Method for preparing 5-hydroxymethylfurfural from caprolactam/lithium chloride catalytic glucose

A technology of hydroxymethylfurfural and caprolactam, applied in the direction of organic chemistry, etc., can solve the problems of high raw material cost, difficulty in product purification, and failure to find industrialized preparation of 5-hydroxymethylfurfural, etc., to achieve industrial production, low cost, High yield effect

Inactive Publication Date: 2015-03-04
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing ionic liquid preparation methods have problems such as high cost of raw materials, difficulty in product purification, and unsuitability for large-scale industrial production applications. The cost of raw materials is generally more than twice that of commonly used organic solvents.
[0004] Although a lot of research has been done on the reaction of sugars to prepare 5-hydroxymethylfurfural, and the catalytic methods are various, so far, no industrialized method for preparing 5-hydroxymethylfurfural has been found.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of method that caprolactam / lithium chloride catalyzes glucose to prepare 5-hydroxymethylfurfural, described method operation steps are as follows:

[0019] 1. Preparation of caprolactam / lithium chloride ionic liquid: Take 5.000g of caprolactam and put it into a 50ml three-neck flask, then add lithium chloride, wherein the molar ratio of caprolactam to lithium chloride is 5:1, then heat in an oil bath, and magnetically stir to 120°C , kept in the colorless transparent liquid for 2h, namely the ionic liquid.

[0020] 2. To the ionic liquid obtained in step 1, add a solid water-absorbing agent in an amount of 21% of the mass of the ionic liquid, and cool to 80°C. The solid water-absorbing agent includes phosphorus pentoxide, calcium chloride, aluminum oxide, and color-changing silica gel .

[0021] 3. Add glucose with an amount of 10% of the mass of the cooling ionic liquid to the cooled ionic liquid obtained in step 2. After reacting with 120°C for 4 hours, the re...

Embodiment 2

[0025] A kind of method that caprolactam / lithium chloride catalyzes glucose to prepare 5-hydroxymethylfurfural, described method operation steps are as follows:

[0026] 1. Same as Step 1 of Example 1.

[0027] 2. To the ionic liquid obtained in step 1, add a solid water-absorbing agent in an amount of 22% of the mass of the ionic liquid, and cool to 80°C. The solid water-absorbing agent includes phosphorus pentoxide, calcium chloride, aluminum oxide, and color-changing silica gel .

[0028] 3. Same as Step 3 of Example 1.

[0029] 4. Same as Step 4 of Example 1.

[0030] It is measured that the yield of 5-hydroxymethylfurfural in caprolactam / lithium chloride ionic liquid without adding solid water-absorbing agent is 43.5%, and adding solid water-absorbing agent phosphorus pentoxide in caprolactam / lithium chloride ionic liquid The yield of furfural increased by 37.8%, reaching 81.3%. The yield of 5-hydroxymethylfurfural in the caprolactam / lithium chloride ionic liquid was ...

Embodiment 3

[0032] A kind of method that caprolactam / lithium chloride catalyzes glucose to prepare 5-hydroxymethylfurfural, described method operation steps are as follows:

[0033] 1. Same as Step 1 of Example 1.

[0034] 2. To the ionic liquid obtained in step 1, add a solid water-absorbing agent in an amount of 23% of the mass of the ionic liquid, and cool to 80°C. The solid water-absorbing agent includes phosphorus pentoxide, calcium chloride, aluminum oxide, and color-changing silica gel .

[0035] 3. Same as Step 3 of Example 1.

[0036] 4. Same as Step 4 of Example 1.

[0037] It is measured that the yield of 5-hydroxymethylfurfural in caprolactam / lithium chloride ionic liquid without adding solid water-absorbing agent is 43.5%, and adding solid water-absorbing agent phosphorus pentoxide in caprolactam / lithium chloride ionic liquid The yield of furfural increased by 46.2%, reaching 89.7%. The yield of 5-hydroxymethylfurfural in the caprolactam / lithium chloride ionic liquid was ...

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PUM

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural from caprolactam / lithium chloride catalytic glucose. The method comprises the following steps: adding a prepared caprolactam / lithium chloride ionic liquid into a solid water absorbent, cooling to be 80 DEG C, adding glucose, reacting for 4 hours at 120 DEG C, taking out a reaction liquid with hot water from a three-port flask, moving into a volumetric flask of 100mL, fixing the volume, sampling, and storing, wherein the yield of 5-hydroxymethylfurfural is taken as an inspection index. The method disclosed by the invention not only has the advantages of high yield and low cost, but also is capable of improving the selectivity that glucose is converted into 5-hydroxymethylfurfural and reducing further hydrolysis of 5-hydroxymethylfurfural, and is beneficial for industrial production.

Description

technical field [0001] The invention belongs to a preparation method of 5-hydroxymethylfurfural. Specifically, it is a method for preparing 5-hydroxymethylfurfural from glucose catalyzed by caprolactam / lithium chloride. Background technique [0002] 5-hydroxymethylfurfural (5-hydroxymethylfurfural, referred to as HMF), the molecular formula is C6H6O3, the relative molecular weight is 126.1, and its pure product is light yellow solid. The product is easily soluble in water, ether, ethanol, carbon tetrachloride, acetone and other common solvents. It has low toxicity and hygroscopicity, and hardly decomposes under normal temperature and pressure. [0003] The production methods of 5-hydroxymethylfurfural are mainly divided into three types according to the different reaction solvent systems: single-phase method, two-phase method and ionic liquid. Single-phase solvent systems such as water and organic solvents, water is the most ideal reaction solvent, green and cheap, but 5-h...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 姚双全覃程荣聂双喜牛芬洁袁月
Owner GUANGXI UNIV
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