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›› 2008, Vol. 8 ›› Issue (6): 1198-1102.

• 反应与分离 • 上一篇    下一篇

甘油法制备二氯丙醇反应副产物的鉴别与机理分析

赵镇 乔旭 陈献 汤吉海 崔咪芬   

  1. 南京工业大学化学化工学院 南京工业大学化学化工学院 南京工业大学化工学院 南京工业大学化学化工学院 南京工业大学化学化工学院
  • 收稿日期:2008-06-12 修回日期:2008-09-12 出版日期:2008-12-20 发布日期:2008-12-20
  • 通讯作者: 乔旭

Discrimination of By-products and Analysis of Reaction Mechanism in Preparation of Dichloropropanol from Glycerol

ZHAO Zhen QIAO Xu CHEN Xian TANG Ji-hai CUI Mi-fen   

  1. College of Chemistry and Chemical Engineering, Nanjing University of Technology College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing
  • Received:2008-06-12 Revised:2008-09-12 Online:2008-12-20 Published:2008-12-20
  • Contact: QIAO Xu

摘要: 以甘油为原料,氯化氢气体为氯化剂,分别在自制无机催化剂和有机酸的催化作用下制取了二氯丙醇. 采用气相色谱-质谱联用分析,对反应副产物进行了鉴别,分析了羧酸催化甘油氯化时副反应的反应历程,发现副产物主要包括羧酸甘油酯、羧酸自聚物、羧酸氯丙醇酯及甘油自聚物. 同时比较了有机酸与无机催化剂的优缺点,结果表明,无机催化剂催化下甘油氯化反应对一氯丙醇及二氯丙醇的总选择性可达99%以上,与有机酸催化相比,提高了4%.

关键词: 甘油, 二氯丙醇, 气相色谱-质谱联用, 副反应

Abstract: Dichloropropanol was synthesized by chlorination of glycerol with hydrogen chloride under catalysis of organic acids and self-made inorganic catalyst. The qualitative analysis of by-products was carried out by GC-MS and the side reaction mechanism of catalytic reaction of glycerol by carboxylic acid was studied. And the main by-products of carboxylic glycerin ester, autopolymer of carboxylic acid, carboxylic chloropropyl ester and diglycerine were identified. The advantages and disadvantages between organic acids catalyst and inorganic catalyst on chlorination of glycerol were compared, and the results showed that the total selectivity of monochloropropanediol and dichloropropanol was obtained to above 99%, being 4% higher than that of organic acid catalysis.

Key words: glycerol, chlorination, GC/MS, side reaction

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