Preparation and Application of Natural Dye Extracted From Rubia Cordifolia on Cotton Fabrics for UV Protection

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1 Preparation and Application of Natural Dye Extracted From Rubia Cordifolia on Cotton Fabrics for UV Protection V.Yamuna #1, S.Sudha *2 #1,*2Department of Fashion Technology, PSG College of Technology 2 Abstract - This study concentrates on the preparation of dye from the natural extract of Indian madder plant (Rubia Cordifolia) and its application on cotton fabrics in order to evaluate the Ultraviolet protection factor. Indian madder root powder was purchased and extracted using ethyl acetate and the extracted dye solution was homogenized and centrifuged to produce the dye with reduced particle size. Before applying the dried dye powder on cotton fabric, the dye solution was analysed under spectroscopy to identify the UV visible spectrum which shows peak in the level of nm and the dye was analysed for particle size measurement using Atomic force microscopy (AFM), where the diameter range was obtained between nm. The dye powder was then dyed on cotton fabrics and examined for Ultraviolet protection factor which shows excellent UV protection. The dyed cotton fabric samples were also tested for wash, light and rubbing fastness and showed better results. Keywords - Indian madder Dye, UV Protection, Dye particle size, Fastness Property, Cotton fabric I. INTRODUCTION Ultraviolet radiation (UVR) is an electromagnetic radiation which is emitted by the natural or artificial sources. The UVR spectrum can be subdivided either as near UV ( nm), middle UV ( nm) and vacuum UV regions ( nm) by physicists, or as UVA ( nm), UVB ( ), UVC ( nm) and UVD (100-10nm) regions by biologists [1]. Among these UV spectrum, UVA and UVB rays will damage the human skin and thereby causes skin cancer. The study shows that 90% of skin cancers and premature aging are mainly due to UV exposure. Hence, Skin Cancer Foundation considers clothing to be the most safe and effective tool to defend our body by fighting against skin cancer and aging. Thus, several researches have been carried out and product has been developed for the past ten years on protecting the skin using fabrics against Ultraviolet radiation. In addition, many UV absorbers have been on the market for over twenty years to protect various substrates (tires, coated fabrics, etc.) against UV degradation or to improve the light fastness of the product. These developed fabrics can reflect, absorb and scatter the incident solar wavelengths that reach the earth's surface and protects from damages. This protection through fabric depends on fiber composition, fibre moisture content, type of dye used, concentration of dye applied, use of optical brighteners and UV protective agents. Among these various methods, the incorporation of protective agent through dyeing, printing and finishing gives better effect than using heavyweight fabrics which are not suitable for summer conditions [2]. The major drawback with the conventional dyeing, printing and finishing method is the fastness of the applied agent and amount of protective agent per unit area available for the application. This pave way for the use of nano dyeing process which reduces the particle size of dyes smaller than 100nm [3]. This nanodyeing process gives higher UV protection by producing deeper shades by easy penetration and availability of more dyes per unit area on fabric. 215

2 It is also observed that currently demand for UV protective textiles are highly satisfied by using synthetic dyes which in turn leads to environmental problems. This issue can be overcome by using the natural agents which has inherited UV protective property. Natural dyes are biodegradable, non-harmful, eco-friendly in nature, producing highly, attractive and smooth shades [4]. Studies show that various natural dyes like Indian Madder, Indigo, Turmeric, Henna, Logwood, French marigold and knot grass etc. are identified as UV protective agents. Among these plants, Madder has been a promising plant for dyeing from the ancient times and worked upon to produce red dyed textiles of varying characteristics with the help of advance techniques and mordants [5]. Madder roots contain dye present in the free or bound glucosides which are anthraquinone derivatives mainly purpurin (CI-75410) and munjistin (CI-75370). The roots also contain small amount of xanthopurpurin (CI-75340), pseudopurpurin (CI-75420), nordamncanthal and rubiadin as shown in Fig. 1 [6]. Fig. 1 Chemical compounds of Rubia Cordifolia Indian madder extract is also used in most of Sun block creams as it provides protection against broad spectrum of UV A & UV B radiation. Reference [7] shows excellent UV protection on linen and Hemp fabrics dyed with Indian madder. Thus an attempt has been made in this research to develop the dye with reduced particle size of Indian Madder root extract for applying it on cotton fabric inorder to get protection against UV radiation. II. MATERIALS AND METHODS Materials Plain woven bleached cotton fabric of 40 s was purchased from textile mill, Indian madder root powder, Casein enzyme, Ethyl acetate, dye fixing agents and other chemicals were used. Methodology Dye Extraction 20g of Indian madder root powder was taken and added with 100ml of Ethyl Acetate for extracting the dye solution. This mixture was refluxed for 4 hrs at 70 o C and the mixture was poured on filtering apparatus to filter the dye. Then the dye solution was taken for further processes. Homogenizing The extracted dye solution was taken in a beaker and homogenized in High Speed Homogenizer at F level (F Level = 33,000 RPM/min) for 12 minutes to reduce the dye particle size. The homogenized dye solution was then centrifuged for 15 minutes at 6000rpm/min to settle down large particles and the clear solution was dried using spray dryer. The dye solution was then analyzed for UV absorbency spectrum using T90+UV/VIS Spectrometer and the dye powder was taken to evaluate the particle size using Atomic force microscopy (AFM). Pretreatment of cotton fabric using Enzyme Bleached cotton fabric samples were soaked and washed in water using 2% liquid soap for one hour at 60 c.then the samples were treated with 4% Casein enzyme at C for 3 hours and Sodium hydroxide was added to maintain the ph of the bath to 8.5. After pretreatment, the samples were boiled in water for 10 minute to deactivate enzymes. 216

