Indian Journal of Fibre & Textile Resea rch Vol. 21, March 1996, pp. 79~89 Recent advances in the development of silk-like polyester fabrics Pushpa Bajaj Department of Textile Technology, Indian In stitute of Technology, New Delhi 110016, India Silk-like po lyes ter fibres ha ve been one of the most important targets for the textile industry in the present era. Key technologies starting from fibre engineering to finishing process have been illustrated for producing silky polyester fabric s with bulk y hand touch and superior drape. Effects of polymer additives, delustrant s, surfact a nt s, e tc. on a lkaline hydro lysis of polyester fabrics for improving silk-like characteristics have a lso been highl ighted. Keywords: Alkaline hydrol ysis, Bicomponent fibres , Micro-crator pol yes ter, Microfibrcs. Shingosen, Silk-like pol yes ter. Spinning tec hn o fogies by simulating the characteristic features of silk fibre , I Introduction Polyester fibre has conquered the leading position VIZ. • The design of cross-sectional shape, among the three major synthetics because of its • Enhancement of drape characteristics through excellent properties such as high strength, abrasion resistance, wash and wear, and wrinkle-free weight reduction of conventional pol yes ter fibres or by the development offine denier fibres. characteristics. However, polyester does have some and deficiencies, i.e. it is hydrophobic and oleophilic. Due to this, 1t is easily soiled and accumulates the static • Creation of moderate bulk and soft handle. History of the progress made in silk-like pol yester charge. Oily stains are also difficult to remove . Polyester fabrics are, therefore, not as comfortable as fibres is given in Table I and the technologies natural fibre fabrics. developed for the production of Shin-Go sen (Shin = On the basis of consumers' comments, Latta I has new & Gosen = synthetic fibre) in Japan are . also mentioned the following limitations of illustrated in Fig.l . synthetics: In this review, the va rious processes developed for • Unnatural hand and unfamiliar skin cqntact sensations, Table I- Histpry of the progress of silk-like polyester fibres9 • Unpleasant thermal sensations, Generation Properties Idea of technology • Lack of moisture absorbancy, Brightness • Clamminess of fabric in contact with skin, and Copy of natural Lustre Drape Shape of cross-section silk • Static related problems. To overcome some of these problems, blending with natural fibres, particularly cotton, gained a big market. An extensive work related primarily to polyester fabrics comfort has been published in excellent reviews 2 - 6 in the recent past. From the wearer trials using knit fabrics it was reported that the comfort of polyester was substantially improved by cross-section variations, pressure jet treatments and certain engineering modifications of the ·polyester. The Japanese industry has also made great strides in improving the comfort and aesthetic properties of I "Sh'mgosen " h as b een po Iyester. S I'lk - I'k I e po yester developed by different technologies? Various approaches have been tried to develop silky polyester (trilobal, triangle) ( 1964-) Rustle of clothes Copy of silk touch (1975-) Fullness and softness Shrinkage-mix fibres Drape Structure of crimps Delicacy Persuit for the aesthetic properties (1979-) Persuit for micro shape of cross-section (1983-) Silky-spun like Naturality Dry touch Air texturing False twisting Thick and thin ya rns Lustre Fullness and softness Drape Rustle of clothes Naturality Tri-petal like crosssection Microfibres Cross-sectional shape Very nice ta ilored Aim for high sense and quality fini sh characteristics (1988-) Liveliness Development of new polymer 80 INDIAN J. FIBRE TEXT. RES., MARCH 1996 Shrinkag~-mix filam~nt - - - - i High shrinkage yarn t - - - { Difference in fibre length High spQed spinning yarn Spontaneous extension Polymer modification ------I Polymer with partic~s from catalyst residue Polym~r with added particles Brightness '"r---Fullness and softn~ss . )----.Lu~e r:s-ur--:f:-a-ce-ro-u-g-:-hn-e-s.... s\.