DYEING OF ORGANIC COTTON FABRIC USING ULTRASONIC DYEING TECHNIQUE

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1 14 th AUTEX World Textile Conference May 26 th to 28 th 2014, Bursa, Turkey DYEING OF ORGANIC COTTON FABRIC USING ULTRASONIC DYEING TECHNIQUE Uzma Syed, Rafique Ahmed Jhatial, Mazhar Hussain Peerzada Department of Textile Engineering, Mehran University of Engineering and Technology, Pakistan, Abstract In this research the dyeing behaviour of organic cotton woven fabric samples dyed by ultrasonic technique with reactive dyes were investigated. Fabric samples were dyed with reactive dyes; Drimarene Red Cl-5B and Drimarene Blue Cl-BR (0.5% o.w.f) using exhaust dyeing method. The samples were ultrasonically dyed at varied temperature 60 ᵒC, 50 ᵒC and 40 ᵒC and time 60 min, 50 min, 40 min and 30 min. Furthermore, for optimizing the dyeing behaviour, the samples were causticized by pad batch method and then dyed with reactive dyes at varied temperature (60ᵒC, 50ᵒC, 40 ᵒC) and time (60 min, 50 min, 40 min, and 30 min). After dyeing, assessment was carried out such as colour strength, dye uniformity, fastness to washing and surface deterioration using S.E.M. It has been revealed that organic cotton fabric dyed using ultrasonic exhaust method at 60 ᵒC for 50 min gives highest colour strength value, excellent wash fastness, deeper dye diffusion, and less surface deterioration. Moreover, causticized and then dyed sample gives excellent dyeing behaviour even at 60ᵒC for 30 min; almost half the dyeing time. Hence dyeing of organic cotton fabric samples using ultrasonic exhaust method saves energy, time and cost. Key Words: Exhaust method, Temperature, Time, Environmental friendly. Introduction Organic cotton fibres are produced from non-genetically modified plants [1]. It offers surface protection of ground water quality and reduces environmental damage. In addition along with textile fibres, textile processing sector is focusing on the conservation of energy using various technique such as infrared heating, ultrasonic waves, microwaves, plasma technique etc each of these techniques are applied by different methods [2-4]. It was observed from literature that ultrasonic waves (high frequency and high energy waves than the sound waves) were used for variety of purpose in textile processing such as pretreatment and dyeing of conventional cotton, polyester, wool and nylon fibres [5-10]. Radcure using ultrasonic technique is an environmental friendly and sustainable dyeing method saves dyeing assistance, time and temperature. Therefore, in this research dyeing behaviour of organic cotton fabric using ultrasonic technique at varied temperature and time has been investigated and compared. Material

