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Method for preparing 5-hydroxymethylfurfural by solid acid catalysis

A technology catalyzed by hydroxymethylfurfural and solid acid, which is applied in chemical instruments and methods, catalyst carriers, physical/chemical process catalysts, etc., can solve problems such as resource waste, physical and chemical properties and processing performance obstacles, and achieve easy separation and reduce Reaction activation energy, high activity effect

Inactive Publication Date: 2012-04-04
XISHUANGBANNA TROPICAL BOTANICAL GARDEN CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the physical and chemical properties, processing properties, and technology of lignin have become obstacles to the current lignin research, and most of the lignin is directly discarded, resulting in a huge waste of resources
Using lignin as the raw material for carbohydrate dehydration reaction catalyst has the advantages of turning waste into wealth, solving environmental pollution, and sustainable development, but there is no report in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The residual lignin sample was dried at 105°C, and 10g of dry lignin was carbonized at 400°C for 10h under the protection of an inert gas to obtain a black solid Powder, porous carbon carrier:concentrated sulfuric acid mass ratio 1:5, black solid powder washed with deionized water and dried to obtain lignin-based solid acid.

[0022] Add 10mL deionized water to the autoclave, preheat to 80°C, then add 0.5g lignin-based solid acid and 2g fructose, stir, heat to 150°C within 10min, and react at constant temperature for 300min. After the reaction, samples were taken and cooled with cold water at 0-20° C., diluted with ultrapure water, and analyzed by liquid chromatography for the content of fructose and 5-hydroxymethylfurfural. The conversion rate of fructose was 100%, and the yield of 5-hydroxymethylfurfural was 16%.

Embodiment 2

[0024] The residual lignin sample was dried at 105°C, and 10g of dry lignin was carbonized at 400°C for 5 hours under the protection of an inert gas to form a porous carbon carrier, and the porous carbon carrier was sulfonated with 98% concentrated sulfuric acid at 200°C for 10 hours to obtain a black solid Powder, porous carbon carrier:concentrated sulfuric acid mass ratio 1:10, washed with deionized water and dried to obtain lignin-based solid acid.

[0025] Add 20mL of deionized water to the autoclave, preheat to 80°C, then add 1g of lignin-based solid acid and 4g of fructose, stir, heat to 150°C within 5min, and react at constant temperature for 60min. After the reaction, samples were taken and cooled with cold water at 0-20° C., diluted with ultrapure water, and analyzed by liquid chromatography for the content of fructose and 5-hydroxymethylfurfural. The conversion rate of fructose was 100%, and the yield of 5-hydroxymethylfurfural was 39%.

Embodiment 3

[0027] The residual lignin sample was dried at 105°C, and 10g of dry lignin was carbonized at 400°C for 5 hours under the protection of an inert gas to form a porous carbon carrier, and the porous carbon carrier was sulfonated with 98% concentrated sulfuric acid at 200°C for 5 hours to obtain a black solid Powder, porous carbon carrier:concentrated sulfuric acid mass ratio 1:10, washed with deionized water and dried to obtain lignin-based solid acid.

[0028] Add 2g of [Bmim]Cl into the microwave reactor, heat to 120°C within 5min, then add 0.2g of lignin-based solid acid and 0.2g of fructose, stir, and react at constant temperature for 30min. After the reaction, samples were taken and cooled with cold water at 0-20° C., diluted with ultrapure water, and analyzed by liquid chromatography for the content of fructose and 5-hydroxymethylfurfural. The conversion rate of fructose was 85%, and the yield of 5-hydroxymethylfurfural was 71%.

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural by solid acid catalysis. The method comprises the following steps of taking lignin residue hydrolyzed by biomass as carrier raw material of solid acid; synthesizing the raw material into solid acid through a two-step way of carbonization and sulfonation, so that the waste material is recycled and the problem of disposal of pollutants is solved. In the dehydration reaction of lignin-based solid acid catalyzed fructose and glucose, the yield of 5-hydroxymethylfurfural can be respectively 84% and 68%; after the dehydration reaction, the lignin-based solid acid is easy to separate and reusable, the acid density of the solid acid can be reduced after being reused five times, and the yield of the 5-hydroxymethylfurfural is still higher than 75%. The method provided by the invention can be used for realizing emission without pollution, and is helpful for realizing environment-friendly producing process of 5-hydroxymethylfurfural.

Description

technical field [0001] The invention belongs to the technical field of renewable energy production, and in particular relates to a method for preparing 5-hydroxymethylfurfural by using a solid acid catalyst. Background technique [0002] Oil, natural gas and coal have always been important sources of energy and chemical raw materials for human beings. However, with the increasingly serious environmental pollution and energy problems caused by the combustion of fossil fuels, the development of biomass energy and the reduction of dependence on mineral energy have become a priority for many countries. important energy strategy. Among many possible bio-based chemicals, 5-Hydroxymethylfurfural is an important chemical for the production of chemicals from biomass, which can be directly converted into various products with high added value and new polymer materials, such as pharmaceuticals , resinous plastics, diesel fuel additives, etc. [0003] Heterogeneous acid catalysts have...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46B01J27/02B01J32/00B01J21/18
Inventor 郭峰方真
Owner XISHUANGBANNA TROPICAL BOTANICAL GARDEN CHINESE ACAD OF SCI
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