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Preparation method of 5-hydroxymethylfurfural

A technology of hydroxymethylfurfural and dimethyl sulfoxide, applied in the field of hydroxymethylfurfural preparation, achieves the effects of simple operation, increased reaction efficiency, and high extraction rate

Active Publication Date: 2013-03-13
SHENGQUAN HEALTANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the reaction process and the high post-treatment cost and the high industrialization cost caused by the low solid content of the reaction solution in the preparation of the above prior art 5-hydroxymethylfurfural , low yield, the present invention provides a method for preparing 5-hydroxymethylfurfural with low cost, suitable for industrialization, high solid content in the reaction liquid, and high yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 25 g of solvent DMSO (dimethyl sulfoxide) to a 100 mL single-necked round-bottom flask with magnetic stirring and water bath condensation, add 12.50 g (33.33%) of D-fructose under stirring conditions, heat up to 120 °C, and add catalyst chlorine Chromium 1.88g (15.04%), constant temperature reaction, use a spectrophotometer to detect the reaction yield of 5-hydroxymethylfurfural, when the yield is greater than 90%, place the reaction bottle in cold water to quench the reaction.

[0031] The reaction system was subjected to pressure distillation at 70°C under a vacuum condition lower than 100 Pa. After most of the DMSO was removed, the reaction system was taken out and cooled to room temperature to obtain the extract, and 20 g of saturated saline (approx. 2 times of the extract), and the residual DMSO and catalyst were dissolved in water; then extracted 5 times with 20 mL of ethyl acetate, combined the organic phases, dried overnight with 50 g of anhydrous sodium sulf...

Embodiment 2

[0035] Add 450 g of solvent DMSO to a 1000 mL single-necked round bottom flask with magnetic stirring and water bath condensation, add 225 g (33.3%) of sugar under stirring, heat up to 160 °C, add 11.25 g (5%) of catalyst, and react at constant temperature. The reaction yield of 5-hydroxymethylfurfural was detected with a spectrophotometer, and when the yield was greater than 90%, the reaction bottle was placed in cold water to quench the reaction.

[0036] The reaction system was subjected to pressure distillation at 70°C under a vacuum condition lower than 100 Pa. After most of the DMSO was removed, the reaction system was taken out and cooled to room temperature to obtain the extract, and 1500 g of saturated saline (approximately 10 times of the extraction solution), the residual DMSO and catalyst were dissolved in water; then extracted three times with 400mL ethyl acetate, the organic phases were combined, dried overnight with 500g anhydrous sodium sulfate, and the ethyl ac...

Embodiment 3

[0039] Add 50 g of solvent DMSO (dimethyl sulfoxide) to a 100 mL single-necked round-bottom flask with magnetic stirring and water bath condensation, add 25 g (33.3%) of D-fructose under stirring conditions, heat up to 80 °C, add catalyst to chlorinate Chromium 2.5g (10%), constant temperature reaction, use a spectrophotometer to detect the reaction yield of 5-hydroxymethylfurfural, when the yield is greater than 90%, place the reaction bottle in cold water to quench the reaction.

[0040] The reaction system was subjected to pressure distillation at 70°C under a vacuum condition lower than 100 Pa. After most of the DMSO was removed, the reaction system was taken out and cooled to room temperature to obtain the extract, and 60 g of saturated saline (approx. 3 times of the extract) to dissolve the residual DMSO and catalyst in water; then extract 4 times with 40mL ether, combine the organic phases, dry with 100g anhydrous sodium sulfate overnight, and remove ethyl acetate under ...

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Abstract

The invention relates to the technical field of hydroxymethylfurfural preparation, particularly a preparation method of 5-hydroxymethylfurfural, which comprises the following steps: dissolving a saccharide raw material in a dimethylsulfoxide solvent, heating to 80-160 DEG C, adding chromium chloride to react, and detecting the reaction yield of the 5-hydroxymethylfurfural; and when the yield is greater than 90%, quenching the reaction, carrying out vacuum distillation to remove the solvent, diluting the residual liquid with a saturated sodium chloride water solution to obtain a solution to be extracted, extracting with an organic solvent, and drying by distillation to obtain the 5-hydroxymethylfurfural. The mass ratio of the saccharide raw material to the dimethylsulfoxide is 1:(1.5-20), and the addition amount of chromium chloride is 5-20 wt% of the saccharide raw material. The synthetic route is easy and simple to operate, and does not need any inert gas protective atmosphere; the total mass yield is up to higher than 90%, and the purity is up to higher than 96%; and the invention is suitable for industrial production, and enhances the solid content of the reaction to 33%, thereby greatly enhancing the reaction efficiency.

Description

technical field [0001] The invention relates to the technical field of hydroxymethylfurfural preparation, in particular to a preparation method of 5-hydroxymethylfurfural. Background technique [0002] With the decreasing reserves of petrochemical resources and the rising prices of petrochemical downstream products, it is becoming more and more important to seek sustainable alternatives. In recent years, biomass, as a renewable resource that is expected to replace fossil energy in the future, has received more and more attention. Among them, the synthesis of furan products from glucose, fructose and sucrose is one of the important processes of biomass conversion and utilization. Studies have shown that 5-hydroxymethylfurfural, which is produced after fructose loses three molecules of water through catalytic dehydration reaction, is an important platform chemical connecting biomass conversion and large-scale industrialization. It can be used to synthesize many high value-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/48
Inventor 江成真胡廷峰焦芬王芳芳
Owner SHENGQUAN HEALTANG
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