间苯二甲酸二甲酯-5-磺酸钠的催化合成研究

Catalytic synthesis of sodium dimethyl isophthalate-5-sulfonate

目的探究制备SIPM中磺化、酯化、中和过程中的各种因素对产品得率的影响。方法运用正交设计,以间苯二甲酸(IPA)为原料制备SIPM,将IPA用发烟硫酸磺化,磺化物不经分离,利用剩余废酸及催化剂直接进行酯化,再经中和,精制SIPM。结果得出各因素对产率影响的大小顺序及各因素的数值。结论反应最佳条件为:IPA∶发烟硫酸为1∶1;加二氧化硅时温度为165℃;加硫酸镉时温度为130℃;酯化温度为66℃;IPA∶甲醇为1∶1.1;酯化时间为4 h;磺化时加硫酸镉后的保温时间为40 min;加入硫酸汞后的保温时间为50 min;加入SiO2后升温至170℃,升温前的保温时间为50 min。

Objective:To study the effects of various factors on the yield of product in the process of preparing SIPM, esterification and neutralization. Methods:In this experiment, isophthalic acid(IPA) is the materials for the preparation of SIPM. The IPA is sulfonated with oleum, then the sulfonated material is not separated, and the remaining waste acid and catalyst are directly used for esterification, and then neutralization and purification SIPM. Results:The order of magnitude of the factors affecting the yield and the numerical value of the factors are obtained. Conclusion: The best reaction conditions were: IPA:∶Oleum=1∶1;to add silica when temperature is 165℃;to add cadmium sulfate when temperature is 130℃;the esterification temperature is 66℃;IPA∶methanol =1∶1.1;the esterification time is 4 h;after adding cadmium sulfate the heat preservation time is 40 min;after adding mercury sulfate the heat preservation time is 50 min;after joining SiO2, rising temperature to 170℃, the heat preservation time is 50 min before rising temperature.