Study of thermal properties of flame retardant epoxy resin treated with hexakis[ p -(hydroxymethyl)phenoxy]cyclotriphosp
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Study of thermal properties of flame retardant epoxy resin treated with hexakis[p-(hydroxymethyl)phenoxy]cyclotriphosphazene Jianzhong Xu • Zhanmeng He • Weihong Wu Haiyun Ma • Jixing Xie • Hongqiang Qu • Yunhong Jiao
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Received: 3 December 2012 / Accepted: 19 March 2013 Ó Akade´miai Kiado´, Budapest, Hungary 2013
Abstract Hexakis[p-(hydroxymethyl)phenoxy]cyclotriphosphazene (HHPCP) is prepared and characterized by FTIR, 1H-NMR, and 31P-NMR spectroscopy. Then an investigation of the flame retardancy, thermal decomposition behavior of epoxy resin (EP) containing HHPCP is carried out using limiting oxygen (LOI) test, horizontal flame test, smoke density rate (SDR) test, thermogravimetric analysis (TG), and thermal gravimetric analyzermass spectrometry (TG-MS). The decomposition process of HHPCP is studied by TG-MS and FTIR. The result shows that the LOI value of EP increase from 20.5 to 26.5 %, when 7.5 mass% HHPCP is added into EP. The addition of 1 mass% nano-montmorillonite (nMMT) into EP–7.5 mass% HHPCP sample as synergist can increase the LOI value of EP–7.5 mass% HHPCP–1 mass% nMMT sample from 26.5 to 27.5 %. The SDR test indicates that smoke suppression of HHPCP on EP is not significant. TG analysis reflects that the EP–7.5 mass% HHPCP sample and EP–7.5 mass% HHPCP–1 mass% nMMT show higher thermal stability properties with an increasing Tonset and Tmax comparing with neat-EP. TG-MS result indicates that the main pyrolysis product of EP is H2O, CO, CO2, C6H6, C6H5OH, HOC6H4CH3, and flammable hydrocarbon J. Xu (&) Z. He H. Ma J. Xie H. Qu Y. Jiao College of Chemistry and Environmental Science of Hebei University, Baoding 071002, China e-mail: [email protected] Z. He e-mail: [email protected] H. Qu e-mail: [email protected] W. Wu College of Science, Agriculture University of Hebei, Baoding 071002, China
fragments CxHy. Compared with neat-EP sample, nonflammable water vapor of EP–7.5 mass% HHPCP sample increased, whereas CO2 and the flammable hydrocarbon fragments CxHy and flammable gas CO decreased. TG-MS and FTIR result suggests that HHPCP decomposed first by inter-molecular dehydration, then P–N hexatomic ring of HHPCP decomposed during 470 and 560 °C, and a little no-flame gas containing nitrogen element volatilized into the gaseous phase. Keywords Cyclotriphosphazene EP Flame retardant Degradation
Introduction Epoxy resin is a kind of thermosetting plastic that is widely used in adhesive, coating, aerospace field, and electronic industry due to its excellent mechanical properties, small contraction, and chemical resistance properties. However, the limiting oxygen index (LOI) value of neat epoxy resin is about 20 %, which mean that epoxy resin is very easy to ignite. Therefore, the researchers have drawn considerable attention on flame-retardant epoxy resin in recent years [1, 2]. A lot of investigations are conducted on flame-retardant epoxy resin, especially for the epoxy resin treated with halogen-free flame retardants, which have received increasing attention when the European Union app
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