Method for synthesizing 5-hydroxymethyl-furfural

A technology of hydroxymethylfurfural and synthetic method, which is applied in the field of bioorganic synthesis of 5-hydroxymethylfurfural, and can solve problems such as complicated processing, high price, and limited use

Active Publication Date: 2008-12-31
ANHUI RUISAI BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the content in plants is less than 7%, and the extraction and other processing processes are very complicated, the market price of 5-hydroxymethylfurfural is expensive, and the supply is tight, and the supply exceeds demand
Due to its high price, its many uses are greatly limited, making it possible to use 5-Hydroxymethylfurfural to produce more than a hundred kinds of important fine chemicals, most of which can only be sighed in anticipation of the price
In foreign countries, the plant extraction method is still the main production method of 5-hydroxymethylfurfural, but the synthesis technology of sugar conversion such as high-temperature two-step catalytic dehydration of fructose has appeared, but its cost is still relatively high, and there are also problems in quality

Method used

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  • Method for synthesizing 5-hydroxymethyl-furfural

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Effect test

Embodiment 1

[0012] Add 40g of chromium chloride and 160g of caprolactin to the flask, heat to increase the temperature (before 60°C, increase the temperature by 20°C per hour, and then increase the temperature by 10°C per hour) to melt at 120°C to become a uniform ionic liquid. The configured ionic liquid was slowly cooled to below 80°C, and 45 g of glucose (pharmaceutical grade) was added in batches, while stirring. After adding and dissolving evenly, slowly increase the temperature and depressurize (control pressure 0.05~0.07MPa) for dehydration. When the temperature rises above 100°C, keep the temperature, continue the reaction and dehydration until no water volatilizes to obtain the post-reaction The mixture of ionic liquid and dark gray liquid together.

[0013] The reaction mixture is transferred to a set of vacuum rectification device while it is hot, and the system pressure is maintained at 150-180KPa and the temperature is 90-105°C, and a certain material transfer rate is controlled ...

Embodiment 2

[0016] Add 50g of chromium chloride and 200g of caprolactin to the flask, heat to increase the temperature (before 60°C, increase the temperature by 20°C per hour, and then increase the temperature by 10°C per hour) to melt at 120°C to become a uniform ionic liquid. The configured ionic liquid was slowly cooled to below 80°C, and 60 g of glucose (pharmaceutical grade) was added in batches, while stirring. After adding and dissolving uniformly, slowly increase the temperature and depressurize (control pressure 0.05~0.06MPa) for dehydration. When the temperature is above 100℃, keep the temperature, continue the reaction and dehydration until no water volatilizes, and obtain the reacted Dark gray liquid with mixture and ionic liquid.

[0017] Transfer the reaction mixture to a set of vacuum rectification device while it is hot, and keep the system pressure 150~160KPa and temperature 95~103

[0018] ℃, control a certain material transfer speed, so that products, by-products and remain...

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Abstract

The invention relates to a synthesis method for 5-hydroxymethylfurfural and is characterized in that glucose is used as raw material and the 5-hydroxymethylfurfural is generated in the ionic liquid of chromium chloride through intramolecular mutarotation and dehydration; the reaction mixture firstly goes through flash evaporation to separate the product, by-product and the residual raw materials from the ionic liquid; the evaporated mixture is extracted and purified with supercritical fluid CO2 to obtain the 5-hydroxymethylfurfural; the ionic liquid is recycled. The synthesis technology has simple and fast courses and is energy-saving and environmentally-friendly; the obtained product has high quality and low cost, with the total mass yield reaching more than 58%.

Description

Technical field [0001] The invention belongs to the technical field of bioorganic synthesis, and relates to a bioorganic synthesis method of 5-hydroxymethyl furfural. Background technique [0002] The synthesis technology of 5-hydroxymethyl furfural has always been an international problem. In China, the preparation of 5-hydroxymethyl furfural mainly adopts the process of plant extraction. For example, the use of rehmannia glutinosa and other plants to process mature rehmannia glutinosa, the use of extraction and other extraction methods, through a complex purification process to obtain 5-hydroxymethyl furfural. Since the content in plants is less than 7%, and the processing process such as extraction is very complicated, the market price of 5-hydroxymethyl furfural is expensive, and the supply is tight, and the supply is in short supply. Due to its high price, its many uses are greatly restricted, and most of the hundreds of important fine chemicals that can be prepared from 5-h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/48
CPCY02P20/54
Inventor 胡晓王玉成王理想王友志王庆华周飞丁庆燚瞿志荣赵红胡丹红
Owner ANHUI RUISAI BIOCHEM TECH
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