Meer Md Rasel Khan*, Ashraful Islam, Md. Ahsan Habib, Md. Nahid Pervez

Transcription

1 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 9 ISS 9-8 Raw Silk Processing to Textile Fibre and Comparative Analysis between Acid and Reactive Dyed Samples of Silk Fabric by Laboratory Experiment Meer Md Rasel Khan*, Ashraful Islam, Md. Ah Habib, Md. ahid Pervez School of Chemistry and Chemical Engineering, Wuhan Textile University, Wuhan, P. R. China Corresponding author: Meer Md Rasel Khan; rasel.texbd@gmail.com Abstract Silk fibre is one of the important and demanded textile fibre in the sector of textile fabric and garments manufacturing. In the industrial sector the coloration of silk fabric is done by acid dyes. In this paper, laboratory experiments were done for coloration of silk fabric. For coloration two different dyes, acid dye (ylo RL) and reactive dye (Lanasol ) have been used with their Different recipe, separately applied on different samples but with same properties of silk fabrics. Different tests like wash fastness, rubbing fastness, perspiration test, tensile strength and elongation were conducted on the dyed samples and comparison was made among all the results from Acid dyed and s. Getting better wash fastness, better absorbency and other positive test results for reactive dyes leads to the conclusion, that dyeing of silk with reactive dye has a great prospect in textile coloration. Keywords Acid dye, Lanasol, ylo RL, Raw Silk, Reactive dye, Silk fibre. ITRODUCTIO Table ) Silk is a natural protein fibre of animal origin. The dyeing mechanism of silk dependents on free amino groups, TABLE : MECHAICAL PROPERTIES OF SILK FIBRE [] carboxyl groups and phenolic with accessible OH group. Because of slightly cationic character of silk with isoelectric point at above ph.0, it can be dyed with anionic dye such Types Tensile Young's Elongation Density as acid, metal complexes, reactive and selected direct dyes. of Material Strength Modulus at (g/cm) Fibre (MPa) (GPa) Failure () But the main objective of coloration of a textile fibre is that the permanency of the color and should not allow dama Spider of natural abstract of fibre. This implies that it should not Silk destroy its color during processing following coloration Enhance atural d B.Mori and dyeing & subsequent useful life (i.e. washing, light, Fibres Silk rubbing, perspiration, and saliva). Silk contain very small amount of sulphur. There are two main types of silkworm, B. Mori mulberry silk also called cultivated silk and wild silk of Silk which Tussah silk is the most important representative []. The mechanical properties of silk fibres are shown below ( CHEMICAL COMPOSITIO OF SILK: Author Meer Md Rasel Khan has completed M.Sc. in Dyeing & Finishing Engineering from Wuhan Textile University, Wuhan, China- 4007, PH rasel.texbd@gmail.com Co-Author Ashraful Islam is currently pursuing M.Sc. in Dyeing & Finishing Engineering from Wuhan Textile University, Wuhan, China- 4007, PH ashrafulislam7@gmail.com 0 The strands of raw silk as they are unwound from the cocoon consist of the two silk filaments mixed with sericin and other materials. About 7 of the strand is silk i.e. fibroin and. is sericin; the remaining materials consist of fat and wax ( ), ash of silk fibroin (0.) and mineral salts (0. ). As a consequence of the spinning process, the fibre has two main part sericin and fibroin. Sericin called silk gum a minor component of the fibre. Sericin is yellow, brittle, and inelastic substance. It acts a twin fibroin filament and conceals the unique lustre of the fibroin. Sericin is an amorphous structure and it is dissolved in a

