FeCl_3/ZnCl_2加压催化酰化制备4-氯二苯甲酮工业化技术

A Study on the Industrial Technology for the Manufacture of 4-Chlorobenzophenone by Acylation Under Pressure

研究了在加压和FeCl3/ZnCl2催化下,4-氯苯甲酰氯和苯发生Friedel-Crafts反应制备4-氯二苯甲酮的工艺。157.6 g苯、88.2 g 4-氯苯甲酰氯和1.3 g FeCl3/ZnCl2混合于1 L的高压釜中,在压力为(0.85～1.1)×106Pa、温度为175～185℃的条件下反应8 h,经纯化处理得到4-氯二甲苯酮93.1 g,摩尔收率为86.2%,w(4-氯二苯甲酮)=99.8%(HPLC)。探讨了压力、催化剂和投料比等对收率的影响。经过一次性投料4-氯苯甲酰氯175 kg的生产型中试验证,4-氯二苯甲酮摩尔收率为82.7%。

The preparation of 4-chlorobenzophenone by acylation of benzene with 4-chlorobenzoyl chloride in the presence of FeC13/ZnC12 catalyst under pressure was studied. 157.6 g benzene was mixed with 88.2 g 4-ehlorobenzoyl chloride and 1.3 g FeC13/ZnC12 in a 1 L autoclave. The mixture reacted for 8 h under （0. 85 - 1.1 ） × 106 Pa and at 175 - 185 ℃ to give 93.1 g 4-chlorobenzophenone with a yield of 86.2% and a purity of 99.8% （by HPLC）. The effects of pressure,catalyst and ratio of raw materials on the yield were also investigated. The experimental results were proved by a productive scale-up test, in which 175 kg 4-ehlorobenzoyl chloride was used as raw material to afford 4- chlorobenzophenone in a molar yield of 82.7 %.