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复合固体超强酸催化合成丁酮乙二醇缩酮
Synthesis of butanone glycol ketal by the composite solid superacid catalyst S2O82-/TiO2
【摘要】 以钛酸丁酯和过硫酸铵为主要原料,采用溶胶-凝胶法制备新型固体超强酸催化剂S2O82-/TiO2,并用于丁酮乙二醇缩酮的合成反应.该催化剂制备的最优条件为:焙烧温度500℃,(NH4)2S2O8,浸渍浓度0.6 mol/L,焙烧时间2.5 h.采用该催化剂通过正交试验得到合成丁酮乙二醇缩酮的最佳条件为:n(乙二醇)∶n(丁酮)=1.5∶1.0,催化剂用量为0.6 g(以0.1 mol丁酮为准),带水剂环己烷用量10 mL,反应时间1.5 h,其收率可达87.6%以上.
【Abstract】 The novel composite solid superacid catalyst S2O82-/TiO2 was prepared by Ti(OC4H9)4and(NH4)2S2O8 as the raw material with sol-gel method,and it was used in the synthesis of butanone glycol ketal.The optimal conditions of catalyst preparation were: calcination temperature 500 ℃,impregnation concentration of ammonial peroxodisulfate 0.6 mol/L,calcination time 2.5 h.Based on the orthogonal experiment,the optimal synthetic conditions of butanone glycol ketal were resulted as follows: the molar ratio of glycol to butanone was 1.5∶1.0,mass of the catalyst was 0.6 g(when butanone was 0.1 mol),the volume of the water removing reagent cyclohexane was 10 mL,and the reaction time was 1.5 h.The yield was more than 87.6% under above conditions.
【Key words】 solid superacid; catalyst reaction; butanone glycol ketal; organic synthesis;
- 【文献出处】 郑州轻工业学院学报(自然科学版) ,Journal of Zhengzhou University of Light Industry(Natural Science) , 编辑部邮箱 ,2009年01期
- 【分类号】TQ224.2;TQ655
- 【被引频次】6
- 【下载频次】156