Method for preparing 2,5-furandicarboxylic acid through electrocatalytic oxidation by using nickel-vanadium phosphide catalyst

A technology of electrocatalytic oxidation and furandicarboxylic acid, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of complex production process, high catalyst cost, and high reaction efficiency, and achieve raw material conversion High efficiency, high product yield, good selectivity

Active Publication Date: 2019-06-04
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide an electrocatalytic oxidation of 5-hydroxymethylfurfural (HMF) to overcome the problems of high raw material and catalyst cost, complex production process, and environmental pollution in the existing FDCA synthesis process. 2,5-furandicarboxylic acid (FDCA) method, 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 preparing 2,5-furandicarboxylic acid through electrocatalytic oxidation by using nickel-vanadium phosphide catalyst
  • Method for preparing 2,5-furandicarboxylic acid through electrocatalytic oxidation by using nickel-vanadium phosphide catalyst
  • Method for preparing 2,5-furandicarboxylic acid through electrocatalytic oxidation by using nickel-vanadium phosphide catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: Synthesis of NiVP / NF catalyst and its electrocatalytic oxidation of HMF to prepare FDCA

[0035] (1) According to the feeding ratio, 291 mg of nickel nitrate and 117 mg of ammonium metavanadate were dissolved in 40 mL of water, and ultrasonically dispersed at room temperature for 30 minutes, called A solution;

[0036] (2) Combine the solution A in step (1) and the nickel foam carrier (the size is about 2 × 4 cm 2 ) into a hydrothermal kettle, after hydrothermal reaction at 120°C for 12 hours, cool to room temperature, take out nickel foam, wash twice with distilled water and ethanol alternately, and vacuum dry at 60°C to obtain a supported catalyst;

[0037] (3) Place the dried supported catalyst in step (2) in a tube furnace, place 500 mg of sodium phosphate upstream of the catalyst, and bake at 400°C for 2 hours in an atmosphere of nitrogen gas, then cool to room temperature, the nickel vanadium phosphide catalyst is obtained, marked as NiVP / NF, and its S...

Embodiment 2

[0043] Example 2: Synthesis of NiV / NF catalyst and its electrocatalytic oxidation of HMF to prepare FDCA

[0044] (1) According to the feeding ratio, 291 mg of nickel nitrate and 117 mg of ammonium metavanadate were dissolved in 40 mL of water, and ultrasonically dispersed at room temperature for 30 minutes, called A solution;

[0045] (2) Combine the solution A in step (1) and the nickel foam carrier (the size is about 2 × 4 cm 2 ) into a hydrothermal kettle, reacted hydrothermally at 140°C for 10 hours, cooled to room temperature, took out the nickel foam, washed it twice with distilled water and ethanol alternately, and dried it in vacuum at 60°C to obtain the nickel vanadium compound Catalyst, labeled NiV / NF.

[0046] The catalytic performance of the NiV / NF catalyst prepared in embodiment 2 is tested, and the specific method is as follows:

[0047] Cut the NiV / NF catalyst to about 2 × 2 cm 2 size, directly as the working electrode. The current is controlled by a galvan...

Embodiment 3

[0051] Example 3: Synthesis of NiP / NF catalyst and its electrocatalytic oxidation of HMF to prepare FDCA

[0052] (1) Dissolve 582 mg nickel nitrate in 40 mL water and ultrasonically disperse at room temperature for 30 minutes, called A solution;

[0053] (2) Combine the solution A in step (1) and the nickel foam carrier (the size is about 2 × 4 cm 2 ) into a hydrothermal kettle, reacted hydrothermally at 160°C for 6 hours, cooled to room temperature, took out the nickel foam, washed it twice with distilled water and ethanol alternately, and vacuum-dried at 60°C to obtain a supported catalyst;

[0054] (3) Place the dried supported catalyst in step (2) in a tube furnace, place 500 mg of sodium hypophosphite upstream of the catalyst, and bake it at 300°C for 1.5 hours under an atmosphere of argon. , cooled to room temperature to obtain the nickel phosphide catalyst, marked as NiP / NF.

[0055] The catalytic performance of the NiP / NF catalyst prepared in embodiment 3 is tested,...

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Abstract

The invention relates to a method for preparing 2,5-furandicarboxylic acid by electrocatalytic oxidation of a nickel-vanadium phosphide catalyst. A reaction is carried out in an H-shaped electrolyticcell; in an anode chamber, the nickel-vanadium phosphide catalyst servers as a working electrode, and 5-hydroxymethylfurfural, serving as a reaction substrate, is dissolved in an alkaline solution toform an anode solution; in a cathode chamber, a platinum sheet is used as a counter electrode, and an alkaline solution is used as a cathode solution, so that an electrocatalytic oxidation reaction iscarried out for 0.5-3 h under the conditions that the temperature is 20-60 DEG C, the current is 5-50 mA and the cell voltage is 1-20 V; and after the reaction is finished, post-treatment is carriedout to obtain the 2,5-furandicarboxylic acid. The electrocatalytic oxidation reaction process of the method is mild in condition, so that the method is green and pollution-free, the raw material conversion rate is high, the FDCA selectivity is good, and the Faraday efficiency is high. Compared with precious metal catalysts commonly adopted in the prior art, the transition metal nickel-vanadium phosphide catalyst used in the method is low in cost, so that consumption of rare precious metal is avoided.

Description

technical field [0001] The invention relates to a synthesis method of organic chemical products, in particular to a method for preparing 2,5-furandicarboxylic acid by electrocatalytic oxidation of a nickel vanadium phosphide catalyst. Background technique [0002] 2,5-furandicarboxylic acid (FDCA) is a furan dibasic acid, which is a bio-based chemical product extracted from lignocellulose. It is an important intermediate in organic synthesis and is widely used in the synthesis of chiral Catalysts and polymer materials, and also used in food and cosmetic flavors. In addition, FDCA is similar in structure to terephthalic acid, and is considered to be an ideal substitute for petroleum-based monomer terephthalic acid, which is used in high polymers such as synthetic plastics. In addition, due to the development of many new uses of FDCA in recent years, the market demand continues to increase. [0003] At present, most of FDCA is prepared by heterogeneous catalytic oxidation of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/02C25B11/06B01J27/198C25B3/23
Inventor 钟兴李随勤王建国谷雨蒋文斌
Owner ZHEJIANG UNIV OF TECH
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