The Study on Cotton Fabric Dyeing by Indigo Blue from Baphicacanthus Cusia, Indigofera Tinctoria and Polygonum Tinctorium

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1 Technical Paper The Study on Cotton Fabric Dyeing by Indigo Blue from Baphicacanthus Cusia, Indigofera Tinctoria and Polygonum Tinctorium Chonyu Chen 1,Chiehyi Lin, and HanchiehWang 2 1 Department of Fashion Design, Shu-Te University, No. 59, Hun Shan Road, Yen Chau, Kaohsiung 824, Taiwan (R.O.C) 2 Department of Cosmetic Applications & Management, Yuh-Ing Junior College Of Health Care & Management, No. 15, Lane 420, Dachang 2nd Road, Sanmin District, Kaohsiung City 807, Taiwan (R.O.C) Abstract : In this study, 750 g of Taiwan plant- polygonum tinctorium, with two reducing agents-60 g sodium hydrosulfite and 12 g thiourea dioxide were added to dye the cotton fabric for seconds, 1-15 times repeatedly. After this, take the cloth specimen being dyed for 3 minutes with the 15th times to compare with the original cloth for color difference ( E). According to the experiment, with the addition of sodium hydrosulfite, E value of the polygonum tinctorium specimen was 71.70, and respectively, while with the addition of thiourea dioxide, the E value of baphicacanthus cusia, indigofera tinctoria and polygonum tinctorium specimen was 73.43, and respectively. As for washing fastness test, when indigofera tinctoria was reduced with sodium hydrosulfite, the washing fastness test was rated as grade 3-4. For other specimens, they were just grade 3. In the softness test, when the sodium hydrosulfite was added to indigofera tinctoria, the lowest flexural degree was 5.6 cm. In the ultraviolet resistance test, the sodium hydrosulfite with polygonum tinctorium showed the best result with T% The dyed cotton fabric also revealed the characteristic functional peak of indigo blue at 1624 cm -1 via FT-IR test. (Received 9 January, 2008 ; Accepted 29 May, 2008) 1. Introduction The plants such as baphicacanthus cusia, indigofera tinctoria and polygonum tinctorium contain abundant indigo blue C14H17NO6 [1]. Taiwan has currently been using two methods to produce indigo blue : one is the immersing and depositing method, which is applicable to the climate in Taiwan. This method is widely used and time saving. In the process of production, stirring is required to release the water-soluble dye completely ; meanwhile, dump the hydrated lime into the barrel and stir quickly and evenly to make sure large amount of bubbles in the air to be oxidized. This can help produce non-water-soluble indigo blue deposition ; then dump out the upper layer of brown dye and utilize the cotton fabric bag to filter. The abundant water can be dripped out to produce mud-water mixture. After being exposed under the sun, the water content can be minimized for blue mud [2-4]. Another method is called piling and fermenting method [5], which is applicable to the climate with slight difference humidity. For instance, in Japan, the smashed herb made of the polygonum tinctorium plant after being solarized can be piled and fermented to produce blue indigo dye called sukumo. The smashed herb of dry and stored polygonum tinctorium in the first reaping can be piled in a special fermenting platform (also called sleeping bed). This kind of platform is the indoor location for production of polygonum tinctorium indigo. Apart from this, Stokerm [6] published the latest improved technology concerning mass extraction for the blue indigo pigment in The woad leaves are dewaxed and immersed in the mild water solution with low ph value for extraction. Then mix the extracted liquid with ammonium solution to form the mixture with ph After being adequately oxidized, the blue mud can be obtained. In this technology, the extraction rate of blue mud can reach up to 2 %, which is higher than the ordinary indigo blue extraction rate (approximately %). The blue mud can only be used after the process of reduction. The rapid chemical reduction is one of the most popular methods, through which some chemical alkalis such as sodium carbonate, sodium bicarbonate and NaOH can be dissolved into the non-water-soluble blue pigment, while the chemical reducing agent can speed up

