Method for preparing 5-hydroxymethyl furfural

An ionic liquid, biomass sugar technology, applied in the field of product 5-hydroxymethyl furfural, can solve the problems of large mass transfer and diffusion resistance, high preparation cost, low product yield, etc., and achieve unique catalytic characteristics, three waste emissions The effect of less and stable catalytic performance

Inactive Publication Date: 2013-07-17
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Traditional acid catalysis has problems such as many side reactions, low product yield, complex product separation operation, corrosion equipment and large environmental pollution; the preparation cost of heterogeneous catalysts such as solid superacids is high, easy to be poisoned and deactivated by coking; ions Exchange resin catalysts have problems such as easy loss during separation, poor preparation reproducibility, and high mass transfer and diffusion resistance, which limit their application in the preparation of HMF.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: 2g sucrose, 20mL dimethyl sulfoxide, 2mL water and 0.4g ionic liquid 1-(3-sulfonic acid)-propyl-3-methylimidazolium chlorochromate (acidified inner salt and chlorinated Chromium molar ratio 1:2), was added into the autoclave, heated and stirred, and reacted at 180°C for 30min. The mass fraction of 5-hydroxymethylfurfural in the obtained product was measured by an ultraviolet spectrophotometer, and the yield of HMF was calculated to be 84.7%.

Embodiment 2

[0018] Embodiment 2: 2g glucose, 15mL n-butanol, 1mL water and 0.7g ionic liquid 1-(3-sulfonic acid)-butyl-3-ethylimidazolium ferric chloride (acidified internal salt and ferric chloride mole Ratio 1:2), added into the autoclave, heated and stirred, and reacted at 200°C for 15min. The mass fraction of 5-hydroxymethylfurfural in the obtained product was measured by a spectrophotometer, and the yield of HMF was calculated to be 48.5%.

Embodiment 3

[0020] Embodiment 3: 2g sucrose, 10mL dimethyl sulfoxide, 2mL water and 0.2g ionic liquid 1-(3-sulfonic acid)-propyl-3-propylimidazole chloride zincate (acidified inner salt and chloride Zinc molar ratio 1:2), added into the autoclave, heated and stirred, and reacted at 160°C for 60min. The mass fraction of 5-hydroxymethylfurfural in the obtained product was measured by an ultraviolet spectrophotometer, and the yield of HMF was calculated to be 65.3%.

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PUM

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Abstract

The invention discloses a method for preparing 5-hydroxymethyl furfural, namely a method for preparing 5-hydroxymethyl furfural by catalyzing biomass sugar with a double-acid catalyst. The method is characterized in that double-acid compound consisting of acid quaternary ammonium salt cations functionalized by alkyl sulfonic acid and Lewis acid inorganic anions is used as a catalyst, and the target of improving the yield of hydroxymethyl furfural (HMF) is reached on the basis of the adjustable features of acid intensity and the concerted catalysis effect of the acid quaternary ammonium salt cations functionalized by alkyl sulfonic acid and the Lewis acid inorganic anions, wherein the reaction conditions are that the volume ratio of water to an organic solvent is (1:5) to (1:20); the mass ratio of the catalyst to the biomass sugar (fructose, glucose and cane sugar) is (1:2) to (1:10); the reaction temperature is 160-220 DEG C; and the reaction time is 5-60 minutes, and preparing the HMF. Compared with the prior art, the method has the advantages that the catalyst has unique catalytic characteristic, is stable in catalytic performance, and easy to separate, and can be repeatedly used; the process is simple, and emission of the 'three wastes' is low; and the selection range of biomass sugars serving as raw materials is wide and the biomass sugar such as cheap cane sugar can be used as a reactant to produce high value-added products.

Description

technical field [0001] The present invention involves the use of Biacid-type ionic liquids catalyze the dehydration of biomass sugar to prepare 5-hydroxymethylfurfural, which involves the use of A new method for efficiently converting biomass sugars such as fructose, glucose, and sucrose into 5-hydroxymethylfurfural catalyzed by bis-acid ionic liquids. Background technique [0002] 5-Hydroxymethylfurfural (HMF) is an important new platform compound, which can prepare hundreds of chemicals through reactions such as hydrogenation, dehydrogenation, esterification, halogenation, polymerization and hydrolysis, and is widely used in medicine , Resin plastics, diesel fuel additives, etc. Biomass such as starch and cellulose can be hydrolyzed to produce biomass sugars such as glucose and fructose, and then dehydrated to prepare HMF. Commonly used catalysts for the preparation of HMF include acids, solid acids, ion exchange resins, and the like. Traditional acid catalysis has p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
Inventor 刘仕伟李露于世涛解从霞刘福胜孔珊珊
Owner QINGDAO UNIV OF SCI & TECH
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