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以 1,4 -丁二醇 ,马来酸酐 ,十二醇聚氧乙烯醚 (AEO2 )为原料 ,合成了一种结构新型的化合物——— 1,4 -丁二醇双马来酸AEO2 双酯 ,此化合物的合成由两步酯化反应组成 ,酯化反应Ⅰ采用正交实验 ,确定最优工艺条件为 :n(马来酸酐 ) :n(1,4 -丁二醇 ) =2 .15 :1.0 0 ,反应时间 1h ,催化剂用量ω(乙酸钠 ) =1.0 % .酯化反应Ⅱ采用活性炭负载杂多酸(PW1 2 C)为催化剂 ,该催化剂的最优制备条件为 :m(PW1 2 ) :m(C) ==4 :6 ,回流时间 4h ,烘干温度 15 0℃ ,烘干时间4h .酯化反应Ⅱ采用均匀实验优化工艺条件 ,最优工艺条件为 :n(1,4 -丁二醇双马来酸单酯 ) :n(AEO2 ) =1.0 0 :2 .15 ,反应温度 15 0℃ ,反应时间 14h ,催化剂用量ω(PW1 2 C) =1.5 % ,对每步合成的产物结构用IR和 1HNMR进行表征
A novel compound of 1,4 - butanediol bismaleic acid (AEO2) was synthesized by using 1,4 - butanediol, maleic anhydride and dodecanol polyoxyethylene ether (AEO2) The synthesis of this compound consisted of two steps of esterification. The orthogonal experiment was used to determine the optimum conditions for the esterification reaction Ⅰ: n (maleic anhydride): n (1,4 - butanediol) = 2. 15: 1.0 0, the reaction time was 1h and the amount of the catalyst, ω (sodium acetate) = 1.0%. Esterification Ⅱ The active preparation of PW1 2 C 2): m (C) == 4: 6, reflux time 4h, drying temperature 15 0 ℃, drying time 4h esterification reaction Ⅱ using uniform experiments to optimize the process conditions, the optimum process conditions: n 4-butanediol bismaleic acid monoester): n (AEO2) = 1.0 0: 2.15, reaction temperature 15 0 ℃, reaction time 14h, the amount of catalyst ω (PW1 2 C) = 1.5% The synthesized product structure was characterized by IR and 1HNMR