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富马酸二甲酯的合成工艺研究
STUDY ON PROCESSING CONDITION OF THE SYNTHESIS OF DIMETHYL FUMARATE
【摘要】 以马来酸酐为原料二步法合成富马酸二甲酯。首先,马来酸酐水解异构化合成富马酸,采用一种新的异构化催化剂,反应的最优条件为15g马来酸酐和25ml水反应,加入0.1g催化剂,回流1h,产率为93.2%。然后,富马酸酯化合成富马酸二甲酯,采用对甲苯磺酸作催化剂,通过正交实验得到反应的最佳条件为:富马酸15g,对甲苯磺酸3g,醇酸摩尔比12:1,回流4h,产率67.5%。二步法的总产率可达62.9%。
【Abstract】 Dimethyl fumarate was prepared from maleic anhydride by two reaction steps. First, fumaric acid was yielded by hydrolysis and isomerization from maleic anhydride with a new catalyst. The yield of fumaric acid was 93.2% on the optimum condition of 15g of maleic anhydride, 25mL of water, 0. 1g of catalyst and reaction time being 1h. With the second step, dimethyl fumarate was yieldal by meth - esterificaion from fumaric acid. The catalyst of this reartion was p - toluene sulfonic acid. The optimum reaction condition obtained by means of orthogonal test was 15g of fumaric acid,3. 0g of p - toluene sulfonic acid, the mole ratioof methane alcohol to fumaric acid being 12 to 1 and reaction time being 4h .The yield of dimethyl fumaratewas 67.5% .The total yield of the two steps was 62.9%.
- 【文献出处】 化学工程师 ,Chemical Engineer , 编辑部邮箱 ,1999年02期
- 【分类号】TQ22
- 【被引频次】8
- 【下载频次】206