--L- Dee p co 10 ur Vi vid colour Dry hand Special spinning - - - - - - - 1 Denier mix Non-circul~r crosssection Conjugated yarn I ' - - - { Shape of (ross - ' f f - - - Soft hand He<lvy denier Fine dQnier I-----{ section Rustle of (Iothes Difference of denier 'c---\-- Spread anti-drap! Texturing - - - - - - - - - - 1 False twisting Air tuturing 1----;rr;(o~m;;;m;;ii~ng~l;in;;;g-:-·-~~r\--~ Naturality Afttr treatment - - - - - - - 1 Twisting (austic reduction After finish Fabric density l---'~S;;tr~u::-ct:tu:r:e--:of;-""""":----+-~S t iff ness dagree fabrics Springy properties Drape Fig. I- Fabric properties of Shingosen and key technologies 51 L~ SI LOOK ROYAL I I 1 fI 1\ ..... 1...- \I / " o SILK I" / '" -- I \../ \V 1/ 10 20 30 0 10 20 30 0 10 20 30 Tim~Jms fr----o A-Sompl, 'tobric I B- '" ie rophont c- W, ight , SOOt 14 em I 0-"'0_ '1Oem Imin I Fig. 2- Wave of ru stli ng sound of three typical fabrics the production of silk-like polyester have been highlighted . Special emphasis has been made on the saponification or caustic reduction treatments for prod ucing si lk-like polyester fabrics . 2 Cross-sectional Shape 7 The shape of a silk fibre after removing se ricine during scouring is triangular. For imitating the triangular shape of silk fibres, polyester fibres ha ve <) been developed with triangular or trilobal cross-sections. This resulted in lustrous polyester fibres. The appearance also changed from that of plastic to a silk eq ui valent. PET fibres with a tripetal cross-section have also been developed to provide silky look . There is a groove at the tip of each lobe oftrilobal cross-section. This unique cross-section is believed to bring the rustling so und to polyester fabrics when friction occurs among them. The wave of rustling sound of three typical fabrics has been compared (Fig.2) . 'Sillook Royal' has, therefore, not only the lustre of natural silk, but also a rustling sound similar to that of the natural sil k. Polyester fibres wit h petal-like cross-sectio ns ha ve been produced by conjugate spin ning technologylo. In this process, small a mounts of easily hydro lysable components are located at the tips of each lobe. During saponification or ca ustic trea tment, this component gets dissolved and grooves a re formed. The width and depth of each groove can be controlled at the sub micron level. 3 Differential Shrinkage Polyester Yarn One o f the techno logies to bring out silk-like bulk and handle in PET is to use differenti a l shrinkage polyester component yarn. T wo method s have been tried to produce different shrinkage levels in mixed BAJAJ: SILK-LIKE POLYESTER FABRICS yarns. One is a parallel sort of mixture, just like Quiana (nylon ya rn produced by Du Pont) and the other is a se rial kind (Fig. 3). The parallel structure is made by mixing fibres of different shrinkage levels either by using different polymer fibres or by mixing fibres of polyester drawn at different temperatures. The serial type is produced by random heat setting along individual fibres during fibre processing 1 I . The fibres shrink randomly with TYPE PARALLEL Mi Xlld Yarn of I'ETHOO D~rmt Shrinkage Lt'it I SERIAL Rnndom Hrat- set AmollJ Individual Fibre .. _........................................ ... ...... YARN I--------:--+------:::---~ .~. '"'-./ .... ..../V..... --v-..... J"'v... _. ~ ....... "'-." ..... ~ ""'" 81 the heat treatment. In the parallel structure, higher shrinkage components form a core, and lower shrinkage components form waves or loops around the core. On the other hand , in the serial type structure, higher and lower shrinkage parts are di stributed randomy in the yarn and there is no core (Fig.3). The resulting fabric from serial type arrangement of different shrinkage level fibres showed a more natural silk look than the parallel type. Uchida 12 has also demonstrated the role of shrinkage in producing Shingosen. Fukuhara 7 from Toray Industries has shown that for the production pf Shingosen, initially dry heat shrink process was tried and later the wet-heat shrink process. But, a double shr'unk fabric appears to be closest to silky textiles (Fig. 4). It has comparatively hi'gher bulkiness and is more airy and soft. Sillook Sildew, produced recently, is a double shrunk fabric with