2 100% Bleached organic cotton plain woven fabric (150 GSM) was purchased from Yunus Textile Mills, Pakistan. Reactive dyes, Drimarene Red Cl-5B and Drimarene Blue Cl-BR and other auxiliaries such as detergent, Ladipur RSK and levelling agent, Drimagen E2R were kindly supplied from Clariant, Karachi, Pakistan. Other auxiliaries, NaCl and acetic acid were marketed by Merck, Germany. Method Organic cotton sample of weight 3gm was taken and dyed (0.5% o.w.f) on Ultrasonic Cleaner KB200 Series. The dyeing process was carried out at liquor to goods ratio of 20:1 at varied temperatures such as 60ᵒC, 50ᵒC and 40 o C with reactive dye, Drimagen E2R solution w/v (2 g l -1 ) and salt solution w/v (60 g l -1 ). After exhaustion (20, 15, 10 and 6 min) alkali solution w/v (15 g l -1 ) was added and then processed for further 40, 35, 30 and 25 min at the same temperatures (60ᵒC, 50ᵒC and 40 ᵒC). After dyeing, fabric samples were washed with cold water for 10 min then warm water at 80ºC for 10 min. The soaping was done at 90 C for 30 min and before dried in an oven it was again warm and cold wash for 10 min each. Furthermore, the organic cotton woven fabric samples were pre-treated using sodium hydroxide (2 mol dm -3 ) by pad-batch method for 30 min [11]. The fabric samples were then dyed by ultrasonic dyeing technique at varied temperature and time as discussed in preceding paragraph. The washing was carried using the same method as discussed above. Dyeing Assessment Fastness to washing test was performed according to the standard of ISO-105 CO3. After washing, fabric sample and multi fibres stripes were then rated (1 to 5) using grey scale and staining scale. Where 1 means poor fastness and 5 means excellent fastness. Uniformity of dyeing was assessed using Motic video microscope. For preparing the yarn cross-sectional images; 7-10 yarns were taken from the dyed fabric and were laid parallel [12]. The yarn was then passed from the slide; the extra yarns were then cut using sharp blade. The slide was then placed on a video microscope and at constant magnification yarns cross-sectional images were then captured and visually analysed. For assessing the surface distortion of dyed fabric sample with ultrasonic exhaust dyeing method, fabric samples of 1x1 cm was taken. The fabric images at 700 magnifications were taken using JEOL JSM 5380 LV. The fabric images were then visually analyzed. Result and Discussion Colour Strength (K/S) max The average colour strength values of Drimarene Blue Cl-BR and Drimarene Red Cl-5B (0.5% o.w.f) are shown in Figure 1. It has been observed that the colour strength value, (K/S) max of ultrasonic dyed samples increases with the dyeing temperature. Dyeing carried out at recommended temperature (60 o C) gives highest colour strength value than the 50 and 40 o C dyeing temperature. This is because both reactive dye molecules contain vinyl sulphone as a reactive group. However, increase dyeing cycle makes the fabric surface rough, causes fibres fibrils to propensities on the fabric surface and gives less colour strength value. Hence, hinder the reflectance of light. That is why; dyeing for 50 min gives high colour strength value as

3 compared to 60 min dyeing time. Furthermore, lower dyeing time such as 40 and 30 min gives less colour strength value at all temperature 60, 50 and 40 o C. It is owing to less diffusion of dye molecules into the fibre of the fabric. Hence, it is clear from Figure 1, dyeing of organic cotton woven fabric using monfuncltional vinylesulphone (Drimarene Blue Cl-BR) and bisfunctional vinylsulphone and monochlrotriazine (Drimarene Red Cl-5B) gives highest (K/S) max values at 60 ᵒC dyeing temperature for 50 min exhaustion and fixation phases. Moreover, when compare the dyeing behaviour of ultrasonic dyeing technique to conventional HT dyeing techniques. It was observed that conventional dyeing gave colour strength value, 3.3 at max [13], which is lower than the ultrasonic dyeing method except dyeing for 40 and 30 min at 60 and 50 o C. This is because ultrasonic waves provide much higher energy to dye molecules thus increases the rate of diffusion as compared to conventional dyeing method. Figure 1. Average of (K/S) Max Values of Samples Dyed With Drimarene Blue Cl-BR and Drimarene Red Cl- 5B. (K/S) max values of Causticized Dyed Samples Figure 2 shows the average colour strength value at max of samples pre-treated and then dyed with Drimarene Blue Cl-BR and Drimarene Red Cl-5B (0.5% o.w.f). The pre-treatment of fabric samples using sodium hydroxide improve the colour intensity. However, trend of (K/S) max value is almost same as shows in Figure 1. It has been observed that the pretreatment and then dyeing using ultrasonic technique minimize the dyeing time. The dyeing cycle for 30 min at recommended dyeing temperature (60 ᵒC) gives colour strength value comparable to achieved from conventional HT dyeing technique. Sodium hydroxide swells up the cellulosic fibres, increase the hydroxyl groups on the fabric surface, hence allow the dye molecules to adsorb and then absorb into the fibre filaments. Similarly, ultrasonic cavitations support the dye molecules to exhaust towards the fibre filaments. Thence, improves the dyeing behaviour of organic cotton fabric by decreasing the dyeing cycle.

