第 39 卷第 2 期Vol. 39 No. 2
2009 年 4 月Apr 2009

所属栏目:有机合成原料

连续酯化制备1,6-己二酸二甲酯
石鸣彦 (中国石油 辽阳石化分公司研究院,辽宁 辽阳 111003)
摘 要:以DNW-Ⅰ型强酸型阳离子交换树脂(DNW-Ⅰ型催化剂)为催化剂,己二酸和甲醇为原料,经间歇酯化和连续酯化反应后通过精馏可制备选择性为100%的1,6-己二酸二甲酯。结果表明,当DNW-Ⅰ型催化剂用量为5%(以己二酸计,m/m,下同)时,己二酸间歇及连续酯化后转化率分别大于68%和98%。优化实验条件为:间歇酯化:催化剂用量5%,n(甲醇)∶n(己二酸)=2.5∶1.0,反应温度80~85℃,反应时间4 h;连续酯化:间歇酯化产物进料为30~70 mL/h,甲醇进料为95~210 mL/h,醇酸摩尔比>60。
关键词:1,6-己二酸;甲醇;1,6-己二酸二甲酯;酯化反应
中图分类号:TQ225.24+2  文献标识码:A  文章编号:1009-9212(2009)02- 0047-03
Preparation of Dimethylene Adipate by Continuous Esterification
SHI Ming-yan (Research Institute of Liaoyang Petrochemical Company,Sinopetro,Liaoyang 111003,China)
Abstract:1,6-Dimethyl adipate was synthesized from adipic acid and methanol with 100% selectivity in a batch-continuous esterification process. DNW-I strong-acid cation exchange resin was used as catalyst. The results showed that the conversion of adipic acid in the batch step and the continuous step were more than 68% and 98%,respectively,at the catalyst level of 5%. The optimum conditions were as following:for the batch process,the mass fraction of catalyst 5%,methanol/adipic acid(mole ratio)2.5∶1.0,temperature 80~85℃,time 4 h;for the continuous step,the flow rate of the batch process product 30~70 mL/h,methanol 95~210 g/h,methanol/adipic acid(mole ratio)more than 60.
Key words:adipic acid;methanol;1,6-dimethyl adipate;esterification
作者简介:石鸣彦(1974-),女,山东莱州人,工程师,主要从事精细石油化工产品技术研发。(E-mail:shimy@petvcchina.com.cn)
收稿日期: 2008-11-1