min) technique. The suitability of low temperature (70°C) conditions of acrylamide grafting with K2S2O8 initiation was studied earlier from this laboratory. After this treatment the fabric was washed in hot water followed by washing with normal running water, and then squeezed and finally dried in air.

(iii) Ester Cross-Linking Using Citric Acid

In another set of experiment, specific dose of citric acid treatment was carried out on desized, scoured and H2O2 bleached jute-cotton union fabric in presence of equal amount of Na3PO4 (as catalyst) at 30°C for 30min followed by squeezing and drying the same at 90°C for 10min followed by subsequent curing at 140°C for 5min for effecting ester cross-link formation between jute cellulose chains and citric acid3. After this treatment, the treated fabric sample was repeatedly washed in hot water followed by

washing with normal running water and then squeezed and finally dried in air.

2.2.3. Application of Catasoftener,

Poly-Oxo-Ethylene and Aminosilicone

Emulsion Softeners

4% (owf) catasoftener (CS) and 4% poly-oxo-ethylene (POE) emulsion softener were individually applied separately on desized, scoured and H2O2 bleached jute-cotton union fabric by pad (2 dip-2 nip, 100% wet pick-up) – dry (90-100°C for 10 min) technique using lab-2-bowl padding mangle and lab hot air stenter. 4% (owf) overall dosages of the mixture of catasoftener (CS) and poly-oxo-ethylene (POE) emulsion softener in varying ratios (100: 0, 75: 25, 50: 50, 25: 75 and 0: 100) was also applied on desized, scoured and H2O2 bleached jute-cotton union fabric by the above said same pad-dry technique and conditions [6].

4% (owf) aminosilicone (AS) softener or 4% overall dosages of mixture of catasoftener and amino-silicone emulsion of varying ratios (100: 0, 75: 25, 50: 50, 25: 75, and 0: 100) was applied on desized, scoured and H2O2 bleached jute-cotton union fabric by the above said same pad-dry technique and conditions followed by additional curing at 140°C for 5min for presence of aminosilicone, which needs to be cured at high temperature for reaction with jute [7].

4% (owf) dosages of catasoftener or aminosilicone or poly-oxo-ethylene softener individually and 4% overall dosages of either the mixture of aminosilicone and catasoftener in specific proportions (AS: CS = 25: 75) or mixtures of catasoftener and poly-oxo-ethylene in specific proportion (CS: POE = 25: 75) or mixtures of aminosilicone and poly-oxo-ethylene softener in specific proportion (AS: POE = 25: 75) were also applied separately during citric acid cross-linking treatment on jute-cotton union fabric by adding specific dosages of single or mixtures of the said softeners along with citric acid and Na3PO4 solution by the above said same pad-dry technique and conditions followed by additional curing at 140°C for 5 min. In each case, after the curing, all the finished fabric samples were repeatedly washed with hot water and normal running water and finally dried in air.

2.2.4. Dyeing of Jute-Cotton Union Fabric

with Acid Dye

Control bleached and differently treated jute-cotton union fabric samples were separately dyed with an acid dye Polar Red-3BN (CI Acid Red-131). For 10g of fabric sample, 0.10g of acid dye (for 1% shade depth) was taken in 200 ml (using material to liquor ratio i. e. MLR 1:20) aqueous solution of 5% Na2SO4 and a requisite volume of 2% HCOOH solution was added to adjust pH to 4-4.5 and the dyeing was carried out following a standard method [6,11] using EEC- a laboratory beaker dyeing machine for 1 h at 90±5°C.

2.2.5. Dyeing of Jute-Cotton Fabric with

Reactive Dye

Control bleached and differently treated jute-cotton union


fabric samples were separately dyed at 1% shade depth using 0.1% aqueous solution of selected reactive dye (Procion Green HE 4 BD), using a lab beaker dyeing unit maintaining a dyeing temperature of 80 ± 5°C and material to liquor ratio of 1:20 and also using appropriate dose level of sodium chloride (70 g/l) and sodium carbonate (10 g/l) following a standard method [6, 11, 12] using EEC- Lab beaker dyeing machine for 1½h.

2.2.6. Determination of Weight Loss or Gain

and Moisture Regain

Loss or gain in weight after selective chemical treatment/modification of jute-cotton union fabric was determined by gravimetric principle following oven dry weight method [13, 14], taking bone dry weights of the samples before and after the treatments and expressing the results as a percentage of the initial bone dry weight of the material taken. The moisture regain of selected bone dried jute-cotton fabric samples were determined according to ASTM–D2654–76 method [15] by taking the weights before and after oven drying of the selective samples, after conditioning all the sample in standard atmospheric conditions (65±2% relative humidity and 27±2°C temperature) in a NaNO3 desicator for 48h.

2.2.7. Determination of Fabric Shrinkage

During Selective Treatments

Linear warp-way and weft-way shrinkage of jute-cotton union fabric samples were determined according to IS: 2977-1964 method [14] using the following relationship:

Shrinkage% = � − � � × 100

Where, Lo is the initial length of datum line before washing and L1 is the final length of datum line after washing.

