Optimisation Of Extraction And Dyeing Application Process Of Juglan Regia For Sustainable Dyeing Practices In Garhwal Himalayas Dr. Nidhi L. Sharda, Fashion & Textiles Research Consultant, Foster city, CA Dr. Deepali Rastogi, Department Of Fabric and Apparel Science, Lady Irwin College, Delhi University India Abstract The Garhwal Himalayan region is gifted with a variety of plants, which have been considered as a source of number of natural products. Decades ago these plants were used by Bhotiya people for wool dyeing. The art of dyeing with these natural dyes, was limited to a few people and was kept a big secret by those who excelled by this art. The indigenous practice has declined manifold due to invasion of use of synthetic dyes. Today also the diversity, copiousness as well as uniqueness of the plant component in various habitats retained sound and aesthetic environment of the Garhwal Himalayas. Most of the plants of the Garhwal region are well known for their heterogeneous uses. However a number of plants found in abundance are still in adequately explored and need a thorough chemical investigation for their proper utilization. This paper deals with experimentation extraction, standardization and application on for its sustainable viability in small scale dyeing units of Garhwal Himalayas and hence uplifting the local craft of the region. was identified for the experimentation from the explored flora of the Garhwal Himalayas. Physico chemical analysis of the raw material was carried out in order to standardize extraction method as raw material for the dye. The parameter studied were color, physical appearance, ph, moisture content, total ash content, acid insoluble content and water soluble extractive value. Extraction and application of the dye was carried out and the conditions of extraction and application on wool were standardized by studying the effect of time, ph and temperature on degree of extraction and percentage shade on degree of exhaustion of the dye by the substrate. In this study an effort was made to develop and standardize natural dye for sustainable practices with view to revive natural dyeing in woolen industry of Garhwal Himalayan region. This study infers that the hulls of, which are otherwise waste after the fruit is taken out has significant potential for being used as natural dye as it possess good light fastness, good to excellent washing fastness and good to fair rubbing fastness. It is found in abundance and has good affinity for wool dyeing. This technical intervention will help in up gradation of the unorganized less privileged textile craft sector by using indigenous natural dyes keeping environmental concerns in mind. Keywords: Textiles,, Natural Dye, extraction, sustainable dyeing, woolen dyeing 1. Introduction In last few decades use of non-sustainable synthetic dyes was part of every big or small textile industry. Research reveals that there are certain forbidden amines, including benzamine. The dyes and pigments based upon these amines contain azo groups that are considered carcinogenic and therefore non eco-friendly. Some of them may not be carcinogenic but have been included in the list of forbidden dyes due to their toxic nature to human life. (Chavan, 1995) These banned dyes are a great challenge to the textile world because today market demands something more beyond colors and that is safety and Sustainability, the dyes that would not affect human health and ecosystem. In recent years a growing interest in the revival of natural dyes has been manifested. This interest is a result of the worldwide movement of sustainability to protect the environment from indiscriminate exploitation and pollution. The synthetic dyes that produce a large variety of colors also produce toxic waste which is hazardous. (Gulrajani, 1992) Garhwal region is at an advantageous position since the region holds a rich reservoir of natural resources with potential products. Garhwal Himalayan region is full of a variety of dye yielding plants. (Atkinson, 1989). Decades ago these plants were used by local folk for textiles dying of woolen articles which are traditional craft of Bhotiya community in the region. (Chawala, 1996) Synthetic dyes were introduced as a government movement because the State Government had put the restrictions on plucking certain plants as they are rare and some of them have medicinal utility. Slowly these people shifted from traditional vegetable dyeing to synthetic dyeing because of ease of dyeing and ease of availability of these dyes. Most of the plants of the Garhwal region are well known for their heterogeneous uses. However a number of plants found in abundance are still in adequately explored and need a thorough chemical investigation for their proper utilization. (C.S.I.R, 1985) www.borjournals.com Blue Ocean Research Journals 33