large waves or loops on the surface of the fabric. For making double shrinkage fibres, the researchers have to first design the polymers by selecting a suitable comonomer and its content for accomplishing the desired shrinkage level. Degree of polymerization (DP) should also be controlled as a polymer with higher DP is likely to provide higher shrinkage. Parallel yarn str ucture After screening the polymer with a desired composition and DP, the fibres can be made from two , or more polymer components by the same spinneret from different nozzles. This kind of conjugate spinning provides fibres with in situ differential shrinkage. So, additional step for mixing fibres as discussed earlier is not required and the resulting Strial yarn structure mixture directly produced from spinning line is Fig. 3- Two kinds of shrinkage. Parallel a nd seri al ya rn uniform. structures ~I Double shrin k type ----,.......... I ____~D_r_y_-_he_a_t_s_h_ri~nk~tY_p_e ~ ~~ Grey fabric Fig, 4 '----- __ ~_~ 1st 2nd Final hQat-set ntat-set heat-~t scouring caustic dyeing reduction Shrinkage d'iagram of polyest .r fab ri c after caustic treatment 4 Topical Finishes Finishes also modify the tactile, static and moisture related properties of polyester fabrics. The enhancement of polyester properties by treatment with aqueous sodium hydroxide was recognized soon after the invention of polyester 13 . Treatment of untextured yarn fabric with alkali produces softer tactility with a less synthetic hand . A calendar, heat-set' and caustic soda saponified fabric was patented a few.years later as the treatment was said to produce high fabric lusture without paper-like , handle l4 . Polyester undergoes nucleophilic substitution and is hydrolyzed by aqueous sodium hydroxide . The hydroxyl ions attack the electron-deficient carbonyl carbons of the polyester to form an intermediate anion, 82 rNDiAN 1. FIBRE TEXT. RES., MARCH 1996 Table 2- Summary of alkalization processes SI.No . Materials 2 3 Formulations Conditions Remarks Po lyeste r fa bric 0.3% NaOH in ethano l 50% pick up and stored Weight loss 2 1% Po lyes ter fabric Kodel IV drawn P ET fibre & hea t-set 6% NaOH in 5% ethano l -do- -do- 5- 15% sodium hydroxide lOOT, I h 90 e Weight loss 12-43 % OH < t-but ox id e < sec. pro pox id e < methoxide < ethoxide Wei ght loss 12. 15-29.7 % 4 Terene fibres 1. 5 in . sta ple le ngth 5- 15% 5 Trevi ra fabric Batch: 1.5-2 % NaOH 0.2% di spersing agent H .T. beam: 0.05 % accelerator Pad-ba tch: 19% NaOH 0.2% wetting agent C ontinuo us: 19% NaOH 0 .2% accelerator 90 g/m2 aOH 0 I h I lOT, 20 min Weight loss 18% R.T. fo r 24 hr batching 120 e I min Silk-like handle Silk-like fini sh More unce rtain 16-20% weight loss Weight loss, % 17.5 20.1 21 .9 24.4 Wei ght loss 15 °;.) Silk:like effec t 0 6 Textured P ET fi la ment l. 87 oz!ya rn Celenese Fortrel 73 1 15% NaOH 0.56 o r 0.87 % quate rnary Lauryl dimethyl ben zyl a moniull1 chloride Bath ratio 10: 1 30-60 min 60 min 30 min 60 min 7 Po lyes ter 3% NaOH 95°C 8 100 % Dacron P ET fa bri c 10% w e 9 Li ght weight PET '68.5 g/m 2 Po lyeste r 4 % aO H 4% NaOH + I % accele ra to r WY., Na O H 90T. 60 m in M:L: : 1:60 lOOT. 15 min II Po lyester c re pe 100 g/m 2 10% NaOH n. 1% s url~l c tant IJOT M : L::1: 30 12 13 Pol yes ter Po lyes te r 14 Polyester textured yarn Polyester textured fabric Polyester Polyester yarn PET fibre , fabric 10 15 16 17 18 PET & POY fibre s Heat-set delustred PET fabric aO H 120min 30T 70T Weig ht loss 21-23 % aft e r 60 min 20% afte r 15 min Strength loss 10-70% warp WI. loss of tex t > flat > spun yarn Weight loss STEG > SD EG > SEG Fle x. rigidit y STEG < SDEG < SEG Weight loss 41 % Weight loss 27 % Weight loss 26 .8% Weight loss 18-25 % Weight loss 23 % 15 % 90T. I h Weight loss 20-80% 60T 0-70 h Weight loss 0-90% Pad-ba tch Sodium tri eth ylene gl ycolate (STEG» Sodium d ie th ylene gl yco late (SDEG ) > Sodium e th ylene gl yco late (SEG) 3-5 % NaOH 5% NaOH 7. 5% Meth o no lic NaOH 10 % NaOH 15 % Hydrazin hydrade or ethylene diamine M:L: : I :20 10% NaOH M :L:: I: 150 2-8 mol NaOH I % cet yl trimethy l ammonium bromide ( 1% w / w) Weig ht loss 10. 