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

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。

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

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 m3 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.