阻燃剂赛克三硅酸二溴丙酯的合成及应用研究

摘要

The flame retardant of THEIC trisilicate dibromopropyl ester was synthesized with tri( 2-hydroxyethyl)isocyanurate( THEIC),silicon tetrachloride and 2,3-dibromopropanol as the raw materials. Effects of solvent,reaction temperature and loading ratio of substance on the yield of the product were dis-cussed. The optimal conditions were as follows:the mass ratio of n(silicon tetrachloride):n(2,3-dibromopro-panol):n(THEIC):n(2,3-dibromopropanol)was 3:3:1:6. 7. Silicon tetrachloride first reacted with 2,3-di-bromopropanol for 2 hours at 45℃,and then THEIC was added at 90℃ reacting for 11 hours,finally 2,3-di-bromopropanol was added at 90℃ reacting for 8 hours. The yield of product was 93. 3%. The structure and properties of the flame retardant products were characterized by FTIR,1H NMR,DTA and limiting oxygen in-dex techniques. Experimental results showed that the product was an ideal flame retardant for PVC and other materials,with high synergistic flame retardant. The limiting oxygen index of PVC was 25%,with good flame retardancy and carbon anti-dropping resistance.%以三（2-羟乙基）异氰尿酸酯（赛克）、四氯化硅与2，3-二溴丙醇为原料，合成阻燃剂赛克三硅酸二溴丙酯。探讨了溶剂、反应温度与物质的量之比对产物收率的影响，优化的工艺条件：四氯化硅、2，3-二溴丙醇、赛克与2，3-二溴丙醇的量之比为3：3：1：6.7。四氯化硅先与2，3-二溴丙醇在45℃反应2 h，再加入赛克于90℃反应11 h，最后滴入2，3-二溴丙醇保温90℃反应8 h；产物收率为93.3%。通过FTIR、1 H NMR、差热分析及极限氧指数等表征产物的结构及性能；应用实验表明该产物阻燃效能高，适合作聚氯乙烯（ PVC）等材料的阻燃剂。在较佳用量下PVC材料的极限氧指数为25%，具有良好的阻燃性、成炭防滴落性能。