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2013•Acta Petrolei Sinica(Petroleum Processing Section)Requires access

Preparation and Characterization of H_6P_2W_(18)O_(62)/MCM-48 and Its Application in Catalytic Synthesis of Adipic Acid

Yan Ping

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Abstract

Dawson structure phosphotungstic acid supported on MCM-48 was prepared by impregnation method and characterized by FT-IR,XRD,SEM and EDS.The synthesis of adipic acid with cyclohexanone and 30% hydrogen peroxide under microwave irradiation was carried out as a probe reaction to study the catalytic activity of H6P2W18O62/MCM-48.The main reaction conditions were optimized with orthogonal experiments.The results showed that with 40% H6P2W18O62/MCM-48 as catalyst,under the optimal conditions of the catalyst to cyclohexanone mass ratio of 5.1%,n(C6H10O)∶n(H2O2)∶ n(H2C2O4·2H2O)=100∶450∶1.88,the reaction temperature of 95℃,microwave power of 300 W,irradiation time of 3.5 h,the isolated yield of adipic acid could reach 81.3%,and the catalyst could be reused five times with the isolated yield of adipic acid still above 64.6%.

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Dawson structure phosphotungstic acid supported on MCM-48 was prepared by impregnation method and characterized by FT-IR,XRD,SEM and EDS.The synthesis of adipic acid with cyclohexanone and 30% hydrogen peroxide under microwave irradiation was carried out as a probe reaction to study the catalytic activity of H6P2W18O62/MCM-48.The main reaction conditions were optimized with orthogonal experiments.The results showed that with 40% H6P2W18O62/MCM-48 as catalyst,under the optimal conditions of the catalyst to cyclohexanone mass ratio of 5.1%,n(C6H10O)∶n(H2O2)∶ n(H2C2O4·2H2O)=100∶450∶1.88,the reaction temperature of 95℃,microwave power of 300 W,irradiation time of 3.5 h,the isolated yield of adipic acid could reach 81.3%,and the catalyst could be reused five times with the isolated yield of adipic acid still above 64.6%.

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Available abstract

Dawson structure phosphotungstic acid supported on MCM-48 was prepared by impregnation method and characterized by FT-IR,XRD,SEM and EDS.The synthesis of adipic acid with cyclohexanone and 30% hydrogen peroxide under microwave irradiation was carried out as a probe reaction to study the catalytic activity of H6P2W18O62/MCM-48.The main reaction conditions were optimized with orthogonal experiments.The results showed that with 40% H6P2W18O62/MCM-48 as catalyst,under the optimal conditions of the catalyst to cyclohexanone mass ratio of 5.1%,n(C6H10O)∶n(H2O2)∶ n(H2C2O4·2H2O)=100∶450∶1.88,the reaction temperature of 95℃,microwave power of 300 W,irradiation time of 3.5 h,the isolated yield of adipic acid could reach 81.3%,and the catalyst could be reused five times with the isolated yield of adipic acid still above 64.6%.

Key concepts: Adipic acid, Cyclohexanone, Catalysis, Phosphotungstic acid, Yield (engineering), MCM-41, Hydrogen peroxide, Nuclear chemistry

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