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Method for preparing 5-hydroxymethylfurfural through conversion of cellulose in composite molten salt hydrate

A technology of hydroxymethyl furfural and composite molten salt, which is applied in the field of biomass resource utilization, can solve the problems of insoluble cellulose, low yield of 5-hydroxymethyl furfural and the like, achieves simple preparation, low price, and prevents side effects. The effect of product formation

Pending Publication Date: 2021-09-17
SHANDONG UNIV OF TECH
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Problems solved by technology

[0013] At present, the main obstacles to the direct conversion of cellulose into 5-hydroxymethylfurfural are: first, cellulose is difficult to dissolve
In addition, the conversion of cellulose to 5-hydroxymethylfurfural involves multi-step reactions, and each step needs to be regulated and catalyzed by different acids, which easily produces by-products such as humin and levulinic acid, resulting in a relatively low yield of 5-hydroxymethylfurfural. Low

Method used

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  • Method for preparing 5-hydroxymethylfurfural through conversion of cellulose in composite molten salt hydrate

Examples

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Effect test

example 1

[0029] (1) ZnCl 2 ·3H 2 O and FeCl 3 ·6H 2 O two kinds of molten salt hydrates are mixed according to a volume ratio of 3:1 to obtain a composite molten salt hydrate;

[0030] (2) Mix 5ml of composite molten salt hydrate with 0.2g of cellulose, then add 15ml of methyl isobutyl ketone to the composite molten salt hydrate to obtain a two-phase system mixture;

[0031] (3) Put the two-phase mixed solution obtained in step (2) into a hydrothermal kettle, and when the temperature in the oil bath reaches 110° C., put it into the hydrothermal kettle and start stirring, carry out a catalytic reaction for 120 minutes, and after the reaction finishes, take The organic phase is separated and purified to obtain 5-hydroxymethylfurfural.

[0032] According to high performance liquid chromatography analysis, 5-hydroxymethylfurfural was obtained in a yield of 47.6%.

example 2

[0034] (1) ZnCl 2 ·3H 2 O and CuCl 2 2H 2 O two kinds of molten salt hydrates are mixed according to a volume ratio of 2:1 to obtain a composite molten salt hydrate;

[0035] (2) Take 5ml of composite molten salt hydrate and mix it with 0.15g of cellulose, then add 5ml of petroleum ether to the composite molten salt hydrate to obtain a two-phase system mixed solution;

[0036] (3) Put the two-phase mixed solution obtained in step (2) into a hydrothermal kettle, and when the temperature in the oil bath reaches 120° C., put it into the hydrothermal kettle and start stirring, and carry out a catalytic reaction for 30 minutes. After the reaction, take The organic phase is separated and purified to obtain 5-hydroxymethylfurfural.

[0037] According to HPLC analysis, 5-hydroxymethylfurfural was obtained in a yield of 20.5%.

example 3

[0039] (1) FeCl 3 ·6H 2 O and CuCl 2 2H 2 O two kinds of molten salt hydrates are mixed according to a volume ratio of 1.5:1 to obtain a composite molten salt hydrate;

[0040] (2) Take 5ml of composite molten salt hydrate and mix it with 0.1g of cellulose, then add 10ml of hexane to the composite molten salt hydrate to obtain a two-phase system mixed solution;

[0041] (3) Put the two-phase mixed solution obtained in step (2) into the hydrothermal kettle, and when the temperature in the oil bath reaches 125° C., put it into the hydrothermal kettle and start stirring, carry out the catalytic reaction for 45 minutes, and after the reaction finishes, take The organic phase is separated and purified to obtain 5-hydroxymethylfurfural.

[0042] According to high-performance liquid chromatography analysis, 5-hydroxymethylfurfural was obtained in a yield of 27.8%.

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Abstract

The invention belongs to the technical field of biomass resource utilization, and particularly relates to a method for preparing 5-hydroxymethylfurfural through conversion of cellulose in a composite molten salt hydrate. The method comprises the following steps: mixing different types of molten salt hydrates according to a certain ratio to prepare the composite molten salt hydrate, adding cellulose and an organic solvent, carrying out a catalytic reaction under a hydrothermal condition, cooling, and separating an organic phase to obtain the 5-hydroxymethylfurfural. The composite molten salt hydrate is used as a catalyst and a reaction solvent, so that on one hand, cellulose can be dissolved, and on the other hand, the composite molten salt hydrate can provide a catalytic activity center needed by cellulose conversion, and the cellulose conversion rate and the product yield are improved.

Description

technical field [0001] The invention belongs to the technical field of biomass resource utilization, and specifically relates to a method for preparing 5-hydroxymethylfurfural by converting cellulose in a hydrothermal kettle by using composite molten salt hydrate as a catalyst and reaction system. Background technique [0002] Biomass generally refers to all substances derived from photosynthesis in nature. As cellulose is the most widely sourced biomass energy on earth, how to convert cellulose into valuable platform compounds is very important. 5-Hydroxymethylfurfural is a very valuable chemical, which is an important component of fuel precursors, and some of its derivatives (such as dimethylfuran, ethoxymethylfurfural, etc.) The fuel has a higher energy density and octane rating. At the same time, 5-hydroxymethylfurfural can also be converted into valuable chemical compounds such as 1,6-hexanediol, polyvinyl furanic acid, 5-hydroxymethyl-2-furancarboxylic acid, 2,5-fura...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46B01J27/138B01J27/128B01J27/122
CPCC07D307/46B01J27/138B01J27/128B01J27/122
Inventor 解玉姣刘刚孙中远崔洪友魏春杰
Owner SHANDONG UNIV OF TECH
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