2 the process of dyeing reduction. After the consumption of chemical reducing agent in the dyeing liquid, the dyeing ability might be lost gradually. Therefore, some more reducing agent needs to be added in the process of each dyeing process [7]. However, because of the low affinity of natural indigo dye to cotton, repeated dyeing process is often needed and the contact between the dyeing material and the cloth should be increased to improve the dyeing ability [8]. From the study by Hang in 2000, thiourea dioxide can be used to replace the sodium hydrosulfite as the reducing agent for cold rolling dyeing process [9]. According to the experiment, component and structure of some natural dyes can function to prevent allergy, kill bacterium and prevent insects and ultraviolet radiation. It also showed the darker color with better ultraviolet resistance [10-12]. In addition, from the study by Wang 2000 [13], cotton after being dyed with yellow and blue colorant, the UPF value increase by 544 % and 212 %, respectively. By increasing the texture density of cotton fabric can also improve the effect of ultraviolet resistance [14]. This research purpose is to understand the difference of indigo dyeing properties by using indigo blue from Polygonum tinctorium. Two reducing agents : thiourea dioxide or sodium hydrosulfite is also selected to compare their reducing ability and other dyeing properties effect. 2. Materials and Methods 2.1 Experimental materials This experiment uses three different blue indigo mud and dyeing materials purchased from Taipei-Sansia Yuyulian Works (baphicacanthus cusia), Taitung-Sunrise Blue Dyeing Works (indigofera tinctoria)and Chungliao- Sidiyao Farm (polygonum tinctorium). As for sodium hydroxide (NaOH), 93.0 % is purchased from Shimada Chemical Works while the sodium hydrosulfite (Na2S2O4) and the thiourea dioxide ((NH2)2CSO2) are purchased from the First Chemical Works. The pure cotton fabric (40 40/110 76) is purchased from Lianchang Cotton Works. 2.2 Procedures for Indigo reduction Add pure water 15 L (Millipore), g sodium hydroxide solution (27.2 w/w%), 160 g sodium hydrosulfite (37.5 w/w%) and 120 g thiourea dioxide (10 w/w%) to three blue mud-baphicacanthus cusia, indigofera tinctoria and polygonum tinctorium (750 g for each) for reduction. After the reduction for one hour, the ph value is about 12 ± 1. This can be prepared into different dyes and added to different reducing agents as six experimental specimens. Thename and abbreviations are as follows : baphicacanthus cusia with sodium hydrosulfite (BCS), baphicacanthus cusia with thiourea dioxide (BCT), indigofera tinctoria with sodium hydrosulfite (ITS), indigofera tinctoria with thiourea dioxide (ITT), polygonum tinctorium with sodium hydrosulfite (PTS), polygonum tinctorium with thiourea dioxide (PTT). 2.3 Cotton fabric processing Place 140 g experimental cotton fabric into the stainless wok and add 4.2 L water, 0.75 g soap and 3.75 g sodium hydroxide. Stirring the mixture evenly and keep stirring for 40 minutes washing then dry under with sun. After this, place the cotton fabric into the blue indigo barrels separately. Dye the cotton fabric with 1-minute and 3-minute dyeing process repeatedly for 1-15 times. In the process of repeated dyeing, if the ph value changes, add at anytime according to the previously mentioned proportion of alkaline solution and reducing agent to keep the ph value at the same level. 