2.2.8. Evaluation of Tensile Properties

Warp-way and weft –way tenacity, initial modulus (modulus of 0.5% extension) and the breaking extension values of the control bleached and selectively treated jute-cotton union fabric samples were determined by the raveled strip method as per IS: 1969: 1968 procedure [14] with sample size 50×20mm under the jaws after raveling, using an

Instron (model-1445) CRT-Universal tensile tester with traverse speed of 100mm/min and pretension of 0.5N.

2.2.9. Determination of Fabric Stiffness

(Bending Length)

The bending length of control bleached and selectively treated jute-cotton union fabrics were measured as per IS: 6490-1971 (cantilever test) method [14] using Sasmira Stiffness tester with a specimen size of 200 mm X 25 mm.

2.2.10. Measurement of Total Crease

Recovery Angle

The total (warp-way plus weft-way) crease recovery angle (CRA) of control bleached and selectively treated jute-cotton union fabric samples was measured as per IS: 4681-1968 method [14] with 5 min loading (with 1000g standard load) and 5 min recovery time using Sasmira crease recovery tester.

2.2.11. Measurement of Surface Appearance

and Colour Strength

K/S value (a measure of surface colour strength) of the control bleached and selectively treated and dyed jute-cotton union fabric samples were determined using following Kubelka Munk relationship [16]:

KS��

= Co − efficientofabsorptionCo − efficientofscattering = (1 − Rλ��)2

2Rλ��= αC&

Where K= the co-efficient of absorption, S = the co-efficient of scattering, Cd = the concentration of dye, Rλmax = the surface reflectance value at maximum absorbance wave length (λmax), and α = a constant.

Whiteness index was determined as per Hunter Lab-Scale formula [17], the yellowness index was determined as per ASTM-E- 313 -1973 formula [18] and brightness index was determined as per ISO-2470- (1977) formula [19] using computer aided Macbeth 2020 Plus reflectance spectrophotometer and associated software with the help of following relationships:

Whiteness Index (Hunter Lab-Scale) =L− 3b = 10√Y− [21 (Y−Z %)] / √Y

YellownessIndex -ASTM − E31319735 = 100 -1 − B

G5 = 100 ×(1 − 0. 847ZY )

BrightnessIndex(ISO − 2470 − 1977) = Reflectancevalueofthesubstrateat457nmReflectancevalueofthestandardwhitediffuser/whitetileat457nm× 100

where, X, Y and Z are the tristimulus values of the sample, L is the lightness/darkness indicator in CIE Lab-Scale [L* or simply L = 16 (Y/Yo)

1/3- 16 as per CIE Lab-1976 formula [16]], b is the blueness/yellowness indicator in the CIE Lab-Scale [16] {b* or simply b = 200 [(Y/Yo)

1/3 – (Z/Zo)1/3]}, B =

Z/1. 181 = 0. 847 Z, G = Y= L2/100 and Xo, Yo and Zo are the CIE-tristimulus values [16] for D65 standard illuminant and 10° standard observer.

2.2.12. Study of Surface Morphology by

Scanning Electron Microscopy (SEM)

The surface morphology of control bleached and differently treated jute and cotton fibre samples taken out from respective jute yarns and cotton yarns of the control and correspondingly treated jute-cotton union fabrics was examined using JEOL Scanning Electron Microscope (Model: JSM-5200) at an operating voltage of 20 κγ, using a


magnification of 1000X. The fibre samples for the SEM study were prepared with Gold-Palladium alloy coating

following standard procedure [20].

3. Results and Discussion

3.1. Effect of Application of Single and Mixture of Chemical Softeners

Table 1. Effects of single acid and alkali pre-treatments on important textile related properties of jute-cotton (J/C) union fabric.

Treatments

Weight Loss

(-) or gain

(+)%

Treatment shrinkage% Initial ModulusN/mm TenacitycN/tex Breaking extension%

Warp

(Cotton)

Weft

(Jute)

Warp

(Cotton)

Weft

(Jute)

Warp

(Cotton)

Weft

(Jute)

Warp

(Cotton) Weft (Jute)

1) Nil (Raw control J/ C fabric)

- - - 30. 0 98. 6 5. 04 8. 42 12. 24 4. 02

2) Treatment with dilute aqueous solution of different acids at 30° C for 30 min using MLR 1: 10.

1% HCl (-) 2. 10 7. 2 3. 6 26. 4 81. 4 4. 84 7. 94 11. 20 3. 58 1% Acetic acid (-) 1. 52 9. 5 2. 6 27. 6 82. 6 4. 78 8. 14 11. 62 3. 90

1% formic acid (-) 2. 25 10. 4 2. 9 25. 6 83. 4 4. 68 7. 86 11. 62 3. 72

1% Citric acid (+)0. 48 10. 5 3. 7 29. 2 90. 2 4. 52 7. 74 10. 64 3. 54 3) Treatment with aqueous solution of NaOH at 30° C for 30 min using MLR 1: 20.

