对氯苄叉二氯相转移催化水解制备对氯苯甲醛工艺研究
|
摘要
采用相转移剂催化水解对氯苄叉二氯制备对氯苯甲醛,考察了催化剂种类和用量、水的用量、水解反应温度对水解反应的影响。实验结果表明,以PTC-1相转移剂为对氯苄叉二氯水解制备对氯苯甲醛的催化剂,适宜的水解反应条件为:催化剂用量为对氯苄叉二氯质量的0.15%,水与对氯苄叉二氯的质量比为2.0∶1,反应温度100℃。在此条件下,对氯苄叉二氯水解转化率达99%以上。
p-Chlorobenzaldehyde was prepared by the catalytic hydrolysis reaction of p-chlorobenzal chloride with phase transfer agent. The influence of catalyst type and amount, amount of water and temperature on hydrolysis reaction, were investigated. The results showed, in the preparation of p-chlorobenzaldehyde by hydrolysis of p-chlorobenzal chloride, PTC-1 was applied as the phase transfer catalyst agent, and the optimum hydrolysis reaction conditions were: catalyst dosage was 0.15% of p-chlorobenzal chloride, the mass ratio of water to p-chlorobenzal chloride was 20:1, and temperature was 100 ℃. Under these conditions, the hydrolysis conversion rate of p-chlorobenzal chloride was more than 99%.
p-Chlorobenzaldehyde was prepared by the catalytic hydrolysis reaction of p-chlorobenzal chloride with phase transfer agent. The influence of catalyst type and amount, amount of water and temperature on hydrolysis reaction, were investigated. The results showed, in the preparation of p-chlorobenzaldehyde by hydrolysis of p-chlorobenzal chloride, PTC-1 was applied as the phase transfer catalyst agent, and the optimum hydrolysis reaction conditions were: catalyst dosage was 0.15% of p-chlorobenzal chloride, the mass ratio of water to p-chlorobenzal chloride was 20:1, and temperature was 100 ℃. Under these conditions, the hydrolysis conversion rate of p-chlorobenzal chloride was more than 99%.
引文
[1]章思规.实用精细化学品手册(有机卷)[M].北京:化学工业出版社,1996.
[2]徐克勋.精细有机化工原料及中间体手册[M].北京:化学工业出版社,1998.
[3]吕早生,等.从煤焦油洗油中提取喹啉的研究[J].武汉科技大学学报:自然科学版,2003,26(4):367-369.
[4]吕咏梅.对氯苯甲醛合成技术进展与市场分析[J].现代农药,2002(3):34-36.
[5]袁志庆,慎炼,葛忠华.对氯苯甲醛的合成[J].浙江化工,2001,32(1):5-6.
[6]管泽民,祁国珍.相转移催化反应的研究——Ⅱ.聚乙二醇作催化剂合成对硝基苯甲醚[J].华东化工学院学报,1992,18(2):215-220.
[7]罗海航,等.亲电取代反应中相转移催化剂结构和性能的关系[J].华东理工大学学报,1996,22(2):153-157.
[2]徐克勋.精细有机化工原料及中间体手册[M].北京:化学工业出版社,1998.
[3]吕早生,等.从煤焦油洗油中提取喹啉的研究[J].武汉科技大学学报:自然科学版,2003,26(4):367-369.
[4]吕咏梅.对氯苯甲醛合成技术进展与市场分析[J].现代农药,2002(3):34-36.
[5]袁志庆,慎炼,葛忠华.对氯苯甲醛的合成[J].浙江化工,2001,32(1):5-6.
[6]管泽民,祁国珍.相转移催化反应的研究——Ⅱ.聚乙二醇作催化剂合成对硝基苯甲醚[J].华东化工学院学报,1992,18(2):215-220.
[7]罗海航,等.亲电取代反应中相转移催化剂结构和性能的关系[J].华东理工大学学报,1996,22(2):153-157.