H_(13)Si_2Mo_(13)V_5O_(62)·24H_2O的制备、表征及催化合成乙酸正丁酯的研究

Preparation and Characterization of H_(13)Si_2Mo_(13)V_5O_(62)·24H_2O and Its' Catalytic Performance on Synthesis of n-Butyl Acetate

采用分步加酸、乙醚-丙酮萃取的方法制备了H13Si2Mo13V5O62·24H2O杂多酸,通过IR、XRD、TG对其结构进行了表征.研究了其催化合成乙酸正丁酯的反应,考察了酸醇比、杂多酸用量、反应时间和反应温度等因素对反应的影响.最终确定最优反应条件为:催化剂用量为5%(按乙酸质量计算),酸醇摩尔比是1.0∶2.0,反应时间为75 min,反应温度为115℃.

H13Si2Mo13V5O62·24H2O is synthesized by the modified method of gradually adding acid and being extracted by acetone-ether.Its structure is then characterized by means of IR,XRD and TG.Its′catalytic per-formance on synthesis of n-butyl acetate are then studied.The molar ratio of n-butyl alcohol to acetic acid,a-mount of catalyst,reaction time and temperature are investigated.The optimized condition are as follows：the a-mount of catalyst is 5% of the amount of acid;molar ratio of acetic acid and butyl alcohol is 1. 0∶2. 0;reaction time is 75 minutes;and temperature is 1 15 ℃.