2 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 0 ISS 9-8 hot soap solution. The greatest sericin content is present in outer layer of cocoon whereas the least sericin is present in the innermost layer of the cocoon. Fibroin is the principal water insoluble protein (i.e. 7 of the weight of raw silk). Fibroin has highly oriented and crystalline structure and it is composed of 6 various amino acids. Raw silk is treated for removing the gummy materials and various types of impurities from the silk by scouring process. Then the silk fiber is collected and supplied for producing silk fabric by weaving process [], [], [] C.I. Acid 6 CAS Registry umber:0-0-9 ao S H CH CO (Double azo class) Although, in acid dyes the functional group like CH TABLE : EFFECT OF DIFFERET TYPES OF CHEMICALS O SILK FIBRE [] Particulars Effect of Acids Resultant Effect The Fibroin of silk can be decomposed by strong acids into its constitute amino acids. In moderate concentration, acids cause a contraction in silk. Dilute acids do not attack silk under mild conditions. SO a or SO are responsible for dye solubility in water (Solubilizing group) and also create ionic bond with protein fibre (e.g.: Silk). The reaction between silk fibre and acid dyes is given below: Fibre-H(S) + H+ (aq) + HSO4- (aq) Fibre-H+HSO4- Fibre-HHSO4(S) + Dye-SO-(aq) Fibre-H+Dye- SO-(S) + HSO4-(aq) Effects of Alkalis Color Index (C.I.) & CAS Registry umber Silk is less readily damad by alkalis than wool. Weak alkalis such as soap, borax and ammonia cause little considerable dama. Silk dissolves in solutions of concentrated caustic alkalis. Effect of Organic Silk is insoluble in the dry-cleaning Solvent solvents in common use. Effects of Insects Insect does not affect silk. Figure : Silk fibre dyeing with acid dyes [4]. Effect of Mildew Silk is affected by mildew slightly. SILK DYEIG WITH REACTIVE DYES: SILK DYEIG WITH ACID DYES: Acid dyes contains acid groups, such as COOH and SOH which form attractions to the slightly basic H groups in the amide links of wool, silk and nylon [4] Reactive dyes are anionic water soluble colored organic compounds that are capable of forming a covalent bond between reactive groups of the dye molecule and neucleophilic groups on the polymer chain within the fibre. Consequently, the dyes become chemically part of the fibre TABLE : THE CHEMICAL COSTITUTIOS OF SOME TYPICAL ACID by producing dyepolymer linkas. In this regard, covalent DYES [] dye-polymer bonds are formed, for instance, with the hydroxyl groups of cellulose, the amino, hydroxyl, mercapto groups of proteins and the amino groups of ame Chemical Structure polyamides. HO WH C.I. Acid 97 C.I. umber:890 CAS Registry umber: ao S OH H (Single azo,: Metal Complexes) O CH 0 Dye H HR W H Dye H HR H Figure : Reaction of a mono-chlorotriazine dye with amino group of protein Forming a covalent bond between dyes and fibres had long been attractive to dye chemists, since attachment by physical adsorption and by mechanical retention had the disadvanta of either low wash fastness or high cost. It was anticipated that the covalent attachment of the dye

3 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 ISS 9-8 molecules to the fibre would produce very high wash Material and Liquor Ratio fastness because covalent bonds were the stronst known (M:L) :0 binding forces between molecules. The energy required to break this bond would be of the same order as that required Temperature 80 c breaking covalent bonds in the fibre itself. Reactive dyes Time 90 min. were initially introduced commercially for application to cellulosic fibres and this is still their most important use. ph 0 Reactive dyes have also been developed commercially for application on protein and polyamide fibres [] TABLE 4: THE CHEMICAL COSTITUTIOS OF SOME REACTIVE DYES APPLICABLE O SILK [6] Trade ame and Manufacturer Reactive Group TABLE 6: RECIPE CALCULATIO FOR SILK DEGUMMIG PROCESS Particulars Calculation Procion MX (Zeneca) D H Fabric weight Liquor (49 0) Soap 49 g 40 ml ( 40)/000=6.7g D HOC C CH Wetting ant ( 40)/000=4.9g Lanasol (CGY) ph 0 Br Weight after degumming 47.7 g Weight loss ( )/49 =.6 Sumifix Supra D H (SK) Procedure for silk degumming: H SO CH CH OSO a At first the weight of the raw fabric was measured with electrical balance. Required amount of water was taken into the bath. Then required amount of wetting ant and soap. METHODS AD MATERIALS was added into the bath and dissolved it properly. The ph of the bath was checked and the fabric was added into the. RAW MATERIALS Raw materials/samples: Raw Silk, Silk Fabric (Weaved) Dyeing Materials: ylo RL (Acid Dye), bath. Then, the temperature of the bath raised to 90 degree Celsius and continued for 90 min. After 90 min, the fabric was taken out from the bath and washed with cold water then dried it using woven. Then the dried weight of the Lanasol (Reactive Dye), Dyeing chemicals and fabric was taken and the amount of weight loss was auxiliaries, Laboratory dyeing machine, Woven fabric calculated. testing instruments.. SILK DEGUMMIG PROCESS. SILK BLEACHIG PROCESS TABLE 7: RECIPE FOR SILK BLEACHIG Silk degumming process is applied on raw silk (Table & Chemicals and Parameters Recipe TABLE 6). Hydron per oxide (HO) Invatex AC (Organic acid) Wetting ant 0 ml/l 0. g/l g/l TABLE : RECIPE FOR SILK DEGUMMIG PROCESS Tri-sodium-phosphate to adjust ph 8-9 Chemicals and Parameters Recipe EDTA g/l Soap Wetting Ant g/l g/l M: L :70 Time 90min. 0