3 Casein is the milk protein and in ancient days, fabrics were treated with cow or buffalo milk before dyeing inorder to improve the dye absorbency of fabric [8]. Dyeing process Optimized dye concentration of 25% Indian madder dye extract at 40:1 M:L ratio were boiled for one hour and filtered. Then the dye solution, tannin extract and the enzymes were taken in the ratio of 2:1:1. The moist fabric sample was immersed in the dye bath for 3 hours at a temperature of C and 1% calcium carbonate was added to increase the brightness and 5% of sodium hydroxide was added to solubilize alizarin and purpurin as they are soluble in alkaline medium. The ph of all the dye baths was maintained between ph as dyeing process will take place in alkaline condition. Dye fixation was done by dipping the dyed samples in 5% ferrous chloride solution with M:L ratio of 40:1 for 30 minutes. Then the fabrics were washed in cold water and shade dried. Color fastness test Color fastness of dyed samples was assessed for washing, light and rubbing fastness property according to IS standards IS , IS: 2454:1985 and IS UV analysis UV protective activity of dyed fabric samples were carried out under the standard AATCC test method 183: Transmittance or Blocking of Erythemally Weighted Ultraviolet Radiation through Fabrics developed by AATCC Committee RA106. UPF of the dry and wet samples of dyed cotton fabric samples were calculated with the Transmittance and Blocking % of UVA & UVB radiation. III. RESULT AND DISCUSSION UV Visible Spectroscopy Analysis Homogenized madder dye solution was assessed under T90+UV/VIS Spectrometer to analyse the UV visible spectral region which is shown in the Fig. 2&3. The radiations from the sun consist of several types of radiations that reach the earth and it can be felt as light and heat. Among that UV A and UV B having the wavelength of nm and nm respectively are the rays that are not completely absorbed by the Ozone layer. These rays on exposure to skin cause carcinogenic effects. The peaks obtained from spectroscopy analysis of homogenized Indian madder shows 283 nm and 327 nm which corresponds to UV A and UV B range. This results shows that the Indian madder dye solution has the ability to absorb UV A and UV B radiation that reaches its surface. Fig. 2 UV absorption graph of dye solution 217

4 Fig. 3 UV transmittance graph of dye solution The madder finish on receiving the energy of UV photons corresponds to UVA and UVB undergoes conformational molecular changes through vibration or rotation as shown in Fig. 4. Incident UVA and UVB radiations Emitted UVA and UVB radiations Absorbed by the surface coating of Indian Madder On absorption of UV radiation Molecular conformational change Fig. 4 Mechanism of absorption of UV radiation by madder finish Particle size analysis by Atomic Force Microscopy (AFM) The particle size of the dye powder was analyzed using Atomic Force Microscopy and 3D image is shown in Fig. 5. The average size of the article diameter varies from 127nm to 305nm. The shape of the dye particle observed is rod shape. The length of this rod varies from 400 nm to 1800nm. Thus the particle size of the dye exist in the range of nm. Thus, AFM results shows that the Indian Madder dye particles are homogenized properly and the particle size range from Nano to micron level. 218

Fig. 5 3D AFM image of Indian Madder dye Thus the application of the reduced dye particles on fabric, increases the dye uptake and gives more dye affinity to the cotton fabric samples.

This will also helps in high concentration and dispersion of dye molecules throughout the surface that leads to better UV absorption as shown in the Fig. 6.

5 Fig. 5 3D AFM image of Indian Madder dye Thus the application of the reduced dye particles on fabric, increases the dye uptake and gives more dye affinity to the cotton fabric samples. This increased dye affinity gives more UV protection than the conventional dyeing process as there is more number of dye particles available in unit square surface area. This will also helps in high concentration and dispersion of dye molecules throughout the surface that leads to better UV absorption as shown in the Fig. 6. Incident rays Dye particles Rays are absorbed by the dye particles present in the fabric Dyed fabric with reduced dye particles Some of the rays are absorbed by the dye particles present in the fabric and the remaining rays are transmitted to the other part of the fabric Conventionally dyed fabric Fig. 6 High concentration and high dispersion of dyes in the fabric for UV absorption UPF Evaluation of Indian madder Dyed Cotton Fabric Samples The UPF rating indicates how effective a fabric is at blocking out solar ultraviolet radiation. Table 1 shows the UPF ratings of Indian Madder dyed sample both in dry and wet state. It is observed from the table that UV transmittance is very low and the UV blocking % from the fabric to the skin is very high, both in dry and wet state. Hence the dyed cotton samples shows excellent UV protection with high UPF rating. It is also observed that UV blocking is more in the wet state rather than in the dry state. 219