1% Stre ngth loss 29'10 Weight loss 10.5-1 7.0 % Stre ngth loss 25% Weight loss 13.74-14 . 11 % 93-1 2 1°e Ih 104T,. 1 h 2 1°C, I h 59T, 1-6 h BAJAJ: SILK-LIKE POLYESTER FABRICS Chain scission follows and results in the production of hydroxyl a nd carboxylate end-gro ups. 83 Table 3- Properties of polyester sa mples sapon ified pad -steam techniques [Ca ust ic cone .. 150 gi L; Steaming temp ., 102°C] Sample No . Time of .steaming (min) Weight loss (%) Flexural ri gidity (mg. em) 5 10 15 20 12.3 15.7 18.6 2 1.1 24.77 11.99 9.28 8.39 6.55 I 2 3 4 5 by Strength loss (%) 7.3 15.8 17. 1 26.2 The effect of ca ustic solution on a PET fabric depends on the following parameters 15 - 19: • Concentration of a lk a li , • Time and temperature of alka li treatment, • Use of surfactants, 40r------------------------------, • Fibre type (composition and cross-section), and o~ • Heat se tting. - 30 The fibre loses weight as the reaction occurs. Over a \II \II wide range of temperature, the relatio n between o weight loss and time or sq uare root of residual weight ~ 20 and time has been found to be linear provided that a large exee ,; of alka li is used so that the reagent is not large ly comumed during the treatment time. If an excess oT alkali is not used and its concentration decreases as the reaction continues, then the weight loss/time relation becomes exponential. Various conditions used for saponification and the weight Treatment Time (h) reduction for polyester fabrics with aq ueous sodium Fig. 5Rdationship between weight loss and treatment time for hydroxide are listed in Table 2. It has been concluded polyester fabric treated with aqueous ca ustic soda [( +) regular that the influence of temperature on the rate of the polyester, (0) regular pol yester havi ng CTAM, ( x ) AMPET reaction is greater than that of concentration of alka li, substituted for regular polyester) which, in turn , is greater than that of time. Use of quaternary ammonium salts as accelerators for saponification has also been recommended 6.20.2 1. In presence ofCEMDA and CTAM, weight loss of Samples hydrolyzed using 10% aqueous sodi um 24% co uld be achieved on ly in 40 min at 130°C. hyd roxide a t 60°C showed linear relationship Correlation between weight loss, strength loss a nd between the weight loss and the alkali treatment time flexural rigidity (Table 3) points out that the silk-like (Fig. 5). Further, the addition of a cationic surfactant, soft handle of polyester can be realised 22 when the namely certrimmonium bromide (cetyl ammonium fabric loses a weight of about 16% and the flexura l bromide) CTAM, or the replacement of PET with an rigidity reduces to about 9 mg. cm by trea ting with anionically modified polyester (AMPET) increases 15% NaOH at 130°C. the rate of saponi fication considerably. G awish and End group analysis of saponified polyester coworkers 21 have shown that the rate of hydrolysis of indicates that with increasing weight loss of polyester crqe fabric in \0 % NaOH (owl) at 130°C saponified polyester, the number of end groups of was vcry slow and it required six hours to the [COOH] increased and a valu e of 47.10 theoretical weight loss of 24%. However, with the equivalents/10 6g was achieved at 2 1% weight loss addition of different quaternary ammonium (Fig.6). The number for control being 32.8 surfactants as accelerators, the rate of hydrolysis equivalents/ I 06 g. The increased number of [COO H) co ul d be enhanced significantly. The activity of the end groups after the saponification suggests that the quaternary a mmonium surfactants was in the reaction of a lk a li wi th polyester is of hydrolysis with scission of polyester chain molecules, resulting in following order: Cetyl ethyl methacrylate dimethyl ammoni um more number of [COO H) end groups, and confirms bromide (CEMDA) > cetyl trimethyl ammonium the mechanism of hydrolysis as shown earlier. bromide (CT AM) < oleyl bis-(2-hydroxylethyl)The data on sa ponified polyester indicates that both the acc umula ted charge (acceptance potential ) cetyl ammonium bromide. 84 IN DI A N 1. F IBR E TEXT. R ES., MA RC H 1996 Tah k 4 48 250 Sa mple No. 46 CII 200 ., c: o ">" 90 3 5. 24 160 240 .. 