改性二氧化硅固载磷钨酸催化合成环己酮甘油缩酮

Phosphotungstic acid supported on silylated activated silica for the condensation of cyclohexanone with glycerol

摘要:

以酸活化的活性二氧化硅为载体，采用化学键合的方法制备了3-氨丙基三乙氧基硅烷(APTES)化二氧化硅负载的Keggin型磷钨酸催化剂(HPW/APTES-SiO2)，并用红外光谱分析、X 射线衍射、比表面积(BET)测定，热重-差热分析等对催化剂进行了表征。并进行了催化合成环己酮甘油缩酮的反应实验。结果表明：2-羟甲基-1, 4-二氧杂螺环[4, 5]癸烷是主要的生成产物。在优化反应条件下得到环己酮转化率为92.7%，主产物的选择性达到97.8%。且催化剂便于从反应体系中分离,能重复使用多次。

Abstract:

The catalyst (HPW/APTES-SiO2) of heteropoly acid supported on acid activated and silanizing silica (APTES-SiO2) by 3-aminopropyl-triethoxysilane (APTES) was prepared via chemical bonding. The properties of the catalyst was characterized by infrared spectroscopy, X-ray diffraction, Brunauer–Emmett–Teller (BET) specific area measurement and thermogravimetric analysis（TG-DTA）.The catalytic activity of the catalyst was determined by the condensation of cyclohexanone with glycerol. The highest conversion of cyclohexanone and the selectivity of 1,4-dioxasp iro[4,5] decane-2-methanol reached 92.7% and 97. 8%, respectively, by using HPW/APTES-SiO2 as the catalyst under the optimum reaction conditions .The recycling tests show that the catalyst can be easily separated from the reaction system and to be reused many times.