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| FeCl_3/ZnCl_2加压催化酰化制备4-氯二苯甲酮工业化技术 | |
| 引用本文： | 李树安,李润莱,张珍明,葛洪玉,齐家娟. FeCl_3/ZnCl_2加压催化酰化制备4-氯二苯甲酮工业化技术[J]. 精细化工, 2013, 30(6) |
| 作者姓名： | 李树安 李润莱 张珍明 葛洪玉 齐家娟 |
| 作者单位： | 1. 淮海工学院 江苏省资源开发研究院,江苏连云港,222001 2. 香港科技大学 化学工程及生物分子工程系,香港,999077 3. 淮海工学院 江苏省资源开发研究院,江苏连云港222001;中国矿业大学 环测学院,江苏徐州221116 4. 中国矿业大学 环测学院,江苏徐州,221116 |
| 基金项目： | 江苏省高校产业化推进项目，江苏省连云港市产学研联合研究项目，江苏省高校优势学科“海洋科学与技术”建设工程资助项目，Industrial Promotion Project of Jiangsu University，Lianyungang United Research Project of Production-University-Institute，Project of Advantages Disciplines of Science and Technology of Marine in Jiangsu Universities Construction |
| 摘 要： | 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%。 |
| 关 键 词： | 4-氯二苯甲酮 加压酰化 FeCl3/ZnCl2 工业技术 精细化工中间体 |
A Study on the Industrial Technology for the Manufacture of 4-Chlorobenzophenone by Acylation Under Pressure |
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| Abstract: | 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%. |
| Keywords: | 4-chlorobenzophenone acylation under pressure FeCl3/ZnCl2 industrial technology fine chemical intermediates |
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