1% NaOH (-) 3. 02 9. 4 0. 85 30. 5 80. 8 4. 82 7. 46 13. 64 6. 08 5% NaOH (-) 6. 14 11. 2 2. 9 32. 1 70. 8 4. 60 6. 90 15. 04 9. 26

10% NaOH (-) 8. 64 13. 2 7. 54 35. 0 65. 8 4. 34 5. 64 17. 24 15. 04

18% NaOH (-)12. 46 15. 6 14. 68 40. 04 60. 4 4. 84 5. 04 19. 27 18. 80

Table 1. Continue.

Treatments

Total CRAa

(Warp+Weft)

Degree

Bending Length

(cm)

Surface appearance

Properties (K/SValue at λmax)

Warp

(Cotton)

Weft

(Jute) WIb YIc BId

Before

dyeing

After dyeing with

Acid dye Reactive dye Basic dye

1) Nil (Raw control J/ C fabric)

145 1. 7 4. 0 52. 1 34. 0 25. 4 1. 20 13. 26 12. 84 10. 84

2) Treatment with dilute aqueous solution of different acids at 30° C for 30 min using MLR 1: 10.

1% HCl 122 1. 3 3. 3 51. 8 36. 4 29. 6 1. 30 - - 10. 96

1% Acetic acid 124 1. 4 3. 4 50. 4 37. 2 26. 9 1. 36 - - 10. 89 1% formic acid 124 1. 3 3. 4 50. 9 37. 5 26. 2 1. 34 - - 11. 04

1% Citric acid 154 1. 4 3. 6 52. 0 36. 1 27. 4 1. 38 - - 11. 88 3) Treatment with aqueous solution of NaOH at 30° C for 30 min using MLR 1: 20.

1% NaOH 140 1. 6 3. 8 49. 4 37. 6 23. 2 1. 30 13. 42 12. 96 -

5% NaOH 136 1. 5 3. 6 45. 1 42. 4 21. 6 1. 46 13. 98 13. 24 - 10% NaOH 130 1. 4 3. 4 38. 2 45. 5 18. 6 1. 82 14. 64 13. 62 -

18% NaOH 125 1. 2 2. 8 34. 4 49. 4 16. 4 1. 98 15. 08 14. 14 -

a Crease recovery angle, bWI – whiteness index, cYI-yellowness index, dBI-brightness index.

Table 2. Effects of different dosages of citric acid pretreatment on important textile related properties of jute-cotton (J/C) union fabric.

Treatments Weight Loss (-)

or gain (+)

Treatment shrinkage% Initial Modulus N/mm Tenacity cN/tex

Warp (Cotton) Weft

(Jute) Warp (Cotton)

Weft

(Jute)

Warp

(Cotton)

Weft

(Jute)

1) Nil (Raw control J/C fabric) - - - 30. 0 98. 6 5. 04 8. 42 4) Treatment with dilute aqueous solution of Citric acid using varying concentrations of citric acid and varying treatment time as follows: 0. 5% Citric acid treatment at 30°C for 30 min.

+ 0. 24 10. 2 3. 4 29. 9 94. 2 4. 81 7. 98

5) Treatment with 1% Citric acid solution at 30°C for varying treatment period as follows: - 15 min + 0. 32 10. 3 3. 6 29. 6 92. 4 4. 74 7. 90 - 30 min + 0. 48 10. 5 3. 7 29. 2 90. 2 4. 52 7. 74 - 60 min + 0. 62 10. 8 3. 8 28. 6 86. 4 4. 44 7. 62 - 120 min + 0. 74 11. 2 4. 0 26. 9 84. 0 4. 28 7. 64 6a) 1. 5% Citric acid treatment at 30°C for 30 min.

+ 0. 54 11. 0 4. 1 27. 2 80. 2 4. 26 7. 60

6b) 2% Citric acid treatment at 30°C for 30 min.

+ 0. 82 11. 4 4. 2 26.. 8 79. 4 4. 20 7. 12


Table 2. Continue.

Treatments

Breaking

extension % Total CRAa

(Warp+ weft)

Degree

Bending Lengthcm Surface appearance

Properties K/SValue at λmax

Warp

(Cotton)

Weft

(Jute)

Warp

(Cotton)

Weft

(Jute) WIb YIc BId

Before

dyeing

After

dyeingf

1) Nil (Raw control J/C fabric)

12. 24 4. 02 145 1. 7 4. 0 52. 1 34. 0 25. 4 1. 20 10. 84

4) Treatment with dilute aqueous solution of Citric acid using varying concentrations of citric acid and varying treatment time as follows:

0. 5% Citric acid treatment 30°C for 30 min.

11. 12 3. 84 148 1. 5 3. 7 50. 2 37. 3 27. 1 1. 26 11. 46

5) Treatment with 1% Citric acid solution at 30°C for varying treatment period as follows:

- 15 min 11. 02 3. 68 152 1. 4 3. 6 51. 9 36. 3 27. 3 1. 32 11. 65

- 30 min 10. 84 3. 54 154 1. 4 3. 5 52. 0 36. 1 27. 4 1. 36 11. 88

- 60 min 10. 62 3. 24 158 1. 3 3. 4 52. 4 37. 8 27. 7 1. 40 11. 94

- 120 min 10. 49 3. 06 164 1. 2 3. 3 52. 6 37. 6 27. 8 1. 42 12. 28

6a) 1. 5% Citric acid treatment 30°C for 30 min.

10. 48 3. 32 156 1. 3 3. 3 51. 4 37. 4 27. 9 1. 44 12. 64

6b) 2% Citric acid treatment 30°C for 30 min.

10. 34 3. 14 160 1. 2 3. 2 50. 4 37. 6 28. 0 1. 46 13. 18

a Crease recovery angle, bWI – whiteness index, cYI-yellowness index, dBI-brightness index, e using MLR 1: 10, f After dyeing with 1% basic dye (Auramine – O, C. I. Basic yellow 2).

Table 3. Effects of Citric acid initiated grafting of acrylamide and acid catalysed cross linking on textile related properties of desized, scoured and bleached

jute-cotton (J/C) union fabric.

Treatments

Weight

Loss

(-) or gain

(+)

Initial Modulus

N/mm

Tenacity

cN/tex Elongation at break %

Warp

(Cotton)

Weft

(Jute)

Warp

(Cotton)

Weft

(Jute)

Warp

(Cotton)

Weft

(Jute)

1. Nil (Control bleached J/C union fabric). - 28.4 48.4 4.77 7.27 13.5 4.7

7)1% Citric acid treatment at 30°C for 30 min (MLR – 1:10) on bleached jute-cotton union fabric.

(+) 0.52 27.6 40.0 4.25 6.59 12.1 4.2

8) Control bleached J/C union fabric treated with 1% citric acid solution at 30°C for 30 min (MLR – 1:10) in exhaust process before further subjected to UV light exposure for 30 min and subsequently padded with 8% (owf) acrylamide followed by curing at 70°C for 30min.

(+) 3.08 31.6 50.2 5.26 8.10 14.0 4.8

9) Control bleached J/C union fabric padded with 10% (owf) citric acid at 30°C for 30 min (MLR – 1:10) followed by UV light exposure for 30 min and subsequently padded with 8% (owf) acrylamide followed by curing at 70°C for 30min.

(+) 3.32 33.8 53.0 5.79 8.45 13.3 4.2

10) Control bleached J/C union fabric treated with aqueous solution of mixture of 1% citric acid and1% Na3PO4 (MLR 1:10) at 30°C for 30 min followed by drying at 90°C for 10 min and then curing at 140°C for 5min.

(+) 4.03 36.8 56.2 4.64 6.75 11.8 4.1

11)Control bleached J/C union fabric padded with mixture of 10% (owf) citric acid and 10% (owf) Na3PO4at 100% weight pickup and then dried at 90°C for 10 min followed by curing at 140°C for 5 min.

(+) 4.62 38.9 60.3 4.23 6.20 11.1 3.7


Table 3. Continue.

Treatments

Total CRAa

(Warp+ weft)

Degree

Bending Length

cm

Surface appearance

Properties

K/S Value

at λmax

WIb YIc BId

Warp

(Cotton)

Weft

(Jute)

1. Nil (Control bleached J/C union fabric). 150 1.6 3.8 72.4 18.6 44.2 0.42

7)1% Citric acid treatment at 30°C for 30 min (MLR – 1:10) on bleached jute-cotton union fabric.

160 1.3 3.3 72.3 20.7 46.2 0.58

8) Control bleached J/C union fabric treated with 1% citric acid solution at 30°C for 30 min (MLR – 1:10) in exhaust process before further subjected to UV light exposure for 30 min and subsequently padded with 8% (owf) acrylamide followed by curing at 70°C for 30min.

172 1.2 3.2 71.5 21.1 47.1 0.63

9) Control bleached J/C union fabric padded with 10% (owf) citric acid at 30°C for 30 min (MLR – 1:10) followed by UV light exposure for 30 min and subsequently padded with 8% (owf) acrylamide followed by curing at 70°C for 30min.

175 1.1 3.1 72.0 21.9 47.1 0.68

10) Control bleached J/C union fabric treated with aqueous solution of mixture of 1% citric acid and1% Na3PO4 (MLR 1:10) at 30°C for 30 min followed by drying at 90°C for 10 min and then curing at 140°C for 5min.

205 1.8 4.0 69.7 22.4 42.4 0.74

11)Control bleached J/C union fabric padded with mixture of 10% (owf) citric acid and 10% (owf) Na3PO4at 100% weight pickup and then dried at 90°C for 10 min followed by curing at 140°C for 5 min.

220 2.0 4.3 68.2 22.6 47.4 0.76

a Crease recovery angle, bWI – whiteness index(Humter Lab Scale), cYI-yellowness index (ASTM-E-313,1973), dBI-brightness index (ISO-2470-1977) .

