壳聚糖硫酸盐催化合成衣康酸二甲酯  

Synthesis of dimethyl itaconate with chitosan sulfate as catalyst

作　　者：乔艳辉[1] 滕俊江[1] 李晓英[1] 苏志聪 

机构地区：[1]广东石油化工学院化学与生命科学学院,广东茂名525000

出　　处：《化工进展》2011年第4期862-865,共4页Chemical Industry and Engineering Progress

基　　金：广东省科技计划项目(2009B020312016)

摘　　要：以壳聚糖和硫酸为原料,制备了壳聚糖硫酸盐,利用红外及元素分析对壳聚糖硫酸盐进行了结构表征。将其用于催化衣康酸与甲醇合成衣康酸二甲酯的反应,考察了酸醇比、时间、催化剂用量、温度等条件对衣康酸二甲酯收率的影响,得到的最佳工艺条件为:壳聚糖硫酸盐用量占反应物料总质量的2%,n(甲醇):n(衣康酸)=7:1,反应温度为140℃,反应时间6 h,在此条件下,产品收率为86.6%。衣康酸二甲酯经气质定性分析,气相色谱检测纯度大于98%。催化剂经简单干燥处理,循环使用5次后产品收率为84.0%。Chitosan sulfate prepared from chitosan and sulfuric acid was characterized by IR and EA.Under the catalysis of chitosan sulfate,dimethyl itaconate was synthesized with itaconic acid and methanol as raw materials.The influence of synthesis conditions,such as ratio of acid to alcohol,time,amount of catalyst and temperature on dimethyl itaconate yield was studied.The optimum conditions were as follows：The amount of chitosan sulfate was 2% of the total mass of reactants.n（methanol）：n（itaconic acid）=7：1,reaction temperature 140 ℃ and reaction time 6h.Under the conditions mentioned above,the yield of product was 86.6%.Dimethyl itaconate was qualitatively analyzed by GC-MS and its purity analyzed by GC was above 98%.The catalyst used was treated by drying and the yield of treated catalyst was up to 84.0% with the catalyst used for 5 times.

关 键 词：壳聚糖硫酸盐 衣康酸 催化合成 衣康酸二甲酯 

分 类 号：TQ314[化学工程—高聚物工业]