SYNTHESIS OF NON HALOGENATED ACRYL PHOSPHATE FLAME RETARDANT AND ITS APPLICATION ON JUTE

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International Journal of Textile and Fashion Technology (IJTFT) ISSN(P): 2250-2378; ISSN(E): 2319-4510 Vol. 5, Issue 1, Feb 2015, 23-28 TJPRC Pvt. Ltd.

1 International Journal of Textile and Fashion Technology (IJTFT) ISSN(P): ; ISSN(E): Vol. 5, Issue 1, Feb 2015, TJPRC Pvt. Ltd. SYNTHESIS OF NON HALOGENATED ACRYL PHOSPHATE FLAME RETARDANT AND ITS APPLICATION ON JUTE USHA SAYED 1, PRAVIN KOKATE 2 & PRASHANT GANGAWANE 3 1 Associate Professor, Department of Fibers and Textile Processing Technology, Institute of Chemical Technology, Matunga (East), Mumbai, Maharashtra, India 2,3 Research Scholar, Department of Fibers and Textile Processing Technology, Institute of Chemical Technology, Matunga (East), Mumbai, Maharashtra, India ABSTRACT Jute fabrics are now widely used in furnishing textiles, upholstery and home textiles. However being a cellulosic fibre, jute ignites easily and in fires jute products such as curtains, upholstered furniture, home textile products, automobile interior products become quickly damaged and are difficult to extinguish. Since consumers are now increasingly aware of safe life style, expectation and demand for diversified value added flame retardant jute products are steadily increasing. The halogen based flame retardants are hazardous and therefore the research for non halogenated flame retardant products is need of hour. In this present work, non-halogenated flame retardant acrylatephosphate was synthesized by using 2-Hydroxyethyl methacrylate, Phosphorus Pentoxide and 2, 2 -Azobis-(isobutyronitrile). Further it impart on jute by pad dry cure method. The burning behaviour and weight loss values evaluated using the standard vertical flammability test method. Results shows that synthesised acrylatephosphate treated jute fabric having food flame resistance. KEYWORDS: Flame Retardant, Jute, Acrylatephosphate, 2-Hydroxyethyl Methacrylate, Phosphorus Pentoxide, 2, 2 -Azobis-(Isobutyronitrile), Limiting Oxygen Index INTRODUCTION Jute is one of the most important biodegradable, ecofriendly, annually renewable agricultural product and natural textile fibre. Jute traditionally uses as packaging material. [1,2,3] Apart from its traditional use as packaging material, jute fabrics are now widely used in furnishing textiles, upholstery and home textiles. Jute is a natural fibre composed of cellulose, lignin, hemicellulose, waxes and protein mineral matters. However being a cellulosic fibre, jute ignites easily and in fires jute products such as curtains, upholstered furniture, home textile products, automobile interior products become quickly damaged and are difficult to extinguish. Since consumers are now increasingly aware of safe life style, expectation and demand for diversified value added flame retardant jute products are steadily increasing. Therefore effort is going on to develop fire retardant cellulosic fabric for home textile and home furnishing application. Different chemical formulations have been reported for preparing fire retardant jute fabrics. It has been found that different inorganic salts, borax-boric acid composition, hydrated metal oxide like sodium silicate, different phosphorous and nitrogeneous compound and their combinations has been mostly used to make fire retardant jute. [4] 6, 7] Now halogen-free compounds have received increasing interest because of their environment-friendly property. [5, editor@tjprc.org

