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A kind of two-step method catalyzing fructose to prepare the method for 2,5-furandicarboxaldehyde

A technology of furandicarbaldehyde and fructose, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve expensive, difficult HMF separation, separation and purification technology Difficulties have not been effectively resolved and other problems, to achieve the effect of mild reaction conditions, mild oxidation, and cost reduction

Active Publication Date: 2022-08-09
徐新杰
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the preparation process of HMF, its separation and purification technical difficulties have not been effectively resolved, resulting in a certain degree of limitation in the research and industrial application of related derivatives
Therefore, it is an effective way to solve this problem by synthesizing HMF oxidized derivatives directly from sugar compounds such as fructose, glucose, and sucrose through a "one-pot method". However, the separation of raw material HMF is difficult and expensive, making 2,5- Furandicarbaldehyde is expensive to produce

Method used

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  • A kind of two-step method catalyzing fructose to prepare the method for 2,5-furandicarboxaldehyde

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Experimental program
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Effect test

Embodiment 1

[0020] A method for preparing 2,5-furandicarboxaldehyde by two-step method catalyzing fructose, comprising the following steps:

[0021] 1) in parts by weight, 30 parts of fructose, 0.3 part of catalyst ceria, 1 part of sodium dodecylbenzene sulfonate and 100 parts of DMF are placed in the reaction kettle, and after sealing, they are uniformly stirred at a speed of 300r / min to form. mixture;

[0022] 2) Continue to feed air into it under the condition of stirring, keep the pressure in the reactor to be 4MPa, the temperature is 80 ℃, stop the reaction after 1 hour of reaction, naturally cool to room temperature, and obtain 2,5-furandicarbaldehyde as the main component of the mixture.

[0023] The product was analyzed by high performance liquid chromatography, and the following results were obtained: the conversion rate of fructose was 100%, and the yield of 2,5-furandicarbaldehyde was 91%.

Embodiment 2

[0025] A method for preparing 2,5-furandicarboxaldehyde by two-step method catalyzing fructose, comprising the following steps:

[0026] 1) In parts by weight, 20 parts of fructose, 0.2 part of catalyst ceria, 1 part of anionic polyacrylamide and 100 parts of THF are placed in the reaction kettle, and after sealing, stirring at a speed of 300r / min is uniform to form a mixed solution;

[0027] 2) Continue to feed air into it under the stirring condition, keep the pressure in the reactor to be 3MPa, and the temperature is 70 ° C, stop the reaction after 2 hours of reaction, naturally cool to room temperature, and obtain 2,5-furandicarbaldehyde as the main component of the mixture.

[0028] The product was analyzed by high performance liquid chromatography, and the following results were obtained: the conversion rate of fructose was 100%, and the yield of 2,5-furandicarbaldehyde was 89%.

Embodiment 3

[0030] A method for preparing 2,5-furandicarboxaldehyde by two-step method catalyzing fructose, comprising the following steps:

[0031] 1) In parts by weight, 40 parts of fructose, 0.5 part of catalyst ceria, 2 parts of sodium lauryl sulfate and 80 parts of acetone are placed in the reaction kettle, and the mixed solution is formed by stirring at a speed of 300r / min after sealing. ;

[0032] 2) Continue to feed air into it under the condition of stirring, keep the pressure in the reactor to be 5MPa, and the temperature is 70 ° C, stop the reaction after 2 hours of reaction, and naturally cool to room temperature, to obtain 2,5-furandicarbaldehyde is the main component of the mixture.

[0033] The product was analyzed by high performance liquid chromatography, and the following results were obtained: the conversion rate of fructose was 100%, and the yield of 2,5-furandicarbaldehyde was 93%.

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Abstract

The invention relates to a method for preparing 2,5-furandicarboxaldehyde by catalyzing fructose by a two-step method. The catalyst and 80-100 parts of organic solvent are placed in the reaction kettle, and after sealing, stirring is uniform to form a mixed solution, and the catalyst is ceria with a particle size of less than 100 nm; 2) Under the condition of continuous stirring, air is introduced into it to keep the reaction kettle. The pressure inside is 2~5MPa, the temperature is 70~90 ℃, the reaction is stopped after 1~2 hours of reaction, and it is naturally cooled to room temperature to obtain a mixed solution with 2,5-furandicarbaldehyde as the main component. The reaction conditions of the invention are mild, high temperature and high pressure are not required, the yield of 2,5-furandicarboxaldehyde is high, the complicated separation steps of HMF can be omitted, the cost is reduced, and the goal of green chemistry is more complied with.

Description

technical field [0001] The invention relates to a method for preparing 2,5-furandicarbaldehyde, in particular to a method for catalyzing fructose to prepare 2,5-furandicarbaldehyde, and belongs to the technical field of industrial catalysis. Background technique [0002] With the continuous consumption of fossil resources and the increasingly prominent environmental problems, the use of biomass raw materials to replace fossil resources to prepare bulk chemicals, fine organic intermediates and polymer materials has become one of the research hotspots in the field of biomass-based development and utilization in recent years. [0003] 5-Hydroxymethylfurfural (5-HMF), as one of the biomass-based platform compounds, is also an important intermediate for the synthesis of various fine chemicals and furan-based polymers, which can be obtained from carbohydrates such as glucose, fructose and cellulose. . 2,5-Furandicarbaldehyde (DFF) is an important downstream product obtained by se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46B01J23/10
CPCC07D307/46B01J23/10Y02P20/584
Inventor 徐新杰郑素娟
Owner 徐新杰