Revival of the art of natural dyeing in the woolen industry of Garhwal using available indigenous natural resources could significantly result in much higher value addition to the existing woolen products with sustainable craft cluster. The present study was targeted to explore some of the high altitude dye yielding plants that can be a sustainable alternative to the health hazardous banned dyes. 2. Objectives This paper deals with experimentation extraction, standardization and application on for its commercial viability for dyeing and implementation for the revival of natural dyeing art and hence uplifting the local craft. The objectives of the study are: 1. To extract and optimize extraction process of outer skin of (Akhrot) 2. Optimization of dyeing technology on the wool fiber. 3. Evaluation of the dye. was identified for the experimentation, from the explored flora of the Garhwal region based on the following criteria: a) Ease of availability. b) Based on by-products c) Found in abundance. d) Commercial viability., a large deciduous, monoecism tree with tomentose shoots, found throughout the Himalayas at altitude of 3000 to 11000 feet. Fruit is green drupe with leathery exocrap, hard, woods wrinkled, two valved enclosing four lobed corrugated oily seed. The western region of Himalayas is well adapted for growing walnut. In India Kashmir is the principal walnut growing state. Uttarakhand and Himachal Pradesh are other walnut growing states but the quality of production is not that good here. They grow easily on hill or mountainside at an elevation of,000 to 7,000 feet. Green hulls separated from the mature walnut contain 0. to 0.8 % ascorbic acid. Unripe fruit and other parts of the plant contain a substance, which reduces indophenols dye. This substance has been identified as alpha- hydrojuglon glycosides (C6H18O8), which on hydrolysis releases alpha- hydrojuglon and glucose. The glycoside forms up to 15%of total indophenols dye. Another reducing substance is flavones. 3. Physico Chemical Analysis Of The Raw Material Phisico- chemical analysis of raw material was carried in order to standardize extraction methods as raw material for dyes can be procured from various sources that can be significantly different in geographical and climatic factor thus making difference in vegetation and phisico chemical property. The parameters studied were color, physical appearance, ph, moisture content, total ash content, acid insoluble content, and water-soluble extractive value. Results of physico- chemical analysis of is given in table no 1. S.No. 1 Physico Chemical Parameter Color of the Raw Material 2 Physical Appearance Hulls 3 Moisture Content (%) 9.11 Brown Hulls (Dried) Soft Fruit Total Ash Content (%) 5.55 5 Total Acid Insoluble Ash Content (%) 1.6786 6 Water-Soluble Extractive Value (%) 39.05 7 Ph. At 0.1%Solution 7.73 Table 1: Physico- Chemical Analysis of the Raw Materials. Optimization Of The Extraction Method The conditions of extraction were standardized by studying the effect of time, ph, and temperature on degree of extraction. The standardized recipe, Juglan regia, is as follows. M: L = 1:10 ph = 7 Temperature =100 o C Time =30 minutes Method of Extraction Raw material was crushed and ground to fine particles. It is then soaked overnight in cold water. Extraction at ph 7 was selected as in alkaline extraction the raw material release large amounts of tannins, which destroy, color quality. Material to liquor ratio was maintained to 1:10. Boiling the raw material for 30 minutes carries out further extraction. After 30 minutes extract is filtered and residue is discarded. This is mother liquor for making dye. Drying Drying was done in low temperature. Dried material was collected and grounded to fine dye powder. Yield in terms of weight was found to be approximately 26 grams. Physico- Chemical Analysis of the Dye powder is shown in Table 2 www.borjournals.com Blue Ocean Research Journals 3
