应用化学 ›› 2011, Vol. 28 ›› Issue (05): 605-607.DOI: 10.3724/SP.J.1095.2011.00436

• 研究简报 • 上一篇    下一篇

5,5-二甲基-2-磷杂-1,3-二噁烷-2-基烯丙基磷酸酯的制备

徐玲1,程博闻1*,任元林1,2   

  1. (1.天津工业大学中空纤维膜材料与膜过程省部共建国家重点实验室培养基地 天津 300160;
    2.天津工业大学纺织学院 天津)
  • 收稿日期:2010-07-29 修回日期:2010-09-18 出版日期:2011-05-10 发布日期:2011-05-10
  • 通讯作者: 程博闻,教授; Tel:022-24528358; Fax:022-24528018; E-mail:bowen15@tjpu.edu.cn; 研究方向:功能高分子材料
  • 基金资助:
    天津市自然科学基金资助项目(10JCZDJC22200)

Preparation of 5,5-dimethyl-2-phospha-1,3-dioxan-2-yl-allyl Phosphate

XU Ling1, CHENG Bowen1*, REN Yuanlin1,2   

  1. (1.State Key Laboratory of Hollow Fiber Membrane Materials and Processes,
    Tianjin Polytechnic University,Tianjin 300160;2.School of Textile,Tianjin Polytechnic University,Tianjin)
  • Received:2010-07-29 Revised:2010-09-18 Published:2011-05-10 Online:2011-05-10
  • Contact: bowen

摘要:

以新戊二醇、三氯氧磷、烯丙醇和金属钠为原料,经过2步反应合成了新型反应型阻燃化合物5,5-二甲基-2-磷杂-1,3-二噁烷-2-基烯丙基磷酸酯。 采用元素分析、FTIR、MS和1H NMR等测试技术对其结构进行了表征。 对合成工艺进行了探讨,当n(Na)∶n(烯丙醇)=1∶2,于冰水浴反应2 h,再于30 ℃反应6 h时,产率可达55.5%。 TG分析显示,该化合物的起始分解温度为130.2 ℃,800 ℃时仍有23%的残炭率,说明该化合物具有较好的热稳定性和成炭性。

关键词: 新戊二醇, 三氯氧磷, 阻燃剂, 丙烯醇, 热性能

Abstract:

A novel reactive flame retardant, 5,5-dimethyl-2-phospha-1,3-dioxan-2-yl-allyl phosphate, was synthesized by reacting neopentyl glycol, phosphorus oxychloride, allyl alcohol with sodium through two steps. The title compound was characterized by elemental analysis, FTIR, MS and 1H NMR. The thermal properties of the title compound were studied by TG and DSC techniques. The results show that the synthesized compound is consistent with the expected structure. The yield of the compound is 55.5% with the molar ratio of allyl alcohol to sodium being 2∶1, the reaction temperature being at 0 ℃ using an ice bath for 2 h at first, and then at 30 ℃ for 6 h. The TG curves show that the initial thermal decomposition temperature of the compound is about 130.2 ℃, and there is about 23% char residue left at 800 ℃, indicating that the title compound has a good thermal stability and a char forming capability.

Key words: neopentyl glycol, phosphorus oxychloride, flame retardant, allyl alcohol, thermal property

中图分类号: