六溴环十二烷合成的溶剂-催化剂体系研究

Research on Solvent- Catalyst System of High Thermal Stability Hexabromocyclododecane Flame Retardant Synthesis

以环十二碳三烯(CDT)和溴素为原料在溶剂中进行加成反应,合成六溴环十二烷(HBCD)阻燃剂。以醇-卤代烃溶剂体系,开展高热稳定性、高熔点、高溴含量的六溴环十二烷阻燃剂制备研究。结果表明:使用异丁醇-二氯乙烷混合溶剂,溶剂与CDT质量比为4∶1,溴和CDT质量比为3.05∶1,异丁醇/二氯乙烷为1∶2,原料滴加过程梯级升温至50℃,保温熟化,添加溶剂质量10%的氢溴酸,总反应时间在2 h,制备的产物最高熔点大于190℃;溴含量大于72%。

H （HBCD） flame retardant was synthesized by addition of cyclododecatriene and bromine to mixed solvent. High thermal stability with high melt point and high brominated products were prepared in alcohol - halohydrocarbon mixed solvent system. The resuits showed that when solvent and CDT mass ratio was 4 ： 1, bromine and CDT mass ratio was 3. 05 ： 1, alcohol and halohydrocarbon mass ratio was 1 ： 2, cascade heating up to 50 ℃, adding 10% hydrobromic acid to system, maintaining reaction time in 2 h, prepared products got highest melt point that was above 190 ℃, and the bromine content was greater than 72%.