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Method for preparing dimethyl furan-2,5-dicarboxylate

A technology of dimethyl furandicarboxylate and hydroxymethyl furfural, which is applied in chemical instruments and methods, catalyst activation/preparation, organic chemistry, etc., can solve the problem that the oxidation of 5-hydroxymethyl furfural is difficult and the metal resources are not suitable for extensive use. It can save the preparation cost, facilitate the activity, and avoid the agglomeration effect.

Inactive Publication Date: 2021-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the related art, dimethyl 2,5-furandicarboxylate is prepared by 5-hydroxymethylfurfural (HMF). Not only is the preparation process complicated, but also the oxidation of 5-hydroxymethylfurfural is difficult compared to monofunctional compounds. Even under the catalysis of precious metals, most of them still need to add additional basic additives, which will pollute the environment to a certain extent, and expensive metal resources are not suitable for wide application in industry.

Method used

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  • Method for preparing dimethyl furan-2,5-dicarboxylate
  • Method for preparing dimethyl furan-2,5-dicarboxylate
  • Method for preparing dimethyl furan-2,5-dicarboxylate

Examples

Experimental program
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Effect test

Embodiment 1

[0061] 1. Preparation of non-noble metal catalyst Mn-N / C:

[0062] (1) Prepare non-precious metal salt impregnation solution: take pyridine and manganese acetate with a mass ratio of 3:2, add them to 30mL of methanol, and stir thoroughly for 1h;

[0063] (2) Add nitrogen-containing carrier urea to the non-precious metal salt impregnating solution configured in step (1), wherein the mass ratio of nitrogen-containing carrier urea to the manganese acetate added in step (1) is 10:2, fully impregnated;

[0064](3) Drying the non-precious metal salt impregnating solution impregnated with the nitrogen-containing carrier obtained in step (2) at 60° C., and loading the non-noble metal complex precursor;

[0065] (4) in N 2 Under the atmosphere, pyrolyze the non-noble metal-loaded complex precursor obtained in step (3). The pyrolysis condition is to raise the temperature to 800 °C at a rate of 10 °C / min, and keep it at this temperature for 2 hours to obtain a non-noble metal catalyst. ...

Embodiment 2

[0071] 1. Preparation of non-precious metal catalyst Fe-N / C:

[0072] (1) Prepare non-precious metal salt impregnation solution: take imidazole and ferric sulfate with a mass ratio of 3:4, add them to 40mL of methanol, and stir thoroughly for 1h;

[0073] (2) Add nitrogen-containing carrier melamine to the non-precious metal salt impregnating solution configured in step (1), wherein the mass ratio of nitrogen-containing carrier melamine to the ferric sulfate added in step (1) is 10:2, fully impregnated;

[0074] (3) Drying the non-precious metal salt impregnating solution impregnated with the nitrogen-containing carrier obtained in step (2) at 60° C., and loading the non-noble metal complex precursor;

[0075] (4) Under an Ar atmosphere, pyrolyze the non-noble metal-loaded complex precursor obtained in step (3). The temperature was kept for 2 hours to obtain the non-noble metal catalyst Fe-N / C.

[0076] 2. Oxidative esterification of 5-hydroxymethylfurfural:

[0077] (1) Pu...

Embodiment 3

[0081] 1. Preparation of non-precious metal catalyst Co-N / C:

[0082] (1) Prepare non-precious metal salt impregnation solution: take 1,10-phenanthroline and cobalt nitrate with a mass ratio of 1:1, add them to 50mL of methanol, and stir thoroughly for 1h;

[0083] (2) Nitrogen-containing carrier dicyandiamide is added to the non-precious metal salt impregnating solution configured in step (1), wherein the mass ratio of nitrogen-containing carrier dicyandiamide to the cobalt nitrate added in step (1) is 10: 2. Full impregnation;

[0084] (3) Drying the non-precious metal salt impregnating solution impregnated with the nitrogen-containing carrier obtained in step (2) at 60° C., and loading the non-noble metal complex precursor;

[0085] (4) in N 2 Under the atmosphere, pyrolyze the non-noble metal-loaded complex precursor obtained in step (3). The pyrolysis condition is to raise the temperature to 800° C. at a rate of 10° C. / min due to 25° C., and keep it at this temperature ...

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Abstract

The invention discloses a method for preparing dimethyl 2,5-furandicarboxylate. The method comprises the following step: in an oxidizing atmosphere, carrying out catalytic oxidation on 5-hydroxymethylfurfural in the presence of a non-noble metal catalyst to prepare the dimethyl 2,5-furandicarboxylate, wherein the non-noble metal catalyst comprises a nitrogen-containing carrier and a non-noble metal active component loaded on the nitrogen-containing carrier. According to the method, no extra alkaline additive is needed, pollution is small, the use of a noble metal catalyst is avoided, the preparation cost of the dimethyl furan-2,5-dicarboxylate is reduced, a process is simple, and the method is suitable for wide industrial application.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysis, and in particular relates to a method for preparing dimethyl 2,5-furandicarboxylate. Background technique [0002] Fossil resources are non-renewable primary energy, and the annual consumption is gradually increasing. If things go on like this, the depletion of fossil energy is inevitable. Biomass resources are widely stored on the earth, but only a small part of them are utilized. Therefore, the conversion of biomass-derived substrates into value-added platform chemicals and fuels has become one of the current scientific research priorities. [0003] Dimethyl 2,5-furandicarboxylate is an important biomass-derived platform compound with strong practicability, for example, it can be used to prepare a variety of high value-added fuels and chemicals. In the related art, dimethyl 2,5-furandicarboxylate is prepared by 5-hydroxymethylfurfural (HMF). Not only is the preparation process compl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68B01J27/24B01J37/02B01J37/08
CPCC07D307/68B01J27/24B01J37/0201B01J37/082
Inventor 徐杰张美云马红高进刘鑫张树静罗杨
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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