六溴环十二烷合成新工艺  

New Method to Synthesize Hexabromocyclododecane

作　　者：杨建伟[1] 杨锦飞[1] 

机构地区：[1]南京师范大学化学与环境科学学院,南京210097

出　　处：《精细石油化工进展》2005年第5期44-46,共3页Advances in Fine Petrochemicals

摘　　要：以1,5,9-环十二碳三烯(CDT)和溴素为原料,乙二醇二乙醚作溶剂,在自制催化剂作用下,合成了六溴环十二烷。考察了反应条件对产品收率的影响,结果表明,温度从10℃分三个阶段逐步升温到70℃,CDT与溶剂及催化剂质量比1:3:0.06时,产品收率75.1%。抽滤后的母液可直接循环使用2次。热重分析显示,产品失重5%时的温度为251℃。液相色谱分析产物,α,β和γ构型的六溴环十二烷分别为13.0%,8.7%和77.3%。Hexabromocyclododecane with the yield of 75 .1 % was synthesized using 1,5,9- cyclododecatriene and bromine as raw material and ethylene glycol diethyl ether as solvent in the presence of self - made catalyst. The effects of reaction conditions on the product yield were examined and the optimum reaction conditions were obtained as follows:the temperature increase from 10 ℃ to 70 ℃ in three steps,the mass ratio of 1,5,9 - cyclododecatriene to solvent and catalyst 1:3:0.06. The mother liquor after extraction could be recycled twice. The thermogravimetric analysis showed that the weight loss 5 % took place at the temperature of about 251 ℃. The result of HPLC showed that the product had three configurations such as α,β,γ with their contents of 13.0% ,8.7% and 77.3% respectively .

关 键 词：六溴环十二烷 合成工艺 反应条件 产品收率 反应温度 质量比 

分 类 号：TQ232[化学工程—有机化工]