云南化工2024,Vol.51Issue(9) :42-47.DOI:10.3969/j.issn.1004-275X.2024.09.09

光气法合成苯乙酰氯的工艺研究

Research on the Synthesis of Phenylacetyl Chloride by Phosgene Method

李舒涛 陶宗树 唐思 付华权 彭勇 段勇 杜佳芸
云南化工2024,Vol.51Issue(9) :42-47.DOI:10.3969/j.issn.1004-275X.2024.09.09

光气法合成苯乙酰氯的工艺研究

Research on the Synthesis of Phenylacetyl Chloride by Phosgene Method

李舒涛 1陶宗树 1唐思 1付华权 1彭勇 1段勇 1杜佳芸1
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作者信息

  • 1. 重庆长风化学工业有限公司 光气衍生物工程技术研究中心,重庆 401221
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摘要

采用光气和苯乙酸为原料合成苯乙酰氯,对影响反应的温度、搅拌速度、光气通入速度、原料配比、保温时间及催化剂种类、用量等各类关键因素进行了优化,挖掘出了最佳合成条件,即以N,N-二甲基甲酰胺为催化剂,加入的量为苯乙酸质量的2%,苯乙酸与光气的物质的量比为1∶1.5,搅拌速度控制在90 r/min,在85 ℃的温度下,以70 g/h的速度通入光气,光气通入结束后保温反应0.5 h.此优化条件下合成的苯乙酰氯纯度达99.74%,收率96.50%,催化剂可循环再利用.相比于二氯亚砜法合成的苯乙酰氯,具有绿色环保、尾气易回收利用以及产品品质较高的优势.

Abstract

Phenylacetyl chloride was synthesized from phosgene and phenylacetic acid.The key factors of the reaction system(including temper-ature,stirring speed,phosgene introduction speed,material ratio,holding time,catalyst type and dosage,etc.)were optimized.The optimal synthesis conditions were discovered,in which the product was prepared in 99.74%yield with 96.50%purity was obtained as follows:N,N-dimethylformamide was used as the catalyst,the mass of catalyst was 2%(based on phenylacetic acid),the molar ratio of phenylacetic acid to phosgene was 1∶1.5,and the stirring speed was controlled at 90 r/min,at a reaction temperature of 85 ℃,introduce phosgene at a rate of 70 g/h,and keep the reaction for 0.5h after the completion of the introduction of phosgene,and the catalyst can be recycled.In comparison with the dithionyl chloride method,the phosgene method has advantages of green environmental protection,easy recycling of exhaust gas,and higher product quality.

关键词

苯乙酰氯/光气/N,N-二甲基甲酰胺

Key words

Phenylacetyl Chloride/Phosgene/N,N-dimethylformamide

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出版年

2024
云南化工
云南省化工研究院 云天化集团有限责任公司 云南煤化工集团有限公司 云南省化学化工学会

云南化工

影响因子:0.272
ISSN:1004-275X
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