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化学学报
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化学学报 ›› 2010, Vol. 68 ›› Issue (15): 1532-1536. 上一篇    下一篇

研究论文

新型无卤阻燃剂新戊二醇二焦磷酸酯的合成、晶体结构及热分解性能研究

卢林刚*,1，陈淮思2，曹飞2，董希琳1，唐凯1   

  1. (1中国人民武装警察部队学院科研所 廊坊 065000)
    (2中国人民武装警察部队学院消防工程系 廊坊 065000)
  • 投稿日期:2009-12-16 修回日期:2010-02-06 发布日期:2010-03-10
  • 通讯作者: 卢林刚 E-mail:llg@iccas.ac.cn
  • 基金资助:

    “十一五”国家科技支撑计划项目

Synthesis, Structure and Thermal Decomposition Behavior of Novel Free-Flame Retardant Neopentyl Glycol Dipyrophosphate

Lu Lingang*,1 Chen Huaisi2 Cao Fei2 Dong Xilin1 Tang Kai1   

  1. (1 Institute of Science and Technology, Chinese People s Armed Police Force Academy, Langfang 065000)
    (2 Department of Fire Protection Engineering Chinese People s Armed Police Force Academy, Langfang 065000)
  • Received:2009-12-16 Revised:2010-02-06 Published:2010-03-10

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被引次数

22 | 5

以新戊二醇、三氯氧磷为原料, 合成得到5,5-二甲基-1,3-二氧杂己内磷酰氯(II), 化合物II经过水解反应合成新型无卤阻燃剂新戊二醇二焦磷酸酯, 两步反应总产率72%. 采用元素分析、FT-IR、MS、1H NMR及X射线四圆衍射等技术确定了标题化合物的分子结构. 结构分析表明, 该标题化合物属于正交晶系, pbca空间群, 每个结构单元含有2个分子, 晶胞参数为a＝0.97690(2) nm, b＝1.1283(2) nm, c＝2.6506(5) nm, α＝90(3)°, β＝90(3)°, γ＝90(3)°, V＝2.9217(10) nm3, Z＝38, Dc＝1.429 g/cm3, μ＝0.322 mm－1, F(000)＝1328, 由3327个独立衍射点得到最终偏离因子[I＞2σ(I)] R＝0.0507, Rw＝0.1254. 热失重分析表明该标题化合物具有较高的热稳定性和良好的成炭性.

关键词: 阻燃剂, 合成, 晶体结构, 热分解

Dibromoneopentyl glycol chlorophosphate (II) was prepared by reaction of neopentyl glycol and phospous oxychloride. Then novel free-flame retardant neopentyl glycol dipyrophosphate (III) was synthesized by the hydrolysis reaction of compound II. The over yield was 72% and its structure was identified and studied by elemental analysis, IR, 1H NMR, MS techniques and X-ray diffraction analysis. The crystal belongs to orthorhombic, space group pbca with unit cell dimensions a＝0.97690(2) nm, b＝1.1283(2) nm, c＝2.6506(5) nm, α＝90(3)°, β＝90(3)°, γ＝90(3)°, V＝2.9217(10) nm3, Z＝38, Dc＝1.429 g/cm3, μ＝0.322 mm－1 and F(000)＝1328. The final R＝0.0507 and Rw＝0.1254 for 3327 unique reflections [I＞2σ(I)]. The result of thermal analysis shows that the novel flame retardant has a high thermal stability and excellent char forming ability.

Key words: flame retardant, synthesis, crystal structure, thermal decomposition