4 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 ISS 9-8 Temperature (6-70) C EDTA g/l M: L :60 Temperature Time (7-8) C min TABLE 8: RECIPE CALCULATIO FOR SILK BLEACHIG PROCESS Particulars Calculation Fabric weight 47.7 g Liquor =9 ml Hydron per oxide (0 9)/000=66.6 Invatex AC (0. 9)/000=0.66 g After Treatment ylofixan P Liq Acetic acid.00 Temperature 70oC Time 0 min. Rinse Cold Rinse Wetting ant EDTA Tri-sodium-phosphate ( 9)/000=. g ( 9)/000=. g (..9)/000=6.98 g ph 8. Weight loss 0.7 Fabric weight.97 g.6 g.7 g.96g Liquor 8. ml 89.6 ml. ml 77.6 ml Lyon PAM Procedure for silk bleaching: 0. ml 0.9 ml 0.ml 0.77 ml Liq At first fabric weight was measured with electrical balance. Opticid 0.04 ml 0.0 ml 0.0 ml 0.9 ml The operation bath was filled with required amount of water. Then wetting ant, EDTA, Invatex AC added into Wetting ant 0. ml 0.9 ml 0. ml 0.77 ml the bath and the ph of the solution was measured and trisodium-phosphate was added to adjust the ph of the EDTA 0.ml 0.9 ml 0. ml 0.77 ml solution. Then the fabric was inserted into the bath and the temperature raised to 0oC. Then hydron per oxide was Dye.97 ml 4.74 ml 7.44 ml 8.88 ml added into the solution. Then the temperature raised to After Treatment 70oC. The temperature of the bath was kept around 6- ylofixan P 70oC for 90 min. After 90 min. the fabric was taken out Liq from the bath. Then washed it once in cold water and once in hot water, followed by rinsing in water. At last weight 0.4 ml 0. ml 0. ml 0.07 ml (to 0.06 ml Acetic acid 0.08 ml 0.06 ml adjust ph 0. ml was taken to calculate the loss in weight due to bleaching. 4.).4 SILK DYEIG WITH ACID DYE TABLE 0: SILK DYEIG RECIPE CALCULATIO FOR DIFFERET SHADE WITH ACID DYE Parameters For For For For TABLE 9: APPLIED RECIPE FOR SILK DYEIG WITH ACID DYE Parameters Recipe Dye (ylo RL) x Lyon PAM Liq g/l Opticid (acid nerator) 00 ( ph 4-) Wetting ant g/l 0

5 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 ISS 9-8 Glauber Salt 98g 66g g 06g Soda ash 0.4 g 0.4 g 0.4 g 0.40 g Sequestering ant g 0.8g 0.78 g 0.68 g Wetting ant 0.88 g 0.8g 0.78 g 0.68 g Figure : Dyeing curve of silk dyeing with acid dye (ylo RL).. SILK DYEIG WITH REACTIVE DYE TABLE : GEERAL RECIPE FOR SILK DYEIG WITH REACTIVE DYE Parameters Recipe Dye (Lanasol ) X.6 TEST PROCEDURES FOR DYED MATERIALS Glauber Salt (aso4. 0 HO) 0-80 g/l.6. COLOR FASTESS TO WASHIG Soda ash - g/l (ph 8.) Sequestering ant g/l Wetting ant g/l.6. COLOR FASTESS TO RUBBIG Cool bath and rinsing Soaping After Treatment g/l; ERIOPO R liq. (anionic soaping ant); ( min. at 80 c) Figure 4: Dyeing curve of silk dyeing with reactive dye (Lanasol ). ISO 0 C0 was followed to carry out the wash fastness test of both acid and reactive dyed samples. ISO 0 X was followed to carry out the rubbing fastness test of both acid and reactive dyed samples..6. COLOR FASTESS TO PERSPIRATIO ISO 0 E04 was followed to carry out the perspiration fastness test of both acid and reactive dyed samples. Cold rinsing Scooping (acetic acid) ml/l (0 min. at 40 C).6.4 STREGTH TESTIG Strength test was carried out following the standard method of ASTM D04. TABLE : SILK DYEIG RECIPE CALCULATIO FOR DIFFERET SHADE WITH REACTIVE DYE Parameters For For For For Fabric weight.77 g.6 g.6 g.6 g Required liquor 88. ml 8 ml 78 ml 68 ml Dye.77 ml 8.44 ml ml 6.08 ml Equipment: A computerized strength test machine namely Universal Strength Tester (Titan) was used to measure the strength of the samples. The samples used in this test are: Raw Silk Bleached silk Acid dyed silk Reactive dyed silk 0

