ࡱ> Z`[VWXY [$@$NormalmH <A<Default Paragraph Font  l,b$nnN}YT @n(   6   AB S  ?t@@GTimes New Roman5Symbol3"Arial9CG Times"hߚF&ߚF&APPLICATION OF ELECTROMAGNETIC WAVES IN DURABLE PRESS FINISHING WITH POLYCARBOXYLIC ACID Sandra Bischof Vukusic and Drago Katovic Faculty of Textile Technology, Zagreb, HR ABSTRACT Stabilisation of cellulose material dimensions and shape has always been field of a great concern for consumers. Finding competitively priced nonformaldehyde Durable Press (DP) finishes has become among highest priority for the textile finishing industry. From the ecological point of view polycarboxylic acids (PCA) are highly justified, while economical problem of high price was tried to be sold with different solutions. Maximum effects of DP finishing among PCA were obtained with 1,2,3,4-butanetetracarboxylic acid (BTCA), whose exceedingly high cost is well known. Because of the widespread availability and its low cost, citric acid (CA) has became interesting for the DP finishing treatment. Greatest disadvantage of CA is its negative tendency to impart noticeable fabric yellowing under the elevated cure conditions. Yellowing of the textile material can be explained by the formation of unsaturated polycarboxylic acids. Instead of the usual curing process performed at very high temperatures we have used electromagnetic (EM) waves from the microwave owen. With this procedure we have accomplished even better results of the fabric resilience while the whiteness degree have not been significantly lowered. The influence of EM waves on the efficiency of esterification was studied by FT-IR spectroscopy method. By measuring the ester carbonyl band intensity of textile materials cured in two different ways the amount of ester was determined. Although this treatment has been tested only in a laboratory jet, first results are showing great promise for its future application in this field. Introduction As was the case with many other big discoveries, the activity of electromagnetic (EM) field of high frequency was discovered accidentally, during a radar-related research project. While testing a new vacuum tube, called a magnetron, the power of microwaves was discovered. After more than 30 years of investigations and development in the field of microwave engineering, the technology of microwaves is widely used in a number of fields, from food preparation, chemical sludge, medical waste, curing of hi-tech polymers to industrial drying processes. In textile technology, EM waves are used in high-frequency (HF) dryers for thick and multi-layer materials. In these machines, energy is transferred by means of two metal electrode plates, between which the fabric is transported on a conveyor belt. An alternate electric field is created between the electrodes with alternate voltage, created by a HF generator. Under the impact of the energy thus created in the alternate electric field, dipole water molecules start vibrating, which causes them to heat up and be transformed into water vapour. Unfortunately, due to the nature of the EM field in microwave ovens, it is hard to achieve uniform energy distribution, which means problems in monitoring and control of temperature distribution. There are a number of papers dealing with synthesis of organic compounds using microwave ovens. Numerous chemical reactions are discussed and presented, e.g. substitution, addition, esterification, transesterification, acetilization, amidation, decarboxylation etc. 1, 2 In esterification under the influence of alternate field energy, molecules start vibrating, which speeds up the process of esterification itself. Besides influencing dipole water molecules, alternate EM field also acts upon partially polar molecules of the textile material, such as polyurethane (PU), polyacrilonitrile (PAN) or polyamide (PA). Heating up can also occur due to the shift of electrons in the atomic bond. Literature search has not revealed papers dealing with the application of electromagnetic waves in esterification of polycarboxylic acids (PCA) and cellulosic materials. The treatment in a microwave oven described here has been done for the purpose of preliminary research. Favourable results would indicate the need for further investigations of the application of HF in dryers, including partial modification of the equipment as well. New and innovative thermal treatments are presented, aimed at achieving better effects in crease-resistant treatments of cellulosic fabrics. Results obtained after treatment in a microwave oven are compared with those obtained after conventional thermal condensation treatment in a stenter. Experimental Materials Cotton and viscose fabrics