三相相转移催化合成对苯二甲酰氯的研究

Study on synthesis of terephthaloyl dichloride by triphase phase-transfer catalysis

合成制备了既有聚醚链段又有季铵盐的新型聚合物固载相转移催化剂,并以之用于对苯二甲酸合成标题化合物。考察了催化剂、氯化亚砜、甲苯等的用量对反应收率的影响,得到了适宜的合成工艺条件为:n(TPA)∶n(SOCl2)∶n(PhCH3)∶n(PTC)=1∶3∶3∶0.06,反应温度85℃,反应时间6 h。在该条件下,对苯二甲酰氯收率>89.6%,HPLC法测定纯度>99.6%,该聚合物固载相转移催化剂可重复使用6次以上。

A novel phase-transfer catalyst with polymer-supported polyether chain and onium ions was synthesized and used as a triphase phase-transfer catalyst to be used in the synthesis of terephthaloyl dichloride from terephthalic acid. Effects of the dosage of catalyst, methylbenzene, and SOCl2 on the reaction product yield were studied and optimal synthesis conditions were derived as follows： a ratio of n （TPA） ： n （ SOC12 ） ： n （ PhCH3 ） ： n（PTC） = 1：3：3：0.06,a temperature of 85℃ and a reaction time of 6 h. Under such conditions the yield of terephthaloyl dichloride could be higher than 89.6% ,with the product purity measured by HPLC reaching 99.6%. The catalyst can be used six times or even more.