Method for synthesizing 5-hydroxymethyl-furfural

A technology of hydroxymethyl furfural and a synthesis method, applied in the field of bio-organic synthesis of 5-hydroxymethyl furfural, can solve the problems of short supply, high cost, high market price of 5-hydroxymethyl furfural and the like

Active Publication Date: 2012-05-09
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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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 40g of chromium chloride and 160g of caprolactam into the flask, heat up (before 60°C, increase the temperature by 20°C per hour, and then increase the temperature by 10°C per hour), and melt to 120°C to become a uniform ionic liquid. Slowly lower the temperature of the configured ionic liquid to below 80° C., add 45 g of glucose (pharmaceutical grade) in batches, and stir while adding. After adding and dissolving evenly, slowly raise the temperature and depressurize (control pressure 0.05-0.07MPa) to dehydrate at the same time. When the temperature rises above 100°C, keep the temperature and continue the reaction and dehydration until no water evaporates. A mixture of dark gray liquids together with ionic liquids.

[0013] Transfer the reaction mixture to a vacuum rectification device while it is hot, keep the system pressure at 150-180KPa and temperature at 90-105°C, and control a certain material transfer rate so that the product, by-product and remaining raw mat...

Embodiment 2

[0016] Add 50g of chromium chloride and 200g of caprolactam into the flask, heat up (before 60°C, increase the temperature by 20°C per hour, and then increase the temperature by 10°C per hour), and melt to 120°C to become a uniform ionic liquid. Slowly lower the temperature of the configured ionic liquid to below 80° C., add 60 g of glucose (pharmaceutical grade) in batches, and stir while adding. After adding and dissolving evenly, slowly raise the temperature, and at the same time depressurize (control pressure 0.05-0.06MPa) for dehydration. When the temperature reaches above 100°C, keep the temperature, continue the reaction and dehydration until no water volatilizes, and obtain the reacted Dark gray liquid in mixture with ionic liquid.

[0017] Transfer the reaction mixture to a set of vacuum distillation equipment while it is hot, keep the system pressure at 150-160KPa and temperature at 95-103°C, control a certain material transfer rate, and completely separate the produ...

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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 method for bioorganic synthesis of 5-hydroxymethylfurfural. Background technique [0002] The synthesis technology of 5-hydroxymethylfurfural has always been an international problem. In China, the preparation of 5-hydroxymethylfurfural mainly adopts the process of plant extraction, such as using rehmannia glutinosa and other plants to process mature rehmannia glutinosa, and using extraction methods such as extraction to obtain 5-hydroxymethylfurfural through complicated purification processes. 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/48
CPCY02P20/54
Inventor 胡晓蔡佩君商永嘉李玉平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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