中国塑料 ›› 2017, Vol. 31 ›› Issue (6): 105-110 .DOI: 10.19491/j.issn.1001-9278.2017.06.018

• 助剂 • 上一篇    下一篇

季戊四醇磷酸酯三聚氰胺盐的合成及其应用

李来丙   

  1. 湖南工学院
  • 收稿日期:2017-03-08 修回日期:2017-03-19 出版日期:2017-06-26 发布日期:2017-09-26

Synthesis and Characterizations of Pentaerythritol Phosphate Melamine Salt

  • Received:2017-03-08 Revised:2017-03-19 Online:2017-06-26 Published:2017-09-26

摘要: 用季戊四醇(PER)、磷酸和三聚氰胺为原料,以无水乙醇作为分散剂,通过两步反应合成了膨胀型阻燃剂季戊四醇磷酸酯三聚氰胺盐(PPMS)。研究了PER、磷酸和三聚氰胺物料配比、反应时间和温度对反应的影响,并用傅里叶变换红外光谱仪对合成的产物进行结构表征,并对比研究了合成产物与市售阻燃聚磷酸铵(APP)的阻燃效果。结果表明, PPMS的优化合成条件为nPER∶n磷酸∶n三聚氰胺=1∶3∶1.09(摩尔比,下同)、酯化温度为100 ℃、酯化时间为1.5 h、成盐温度为80 ℃、成盐时间为6 h; PPMS的膨胀度为25.5 cm3/g,残炭率为54.3 %;PPMS阻燃聚氨酯弹性体(TPU)时MTPU∶MPPMS(质量比,下同)>100∶30,阻燃级别达到UL 94 V0级,点燃时间长,自熄时间短,成炭效果好,且阻燃效果优于APP。

关键词: 阻燃剂, 季戊四醇磷酸酯三聚氰胺盐, 膨胀度, 残炭率

Abstract: Pentaerythritol phosphate melamine salt (PPMS) as an expansion-type flame retardant was synthesized through a two-step pathway by using pentaerythritol, melamine and phosphoric acid as raw materials, and its chemical structure was characterized by Fourier-transform infrared spectroscopy. The effects of raw material ratio, the time and temperatures for esterification and saltforming reactions on the molecular structure of the product were investigated. The results indicated that the optimum synthetic condition was determined as a molar ratio of pentaerythritol/phosphoric acid/melamine at 1∶3∶1.09, an esterification temperature of 100 ℃, a reaction time of 1.5 h, a salt-forming temperature of 80 ℃, and a salt-forming reaction time of 6 h. The resultant PPMS achieved an expansion degree of 25.5 cm3/g and a char yield of 54.3 % while being synthesized at such an optimum condition.

Key words: flame retardant, pentaerythriol phosphate melamine salt, expansion degree, char yield