2.4 CIE 1976 L* a* b* test According to the CIE 1976 L* a* b* standard, take the different cotton fabric that have been dyed for 1 and 3 minutes for 1-15 times repeatedly and test them for three times in any five points via the spectrophotometer (X-rite, SP60). This is to seek the E value difference of cotton fabric after being dyed from 1 to 15 times, which can help identify the dyeing affinity change of different repeated dyeing process. Comparison of hue change between before washing and after washing of different indigo dyed fabric is also conducted. The formulation can be expressed as : E = (L * 2-L * 1) 2 +(a * 2-a * 1) 2 +(b * 2-b * 1) 2 1/2 (1) Notes : +a refers to red, -a refers to green, +b refers to yellow, -b refers to blue, the brightness of the color is expressed byl. 2.5 Washing fastness test In accordance with CNS 1494 A-2 method, this study conducts the washing fastness test on cotton fabric that have been dyed for 3-minute and 15 times with six blue dye formulations. 2.6 Softness test In line with the CNS standard, the fabric softness tester (INTTECO) is used to test the six blue dye formulations, in which the fabric specimens with 3- minute repeated dyeing for 15 times are used after the washing fastness test. In the process of experiment, 45-

3 degree beam suspending method is used. Cut the fabric into the shape in 12 centimeters long and 3 centimeters wide. Place them on a platform with a 45-degree slope angle in the front and make sure that the fabric itself is flat and no crimple is allowed. Push the fabric towards the end slope at an appropriate speed. The self-weight of the fabric shall make the front droop until it touches the slope. The distance for which it travels will be recorded in the experiment. Finally, repeat the experiment for five times to get an average value. The shorter the distance is, the softer the fabric is and the longer the distance is, the harder the fabric is. 2.7 Ultraviolet resistance test The ultraviolet radiation analyzer (UV Mecasys OPTIZEN 2120) is used for the test. The test method is in accordance with Australia/New Zealand (AS/NZS 4399 ; 1996). The measuring wavelength is between nm and the Ultraviolet Protection Factor (UPF) coefficient assessment is as follows : When the T % value is between 6.7~4.2, it indicates good. (UPF=15, 20) ; When the T % value is between 4.1~2.6, it indicates excellence. (UPF=25, 30, 35) ; When the T % is 2.5, it indicates super (UPF=40, 45, 50, 50+). The formula for UPF calculation is as follows : the same dyeing condition, E value of BCT of the dyed cotton fabric specimen is and 73.43, respectively. minute process and under the same repeated dyeing process, formulation BCT is slightly better than Table 1 E in Repeated Dyeing for BCS and BCT Eλ : refer to the ultraviolet energy that forms red spots ; Sλ : refer to the radiation energy ofthe sun spectrum (W. M -2.nm -1 ); Tλ : refer to the ultraviolet penetration rate when the wavelength is λ ; λ : refer to the interval of ultraviolet wavelength (nm) ; λ : refer to the wavelength of the ultraviolet radiation (nm). 2.8 FTIR Chemical structure test Fourier transform infrared spectroscopy (FTIR, Bio Red Digilab FTS-40) is a useful instrument to obtain fabric structural information. Cotton fabric of ITT and ITS, and pure cotton fabric are tested to compare the major structure difference. (2) formulation BCS. 3.2 E value of ITS and ITT for 1-minute and 3- minute repeated dyeing According to Table 2, when ITS is dyed for 1 and 3 minutes until the 15 th times, the E value is and 69.57, respectively. Under the same dying condition, the Table 2 E in Repeated Dyeing for ITS and ITT 3. Results and discussions 3.1 E value of BCS and BCT for 1-minute and 3-minute repeated dyeing According to Table 1, when BCS is dyed for 1 and 3 minutes until the 15th times, E value of the dyed cotton fabric specimen is and 71.70, respectively. Under