Table 4. Effect of application of single and mixed chemical softeners during ester cross-linking with citric acid in presence of Na3PO4 on desized, scoured and

H2O2 bleached jute-cotton union fabric using citric acid.

Treatments

Weight

Loss

(-) or

gain (+)

Initial Modulus

N/mm

Tenacity

cN/tex

Elongation at

break %

Warp

(Cotton)

Weft

(Jute)

Warp

(Cotton)

Weft

(Jute)

Warp

(Cotton)

Weft

(Jute)

1. Nil (Control bleached J/C union fabric). - 28.4 48.4 4.77 7.27 13.5 4.7

12. . Control bleached J/C union fabric padded with mixture of 10% (owf) citric acid and 10% (owf) Na3PO4at 100% weight pickup and then dried at 90°C for 10 min followed by curing at 140°C for 5 min.

(+)4.62 38.9 60.3 4.23 6.20 11.1 3.7

13.Control bleached J/C union fabric padded with mixture of 10% (owf) citric acid and 10% (owf) Na3PO4at 100% weight pickup and then dried at 90°C for 10 min followed by curing at 140°C for 5 min with additional of the 4% (owf) overall dosages of following chemical softeners

a) 4% POE emulsion along with citric acid and Na3PO4 as above. (+)6.42 39.8 63.0 4.55 6.68 11.5 4.0

b) 4% catasoftener along with citric acid and Na3PO4 as above. (+)5.32 43.8 62.3 4.11 5.90 12.5 4.3

c) 4% AS along with citric acid and Na3PO4 as above. (+)6.20 44.6 64.4 4.01 5.73 11.4 3.9

d) 1%AS and 3%CS(AS:CS=25:75) along with citric acid and Na3PO4 as above.

(+)6.05 43.3 62.0 4.08 5.80 11.8 4.1

e) 1 e) 1%CS and 3%POE emulsion (CS:POE=25:75) along with citric acid and Na3PO4 as above.

(+)6.50 42.5 65.1 4.30 6.20 12.9 4.4

f) 1%AS and 3%POE emulsion (AS:POE=25:75) along with citric acid and Na3PO4 as above.

(+)6.63 45.6 66.5 4.20 6.05 12.5 4.2


Table 4. Continue.

Treatments

Total

CRAa

(Warp+

Weft)

Degree

Bending Length

cm

Surface appearance

Properties

K/S

Value

at

λmax

WIb YIc BId Warp

(Cotton)

Weft

(Jute)

1. Nil (Control bleached J/C union fabric). 150 1.6 3.8 72.4 18.6 44.2 0.42 12. . Control bleached J/C union fabric padded with mixture of 10% (owf) citric acid and 10% (owf) Na3PO4at 100% weight pickup and then dried at 90°C for 10 min followed by curing at 140°C for 5 min.

220 2.0 4.3 68.2 22.6 47.4

13.Control bleached J/C union fabric padded with mixture of 10% (owf) citric acid and 10% (owf) Na3PO4at 100% weight pickup and then dried at 90°C for 10 min followed by curing at 140°C for 5 min with additional of the 4% (owf) overall dosages of following chemical softeners a) 4% POE emulsion along with citric acid and Na3PO4 as above. 215 1.8 4.0 60.7 22.8 46.2 0.76 b) 4% catasoftener along with citric acid and Na3PO4 as above. 210 1.7 3.9 66.5 24.3 42.4 0.74 c) 4% AS along with citric acid and Na3PO4 as above. 220 1.8 4.3 70.6 21.5 48.3 0.82 d) 1%AS and 3%CS(AS:CS=25:75) along with citric acid and Na3PO4 as above.

218 1.8 4.1 66.9 23.8 43.4 0.70

e) 1 e) 1%CS and 3%POE emulsion (CS:POE=25:75) along with citric acid and Na3PO4 as above.

217 1.6 3.8 70.3 22.0 45.2 0.77

f) 1%AS and 3%POE emulsion (AS:POE=25:75) along with citric acid and Na3PO4 as above.

225 1.8 4.0 69.5 22.5 46.2 0.72

a Crease recovery angle, bWI – whiteness index (Humter Lab Scale), cYI-yellowness index (ASTM-E-313,1973), dBI-brightness index (ISO-2470-1977)..

Results of another set of study shown in Table 2 relating to application of either single Poly-oxo-ethylene softener or mixture of catasoftener and poly-oxo-ethylene emulsion softener in varying ratios indicate that 4% (owf) overall dose of application of a mixture of catasoftener and poly-oxo-ethylene emulsion softener in a 25: 75 ratio gives most desirable balance in textile related property parameters with better softening action maintaining relatively higher weight gain and comparable level of surface appearance property parameters as compared to that obtained by application of the overall same dose level of 25: 75 aminosilicone and catasoftener mixture for bleached jute-cotton union fabric.