6 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 4 ISS 9-8 Diacetate RESULT AD DISCUSSIO. SILK FABRIC DYED SAMPLES WITH ACID DYE AD REACTIVE DYE Bleach ed cotton Polya mide Polyes ter Acryli c Wool Figure : Silk fabric dyed samples with acid dye and reactive dye From Table 4 it can be seen that incase of acid dye Bleached cotton, Polyester, Acrylic and Wool gives very good result and for these fabrics the staining result belongs to 4-. For Polyamide the grading for staining is good up to shade but in case of shade it gives poor result (-4). In case of Di-acetate no continuing result has been found but it gives the lowest grading among all of the samples for (Grey scale grading ).. GREY SCALE EVALUATIO FOR COLOR FASTESS TO On the other hand, for reactive dye Di-acetate, bleached WASHIG cotton, Acrylic gives very good result (Grey scale grading TABLE : GREY SCALE ASSESSMET OF CHAGE I COLOR FOR ran 4-), Wool also gives good result except high shade COLORFASTESS TO WASHIG OF ACID AD REACTIVE DYED SILK (-4 for shade), polyamide also gives excellent result WOVE FABRICS except shade but in case of Polyester the staining result is very poor and lowest among other samples for higher shade (Grey scale grading for shade). Lanas Lanas Lanas Lanas ylos ylos ylos ylos From above circumstance, the conclusion is that more or ol ol ol ol an an an an less all fibres of multifibre fabric is stained by acid dyed silk g g g g and reactive dyed silk. But it is noticeable in assessment e RL e RL e RL e RL that Di-acetate, polyamide, polyester is more stained by both dyed samples than any other fibre of multifibre fabric Comparing the grey scale grading for chan in color for the test of color fastness to washing (Table ), it can be seen that reactive dyed sample gives excellent () result in case of all kinds of tested shade than acid dyed samples (4-). TABLE 4: GREY SCALE ASSESSMET OF STAIIG FOR COLORFASTESS TO WASHIG OF ACID AD REACTIVE DYED SILK WOVE FABRICS Multif ibre fabric ylo RL ylo RL ylo RL ylo RL Lana sol n Lana sol n Lana sol n Lana sol n. COLOR FASTESS TO RUBBIG TABLE : ASSESSMET RESULT OF RUBBIG FASTESS AT WARP WAYS FOR ACID AD REACTIVE DYED WOVE FABRICS Dry Wet Dry Wet ylo RL ylo RL Lanasol Lanasol 0

7 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 ISS 9-8 TABLE 6: ASSESSMET RESULT OF RUBBIG FASTESS AT WEFT e WAYS FOR ACID AD REACTIVE DYED WOVE FABRICS Dry Wet Dry Wet ylo RL ylo RL Lanasol Lanasol From Table and Table 6 it can be seen that, in case of both acid and reactive dyed silk fabric samples the grey scale grading is. Which is to say, no color transferred to undyed cotton cloth. So it can be said that color fastness to rubbing for both acid and reactive dyed silk is totally satisfactory..4 COLOR FASTESS TO PERSPIRATIO TABLE 7: ASSESSMET RESULT OF COLOR CHAGE TO PERSPIRATIO O ACID AD REACTIVE DYED WOVE FABRICS. TESILE STREGTH TEST REPORT Acidic Alkaline Acidic Alkaline perspiration perspiration perspiration perspiration solution solution solution solution ylos ylos ylos ylos Lanas Lanas Lanas Lanas an an an an ol ol ol ol g e RL g e RL g e RL g e RL Bleac hed cotton Polya mide Polyes ter Acryli c Wool From Table 7 it can be seen that, for both acid and reactive dyed silk fabric, there was not any chan in color due to the perspiration test. From Table 8 it can be seen that, for staining to perspiration test, only polyamide fibre among different fibres of multifibre fabric is stained by acid dyed silk, none of fibre from multifibre fabrics is stained by reactive dyed silk. The result of tensile strength test of raw silk, degummed and bleached silk, acid and reactive dyed silk are shown as below: TABLE 8: ASSESSMET RESULT OF STAIIG TO PERSPIRATIO O ACID AD REACTIVE DYED WOVE FABRICS Multif ibre fabric Acidic perspiration solution ylo RL ylo RL Alkaline perspiration solution ylo RL ylo RL Acidic perspiratio n solution Lan asol n Lan asol n Alkaline perspiratio n solution Lan asol n Lan asol n Figure 6: Graphical Representation of Tensile Strength of Raw Silk Diacetat 0

