Method for preparing 5-hydroxymethyl furfural

A hydroxymethyl furfural and reaction technology, applied in the field of direct preparation of 5-hydroxymethyl furfural, can solve the problem that it is difficult to realize the direct conversion of cellulose to prepare 5-hydroxymethyl furfural, unfavorable cellulose full contact, heterogeneous catalyst surface area Low problems, to achieve the effect of large-scale green industrial production, increased stability, and reduced viscosity

Active Publication Date: 2013-01-02
TIANJIN POLYTECHNIC UNIV
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AI Technical Summary

Problems solved by technology

Although 5-hydroxymethylfurfural can be directly synthesized from cellulose, it is still mainly prepared by dehydration of fructose at present, because there are many technical difficulties in the method of directly synthesizing 5-hydroxymethylfurfural
Studies have shown that in industrial production and experimental research, some commonly used heterogeneous catalysts such as sulfonic acid resins, SO 4 /ZrO 2 , sulfonic acid hybrid SBA-15, ion exchange resin, HTiNbO 5 、HTi 2 NbO 7 , HNb 3 o 8 、H 4 Nb 6 o 17 、H 2 Ti 3 o 7 , Mordenite, TiO 2 and ZrO 2 , Nb 2 o 5 /Al 2 o 3 etc., are beneficial to the pr

Method used

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preparation example Construction

[0012] The preparation method of 5-hydroxymethylfurfural (method for short) designed by the present invention is a technical scheme designed to improve the conversion rate of cellulose, starch, sucrose, glucose and fructose, etc. and the yield of 5-hydroxymethylfurfural . Its main feature is the use of sulfonated polyphenylene sulfide, sulfonic acid and sulfide synergistically hybridized organic materials or inorganic materials, sulfonic acid and metal ions synergistically hybridized organic-inorganic materials as catalysts, and achieved by adjusting the molar ratio of sulfonic acid and thioether Effective conversion of sugars, the process is that sulfonic acid and thioether synergistically promote the hydrolysis of polysaccharides into glucose, and then isomerize into fructose, and then dehydrate to prepare 5-hydroxymethylfurfural.

[0013] Specifically, the method of the present invention uses biomass sugar as raw material, and adopts the following biomass conversion reactio...

Embodiment 1

[0027] Take 20 grams of cellulose, 100ml of 1-ethyl-3-methylimidazole bromide, 2g of sulfonated polyphenylene sulfide, and 8% sulfonation degree of sulfonated polyphenylene sulfide, and put them into a 250ml round bottom flask ; replace the air in the reactor with nitrogen; under magnetic stirring, heat an oil bath at 180°C for 3 hours under normal pressure; after the reaction is completed and cooled, use ethyl acetate to extract and separate the target product; The same below), the molar yield of 5-hydroxymethylfurfural is 47.4%.

Embodiment 2

[0029] Take 20 grams of cellulose, 100 ml of 1-ethyl-3-methylimidazole bromide, 2 g of sulfonated polyphenylene sulfide, and the degree of sulfonation of sulfonated polyphenylene sulfide is 26.2%, and put them into a 250 ml round bottom flask; Replace the air in the reactor with nitrogen; under magnetic stirring, heat an oil bath at 180°C for 3 hours under normal pressure; after the reaction is completed and cooled, use ethyl acetate to extract and separate the target product; the molar yield of 5-hydroxymethylfurfural is 74.4%.

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Abstract

The invention discloses a method for preparing 5-hydroxymethyl furfural. In the method, biomass sugar is taken as a raw material and a biomass transformation technology is adopted. The method comprises the steps of: putting 50-150ml of ionic liquid, 6-40g of biomass sugar and 0.5-6g of catalyst with the sulfonation degree of 8-100% into a 250mol of round-bottom flask together; replacing the air with nitrogen; heating up to 140-180 DEG C by oil bath under the stirring of magnetic force, reacting for 0.5-8 hours and then cooling; and then, extracting with ethyl acetate and separating out the 5-hydroxymethyl furfural, wherein the ionic liquid is N-methyl imidazole ionic liquid, pyridine ionic liquid, amino acid ionic liquid or morpholine ionic liquid, the biomass sugar is cellulose, starch, inulin, cane sugar, glucose or fructose, and the catalyst is collaborative hybrid organic material formed by polyphenylene sulfide, sulfonic acid and sulfur ether, or collaborative hybrid organic inorganic material formed by inorganic material, sulfonic acid and metal ions.

Description

technical field [0001] The invention relates to biomass conversion technology and chemical production technology, in particular to a method for directly preparing 5-hydroxymethylfurfural by using renewable substances as raw materials. Background technique [0002] Cellulose is one of the renewable resources. The research on its hydrolysis to prepare HMF (5-hydroxymethylfurfural) is gradually attracting people's attention. 5-Hydroxymethylfurfural can synthesize high value-added products such as 2,5-furandicarbaldehyde, 2,5-furandicarboxylic acid, levulinic acid and alkanes through oxidation, hydrogenation and condensation reactions, so 5-Hydroxymethylfurfural It is considered to be a key intermediate for biomass to replace petroleum and coal in the production of organic chemicals. Although 5-hydroxymethylfurfural can be directly synthesized from cellulose, it is still mainly prepared by dehydration of fructose at present, because there are many technical difficulties in the...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCY02P20/54
Inventor 李振环程博闻苏坤梅丁敏张磊杨东江
Owner TIANJIN POLYTECHNIC UNIV
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