Dyeing of ecru denim with onion extract. using natural mordant combinations

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Indian Journal of Fibre & Textile Research Vol. 2, June 2000, pp. 12-17 Dyeing of ecru denim with onion extract.

1 Indian Journal of Fibre & Textile Research Vol. 2, June 2000, pp Dyeing of ecru denim with onion extract. using natural mordant combinations H T Deo" & Roshan Paul Division of Technology of Fibres and Textile Processing, Department of Chemical Technology, University of Mumbai, Matunga, Mumbai , India Received 2 October 1998; revised received and accepted I March 1999 Ecru denim swatches were dyed with onion extract using natural mordants such as harda, tartaric acid and tannic acid separately and in combinations. Harda-tartaric acid combination was found to be the best followed by tannic acid -harda and tartaric acid- tannic acid combinations. Synergistic effect of mordant was observed while usi ng the binary combinations of mordants. Meta-mordanting gave the best results for harda-tartaric acid and tartaric acid-tannic acid combinations, while pre-mordanting gave the best results for tartaric acid-harda combination. There was an overall improvement in performance properties of the samples dyed with various c mbinations over that of the single mordanted and the control samples. This new technique has immense potential in the modem concept of natural denim wear dyed with natural dyes using natural mordants. Keywords: Ecru denim, Mordanting, Natural mordants, Onion extract, Synergism 1 Introduction The production of synthetic dyes involves many violent reactions, which are conducted at high temperature and pressure. The recent realization that the intermediates and chemicals used in synthetic dyes are toxic, and thus hazardous to human health and environment, has led to the revival of interest in the non-toxic and eco-friendly natural dyes 1.2. Natural dyes can exhibit better biodegradability and generally have a higher compatibility with the environmene. Natural dyes cover all the dyes derived from the plants, insects and minerals i.e. derived from natural resources'. Colour Index lists 2 natural reds, 6 natural oranges, natural blues,s natural greens, 28 natural yellows, 12 natural browns and 6 natural blacks. The majority of natural dyes needs a chemical in the form of a metallic salt to create an affinity between the fibre and the pigment. A mordant is now regarded as a chemical that can itself be fixed on the fibre which also combines with the dyestuff. Onion (Allium cepa) is a natural brown dye belonging to the Liliaceae family and originated in the middle east. The outermost dry papery skin of onion yields the dye c.r. Natural Yellow 10 which dyes wool and silk in a range of colours from golden yellow to "To whom all the correspondence should be addressed. Present address: 18 Safalya, Nath Pai Nagar, Ghatkopar (East), Mumbai 00077, Indi a copper red on application of mordants. These colours are of remarkable brightness and are fast to light and washing. The main colouring component in the skin of onion is 'Quercetin' which is chemically,, 7, ', -pentahydroxy flavone (C'H'007) and found as yellow crystals with m.p C. Also, there are some protocatechuic acid, tannins and anthocyanidins in the red and violet varieties of skin 6. The only problem with the natural dyes is that to obtain a full colour range, the mordants must be used and whilst the natural dyes are themselves generally harmless, the chemicals used for rnordanting the dyes are generally not environmentally acceptable. The metal contaminants in the spent bath have adverse effects on the environment 2. According to Durig7, 1.8 ppm of aluminium, 1-80 ppm of chromates, 1-2 ppm of iron, ppm of copper, ppm of zi nc and 2 ppm of tin in water systems can have adverse effects on fish and other aquatic animals. The sources of tannin and its role in dyeing of cotton are of great importance in this context l. The emergence of a new classification of natural mordants is inevitable, even though there is no mention about it in literature. This paper reports the dyeing of ecru denim swatches with onion extract using different natural mordants separately and in combinations (harda-tartaric acid, tartaric acid-tannic acid and tannic acid-harda).

DEO & PAUL: DYEING OF ECRU DENIM WITH ONION EXTRACT 1 2 Materials and Methods 2.1 Materials Ecru denim (/1 warp faced twill fabric) having the fabric construction details: 2x 19 ; x tex; 1.

