Method for preparing 5-hydroxymethylfurfural with carbohydrate

A technology of carbohydrates and hydroxymethylfurfural, applied in the direction of organic chemistry, can solve the problems of limited scale application, unfavorable separation, high price of ionic liquid, etc., and achieve economical and environmental protection, good economy and environmental protection , good reproducibility effect

Active Publication Date: 2016-01-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the high boiling points of DMF, DMSO and GVL are not conducive to separation. The two-phase solvent system requires a large amount of extraction solvent and usually needs to add NaCl and other salts to improve the extraction effect, which increases the complexity and energy consumption of the reaction system.
In addition, the use of ionic liquids as reaction solvents can also achieve higher HMF yields. When glucose is used as a raw material, the yield of HMF can reach 70mol%. However, the disadvantages of expensive ionic liquids, high viscosity and difficult separation of products Its large-scale application (GreenChemistry, 2014, 16, 548-572.)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Mix 10mmol fructose, 50mL water-ethylene glycol dimethyl ether mixed solvent, water-ethylene glycol dimethyl ether volume ratio is 1:2, 0.5mmolH 3 PO 4 Add to the reaction kettle and mix evenly. The reaction conditions are as follows: a reaction temperature of 150° C., a reaction time of 45 minutes, and a stirring rate of 300 rpm. After the reaction was finished, it was air-cooled to room temperature, and the HMF content was measured by high-performance liquid chromatography and the yield was calculated, and the yield of HMF was 45.1%.

Embodiment 2

[0035] Mix 10mmol fructose, 50mL water-ethylene glycol dimethyl ether mixed solvent, water-ethylene glycol dimethyl ether volume ratio is 1:4, 0.5mmolH 3 PO 4 Add to the reaction kettle and mix evenly. The reaction conditions are as follows: a reaction temperature of 150° C., a reaction time of 45 minutes, and a stirring rate of 300 rpm. After the reaction was finished, it was cooled to room temperature by air cooling, and the HMF content was measured by high-performance liquid chromatography and the yield was calculated, and the yield of HMF was 61.5%.

Embodiment 3

[0037] Mix 10mmol fructose, 50mL water-ethylene glycol dimethyl ether mixed solvent, water-ethylene glycol dimethyl ether volume ratio is 1:7, 0.5mmolH 3 PO 4 Add to the reaction kettle and mix evenly. The reaction conditions are as follows: a reaction temperature of 150° C., a reaction time of 45 minutes, and a stirring rate of 300 rpm. After the reaction was finished, it was air-cooled to room temperature, and the HMF content was measured by high-performance liquid chromatography and the yield was calculated, and the yield of HMF was 68.4%.

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PUM

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural with carbohydrate. The method comprises the steps of mixing the carbohydrate A, a mixed solvent B, a Lewis acid catalyst C and a Bronsted acid catalyst D, heating a mixture at 120-200 DEG C, and controlling reaction time to be 15-180min to synthesize 5-hydroxymethylfurfural, wherein the carbohydrate A is monosaccharide, disaccharide or polysaccharide; Lewis acid catalyst C is a metal halide; the Bronsted acid catalyst D is inorganic acid; and the mixed solvent B is a mixed solvent of water and ethers. A reaction system is simple in composition, economical and environment-friendly; operating conditions are mild; the technical complexity of preparing 5-hydroxymethylfurfural with the carbohydrate taking glucose as a source is effectively simplified; and the productivity of 5-hydroxymethylfurfural is greatly improved at the same time.

Description

technical field [0001] The invention relates to a method for preparing 5-hydroxymethylfurfural, especially a method for preparing 5-hydroxymethylfurfural from carbohydrates. Background technique [0002] As the only renewable carbon-based resource, biomass can be used to produce a variety of fine chemicals and fuels, thereby reducing dependence on petroleum and coal resources, which is of great significance to China's energy security and environmental protection. 5-hydroxymethylfurfural (5-hydroxymethylfurfural, HMF) is a platform compound that can be produced from biomass carbohydrates. A series of chemicals and new liquid fuels can be further synthesized through HMF. Therefore, HMF will be an important bridge connecting biomass resources and fuel chemicals. [0003] At present, many HMF preparation technologies are based on the use of fructose or polyfructose as raw materials, because the unique furan ring configuration of fructose makes it easy to convert into HMF. Howe...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 王树荣林海周周劲松骆仲泱倪明江岑可法
Owner ZHEJIANG UNIV
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