三(2,3-二溴丙基)异三聚氰脲酸酯合成研究

Study on the synthesis of tris(2,3-dibromopropyl)isocyanurate

研究了一种以氰酸钠与氯丙烯为原料合成三烯丙基异氰脲酸酯,并与液溴加成反应制备三(2,3-二溴丙基)异三聚氰脲酸酯的方法,对反应配比、反应温度.结晶溶剂等因素进行了试验。得到的较佳的工艺条件为:①在三烯丙基异氰脲酸酯的合成中,氰酸钠与氯丙烯的摩尔比为1:1.05,反应温度为95~100℃,反应溶剂采用二甲基甲酰胺,催化剂采用溴化钠,脱水剂采用氯化钙的条件下,产品收率在95%以上。②在三(2,3-二溴丙基)异三聚氰脲酸酯的合成中,液溴过量1%(摩尔分数)左右,反应温度为35℃,结品溶剂采用石油醚,用量与三氯甲烷的体积比为2:1的条件下,产品收率在92%以上。

The synthesis of triallyl isocyanurate using sodium cyanate and chloropropene as raw materials and the addition reaction with bromine to prepare tris(2,3-dibromopropyl)isocyanurate were studied.The factors were tested such as reaction ratio,reaction temperature,crystallization solvent,etc.,and better process conditions were obtained.The results were as follows:(1)in the synthesis of triallyl isocyanurate,the molar ratio of sodium cyanate to chloropropene was 1:1.05,the reaction temperature was 95—100℃,the reaction solvent was dimethylfbrmamide,the catalyst was sodium bromide,and the dehydrating agent was calcium chloride,the yield of the product was more than 95%.(2)In the synthesis of tris(2,3-dibromopropyl)isocyanurate,the excess of liquid bromine was about 1%(mole fraction),the reaction temperature was 35℃,the crystallization solvent was petroleum ether in the volume ratio to chloroform 2-1,the yield of the product was more than 92%.