五溴苄基溴的合成新工艺研究

摘要

Pentabromobenzyl bromide synthetized by pentabrominated toluene and bromine with composite initiators of the mixture of AIBN and BPO was studied. The effects of different factors such as initiation efficiency, the amount of composite initiators, mass ratio of bromine to pentabrominated toluene, reaction time were investigated in detail. The results showed that it exhibited excellently initiation efficiency for composite initiators of AIBN and BPO to be mixed mass ratio of 1: 1.5 as composite initiators. When the dosage of composite initiators was based on 0.6 % of the massl of pentabrominated toluene, the mass ratio of bromine to pentabrominated toluene was 2.5:1, carbon tetrachloride was solvent, the reaction time was 6 h, the yield of pentabromobenzyl was 90.1%.%以AIBN和BPO混合物为复合引发剂，由五澳甲苯和溴合成五溴苄基溴。重点考察了复合引发剂的掺杂比，以及对复合引发剂引发效率、引发剂的用量、原料配比、反应时间等工艺参数进行优化。实验结果表明，m（AJBN）：m（BPO）=1．5为复合引发剂，对合成五溴苄基溴的合成：行着良好的引发效率，当w（复合引发荆）=0．6％（以五溴甲苯的质量为参比），n（溴）：n（五溴甲苯）=2，5：1，CCl4为溶剂，反应6h后，五澳苄基溴的产率达90．1％。