used were chemically bleached and optically brightened. Cotton fabric properties were as follows: 100 % cotton, surface mass: 97 g/cm2, fineness: warp/weft: 60/60 tex, density: warp/weft 27.5/27 yarns/cm. Viscose fabric properties were as follows: surface mass: 120 g/m2, fineness: 110 dtex f 24 S 100/17 tex Z 900, density: 48/27. Fabric Treatment The fabrics were passed through squezze rolls on a laboratory foulard Benz (Switzerland) to give a wet pickup of 100 % owf. Baths content can be seen in the tables. Besides standard recipes with butanetetracarboxylic acid (BTCA) and citric acid (CA) with sodium hypophosphite monohydrate (SHP) as a catalyst, recipes were applied with additional catalysts 1-hydroxyethane 1,1-diphosphonic acid (HEDPA) and diethylene-triamine-pentamethylen phosphonic acid (DETMPA), in order to lower the SHP content. After finishing, the fabric was dried on a stenter at 110oC for 2 minutes. Half of it was thermally treated employing a conventional procedure in a stenter, at 180oC for the duration of 90 seconds. The other half was treated in a microwave oven, at 900 W for 20 minutes. Microwave oven Moulinex was used, with maximum power of P= 900W, so longer curing time (20 minutes) was employed to obtain good resilience effects. Industrial microwave machines are usually employing much higher power, so consequently the necessary curing time would be much lower. Testing Methods Whiteness (CIE wh.) and yellowness index (YI) of the treated samples were measured on a reflection spectrophotometer Datacolor 3890. Tensile strength (TS) was measured according to DIN 53837, and wrinkle recovery angle (WRA) according to DIN 53891. Perkin Elmer System 2000 Fourier Transform (FT) - IR with the programme Infra Red Data Manager (IR-DM) was used for spectroscopic measurements. Spectra of solid matter, insoluble in IR transparent solvent, are usually obtained by dispersing the samples in a solid or liquid matrix. The technique requires that tested solid particles must be smaller than the wavelength of the IR ray used, as a considerable part of the irradiation is lost through dissipation if this condition is not fulfilled. One of the techniques of sample preparation, also used in the investigation described here, uses dry KBr, where approximately 100 mg of KBr is mixed with 1 mg of finely ground sample. Mixing can be done in a mortar, or Wiley mill. The mixture is pressed under specified pressure to obtaine a transparent disk. The best results in sample preparation are achieved if the procedure is done in vacuum; thus eliminating the air previously absorbed. The spectra obtained exhibited peaks at 3450 and 1640 cm-1 (2.9 and 6.1 (m), due to the moisture absorbed. To perform semi-quantitative determination of the finishes on the fabrics, normalisation of the carbonyl intensities in the infrared spectra was done against the 1317 cm-1 band, which represents C-H structures in cellulose molecules. Results and discussion The effects of crease-resistant finishing of cotton fabric can be seen in Table I and III, while the results for the viscose material tested are given in Table II and IV. The treatment in a microwave oven resulted in approximately the same improvement of cond. wrinkle recovery angles for CA and BTCA treatments, for both materials (Table I, II). The improvement was more pronounced on the viscose fabric, and was between 50 and 60 degrees. Wet recovery angles on the viscose fabric were rather low, both after conventional heat treatment and after the treatment in a microwave oven (Table II). Cotton fabric treated in a microwave oven exhibited improved wet recovery angles only with the BTCA finishing treatment. Tensile strength (TS) retention was higher for the viscose than cotton material, which is especially pronounced after the treatment in a microwave oven. The strength of cotton fabric is higher in wet state and lower in dry, while the situation is opposite with viscose. Tensile strength loss is less pronounced with viscose than with cotton, which is generally true for this type of finishes. Moreover, strength of a viscose fabric can be increased after crease-resistant treatments. It is generally explained by reduction of moisture regain after crease-resistant finishes. Reduction of whiteness index after the heat treatment is more pronounced on the cotton material than on the viscose. Considerable reduction of whiteness, which means more pronounced yellowing of the cotton fabric, results primarily from the use of citric acid. CA decomposes at elevated temperatures to acids with double bonds, which are the primary cause of this detrimental effect.3 Application of microwave technology results