Method for preparing and separating 5-hydroxymethylfurfural from glucose

A technology for hydroxymethyl furfural and glucose, applied in the field of glucose preparation and separation of 5-hydroxymethyl furfural, can solve the problems of low initial sugar concentration, uneconomical, large consumption of reaction solvent, etc. Equipment, good selective effect

Pending Publication Date: 2020-12-29
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] Aiming at the problems of large consumption of reaction solvent, low initial sugar concentration, uneconomical etc. in the prior art, the present invention provides an efficient method for preparing and separating 5-hydroxymethylfurfural from glucose

Method used

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  • Method for preparing and separating 5-hydroxymethylfurfural from glucose

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Experimental program
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Effect test

Embodiment 1

[0026] Weigh 3.0 g of glucose and 1.5 g of choline chloride and mix them in a 50 mL round bottom flask, heat at 20° C. until it completely melts to a colorless transparent liquid to obtain a glucose-choline chloride mixed solution. Then add 0.18g of ZnCl 2 and 30mL of methyl isobutyl ketone, stirred at 125°C, condensed and refluxed, and reacted for 1.5h. Then collect the upper layer in the round-bottomed flask, carry out vacuum distillation through a rotary evaporator, recover the evaporated organic solvent, and use it as a solvent for the next experiment, and dry and cool the remaining product to obtain the product 5-hydroxymethyl Base furfural quality is 2.22g, utilizes liquid nuclear magnetic resonance analysis to know that its purity is 92%.

Embodiment 2

[0028] Weigh 3.0 g of glucose and 1.5 g of choline chloride and mix them in a 50 mL round bottom flask, heat at 80° C. until it completely melts to a colorless transparent liquid to obtain a glucose-choline chloride mixed solution. Then add 0.18g of ZnCl 2 and 30mL of methyl isobutyl ketone, stirred at 125°C, condensed and refluxed, and reacted for 1.5h. Then collect the upper layer in the round-bottomed flask, carry out vacuum distillation through a rotary evaporator, recover the evaporated organic solvent, and use it as a solvent for the next experiment, and dry and cool the remaining product to obtain the product 5-hydroxymethyl Base furfural quality is 2.28g, utilizes liquid nuclear magnetic resonance analysis to know that its purity is 92%.

Embodiment 3

[0030] Weigh 0.5g of glucose and 3.0g of choline chloride and mix them in a 50mL round bottom flask, heat at 80°C until it completely melts to a colorless transparent liquid to obtain a glucose-choline chloride mixed solution. Then add 0.03g of ZnCl 2 and 1mL of methyl isobutyl ketone, stirred at 125°C, condensed and refluxed, and reacted for 1.5h. Then collect the upper layer in the round-bottomed flask, carry out vacuum distillation through a rotary evaporator, recover the evaporated organic solvent, and use it as a solvent for the next experiment, and dry and cool the remaining product to obtain the product 5-hydroxymethyl Base furfural quality is 0.31g, utilizes liquid nuclear magnetic resonance analysis to know that its purity is 89%.

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Abstract

The invention belongs to the field of biomass catalytic conversion, and particularly relates to an efficient method for preparing and separating 5-hydroxymethylfurfural from glucose. Aiming at the problems of large reaction solvent consumption, low initial sugar concentration, dieconomy and the like in the prior art, choline chloride and glucose are adopted to form a mixed liquid at a lower temperature to prepare the 5-hydroxymethylfurfural, and an inorganic salt Lewis acid is used as a catalyst, so that the method is environment-friendly, low in price, mild in reaction condition and suitablefor industrial production. Good selectivity is realized on the 5-hydroxymethylfurfural. Glucose can be continuously supplemented in the reaction process to serve as a reactant and also serve as a reaction solvent, and continuous production of 5-hydroxymethylfurfural is achieved.

Description

technical field [0001] The invention belongs to the field of catalytic conversion of biomass, in particular to a method for preparing and separating 5-hydroxymethylfurfural from glucose. Background technique [0002] "Green" has now become one of the most important factors to be considered in the preparation of various chemicals. Cellulose is the most widely distributed and abundant biomass on the earth. Its monomer glucose has been used to prepare various green products, among which 5-hydroxymethylfurfural (HMF) is an important platform chemical in the downstream products of glucose. Its molecule contains an aldehyde group and a hydroxymethyl group, its chemical properties are very active, and it is prone to various reactions such as hydrogenation, oxidation, esterification, polymerization, and hydrolysis, making its derivatives widely used in fine chemicals, medicine, and degradable plastics. and other fields have great application prospects. However, the synthesis of 5-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 邓天昇王驰洲侯相林
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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