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化学学报
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化学学报 ›› 2009, Vol. 67 ›› Issue (14): 1695-1699. 上一篇    下一篇

研究简报

新型磷系阻燃剂1,3,5-三(5,5-二甲基-1,3-二氧杂-2-氧代己内磷酰基- 2-氧)苯的合成及热分解动力学研究

卢林刚*,a 杨守生b 张 燕b 黄晓东b

  

  1. (a中国人民武装警察部队学院 科学技术研究所 廊坊 065000)
    (b中国人民武装警察部队学院 消防工程系 廊坊 065000)

  • 投稿日期:2009-01-11 修回日期:2009-05-04 发布日期:2009-07-28
  • 通讯作者: 卢林刚

Synthesis and Thermal Decomposition Kinetics of Novel Flame Retardant 1,3,5-Tris(5,5-dimethyl-1,3-dioxa-2- oxophosphorinanyl-2-oxy)benzene

Lu, Lingang *,a Yang, Shousheng b Zhang, Yan b Huang, Xiaodong b   

  1. (a Institute of Science and Technology, Chinese People’s Armed Police Force Academy, Langfang 065000)
    (b Department of Fire Protection Engineering, Chinese People’s Armed Police Force Academy, Langfang 065000)
  • Received:2009-01-11 Revised:2009-05-04 Published:2009-07-28
  • Contact: Lu, Lingang

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1407

被引次数

26

以新戊二醇、三氯氧磷及1,3,5-三羟基苯等为原料, 经过两步反应合成新型磷系阻燃剂1,3,5-三(5,5-二甲基-1,3-二氧杂-2-氧代己内磷酰基-2-氧)苯, 采用元素分析、FT-IR、MS及1H NMR等技术确定了标题化合物的分子结构. 以TG-DTG为手段, 研究该新型磷系阻燃剂在氮气气氛中的热分解动力学; 利用Kissinger法、Flynn-Wall-Ozawa (FWO)法对其进行热分解动力学研究, 求出该阻燃剂的热分解动力学参数; 利用Coast-Redfern法研究该阻燃剂的热分解机理. 结果表明, Kissinger法所求得的表观活化能为171.72 kJ•mol－1, 指前因子ln A为37.57; Flynn-Wall-Ozawa法所求得的表观活化能为172.05 kJ•mol－1. 标题化合物的热分解动力学方程g(α)＝α1/4, 反应级数n＝1/4.

关键词: 1,3,5-三(5,5-二甲基-1,3-二氧杂-2-氧代己内磷酰基-2-氧)苯, 合成, 热分解动力学, 活化能, 机理

The novel flame retardant 1,3,5-tris(5,5-dimethyl-1,3-dioxa-2-oxophosphorinanyl-2-oxy)-ben- zene was synthesized via neopentyl alcohol, phosphous oxychloride and 1,3,5-trihydroxybenzene by a two step reaction, and its structure was identified and studied by elemental analysis, IR, 1H NMR and MS techniques. The thermal decomposition kinetics of the novel flame retardant were studied by TG-DTG techniques. The kinetic parameters, including the activation energy and frequency factor of the decomposition process for the title compound were calculated through the Kissinger and Flynn-Wall-Ozawa (FWO) method and the thermal decomposition mechanism was also studied with the Coast-Redfern method. The results show that the activation energy and pre-exponential factor are 171.72 kJ•mol－1 and 37.57 s－1 with the Kissinger method and 172.05 kJ•mol－1 with the Flynn-Wall-Ozawa method respectively. The kinetic equation of the novel flame retardant can be expressed as g(α)＝α1/4, and the reaction order is n＝1/4.

Key words: 1,3,5-tris(5,5-dimethyl-1,3-dioxa-2-oxophosphorinanyl-2-oxy)benzene, synthesis, thermal decomposition kinetics, activation energy, mechanism