4 Table 3 E in Repeated Dyeing for PTS and PTT All specimens reveal similar washing fastness with grade 3tograde 3-4. The softness test shows different indigo blue dyed fabric with similar softness close to the value of 6cm. It also expresses slightly softness increasing after washing. As for T%, all specimens reveal UV T % 0.5 (super UPF 50+), even after washing the UV T% is still with very low value. E value of ITT is and 68.91, respectively. minute process. The E value of ITT (fourteen and fifteen times, 1 and 3 minute) and ITS (fourteen and fifteen times, 3 minute) all show about 69 which might mean reaching a dyeing saturation condition. 3.3 E value of PTS and PTT for 1-minute and 3-minute repeated dyeing According to Table 3, when PTS is dyed repeatedly for 1 and 3 minutes until the 15th times, the E value is and 70.91, respectively. Under the same dyeing condition, the E value of PTT is and respectively. minute process. The E value of PTS (twelve to fifteen times, 3 minute) and PTS (fourteen and fifteen times, 1 minute) all show about 70 which might mean reaching a dyeing saturation condition. 3.4 Comparison of a*b* Value for different indigo blue formulations According to Fig. 1, a* b* valueof BCS, BCT, ITT, PTS, PTT all show similar tendency with slight change after dyed cotton specimens being washed. It also means the red and yellow hue fading faster after washing but only ITS reveals very tiny change with different tendency. 3.5 Washing fastness, softness and UV T% of different indigo blue formulations In Table 4, different testing results of indigo blue formulations (with 3 minute and 15 times) were compared. Fig. 1 The arrows express the a* b* Value of the before washing dyed cotton fabric specimens to after washing dyed cotton fabric specimens Table 4 Washing fastness, softness and T% of different indigo blue formulations 3.6 FT-IR Test Cotton, ITS and ITT were selected for FT-IR test and analysis. According to Fig. 2 of FT-IR spectrum, ITS and ITT show the functional group absorption peak l (C= O) of the indigo blue at 1624 cm -1. Fig. 2 FT-IR spectrum of cotton, ITS and ITT

5 4. Conclusions References This study used three different indigo blue from polygonum tinctorium. Sodium hydrosulfite and thiourea dioxide were selected as reducing agents. Several test results make the conclusions are as follows : 1. According to the dyeing results (observation of E change), both sodium hydrosulfite and thiourea dioxide can work as effective reducing agents for baphicacanthus cusia, polygonum tinctorium and Indigofera tinctoria. 2. For repeated dyeing process, normally 3-minute dyeing process is a little better than that of the 1- minute process. It is also easier to reach dyeing saturation condition. 3. Most specimens show similar tendency with hue change after washing. Normally, the red and yellow hue fades faster after washing. 4. The washing fastness reveal average grade 3. The softness test shows the average value about 6 cm with slightly softness increasing after washing. 5. The effect of ultraviolet resistance for polygonum tinctorium with the sodium hydrosulfite and thiourea dioxide are all very good with UV T % 0.5 (super UPF 50+). 6. FT-IR spectrum of ITS and ITT show the functional carbonyl group (C=O) peak at 1624 cm -1 increased significantly, which proves that the indigo has been colored in the cotton fabric. 1. B. C. Liau, T. T. Jong, M. R. Lee, and S. S. Chen, J. Pharm. Biomed. Anal., 43, 346 (2007). 2. E. Campeol, L. G. Angelini, S. Tozzi, and M. Bertolacci, Environ. Exp. Bot., 58, 223 (2006). 3. C. L. Chen and Y. H. Ma, Beauty of Formosa- Dictionary of Taiwan Natural Dyeing,Taichung : Taichung County Culture Center (2002). 4. F. M. Ma, Taiwan Crafts, 67,16(1998). 5. M. Kawahito and F. M. Matrans, Taiwan Crafts., 6, 67 (2001). 6. G. K. Stoker, T. D. Cooke, and J. D. Hill, J. AGR. ENG.. RES., 71, 315 (1998). 7. T. Bechtold, A. Turcanu, S. Geissler, and E. Ganglberger, Bioresour. Technol., 81, 171 (2002). 8. H. M. Li, Journal of Xi an University of Engineering Science and Technology, 20, 378 (2006). 9. H. C. Huang and C. C. Wang, J. Hwa. Gang. Textile, 7, 384 (2000). 10. Y. J. Wei and S. L. Chai, Dyestuffs and Coloration, 43,12(2006). 11. E. G. Tsatsaroni and I. C. Eleftheriadis, Dyes. Pigments, 61, 141 (2004). 12. K. Schumacher, E. Heine, and H. Höcker, J. Biotechnol., 89, 281 (2001). 13. Q. S. Wang, W. A. Kopf, J. Marx, A. Bogdan, D. Polsky, and S. R. Bart, J. Am. Acad. Dermatol., 44, 767 (2001). 14. C. V. d. Keybus, J. Laperre, and R. Roelandts, J. Am. Acad. Dermatol., 54,86(2006).