FeCl3/ZnCl2加壓催化酰化制備4-氯二苯甲酮工業化技術

研究了在加壓和FeCl3/ZnCl2催化下,4-氯苯甲酰氯和苯發生Friedel-Crafts反應制備4-氯二苯甲酮的工藝。157.6 g苯、88.2 g 4-氯苯甲酰氯和1.3 g FeCl3/ZnCl2混合于1 L的高壓釜中,在壓力為(0.85～1.1)×106Pa、溫度為175～185℃的條件下反應8 h,經純化處理得到4-氯二甲苯酮93.1 g,摩爾收率為86.2%,w(4-氯二苯甲酮)=99.8%(HPLC)。探討了壓力、催化劑和投料比等對收率的影響。經過一次性投料4-氯苯甲酰氯175 kg的生產型中試驗證,4-氯二苯甲酮摩爾收率為82.7%。 The preparation of 4-chlorobenzophenone by acylation of benzene with 4-chlorobenzoyl chloride in the presence of FeCl3/ZnCl2 catalyst under pressure was studied.157.6 g benzene was mixed with 88.2 g 4-chlorobenzoyl chloride and 1.3 g FeCl3/ZnCl2 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-chlorobenzoyl chloride was used as raw material to afford 4-chlorobenzophenone in a molar yield of 82.7%