2 DEO & PAUL: DYEING OF ECRU DENIM WITH ONION EXTRACT 1 2 Materials and Methods 2.1 Materials Ecru denim (/1 warp faced twill fabric) having the fabric construction details: 2x 19 ; x tex; 1. ounces/yard 2 and supplied by Arvind Mills Ltd, Ahmedabad, was used for the study. The fabric sample was not subjected to the processes affecting the natural grey colours. Control sample which was desized, scoured and dyed without using any mordant was also used for the comparison. Onion extract (C.I. Natural Yellow 10) was used for dyeing. Natural mordants such as tannic acid (supplied by Tetrahedron Ltd, Chennai), tartaric acid (suppled by s. d. Fine Chern Ltd, Boiser) and harda were used for the study. Hydrochloric acid, sodium hydroxide, sodium sulphate and tartar emetic, all supplied by Loba Chemie, Mumbai, were used. Lissapol 100X (an auxiliary) supplied by ICI India Ltd, Thane, was used. 2.2 Methods Desizing Ecru denim swatches were desized using 0.2% hydrochloric acid at 0 C for h. To avoid drying, the samples were covered with moistened fabric. The samples were washed thoroughly with water and dried Scouring Desized ecru denim swatches were scoured using % sodium hydroxide at 'boil for h, washed thoroughly with water and dried Mordanting Different combinations of natural mordants such as harda-tartaric acid (H-TR), tartaric acid- tannic acid (TR-TN) and tannic acid-harda (TN-H) were used. The ratio of mordants was varied from 0: 10 to 10:0 for each combination. The mordant bath was set for 10% mordant combination (on weight of the fabric), keeping the material-to-liquor ratio at I :0. The desized and scoured ecru denim swatches were introduced into the bath at 60 C and treated for 0 min. The temperature was then raised to boil and mordanting continued for another min. Samples were then taken out, squeezed and dried. The mordant combinations were applied to the substrate prior to dyeing (pre-mordanting); in the dye bath (metamordanting) so that mordanting and dyeing take place simultaneously; and after dyeing (post-mordanting). The tannic acid mordant was fixed on denim by treating with % solution of tartar emetic in cold for 0 min Preparation of Dye Extract 1 kg of dry papery outer skin of onion on bone dry basis (i.e. considering 10% moisture, I kg and 100 g of onion skin) was boiled in 10 litres of water for h, kept overnight, filtered and used as the dye extract Dyeing of Ecru Denim The samples were dyed in a laboratory open bath beaker dyeing machine, manufactured by Electronic and Engineering Company, Mumbai. The dye bath was prepared with onion extract (extract basis), keeping the material-to-liquor ratio at 1 :0. The material was put into the dye bath at 60 C, kept as such for 0 min and 20% sodium sulphate solution was then added to it. The temperature of the dye bath was raised to 90 C and dyeing continued for Ih.The material was then removed, rinsed well, squeezed, soaped with Lissapol 100X and air dried Colour Value Measurement All the samples were analysed on Spectraflash SF 00 computer colour matching system by Datacolor International, USA Fastness Properties The wash fastness of dyed samples was determined by the method described in BS EN 20 I 0-C 02: 199 (ref. II). Composite samples of 10 cmx cm size were subjected to treatment with gpl non-ionic soap at 0 C for min on a wash wheel. The samples were then removed, opened, washed and dried. Staining was then assessed on grey scale. The rub fastness of dyed samples was determined by the method described in BS EN ISO 10-X 12: 199 (ref. 11). Dry and wet rub fastness of the dyed samples were determined using the crock tester. Under the load of about 900 g, 0 strokes were given where the undyed fabric was rubbed against the dyed sample. Staining was then assessed on grey scale. The light fastness of dyed samples was determined by the method described in BS EN 2010-B 02: 199 (ref. 11). The fastness to light was tested using Heraeus Suntest cps, where the samples were partially exposed to the xenon arc lamp for 8 h. The colour change was evaluated from the grey scale by giving appropriate gradings.

1 INDIAN J. FIBRE TEXT. RES., JUNE 2000 Results and Discussion Ecru denim, mordanted by pre-mordanting, metamordanting and post-mordanting processes, was dyed with onion extract.