4 In addition, pre-treatment and then dyeing using ultrasonic technique minimize the dyeing temperature. It is clear from Figure 2, dyeing at 50ᵒC for 60 min gives compromise colour strength value compared to 40ᵒC dyeing temperature at the same dyeing time. Hence, saves energy, although causticization process requires an extra cost. Figure 2. Average of (K/S) Max Values of Samples Pre-treated and Dyed With Drimarene Blue Cl-BR and Drimarene Red Cl-5B. Washing Fastness Reactive dyes, Drimarene Blue Cl-BR and Drimarene Red CL-5B undergo a nucleophilic substitution reaction mechanism and from a strong covalent bond with the hydroxide groups of organic cotton fabric. It is observed from Table 1 and Table 2 dyed fabric samples have very good to excellent wash fastness properties. Hence, sample dyed with reactive dyes shows inconsiderable change in shade and staining rating. As shows in Table 1; dyeing carried out at lower dyeing time and temperature has been given lower colour strength value as well as good to very good rating (4/5 and 4) on organic cotton dyed fabric. However, pre-treatment using sodium hydroxide has been improved the washing fastness rating at 60 o C dyeing temperature for 40 and 30 min dyeing time and at 40 ᵒC dyeing temperature for 60, 50, 40 and 30 min as shown in Table 2. Table 1. Average of Wash Fastness Rating of Samples Dyed with Drimarene Blue Cl-BR and Drimarene Red Cl-5B Temperature/Dye ing Time 60 min 50 min 40 min 30 min in Staini in Staini in Staini Shade ng Shade ng Shade ng Stainin g in Shade 60ᵒC /5 5 4/5 50ᵒC /5 4/5 4/5 4/5 40ᵒC 4/5 4/5 4/5 4/ Table 2. Average of Wash Fastness Rating of Samples Pre-treated and Dyed with Drimarene Blue Cl-BR and Drimarene Red Cl-5B

5 60 min 50 min 40 min 30 min Temperature/Dyeing in in in in Time Staining Shade Staining Shade Staining Shade Staining Shade 60ᵒC ᵒC /5 5 4/5 5 40ᵒC 5 5 4/5 5 4/5 5 4/5 5 Dye Penetration The dyed fabric sample images after capturing using an optical microscope were assessed visually. The undyed fibres are shown in white colour, whereas deep dyed fibres are shown in very dark colour depend on the depth of dye. It is clear from the images (see Figure 3) that the organic cotton fabric dyed using ultrasonic dyeing technique not only gives the highest colour strength value but also gives uniform and deeper diffusion of dye molecules. There is no undyed fibre observed from the images. Simialrly, fabric samples dyed after causticisation shows uniform dyeing and much deeper diffusion of dye molecules as shown in Figure 4. Figure 3. Sample Dyed with Drimarene Red CL-5B and Drimarene Blue Cl- BR at 60 ᵒC for 60 min and 50 min Dyeing Time. Figure 4. Fabric Sample Pre-treated and Dyed with Drimarene Red CL-5B and Drimarene Blue Cl- BR at 60 ᵒC for 60 min and 50 min Dyeing Time

6 Scanning Electron Microscopy (SEM) The SEM images of fabric sample dyed by ultrasonic dyeing technique at different temperatures and time are shown in Figure 5. The sample dyed by ultrasonic technique at 60 o C and 60min shows that surface of dyed fabric sample is deteriorated by ultrasonic waves, making its fibrils protruding hence gives low (K/S) max value as compared to sample dyed for 50 min. Less deterioration of fabric surface gives regular refection of light hence high (K/S) max values. Pre-treated and dyed sample has inconsiderable surface deterioration due to the combined action of causticization and ultrasonic waves during fabric processing. Few fibre fibrils are protruding on the fabric surface thus gives quite high colour strength values as shown in Figure 6. Figure 5 Dyed with Drimarene Red Cl-5B at 60 o C for 60 min and 50 min. Conclusion Figure 6 Pre-treated and Dyed with Drimarene Red Cl-5B at 60 o C for 60 min and 50 min An environmental friendly and sustainable dyeing technique, ultrasonic saves dyeing assistant, time and temperature. Bleached organic cotton fabric samples were dyed with ultrasonic dyeing method at varied temperature and time. It is observed ultrasound waves improve the colour strength values with Drimarene Red Cl-5B and Drimarene Blue Cl-BR (0.5% o.w.f) dyes. Sample dyed using ultrasonic technique at 60ᵒC for 50 min gives highest