4 13.5 1 11 5 ;J 5 25 .1 4 90 10 e 40 '" . '0 c: 38~ c: 0 0 E W . L....J Cl. 36 ~ u -< ci z 50 34 °0~------~----~12~----~18~----~~ 24 0.31 200 30 2U u 0. 29 (5) 190 Cl. .. 100 I (V) 1.6 1 Cl. I (% ) II 2 I 42 "'. - o Accepta nce po ten tia l 2 CII ~150 Weight loss 44CDO ;J > Eifec i ofs url;lce sapo ni fica ti o n o n elect ri c cond uct ivit: of po lyes ter sam pl es Weig~t Loss 0.33 Mo isture (~o I I 0. 35 0. 37 32 I Regain, 'I, Tab le 5- Fi ni s hin g stages of po lyes te r fibre fa brics 15 Sa m ple A Sa m ple B Loo m sta te Loom Relaxa ti o n in washer ( I lOT. 20 min) Relaxa tion in jet d ye ing ( I l OT. 20 min) Hea t-se tti ng in hea tsett ing un it ( 190' C 20 s) Weigh t reduction ( 16'Yo in 40 gi L NaO H ) Hea t-sett ing Weigh t red uctio n (25 % in 40 gi L NaO H ) Dye in g in jet dye ing mac hine (no'c. 30 min) D yei ng in jet dyein g mac hine (130'C. 30 min ) Raising Ra isi ng SI a te ( 190' C 205) Fig. 6--Co rrelations betwee n .weigh t loss. [COO H] end gro u ps and acceptance pote nti a l in saponified po lyes ter and 11 /2 (the time fo r ha lf the accumul ated charge to decay) reduce with increasing we ight l oss~ The va lue of acceptance potentia l red uced from 200 V fo r control sa mple to 90 V for the saponified sa mple (25% weight loss) and the di ssipati on time 11 /2 reduced fro m 240 s to lOs. The data also show that up to about 13% we ight loss the acce pta nce potenti a l dec reased rapidl y to 11 5 V and with furth er increase in we ight loss to 25%, it dropped slowly to 90 V (Ta ble 4). The reducti on in stati c charge acc umul ati on of the alk ali-t rea ted polyes ter may be attributed to th e surface saponi fica ti on of polyester as indica ted by the inc reased nu mbe r of hyd rophili c [COO H] and O H end gro ups, wick ing a nd , to a limited ex tent , th e moisture rega in . T he effect of th e ca usti c solutio n on a po lyester fa bric depe nds a lso o n th e fi bre type, fa bric co nstructi on, and hea t-settin g conditi o ns. Bright fi bres with rou nd cross-section lose we ight slowly th an de lustred fib res with mult ilobal cross-sectio n. Reaso ns fo r thi s di ffe rence in the rate of weight loss co uld be d ue to the fo llowi ng: • For a give n linea r densit y, a multil obal fib re wo uld have a large surface area th an a ro un d fi bre. • The prese nce of de lustrant may acce lerate th e we ight loss of the fib re 23 . 24 . • For peach like effect. hi gh solubility polymers or ino rga ni c pa rticles are inco rpora ted in PET melt, which esse nti all y solubilize or leac h out to give pit effect on surface, thereby affec tin g th e feel and hand le of th e fa bric. Thi s radi ca l alterati on in the surface has bee n ensued by Japanese to prepare dry touch ya rn . Microcraters res ult in low convex-co ncave co nfig urati on. • Samples ap pea r to lose we ight fas ter after tex turin g. Fo r exa mple, th e losses in weight of non-tex tured ya rn and tex tured ya rn when treated with 5% ca ustic soda at 104°C for I h were 36% anri 41 % respectively. Ma tsud aira a nd Matsui 25 have al so studied the effect of various fi nishing stages after the loom state on th e fa bric handl e. The di ffe rence betwee n sa mples A and B is in the stage of relaxi ng and we ight reducti on (Table 5). The effect of relaxing in a washer is expected to be greater than that in ajet dyeing machine. Overall, th e polyes ter fi bre fa bric is remark a bl y softe ned and fa bric hand le by re laxa ti on, whi ch includes desizi ng, ~h rin k i n g of fibres, and relax ing of in te rn al residual stress. Subseq uent we ight reducti on d ue to alka li produces "efrecti ve ga p" betwee n the fi bres/o r ya rn s and th e splitting of fi bres. T be minimum amount of weight red ucti on necessary to split fi bres is ex pected to be a pp rox. 10%. By using di scrimi na nt a nalysis 85 BAJAJ: SILK-LIKE POLYESTER FABRICS with the primary hand values as variables, a distinctive zone for silk-like and peach-skin type polyester fabric can be found. Sodium hydroxide treatment reduces electrostatic charge generation from 280 V to 100 V and the halflife from 5 to 2.5 s. Sol brig and Obendorf2 6 have reported the considerable weight loss after