H4GeW12O40/TiO2-SiO2复合物催化合成乙酸正戊酯

Catalytic synthesis of n-amyl acetate with H4GeW12O40/TiO2-SiO2 Composite

共沉淀法制备TiO2-SiO2,采用浸渍法将锗钨酸H4GeW12O40与TiO2-SiO2复合制得催化剂,以正戊醇和乙酸为原料合成乙酸正戊酯.实验探究了复合物制备条件:锗钨酸负载量、煅烧时间、煅烧温度,乙酸正戊酯的合成条件:n(正戊醇)∶n(乙酸)、带水剂用量、催化剂用量、反应时间等因素对产率的影响.通过XRD、FT-IR、SEM对材料进行表征.实验结果在锗钨酸负载量为30%,催化剂100℃煅烧4 h,n(正戊醇)∶n(乙酸)=1.4∶1,催化剂用量为0.5%,带水剂环己烷8 mL,反应时间90 min为合成乙酸正戊酯的最优条件,产率最高可达95.3%.

TiO2-SiO2 was prepared by coprecipitation method,The catalyst was to combine H4GeW12O40 and TiO2-SiO2 together by impregnation method.And n-amyl acetate was synthesized with n-pentyl alcohol and acetic acid as raw materials.The preparation conditions of the catalyst are explored in the experiment:the load of H4GeW12O40、calcining time and calcining temperature,the synthesis conditions of n-amyl acetate:n(n-pentanol)∶n(acetic acid)、dosage of water carrying agent、amount of catalyst、reaction time and other factors on the yield were investigated.The material was characterized by XRD,FT-IR and SEM.The experiment results showed that the load of H4GeW12O40 was 30%、the catalyst was calcined at 100℃,4 h、n(n-pentanol)∶n(acetic acid)=1.4∶1、the amount of catalyst was 0.5%、the water carrying agent(cyclohexane)was 8 mL and the reaction time was 90 min were the best conditions for the synthesis of n-amyl acetate,the maximum yield could reach 95.3%.