Effects of different chemical softeners and their mixtures on 100% jute fabric has already been studied and reported in our earlier publication [6]. However, due to presence of cotton part in jute-cotton union fabric it is also necessary to examine separately the efficacy of different single and mixture of chemical softeners for effective softening of jute-cotton union fabric. Relevant data in Table 1 and 2 show the results of the observed property parameters of bleached jute-cotton union fabric after application of different dose level of single and mixtures of selective chemical softeners namely catasoftener, aminosilicone (amino-modified poly-siloxane), poly-oxo-ethylene emulsion and their mixtures of varying ratios. It is observed that 4% (owf) application of catasoftener render the fabric relatively higher softness even with low weight gain than that occur for equal dose level of application of aminosilicone emulsion softener. However, catasoftener produce less whiteness and more yellowness in the resultant fabric. Study relating to application of 4% (owf) overall dose of a mixture of aminosilicone (AS) and catasoftener (CS) in different ratios (0: 100, 25: 75, 50: 50, 75: 25, 100: 0) indicate that 25: 75 ratio of aminosilicone: catasoftener render the fabric an overall balance in textile related property parameters (Table 4) including softness of

jute-cotton union fabric which is found to be measurably better than that obtained by application of the said two softeners individually at comparable dose level.

3.2. Effect of Citric Acid Initiated Grafting

with Vinyl Monomer and Acid Catalysed

Cross-Linking

A separate set of study was carried out to examine the (a) effectiveness of citric acid pre-treatment for photofunctionalization (under UV-light exposure) to facilitate subsequent grafting with acrylamide (a vinyl monomer) by pad-cure method and (b) effectiveness of formation of ester cross-links by citric acid treatment in presence of Na3PO4 as an acidic catalyst to get non-formaldehyde crease resistant finish on jute-cotton union fabric.

Relevant results shown in Table 3 indicate that when jute-cotton union fabric pretreated with 1% citric acid in exhaust bath (equivalent to 10% owf citric acid treatment on weight of fabric considering MLR 1: 10) is further exposed to UV-light (using Phillips 500W MBTF Lamp) and subsequently padded with 8% (owf) acrylamide followed by curing at 70°C for 30 min, there is a net higher weight gain around 3%. Moreover, the improvement in the tensile and crease recovery properties is measurably enhanced, if the said citric acid treatment is carried out by padding at 100% expression instead of exhaust bath technique keeping other treatment conditions same.

Grafting of acrylamide under optimised treatment condition on jute [21] fabric and on cotton fabric [22] by K2S2O8 as chemical initiator followed by UV-light exposure has been studied and relevant reaction mechanism has been described in our earlier publications [11, 21, 22]. K2S2O8 initiated graft co-polymerisation and simultaneous acidic poly-condensation forming cross-links on jute with acrylamide formaldehyde have also been reported [23] from this laboratory describing


the possible reaction mechanism for the same. However, following reaction mechanism may be proposed for citric acid initiated grafting of acrylamide on both jute and cotton substrate.

Reaction Mechanism – I:

Proposed Reaction mechanism for citric acid initiated

grafting of acrylamide on jute and cotton substrate

Reaction Scheme A. Photo functionalization (Initiation) of citric acid under UV-light exposure

(i)

(ii)

The I•/ I1•/ I2

• thus helps in generating free-radicals on jute or cotton cellulose/ jute hemicellulose chain as well as on vinyl monomer (acrylamide) in subsequent steps.

Reaction Scheme B: Initiation and Free radical generation

on jute/ cotton celluloseand jute hemicellulose chain.

Reaction Scheme C: Initiation and Free radical generation

on vinyl monomer(acrylamide)

Reaction Scheme D: Chain extension via propagation of

initiated monomer andhomo-polymer formation through

addition polymerisation process

M• + M → M•2;M

•(n-1) + M →M•n; M•

(m-1) + M→M•m; M•

n + M•

m→M(n+m)

Reaction Scheme E: Graft co-polymerisation between jute/

cotton cellulose and jute hemicellulose and oligomers/

monomers of acrylamide (M•n/ M

•m/ M

•)

Reaction Scheme F: Self catalysed ester crosslinking

between jute/ cotton cellulose and citric acid

Citric acid (2-hydroxy-1, 2, 3 propane-tri-carboxylic acid) is believed to generate free radical moieties bearing carboxylic acid groups by photofunctionalization [4] to act as initiator underexposure to UV-light (as shown in Reaction scheme A (i) and (ii), which may then be utilised in initiation reactions (as shown in Reaction schemes B and C) for subsequent chain extension and finally graft co-polymerization of vinyl monomer (acrylamide) with jute or cotton cellulose (as shown in Reaction scheme D and E) or hemicellulose of jute and homopolymerization of vinyl monomers (acrylamide) leading to chain extension forming oligomers and homopolymers (as shown in Reaction scheme C and D). Also limited fibre modification by self catalysed esterification of cellulose / hemicellulose with citric acid (as shown in Reaction scheme F) during and after the photo exposure cannot be precluded. This ester crosslink formation is however pre-dominant, if the citric acid treatment is carried out with equal amount of Na3PO4 as catalyst followed by drying and curing at specific conditions (as shown later in Reaction scheme – G evidencing the effects of such crosslinking reaction improving noticeable crease recovery angles, Table 3). The observed effects in textile related properties of acrylamide modified jute-cotton union fabric may be considered as the outcome of the above said photo-initiated grafting reactions that has been taken place for the photo-active nature [4] of the citric acid. However, completely different nature of changes in textile related properties were observed after ester cross-link formation reactions [24] by citric acid on jute-cotton union fabric. Such crosslinking on jute [3] and on cotton [24] have been also reported earlier which thus corroborates and supports changes in property parameters following more or less the same trendfor the above said reaction mechanisms.