sapon ifying polyester fibre containi ng 2% Ti0 2 (Fig.7) and the pitting on the surface, obsefved through SEM, mainly axiall y oriented a long the fibre surface. Treating polyester fibre with 10% aq. NaOH at 100°C (by steaming) for 45 min produced hygroscopic polyester fibre. In another study, a wide range of particles have been used for creating microvoids on the fibre surface. A common method is to remove microparticles blended in the polyester polymer by a lka li treatment. By applying this method to vario us polyester fibres containing differt'nt types of particles, fibres with vario us patterns of voids on surface are obtained. Originally, this modification was carried out to give depth of colour. 30 Dull 25 Bright Serri().jll ~ 0 - 20 Clear '"'" .3 15 ..... ~ .~ '" ~ 10 5 OE-__L -_ _L -_ _L -_ _ ~ _ _ ~ _ _ ~_ _ _ _ ~ Treatment Time Fig. 7-Change in weight of clear. bright. semi-dull ai1d dull PET yarns over 6 h of treatment with \0 % NaOH solution A method of forming a controlled microcrater on the fibre surface is proposed. The fibre pretreated by a ;pecific resist is exposed to a laser beam and then treated again with chemicals. This process can control the dimensions of voids such as depth , length and height, and their density. A blend containing PET and 4% BaS04 (~ 2%, av o jiam. :::; 9 /-1m) was melt sp un at 1800 m/min to give 290% elongation at Kuraray Co. The fibre wa~ used as sheath and later on textured by Taslan process and causticized to give 30% weight loss. For improved lustre, polyester fibres containing :::; 0.04% inorganic oxide particles and having birefringence 0.03-0.08 were draw twisted for ~ 0.15 s at 130-170° and then untwi sted to give textured yarn with very good lustre 2 7 . The effect of BaS04 on the extent of saponification has a lso been studied in o ur laboratories 28 . As the treatment time and concentration of NaOH progressively increased from I to 2 h and from 5 to 10% respectively , the loss in weight of the polyester fibre increased from 3.03% (Po, 5% NaOH , I h) to 15.2% (Po, 10 % NaOH , 2 h) at 90°C bath temperature. It can be seen from Table 6 that PoSi loses more weight over Po or P oSiF 5. This is perhaps due to th e formation of sodium si licate in the presence of a lk ali. due to si li cone oil coati ng on PET, which see ms to acce lerate the sapon ificat ion process. The reduction in diam.is a lso maximum in PllSi fibres. After hydrolysis, elongated pits, o ri ented in the direction of the fibre ax is, on the surface of PllSi F " sample were noticed . However. unfilled fibres did not show a ny pits. It was found that the size of the pits depended on the length of expowre to alk ali, while the number of pits depended on the concentration of BaS04 in the fibre (Fig.8). As the treatment time and a lk a li concentration increased from I to 2 h and 5 to 10% respectively, the pits en larged mainly in the fibre axis direction. Longer treatment increased th e size of the pits without changi ng their numbers. H ydro lyt ic Table 6-Change in weight and diameter of BaSO.-filled polyester fibres after saponification 5% NaOH Sample \0% NaOH 2h I h Wt loss % Ih Diameter Wt loss Diameter ~m % ~m 39.4 3.03 Po 6.4 . 38.6 PoSi · 4.{)5 39.1 PoSiF s Diameter of Po (unsaponified). 40 ~m; PoSi - 38.9 5.0 38 .3 8.3 5.52 38.8 silane coated; PoSiF s - Wt loss % 2h Diameter Wt loss ~m '1. ~m 15.2 22.2 18.8 36.8 35 .2 36.04 8.4 38.2 13.4 37.22 10.5 37.94 5% BaS04-filled PET Diameter 00 0'1 z o ); z ;- ::!l 0:1 " tTl rri >< :-i fii y') !: » ":t (j '"'" 0\ Fig. 8- SEM of saponified BaSO"-fi lled PET [( a) No rm al PET, (b) PET fill eu wilh 5% B"SO", (e) PET tilled wilh to'Yt, B"SO", (d) Saponified norma l PET. (e) Saponified PET ti lled wi th SU!c, 8:ISO", alld (n Saponified PET fi lled with IO'y', 13aSO"1 87 BAJAJ : SILK-LIKE POLYESTER FA BRICS Table 7- Te nsile properti es of sa ponified po lyeste r fibres [NaOH conc .. 5% ] Treatment time Sample code I h Tenacity cN /tex 2h Strength r<: tenti on % Brea king elongati o n % M odulu s N ' tex P" P"Si 38 96.5 21 10 34 87. 1 IH 8.3 P"SiF, 36 97.0 18 11. 