Indian Journal o f Fiore & Tex tile Research Vol. 28. Dece mber 2003, pp. 450-455 Pseudo single-bath process for ambient temperature bleaching and reactive dyeing of jute S N C hattopadh yay, N C Pan & A Day" Chemi cal & Biochemical Processing Division, National Institute of Research on Jute & Alli ed Fibre Technol ogy. 12 Regent Park , Ko lkata 700 040, Ind ia Received 19 Jlllle 2002; accepted 10 September 2002 Grey j ute fi bre has been bleached at ambient temperature using hydrogen peroxide and th en co ld dyed with Proc ion Red M8B and Remazo l Ye llow FG dyes by four di ffe rent process seq uences. name ly conve nti onal two-step process, trlle si ngle-bath process , pseudo single-bath process and pseudo si ngle-bat h process using spe nt bleach bath . The e ffect of process sequ ences o n colour yield of dyed j ute fi bre has been evaluated usi ng computer colour matching system. It is obse rved th at the colour yield by pseudo si ngle-bath process is we ll co mparab le with that of th e co nventio nal two-step ambi ent temperature bleach ing and cold reactive dye ing process. It is also observed that th e colour yield is max imum in case of pseudo si ngle-bath process and mi nimum in case of true single-bath process. The process o f dyei ng has no effect on A """ value whi ch confi rms no alterati on in the hue and tone of any sample dyed wi th reactive dye by d ifferent sing le-bath processes. The wash fas tn ess is satisfactory in all th e processes . Keywords : Ambient temperature bleac hing, Jute fi bre, Pse udo single-bath process, Reacti ve dye in g 1 Introduction Decreas ing trend in the use of jute fibre in the traditional sector, like packaging, is being well compensated by the increasing use of jute in the di versified sectors. Jute is now finding its use in several di versified applications like curtains, uphol stery, bags / luggage, handicrafts and even in apparel sector. So, the wet process ing of jute has occupied very important pos iti on in jute industry as the diversifi ed use needs attracti ve look where bleac hing, dyeing and fi ni shing are must. But the processi ng of jute requires a lot of energy, water, chemicals, etc. which not only increases the cost of processing but also leads to environment pollution through efflu ents. Several works have been done in the recent past, like ambient temperature bleac hing 1-4, foam application technology and singlebath bleaching-dyeing to combat the above problems. Considering the energy problem, environment pollution, ease of process ing in the rural sector, etc., the present work has been devised in such a way that all the process ings like bleaching and dyeing will be can-ied out at ambient temperature. Moreover, the attempts have also been made to carry out both the processes in the same bath. Al so, the spent liquor after " To whom all the correspondence should be addressed. Phone : 242 12 11 5; Fax : 009 1-033-24 7 12583; E-mail: nirjaft @vsnl.net ambi ent temperature bleaching 5 has been re used for another batch of ambi ent temperature bleac hing. Th is is an integrated approach suitable spec ifica ll y for rural small -scale sector where all the resources like thermal energy, electrica l energy, skill ed manpower, adequa te finance, easy ava il ability of chemica ls, water, etc. are scare. 2 Materials and Methods 2.1 Materials Grey jute fibre of TD-3 vari ety having f ineness of 2.4 tex was used fo r the ex peri ment. The following chemi ca ls of anal yti ca l grade we re used for the stud y : hydrogen peroxide, tri sodium phosphate, sodium hydrox ide, sodium ca rbo nate . sodium hydrosulphite , sodium persulph ate, sod ium si li cate, magnes ium sulphate he ptahydrate, non-i oni c detergent (Ultravon JU) and acetic aci d. Reacti ve dyes Proc ion Red M 8B (n ucleoph ilic substitution type) and Remazol Ye ll ow FG (nucleoph ilic additi on type) were used fo r dye in g of jute fibre. 