催化精馏合成乙酸丁酯工业实验.pdf

学负兔w. xecl ulu.reom
化工进展
2010年第29卷第9期
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
1785
loweree
应用技术
催化精馏合成乙酸丁酯工业实验
李柏春,张昌伟,段贵贤
(河北工业大学化工学院,天津300130)
摘要:建立了一套以强酸型阳离子交換树脂为催化剂、乙酸和丁醇为原料,催化反应精馏合成乙酸丁酯的エ
业实验裝置,反应精馏段为立体催化精馏塔板,精馏段为陶瓷规整填料。通过实验得到了适宜的操作条件:有
机相回流比为0.6~0.8,水相回流比为3.3~4.3,釜液中乙酸浓度为30%~50%时,塔项产品的丁酯含量为80%~
90%,乙酸含量低于0.003%。实验结果表明,该催化精馏エ艺可长期连续稳定操作,年产乙酸丁酯5kt
关键词:催化精馏;乙酸了酯;强酸型阳离子交換树脂;酯化反应;工业实验
中图分类号:TQ028.13
文献标志码:A
文章编号:1000-6613(2010)09-1785-05
An industrial experiment for n-butyl acetate synthesis by
catalytic distillation
LI Baichun, ZHANG Changwei, DUAN Guixian
Department of Chemical Engineering, Hebei University of Technology, Tianjin 300130, China)
Abstract: An industrial device for n-butyl acetate synthesis was constructed with strong acidic
ion-exchange resin as catalyst, acetic acid and n-butanol as starting materials. The process was carried
out in a continuous pilot plant reactive rectification column with structured packing in the upper part
and stereo reactive distillation tray in the lower part. The optimal operation conditions were obtained
with 0.6-0.8 reflu ratio of organic phase, 3.3-4.3 reflux ratio and 30%-50% acetate acid
concentration in the column, under which 84%-90% n-butyl acetate concentration on the column to
could be achieved with acetate acid concentration less than 0.003%. Such a catalytic distillation process
could be long-term continuously operated steadily with a kt n-butyl acetate annual production
capacity.
Key words: catalytic distillation; n-butyl acetate; strong acidic ion-exchange resin; esterification
industrial experiment
乙酸丁酯是一-种重要的基础溶剂,广泛应用于于连续式催化合成乙酸丁酯生产6?。国内外许多
涂料、制革、香料和制药等行业山。国内外市场需学者在固体酸催化精馏合成乙酸丁酯方面进行了大
求日趋增大,所以乙酸衍生物加工中都把乙酸丁酯量的实验和模拟工作,如: Blagov等研究了不同
作为主要乙酸酯类产品来生产。目前工业上一般的离子交换树脂催化剂对乙酸丁酯生产过程的影
是以浓硫酸为催化剂,采用搪瓷反应釜连续法制取响: Anika等和He等?进行了催化精馏合成乙酸
乙酸丁酯刚。由于硫酸腐蚀性强导致设备材质要求丁酯的模拟和实验;廖晓宁等"?将催化剂制成填料
高、后续污染严重等问题,近年来国内外研究开发
了一系列新型的用于酯化反应的固体酸催化剂叫
收稿日期:2010-02-04;修改稿日期:201004-12。
其中强酸型阳离子交换树脂由于不溶于反应体系,
基金项目:河北省自然基金资助项目(B200700001)。
第一作者简介:李柏春(19063-),男,教授,从事新型分离1艺过
且易分离和再生,而且价格便宜、性能稳定,适用程研究。电话22256475:1 E-mail ctstlb163com