Method for preparing and separating 5-hydroxymethylfurfural from fructose

A technology of hydroxymethylfurfural and fructose, which is applied in the field of biomass catalytic conversion, can solve the problems of large consumption of reaction solvent, low initial sugar concentration, and uneconomical problems, and achieve the goal of reducing the amount, improving economy, and increasing yield Effect

Pending Publication Date: 2021-01-29
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 invention provides a method for preparing and separating 5-hydroxymethylfurfural from fructose

Method used

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  • Method for preparing and separating 5-hydroxymethylfurfural from fructose

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Experimental program
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Effect test

Embodiment 1

[0026] Weigh 3.0 g of fructose 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 fructose-choline chloride mixed solution. Then add 0.15 g of phosphotungstic acid and 30 mL of methyl isobutyl ketone, stir at 120° C., condense and reflux, and react for 1 h. 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 2.56g, utilizes liquid nuclear magnetic resonance analysis to know that its purity is 92%.

Embodiment 2

[0028] Weigh 3.0 g of fructose and 1.5 g of choline chloride and mix them in a 50 mL round bottom flask, heat at 30° C. until it completely melts to a colorless transparent liquid to obtain a fructose-choline chloride mixed solution. Then add 0.15g of phosphotungstic acid and 30mL of methyl isobutyl ketone, stir at 120°C, condense and reflux, and react 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 2.60g, utilizes liquid nuclear magnetic resonance analysis to know that its purity is 93%.

Embodiment 3

[0030] Weigh 0.5g of fructose 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 fructose-choline chloride mixed solution. Then add 0.025g of phosphotungstic acid and 2.5mL of methyl isobutyl ketone, stir at 80°C, condense and reflux, and react 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 0.33g, utilizes liquid nuclear magnetic resonance analysis to know that its purity is 88%.

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Abstract

The invention belongs to the field of biomass catalytic conversion, and particularly relates to a method for preparing and separating 5-hydroxymethylfurfural from fructose. The invention provides themethod for preparing and separating the 5-hydroxymethylfurfural from the fructose in order to solve the problems that in the prior art, the consumption of a reaction solvent is large, the initial sugar concentration is low, and the method is not economical. According to the method, choline chloride and the fructose form a mixed liquid at a relatively low temperature to prepare the 5-hydroxymethylfurfural, and an acid is used as a catalyst, so that the method is environment-friendly, low in price and mild in reaction condition, and has good selectivity on the 5-hydroxymethylfurfural. The fructose can be continuously supplemented in the reaction process to serve as both a reactant and a reaction solvent, so that continuous production of the 5-hydroxymethylfurfural is realized.

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 fructose. Background technique [0002] As the most common hexose, fructose and its isomer glucose have been used to prepare various green products, among which 5-hydroxymethylfurfural (HMF) is an important platform chemical in their downstream products. Containing 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 useful in the fields of fine chemicals, medicine, and degradable plastics. Great application prospect. Compared with glucose, fructose can be directly converted into 5-hydroxymethylfurfural, while glucose needs to be isomerized into fructose before conversion, so the conversion of fructose is more efficient. Howev...

Claims

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Application Information

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