2.2 M ethods 2.2.1 Conventional Bleaching of G r ey Jute Fih re Bleachin g of grey j ute fibre was carried ou t in a closed vessel at 90°C fo r 2 h, keepi ng the ma terial- toli q uor rati o at 1: 20, us ing hydrogen perox ide ( I vo l). CHATTOPADHYAY el al. : AMBIENT TEMPERATURE BLEACHING & REACTIV E DYEING OF JUTE trisodium phosphate (5 gIL), sodium hydroxide (1 gIL), sodium silicate (10 gIL) and non-ionic detergent (2 gIL). After bleaching, the fibre samples were washed thoroughly in cold water, neutralized with acetic acid (2mJlL), again cold washed and finally dried in air. 2.2.2 Ambient Temperature Bleaching of Grey Jute Fibre Jute fibre intended for ambient temperature bleaching was dipped in a solution containing hydrogen peroxide (10 vol), sodium silicate (20 gIL), sodium hydroxide (20 gIL), trisodium phosphate (5glL), sodium persulphate (lOglL), magnesium sulphate heptahydrate(0.5 gIL) and Ultravon JU (10 gIL), keeping the material-to-liquor ratio at 1:3, and queezed to give 100 % wet pick-up. The samples were put in a plastic bag and kept as such for overnight. The samples were then washed, neutralized with acetic acid (2 mJlL) and washed again in cold water before drying at room temperature. 2.2.3 Dyeing of Ambient Temperature Bleached Jute Fibre Ambient temperature bleached jute fibres were dyed with two different reactive dyes , namely Procion Red M88 and Remazol Yellow FG, using the following procedure : Pracion Red M8B - Dye bath was made with dye (4%) and Glauber' s salt (60 gIL), keeping the material-to-liquor ratio at 1:20 . The bleached fibre samples were dipped into the dye bath and kept for 1 h with stirring at 30°C. After this treatment, sodium carbonate (20 gIL) was added in the same bath and kept for 45 mjn under the same condition . Thereafter, the samples were washed with cold water, soaped with Ultravon JU (2 gIL) for 15 min at boil followed by usual washing and drying in air. Rernazo! Yellow FG - Dye bath was made with dye (4%) and Glauber' s salt (80 gIL), keeping the material-to-liquor ratio at 1:20 . The bleached fibre samples were dipped into the dye bath and kept for 20 min with stilTing at 30°C. After this treatment, the sodium hydroxide (4 gIL) was added in the same bath and kept for Ih under the same condition. Thereafter, the samples were washed with cold water, soaped with Ultravon JU (2 gIL) for 15 min at boil followed by usual washing and drying in air. 2.2.4 Single-Bath Bleaching - Dyeing of Jute Fibre Ambient temperature bleaching and reactive dyeing of jute fibre was carried out by using three different process sequences, namely true single-bath process, pseudo single-bath process and single-bath process using spent bleach bath. 451 pse ud o 2.2.4.1 True Single-Bath Process For ambient temperature bleaching, grey jute fibre was dipped in a solution containing hydroge n peroxide 00 vol), sodium silicate (20 giL ), sodium hydroxide (20 gIL), tri sodium phosphate (5g/L ). sodium persulphate (10 gIL), magnesium sulph ate heptahydrate (0.5 gIL) and Ultra von JU ( 10 gi L ). keeping the material-to-liquor ratio at 1:3 . After keeping the bath as such for 2 h, sod ium hydrosulphite ( 10 gIL) was added to it and the solution was stirred for 15 min . Procion Red M8B (4%) and Glauber ' s salt (60 giL ) were added to the above bleach bath and kept for I h with stirring at 30°C. After this treatment , the sodium carbonate (20 gIL) was added in the same bath and kept for 45 min under the same condition . Thereafte r. the samples were washed with cold water. soa ped with Ultravon JU (2 giL) for 15 min at boil fo ll owed by usual washing and drying in air. Remazol Yellow FG (4 %) and Glauber 's salt (80 gIL) were added to the above bleach bath and ke pt for 20 min with stirring at 30°C. After this trea tme nt. the sodium hydroxide (4 gIL) was added in the sa me bath and kept for 1 h under the same conditi on. Thereafter, the samples were washed with cold water. soaped with Ultravon JU (2 gIL) for 15 min at bo il followed by usual washing and drying in air. 2.2.4.2 Pseudo Single-Bath Process For ambient temperature bleaching, grey jute fi bre was dipped in a solution containing hydrogen perox ide (10 vol), sodium silicate (20 gIL), sodium hyd rox ide (20 gIL), trisodium phosphate (5glL), sodium persulphate (10 gIL), magnesium sulphate heptahydrate (0.5 gIL) and Ultravon JU (10 gIL), keeping the material- to- liquor ratio at 1:3, and squeezed to give 100% wet pick-up. The samples were put in a pl asti c bag and kept for 2 h .The bleached fibre (with out washing) was then put in a separate bath containing ten times its volume of water (M:L :: 1:10). Sodium hydrosulphite (3 gIL) was added to the bath and kept for 15 min with continuous stirring. Procion Red M8B dye (4 %) and Glauber's sa lt (60 giL) were added to the above bath and kept for I h with stirring at 30°C. After this treatment, the sodium carbonate (20 gIL) was added in the same bath and kept for 45 min under the same condition. Thereafter. the samples were washed with cold water, soaped IND IAN J. FIBRE TEXT. RES., DECEMBER 2003 452 with Ultravon JU (2 gIL) for 15 min at boi l fo llowed by usual washing and drying in air. Re mazol Ye ll ow FG dye (4 %) and G lauber's salt (80 giL ) were added to the above bath and ke pt for 20 min w ith stirring at 30°C. After thi s treatment , the sodium hydrox ide (4 gIL) was added in the same bath and ke pt for 1 h under the same condition. Thereafter, the sa mples were washed with cold wate r, soaped w ith U ltravon JU (2 gIL) for 15 min at boil fo ll owed by usua l washing and drying in air. 2.3.2 A 1IIax> Reflectance and KIS Values Spectrascan-5100 (R) computer colour matc hing system was also used to measure A. max> re fl ectance and KIS va lues of different types of reacti ve dyed jute fib re samples using relevant softwares and following formula: K I S = l (J -R) 2 I 2R ] DC C where K is the coeffi c ie nt of absorption ; S. the coefficient of sca tte ring ; R, the re fl ecta nce of substrate at A. max; and C, the concentration of dye. T he K I S value is viewed as an index of d ye upt ake. 2.2.4.3 Pseudo Single-Bath Process using Spent Bleach Bath The liquor left out after ambient tempe rature bleaching, as described in sec tion 2.2.2, was re used fo r the preparation of second batch of the sa mpl e. Grey jute fibre intended for ambient temperature bleaching using spe nt liquor was dipped in the above liquor and squeezed to give 100% wet pick-up. The samples we re put in a plastic bag and ke pt for 2 h. The bleac hed fibre (without washing) ·was the n pu t in a sepa rate bath containing ten times its volume of wate r (M:L:: I: 10). Sodium hyd ros ul phite (2 gIL) was added to the bath and kept for 15 min with continuous stirring. The dyeing was carried out in the same way as me ntioned in sec tion 2.2.4.2. 2.3.3 Wash Fastness All the reac tive dyed jute fibre sa mpl es we re subjected to wash fastness tes ts in a launder-O-meter as per IS:3361-1979 (ref.6) . Wash fastness ratin gs of a ll the dyed jute fibre samples were eva lu ated w ith the help of computer colour matching system. 3 Resul ts and Discussion Table 1 shows that both the white ness and brightness indices are poor in case of grey jute fibre but after bleaching both the indices improve cons ide rably . There is a substa nti al dec rease in ye llowness index after bleaching. Co nve nti onal bleaching process prod uces bette r bleaching e ffect compa red to ambient te mpe rature bleach ing process. The whiteness a nd brightness ac hi eved after amb ien t te mperature bl eac hing are sa ti sfac tory enou gh fo r subsequent dyeing operation. Table 2 shows that the ambient temperature bl eac hed jute fibre produces higher KIS value as compared to conventiona l bleached jute fibre, indicating that the 2.3 Determination of Physico-chemical Propert ies 2.3.1 Whiteness, Yellowness and Brightness Indices Whiteness index (HUNTER sca le), ye llowness ind ex (ASTM D 1925 sca le) and bri ghtn ess index (TAPPI 45 sca le) of grey, conventional b leac hed and amb ien t te mpe rature bleac hed jute fibre samp les were mea sured by the Spectrascan-5100 (R) computer co lour matching syste m using re levant softwares. Table I Bleaching age nt uscd Bleach ing process Nil Hydrogen peroxide Nil Conventional Hydrogen peroxide Ambient temperatu re 76.27 Sample Grey Bl eached Bl eached Evaluati on of fibre quality Table 2 Parameter Wh iteness index (HUNTER) Yellowness index (ASTM 0 1925) Bright ness index (TA PPI45) 53 .99 46.21 23.96 83 17 18.82 64.59 2 1.9 1 53.99 Effect of different bleaching processes on dyeing behav iou r of jute fibre Procion Red M8B Ambie nt Conventional temperature bleaching bl eaching Remazol Yellow FG Conventional Amoi ent bleaching temperature bleaching A Illax , nm 550 550 420 420 Refl ectance 5.5 1 14. 14 13 .3 I KIS value 8. I I 3-4 4.93 9. 