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

A technology for hydroxymethyl furfural and glucose, applied in the field of preparing 5-hydroxymethyl furfural, can solve the problems of inability to meet production requirements, instability, low selectivity and yield of 5-hydroxymethyl furfural, etc., and achieves improved reaction The effect of conversion rate and selectivity, high selectivity, and easy industrial production

Active Publication Date: 2010-01-20
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
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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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 〔1〕Weigh 10g of glucose and put it into the autoclave, then add 30ml of water, seal it, heat up to 250°C, and inject 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 35°C to obtain 8.1g of light yellow liquid;

[0018] [2] The light yellow liquid was dried and dehydrated, and ethanol crystallized to obtain 6 g of light yellow needle-shaped 5-hydroxymethylfurfural product.

Embodiment 2

[0020] 〔1〕Weigh 10g of glucose into the autoclave, then add 50ml of water, seal it, heat up to 240°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 at 25°C to obtain 8.4g of light yellow liquid;

[0021] [2] The light yellow liquid was dried and dehydrated, and crystallized from acetone to obtain 5.6 g of light yellow needle-shaped 5-hydroxymethylfurfural product.

Embodiment 3

[0023] 〔1〕Weigh 10g of glucose and put it into the autoclave, then add 80ml of water, seal it, heat up to 200°C, and inject 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 8.3g of light yellow liquid;

[0024] [2] The light yellow liquid was dried and dehydrated, and crystallized from ethyl acetate to obtain 6.5 g of light yellow needle-shaped 5-hydroxymethylfurfural product.

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PUM

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural by taking glucose as a raw material, which comprises the steps of: mixing the glucose with water according to the mass ratio of 1: 3-10, loading the mixture into a high-pressure reactor, sealing the high-pressure reactor, increasing the reaction temperature to be between 120 and 250 DEG C, injecting liquid carbon dioxide into the reactor, and controlling the pressure to be between 10 and 25MPa; performing the separation of carbon dioxide and a product on supercritical carbon dioxide with the product dissolved therein through a separator during the reaction, and controlling the separation pressure to be between 5 and 8MPa and the separation temperature to be between 25 and 70 DEG C; and discharging the product 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 of the 5-hydroxymethylfurfural, 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 the integrated preparation of 5-hydroxymethylfurfural by using glucose as a raw material and adopting supercritical phase reaction separation. 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 bio...

Claims

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Application Information

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IPC IPC(8): C07D307/48
CPCY02P20/54
Inventor 侯相林乔欣刚邓天昇
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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