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Method for producing 2,5-dimethyloltetrahydrofuran by electrocatalytic reduction of biomass compounds with a vanadium-based catalyst

A technology of dimethyloltetrahydrofuran and catalysts, which is applied in chemical instruments and methods, physical/chemical process catalysts, and electrolytic organic production. The effect of high conversion rate and avoiding large consumption

Active Publication Date: 2020-01-14
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide an electrocatalytic reduction of furan to replace the existing 2,5-dimethyloltetrahydrofuran (DHMTHF) in order to overcome the problems of high cost of raw materials and catalysts and complicated production process existing in the existing 2,5-dimethyloltetrahydrofuran (DHMTHF) synthesis process. The method for the preparation of DHMTHF, the process is green and environmentally friendly, the production process is simple, the catalyst cost is low, and the reaction efficiency is high

Method used

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  • Method for producing 2,5-dimethyloltetrahydrofuran by electrocatalytic reduction of biomass compounds with a vanadium-based catalyst
  • Method for producing 2,5-dimethyloltetrahydrofuran by electrocatalytic reduction of biomass compounds with a vanadium-based catalyst
  • Method for producing 2,5-dimethyloltetrahydrofuran by electrocatalytic reduction of biomass compounds with a vanadium-based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1: Synthesis of 10%Pd / VN catalyst and its electrocatalytic reduction of HMF to DHMTHF

[0041] (1) Dissolve 234 mg of ammonium metavanadate in 40 mL of water and stir for 30 min at room temperature, the amount of ammonium metavanadate added is 2 mmol;

[0042] (2) Prepare a hydrochloric acid solution with a concentration of 1 mol / L, and prepare an 8 mol / L aqueous solution of hydrazine hydrate for later use;

[0043] (3) Take 1 mL of the hydrochloric acid solution obtained in step (2) and slowly add it dropwise to the solution obtained in step (1). After stirring at room temperature for 10 min, slowly add 2 mL of the aqueous solution of hydrazine hydrate obtained in step (2) dropwise, and Continue stirring for 30 min to obtain a precursor solution;

[0044] (4) Transfer the precursor solution in step (3) into a hydrothermal kettle, and conduct a hydrothermal reaction at 160 °C for 8 h. After the reaction, cool to room temperature and filter with suction. After t...

Embodiment 2

[0055] Example 2: Synthesis of 5%Pd / VN catalyst and its electrocatalytic reduction of HMF to DHMTHF

[0056] (1) Dissolve 368 mg of sodium orthovanadate in 40 mL of water, stir at room temperature for 30 min, and add 2 mmol of sodium orthovanadate;

[0057] (2) Prepare a hydrochloric acid solution with a concentration of 2 mol / L and a 5 mol / L aqueous solution of hydrazine hydrate for later use;

[0058] (3) Take 1 mL of the hydrochloric acid solution obtained in step (2) and slowly add it dropwise to the solution obtained in step (1). After stirring at room temperature for 10 min, slowly add 2 mL of the aqueous solution of hydrazine hydrate obtained in step (2) dropwise, and Continue stirring for 30 min to obtain a precursor solution;

[0059] (4) Transfer the precursor solution in step (3) into a hydrothermal kettle, and conduct a hydrothermal reaction at 120 °C for 12 h. After the reaction, cool to room temperature and filter with suction. After the filter residue is altern...

Embodiment 3

[0067] Example 3: Synthesis of 1%Pd / VN catalyst and its electrocatalytic reduction of HMF to DHMTHF

[0068] (1) Dissolve 244 mg of sodium metavanadate in 40 mL of water, stir at room temperature for 30 min, and add 2 mmol of sodium metavanadate;

[0069] (2) Prepare a hydrochloric acid solution with a concentration of 1 mol / L and a 5 mol / L aqueous solution of hydrazine hydrate for later use;

[0070] (3) Take 1 mL of the hydrochloric acid solution obtained in step (2) and slowly add it dropwise to the solution obtained in step (1). After stirring at room temperature for 10 min, slowly add 2 mL of the aqueous solution of hydrazine hydrate obtained in step (2) dropwise, and Continue stirring for 30 min to obtain a precursor solution;

[0071] (4) Transfer the precursor solution in step (3) into a hydrothermal kettle, and conduct a hydrothermal reaction at 180 °C for 6 h. After the reaction, cool to room temperature and filter with suction. After the filter residue is alternate...

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Abstract

The present invention disclosed a method of reducing the method of electrocatalysting biomassized biomassized compounds of cymbal -based catalysts.As anode liquid; in the cathode chamber, the cymbal catalyst is applied on the carbon cloth as the working electrode, and the biomass type is used as the reaction substrate to dissolve in the acid solution as the cathode solution.10‑50 mA, the groove voltage is 1 10 V, the electrical catalytic reaction is performed, the reaction time is 0.3‑3h, and after the reaction is over, the reaction liquid is treated with 2,5‑ dihydroxytal hydrogenidfirus (DHMTHF).The process method of the present invention, the conditions of the electrical catalytic reaction process are mild, green without pollution, high raw material conversion rate, DHMTHF is better selectively. Compared with the precious metal catalysts commonly used in existing technology, the cost of cymbal catalyst used in the invention is comparedLow.

Description

technical field [0001] The invention relates to a method for synthesizing organic chemical products, in particular to a method for preparing 2,5-dimethyloltetrahydrofuran by electrocatalyzing reduction of biomass compounds with a vanadium-based catalyst. Background technique [0002] 2,5-Dihydroxymethyltetrahydrofuran (DHMTHF) is a high value-added chemical substance. Because DHMTHF is easy to degrade, has low toxicity and is more stable than other unsaturated furan compounds, it is often used as a solvent for special reactions. It has been reported elsewhere It is clearly pointed out that DHMTHF can be used and converted into some linear polyols, such as 1, 5-pentanediol, 1, 6-hexanediol, etc., and then used to synthesize some polymers and special chemicals. The reaction of preparing 2,5-dimethyloltetrahydrofuran from sugars (mainly glucose and fructose) is still mainly in the stage of multi-step reaction system and biphasic system research, and because the reaction is a mu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/04B01J27/24B01J35/08B01J35/10C25B3/25
Inventor 钟兴李随勤王建国郑海洋
Owner ZHEJIANG UNIV OF TECH
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