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作 者:杨泽慧[1] 陈声宗[1] 李文生[1] 张竞[1] 李瑞生[1]
出 处:《精细化工》2002年第1期42-44,共3页Fine Chemicals
摘 要:采用均匀实验设计和单纯形寻优法得出氯化溴法催化合成十溴二苯醚最优工艺条件 :在金属型催化剂HD2 0 0 1存在的条件下 ,n(C12 H10 O)∶n(BrCl) =1∶13 ,m(HD2 0 0 1)∶m(C12 H10 O)=1∶10 ,二苯醚滴加温度为 12℃ ,回流反应时间为 7 2h ,在此条件下 ,十溴二苯醚收率达97 1% ;催化剂HD2 0 0 1克服了传统催化剂易潮解、吸水 ,不易储存、运输的缺点 ,更适于工业化生产 ;使用二甲苯这种经济易得的溶剂 。A new process for catalytic synthesis of decabromodiphenyl ether with improved quality was carried out by brominating diphenyl oxide with bromine chloride in the presence of a metal catalyst HD2001.The optimum process conditions were obtained by uniform test design and simplex optimization.Under the optimized conditions molar ratio of diphenyl ether to bromine chloride 1∶13, m (HD2001)∶ m (C 12 H 10 O)=1∶10,diphenyl ether feeding temperature 12 ℃ and reflux time 7 2 h,yield of purified decabromodiphenyl ether was up to 97 1%.Catalyst HD2001 is more suitable for industrial production of decabromodiphenyl ether compared with traditional ones.Meanwhile,a simple process for purification of decabromodiphenyl ether was also developed by using convenient solvent xylene.
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