阻燃剂2,4,6-三(2,4,6-三溴苯氧基)-1,3,5-三嗪的合成及工业试验研究  

Synthesis and Industrial Experimental Study of Flame Retardant 2,4,6-Tris(2,4,6-tribromophenoxy)-1,3,5-triazine

作　　者：唐安斌[1] 黄杰[1] 王倩[2] 马庆柯 支肖琼[1] 范盈[1] 

机构地区：[1]四川东方绝缘材料股份有限公司国家级企业技术中心,四川绵阳621000 [2]四川大学高分子材料与工程学院,四川成都610065

出　　处：《精细化工》2007年第10期1011-1014,共4页Fine Chemicals

基　　金：国家高技术研究发展计划(863)资助项目(2003AA333030)~~

摘　　要：对阻燃剂2,4,6-三(2,4,6-三溴苯氧基)-1,3,5-三嗪的相转移催化合成工艺进行了改进,完成了工业试验研究。通过向2,4,6-三溴苯酚、三聚氯氰的溶液中滴加氢氧化钠水溶液的方式进行相转移催化合成,考察了有机溶剂、物料摩尔比、反应温度、反应时间对反应的影响。用正交实验确定了最佳物料配比n(2,4,6-三溴苯酚)∶n(氢氧化钠)∶n(催化剂)∶n(三聚氯氰)=3.05∶3.05∶0.05∶1,经工艺优化,产品收率达到96.6%,用IR分析了产品结构。工业试验在3 m3反应釜中进行,消耗定额为:2,4,6-三溴苯酚800 kg、三聚氯氰146 kg、氢氧化钠96.4kg、二氯甲烷1 400 kg、乙醇1 000 kg。溶剂二氯甲烷和乙醇回收率达到90%以上,重复使用10次后,工业试验产品收率仍可达到95%。工业试验产品经热重分析,温度达到320℃时,失重为1%,在H IPS中应用结果表明,其机械性能、热性能和阻燃性能完全满足出口阻燃H IPS的技术指标要求。The flame retardant 2,4,6-tris （ 2,4,6-tribromophenoxy ） -1,3,5-triazine was synthesized through improved phase-transfer catalysis, and the corresponding industrial experimental study was accomplished. The synthesis was performed via dropping aqueous NaOH into the solution of 2,4,6- tribromophenol and cyanuric chloride. The best mole ratio of 2,4,6-tribromophenol to NaOH to catalyst to cyanuric chloride was determined to be 3.05：3.05：0. 05：1 by orthogonal experiment. Under the optimized condition, the yield was up to 96.6%. The industrial experiments were performed in a 3 m^3 reactor,and the consumptions of raw materials were designed as 800 kg 2,4,6-tribromophenol, 146 kg cyanuric chloride, 96.4 kg NaOH, 1 400 kg dichloromethane and 1 000 kg alcohol. The solvents dichloromethane and alcohol could be recovered more than 90%, and the product yield could maintained over 95% even through the organic solvents had been reused for 10 times. The mass loss of industrial experimental product was only 1% in TGA test under 320 ℃. Highimpact polystyrene added with this product exhibited good mechanical properties, thermal properties and flame retardancy enough for exportation.

关 键 词：阻燃剂 2 4 6-三(2 4 6-三溴苯氧基)-1 3 5-三嗪 相转移催化 橡塑助剂 

分 类 号：TQ314.24[化学工程—高聚物工业]