膨胀型阻燃剂三羟甲基丙烷磷酸酯三聚氰胺盐的合成

Synthesis of Melamine Salt of Trimethylolpropyl Phosphate as Intumescent Flame Retardant

以三羟甲基丙烷、磷酸、三聚氰胺为原料,用乙二醇作为分散剂,采用两步法合成了氮磷膨胀型阻燃剂三羟甲基丙烷磷酸酯三聚氰胺盐。对反应温度、反应时间、物料配比和分散剂等条件作了工艺考察。结果表明,第一步反应时间3 h、反应温度为60℃;第二步反应时间1.5 h,反应温度为60℃,分散剂为乙二醇;物料最佳摩尔比n(三羟甲基丙烷)∶n(磷酸)∶n(三聚氰胺)=1∶1∶1,该条件下阻燃剂剩炭率可达41%。通过红外光谱和热重分析对阻燃剂进行了表征,分别表明该阻燃剂具有N-H、C=N、P-O-C等特征峰,能够在有效的温度区间内发生热分解,起到阻燃作用。

Intumescent flame retardant, trimethylolpropyl phosphate melamine was synthetized through two -step method, by trimethylolpropane, phosphoric acid and melamine, with glycol as disperser. Various reaction factors were discussed, The optimum reaction conditions were as follows：the time and temperature of the first-step reaction were 2 h and 60 ℃;and the time and temperature of the second-step reaction were 1 . 5 h and 60 ℃, the disperser is glycol;n（ trimethylolpropane）∶n（ phosphoric acid）∶n（ melamine） =1∶1∶1;the char yield of intumescent flame retardant was 41 %. The analysis of infrared spectra and thermogravimetry indicated that the obtained flame retardant had the characteristic peak of N-H、C=N、P-O-C, and could be decomposed in effective temperature range, then would be useful for suppression of combustion.