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采用立体有择法合成了K6[PW11NiO39H2O]、K6[PW11CoO39H2O]、K6[PW11CuO39H2O]3种钨磷杂多酸盐,用红外光谱、紫外光谱对其进行表征。在红外光谱中有4个特征峰,在紫外光谱中有2个特征峰,证明取代之后的杂多酸盐均具有Keggin结构。通过对乙酸正丁酯进行催化的实验,探讨出酯化反应的最佳反应条件:酸醇比为0.8∶1.0,反应时间5 h,反应温度120℃,催化剂用量占原料总量的2.5%,结果表明,在最佳反应条件下其酯化率可达93.8%。
Three kinds of heteropoly tungstophosphoric acid salts of K6 [PW11NiO39H2O], K6 [PW11CoO39H2O] and K6 [PW11CuO39H2O] were synthesized by stereoselective method. Their structures were characterized by IR and UV. There are four characteristic peaks in the infrared spectrum, and two characteristic peaks in the ultraviolet spectrum, which prove that the substituted heteropolyacid salts have the Keggin structure. Through the experiment of n-butyl acetate catalysis, the optimal reaction conditions of esterification were discussed: the ratio of alcohol to alcohol was 0.8:1.0, the reaction time was 5 h, the reaction temperature was 120 ℃, the amount of catalyst was 2.5% of the total amount of raw materials, The results showed that the best reaction conditions, the esterification rate of up to 93.8%.