2 24 Usha Sayed, Pravin Kokate & Prashant Gangawane In this work we made successful attempt to synthesis non halogenated acryl phosphate flame retardant, applied on jute and its flammability performance in term of LOI (limiting oxygen index ) has been studied. MATERIALS AND METHODS Material Plain woven jute fabric with 150 GSM was used for the experiments. Chemicals Phosphorus Pentoxide, HEMA(2-hydroxyethyl methacrylate),2,2 -Azobis-(isobutyronitrile) AIBN. Methods Synthesis of Non-Halogenated Compound: Acryl phosphate (P) The chemicals namely HEMA (2-Hydroxyethyl methacrylate) (100ml) was taken in three necked flask and temperature was raised to 600C within 15 minutes under reflux condition after which Phosphorus Pentoxide (P2O5) (15 gm) was added slowly and the reaction was carried out for 3 hrs. An initiator AIBN was used for this synthesis. The obtained Product yield was measured. Reaction Scheme 1). HEMA (2-Hydroxyethyl methacrylate) react with Phosphorus Pentoxide (P2O5) to form a FR Compound(Scheme Scheme 1- Synthesis of Phosphorous Flame Retardant Compound Testing of Samples for Limiting Oxygen Index (LOI) The measurement of LOI is conducted according to ASTM D method. Testing of FR treated simple for vertical flammability The FR treated fabrics were teste don vertical flammability tester by standard method where specimen is cut into 76 mm by 300 mm. The specimen is mounted and clamped between the two halves of the holder ensuring bottom of the specimen is lined with the bottom of holder. The flame is exposed to the fabric for the 12+/_ 0.2 second and immediately after that the flame is removed. Stopwatch used to measure flame propagation time. Sample is dismounted and measures for its char length with the help of scale. RESULTS AND DISCUSSIONS In the present work, the Acryl phosphate (P) was synthesized by using methacrylate and phosphorus pentoxide. The product obtained was examined for its physical properties, as well as the infrared spectroscopy of the product has been carried out.the physical properties are given in Table 1 and its infrared spectroscopy in Figure 1. The product obtained is Impact Factor (JCC): Index Copernicus Value (ICV): 3.0

3 Synthesis of Non Halogenated Acryl Phosphate Flame Retardant and its Application on Jute 25 in liquid form having creamish yellow colour, slight viscous in nature, having a ph of 2-3 and insoluble in water but soluble in DMF. The yield of the product was %. The product is obtained acrylatephosphate. Table 1: Physical Properties of synthesized Acryl Phosphate (P) Properties Product P Solubility in water Not Soluble Solubility Soluble in DMF Appearance Creamish yellow Viscosity Highly viscous ph of 1% sol 2-3 Figure 1: FTIR Spectra of Acryl Phosphate (P) Figure 1 describes the FTIR analysis of Product P. The broad peak around /cm illustrates the presence of hydroxyl group. Sharp peak at 1164/cm confirms the presence of phosphate group (C-O-P) which contributes majorly for the flame retarding property of the product. Also carbonyl group (C=O) and alkyl group (R-H) are evident due to the peaks observed at /cm and /cm respectively. This product P was then applied on raw jute fabric by the pad dry cure technique. To optimize the curing concentration, the curing time and temperature, the jute fabric was treated with 10%, 20%, 30% concentration of product P at temperature 1100C, 1200C, 1300C and curing time 2 min, 3 min, 4 min was carried out, to optimize the finishing conditions. As shown in table 2, it is found that for curing temperature of C and 4 minutes curing time product has maximum add on with minimum char length. LOI of this sample was found to be 35, which is more than other treated fabrics. editor@tjprc.org

