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作 者:任建军 张伟 REN Jian-jun;ZHANG Wei(Jiyuan Hengshun New Material Co.,Ltd.,Jiyuan Henan 459000,China)
机构地区:[1]济源市恒顺新材料有限公司,河南济源459000
出 处:《辽宁化工》2024年第1期61-64,共4页Liaoning Chemical Industry
摘 要:以邻氯甲苯为原料,N-氯代丁二酰亚胺为氯化剂进行氯化,在氯化锌作用下滴水进行水解,精馏制备成品邻氯苯甲醛。经过对氯化反应、水解反应条件进行筛选,得到最佳工艺条件:(1)氯化反应:反应温度105℃,物质的量n(N-氯代丁二酰亚胺)∶n(过氧化苯甲酰)∶n(邻氯甲苯)=2.3∶0.05∶1;(2)水解反应:反应温度135~145℃,物质的量n(氯化锌)∶n(邻氯二氯苄)=0.05∶1。该工艺条件下,全程反应收率可达到93%,成品纯度可达到99.5%。o-Chlorotoluene was chlorinated with N-chlorosuccinimide as chlorinating agent,and then hydrolyzed by dripping water under the action of zinc chloride,and the finished product o-chlorobenzaldehyde was prepared by rectification.After screening the conditions of chlorination reaction and hydrolysis reaction,the optimum technological conditions were obtained as follows:in the chlorination reaction,the reaction temperature was 105℃,and n(N-chlorosuccinimide)∶n(benzoyl peroxide)∶n(o-chlorotoluene)=2.3∶0.05∶1;in the hydrolysis reaction,the reaction temperature was 135~145℃,and n(zinc chloride)∶n(o-chlorobenzyl chloride)=0.05∶1.Under this condition,the yield of the whole reaction could reach 93%,and the purity of finished product could reach 99.5%.
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