A method for electrosynthesizing 2,5-furandicarboxylic acid and 2,5-dimethyloltetrahydrofuran in pairs with a vanadium nitride-based catalyst

A technology of dimethyloltetrahydrofuran and vanadium nitride-based catalysts, which is applied in chemical instruments and methods, physical/chemical process catalysts, electrodes, etc., can solve the problems of low catalyst cost, complex production process, and high reaction efficiency, and achieve production The process is simple, the conversion rate of raw materials is high, and the selectivity is good

Active Publication Date: 2021-02-09
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a paired electrosynthesis of vanadium nitride-based catalysts in order to overcome the problems of high cost of raw materials and catalysts, complex production processes, and environmental pollution in the existing FDCA and DHMTHF synthesis processes. The method of 5-furandicarboxylic acid and 2,5-dimethyloltetrahydrofuran, 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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  • A method for electrosynthesizing 2,5-furandicarboxylic acid and 2,5-dimethyloltetrahydrofuran in pairs with a vanadium nitride-based catalyst
  • A method for electrosynthesizing 2,5-furandicarboxylic acid and 2,5-dimethyloltetrahydrofuran in pairs with a vanadium nitride-based catalyst
  • A method for electrosynthesizing 2,5-furandicarboxylic acid and 2,5-dimethyloltetrahydrofuran in pairs with a vanadium nitride-based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1: the synthesis of VN catalyst and 10%Pd / VN catalyst and its use in paired electrosynthesis system FDCA and DHMTHF

[0044] 1) Dissolve 234 mg of ammonium metavanadate in 40 mL of water, stir at room temperature for 30 min, and the amount of ammonium metavanadate added is 2 mmol;

[0045] 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;

[0046] 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 at room temperature for 30 min. Obtain precursor solution;

[0047] 4) Move the precursor solution in step 3) into a hydrothermal kettle, and conduct a hydrothermal reaction at 160°C for 8 hours. After the reaction, cool to room tem...

Embodiment 2

[0062] Example 2: Synthesis of VN catalyst and its electrocatalytic oxidation of HMF to prepare FDCA

[0063] 1) Dissolve 176 mg of ammonium metavanadate in 40 mL of water, stir at room temperature for 30 min, and the amount of ammonium metavanadate added is 1.5 mmol;

[0064] 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;

[0065] 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 minutes, slowly add 1 mL of the aqueous solution of hydrazine hydrate obtained in step 2) dropwise, and continue stirring for 30 minutes at room temperature. Obtain precursor solution;

[0066] 4) Transfer the precursor solution in step 3) into a hydrothermal kettle, and conduct a hydrothermal reaction at 120°C for 12 hours. After the reaction, cool to room temperature and filter with suc...

Embodiment 3

[0074] Example 3: Synthesis of 10% Pd / VN catalyst and its electrocatalytic reduction of HMF to DHMTHF

[0075] 1) Dissolve 351 mg of ammonium metavanadate in 40 mL of water, stir at room temperature for 30 min, and the amount of ammonium metavanadate added is 3 mmol;

[0076] 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;

[0077] 3) Take 3 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 4 mL of the aqueous solution of hydrazine hydrate obtained in step 2) dropwise, and continue stirring at room temperature for 30 min. Obtain precursor solution;

[0078] 4) Transfer the precursor solution in step 3) into a hydrothermal kettle, and conduct a hydrothermal reaction at 180°C for 5 hours. After the reaction, cool to room temperature and filter with suction. The...

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Abstract

The invention discloses a method for electrosynthesizing 2,5-furandicarboxylic acid and 2,5-dimethyloltetrahydrofuran in pairs with a vanadium nitride-based catalyst. It adopts an H-type electrolytic cell for reaction, and the vanadium nitride catalyst is coated with Coated on nickel foam as the electrode of the anode chamber, 5-hydroxymethylfurfural was dissolved in alkaline solution as the anolyte; the palladium vanadium nitrogen catalyst was coated on the carbon cloth as the electrode of the cathode chamber, and 5-hydroxymethylfurfural Dissolved in an acidic solution as catholyte, at a temperature of 25-60°C, a current of 5-50 mA, and a cell voltage of 1-20 V, a paired electrosynthesis reaction is carried out, and the reaction time is 0.5-3 hours. 2,5-furandicarboxylic acid and 2,5-dimethyloltetrahydrofuran are obtained through treatment. The conditions of the paired electrosynthesis process of the present invention are mild, the conversion rate of raw materials is high, and the selectivity is good. Compared with the precious metals commonly used in the prior art Catalyst and single-tank synthesis technology, the vanadium nitride-based catalyst used in the present invention has low cost, and the energy utilization rate of the paired electrosynthesis technology is high.

Description

technical field [0001] The present invention relates to a method for synthesizing organic chemical products, in particular to a method for electrosynthesizing 2, 5-furandicarboxylic acid and 2, 5-dimethyloltetrahydrofuran in pairs with a vanadium nitride-based catalyst. Background technique [0002] 2, 5-Dihydroxymethylfurfural (HMF) is one of the intermediate products of cellulose degradation, which is produced by direct dehydration of glucose or fructose by acidic substances. It is rich in sources, has a wide range of chemical application prospects, and is considered to be one of the most useful basic chemicals. In addition, HMF is a substance acting as a mediator in the corresponding alcohols and acids, and can be used to derive many high value-added furan chemical products through chemical reactions such as catalytic hydrogenation, oxidative dehydrogenation, esterification, and halogenation. In particular, it can be hydrogenated to 2,5-dimethylolfuran (DHMF), 2,5-dimeth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/23C25B3/25C25B3/05C25B3/07C25B11/052C25B11/061C25B11/091B01J27/24
CPCB01J27/24C25B3/23C25B3/25C25B11/091
Inventor 钟兴李随勤王建国
Owner ZHEJIANG UNIV OF TECH
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