Method for preparing 5-hydroxymethylfurfural from biomass

A technology of hydroxymethylfurfural and methyl isobutyl ketone, which is applied in the field of preparing 5-hydroxymethylfurfural, can solve the problems of low activity of heterogeneous catalytic systems and catalyst deactivation, and achieve good stability of catalytic activity and catalytic The effect of high activity and wide source of raw materials

Active Publication Date: 2021-05-04
重庆化工职业学院
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AI Technical Summary

Problems solved by technology

There are many domestic and foreign research reports on the preparation of HMF from glucose dehydration, but with the deepening of research work, people have gradually discovered some problems, which have become the bottleneck restricting the large-scale production of HMF from glucose, such as the relatively low activity of the heterogeneous catalytic system Or the catalyst is seriously deactivated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038]The synthesis method of 5-hydroxymethylhydehyde, the specific steps are:

[0039]A. Preparation of the catalyst: 1 g of maleic acid dissolves into 1 L deionized water to obtain a aqueous solution of maleic acid, and then 0.2 g of choline choline is added to the aqueous maleic acid solution and mix well to obtain a catalyst;

[0040]B. The 1.0012 kg catalyst and 1.2 kg of rice straw obtained in step A were introduced into the glass reactor, sealed, stirred at 80 ° C for 6 h; cooled to room temperature, filter paper filtration, washed, to give glucose, fructose, catalyst and water Mixed solution;

[0041]C. The 1L mixed solution obtained from step B and 0.5 L methyl isobutyl ketone was sequentially introduced into the glass reactor, reacted at 140 ° C for 8 h, i.e., 5-hydroxymethyla, test, 5-hydrooflorida The concentration of the basedehyde is 80g / L.

Embodiment 2

[0043]The synthesis method of 5-hydroxymethylhydehyde, the specific steps are:

[0044]A. Preparation of the catalyst: 5 g of oxalic acid dissolves into 1 L deionized water to obtain an oxalic acid solution, and then 2.5 g of choline choline is added to the oxic acid solution and mix well to obtain a catalyst;

[0045]B. The 1.0075 kg catalyst and 2 kg of the pads obtained in step A are sequentially introduced into the glass reactor, sealed, stirred at 100 ° C for 3 h; cool to room temperature, filter paper filtration, wash, to obtain glucose, fructose, catalyst and water Mixed solution;

[0046]C. The 1L mixed solution obtained from step B and 0.5L sec-butylphenol was introduced into the glass reactor, reacted at 160 ° C for 6 h, i.e., 5-hydroxymethylfurz, detected, 5-hydroxymethylafural The concentration is 120 g / L.

Embodiment 3

[0048]The synthesis method of 5-hydroxymethylhydehyde, the specific steps are:

[0049]A. Preparation of the catalyst: 3 g of butyric acid dissolves 3 g of dikaroic acid to obtain a hydrobutic acid solution, and then 1 g chloride choline is added to the aqueous butyrate solution and mix well to obtain a catalyst;

[0050]B. The 1.004 kg catalyst and 2 kg pepper trunks obtained by step A were sequentially introduced into the glass reactor, sealed, stirred at 110 ° C for 3 h; cooled to room temperature, filter paper filtration, washed, to give glucose and fructose, catalyst, Water mixed solution.

[0051]C. The 1L mixed solution obtained from step B and 1L methyl isobutyl ketone was sequentially introduced into the glass reactor, reacted at 150 ° C for 4 h, i.e., 5-hydroxymethyla, detected, 5-hydroxymethyl The concentration of furfural is 80g / L.

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Abstract

The invention belongs to the technical field of 5-hydroxymethylfurfural, and in particular relates to a method for preparing 5-hydroxymethylfurfural from biomass. The method comprises the following steps: A. introducing the catalyst and the biomass into the reactor successively, sealing it, stirring it at 80-100° C. for 3-6 hours, cooling to room temperature, filtering, and washing to obtain a mixed solution; B. The mixed solution and organic solvent obtained by A washing are introduced into the reactor and heated at 140-160° C. for 6-8 hours to obtain the product; the catalyst includes choline chloride and organic acid solution. Adopt the method of the present invention to prepare 5-hydroxymethylfurfural, the concentration of 5-hydroxymethylfurfural can reach 80-120g / L, the catalyst is reused 10 times, the concentration of 5-hydroxymethylfurfural is almost unchanged, and the stability is very good .

Description

Technical field[0001]The invention belongs to the field of furfural technology, and more particularly to a method of preparing a 5-hydroxymethylhydehyde for biomass as a raw material.Background technique[0002]The increasing fossil resources, especially oil resources, prompts people to develop new renewable energy to replace the current fossil resources. In various ways of energy replacement, such as wind energy, solar, water, geothermal energy, and biomass energy, only biomass energy is directly in the form of a variety of compounds and chemical quality, from existing The perspective of industrial system and social application system, with biomass, can replace oil energy, has natural correlation. Biomass's alternative ways of oil resources are multifaceted, and one other side develop biofuels alternative stone fuels, and on the other hand, there are various biomass chemical products to replace stone products, thus using renewable resources to replace stone fuel ("biomass" Ways and p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 马昱博揭芳芳李小庆宋春雨廖明佳何桅
Owner 重庆化工职业学院
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