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Method for producing hydrogen by coupling dicarboxylic acid prepared by electrocatalytic oxidation of cyclic alcohol/cyclic ketone

An electrocatalytic oxidation and dicarboxylic acid technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, electrolytic organic production, etc., can solve problems such as environmental pollution, corrosive reaction equipment, and non-compliance with green chemistry, and achieve product The effect of high yield and broad application range

Active Publication Date: 2021-12-24
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses a strong acid as an oxidant, which is easy to corrode the reaction equipment, and the nitrogen oxide by-products produced by the reaction also pollute the environment, which does not meet the requirements of green chemistry.

Method used

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  • Method for producing hydrogen by coupling dicarboxylic acid prepared by electrocatalytic oxidation of cyclic alcohol/cyclic ketone
  • Method for producing hydrogen by coupling dicarboxylic acid prepared by electrocatalytic oxidation of cyclic alcohol/cyclic ketone
  • Method for producing hydrogen by coupling dicarboxylic acid prepared by electrocatalytic oxidation of cyclic alcohol/cyclic ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The carbon cloth was sonicated in analytically pure absolute ethanol, analytically pure acetone, and deionized water for 15 minutes to remove surface impurities. Prepare 25mL of an aqueous solution containing 1.5g of urea, 0.9g of ammonium tetrafluoride and 0.5g of nickel nitrate as a hydrothermal reaction solution, soak the carbon cloth in the prepared hydrothermal reaction solution, and react at a constant temperature of 110°C for 8 hours, removed, washed with deionized water and dried to obtain the precursor material. The prepared precursor material was put into a quartz boat together with 100 mg of sodium hypophosphite and transferred into a tube furnace. Phosphating at 300° C. for 2 hours under an argon atmosphere to obtain a porous network nickel phosphide nano-electrocatalyst. The scanning electron microscope image of the porous network nickel phosphide nano-electrocatalyst is shown in figure 2 middle.

[0034] Prepare 20mL of 1M potassium hydroxide solution ...

Embodiment 2

[0036] Sonicate the nickel foam in analytically pure absolute ethanol, analytically pure acetone, and deionized water for 15 minutes to remove surface impurities. Prepare 25mL of the urea that comprises 1.5g, the ammonium tetrafluoride of 0.9g, the cobalt nitrate of 0.5g and the aqueous solution of the nickel nitrate of 0.5g as hydrothermal reaction solution, nickel foam is soaked in the hydrothermal reaction solution of configuration, in React at a constant temperature of 120° C. for 8 hours, take it out, wash with deionized water and dry to obtain a precursor material. The prepared precursor was put into a quartz boat together with 100 mg of potassium hypophosphite and transferred into a tube furnace. Phosphating at 300° C. for 2 hours under an argon atmosphere to obtain cobalt-nickel phosphide nano-electrocatalysts.

[0037]Prepare 20 mL of 1 M potassium hydroxide solution containing 1 mg of cyclohexanone as the electrolyte, use the cobalt-nickel phosphide nano-electrocata...

Embodiment 3

[0039] The nickel sheet was sonicated in analytically pure absolute ethanol, analytically pure acetone, and deionized water for 15 minutes to remove surface impurities. Prepare 25mL of an aqueous solution containing 1.5g of hexamethylenetetramine, 0.9g of ammonium tetrafluoride, 0.5g of cobalt nitrate and 0.2g of manganese nitrate as a hydrothermal reaction solution, and soak the nickel sheet in the configured hydrothermal reaction solution. The reaction liquid was reacted at a constant temperature of 120° C. for 8 hours, taken out, washed with deionized water and dried to obtain a precursor material. The prepared precursor material was put into a quartz boat together with 100mg of red phosphorus and transferred into a tube furnace. Phosphating at 350° C. for 2 hours under an argon atmosphere to obtain cobalt-manganese phosphide nano-electrocatalysts.

[0040] Prepare 20 mL of 1 M potassium hydroxide solution containing 1 mg of cyclopentanol as the electrolyte, use the cobalt...

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Abstract

The invention relates to a method for producing hydrogen by coupling dicarboxylic acid prepared by electrocatalytic oxidation of cyclic alcohol / cyclic ketone, which comprises the specific steps of using a transition metal phosphide nano electrocatalyst as a cathode catalyst and an anode catalyst respectively, and adding cyclic alcohol / cyclic ketone into an electrolyte aqueous solution to assemble an electrolytic tank; and carrying out constant-voltage reaction for 1-20 hours at the voltage of 0.3-10V. Compared with the traditional process for preparing dicarboxylic acid by oxidizing cyclic alcohol / cyclic ketone with nitric acid, the method has the advantages that the transition metal phosphide nano electrocatalyst prepared by a simple method is used as an anode and a cathode, and the dicarboxylic acid is directly synthesized by applying constant voltage at room temperature and normal pressure, so that toxic and harmful gases such as N2O are not generated, and hydrogen co-production is realized. Meanwhile, the application range of the transition metal phosphide electrode material in the field of electrocatalytic organic synthesis is widened.

Description

technical field [0001] The invention relates to the technical field of electrocatalytic organic synthesis and hydrogen production, in particular to a method for electrocatalytically oxidizing cyclic alcohols / cyclic ketones to prepare dibasic carboxylic acid coupled hydrogen production. Background technique [0002] Hydrogen energy is recognized as a clean energy source and is emerging as a low-carbon and zero-carbon energy source. The development of new energy is imminent in today's world. The reason is that the energy used, such as oil, natural gas, coal, and petroleum gas, are non-renewable resources. The stock on the earth is limited, and human survival is always inseparable from energy. Therefore, new energy must be found. With the increasing consumption of fossil fuels, their reserves are decreasing, and one day, these resources and energy will be exhausted, so there is an urgent need to find a new energy containing energy that does not rely on fossil fuels and has abun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/23C25B3/07C25B1/02C25B11/075B01J27/185B01J37/10B01J37/28
CPCC25B1/02B01J27/1853B01J37/10B01J37/28B01J35/23B01J35/33Y02E60/36
Inventor 段昊泓栗振华周华李晓帆孔祥贵
Owner TSINGHUA UNIV
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