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Method for preparing 5-hydroxymethylfurfural by taking cellulose as raw material

A technology of hydroxymethylfurfural and cellulose, which is applied in the field of preparing 5-hydroxymethylfurfural, can solve the problems of 5-hydroxymethylfurfural, such as low selectivity and yield, failure to meet production requirements, instability, etc., and achieve improved Reaction conversion rate and selectivity, elimination of pollution and corrosion, high selectivity effect

Active Publication Date: 2010-01-20
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the 5-hydroxymethylfurfural molecule contains a furan ring and an aldehyde group, its chemical properties are relatively active, and it is extremely unstable in acid-base, high temperature, and polar environments, and it will further dehydroxymethyl to form furfural or ring-opened Other substances such as levulinic acid lead to extremely low selectivity and yield of 5-hydroxymethylfurfural, which cannot meet the production requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 〔1〕Take 200g of sawdust and pretreat it in hydrochloric acid solution with pH=3.5 for 2 hours, neutralize with sodium hydroxide solution, filter, wash the filter residue with water, dry the filter residue, and set aside.

[0022] 〔2〕Weigh 10g of dry filter residue and put it into the autoclave, then add 30ml of water, seal it, raise the temperature to 250°C, and pass in CO 2 Gas, control the pressure at 25MPa, and at the same time, pass the supercritical carbon dioxide dissolved in the product through the separator to separate the carbon dioxide and the product, control the separation pressure in the separator to 5MPa, and the separation temperature to 25°C to obtain 8g of light yellow liquid;

[0023] [3] The light yellow liquid was dried and dehydrated, and crystallized from ethanol to obtain 6 g of light yellow needle-shaped 5-hydroxymethylfurfural product.

Embodiment 2

[0025] [1] Take 200g of bran and place it in dilute sulfuric acid solution with pH = 1.0 for 2.5 hours, neutralize with sodium hydroxide solution, filter, wash the filter residue with water, dry the filter residue, and set aside.

[0026] 〔2〕Weigh 10g of dry filter residue and put it into an autoclave, then add 50ml of water, seal it, heat up to 220°C, and pass in CO 2 Gas, control the pressure at 20MPa, and at the same time, pass the supercritical carbon dioxide dissolved in the product through the separator to separate the carbon dioxide from the product, control the separation pressure in the separator to 7MPa, and the separation temperature to 35°C to obtain 8.5g of light yellow liquid;

[0027] [3] The light yellow liquid was dried and dehydrated, and crystallized from acetone to obtain 5.5 g of light yellow needle-shaped 5-hydroxymethylfurfural product.

Embodiment 3

[0029] [1] Take 200g of corn stalks and place them in a sodium hydroxide solution with a pH of 9.0 to pretreat for 7 hours, neutralize with dilute hydrochloric acid, filter, wash the filter residue with water, dry the filter residue, and set aside.

[0030] 〔2〕Weigh 10g of dry filter residue and put it into an autoclave, then add 80ml of water, seal it, heat up to 150°C, and pass in CO 2 Gas, control the pressure at 15MPa, and at the same time, pass the supercritical carbon dioxide dissolved in the product through the separator to separate the carbon dioxide and the product, control the separation pressure in the separator to 6MPa, and the separation temperature to 40°C to obtain 8g of light yellow liquid;

[0031] [3] The light yellow liquid was dried and dehydrated, and crystallized from ethyl acetate to obtain 6.3 g of light yellow needle-shaped 5-hydroxymethylfurfural product.

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural by taking cellulose as a raw material, which comprises the steps of: pretreating a biomass material rich in the cellulose by utilizing acid or alkali, neutralizing the biomass material, filtering to remove hemicellulose and lignin, washing obtained cellulose filter residue with water, and drying the cellulose filter residue; mixing the cellulose filter residue or pure cellulose with the water, loading the mixture into a high-pressure reactor, sealing the high-pressure reactor, and injecting liquid carbon dioxide into the reactor for reaction; and separating supercritical carbon dioxide dissolved with the 5-hydroxymethylfurfural through a separator during the reaction, discharging the 5-hydroxymethylfurfural from the bottom of the separator, and obtaining a 5-hydroxymethylfurfural product through drying, dehydration and crystallization. The method has the advantages of high selectivity, suitable continuous production, high product content, green and environment-friendly process, and easy industrialized production.

Description

technical field [0001] The invention relates to a method for preparing 5-hydroxymethylfurfural from cellulose-rich biomass. technical background [0002] The huge demand for energy around the world, the instability of oil production, and global warming have once again stimulated people's interest in renewable energy. Biofuels have become the primary "new force" and have attracted the attention of researchers at home and abroad. The reserves of biofuels are huge. It is estimated that the annual energy stored in plants is about 10 times that of the world's main fuel consumption, while the utilization of energy as energy accounts for less than 1% of the total. [0003] The currently widely used biofuels are ethanol and biodiesel, among which the annual production of ethanol in the United States and Brazil both exceeds 10 million tons. With the increase of ethanol production, the production of bioethanol using sugar or grain as raw material is limited by food resources, and it ...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCY02P20/54
Inventor 侯相林邓天昇乔欣刚
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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