阻燃剂2,3-二溴丁二酸二(2,3-二溴丙)酯的合成及应用

Synthesis and Application of Flame Retardant 2,3- Dibromodi - (2,3-dibormopropyl) Succinate

以2,3-二溴丙醇、顺丁烯二酸酐和溴为原料,合成了添加型阻燃剂2,3-二溴丁二酸二(2,3-二溴丙)酯。考察了物料摩尔比、反应时间、反应温度对酯产率的影响。结果表明,在二溴丙醇与顺酐摩尔比2.4:1、反应时间8 h条件下,丁烯二酸二酯中间产品产率为70％;在溴素与中间产品摩尔比1.3:1、温度55-60℃、时间6 h条件下,最终产品2,3-二溴丁二酸二(2,3-二溴丙)酯产率达90％以上。对中间产品和最终产品结构进行了红外光谱表征。将合成的阻燃剂用于环氧树脂,当用量为20％时,环氧树脂氧指数由19.5％提高到25.5％,再与10％Sb2O3复配使用时,氧指数达28.5％,说明合成阻燃剂与Sb2O3的协同性好。

An additive flame retardant 2,3 - dibromodi(2,3 - dibromopropyl) succinate was synthesized using 2,3 - dibromopropanol, maleic anhydride and bromine as raw material. The effects of reaction conditions including the molar ratio of reactants, reaction time, and reaction temperature on ester yield were examined. The result showed the yield of intermediate butene dicarboxylate was 70% when the molar ratio of 2,3 - dibromo - 1 - propanol to maleic anhydride was 2.4:1 for reaction time of 8 hours.The yield of final product 2,3 - dibromodi(2,3 - dibromopropyl) succinate was over 90 % when the molar ratio of bromine to intermediate was 1.3:1 at 55-60℃ for reaction time of 6 hours. The intermediate and final product were characterized by IR spectrum. The synthesized flame retardant could be used in epoxy resin with increase of LOI from 19.5% to 25.5% when the content of flame retardant was 20% . The combination of 20% 2,3 dibromodi - (2,3 - dibromopropyl) succinate and 10% Sb2O3 could increase LOI to 28.5 % showing good synergism.