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A method of preparing levulinates by utilizing furfuryl alcohol

A technology of levulinate and furfuryl alcohol, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of toxic organic solvents, easy to corrode, and difficult to recycle, and achieve good selectivity. Effects of less pollution and less reaction by-products

Active Publication Date: 2016-06-08
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there have been some studies at home and abroad on the use of biomass derivative furfuryl alcohol to prepare chemical product levulinate. Generally speaking, various methods have certain defects, such as some using toxic organic solvents, and some using corrosive and difficult-to-recycle inorganic materials. Acid catalysts, some use acidic resin catalysts with poor thermal stability, etc.

Method used

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  • A method of preparing levulinates by utilizing furfuryl alcohol
  • A method of preparing levulinates by utilizing furfuryl alcohol
  • A method of preparing levulinates by utilizing furfuryl alcohol

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Embodiment 1

[0023] This embodiment relates to a metal oxide (α-Fe 2 o 3 ) convert furfuryl alcohol to prepare the method for ethyl levulinate, and the reaction equation is as follows:

[0024]

[0025] The method comprises the steps of:

[0026] 0.23mmol furfuryl alcohol, 7.5mmol α-Fe 2 o 3 Mix powder and 10mL absolute ethanol evenly in a Teflon-lined high-pressure reactor. Fill the reactor with nitrogen to remove the air and seal the reactor to start the reaction. When the reaction temperature reaches 250°C, start timing and keep at 250°C for 60 minutes. , after the reaction is finished, cool at normal temperature, after the temperature of the reactor drops to normal temperature, the reaction mixture is filtered and the filtrate is collected, and ethyl levulinate is obtained through separation and purification, and GC-MS analysis shows that figure 1 As shown, the calculated ethyl levulinate yield reached 83%.

Embodiment 2

[0028] This embodiment relates to a metal oxide (α-Fe 2 o 3 ) convert furfuryl alcohol to prepare the method for methyl levulinate, comprising the steps:

[0029] 0.23mmol furfuryl alcohol, 12.5mmol α-Fe 2 o 3 Mix the powder and 7.5mL of anhydrous methanol evenly in a Teflon-lined high-pressure reactor, fill the reactor with nitrogen and remove the air, seal the reactor and start the reaction. When the reaction temperature reaches 250°C, start timing and keep the reaction at 250°C After 40 minutes, after the reaction was completed, it was cooled to normal temperature, and after the temperature of the reactor was lowered to normal temperature, the reaction mixture was filtered and the filtrate was collected, and ethyl levulinate was obtained through separation and purification. The yield of ethyl levulinate reached 73% according to gas chromatography analysis. The reaction equation is as follows:

[0030]

Embodiment 3

[0032] This embodiment relates to a metal oxide (α-Fe 2 o 3 ) convert furfuryl alcohol to prepare the method for n-butyl levulinate, and the reaction equation is as follows:

[0033]

[0034] The method comprises the steps of:

[0035] 0.23mmol furfuryl alcohol, 5mmolα-Fe 2 o 3 Mix powder and 7.5mL n-butanol evenly in a Teflon-lined high-pressure reactor. Fill the reactor with nitrogen to remove the air and seal the reactor to start the reaction. When the reaction temperature reaches 250°C, start timing and keep the temperature at 250°C. After 80 minutes, after the reaction was completed, it was cooled to normal temperature, and after the temperature of the reactor was lowered to normal temperature, the reaction mixture was filtered and the filtrate was collected, and ethyl levulinate was obtained through separation and purification. The yield of ethyl levulinate reached 86% according to gas chromatography analysis.

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Abstract

A method of preparing levulinates by utilizing furfuryl alcohol is disclosed. The method adopts the furfuryl alcohol that is a biomass derivative as a raw material, adopts a metal oxide as a catalyst, and includes reacting in a sealed manner in a reactor at 100-300 DEG C for 10-80 min. The highest yields of methyl levulinate, ethyl levulinate or n-butyl levulinate in different solvent systems can be 73%, 83% and 86% respectively. The method can efficiently synthesize the levulinates with high selectivity. The biomass derivative that is rich in reserve in the nature, wide in distribution and reproducible is adopted as the raw material, thus avoiding consumption of a large amount of fossil fuels. The method is free of preparation of complex catalysts and simple in operation, alcohols are adopted as solvents, and reactants are low in environment pollution and high in conversion ratio, thus facilitating industrial production. The levulinates which are products can be widely used as green solvents, perfume, fuel additives, and the like, and can be adopted as intermediates for synthesizing other chemical products with high added value.

Description

technical field [0001] The invention belongs to the technical field of energy and chemical industry, and in particular relates to a method for preparing levulinate by using furfuryl alcohol, a biomass derivative. Background technique [0002] The excessive dependence and consumption of fossil energy such as coal, oil, and natural gas make human beings face serious energy and environmental crises. The development and utilization of renewable clean energy such as solar energy, wind energy, tidal energy, and biomass energy has attracted much attention. Biomass energy is currently the only clean and renewable organic carbon resource, and it has the advantages of low pollution, wide distribution, abundant sources, and large reserves. The effective use of biomass resources can alleviate human demand for fossil energy to a certain extent. At present, there have been some studies at home and abroad on the use of biomass derivatives furfuryl alcohol to prepare chemical products lev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/00
Inventor 霍志保任德章罗将傅骏金放鸣
Owner SHANGHAI JIAO TONG UNIV
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