Results of Table 3 indicate that there is relatively a lesser degree of crosslink formation for the 10% (owf) citric acid treatment in presence of equal amount (10%, owf) of Na3PO4 as catalyst applied in exhaust bath followed by curing at 140°C for 5min than the same treatment being carried by pad-dry-cure technique under comparable dose and treatment conditions. It is observed that use of 10% (owf) Na3PO4 along with 10% (owf) citric acid by pad-dry-cure technique


under comparable conditions of treatment renders the jute-cotton union fabric relatively a higher weight gain, higher initial modulus, higher stiffness (bending length), higher crease recovery angle associated with measurably increased yellowness index and surface colour strength and measurably lower whiteness and brightness indices with noticeable reduction in tenacity and elongation at break. The present findings are further corroborated with our earlier reports [3] on chemical modification of 100% jute fabric with citric acid in presence of different acidic catalysts including Na3PO4 as one of the catalyst. Acid catalysed predominating ester cross-link formation in jute-cotton union fabric may be better appreciated, if the possible reaction mechanism is discussed.

Reaction Mechanism – II:

Proposed Reaction mechanism for ester-crosslink formation

between jute or cotton cellulose chains and citric acid.

The formation of ester cross-link between –OH groups of jute or cotton cellulose and any two carboxylic acid groups of citric acid (Hydroxy-tri-carboxylic acid) can be well appreciated by a look into the suggested possible reaction mechanism:

Reaction Scheme G: Acid catalysed ester crosslink

formation between –OH groups of jute or cotton cellulose

and any two –COOH groups of citric acid

A similar reaction mechanism has been recently reported24for non-formaldehyde ester-crosslink formation in cotton for rendering the fabric anti-crease finish using citric acid for simultaneous dyeing and crease resistant finishing where it is described that on sufficient heating (i. e. by thermal curing) two adjacent –COOH groups of citric acid forms an anhydride leaving behind the third –COOH group as free and in turn the anhydride breaks at high temperature of curing to form an ester-linkage with –OH groups of cotton cellulose, leaving one of the –COOH group made free; which in turn again form another anhydride and finally facilitates the formation of second ester linkage in between –OH group of adjacent cotton cellulose and one of the –COOH group of

citric acid and thus form the said ester-crosslink (as shown in Reaction scheme-G in the final form, without showing the step by step reactions as described in earlier literature [24]) rendering the resultant fabric improved crease resistant property. Hence, it may be said that also in the present case a similar mechanism of crosslink formation occur in both jute and cotton cellulose with citric acid treatment in presence of Na3PO4 as acidic catalyst under specific conditions of treatment by pad-dry-cure process. However, higher the citric acid crosslinking, higher is the stiffness imparted in the jute-cotton union fabric which needs to be softened appropriately.

3.3. Effect of Single and Mixture of Chemical

Softeners

Among the different single chemical softeners applied along with citric acid and Na3PO4 during citric acid cross-linking treatment on jute-cotton union fabric, from the data shown in Table 4, it is observed that application of 4% (owf) poly-oxo-ethylene softener is found to be very useful in better tenacity retention, lesser increase in bending length and yellowness index with marginal loss in improved crease recovery angle, while application of 4% (owf) catasoftener and 4% (owf) aminosilicone individually and separately reveals higher loss in tensile strength for both the softeners, but measurable increase in yellowness index coupled with some lowering in crease recovery angle for catasoftener; while aminosilicone causes higher improvement in crease recovery and more lowering in yellowness index. With these preliminary observations and also considering the results of initial study in the present work on application of different mixed softeners on bleached jute-cotton union fabric (Tables-2and 3), application of (a) mixture of aminosilicone (AS) and catasoftener (CS), (b) mixture of catasoftener (CS) and poly-oxo-ethylene (POE) and (c) mixture of aminosilicone (AS) and poly-oxo-ethylene (POE) emulsions have been tried during citric acid cross-linking of jute-cotton union fabric under specified treatment conditions. Among these three combinations (a, b and c) of application of 4% overall dose of 25: 75 ratio of aminosilicone and poly-oxo-ethylene softener in this case offers an overall better balance in weight gain, tensile strength retention, improvement in crease recovery, bending length, whiteness and yellowness indices indicating a better finished jute-cotton union fabric for upholstery and furnishing applications.