3 1 INDIAN J. FIBRE TEXT. RES., JUNE 2000 Results and Discussion Ecru denim, mordanted by pre-mordanting, metamordanting and post-mordanting processes, was dyed with onion extract. The different mordant combinations, viz. harda-tartaric acid, tartaric acid-tannic acid and tannic acid-harda, selected were natural in origin. Out of these three natural mordants used in dyeing, harda (C.1. Natural Brown 6) can also be used as a dye. Hence, the discoloration of the denim fabric by harda has been determined in terms of K/S value, which is subtracted from the total KIS value of various combinations containing harda such as hardatartaric acid and tannic acid-harda. Table I gives the K/S values of the control sample (desized,scoured and dyed with onion extract without using any mordant), single mordanted samples jind combination- dyed samples. In the case of pre-mordanted H-TR dyed samples, it was found that the substrate H-TR (0: 10), where tartaric acid was the only one mordant, produced K/S value of. and the substrate H-TR (l0:0), where harda was the sole mordant, produced K/S value of.8. Here, the contribution of harda was 2.1 as compared to the KIS value of 2. 1 for the control. The highest K/S value of 7.20 observed for the substrate H-TR (:), where the contribution of harda was 2.08, can be attributed to the synergistic effect of the mordant combination. In case of meta-mordating, the single mordanted substrate H-TR (0: 10) produced the K/S value of.86 and the substrate H-TR (10:0) produced the K/S value of.66, where the contribution of harda was 2.I.The KJS value of 11.8 for the substrate H-TR (2:8), where the contribution of harda was 1.88, was the highest, showing the synergistic effect of this combination. In the case of post-mordanting, the single mordanted substrate H-TR (0: 10) produced the KlS value of 2.61 and the substrate H-TR (10:0) produced the K/S value of 2.6, where the contribution of harda was 2.1. The synergistic effect was found in case of substrate H-TR (:6) with K/S value of 6.9, where the contribution of harda was 1.9. In the case of pre-mordanted TR-TN dyed samples, it was found that the substrate TR-TN (0: 10), where tannic acid was the only one mordant, and the substrate TR-TN (10:0), where tartaric acid was the only mordant, produced the K/S values of.16 and. respectively over the K/S value of 2.1 for the control. All the combination dyed substrates produced higher K/S values with.99 for the substrate TR-TN ( :) being the highest, showing synergistic effect. In the case of meta-mordanting, the single mordanted substrates TR-TN (0: 10) and TR-TN (10:0) produced the KIS values of.27 and.86 Substrate Table I-KIS values of substrates dyed with onion extract using different mordant combinations at 00 nm Am". IUS Pre-mordanting Meta-mordanting Post-mordanting H-TR" TR-TN TN -H" H-TR" TR-TN TN-H" H-TR" TR-TN TN-H" Control : : : : : : ,8.86 6: : : : : H-TR-Harda- tartaric acid combinati on TR-TN-Tartaric acid-tannic acid combination TN-H-Tannic acid-harda combination "The KlS values for these combinations are the sum total of KIS contributed by onion extract and harda, where the contributions of harda are: 1.78, 1. 88, 1.9, 1.9,2.08,2. 10,2.26,2.2, 2.8 and 2.1 parts of harda in these combinations. when the proportion of harda in a particular combination varied from I to 10.

DEO & PAUL: DYEING OF ECRU DENIM WITH ONION EXTRACT 1 respectively, whereas the substrate TR-TN (6:) showed the synergistic effect with a KIS value of.17.

