固体酸催化酯水解制备有机膦酸

Study on preparation of phosphonate and hydrolysis of ester catalyzed by solid acid

以SO_4^(2-)/M_xO_y型固体酸作为水解催化剂,对2-膦酸丁烷-1,2,4-三羧酸五甲酯水解制备2-膦酸丁烷-1,2,4-三羧酸(PBTCA)的反应进行了研究,探讨了催化剂加入量、水酯比、反应温度以及反应时间对水解转化率的影响,确定了反应的最佳工艺条件。结果表明,以SO_4^(2-)/M_xO_y型固体酸催化水解PBTC五甲酯,能有效缩短水解反应时间,提高产品质量,并且催化剂活性高、用量少,产品经^(31)PNMR谱测定,PBTCA物质的量分数达91.6%。

The preparation of PBTCA by hydrolization of 2 - phosphonobutane -1,2,4- tricarboxylic acid pentamethyl ester is studied using SO_4^（2-）/M_xO_y solid acid as hydrolysis catalyst.The effects of the amount of catalyst,the ratio of water to ester, reaction temperature and reaction time on the hydrolysis conversion rate are discussed and the optimum conditions are determined. The results show that using SO_4^（2-）/M_xO_y solid acid as hydrolysis catalyst,the reaction time is shortened effectively and the quality of the product is improved.The catalyst shows high activity and the dosage is small.The molar fraction of PBTCA in the product reaches 91.6%by determination of ^（31）P NMR spectrum.