Synthesis of n-Butyl Acetate Catalyzed by Heteropolyacids H_3PW_6Mo_6O_(40) under Ultrasound Irradiation
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The synthesis of n-butyl acetate catalyzed by heteropolyacids H3PW6Mo6O40 under ultrasound irradiation was investigated.The catalyst was prepared and characterized by IR and XRD.The results indicate that the catalyst retains the Keggin-type structure.Then the effects of calcination temperature of catalyst,amounts of catalyst,the type and amount of water-carrying agent,molar ratio of n-butanol and acetic acid,and the reaction time on the yield of esterification were discussed systematically.The optimum conditions are as follows:when the conditions of ultrasound are 20 kHz and 0.1 W/cm2,the calcination temperature of catalyst is 400 ℃;the amounts of catalyst is 0.6 g;reaction temperature 120 ℃;n(n-butanol)∶n(acetic acid)=1.5∶1(acetic acid is 0.4 mol);reaction time 60 min.Under these conditions,the yield of esterification is 99.3%.Keywords:
Molar ratio
Butyl acetate
n-Butanol
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SO~(2-)_4/ZrO_2 solid acid catalyst was prepared from hydrothermally modified zirconium hydroxide.The liquid phase esterification of acetic acid and 1-butanol was preformed to confirm the optimal conditions of preparation.Compared experiments were made with SO~(2-)_4/ZrO_2 solid acid catalyst prepared by normal method.The catalysts were characterized with XRD and BET.The results show that the optimum preparation conditions for solid acid catalyst through hydrothermal modification are concentration of sulphuric acid 0.5 mol/L,impregnation time 120 min and calcining temperature 500 ℃.Butyl acetate are prepared by reaction at 105～110 ℃ for 2 h with n(1-butanol)∶n(acetic acid)=2∶1 and w(catalyst)=0∶27% based on the total mass of initial materials.Conversion of acetic acid amounts to 99.1%.At the optimum conditions,after the catalyst was used repeatedly four times,the catalytic activity decreased by 5%.
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Solid super strong acid SO 2- 4/TiO 2was applied as a new catalyst to the esterification of acetic acid and sec-butyl alcohol. It has high activity and e xcellent selectivity as well as no corrosion to the facilities. Various reaction parameters such as ratio of alcohol to acid, catalyst amount, reaction time and reaction temperature were carefully studied. The optimum reaction conditions we re: molar ratio of sec-butyl alcohol to acetic acid was 1.4∶1, amount of cataly st was 1.2 g, reaction time was 4 h, reaction temperature was 150 ℃. The conver sion of acetic acid reached 87.71 % and the selectivity of esterification was 100 % under the optimum conditions.
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The synthesis of n-butyl acetate with acetic acid and n-butanol as reactants and solid super acid SO 4 2- /ZrO 2-CeO 2 as catalyst was studied.The influence factors were investigated by experiments arranged by orthogonal design.The results showed that the optimum conditions were as follows: the molar ratio of n-butanol to acetic acid was 2∶1, the amount of catalyst was 1.5% of the mass of mixture charge in the reaction , and the reaction time was 3h . The esterification yield of n-butyl acetate was about 92.6%.
Superacid
Molar ratio
Butyl acetate
n-Butanol
Solid acid
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N-Butyl acetate, a useful organic chemicals, has been synthesized by using n-buthanol and acetic acid as starting materials in the presence of heteropolyacid (HPA) catalyst. The optimizing test of the operation conditions was also established. The optimum reaction conditions, under which the yield of n-butyl acetate is about 88.5%～89%, are as follws: molar ratio: alcohol: acid =1.1∶1, weight of HPA catalyst: 1g/1 mole n-butanol, reaction time: 90 min, cyclohexane as water-taken agent.
Butyl acetate
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Thermogravimetry
Differential thermal analysis
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A novel heterogeneous esterification catalyst,gallium oxide supported on silica gel was prepared for the first time,which was obtained through loading concentration of Ga2O3 20%,calcinating at 500 ℃ for 2 h.The effects of various parameters such as catalyst dosage,molar ratio of n-butanol to acetic acid,amount of cyclohexane,reaction time and reusability of catalyst on esterification rate were investigated.The results indicated that the optimized conditions of synthesizing butyl acetate were:acetic acid 0.2 mol,molar ratio of n-butanol to acetic acid 1.8,dosage of catalyst 1.25 g,reaction time 1 h.The catalytic performance could exhibit high activity with the esterification rate over 99.62%.
Butyl acetate
Molar ratio
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n-Propyl acetate was prepared by esterification of acetic acid with n-propanol catalyzed by solid supported acid Al2O3/SO42-.The effects of the sulfuric acid concentration for catalyst preparation,,feed ratio of 1-propanol to acetic acid,catalyst amount and reaction time on the esterification were investigated.The results showed that the optimum conditions were the sulfuric acid concentration for catalyst preparation 2 mol·L-1,the feed molar ratio of n-propanol to acetic acid 1.3,catalyst loading 1.5 g(relative to 0.2625mol acetic acid) and reaction time 2.0 hours.Under these conditions,the esterification rate was 67%.
Solid acid
Molar ratio
Propanol
Butyl acetate
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SO2-4/ZrO2 solid acid catalyst was prepared by hydrothermal method,the catalyst was phase esterification of acetic acid with n-butanol preformed to confirm the optimal conditions of preparation SO2-4/ZrO2 solid acid catalyst through hydrothermal modification made experiments in comparison with normal preparation method.At the same time,the influence of different factors on conversion of acetic acid was studied,The test results show in esterification reaction of SO2-4/ZrO2 catalyst through hydrothermal modification;the technological conditions of n-butyl acetate are that the reaction time is 2h,n(n-butanol):n(acetic acid)=2:1,and w(catalyst) is 0.2% based on the total mass of initial materials.Conversion of acetic acid amounts to 99.1%.The catalysts were characterized with XRD and IR.
Butyl acetate
Solid acid
Hydrothermal Synthesis
n-Butanol
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n-Butyl acetate was synthesized by acetic acid and n-butyl alcohol in orthogonal experimental design using the Keggin-type P-V-Mo-W heteropolyacids H4PVMoxW11- xO40·nH2O(x = 1,2,3,4) as catalysts.The optimum conditions are:the mole ratio of n-butyl alcohol to acetic acid is 1.2∶ 1;the mass ratio of catalyst to acetic acid is 0.5%,reflux time is 40 minutes and the esterification rate reaches up to 88.52%.As the number of wolfram atom in this Keggin-type P-V-Mo-W heteropolyacids increased,the esterification rate was improved.
Butyl acetate
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MoO3/SiO2 catalyst was prepared by equivalent-volumetic impregnation method,and was used as catalyst to synthesize n-butyl acetate from acetic acid and butanol.The results showed that the optional reaction conditions were as follows:molar ratio of butanol and acetic acid 4:1,reaction time 3h,catalyst amount 1.0g.The conversion rate of acetic acid could reach 95%,the selectivity of n-butyl acetate was 100%,The catalyst can be reused directly for 5 times.
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Butyl acetate
n-Butanol
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