4 DEO & PAUL: DYEING OF ECRU DENIM WITH ONION EXTRACT 1 respectively, whereas the substrate TR-TN (6:) showed the synergistic effect with a KIS value of.17. In the case of post-mordanting, the single mordanted substrates TR-TN (0: 10) and TR-TN (10:0) produced the K/S values of 2.66 and 2.61 respectively, while the synergistic effect was observed with the substrate TR-TN (:), showing a KlS value of.8. In the case of pre-mordanted TN-H dyed samples, the single mordanted substrate TN-H (0: 10), where harda was the sole mordant, produced a KlS value of.8 where the contribution of harda was 2.1 and the substrate TN-H ( 10:0), where tannic acid was the only mordant, produced a KlS value of.16 as compared to KlS value of 2.1 for the control. All the combination dyed samples produced higher KIS values. The substrate TN-H (: 6) with a KIS value of 7.10, where the contribution of harda was 2.10, showed synergistic effect. In the case meta-mordanting, the single mordanted substrate TN-H (0: 10) showt(d the KIS value of.66, where the contribution of hard a was 2. 1, and the substrate TN-H ( 10:0) showed the KlS va lue of.27, whereas the synergistic effect was observed for the substrate TN-H (: 7) showing a KlS value of.. Here, the contribution of harda was In the case of post-mordanting, the KlS value of single mordanted substrate TN-H (0: 10) was found to be 2.6, where the contribution of hard a was 2.1 and the substrate TN-H( I 0:0) showed KlS value of The substrate TN-H (:6) showed synergistic effect with a KIS va lue of.92, where the contribution of harda was Thus, it was concluded that for H-TR and TR-TN combinations, meta-mordanting produced the best results, whereas in the case of TN-M combination, pre-mordanting produced the best results. H-TR combination was found to be the most effective one followed by TN-H and TR-TN combinations, as observed fro m the KIS values. The increase in the KIS value observed JI1 combination dyed substrates' over that of the single mordanted and the control samples can be attributed to the formation of complexes involving quercetin (C l s H IO 0 7 ) of the onion, tannic acid (C76Hs206) 12, tartaric acid (CH )12 and hard a, containjng myrobalan tannin 1.1 which is a naturall y occurring glycoside found in the peel of the dried fruit of Myrobalanus chebula and is a mixture of chebulinic acid (CI H20 27), chebulic acid (CI H I201 1), corilagin (C27H220IS) and chebulagic acid (CIH0027) ' In case of H-TR substrate, the complexes involving quercetin, harda and tartaric acid might have improved the KlS values, whereas the complexes involving quercetin, tartaric acid and tannic acid in case of TR-TN substrate and those involving quercetin, tannic acid and harda in case of TN-H substrate might have also improved the KlS values over those of the single mordanted and the control samples. Table 2 shows the fastness properties of various dyed samples. In all the cases, there was an overall improvement in the fastness properties of combined dyed samples over that of control sample. This may be attributed to the formation of bigger crystals. The light fastness of H-TR dyed samples was better than that of the control with a rating of, the substrates H-TR (: 6 and :) having a rating of being the best. In the case of dry rubbing, the substrates H-TR (:6, : and 6:) with a rating of were found to be the best in comparison with the rating of for the control sample. Whereas the same substrates with a rating of, compared to 2- for the control sample, produced the best wet rub fastness. In the case of wash fastness, the substrate H-TR (:) with a rating of, compared to 2- for the control, produced the best fastness. In the case of meta-mordanted samples, the substrates H-TR ( I :9, 2:8, 7:, 8:2 and 9: I) with a light fastness rating of, compared to for the control sample, produced the best results. The substrates H-TR (2:8, : and 8:2) with a rating of produced the best dry rub fastness results, while the substrates H-TR (2:8, :, 6:, 7: and 8:2) having a rating of showed the highest wet rub fastness. In the case of wash fastness, the substrates H-TR (2:8, 6: and 8:2) having rating of showed the best results. The light fastness ratings of post-mordanted samples show that the substrates H-TR (2:8, :7, :6 and 6:) with a rating of, compared to for the control, produced the best results. In the case of dry rub fastness, the substrates H-TR (:6 and :) with a rating of produced the best results, while the substrates H-TR (: 7, :6, :, 6: and 8:2) with a rat ing of produced the best wet rub fastness. The wash fastness of substrates H-TR (:7 and :6) having a rating of was best among all the samples. The light fastness of pre-mordanted samples showed that the substrate TR-TN ( :) with a rating

5 16 INDIAN J. FIBRE TEXT. RES., JUNE 2000 of produced the best fastness. In the case of dry rub fastness, the substrates TR-TN (:6, :, 6: and 10:0) with a rating of showed the best results, while the wet rub fastness of substrates TR-TN (:6, :, 6:, 9: 1 and 10:0) with a rating of was good. In the case of wash fastness, the sub trates TR-TJ-I (:7 :6, :, 6: and 9: I) with a rating of showed the best results. Substrate Table 2-Fastness properties of substrate dyed with onion extract using harda-tartaric acid, tartaric ~cid- t annic acid and tannic acid- harda mordant combinations Pre-mordanting Light Rub Wash fastness fastness Fastness Dry Wet Meta-mordanting Light Rub Wash fastness fastness fastness Dry Wet Post-mordailli ng Light Rub Wash fastness fastness fastness Dry Wet Harda-Tartarllc acid Control H-TRO:IO H-TR 1:9 H-TR 2:8 H-TR :7 H-TR :6 H-TR : H-TR 6: H-TR 7: H-TR 8:2 H-TR 9:1 H-TR 10: Tartaric acid-tannic acid Control TR-TN 0:10 TR-TN 1:9 TR-TN 2:8 TR-TN :7 TR -TN :6 TR-TN : TR-TN 6: TR-TN 7: TR -TN 8:2 TR-TN 9:1 TR-TN 10: Tannic acid-harda Control TN-H 0: 10 TN-H 1:9 TN-H 2:8 TN-H :7 TN-H :6 TN-H : TN-H 6: TN-H 7: TN-H 8:2 TN-H 9: 1 TN-H 10:

DEO & PAUL: DYEING OF ECRU DENIM WITH ONION EXTRACT 17 In the case of meta-mordanted samples, the substrates TR-TN (: and 6:) showed the best light fastness with a rating of.