4 26 Usha Sayed, Pravin Kokate & Prashant Gangawane Table 2: Effect of Curing Time and Temperature on finishing of Jute Fabric with Product P Curing Temp(ºC) % Product P Curing Time Add on Char Length (min) (%) (cm) LOI As shown in table 3, it is found that, as the concentration of product P increases the percentage add on increases.at 10% concentration of P the percentage add on is 4.68 and at 100% concentration it become Table 3: % Add-On of Product P on Jute Fabric Varying Concentration Sr. Initial Weight Final Weight % Product P No. of Fabric of Fabric % Add On As shown in table 4, untreated jute has a LOI value of 22. While burning untreated jute, a residue (fly ash), is formed and nearly no char residue is remaining. The LOI of all samples treated with products increases with the amount of grafted polymer and consequently with the amount of phosphorus on the fabric. Up to 10% of Product the LOI increases very quickly from 22 to 24 and reached 42 with 100% of Product P application. The formation of char is an evidence for good flame retardant property. Table 4: Flame Retardancy of Jute at Various Concentrations of Product P Concentration Char Flame Propagation of Solution Length Timing LOI Raw Jute 6 cm sec 22 10% 4 cm sec 24 20% sec 26 40% sec 30 60% sec 35 80% sec % sec 42 The difference in the efficiency could be attributed to the fact that CH3 as component of the alkoxy group is beneficial for the phosphorylation compared to CH2CH3. It was observed that as percentage concentration of product P increased the fabric took longer time to propagate flame on testing the flame retardancy. Thus this observation definitely indicate being a phosphate compound has flame retarding effect on jute fabric since the LOI index increases with concentration as the retarding effects increases beside there is no afterglow and after flame. The finish forms a polymer film on curing and hence acts as a good flame retardant. Impact Factor (JCC): Index Copernicus Value (ICV): 3.0

5 Synthesis of Non Halogenated Acryl Phosphate Flame Retardant and its Application on Jute 27 The mechanism of flame retardant is similar to the mechanism of any phosphate compound preventing in propagating the flame. The above product is easy to synthesis and is soluble in DMF. At low concentration it gives a good flame retardant effect. The yield is good and is also found to be eco-friendly. The finish forms a polymer film on curing and hence acts as a good flame retardant. CONCLUSIONS The present study showed that flame retardancy of synthesised Acryl phosphate treated Jute fabric was quite good. The commercial flame retardant finishes are costlier, result in significant strength loss of fabric and are non-durable. The halogen based flame retardants are hazardous and therefore non-halogenated flame retardants are expected to have high demand in the near future. Research for non halogenated flame retardant products becomes need of hour. Therefore non-halogenated flame retardant acrylatephosphate was synthesized and impart on jute by pad dry cure method and hence continuous finishing process is possible. Hence flame retardancy on jute can be imparted effectively and economically. ACKNOWLEDGEMENTS The authors are thankful to the Department of Fibers and Textile Processing Technology, Institute of Chemical Technology, Matunga, Mumbai for providing infrastructural facilities and University Grant Commission (UGC) India for providing financial support for this research work. REFERENCES 1. Prashant Gangawane and Usha Sayed, Innovative use of outdated Tetracycline Hydrochloride drug to dye jute, International Journal of Medicine and Pharmaceutical Sciences 2013; 3(4): Nayak Laxmikanta and Roy Ashim, Utilisation of Jute By- Product: A Review, Agricultural Reviews 2011; 32(1): Mohammad Shahidual Islam and Mohammad Alauddin, International Journal of Management and Business Studies 2012; 2 (1): S. Basak, Kartick. K. Samanta, S. K. Chattopadhyay, R. Narkar, M. Bhowmick, S. Das & A. H. Saikh, Fire Retardant and Mosquito Repellent Jute Fabric Treated with Thio-urea hydrochloride drug, Journal of the Textile Association, 2014:74(5): R.V.Adivarekar, S.D.Dasarwar & N.S.Khurana, Synthesis of halogen free flame retardant and its application on polypropylene, Indian Journal of Fibre & Textile Research, 2013:38(3): Sergei V. Levchik abd Edward D. Well, A Review of Recent Progress in Phosphorus-based Flame Retardant, Journal of Fire Science, (5): Muriel Rakotomalala, Sebastian Wagner and Manfred Döring, Recent Developments in Halogen Free Flame Retardants for Epoxy Resins for Electrical and Electronic Applications, Materials,2010, 3, editor@tjprc.org

Phosphorus Flame Retardants for Textiles. Novecare 18/06/2006 CHALLENGING BOUNDARIES

Phosphorus Flame Retardants for Textiles Summary Introduction How Do Textiles Burn? The Action of a Phosphorus Flame Retardant Flame Retardant Selection Classification of Textile Flame Retardants Inherent