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A method for preparing 5-hydroxymethylfurfural

A technology of hydroxymethyl furfural and alkyl sulfonic acid, 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 properties, Low three-waste emissions and stable catalytic performance

Inactive Publication Date: 2017-10-10
QINGDAO UNIV OF SCI & TECH
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  • Summary
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  • Description
  • Claims
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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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  • A method for preparing 5-hydroxymethylfurfural
  • A method for preparing 5-hydroxymethylfurfural

Examples

Experimental program
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Effect test

Embodiment 1

[0018] 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

[0020] 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

[0022] 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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Abstract

A method for preparing 5-hydroxymethylfurfural, that is, adopting a double-acid catalyst to catalyze biomass sugar to prepare 5-hydroxymethylfurfural, is characterized in that the acidic quaternary ammonium salt cation and Lewis A bis-acid compound composed of acidic inorganic anions is used as a catalyst, and the purpose of increasing the yield of HMF is achieved by utilizing the adjustable acid strength and synergistic catalytic effect between the two. The reaction conditions are: the volume ratio of water to organic solvent is 1:5 to 1:20, the mass ratio of catalyst to biomass sugar (fructose, glucose, sucrose) is 1:2 to 1:10, and the reaction temperature is 160°C to 220°C. Under the condition of reaction time 5min-60min, HMF was prepared. Compared with the prior art: 1. The catalyst has unique catalytic characteristics, and the catalytic performance is stable, easy to separate, and reusable. 2. The process is simple and the discharge of three wastes is small. 3. The raw material biomass sugar has a wide range of choices, and cheap sucrose and other biomass sugars can be used as reactants 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 Patents(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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