7 (K/S) max value, less fabric surface deterioration and deeper diffusion of dye molecules as compared to dyeing process carried out for 60min dyeing cycle. However, combine action of caustic and ultrasonic waves almost half the dyeing time compared to conventional exhaust dyeing method. The dyeing could be carried out at lower temperature up to 50 ᵒC and at minimum dyeing time 30 min. The caustic swell up the fibre filaments causes much deeper diffusion of dye molecules, less surface detoriation and excellent fastness and colour strength value on organic cotton woven fabric. References [1] Lauresn, S. E., Hansen, J., Knudsen, H. H., Wenzel, H., Larsen, H. F., & Kristensen, F. M. (2007). EDIPTEX: Environmental assessment of textiles. Danish Environmental Protection Agency, working report, pp 24. [2] Aravin P, Ultrasonic Assisted Wet Processing, available on [accessed on July 2011]. [3] Qingjie G, Investigation into dyeing acceleration efficiency of ultrasound energy, (2010), Ultrasonic s, Vol 50, pp [4] Rahul G, Recent developments in textile dyeing techniques, available on [accessed on August 2011] [5] Good, J, Zhan, J, Klutz, D, Mock, G and Beckham, H,W, Fundamental Investigations of Ultrasound-Enhanced Dyeing, AATCC, International Conference and Exhibition, Atlanta, GA; pp 8 11, October [6] Yan, G, Zhang M, Ultrasonic wool scouring process, (2006), Journal of Textile Research, Vol 27 (10), pp [7] Ahmed, N.S, El-Shishtawy R.M, and M.M. Kamel, Ultrasound assisted pre-treatment and dyeing of linen fibres with reactive dyes, 2007, Pigment and Resin Technology, Vol 36 (1), pp [8] Akalin, M, Merdan, N, Kocak, D, Usta, I, Effects of ultrasonic energy on the wash fastness of reactive dyes, 2004, Ultrasonics, Vol 24 (1-9), pp [9] Hanna, H.L, Nahed S. E, Ultrasonic-assisted dyeing: I. Nylon dyeability with reactive dyes, 2003,Polymer International Vol 52, Issue 3, pp [10] Milena N. M, Vesna B. I, Aleksandra R. Z, Influence of different parameters on dyeing of knitting material with reactive dyes, 2007, Physics, Chemistry and Technology, 2007, Vol 5 (1), pp [11] Syed, U, Influence of woven fabric structure of tencel woven faric dyed with Reactive Dyes, Ph.D Thesis, 2010, Heriot-Watt University, U.K. [11] Syed, U, Wardman, R.H, Assessment of uniformity of fibre coloration in Tencel woven fabric dyed with reactive dyes, 2011, Coloration Technology, Vol 127 (6), pp [12] Syed, U, Samad, A, Ahmed, F, Dyeing of organic cotton fabric using conventional and ultrasonic exhaust dyeing method, 2013, Mehran University of Research Journal of Engineering and Technology, Vol 32 (2), pp Author(s) Information Please give: 1. Dr Uzma Syed.

8 Textile Engineering Department, Mehran University of Engineering and Technology, Jamshoro, Paksitan. Assistant Professor Prof Dr Rafique Ahmed Jhatial Textile Engineering Department, Mehran University of Engineering and Technology, Jamshoro, Paksitan. Professor Dr Mazhar Hussain Peerzada Textile Engineering Department, Mehran University of Engineering and Technology, Jamshoro, Paksitan. Associate Professor

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