3.4. Study of Surface Morphology of Jute and

Cotton Fibres

It is observed from comparison of micrograph (a) and (a/), Fig 1, for multicellular desized scoured and bleached jute and convoluted cotton respectively, micrographs (b), Fig – 1 for simple 1% citric acid pre-treated bleached jute, and micrograph (b/), Fig 1, for 1% citric acid pretreated bleached cotton reveals that micrograph (b) shows some surface leaching action on jute removing intercellular encrusting materials but with occasional deposition of some powdery material while, micrograph (b/) shows some deconvolution


with some sort of surface roughening action with deposition of some powdery substance on the surface of the cotton probably due to some citric acid molecules perhaps deposited/ anchored superficially. These deposits may be due to self-catalysed cross-linked citric acid anchored with either cotton cellulose or jute cellulose or hemicellulose chain. A comparison among micrographs (a) and (b), Fig 1, for control bleached jute and cotton respectively with corresponding micrographs (c) and (c/), Fig-1, for citric acid initiated acrylamide grafted jute and cotton respectively and micrographs- (d) and (d/), Fig-1, for acid catalysed citric acid cross-linked jute and cotton respectively, reveal much

highersurface deposition effect on both jute and cotton fibres, where the surface film is found to be more uniform and over spread for acrylamide grafted jute and cotton. Among jute and cotton, for both types of chemical modifications, the effect of surface filling and deposition of film is found to be much higher on cotton than jute. Moreover, comparison of micrographs- (e) and (e/), Fig-1, for citric acid crosslinked jute and cotton substrate respectively in presence of Na3PO4along with application of mixture 25: 75 aminosilicone and poly-oxo-ethylene softener show much smoother and high coverage polymeric films on both the fibre surface.

Fig. 1. (a-e) and (a’ - e’): SEM photographs of: (a)Desized, scoured and 2% H2O2 bleached jute fibre (a’) Desized, scoured and 2% H2O2 bleached cotton fibre

(b) 1% citric acid treated bleached jute fibre (b’) 1% citric acid treated bleached cotton fibre (c) 1% citric acid treated jute fibre subjected to photo-exposure

for 15min UV-light followed by grafting with 8% acrylamide (c’) 1% citric acid treated cotton fibre subjected to photo-exposure for 15min UV-light followed

by grafting with 8% acrylamide (d) Conventional bleached jute subjected to 10% citric acid treatment along with 10% Na3PO4 by pad-dry-cure process (d’)

Conventional bleached cotton subjected to 10% citric acid treatment along with 10% Na3PO4 by pad-dry-cure process (e) Conventional bleached jute

subjected to 10% citric acid treatment along with 10% Na3PO4 and 4% (owf) mixture of 25: 75 aminosilicone and poly-oxo-ethylene softener (e’)

Conventional bleached cotton subjected to 10% citric acid treatment along with 10% Na3PO4 and 4% (owf) mixture of 25: 75 aminosilicone and poly-oxo-

ethylene softener.

4. Conclusions

� Simple 1% citric acid treatment interestingly shows an odd effect showing a small weight gain with less reduction in bending length, some enhancement in crease recovery angle and relatively higher retention of initial modulus, superseding the effect of minor weight loss due to surface leaching action and possible acidic degradation.

� Citric acid treatment is when accomplished in presence of equal amount of Na3PO4 catalyst by pad-dry-cure technique it shows notable enhancement in crease recovery angle with measurable increase in bending length along with relatively higher weight gain and relatively higher initial modulus associated with measurably lower whiteness index coupled with low but measurable increase in yellowness index. The observed

effects are believed to be due to ester cross-linking between citric acid and cotton cellulose and jute cellulose / hemicellulose chains.

� If, 1% citric acid treated jute-cotton union fabric is subjected to UV-light exposure for 15-30min, and is subsequently padded with 8% (owf) acrylamide followed by curing at 70°C for 30 min, a net weight gain of around 3% along with measurable increase in initial modulus and tensile strength have been observed. This effect is due to photo-functionalisation of citric acid under exposure to UV-light facilitating grafting of poly-acrylamide on jute-cotton union fabric.

� 4% overall dose of application of 25: 75 mixture of catasoftener and poly-oxo-ethylene emulsion softener on scoured and bleached jute-cotton union fabric is found to give a better balance in textile related property parameters than that obtained by application of single


catasoftener, aminosilicone and poly-oxo-ethylene emulsion softener individually or even than that obtained by 4% dosages of 25: 75 mixture of aminosilicone and catasoftener applied under the comparable condition of treatment.

� Among the different single and mixture of softeners applied during citric acid cross-linking of jute-cotton union fabric, it is observed that either application of 4% single (owf) poly-oxo-ethylene emulsion softener or application of 4% (owf) overall dosages of 25: 75 ratio of mixture of aminosilicone and poly-oxo-ethylene softener offers a good balance in desirable property parameters showing a better finished jute-cotton union fabrics for upholstery and furnishing applications.

Acknowledgement

Authors are thankful to Dr. R. Bhar of Dept. of Instrumentation Science (Formerly USIC), Jadavpur University for providing the instrumental facility for the Scanning Electron Micrographic study.

References

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