in less pronounced reduction of whiteness index with CA. The viscose fabric exhibits better properties of whiteness reduction, compared to cotton fabric with smaller differences between the CA and BTCA treatments. Measuring results dealing with whiteness and breaking strength retention generally indicate that more of CA is linked to the viscose fabric than to the cotton one, which results in reduced content of acids with double links, such as cause yellowing. It was expected, as viscose has a higher content of free OH groups able to be esterified, than cotton. FT-IR Spectroscopy The method enabling determination of ester crosslinked cotton material, employing infrared spectroscopy FT-IR, was developed by C.Q.Yang.4 Carbonyl groups on a cellulosic material treated with PCA are retained in three forms: ester, carboxyl acid and carboxylate anion. All three forms could be present in a single molecule, if PCA contains 3 or more carboxyl groups. The peak in the IR spectrum occurs in the range between 1735 and 1715 cm-1, due to the ester carbonyl group, together with the peak for the carbonyl group of the carboxylic acid. Treatment with diluted NaOH changes free carboxyl groups into carboxylate anion. The fabric was treated in 0.1 M solution of NaOH, and the other part of the sample in 0.1 M HCl for 2 min. at room temperature, and rinsed afterwards. In this way, overlapping of the peaks for the carboxyl and ester groups is avoided.5-8 Intensity of the bond at 1732 cm-1 is the measure of the total number of ester groups present in the textile fabric treated, including the ester bonds between the cellulose and single-side linked acid molecules, as well as the ester group of the PCA which crosslinks the cellulose molecule. Only PCA molecules crosslinked with cellulose have an impact on the recovery angle of the textile fabric treated. The ratio of the carbonyl bond intensity, e.g. the ratio of peak values at 1732/1580 cm-1 can be used as an additional parameter for comparing different crosslinking degrees. The intensity of the peak at 1732 cm-1 is the measure of the quantity of total ester bonds created, including single-side bonded and double-side crosslinked PCA molecules. The ratio of ester and carboxylate is a function of the average number of ester groups created from each PCA molecule, and represents the efficiency of the PCA molecules bonded as crosslinking agents. The results obtained show that the number of ester groups determined generally corresponds to the results of determined recovery angles. The best results of recovery angles were obtained using BTCA on both materials, after the treatment in a microwave oven, and spectroscopic data confirmed the highest number of ester groups under these circumstances (Fig. 1). Results of the ratio of carbonyl intensity show that CA is even more effective on cotton than BTCA, while these results are similar for the viscose material treated in a microwave oven (Table V). Most serious disadvantage of the FT-IR spectroscopic method is that it can only be used for qualitative to semi-qualitative determination of ester bonds on cellulosic material. Additionally, this method cannot be used to identify individual polycarboxylic acids. Conclusions A PCA molecule can be crosslinked within cellulosic chains only when more than one ester link with the cellulose molecule is created. The higher the number of carboxyl groups esterified by a single PCA molecule, the higher is the number of intermolecular ester crosslinks within cellulose molecules concerned, for the same number of ester groups in the cotton fabric in question. Total number of ester groups present in a particular textile fabric can be semi-quantitatively determined by FTIR spectrometry at 1733 cm-1, as a ratio of ester peaks of the sample, treated with HCl and NaOH after the curing treatment. The number includes ester bonds between the cellulose and single-side linked acid molecule, as well as the PCA ester group which crosslinkes the cellulose molecule. Better recovery angles were achieved after treating the fabric in a microwave oven, compared to conventional thermal condensation. The best results for dry recovery angles were on both materials achieved by BTCA treatment. Spectroscopic data confirms the highest number of ester groups in this case. Besides better recovery angles, higher strength retention was also achieved after treating the fabric in a microwave oven, especially significant for the viscose fabric. Investigations with polycarboxyl acids have been done for a number of years, and it is quite possible that thermal treatment described here will contribute to the spread of their usage in practical