16 2.6 1 4 3-4 2.91 3-4 Wash fastness 453 CHATTOPADHYAY el at.: AMBIENT TEMPERATURE BLEACHING & REACT IVE DYEING OF JUTE colour yield is more in case of ambient temperature bleached jute fibre. This finding is true for both Procion Red M8B ( substitution type of reactive dye) and Remazol Yell ow FG ( addition type of reactive dye). The higher dye uptake may be due to the high alka line condition used during ambient temperature bleaching. Wash fastness property is found to be good in all the cases. In true single-bath process (Table 3), the colour yield is very poor when sodium hydrosu lphite is not added for counteracting the oxidising effect of hydrogen peroxide bleached bath and alka li is not added during the fixation stage of reactive dye. Some minor improvement in colour yield is observed when sodium hydrosulphite or alkali is added alone. But more improvement in colour yi e ld is observed whe n both sodium hydrosulphite and alkali are added in the bath . This finding is true for both the reactive dyes studied . In all the cases, the colour yield is very poor when true single-bath process is followed. Wash fastness of all the samp les is moderate. Low liquor ratio, high alkali concentration and very hi gh oxidising agent concentration may be respon s ibl e fo r poor colour yield. Hence, it was decided that the tru e single-bath process wi ll not serve the purpose and the idea of pseudo single-bath process was emerged . In pseudo single-bath process, as the fibre wa s not washed after bleaching, it carried a portion of excess alkali to the dye bath. So, alkali was not add ed in the bath during fixation stage of react ive dyes . The colour yield of dyed samples was found to be poo r in both types of p seudo single-bath processes. For the improvement in fixation of dyes, the alkali wa s added to the dye bath during fixation stage and the colour yield was found to be sati sfactory in all the cases whether it is pseudo sing le-bath process or pse ud o single-bath process using spent bleach bath (Table 4 ). To optimize the concentration of reducin g agenl after bleachin g both in case of pseudo sin gle-ba th process (Table 5) and pseudo single-bath process Table 3 - Effect of intermediate addition o f reducin g agent after bleaching and alkali during fixation stage of reacti ve d ye in g o n dyc ing behaviour o f jute fibre using true single-bath process at ambi ent temperature Addition of sodium hydrosulphite RFL - Addition of alkali A. ma" Procion Red MSB RFL KI S nm Wash fastness A IIll' Remazol Yell o w FG RFL KIS No No 550 37 .34 0.53 3 420 47 .39 0 .29 3-4 No Yes 550 33 .76 0 .65 2-3 420 43.47 0 .37 :1 Yes No 550 32 .SS 0.69 3 420 43.42 0 .3 7 2-3 Yes Yes 550 26.46 1.02 3-4 420 3 1.24 0 .76 3-4 Reflectance Table 4 - Effect of alkali during fixation stage of reactive dye in pse udo single- bath process and pseudo singlc-bath process usin g spent bleach bath at ambient tempcrature <- W a~h ras t nc s~ nm Parameter Pseudo sin gle-bath process Procion Remazol Yellow FG Red MSB With Without With Without alkali alkali alkali alkali Pscudo sin gle-bath process usi ng spent bleach hath Remazo l Procio n Red MSB Yellow FG With Withou t With Without alk ali alk ali alkali alk ali A max , nm 550 6.19 7. 11 550 S.44 4 .97 Rcl1 ectancc KIS 550 23 .S2 1.22 420 10.05 4 .02 420 27 .02 0.99 550 34 . 17 0 .63 420 420 13.07 2 .S9 4645 0 .3 1 Table 5 - Effect o f reducing agent after bleachin g on dyein g behav io ur o f reacti ve d yes using pseudo single-bath process at ambi ent temperature Parameter 0" A max' nln Refl ectance KIS a Sodium Procion Red MSB 2 .0" 3.0" Rcmazo l Yellow FG 2 .0" 3 .0" 5.0" 0" 550 420 420 420 420 5 .0" 550 550 550 23 .S2 12 . 11 6 . 19 6.97 34.42 2609 10.05 12. 13 1.22 3. 19 7. 11 6 .21 0.62 1.05 4 .02 3. IS hydrosulphite concentration in giL INDIAN 1. FIBR E TEXT. RES ., DECEMBER 2003 454 Table 6 - Effect of redu cing age nt after bleachi ng on dyeing behaviour of reactive dyes followin g pseudo single-bath process using spent bleach bath at ambie nt temperature Parameter Procion Red M8B 2.0" 1.5" 0" nm Re Oectance Am;.t.'