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Method for preparing ethyl levulinate by catalyzing biomass sugar to be directly alcoholyzed

A technology of levulinate and biomass sugar is applied in the field of catalyzing the direct alcoholysis of biomass sugar to prepare levulinate, which can solve the problems of reactor corrosion, low yield of levulinate, poor catalytic performance, etc. Mild reaction conditions and strong substrate versatility

Inactive Publication Date: 2014-04-16
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Liquid acid catalysts have high efficiency, but are severely corrosive to the reactor; solid acids have little environmental pollution and are easy to recycle and reuse, but their catalytic efficiency is relatively low, especially for high polysaccharides such as cellulose, because they are insoluble in the reaction solvent, lower catalytic efficiency
In addition, the existing acid catalysts are not universally applicable to the reaction substrate sugars, and usually only show good catalytic performance for one type of sugars, while the catalytic performance for other sugars is poor.
For example, the commonly used sulfuric acid catalyst can obtain a higher yield of levulinate for the alcoholysis of ketose (fructose, inulin, etc.), but for the conversion of aldose (glucose, starch, cellulose, etc.), the target The yield of the product levulinate is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 12 grams of methanol, 1.72 mmol of glucose, 0.34 mmol of Al 2 (SO 4 ) 3 18H 2 O was added into the autoclave, the temperature was raised to 160°C, and the reaction was carried out for 2.5 h. The sugar conversion rate was determined by liquid chromatography analysis, and the glucose conversion rate was 100%. The reaction product was analyzed by gas chromatography-mass spectrometry and compared with methyl levulinate standards to confirm that the main product was methyl levulinate, and quantitatively analyzed by gas chromatography with naphthalene as an internal standard to obtain methyl levulinate The molar yield was 67%.

Embodiment 2

[0023] 12 grams of methanol, 1.72 mmol of glucose, 0.34 mmol of Al 2 (SO 4 ) 3 18H 2 O was added into the autoclave, and the atmosphere in the autoclave was replaced with nitrogen four times, then filled with 0.1 MPa nitrogen, heated to 160 °C, and reacted for 2.5 h. The sugar conversion rate was determined by liquid chromatography analysis, and the reaction product was analyzed by gas chromatography with naphthalene as an internal standard, and the glucose conversion rate was 100%, and the molar yield of methyl levulinate was 64%.

Embodiment 3

[0025] Except that the reaction temperature was 120°C, other conditions were the same as in Example 2, and the conversion rate of glucose was 70%, and the molar yield of methyl levulinate was 10%.

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Abstract

The invention belongs to the technical field of compound synthesis, and particularly relates to a method for preparing ethyl levulinate by catalyzing biomass sugar to be directly alcoholyzed. According to the method disclosed by the invention, Al3<+> salt is used as a catalyst. The method for preparing the ethyl levulinate by catalyzing biomass sugar to be directly alcoholyzed is not only moderate in reaction condition and strong in substrate universality, but also high in yield of the ethyl levulinate.

Description

[0001] technical field [0002] The invention belongs to the technical field of compound synthesis, in particular to a method for preparing levulinate by catalyzing direct alcoholysis of biomass sugar. Background technique [0003] Levulinate is an important platform compound in the process of biomass conversion, and has a wide range of applications in industries such as coatings, spices, seasonings, plasticizers, and pharmaceuticals. The short-chain fatty acid esters of levulinic acid, such as methyl levulinate and ethyl levulinate, have properties very similar to biodiesel, so they can be used as additives for gasoline, diesel and biofuels. In addition, levulinic acid ester molecules contain active ester groups and carbonyl groups, which can be used as reactants to participate in various addition and condensation reactions, and have broad application prospects. At present, levulinic acid esters are mainly produced by levulinic acid esterification in industry, but the raw ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/62
CPCC07C67/00C07C69/716
Inventor 杨晓梅王洋周利鹏
Owner ZHENGZHOU UNIV
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