applications. The results obtained indicate that the application of microwave technology yields much more favourable results in crease-resistant treatments. The research of possibilities of using EM waves in crease-resistance treatments performed until now is only the beginning of much wider investigations to follow. References Cablewski, T., A.F. Faux, C.R. Strauss, J. Org. Chem., Vol. 59, No. 12, Decembar 1994, pp3408-3412 Kabza, K.G., B.R. Chapados, J.E. Gestwicki, J. Org. Chem., Vol. 65, No. 4, April 2000, pp1210-1214 Schramm, C., B. Rinderer, TCC & ADR, Vol. 32, No. 4, April 2000, pp50-54 Yang, C.Q., Textile Research Journal, Vol. 61, No. 8, August 1991, pp433-440 Yang, C.Q., Textile Research Journal, Vol. 63, No.12, December 1993, pp706-711 Choi, H.M., C.M. Welch, N. Morris, Textile Research Journal, Vol. 64, No. 9, September 1994, pp501-507 Von ina, B., Fibres & textiles in Eastern Europe, No. 1-2, January-February 1996, pp69-71 Von ina, B., A. Majcen Le Marechal, S. Jeler, Tekstilec, Vol. 39, No. 9-10, September-October 1996, pp196-199 Address Prof. DRAGO KATOVIC, Ph.D. E-mail: dkatovic@ttf.hr SANDRA BISCHOF VUKUSIC,Ph.D. E-mail: sbischof@ttf.hr Faculty of Textile Technology, University of Zagreb, Pierottijeva 6, 10 000 Zagreb, Croatia; telephone +385 1 4877350, fax + 385 1 4877352 PAGE 7 PAGE 11 YZ  3 #'Cw`a):lm[]mnoR T b c .!1!p!!U$V$W$&(()z*|*}*ﲨ5mH  jmCJOJQJCJH*OJQJ56CJOJQJOJQJmH >*CJOJQJ6H*OJQJ 5OJQJ CJOJQJCJmH 5mH  CJOJQJ6CJOJQJ5CJOJQJ5CJOJQJ9YZ`u]| h  3 U(wdd$d$dd$d$dYZ`u]| h  3 U(w():;3\]mno^o!p!!Ҫ𧤞~{xr ^ J ~  VX E1P8M+():;3\]mno^o!p!!!3"C#W$&|()dd$d$d!!3"C#W$&|()|*}***,-/0134444m679;;;;I<<<B===þ}si_I      .       # w  W-=")|*}***,-/0134444m679;;;;I<<< & Fdd$d$dd$d$dr0hTTFTTF<B===>???@<@@@@@@@@@@@@@@@@@&`#$$d$d$d & Fd=>???@<@@@@@@@@@@@@@@@     [0@0 Normal_HmH sH tH >> Heading 1$$@&a$ 5OJQJD@D Heading 2$@&CJOJQJmH sH u:@: Heading 3$$@&a$5CJ:@: Heading 4$$@&a$5CJ>> Heading 5$$@&a$ CJOJQJ>@> Heading 6$$@&a$ CJOJQJ<@< Heading 7$$@&a$ 56CJB@B Heading 8$$@&a$6CJOJQJF F Heading 9 $$@&`a$ CJOJQJ<A@< Default Paragraph FontFB@F Body Text$a$5CJOJQJmHsHuHP@H Body Text 2$a$CJOJQJmHsHu8Q@8 Body Text 3$a$5CJ, @", Footer  9r &)@1& Page Number;;Z             "(/5:;zke? 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FT-IR spectra of base rinsed cotton and viscose fabrics treated with CA and SHP cured in: a  conventional stenter frame, b  microwave oven Table I. Tensile strength retention (TS %) and wrinkle recovery angle (WRA() A - after the conventional condensation, T=180(C, t=90 s B - after the treatment in a microwave oven, P=900 W, t=20 min. COTTON MATERIAL BTCA g/l CA g/l SHP g/l HEDPA g/l DETMPA g/lT S % AT S % BWRA cond. AWRA cond.BWRA wet AWRA wet BUntreated material:100100106108118137 60 -65--547126428828930041--53602552792802854152-606327528029330541-405762251272279290 - 6965--597324125924823741--58602322702722374152-626520223022922541-526064201225263255 Table II. Tensile strength retention (TS %) and wrinkle recovery angle (WRA() A - after the conventional condensation, T=180(C, t=90 s B - after the treatment in a microwave oven, P=900 W, t=20 min. VISCOSE MATERIAL BTCA g/l CA g/l SHP g/l HEDPA g/l DETMPA g/lT S % AT S % BWRA cond. AWRA cond.BWRA wet AWRA wet BUntreated material:10010084102154150 60 -65--756015821720220341--60731482291991954152-677512619120919141-405664117174193194 - 6965--537613215719017841--41821191661991844152-70879918120819141-52738299153192194 Table III. CIE whiteness and yellowness index for cotton material: Untreated fabric: CIE Wh.=146 YI= -25.86 A - after the conventional condensation, T=180(C, t=90 s B - after the treatment in a microwave oven, P=900 W, t=20 min. COTTON MATERIAL BTCA g/lCA g/lSHP g/lHEDPA g/lDETMPA g/lCIE Wh. ACIE Wh. BYI AYI B 60 -65--117110-14.84-12.1941--116113-14.18-13.014152-117100-14.84-7.7641-40118110-15.31-12.19 - 6965--9395-4.85-6.4741--9084-3.62-1.374152-8895-2.52-6.4641-4089115-3.92-13.76 Table IV. CIE whiteness and yellowness index for viscose material: Untreated fabric: CIE Wh.=141, YI= -27,00 A - after the conventional condensation, T=180(C, t=90 s B - after the treatment in a microwave oven, P=900 W, t=20 min. VISCOSE MATERIAL BTCA g/lCA g/lSHP g/lHEDPA g/lDETMPA g/lCIE Wh. ACIE Wh. BYI AYI B 60 -65--124121-17.33-15.9741--121114-16.89-13.634152-125116-17.87-14.6341-40123106-17.27-10.68 - 6965--117115-14.50-14.0441--125128-17.73-19.074152-123117-17.17-14.9241-40123110-17.27-11.98 Table V. Efficiency parameters for cotton and viscose materials treated with BTCA or CA: A) after the conventional condensation, T=180(C, t=90 s B) after the treatment in a microwave oven, P=900 W, t=20 min. 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