新型磷阻燃剂TPTMA的合成及其阻燃性能研究  

Synthesis of a novel phosphorous flame retardant TPTMA and its flame retardancy research

作　　者：娄兆文 李凯通[1,2,3] 隗兰华 蔡成林 陈兰[1,2,3] 

机构地区：[1]有机化工新材料湖北省协同创新中心,湖北武汉430061 [2]有机功能分子合成与应用教育部重点实验室,湖北武汉430062 [3]湖北大学化学化工学院,湖北武汉430062

出　　处：《磷肥与复肥》2018年第2期22-25,共4页Phosphate & Compound Fertilizer

基　　金：湖北省科技支撑计划(2014BCB028)

摘　　要：以六羟甲基三聚氰胺、三氯氧磷和三聚氰胺为原料,经过两步反应合成新型磷阻燃剂2,4,6-三(磷酸二甲酯基胺基)-1,3,5-三嗪-三-三聚氰胺盐(TPTMA),考察加料温度、中间产物1的分散溶解、酸度和溶剂洗涤对工艺的影响。反应最佳条件为:第一步,加料温度45~50℃,80℃反应5 h;第二步,分散溶解溶剂A,冰水浴下控制pH 4.5反应0.5 h,产率73%,磷质量分数10.5%。阻燃性能研究表明产品有低渗出性特点,在聚乙烯中,产品1和聚磷酸铵以1∶2的质量比协同添加30%,氧指数为27.7。采用^(13)C-NMR、^(31)P-NMR和FT-IR表征其结构,表明产品为TPTMA。A novel phosphorous flame retardant 2,4,6-tri-（aminodimethyl phosphate）-1,3,5-triazine-tri-melaminesalt（TPTMA） is synthesized via the reaction of hexamethylol melamine, phosphorus oxychloride and melaminein two steps. Effects of feed temperature, dispersion and dissolution of intermediate product 1, acidity andsolvent washing on the process are investigated. The optimum reaction conditions are as follow： the first step,feed temperature is 45-50 ℃, reaction 5 h at 80 ℃; second step, solvent of the dispersing and dissolving is A,reaction 0.5 h at pH of 4.5 in the ice bath. The yield is 73%, phosphorus content is 10.5% for product 1 underthe optimum reaction conditions. The research on flame retardant properties indicates that product 1 has lowexudative characteristics, product 1 and ammonium polyphosphate（mass ratio 1∶2）cooperated to add 30% inpolyethylene and the LOI index is 27.7. The structure is characterized by^（13） C-NMR,^（31） P-NMR and FT-IR,itindicates that the product is TPTMA.

关 键 词：六羟甲基三聚氰胺 三氯氧磷 三聚氰胺 磷阻燃剂 

分 类 号：TQ126.35[化学工程—无机化工]