(. KIS a 550 30.82 0.79 550 9.61 4.25 550 8.44 4.97 3.0" 0" 550 8.73 4 .76 420 43.44 0.37 Remazo l Yellow FG 2.0" 1.5" 420 14.24 2.58 3.0" 420 13.68 2.69 420 13.07 2.89 Sodium hydrosulphite co ncentration in giL Table 7 - Effect of differen t single-bath bleaching-dyeing processes at ambient temperature on colour yield usin g two reactive dyes Process A",,, nm True single- bath process Pseudo single-bath process Pseudo single-bath process using spent bleach bath Procion Red M8B KIS RFL fastness Wash A max nm Remazol Yell ow FG RFL KIS Wash fastness 550 26.46 1.02 4 420 31 .24 0.76 3-4 550 6.19 7.11 4 420 10.05 4.02 4 550 8.44 4.97 3-4 420 13.07 2.89 3-4 uSing spent bleach bath (Table 6), different concentrations of sodium hydrosulphite (0,1.5, 2.0, 3.0 , and 5.0 gIL) were used. The colour yield increased with the increase in sodium hydrosulphite concentration up to 3 giL in pseudo single-bath process and up to 2 gIL in pseudo single-bath process using spent bleach bath . Thereafter, a decreasing trend in co lour yie ld was observed . Sodium hydrosulphite reacts with the active hydrogen peroxide remaining ins ide the fibre and in the bath up to the optimized concentration . The higher concentration, than the optimized one, acts on the dyestuff in addition to its action with oxidising agent , thereby reducing the colour yield. Dye ing properties of jute fibre dyed with Procion Red M8B and Remazol Yellow FG at optimized condition using different processes are given in Table 7. It is evident that the colour yield is maximum in case of pseudo single-bath process and minimum in case of true single-bath process . By comparing the colour yie ld s from Table 2 and Table 7 , it is revealed that the pseudo single-bath process is well comparable with the conventional two-step process using ambient temperature bleaching and cold reactive dyeing. Pse udo single-bath process using spent bleach liquor produces higher colour yield than that produced by true sing le-bath process but lower than that produced by pseudo single-bath process. 4 Conclusions 4.1 Whiteness index produced by ambient te mpera- ture process is slightly lower than th at produced by conventional hot bleaching process . The whiten ess and brightness achieved after ambient temperature bleaching is satisfactory enough for subseq uent dyeing operation. 4.2 Dyeing of ambient temperature bleached jute fibre produces higher colour yield as compared to conventional bleached jute fibre. This finding is true for both Procion Red M8B (substitution type) and Remazol Yellow FG (addition type) dyes. High alkaline condition during ambient temperature bleaching results in swelling of fibre which ult imately g ives better colour yield. 4.3 In true single-bath process , the addition of redu cing agent (sodium hydrosulphite) after bleaching and that of alkali during fixation stage is must. But the colour yield is very poor when true si ngle-bath process is followed for ambient temperature bleaching and cold reactive dyeing. Low liquor ratio, high alka li concentration and very high oxidizing agent concentration may be responsible for poor colour yield. So. the true single-bath process was not found to serve the purpose and the idea of pseudo single-bath process was emerged. 4.4 In pseudo sing le-bath process, the addi ti on of 3 gIL sodium hydrosulphite after bleaching and the .. CHATTOPADHYAY el 455 al.: AM BIENT TEMPERATURE BLEACHING & REACTIVE DYEI NG OF JUTE required amount of alkali for fixation of reactive dye is must. Colour yield produced by pseudo single-bath process is well comparable with that produced by conventional two-step process using ambient temperature bleac hing and cold reactive dyeing. 4.5 Pseudo single-bath process using spent bleach bath produced higher colour yield than that produced by true single-bath process but it is lower than that produced by pseudo single-bath process. In this case, the optimized concentration of sodium hydrosulphite is 2 giL to achieve maximum colour yield. As the spent bleach bath can be reused , thi s process becomes simple and economic with minimum effluent disposal problem as after spent liquor bleaching there is hardl y any liquor left out in the bath for disposa l. 4.6 Wash fastness ratings are sati sfactory In a ll the processes . References I Pandey S N, Chattopadh yay S N & Bas u G. Indian .I Fibre Text Res, 20 ( 1995) 102. 2 Basu G & Chattopadhyay S N, Indian J Fibre TexT Res. 2 1 ( 1996) 2 17. 3 Chattopadhyay S N , Pan N C & Day A. TexT Trends. XLlII(200 I) 23. 4 Pan N C. Chattopadhyay S N & Day A. TeXT Asia. XXXII (2001 ) 40. 5 Pan N C, Chattopadhyay S N & Day A, TexT Ind Trade .I. 39(200 I )37. 6 IS: 3361-1979, lSI Handbook oj TeXTile TeSTing ( Bureau of Indi an Standards, New Delhi ), 1982.
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