Method for producing 5-hydroxymethyl furfural by chitin biomass

A technology of hydroxymethylfurfural and chitin, applied in the direction of organic chemistry, etc., to achieve the effect of simple operation process, wide sources and abundant reserves

Active Publication Date: 2013-05-29
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
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AI Technical Summary

Problems solved by technology

However, the preparation of high value-added 5-hydroxymethylfurfural from chitin biomass, the most abundant marine biomass resource, has not been reported yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Prepare 60 g of zinc chloride aqueous solution with a mass concentration of 30%, add 5 g of chitin with a molecular weight of 400,000, and add 0.5 g of CrCl 3 ·6H 2 O mix and react at 120 °C for 8 hours.

[0020] (2) After the reaction, 75 mL of methyl isobutyl ketone was added as an extractant to extract 5-hydroxymethyl furfural.

[0021] (3) The obtained methyl isobutyl ketone phase in which the product 5-hydroxymethyl furfural is dissolved is concentrated and evaporated to dryness, and the solid obtained after concentration is crystallized in petroleum ether to obtain the 5-hydroxymethyl furfural product, 5-hydroxymethyl furfural. The molar yield of furfural was 30%.

Embodiment 2

[0023] (1) Prepare 85 g of zinc chloride aqueous solution with a mass concentration of 67%, add 10 g of chitosan with a molecular weight of 0.1 million and a degree of deacetylation of 100%, and add 10 g of B(OH) 3 , and reacted at 100 °C for 5 hours.

[0024] (2) After the reaction, 120 mL of butanol was added as an extractant to extract 5-hydroxymethylfurfural.

[0025] (3) The obtained butanol phase in which the product 5-Hydroxymethylfurfural is dissolved is concentrated and evaporated to dryness. After the concentration, the obtained solid is crystallized with benzene to obtain the 5-Hydroxymethylfurfural product, the molar yield of the 5-Hydroxymethylfurfural product. 43%.

Embodiment 3

[0027] (1) Prepare 30 g of zinc chloride aqueous solution with a mass concentration of 60%, add 10 g of chitosan with a molecular weight of 120,000 and a degree of deacetylation of 64%, and add 0.2 g of SnCl 4 ·5H 2 O was used as a catalyst, and the reaction was continued for 10 hours at 135 °C.

[0028] (2) After the reaction, 100 mL of 2,5-dimethylpentanone was added as an extractant to extract the product 5-hydroxymethylfurfural.

[0029] (3) The obtained 2,5-dimethylpentanone phase is concentrated and evaporated to dryness, and crystallized with a mixed solvent of 1,4-dioxane-petroleum ether to obtain 5-hydroxymethylfurfural product, 5-hydroxymethylfurfural The molar yield of furfural product was 35%.

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Abstract

The invention discloses a method for producing 5-hydroxymethyl furfural by chitin biomass. The method comprises the steps of preparing a zinc chloride water solution of which mass concentration is 30-72%; evenly mixing the dried chitin biomass material, the zinc chloride water solution and a catalyst; reacting for 10 minutes to 10 hours after the reaction is finished at 60-140 DEG C, wherein the mass ratio of the chitin biomass material to the zinc chloride water solution is 1: (3-180); the mass ratio of the added catalyst to the chitin biomass material is 1: (1-50); extracting the 5-hydroxymethyl furfural from a reaction system by an organic extracting agent after the reaction is finished; then concentrating and drying the extracting agent, and crystallizing to obtain the 5-hydroxymethyl furfural product. The method has the advantages of being wide in source of the chitin biomass, abundant in storage, simple in operation process and high in obtained product purity.

Description

technical field [0001] The invention relates to a method for preparing 5-hydroxymethylfurfural by using chitin biomass as raw material. technical background [0002] In a modern society with increasingly scarce energy and increasingly serious environmental pollution, the demand for renewable energy and chemicals is increasing. At present, the research on replacing petrochemical resources with renewable biomass resources mainly focuses on two directions, one is to directly convert biomass resources into energy substances, and the other is to convert biomass resources into alcohols, aldehydes, ketones, acids, esters, etc. High value-added fine chemical intermediates, and then prepare other commonly used chemicals. The direct conversion of biomass resources into energy materials faces challenges from cleaner energy sources such as hydrogen energy, solar energy, and wind energy. However, these several approaches that can provide clean energy cannot prepare platform compounds an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
Inventor 侯相林王英雄贾时宇邓天昇王玉琪乔岩
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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