季戊四醇磷酸酯三聚氰胺盐的合成及其应用

摘要

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.%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.