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›› 2007, Vol. 7 ›› Issue (1): 100-104.

• 过程与工艺 • 上一篇    下一篇

丁二酸催化酯化-吸附脱水联合工艺

丁斌,陈连发,郝凤岭,关昶,苗乃芬   

  1. 吉林化工学院化工系
  • 出版日期:2007-02-20 发布日期:2007-02-20

Combined Technology of Catalytic Esterification and Adsorption Dehydration of Succinic Acid

DING Bin,CHEN Lian-fa,HAO Feng-ling,GUAN Chang,MIAO Nai-fen   

  1. Department of Chemical Engineering Jilin Institute of Chemical Technology
  • Online:2007-02-20 Published:2007-02-20

摘要: 以阳离子交换树脂NKC-9固体酸为催化剂、丁二酸和甲醇为原料,采用分子筛吸附脱水技术合成丁二酸二甲酯. 考察了原料配比、催化剂用量和反应时间等因素对酯化反应的影响,通过实验得到了最佳酯化反应工艺条件:n甲醇/n丁二酸=3.0:1, NKC-9为3.5%(w)、反应温度≤120℃、反应时间4 h,在该条件下丁二酸的转化率达到98.86%. 催化剂重复使用6次后,丁二酸的转化率仍可达到98.09%. 利用红外光谱、色谱-质谱对产品进行分析,结果显示,产物中没有副产物,反应选择性很高.

关键词: 阳离子交换树脂催化剂, 沸石分子筛吸附剂, 吸附脱水, 丁二酸二甲酯, 酯化

Abstract: Synthesis of dimethyl succinate from succinic acid and methanol on cation exchange resin NKC-9 was studied under adsorption dehydration with 3A zeolite adsorbent. The effects of reaction conditions, such as molar ratio of methanol to succinic acid, catalyst content and reaction time, were investigated. The optimum reaction conditions were obtained, which were nmethanol:nsuccinic acid= 3.0:1, catalyst content 3.5% (relative to total mass of succinic acid and methanol), reaction temperature≤120℃, reaction time 4.0 h. Conversion rate of succinic acid by the process could reach 98.86%, and activity of catalyst was still kept at 98.09% after 6 times used. Analysis of the synthesized product by means of FT-IR and GC-MS showed that no by-product was observed in this process. Selectivity of catalyst was excellent.

Key words: cation exchange resin catalyst, zeolite adsorbent, adsorption dehydration, dimethyl succinate, esterification