第 49 卷第 4 期Vol. 49 No. 4
2019 年 8 月Aug 2019

所属栏目:农药及中间体

微通道反应器法合成1-乙酰基-1-氯环丙烷的工艺优化初探
杨丙连,王建博 (上海泰禾国际贸易有限公司 技术中心,上海 200335)
摘 要:以3,5-二氯-2-戊酮为原料,在相转移催化剂存在的条件下,在微通道反应器中连续反应制备1-乙酰基-1-氯环丙烷。对催化剂、液碱用量、反应温度以及流速条件等进行优化。优化的工艺条件为:反应温度80℃,3,5-二氯-2-戊酮进料流速50 mL·min-1,苄基三乙基氯化铵为催化剂,n(碱)∶n(苄基三乙基氯化铵)∶n(3,5-二氯-2-戊酮)=1.20∶0.02∶1.00,优化条件下,收率可达81.96%。
关键词:1-氯-1-乙酰基环丙烷;微通道反应器;工艺优化
中图分类号:S482.2  文献标识码:A  文章编号:1009-9212(2019)04-0017-03
Synthesis of 1-Acetyl-1-chlorocyclopropane Using Microchannel Reactor
YANG Bing-lian,WANG Jia-bo (R&D Center of CAC Shanghai International Trading Co.,Ltd., Shanghai 200335, China)
Abstract:3,5-Dichloro-2-pentanone as a raw material, under phase transfer catalyst, 1-acetyl-1-chlorocyclopropane was prepared by continuously reacting in a microchannel reactor. The catalyst, liquid base, reaction temperature and flow rate were optimized. The preferred process conditions were as follows: reaction temperature was 80℃, 3,5-dichloro-2-pentanone feed flow rate was of 50 mL·min-1; benzyl triethyl ammonium chloride was used as catalyst, n(sodium hydroxide) ∶ n(benzyl triethyl ammonium chloride) ∶ n(3,5-dichloro-2-pentanone) was of 1.20 ∶ 0.02 ∶ 1.00. Under these conditions the yield was up to 81.96%.
Key words:1-chloro-1-acetylcyclopropane; microchannel reactor; process optimization
作者简介:杨丙连(1984-),男,安徽萧县人,工程师,硕士研究生,主要从事农药及中间体合成工艺技术开发(E-mail:bingliany@126.com)
收稿日期:2019-07-31