TiSiW_(12)O_(40)/TiO_2催化合成苹果酯-B的研究

CATALYTIC SYNTHESIS OF FRAISTONE BY TiSiW_(12)O_(40)/TiO_2

报道了固载杂多酸盐TiSiW12O40/TiO2的制备方法,并以TiSiW12O40/TiO2为多相催化剂,通过乙酰乙酸乙酯和1,2 丙二醇反应合成了苹果酯 B,探讨TiSiW12O40/TiO2对缩酮反应的催化活性,较系统地研究了原料量比、催化剂用量、反应时间诸因素对产品收率的影响。实验表明:TiSiW12O40/TiO2是合成苹果酯 B的良好催化剂,在乙酰乙酸乙酯与1,2 丙二醇的物质的量比为1∶1.5、催化剂用量为反应物料总质量的1.0%、环己烷为带水剂、反应时间1.0h的优化条件下,苹果酯 B的收率可达83.3%。

A new environmental friendly catalyst,TiSiW12O40/TiO2 was prepared and characterized by IR and XRD.Synthesis of fraistone with ethyl acetoacetate and 1,2propylene glycol as reactants and TiSiW12O40/TiO2 as catalyst was studied.Results showed that TiSiW12O40/TiO2 was an excellent catalyst for the synthesis of fraistone,and the optimum reaction conditions was as follows: molar ratio of ethyl acetoacetate to 1,2propylene glycol 1∶1.5, dosage of catalyst 1.0% of feed stock,reaction time 1.0 h.under this condition,yield of fraistone was about 83.3%.The catalyst can be reused for at least six times.