2 degrada ti on of the polyester begins a t the surface o f the fibre an d continues until a BaS04 particle is exposed (Fig.8). Pits appear to develop from preferential hydrol ysis of polymer aro und the fill er particle, locations where alkali can diffuse more easil y due to hyd rophilic nature of the fill er. Thi s action leaves an axially-oriented elli ptica l voi d around the filler particle, forming an entry point for the alkaline solution to attack polymer beneath the original surface. Possibl y, the drawin g process used in th e production of fibres ca uses the pi ts to be ellip tical. Strength ret ent ion Te nacity eN / tex 36.3 29 .5 35. 1 19 9.5 75. 6 14 7.8 94 ..8 17 10.6 .5:.'../:, POlyester..q;~t.". . :rf~(/" J. • .., .h • ..,ft:· .• { . .l "'f' ..... ,f /- ct> 'i" :J!.t!Jzo Sil ica ~.i"'~ f R','N' New $;Jji.~ ~("~ The effect of silica particles on the lustre and handle of po lyester fibres after saponification has a lso been st udied by Yamaguchi 29. The fine concave and convex structure is formed by a difference in solubility in alk al i between the pol yeste r and the particles uniformly dispe rsed in polyester. For making a fine concave and convex st ructure of a specific size, firstly ultrafine particles, which have a-similar refraction rate to fibrcs and an average di ameter below 100 nm . are uniforml y di spersed in polyester fibre wi th out co hesion. Silica has a tendency to cohesion by hydrogen bond of silica surface. So , silica in water is stabilized by Na + cation as silica solution. To prevent silica particles cohesion or agglomeration , silica sol is mixed with et hylene glycol and particles are stabili zed and PET is mad e by direct estc rifica ti on method. 92.1 '~': ~. 5 Te nsile Properties The tenacity, breaking elonga ti on a nd initial modulus decrease wi th the increase in weight loss due to sa ponification (Table 7). Tensi le strength retention in Po fibres is 92% and 73.6% at 5% and 15.2% weight loss res pectivel y. However, under the same condition s of treatment the percentage strength retenti on for P"SiF 5 samples is slig htl y better, i.e. 94.8% and 75.4% at 5.5 % and 18.8% weight loss due to sa ponification . Modulus N/tex % Brea king elongation ala surface Alkaline treatment Fig. 9- Pieture of the fine concave a nd convex mechanism after alkaline treatment Sol-dispe rsed silica as selected particles P ro[)enics Silica So lubilit y rati o a gainst alkali 80 Index of refract ion 1.55 Oi <l me te r( pill) 0.05 Pol yester 1.62 10 ~ 10 The fibre s containing silica are treated with an etc hi ng meth od using alkali . Their surfaces are peeled ofr. Silica's solubili ty ratio against alkali is so ra pid that a fin e concave and convex structure is formed (Fig.9). Kurara y Company ha s dcveloped this fibre as the super microcrator polyester fibre '-' SN 2000" . Fig.1 0 shows the relation between fibre surface area (BET method) and alk aline weight reduction . The effect of microcrator due to alkali treatment o n the depth of black colour has also been shown. So, at high alkaline weight reduction , polyester fibre of fine surface provides not only a deeper colour shade but an improvement in lustre and ha ndl e of the fabrics . Toray Industr ies 30 prepared polyester fibres with mild silk-like luster by polycondensing glyco l slu rries co ntainin g particles with (RI 1.3-2.0) and average 88 - INDIAN J.FIBRE TEXT. RES., MARCH 1996 . 1.2 r-- - -- - - -- - -- - - - - - , 1 5 . ...'" Table 8- Moisture regain , st rength retention and the durability to washing of the chitosan-treated fabrics 33 ~~-.--------r_ Micro-crater polyu.ter Fabric E -0 0 .c; Add-on (%) 1. 0 16 E'" >.... co '"'" OJ d ~ .q: 17 0·8 d QI u ..&-._ ._ ._ . - - 0 d ~ ::> Vl c: -'" u -..vt- .-:: ...a.-r ..