一种含笼状硫代磷酸酯仲胺盐的合成与应用  

Synthesis and application of a secondary amine salt containing cage thiophosphate

作　　者：金涛 潘鑫 姚周钰 罗秋艳 冯芳[1] 马肃 JIN Tao;PAN Xin;YAO Zhouyu;LUO Qiuyan;FENG Fang;MA Su(School of Chemistry and Life Science,Suzhou University of Science and Technology,Suzhou 215009,China;Key Laboratory of Solar Cell Electrode Materials for Petroleum and Chemical Industry,Suzhou 215009,China)

机构地区：[1]苏州科技大学化学与生命科学学院,江苏苏州215009 [2]中国石油和化工行业太阳能电池电极材料重点实验室,江苏苏州215009

出　　处：《工程塑料应用》2024年第11期10-17,共8页Engineering Plastics Application

基　　金：江苏省环境功能材料重点实验室开放基金项目(SJHG1807);江苏省研究生科研与实践创新计划项目(SJCX24_1907)。

摘　　要：不饱和聚酯树脂(UPR)具有优异的工艺性能和较好的拉伸强度等,因此其用途较为广泛,但UPR在燃烧时会产生大量的黑烟,会严重影响人的生命健康安全。为提升UPR的阻燃性能以及热稳定性,采用以三氯硫磷(PSCl3)、季戊四醇、马来酸酐(MA)和哌嗪为原料,合成一种含有含氮、磷、硫三种阻燃元素的协同阻燃剂,并在该阻燃剂分子中引入笼状结构,以提升UPR热稳定性、力学性能以及阻燃性能等。采用傅里叶变换红外光谱、核磁共振氢谱、热重分析等表征方式对合成目标产物进行了结构和热稳定性鉴定。同时,对所合成的最终产物含笼状硫代磷酸酯仲胺盐(PI-MA-SPEPA)的工艺条件进行了优化,探讨了溶剂配比、反应时间、反应温度等对合成产物产率的影响。研究表明反应温度30℃,反应时间4 h,乙醇和水的最佳溶剂配比为1∶1,最终产物的反应产率最高,可达82.9%。最后,通过垂直燃烧测试对添加阻燃剂的UPR进行了阻燃性能的评价。结果表明,在UPR中加入18%的PI-MA-SPEPA,UPR的阻燃性可达到V-0级。Unsaturated polyester resin(UPR)has excellent process performance and good tensile strength,so it is widely used,but UPR will produce a lot of black smoke when burning,which will seriously affect human life and health safety.In order to improve the flame retardancy and thermal stability of UPR,trichlorothion(PSCl3),pentaerythritol,maleic anhydride(MA)and piperazine were used as raw materials to synthesize a synergistic flame retardant containing three flame retardants:nitrogen,phosphorus and sulfur,and a cage structure was introduced into the flame retardant molecules to improve the thermal stability,mechanical properties and flame retardancy properties of UPR.The structures and thermal stability of synthesized products were identified by infrared spectroscopy,nuclear magnetic resonance hydrogen spectrum and thermogravimetry.At the same time,the process conditions of the final product PI-MA-SPEPA were optimized,and the effects of solvent ratio,reaction time and reaction temperature on the yield of the product were discussed.The results show that the reaction temperature is 30℃,the reaction time is 4 h,the optimal solvent ratio of ethanol and water is 1∶1,and the reaction yield of the final product is the highest,up to 82.9%.Finally,the flame retardancy of UPR with flame retardants was evaluated by vertical combustion test.The results show that UPR can reach V-0 level when 18%of PI-MA-SPEPA is added to UPR.

关 键 词：阻燃剂 协同 阻燃性能 不饱和聚酯树脂 笼状磷酸酯化合物 

分 类 号：TQ322[化学工程—合成树脂塑料工业]