6 This is mainly because with the absorption of water, the cotton yarn swells and thereby the interstices between warp and weft get closed. This reduces the space between ends and picks and thus UV transmittance also gets reduced. This leads to the increased UPF in the wet condition rather than in the dry condition. TABLE I UPF OF THE DRY AND WET SAMPLES OF DYED COTTON FABRIC SAMPLES Fastness properties Fastness property of dyed cotton samples were analyzed for wash, light and rubbing and the values are shown in the Table 2 below. From the Table 2, it is observed that the samples show good wash and light fastness property and moderate rubbing fastness property. The dyes of reduced particle size can easily penetrate through the yarn structure and it gets entrapped into the yarn profile, thus provides darker shade. References [9], [10] have demonstrated that the darker the shade of any colour, the higher would be the protection, indicating that the dark coloured fabrics transmit less UV rays than lighter shade fabrics. This gives good wash and light fastness property. Whereas, the rubbing makes the entrapped dye particles to get released from the structure that gives reduced fastness property. TABLE II FASTNESS PROPERTY OF THE DYED SAMPLE Fastness property Grade Wash 4-5 Light 4 Rubbing-wet 3 Rubbing-dry 3-4 IV. CONCLUSION Indian madder root powder was extracted and homogenized to produce reduced particle sized dye and the dye powder was analyzed under Atomic Force Microscopy (AFM) which shows the particle size in the range of nm. Thus the dye obtained was applied on cotton fabric and analysed for UV protection property which shows excellent result with the UPF of 50+ and also good fastness property. It is observed from the experiment that the reduction in particle size of the dye increases the dye affinity and can produce uniform dyeing on fabrics. Thus deeper the shades, higher UPF can be achieved. REFERENCE Samples Transmittance % Blocking % UVA UVB UVA UVB [1] P.Dobnik Dubrovski and M.Brezocnik, Prediction of the Ultraviolet Protection of Cotton Woven Fabrics Dyed with Reactive Dystuffs, Fibres & Textiles in Eastern Europe, Vol. 17, No. 1(72), pp , January/March [2] Arshia Hussain and Shahnaz Jahan, Textiles Protection against Ultraviolet Radiation, The Indian Textile Journal, June [3] G.L. Hornyak, H.F. Tibbals, J. Dutta and J.J. Moore, Introduction to Nanoscience and Nanotechnology, CRC Press, Taylor & Francis Group, LLC, UK; UPF DRY WET

7 [4] SM. Gawish, HM. Mashaly, HM. Helmy, AM. Ramadan, R. Farouk, Effect of Mordant on UV Protection and Antimicrobial Activity of Cotton, Wool, Silk and Nylon Fabrics Dyed with Some Natural Dyes, Journal of Nanomedicine and Nanotechnology, Vol.8, No.1, [5] D. Gupta, S. Kumari, and M.Gulrajani, Dyeing Studies with Hydroxyanthraquinones Extracted from Indian Madder. Part 2: Dyeing of Nylon and Polyester with Nordamncanthal, Coloration Technology, Vol. 117(6), pp , [6] Mohd Yusuf, Faqeer Mohammad, Mohd Shabbir and Mohd Ali Khan, Eco-Dyeing of Wool with Rubia Cordifolia Root Extract: Assessment of the Effect of Acacia Catechu as Biomordant on Color and Fastness Properties, Textiles and Clothing Sustainability, [7] Katarzyna Schmidt-Przewoźna, Małgorzata Zimniewska, Natural Dyeing Plants as a Source of Compounds Protecting against UV Radiation, Institute of Natural Fibres and Medicinal Plants, Vol. 55, No 3, [8] M.Doğru, Z.Baysal and C.Aytekin, Dyeing of Wool Fibres with Natural Dyes: Effect of Proteolytic Enzymes, Prep Biochem Biotechnol., Vol.36(3), pp , [9] G.Reinert, F.Fuso, R. Hilfiker and E.Schmidt, UV Protecting Properties of Textile Fabrics and Their Improvement, AATCC Review 29 (12), pp.31 43, [10] M.T. Pailthorpe and J.I.Chriskis, Sun Protection of Apparel Textiles, in Proceedings of 3 rd Asian Textile Conference, 1995, Vol. II, pp

Subject : Dyeing And Printing. Unit 5: Dyeing process for natural fibers. Quadrant 1 E-Text

Subject : Dyeing And Printing. Unit 5: Dyeing process for natural fibers. Quadrant 1 E-Text Subject : Dyeing And Printing Unit 5: Dyeing process for natural fibers Quadrant 1 E-Text Learning Objectives The learning objectives of this unit are: Describe the dyeing process for cellulosic fibers