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Preparation method of acetylpropionic acid

A technology of levulinic acid and propyl group, which is applied in the field of B-L bis-acid catalyst to catalyze the conversion of cellulose to prepare levulinic acid, which can solve the problems of low substrate conversion rate, low yield of product levulinic acid, and low catalytic activity of the catalyst. Achieve high substrate conversion rate, high product selectivity and high catalytic activity

Active Publication Date: 2018-08-07
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of B-L bis-acid catalyst catalyzes the method that cellulose transforms and prepares levulinic acid, to solve the problem that cellulose transforms and prepares levulinic acid with low catalytic activity of the catalyst, low substrate conversion rate, and product levulinic acid yield. low level problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Put 1 g of cellulose, 0.03 g of catalyst 1-(3-sulfonic acid) propyl-3-methylimidazolium chloride zincate, and 50 g of water into an autoclave with stirring, heat and stir at 140 Reaction at ℃ for 8h. After the reaction, the reaction kettle was quickly lowered to room temperature in an ice-water bath, the reaction solution was filtered, the filter cake was washed three times with 10 mL of water, dried to constant weight, weighed, and the cellulose conversion rate was calculated to be 100%; mother liquor, washing After the liquids were combined, they were extracted 4 times with an equal volume of methyl isobutyl ketone, the extracts were combined, and the extracts were removed to obtain the product levulinic acid. The product yield was calculated to be 67.5% after the liquid chromatography test. The raffinate is distilled to recover the catalyst and reuse it.

Embodiment 2

[0017] Example 2: Put 1 g of cellulose, 0.1 g of catalyst 1-(3-sulfonic acid) propyl-3-methylimidazolium chloroferrate, and 200 g of water into an autoclave with stirring, heat and stir at 80 Reaction at ℃ for 20h. After the reaction, the reaction kettle was quickly lowered to room temperature in an ice-water bath, the reaction solution was filtered, the filter cake was washed three times with 10 mL of water, dried to constant weight, weighed, and the cellulose conversion rate was calculated to be 100%; mother liquor, washing After the liquids were combined, they were extracted 4 times with an equal volume of methyl isobutyl ketone, the extracts were combined, and the extracts were removed to obtain the product levulinic acid. The product yield was calculated to be 67.5% after the liquid chromatography test. The raffinate is distilled to recover the catalyst and reuse it.

Embodiment 3

[0018] Example 3: Put 1 g of cellulose, 0.001 g of catalyst 1-(3-sulfonic acid) propyl-3-methylimidazolium chlorocuprate, and 1 g of water into an autoclave with stirring, heat and stir at 130 Reaction at ℃ for 1h. After the reaction, the reaction kettle was quickly lowered to room temperature in an ice-water bath, the reaction solution was filtered, the filter cake was washed three times with 10 mL of water, dried to constant weight, weighed, and the cellulose conversion rate was calculated to be 75%; mother liquor, washing After the liquids were combined, they were extracted 4 times with an equal volume of methyl isobutyl ketone, the extracts were combined, and the extracts were removed to obtain the product levulinic acid. The product yield was calculated to be 35.9% after the liquid chromatography test. The raffinate is distilled to recover the catalyst and reuse it.

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PUM

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Abstract

The invention discloses a preparation method of acetylpropionic acid. The preparation method is characterized by including: adopting B-L acidic catalyst for reaction for 1.0-20.0h to prepare acetylpropionic acid under the conditions that a mass ratio of cellulose to the catalyst is 1000:1-10:1, a mass ratio of cellulose to water is 1:200-1:1 and reaction temperature is 80-230 DEG C; recycling thecatalyst. Compared with the prior art, the preparation method has the advantages that two acidic sites of the catalyst have synergistic catalysis effect, and the catalyst is high in catalytic activity, substrate conversion rate and product selectivity; the catalyst has good reuse performance.

Description

technical field [0001] The invention relates to a method for preparing levulinic acid, in particular to a new method for preparing levulinic acid by catalyzing cellulose transformation with a B-L bis-acid catalyst. Background technique [0002] Levulinic acid is a new type of platform compound, which has a wide range of applications in medicine, pesticide, petrochemical and so on. At present, there are two main production methods of levulinic acid: biological fermentation and chemical catalysis. The biological fermentation method has problems such as strict requirements on the external environment, long reaction cycle and easy inactivation of biological fermentation enzymes, while the chemical catalytic method is easier to control and realize industrial production. At present, inorganic acids and solid acids are widely used to catalyze the conversion of cellulose to prepare levulinic acid. Inorganic acids (sulfuric acid, hydrochloric acid) have problems such as corrosion o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/00C07C59/185B01J31/02
CPCC07C51/00B01J31/0244B01J31/0271C07C59/185Y02P20/584
Inventor 刘仕伟于世涛吴琼于海龙李露刘福胜宋修艳宋湛谦
Owner QINGDAO UNIV OF SCI & TECH
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