摘要
为了克服反应速度慢、收率低的弱点,在自行设计的实验装置上,以氯磺酸为催化剂、氧气为副反应抑制剂,进行氯气氯化丙酰氯合成2-氯代丙酰氯的反应实验。对反应的时间-转化率-选择性曲线进行了分析,获得反应的基本特点和初步规律。正交试验获得了各因素对产品收率的影响显著程度:丙酰氯和催化剂质量比>氯气与氧气比例(物质的量的比)>氯气流量>反应温度,并初步筛选出最优工艺组合条件。最后单因素优化实验,获得最佳的工艺条件为:反应温度40℃、催化剂氯磺酸与丙酰氯的质量比为6∶100、氯气流量为60L·h^(-1)、氧气与氯气物质的量比为5.5∶100。此条件可使2-氯丙酰氯的反应时间由72h缩短到3h,收率达到97.18%。优化后的工艺具有收率高、时间短等优点,并且制备工艺稳定可行,为2-氯丙酰氯生产的研究提供了技术支持。
In order to overcome the disadvantages of slow reaction rate and low yield,2-chloropropionyl chloride was synthesized by chlorination of propionyl chloride with chlorine gas on a self-designed experimental device using chlorosulfonic acid as catalyst and oxygen as side reaction inhibitor.By analyzing the time-conversion-selectivity curve of the reaction,the basic characteristics and preliminary rules of the reaction were obtained.The results of the orthogonal experiments showed that the effect of different factors on the yield of the product was as follows:propionyl chloride and catalyst mass ratio>chlorine gas to oxygen ratio(molar ratio)>chlorine gas flow rate>reaction temperature,and the optimum process combination conditions were selected.Finally,the optimum process conditions were obtained as follows:reaction temperature 40℃,the mass ratio of catalyst chlorosulfonic acid to propionyl chloride was 6∶100,the chlorine flow rate was 60L·h^(-1),and oxygen chlorine molar ratio was 5.5∶100.Under this condition,the reaction time of 2-chloropropionyl chloride was shortened from 72hto 3h,and the yield was 97.18%.The optimized process has the advantages of high yield and short time,and the preparation process is stable and feasible,which provides technical support for the research of 2-chloropropyl chloride production.
作者
孔令启
郭德来
郑世清
李玉刚
曹传波
KONG Lingqi;GUO Delai;ZHENG Shiqing;LI Yugang;CAO Chuanbo(Institute of Computer and Chemical Engineering,Qingdao University of Science and Technology,Qingdao 266042,China;Qingdao Yinke Hengyuan Chemical Process Information Technology Co.,Ltd.,Qingdao 266042,China)
出处
《青岛科技大学学报（自然科学版）》
CAS
2022年第1期35-40,共6页
Journal of Qingdao University of Science and Technology:Natural Science Edition
基金
山东省重点研发计划项目(2018GGX107004).
关键词
丙酰氯
氯磺酸
选择性
工艺优化
2-氯代丙酰氯
propionyl chloride
chlorosulfonic acid
selectivity
process optimization
2-chloropropionyl chloride
