2007Journal of Henan Polytechnic UniversityRequires access

Synthesis of n-butyl acetate catalyzed by palygorskite supported tungstosilicic acid

Tingting Wu

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Abstract

In order to make a heterogeneous catalyst which can be easily recycled from esterification system and,to some extent,diminish the toxicity and corrosion of widely used liquid catalysts simultaneously,acid Palygorskite supported tungstosilicic acid was prepared by adsorption method through reflux and evaporation,and was characterized by FTIR spectroscopy.The FTIR spectra shows that interaction occurs between carrier and 12-tungstocilicic acid which maintains the Keggin type structure.The synthesis of n-butyl acetate was catalyzed by this kind of catalyst and the reaction conditions were measured by orthogonal experimental design.Under the reaction conditions that molar ratio of n-butanol to acetic acid is 1∶1.1,volume of cyclohexane acting as water carrier is selected as 6 ml,reaction time is 70 min and temperature is at 115℃,the yield could reach 77.3%.The catalyst recycling result has shown that a deactivation occurs,which due to the redissolution of the polyanion in the reaction medium.

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In order to make a heterogeneous catalyst which can be easily recycled from esterification system and,to some extent,diminish the toxicity and corrosion of widely used liquid catalysts simultaneously,acid Palygorskite supported tungstosilicic acid was prepared by adsorption method through reflux and evaporation,and was characterized by FTIR spectroscopy.The FTIR spectra shows that interaction occurs between carrier and 12-tungstocilicic acid which maintains the Keggin type structure.The synthesis of n-butyl acetate was catalyzed by this kind of catalyst and the reaction conditions were measured by orthogonal experimental design.Under the reaction conditions that molar ratio of n-butanol to acetic acid is 1∶1.1,volume of cyclohexane acting as water carrier is selected as 6 ml,reaction time is 70 min and temperature is at 115℃,the yield could reach 77.3%.The catalyst recycling result has shown that a deactivation occurs,which due to the redissolution of the polyanion in the reaction medium.

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Available abstract

In order to make a heterogeneous catalyst which can be easily recycled from esterification system and,to some extent,diminish the toxicity and corrosion of widely used liquid catalysts simultaneously,acid Palygorskite supported tungstosilicic acid was prepared by adsorption method through reflux and evaporation,and was characterized by FTIR spectroscopy.The FTIR spectra shows that interaction occurs between carrier and 12-tungstocilicic acid which maintains the Keggin type structure.The synthesis of n-butyl acetate was catalyzed by this kind of catalyst and the reaction conditions were measured by orthogonal experimental design.Under the reaction conditions that molar ratio of n-butanol to acetic acid is 1∶1.1,volume of cyclohexane acting as water carrier is selected as 6 ml,reaction time is 70 min and temperature is at 115℃,the yield could reach 77.3%.The catalyst recycling result has shown that a deactivation occurs,which due to the redissolution of the polyanion in the reaction medium.

Key concepts: Catalysis, Palygorskite, Cyclohexane, Yield (engineering), Chemistry, Acetic acid, Fourier transform infrared spectroscopy, Adsorption

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