Journal of South China University of Technology (Natural Science Edition) ›› 2014, Vol. 42 ›› Issue (10): 25-30.doi: 10.3969/j.issn.1000-565X.2014.10.005

• Materials Science & Technology • Previous Articles     Next Articles

Synthesis and Properties of Spiro and Caged Bicyclic Phosphate

Liu Shu-mei  Feng Meng  Sun Zhi-song  Zhao Jian-qing  Yuan Yan-chao   

  1. School of Materials Science and Engineering, South China University of Technology, Guangzhou 510640, Guangdong, China
  • Received:2014-01-27 Revised:2014-04-30 Online:2014-10-25 Published:2014-10-01
  • Contact: 刘述梅（1968-）,女,博士,副教授,主要从事有机硅合成、高分子材料改性等的研究. E-mail:liusm@scut.edu.cn
  • About author:刘述梅（1968-）,女,博士,副教授,主要从事有机硅合成、高分子材料改性等的研究.
  • Supported by:

    广州市科研条件建设项目(2012224-7)；广东高校轻化工清洁生产工程技术研究中心开发课题基金（31117004）

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Abstract:

A spiro and caged bicyclic phosphate flame retardant named as PDD-PEPA was synthesized with pentaerythritol diphosphate dichloride (PDD) and caged bicyclic phosphate 1-oxo-1-phospha-2, 6, 7–trioxabicyclo [2.2.2]-4-hydroxymethyl octane (PEPA) as reactants, and the synthesis conditions of the flame retardant, namely the dosage of triethylamine as a catalyst and the reaction time, wereare optimized. Then, the structure of PDD-PEPA was characterized by means of MS, IR and NMR, and the thermal stability and charring capacity of PDD-PEPA were investigated in N2 atmosphere through thermalgravimetric analysis. The results show that (1) when PDD- and PEPA reacts with a mole ratio of triethylamine to theoretical hydrogen chloride of 1:2 in the acetonitrile solvent at a reflux temperature for 10 h, the yield of PDD-PEPA is higher, and (2) under such conditions, the theoretical phosphorus content of the flame retardant is 21.2%, the initial decomposition temperature is 351℃, and the carbon yield is 63.6% at 650℃.

Key words: spiro phosphate, caged bicyclic phosphate, flame retardants, thermal stability, carbon yield

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