8 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 6 ISS 9-8 ) ) Raw Silk Degummed and Bleached Silk Acid Dyed Silk Fabric Reactive Dyed Silk Fabric From Figure 7: Graphical Representation Tensile Strength of Degummed and Bleached Silk Figure 8: Graphical Representation of Tensile Strength of Acid dyed silk (&) and Reactive Dyed Silk (&4) fabric TABLE 9 it can be seen that, the tensile strength is increased in every step of processing but in case of reactive dyed sample (4.7, 4 ) the tensile strength is comparatively very poor than acid dyed sample (9.7, 9.87 ) Maximum Breaking Force (C) Acid Dye()Reactive Dye ()Acid Dye ()Reactive Dye () Dye Concentration () Figure 9: Maximum Breaking Force vs. Dye Concentration Acid Dyed Sample Reactive Dyed Sample From Figure 9 it can be seen that, with the increase of Dye Concentration the Maximum Breaking Force has been increased for both acid and reactive dyed samples but in case of reactive dyed sample it is comparatively poor than acid dyed sample. TABLE 9: DATA AALYSIS OF TESILE STREGTH () AT DIFFERET STATES OF THE SILK FABRICS Different States Data (Max. Force Data (Max. Force 0

9 International Journal of Scientific & Engineering Research, Volume 6, Issue 6, June-0 7 ISS 9-8 Extension () Acid Dye ()Reactive Dye ()Acid Dye ()Reactive Dye () Dye Concentration () Figure 0: Extension vs. Dye Concentration Acid Dyed Sample Reactive Dyed Sample From Figure 0 it can be seen that, with the increase of Dye Concentration the Extension does not show any significant chans for both acid and reactive dyed samples. Comparing the consequential data of different tests for acid dyed and reactive dyed silk fabrics, it has come that, application of reactive dye on silk fabric gives satisfactory result comparing to acid dyed samples. For light shade reactive dyed samples were relatively dull than acid dyed samples of same shade but with the increase of shade the depth of color increased for reactive dyed samples comparing with acid dyed samples which indicates well fixation of reactive dyes on silk fabric. In case of wash fastness test, reactive dyed samples showed even better result than acid dyed samples. In case of other fastness tests like rubbing and perspiration tests reactive dyed samples gave almost similar and somewhere way better results than acid dyed samples. In case of tensile strength the comparative analysis showed that reactive dyed samples tears at low force () than acid dyed samples, in case of acid dyed samples the tensile strength is increased like twice that raw silk, but in case of reactive dyed sample the increase percenta of tensile strength is not that much. In case of elongation there is not much difference between acid dyed and reactive dyed samples. Treating silk in alkali medium during reactive dyeing process is the possible cause for loosing or not gaining that much strength like acid dyed samples. 4. COCLUSIO This paper contains two parts, one part contains the Although with few obstacles, this experiment came out processing of raw silk and another part contains the with great prospect for silk dyeing with reactive dyes and comparative consequences from Acid dyed and Reactive lead to a way for reactive dyes to be a well substitute of dyed Silk woven fabrics. acid dyes. REFERECES [] Md. Koushic Uddin and Ms. Sonia Hossain, International Journal of Engineering & Technology IJET-IJES, 0 (00). [] Kelvin Loh and Willy Tan (0). atural Silkworm-Epoxy Resin Composite for High Performance Application, Metal, Ceramic and Polymeric Composites for Various Uses, Dr. John Cuppoletti (Ed.), ISB: , InTech, Available from: [] Silk fibre Physical and Chemical Properties of Silk Fibre, Textile Fashion Study, Textile Engineering and Fashion Design Blog ( (0). [4] How dyes attach themselves to fabric, Salter s Chemistry ( [] Dye World Dye Variety ( ) [6] M L Gulrajani, Society of Dyers and Colourists (SDC), Coloration Technology, (008) 0