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Method for preparing 2, 5-furandicarboxaldehyde by catalyzing fructose through two-step method

A furandiformaldehyde and fructose technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the technical difficulties of separation and purification. Expensive, difficult separation of HMF, etc.

Active Publication Date: 2021-05-18
徐新杰
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  • Summary
  • 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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  • Method for preparing 2, 5-furandicarboxaldehyde by catalyzing fructose through two-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020]Two-step catalytic fructose preparation of 2,5-furan methylene formaldehyde, including the following steps:

[0021]1) According to the weight of the mass, 30 parts of jug, 0.3 parts of catalyst cerium oxide, 1 part of dodecyl benzene sulfonate and 100 parts of DMF are placed in the reaction vessel, and the mixing of 300 r / min is mixed and uniformly formed at speeds of 300 r / min. mixture;

[0022]2) Continue to vent the air under the stirring conditions, maintain the pressure of 4 MPa in the reactor, and the temperature is 80 ° C, and the reaction is stopped after 1 hour, naturally cooled to room temperature, that is, 2,5-furan methylene formaldehyde is the main component. Mixed mixture.

[0023]The product was analyzed by high performance liquid chromatography, resulting in the following results, fructose conversion rate of 100%, and the yield of 2,5-furan methylene formaldehyde was 91%.

Embodiment 2

[0025]Two-step catalytic fructose preparation of 2,5-furan methylene formaldehyde, including the following steps:

[0026]1) Press by weight, 20 parts of jug, 0.2 parts of catalyst cerium oxide, 1 part of anionic polyacrylamide and 100 parts of THF, and the mixing solution is mixed after the speed of 300 r / min after the speed of 300 r / min is sealed.

[0027]2) Continue to vent the air under the stirring conditions, keep the pressure in the reactor to be 3 MPa, the temperature is 70 ° C, and the reaction is stopped after 2 hours, naturally cooled to room temperature, that is, 2,5-furan methylene formaldehyde is the main component Mixed mixture.

[0028]The product was analyzed by high performance liquid chromatography, resulting in the following results, fructose conversion rate of 100%, 2,5-furan methylene formaldehyde was 89%.

Embodiment 3

[0030]Two-step catalytic fructose preparation of 2,5-furan methylene formaldehyde, including the following steps:

[0031]1) 40 parts of juicy, 0.5 parts of catalyst cerium oxide, 2 parts of dodecyl sulfate, and 80 parts of acetone in the reactor, and the mixing solution is mixed after 300 r / min after stirring at a rate of 300 r / min after stirring. ;

[0032]2) Continue to vent the air under stirring, maintain the pressure of 5 MPa in the reactor, and the temperature is 70 ° C, and the reaction is stopped after 2 hours, naturally cooled to room temperature, that is, 2,5-furan methylene formaldehyde is the main component. Mixed mixture.

[0033]The product was analyzed by high performance liquid chromatography, resulting in the following results, fructose conversion rate of 100%, and the yield of 2,5-furan methylene formaldehyde was 93%.

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Abstract

The invention relates to a method for preparing 2, 5-furandicarboxaldehyde by catalyzing fructose through a two-step method, which comprises the following steps: 1) putting 20-40 parts by weight of fructose, 0.2-0.5 part by weight of a catalyst, 1-2 parts by weight of a dispersant and 80-100 parts by weight of an organic solvent into a reaction kettle, sealing and uniformly stirring to form a mixed solution, the catalyst being cerium dioxide with the particle size of less than 100nm; and 2) introducing air into the reaction kettle under the condition of continuously stirring, keeping the pressure in the reaction kettle at 2-5MPa and the temperature at 70-90 DEG C, reacting for 1-2 hours, then stopping the reaction, and naturally cooling to room temperature to obtain a mixed solution with 2, 5-furandicarboxaldehyde as a main component. The method has the advantages of mild reaction conditions, no need of high temperature and high pressure, high yield of 2, 5-furandicarboxaldehyde, omission of the complicated separation step of HMF, cost reduction, and better conformity to the target of green chemistry.

Description

Technical field[0001]The present invention relates to a method for preparing 2,5-furan methylene formaldehyde, and more particularly to a method of catalytic frugese preparation 2,5-furanium dimethylmethylene, which belongs to the industry catalytic technology.Background technique[0002]With the continuous consumption of fossil resources and the increasing environmental problem, it has prepared bulk chemicals, fine organic intermediates and polymer materials in the production of biomass raw materials, and has become one of the research hotspots in the field of biomass development and utilization in recent years.[0003]5-hydroxymethyla (5-HMF) is one of the biomass platform compounds, and is also an important intermediate synthesizing a variety of fine chemicals and furan-based polymers, which can be prepared by carbohydrates such as glucose, fructose and cellulose. . 2,5-furan diehyde (DFF) is an important downstream product of HMF selective oxidation, which has typical chemical prope...

Claims

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Application Information

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