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A kind of method utilizing furfuryl alcohol to prepare levulinate

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 easy corrosion, difficult recovery, and toxic organic solvents, so as to reduce pollution and react Fewer by-products and good selectivity

Active Publication Date: 2018-02-09
SHANGHAI JIAOTONG 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 kind of method utilizing furfuryl alcohol to prepare levulinate
  • A kind of method utilizing furfuryl alcohol to prepare levulinate
  • A kind of method utilizing furfuryl alcohol to prepare levulinate

Examples

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Effect test

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

The invention discloses a method for preparing levulinate by utilizing furfuryl alcohol; the method uses furfuryl alcohol, a biomass derivative, as a raw material, and uses a metal oxide as a catalyst, and reacts in a sealed reactor at 100-300°C for 10-80 minutes. In different solvent systems, the yields of methyl levulinate, ethyl levulinate or n-butyl levulinate can be as high as 73%, 83% and 86%, respectively. The invention can efficiently and selectively synthesize levulinic acid ester, uses abundant reserves, widely distributed and renewable biomass derivatives in nature as raw materials, avoids the consumption of a large amount of fossil energy, does not need to prepare complex catalysts, is simple to operate, and uses Alcohol as a solvent and reactant has little environmental pollution and high conversion rate, which is beneficial to industrial production. The product levulinic acid ester can be widely used as green solvents, spices, fuel additives, etc., and can also be used to synthesize other high value-added chemical products chemical intermediates.

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 Patents(China)
IPC IPC(8): C07C69/716C07C67/00
Inventor 霍志保任德章罗将傅骏金放鸣
Owner SHANGHAI JIAOTONG UNIV
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