absorbance Journal of Engineering, Computers & Applied Sciences (JEC&AS) ISSN No: 2319-5606 S.No. Physico Chemical Parameter 1 Dye Color Juglan regia Black Brown 2 Physical Appearance Powder 3 Moisture Content (%) 3.75 Total Ash Content (%) 30.912 5 Total Acid Insoluble Ash Content (%) 1.705 6 Water-Soluble Matter (%) 6.11 7 Ph At 0.1%Solution 7.91 8 Wave Length Of Absorbance 511 Nm Table 2: Physico- Chemical Analysis of the Dye 5. Absorbance Of Juglan Regia Absorbance of dye solution of.01% dye powder in water is shown in Figure 1. It is evident that absorbance starts at 1056.00 nm and starts increasing sharply. In visible region there is no clear peak, although at 365.00 nm slight peak with absorbance of 2.02 can be seen. This can be inferred that brown color in Juglan regia is because of mixture of tannins and other plant pigments which do not show absorbance in the visible region. Time = 30 Min % Shade = 15 On the weight of the material 15 % of the dye was taken. It was made into smooth solution by adding water in the ratio of 1:30. ph was maintained by adding small drops of organic acid (CH3COOH), drops of acid are added till required level of ph was attained. Further temperature of dye bath was increased to 80 o C. Scoured wool hanks were immersed into the dye bath. Dyeing was carried for 30 minutes with continuous stirring. 7. Effect Of Mordants Mordanting did not have much effect in degree of intensity or change in hue in. The unmordanted sample was of brown in color. On Plate.21: Shades with different mordant on Akhrot Dye examination of a*b* plots of the samples it was observed that the samples dyed with the mordanting shift towards green blue zone (Figure 2). Figure 2: Shades with different mordant Unmordanted Pre mordant with Aluminium Sulphate + tartaric acid on ABSORBANCE CURVEI()0.01% dye in water.5 Pre mordant with Aluminium Sulphate + Tartaric acid Post mordant with Ferrous Sulphate 3.5 3 Pre mordant with Aluminium sulphate + Tartaric acid post mordant with Copper sulphate 2.5 2 1.5 Series1 Pre mordant with Aluminium Sulphate + Tartaric acid Post mordant with Stannous Chloride 1 0.5 0 0 200 00 600 800 1000 1200 wave length(nm) Figure 1: Absorbance 6. Application Of Natural Dye Hanks of wool were boiled at the temperature of 80oC in 25% solution of sanodozniti (nonionic detergent) for 5 minutes. Finally hanks were removed from the solution washed and dried. This is scoured wool a prepared substrate for wool dyeing. Optimization of dyeing Method for wool: : M: L = 1:30 ph = 5 Temperature 80 o C On mordanting with tartaric acid and alum color space shifts slightly from the center point indicating all most mixed zone of yellow red green and blue and can be concluded that mordanting with Tartaric acid and alum does not change hue of the dye. However, effect on color value was evident as original hue became little bit darker in shade, this can also be seen by K/S values. Material, which was subjected to pre mordanting with aluminum Sulphate and tartaric acid and post-mordanted with ferrous sulphate, gave black-brown color. It is evident in a*b* plot also that, color space shifts intensely towards blue green zone indicating big change of color to blue green. Similar pretreatment and post-mordanting with copper sulphate gave dark brown color. With similar pre-treatment again and post treatment with stannous chloride had no significant change in value or intensity of the color as color space shifts slightly from the center www.borjournals.com Blue Ocean Research Journals 35
00 20 0 60 80 500 520 50 560 580 600 620 60 660 680 700 K/S Journal of Engineering, Computers & Applied Sciences (JEC&AS) ISSN No: 2319-5606 point indicating mixed zone of yellow red green and blue. Color palette obtained can be seen in (Figure 2) The L* values of the samples mordanted with tartaric acid and alum and samples post-mordanted with stannous chloride did not change whereas L* values of the samples decreases significantly when postmordanted with ferrous sulphate and copper sulphate, indicating darker tones. It is evident from the Figure 3 that in case of dye, mordanting generally deepens the shades of the dye. All samples on mordanting showed trend of increased K/S values which means deeper shades (Figure ). the fact that light affected the dye molecules, setting in motion some photochemical reaction, which brought about the darkening or discolouration of the samples. Stout (1970) stated that color change might be due to fading, darkening, change in hue or bleeding. Comparing the contrast between the exposed and unexposed portion with grey scales rating of the samples was done 1) Color Fastness to Light Light fastness of un-mordanted sample is as it failed to withstand 5th cycle. Samples pre-mordanted with Aluminum sulphate and tartaric acid, samples postmordanted with ferrous sulphate, samples postmordanted with copper sulphate, and samples mordanted with stannous chloride also posses