&. .............. __ ----------r J. co Untreated Chitosan-treated without curing Chitosan-trea ted with c uring" 6.6 15.3 6.4 16.7 Moisture Strengt~ Durability to regain retenti on washing (%) (°lc,) (weight remained, % ) 0.4 I.7 2.4 1.6 2.4 100 75.6 87.6 138.0 150.0 2.5 2.3 95.0 84.4 Alkali trea tment: 10% Sodium hyd roxide, 90 min, 60' C C uring condition: 130' C, 90 min Regular polyesf~r Alkaline Weight Reduction (%) Fig. I O-Relationships between the surface area, blackness and a lkaline weight reduction (Black dyed Georgette fabric) primary particle diam.45 J.1m and average secondary particle ciiam.350 J.1m with polyacids to form PET, melt-spun and drawn to give trilobal fibres with silica content of 0.01-0.4% . For rapidly hydrolyzable PET fibres , melt blending of PET with 2-10% sulfo containing aromatic diol(l) was carried out by Teijin Ltd 3J . H-t 0 C2H4)mO ----@{-OC C2H4 0 (I) ~H S03 M . application and the nature of amine. Amide formation results in chain scission. Amines were found to reac t and attack amorphous as well as crystalline regions. It appears, according to Zironian, that the weight loss/time curves are affected by the fine structure of the polymer and the location of attack. 7 Aftereffects o Deterioration in tensile properties o Broadens dye class for PET o Improved wettability o Oily soi l release improved o Good antistatic property o Increased moisture regain o Cracks developed on fibre surface o Brittleness increased o Flex life decreased o Shift in endothermic melting peak to lower temperature o Improved pilling resistance. References A woven fabric of the fibre showed weight reduction rate of 41 % / h in boiling aqueous NaOH. Ester Co. Ltd has developed polyester fibre with superior softness and gloss by dispersing 0.5-20% EPR in PET fibre. M~lt kneading was carried out and then spun into fibre 32 • Matsukawa et al. 33 have shown the recovery in tensile strength of alkali-treated polyester fabrics by subsequent treatment with chitosan (Table 8). The chitosan was fixed to the surface of saponified PET hy the reaction of the carboxyl groups .arid the amino groups of the chitosan molecu·les. 6 Weight Reduction by Amines 1s The reaction is similar to that by NaOH . The location of attack varies and depends on the mode of I Latta B M, Clothing com/ ort : . Interaction of thermal. ventilation . construction and assessment faClors (Ann Arbor Science, Ann Arbor, Michigan, USA), 1977, .33-35 . 2 Slator K , Text Prog . 9(4) (1977). 3 Yoon H N & Buckley A , Text Res l. 54 (1984) 289. 4 Yoon H, Sawyer LC& BuckleyA, Text Res l . 54(1984)357. 5 Zeronian S H & Collins M J, Text Chern C%r . 20(4) (1988) 25 . 6 Matsumoto M, Indian Text l . (Jan. 1991) 'J4 . 7 Fukuhara M, Text Res l . 63(7) (1993) 387. R Wada 0 , 1 Text Inst . R3 (1992) 322. 9 Sato M, Takakashi H, Sato Y, Sasaki H & Na beshiwa K, Proc. ISF'94 . (The Society of Fibre Science & Technology, Yokohama, Japan), 1994, 323. 10 lap Pat 62-53606; II November 1987. II lap Pat 51-30620; 2 September 1976. 12 Uchida A , Kakogijulsj. 25(4) (1990) 226. 13 Hall J D H, Ridge B P & DeMartino R N, US Pat 2,590,402 ( 1952). 14 Gajjar N J , U S Pat 2,828,528; I April 1958. BAJAJ: SILK-UKE POLYESTER FABRICS 15 16 17 18 19 20 21 22 23 24 25 Zeronian S H & Collins M J, Text Prog, 20(2) (1989) 70. Houser K D, Text Chem Color. 15 (1983) 70. Gawish S M & Ambrioise G , Am Dyest Rep , (Feb. 1986) 30. Rane S S, Man-Made Text India, (July 1992) 251. Ichida E, Uyama Y & Ikada Y, Text Res}, 61(8) (1991)4iD. Yasutome K & Watanabe K, Jap Sen'e Kako , 33(2) (1981) 336. Gawish S M, Bourgeois M & Ambrioise G , Am Dyest Rep , (Dec. 1984) 37. Rao A L N, Silk likefinish onpo/yestei and itsb/ends, M. Tech. thesis, Indian Ins~itute of Technology, Delhi. 1986. Solbrig C M, The alkaline hydrolysis of titimium dioxide delustred PET, Masters thesis, Cornell University, 1986, 44-45. Solbrig C M & Obendorf S K, Text Res J , 61 (1991) 177. Matsudaira M & Matsui M, J Te'x t Inst , 83 (1992) 144. 89 26 Kurara y.£:"o .. Jap Po/ 07,90,736; C/refll Airs/I', 123 (1995) I I 5250g. 27 Toray Ind, Jap Pat 06,322.625; Chem Abstr, 122 (1995) 108592w. 28 Koul R, X-ray and (m/isra/ic polyester fibres, Ph . D thesis, Indian Institute of Technology, Delhi , 1994. 29 Yamaguchi S. Proc. ISF'94 , (The Society of Fibre S cience & Tec/rnology , Yokohama , Japan) , 1994, 326. 30. Toray lrid .. Jap Pat 05.171,516; Chem Abstr, 1201(994) 56600j. 31 Teijin Ltd, Jap Pal 06.263.971; C/rern Abstr, 122 (1995) 190257x. 32 Nippon Ester Co. Ltd. Jap Pat 06,313,214; Chern Abs/r, 122 (1995) 1902601. 33 Matsukama S. Kasai M & Mizuta Y. Sen-i-Gakkaishi, 51 (I) (1995) 17.
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