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苯甲醛直接氯化法合成间氯苯甲醛的研究

Studies on Synthesis of m-Chlorobenzaldehyde from Benzaldehyde by Direct Chlorination

【作者】 童刚生

【导师】 杨运泉;

【作者基本信息】 湘潭大学 , 化学工程, 2002, 硕士

【摘要】 本文研究了以苯甲醛为原料直接氯化合成间氯苯甲醛的方法。建立了对氯化产物和原料同时分析的毛细管气相色谱分析手段;通过对可能的几种催化剂进行择优比较,选择了无水三氯化铝做为该氯化反应的催化剂;通过大量实验探讨了苯甲醛直接氯化的反应规律,在合理假设及简化的基础上建立了该氯化反应的动力学方程式:r=0.6752·exp(-1131.1/T)[Ca][Wb];运用单因素和正交实验方法考察了原料液浓度、催化剂用量、反应温度、反应时间等条件对氯化反应的影响,得到了较优的氯化反应条件。实验结果表明:该反应是一个快反应和典型的串联反应,最佳反应条件为:苯甲醛1.33mol·L-1;催化剂1.70mol·L-1;反应时间30min;反应温度50℃。 实验结果还表明:在优化反应条件下,苯甲醛的转化率可达90%以上,间氯苯甲醛的收率达到79%以上,反应选择性可达88%,氯化产物中基本无同分异构体。

【Abstract】 In the paper,the method of synthesis of m-chlorobenzaldehyde from benzaldehyde by direct chlorination has been studied.According to the references,the capillary column GC quantitative analysis method has been developed to simultaneous determination of the products and the raw material.Anhydrous aluminium is picked out as the better catalyst from many kinds of catalysts.The chlorination rule is researched by experiments and the kinetic equation is built based on the reasonable simplification for the reaction: r=0.6752· exp(-1131.1/T) [Ca] [Wb]. By parameters and orthogonal test,the effects of the concentration of the raw material and the catalyst,reaction temperature and time have been investigated,the optimized conditions for reaction are obtained. The paper also has investigated the process of chlorination,and the results show mat it is a fast reaction and a typical tandem one,the optimized conditions for the reaction are as follows: benzaldehyde 1.33 mol · L-1; anhydrous aluminium 1.70 mol · L-1; reaction time 30min; reaction temperature 50℃.Under the optimized conditions, the conversion of benzaldehyde is over 90%. The overall yield of m-chlorobenzaldehyde is 79% with 88% selectivity and almost have no structural isomer as byproducts.

  • 【网络出版投稿人】 湘潭大学
  • 【网络出版年期】2003年 02期
  • 【分类号】O625.2
  • 【下载频次】325
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