Condensation of Glycerol With Acetone Over the Silica-SupportedPhosphotungstic Acid Catalysts

Abstract

Abstract: Silica-supported H3PW12O40catalysts (TPA/SiO₂) with different TPA loadings were prepared by sol-gel method and characterized by XRD and N2-adsorption．Their activities in the condensation of glycerol with acetone to produce acetone ketal of glycerol were studied. The effects of calcination temperature of catalyst, TPA loading, catalyst dosage and reaction time were investigated in detail. It is found that the TPA/SiO₂ catalyst, with mean grain size of 20.9~26.4 nm in typical amorphous phase, exhibited excellent catalytic activity and good stability for synthesis of acetone ketal of glycerol. The optimal conditions areasfollows: catalyst calcination temperature 500 ℃, the mass radio of the TPA loading 15.0%, n(acetone)∶n(glycerol)=1∶3, catalyst/glycerol mass ratio 8.0%, cyclohexane 15 mL and reaction time 6.0 h. The yield of Solketal can reach over 93.2% at the optimum conditions.

Key words: Sol-gel, TPA/SiO₂, Solid acid, Condensation reaction, Solketal

摘要：

利用溶胶-凝胶法制备了二氧化硅负载的磷钨酸（TPA/SiO₂）固体酸催化剂，用XRD和N₂-吸附脱附对TPA/SiO2固体酸催化剂进行了表征，研究了催化剂在甘油与丙酮缩合反应中的催化性能，考察了催化剂的焙烧温度、磷钨酸质量分数、反应时间和催化剂质量等对反应性能的影响。结果表明:TPA/SiO2固体酸是平均颗粒为20.9~26.4 nm的无定形催化剂，在甘油与丙酮缩合反应中具有高催化活性和良好稳定性。最佳条件为：催化剂的焙烧温度500 ℃，TPA质量分数15.0%，n(甘油)∶n(丙酮)=1∶3，催化剂质量为甘油质量的8.0%，环己烷15 mL，反应时间6.0 h。在最佳的反应条件下，丙酮甘油缩酮收率为93.2%。

关键词: 溶胶-胶凝, 〓TPA/SiO2, 〓固体酸, 〓缩合反应, 〓丙酮甘油缩酮

REN Li-guo, ZHANG Xiao-li, GAO Wen-yi. Condensation of Glycerol With Acetone Over the Silica-SupportedPhosphotungstic Acid Catalysts [J]. Journal of Liaoning Petrochemical University, 2011, 31(4): 9-13.

任立国，张晓丽，高文艺. 二氧化硅负载磷钨酸催化甘油与丙酮的缩合反应[J]. 辽宁石油化工大学学报, 2011, 31(4): 9-13.

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Condensation of Glycerol With Acetone Over the Silica-SupportedPhosphotungstic Acid Catalysts

二氧化硅负载磷钨酸催化甘油与丙酮的缩合反应

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