rating of on grey scale. Light fastness of was rated good and effect of mordanting on the light fastness property was not very much significant. Experiments Blank Pre Al +T.A Post CuSO Table 3: Color Fastness to Light Figure 3: L*a*b* Values of.00 3.50 3.00 2.50 2.00 1.50 1.00 0.50 0.00 K/S Values Vs Wave length (Akhrot ) Wave Length (NM) Figure : K/S values of Un-mordanted Aluminium Sulphate & Tartric acid Copper Sulphate Stannous Chloride Ferrous Sulphate 8. Product Evaluation During the testing of light fastness of samples it was observed that instead of fading, some of the samples became darker on exposure to light. This could be due to 2) Color Fastness to Wash showed rating of /5 in grey scales for color change and was rated 5 for staining in adjacent fabrics. Samples pre-mordanted with aluminum sulphate and tartaric acid showed similar rating as of unmordanted samples. Post treatment with ferrous sulphate, post treatment with copper sulphate and post treatment with stannous chloride showed rating equal to 5 for both color change and staining. It can be inferred that wash fastness of is good to excellent. Postmordanting with ferrous sulphate, stannous chloride and copper sulphate further improves wash fastness of the dye. Experiments *CC *CA Blank / Post CuSO / www.borjournals.com Blue Ocean Research Journals 36
Table : Colorfastness to Wash *CC=color change, *CA=color in the adjacent fabric 3) Color Fastness to Rubbing Dry rub fastness rating of the un-mordanted sample of was found to be /5 while wet rubbing fastness rating was 3/ which indicates that rubbing fastness of is fair to good. Samples premordanted with aluminum sulphate and tartaric acid rated similar dry as well as wet rub fastness as of unmordanted sample. Post treatment with ferrous sulphate showed rating of /5 for dry rub fastness while wet rubbing fastness was found to be 3 indicates fair rubbing fastness. Whereas post treatment with copper sulphate and stannous chloride showed rating of 5 for dry rubbing fastness and and 3/ for wet rubbing fastness. Dry rub fastness of was found to be good to excellent whereas wet rubbing fastness is fair to good. Post-mordanting with ferrous sulphate decreases rubbing fastness of the dye. Experiments Dry Wet Blank /5 /5 Pre Al + Tartaric acid 5 /5 /5 / Post CuSO / Table 5: Colourfastness to Rubbing 9. Bulk Extraction Of Natural Dyes In The Pilot Plant To study the viability for mass production raw material was extracted in large scale. The bulk extraction was done using standard recipe, extraction and drying was done for 5 Kg. of the raw material. The percentage yield was found to be little less than laboratory experiments. The reason for less percentage yield was that, there was lot of wastage in the milling machine while grinding the raw material. The significant amount of wastage was also found because of manual method of filtering bulk extract from the pilot plant extractor which was not efficient in terms of filtering bulk quantity. This study infers that has significant potential for being used as natural dye. It is found in abundance and has good affinity for wool dyeing. The dye can be stored in the dry form and therefore is not seasonal dependent. It can be a sustainable solution for a small craft based woolen industry of Garhwal Himalayas. References [1] Atkinson, E.T. 1989, Economic Botany of Himalayan Region, Cosmo Publication, New Delhi, pp. 773-778. [2] C.S.I.R. 1985, The Wealth of India-Raw Materials, Publication and Information Directorate, New Delhi, vol. 6, pp. 23 [3] Cannon, M. et al. 1997, Dye Plants and Dyeing, A&C Black and Royal Botanic Gardens, kew, pp. 82, 26, 28. [] Chavan, R.B. 1995, Revival of natural dyes: a word of caution to environmentalist, Clothes line, vol. 8, no., pp. 96-100. [5] Chawala, J. 1996, Bhotia Carpets- New Notes to an Unsung Legacy MSc. Thesis, Lady Irwin College, New Delhi. [6] Gulrajani, M.L.1992, Introduction of natural dyes, Natural Dyes and their application to Textiles, Indian Institute of Technology, New Delhi. [7] Stout E. 1970, Introduction to Textiles, 3rd ed, Wiley publication, the University of Virginia, pp. 223-300. [8] Victoria, A. et al. 1999, Colors from common weeds, Paper submitted to National Convention on Natural Dyes, Department of Textiles Technology, IIT New Delhi, pp 7 10. Conclusion In this study an effort was made to develop and standardize natural dye for commercial application with view to revive natural dyeing in woolen industry of Garhwal Himalayan region with sustainable approach. www.borjournals.com Blue Ocean Research Journals 37