加压酰化反应制备4-氯二苯甲酮工业化技术研究

Study on the Industrial Technology for Preparation of 4-Chlorobenzophenone under Pressure Acylation

摘要:

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 g4-氯苯甲酰氯和1.3g FeCl3/ZnCl2混合于1L的高压釜中，在压力为0.85×106～1.1×106Pa、温度为175～185°C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%，含量w（4-氯二苯甲酮)= 99.8%(HPLC)。探讨了压力、催化剂和投料比等收率的影响。研究该实验结果经过一次性投料4-氯苯甲酰氯175kg的生产型中试验证，4-氯二苯甲酮摩尔收率为82.7％。

Abstract:

Abstract: Preparation of 4-chlorbenzophenone by acylation of benzene with 4-chlorobenzoyl chloride in the presence of FeCl3/ZnCl2 catalyst under pressure was studied. Thus, 157.6 g benzene was mixed with 88.2 g 4-chlorobenzoyl chloride and1.3 g FeCl3/ZnCl2 in a 1L autoclave. The mixture was reacted for 8 h under 0.85×106～1.1×106Pa and 175～185°C to give 93.1g 4-chlorobenzophenone with yield of 86.2% and purity of 99.8%(by HPLC). The effects of pressure, catalyst and ratio of raw materials on the yield were also investigated. The result of our experiments was proved by productive scale up test, in which 175 kg 4-chlorobenzoyl chloride was used as raw material to afford 4-chlorobenzophenone in a molar yield of 82.7%.