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Method for preparing enol by electrocatalytic selective hydrogenation of alkynol

A selectivity and hydrogen preparation technology, applied in the direction of electrodes, electrolysis process, electrolysis components, etc., can solve the problems of expensive noble metal catalysts, high reaction temperature, long reaction time, etc., to avoid excessive hydrogenation, reduce energy consumption, reduce and potential dangerous effect

Pending Publication Date: 2022-04-12
NORTHWESTERN POLYTECHNICAL UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0009] The above previous studies have shown that the selective hydrogenation of acetylenic alcohols to enols based on traditional thermocatalytic processes still has high-pressure hydrogen, high reaction temperature, expensive noble metal catalysts, low selectivity, long reaction time, high energy consumption, and many by-products. a series of questions

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  • Method for preparing enol by electrocatalytic selective hydrogenation of alkynol
  • Method for preparing enol by electrocatalytic selective hydrogenation of alkynol
  • Method for preparing enol by electrocatalytic selective hydrogenation of alkynol

Examples

Experimental program
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Effect test

Embodiment 1

[0067] (1) Preparation of Ag nanoparticle catalyst slurry: Disperse 10 mg of Ag nanoparticle catalyst powder in 6 mL of isopropanol, then add 50 μL of Nafion solution (5%), stir and ultrasonically disperse for 90 min.

[0068] (2) Spray the Ag nanoparticle slurry evenly on both sides of the conductive substrate as the cathode of the electrolytic cell, Hg / HgO as the reference electrode of the electrolytic cell, insert the working electrode and the reference electrode into the cathode chamber and fix the distance; The anode of the pool is inserted into the anode chamber and parallel to the exchange membrane; both the catholyte and the anolyte are 1M KOH solution, separated by an anion exchange membrane. Add 5 mL of the reactant 2-methyl-3-butyn-2-ol to the catholyte and expedite mass transfer through a stirrer.

[0069] (3) A split H-type electrolytic cell with a three-electrode system is used, and the electrochemical performance test is performed through an electrochemical work...

Embodiment 2

[0071] (1) Preparation of Cu nanoparticle catalyst slurry: Disperse 10 mg of Cu nanoparticle catalyst powder in 6 mL of isopropanol, then add 50 μL of Nafion solution (5%), stir and ultrasonically disperse for 90 min.

[0072] (2) Spray the Cu nanoparticle slurry evenly on the hydrophobic surface of the carbon paper as the cathode of the electrolytic cell, Hg / HgO as the reference electrode of the electrolytic cell, nickel foam as the anode of the electrolytic cell, and both the cathode and anode electrolytes are 1M KOH solution. separated by an anion exchange membrane. Add 5 mL of reactant 2-methyl-3-butyn-2-ol to the catholyte.

[0073] (3) A flow-type electrolytic cell with a three-electrode system is used, and the electrochemical performance test is carried out through an electrochemical workstation. The catalytic activity of the catalyst Cu nanoparticles was characterized by potentiostatic method. The reactant acetylenic alcohol was reacted for 1 hour, and the liquid phase ...

Embodiment 3

[0075] (1) Preparation of membrane electrode slurry: Disperse 10 mg of Cu nanoparticle catalyst powder in 6 mL of isopropanol, then add 50 μL of Nafion solution (5%), stir and ultrasonically disperse for 90 min.

[0076] (2) The Cu nanoparticle slurry is evenly sprayed on the surface of the proton exchange membrane by a precision spraying device as the cathode of the electrolytic cell, and the nickel foam is used as the anode of the electrolytic cell. Both the catholyte and the anolyte are 1M KOH solution, and an exchange membrane is used between isolation. Add 5 mL of the reactant 1,4-butynediol to the catholyte.

[0077] (3) A flow-type electrolytic cell with a two-electrode system is used, and the electrochemical performance test is carried out through an electrochemical workstation. The catalytic activity of the catalyst Cu nanoparticle membrane electrode was characterized by potentiostatic method. The reactant acetylenic alcohol was reacted for 1 hour, and the liquid pha...

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Abstract

The invention relates to a method for preparing enol by electrocatalytic selective hydrogenation of alkynol, which comprises but is not limited to terminal alkynol such as 2-methyl-3-butyne-2-ol, 1, 4-butynediol, methyl butynol, ethynyl cyclohexanol, dehydrolinalool and the like, non-terminal alkynol, cyclic alkynol, alkynodiol and the like. Different types of electrolytic tanks can be adopted; the contact resistance between a catalyst and an ion exchange membrane can be reduced by a preparation process of a membrane electrode in a flow type electrolytic tank; the split H-type electrolytic tank can control the mass transfer rate of alkynol selective hydrogenation. The method is an electro-catalysis mode which is green, safe, low in cost and high in efficiency, compared with a traditional thermal catalysis technology, the method can selectively reduce reactant alkynol into enol at the room temperature and normal pressure, water serves as a hydrogen source to replace flammable and explosive hydrogen, energy consumption and potential risks in the process can be greatly reduced, the requirement of green chemical engineering is met, and the method is suitable for industrial production. The method has great strategic significance.

Description

technical field [0001] The invention belongs to the field of selective catalytic hydrogenation, and relates to a method for preparing enol by electrocatalytic selective hydrogenation of acetylenic alcohols. Background technique [0002] As an important class of fine chemical products, enols are mainly used in the production of vitamin E, vitamin A, and carotenoid intermediates, and have been widely used in the fields of medicine, pesticides, and new materials. Due to the unclear understanding of enol structure relationship, the synthesis and development of enol compounds are severely restricted. How to synthesize enols with high conversion, high selectivity and stability has become one of the important hotspots in the study of enols. Among them, the selective hydrogenation reaction of acetylenic alcohols is not only the key to the synthesis process of vitamin E and vitamin A, but also an ideal technical route for the synthesis of enols. [0003] At present, thermal catalys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/07C25B3/25C25B11/075C25B11/081C25B11/089C25B11/031
Inventor 张健常思雨卜军
Owner NORTHWESTERN POLYTECHNICAL UNIV
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