阳离子交换树脂催化水解多元酸酯的研究

Research on hydrolysis of multi-acid ester catalyzed by the cation exchange resin

以阳离子交换树脂作为水解催化剂,对2-膦酸丁烷-1,2,4-三羧酸五甲酯水解制备α-膦酸丁烷-1,2,4-三羧酸(PBTCA)的反应进行了研究,确定了适宜的工艺条件:水酯质量比为(1.1～1.2): 1,催化剂质量分数(占酯总质量)3.5%～4%,反应温度115～120℃,反应时间16h。以阳离子交换树脂代替液体酸作催化剂催化水解2-膦酸丁烷-1,2,4-三羧酸五甲酯,具有不腐蚀设备,反应后易于分离,催化剂用量少且可以再生重复利用,反应时间短,产品质量较高等优点;经^(31)P NMR谱测定,确认产品为PBTCA,并测得产品中PBTCA的物质的量分数为90.5%。

The reaction of preparing PBTCA by hydrolysis of 2-phosphonobutane-1, 9 4 tricarboxylic acid pentamethyl ester using cation exchange resin as hydrolysis catalyst is studied. Proper process conditions of hydrolysis reaction have been determined., mass ratio 120 C, reaction time of water to ester is 1.1 - 1.2,mass ratio of catalyst to ester is 3.5 %- 4 %, reaction temperature is 115 is 16 h. The method of using cation exchange resin as hydrolysis catalyst to replace liquid acid has advan tages of no corrosion, separating easily from products, small dosage and reuse of catalyst, short reaction time and high product quality. The molecular structure of the product is verified as PBTCA, and the PBTCA content of this product is 90.5% by ^31P NMR spectrum.