6 DEO & PAUL: DYEING OF ECRU DENIM WITH ONION EXTRACT 17 In the case of meta-mordanted samples, the substrates TR-TN (: and 6:) showed the best light fastness with a rating of. The dry rub fastness of substrate TR-TN (6:) was the best among all the substrates with a rating of, whereas the substrates TR-TN (:6, :, 6: and 8:2) with a rating of showed the best wet rub fastness. The wash fastness of the substrates TR-TN (:7, : and 6:) with a rating of was better than those of the other substrates. The light fastness of post-mordanted samples show that the substrates TR-TN (:6, :, 6: and 7:) with a rating of showed the best light fastness. In the case of dry rub fastness, the substrate TR-TN (:) with a rating of was found to be superior to other substrates, whereas the substrates TR-TN(2:8, :7, :6, : and 6:) with a rating of produced. superior wet rub fastness. The substrate TR-TN ( :) with a rating of - showed the best wash fastness. Table 2 shows that the li ght fastness of premordanted samples TN-H (:6 and :) with a rating of was excellent. The dry rub fastness of substrate TN-H (:6) was superior to that of the other substrates, while the substrates TN-H (: 7, :6 and 9: 1) with a wet rub fastness rating of produced the better results compared to other samples. The wash fastness of the substrates TN-H (2:8, :7, :6 and 9: I) having a rating of was superior to those of the other substrates. In the case of meta-mordanting, the light fastness of substrates TN-H ( :7 and. :6) with a rating of was found to be superior to those of the other substrates. In the case of dry rub fastness, the substrates TN-H (2:8, :7 and :6) with a rating of showed the best results, while the substrate TN-H (:7) having a wet fastness rating of was superior to other substrates. The wash fastness of substrates TN H (2:8, :7, :6 and 7:) was found to be superi or to those of the other substrates. In the case of post-mordanting, the substrates TN H ( :7, :6, :, 6: and 7:) having a light fastness rating of produced good results. The dry rub fastness of substrates TN-H (2:8, :7, :6, : and 7:) with a rating of was found to be superior to those of other substrates, whereas the substrates TN- H (:6, : and 6:) with a rating of produced the best wet rub fastness. In the case of wash fastness, the substrates TN-H (:7 and :6) with a rating of - showed superior results in comparison to other substrates. It was observed that with the increase in KlS values, the various performance properties of the substrates also improved. This can be attributed to the bigger crystals formed due to the complex formation involving quercetin of onion and various mordants. Conclusion The natural mordants showed synergistic effect when used in binary combinations for the dyeing of onion on denim. Harda-tartaric acid combination was found to be the most effective followed by tannic acid-harda and tartaric acid-tannic acid combinations. Meta-mordanting produced the best results for hardatartaric acid and tartaric acid-tannic acid combinations, whereas pre-mordanting produced the best results for hard a-tartaric acid combination. There was an overall improvement in the performance properties of the samples dyed with various combinations over single mordanted as well as control sample. References I Gupta D R, Text Dyer Printer, 2 (1990) Dalby G, J Soc Dyers Colollr, 109 (199) 8. Tsatsaroni E G & Eleftheriadis I C, J Soc Dyers Colollr, 110 (199) 1. Venkidu Samy P, Raj a A S M & Ramsingh G, Man Made Text India, 1 (1998) 12. Gulrajani M L & Gupta D, Natllral Dyes and their Application to Textiles (Department of Textile Technology, lit, New Delhi), 199, Gulrajani M L, Gupta D B, Agarwal V & Jain M, Indian Text J, 102 (1992) Durig G, Rev Prog Color, 7 ( 1976) Tubbs M C & Daniels P N, Textile Terms and Definitions (The Textile Institute, Manchester), 199 1, 8. 9 Peters R H, Textile Chemistry, Vol II (Elsevier Publishing Company, Amsterdam), Hsieh Y L, Thompson J & Miller A, Text Res J, 66 (1996) 6. II Hall A J, J Soc Dyers Colollr, 112 (1996) Th e Merck Index, l2'h edl/, (Merck & Co, Inc, Whitehouse Station, NJ), 1996, Yamaguchi K, Spectral Data of Natllral Prodllcts, Vol I (Hirokawa Publishing Co, Inc, Tokyo), 1970, 128.

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