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A kind of method for preparing cyclohexanol and cyclohexanone by electrochemical catalytic oxidation of cyclohexane

A technology of catalytic oxidation and cyclohexane, which is applied in the direction of electrolysis process, electrolysis components, electrolysis organic production, etc., can solve the problems of separation of reactants and products, high energy consumption, hindering new reactions, etc., to achieve high efficiency and high selectivity, The process is simple and the effect of promoting high efficiency

Inactive Publication Date: 2016-06-15
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0028] Although organic electrochemistry has its unique features, there are also some shortcomings: (1) Electrochemical synthesis cannot separate reactants and products in time after the reaction, which will lead to side reactions such as further oxidation of products, Ultimately affect the selectivity of the reaction and the yield of the target product; (2) The reactant can only be transferred from the solution body to the electrode surface by the action of the electric field, and then the electrochemical reaction occurs, and the product cannot leave the electrode surface in time after the reaction is completed. This hinders the progress of new reactions, so organic electrochemical synthesis still has the problems of low current efficiency and high energy consumption.
However, cyclohexane is a non-polar organic compound, insoluble in water, and it is usually difficult to undergo electrochemical oxidation reactions in aqueous systems

Method used

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  • A kind of method for preparing cyclohexanol and cyclohexanone by electrochemical catalytic oxidation of cyclohexane
  • A kind of method for preparing cyclohexanol and cyclohexanone by electrochemical catalytic oxidation of cyclohexane
  • A kind of method for preparing cyclohexanol and cyclohexanone by electrochemical catalytic oxidation of cyclohexane

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Effect test

Embodiment 1

[0055] The porous titanium-based electrocatalytic membrane loaded with titanium dioxide is used as the anode, and the auxiliary electrode is used as the cathode to form an electrocatalytic membrane reactor;

[0056] The reaction raw material solution is prepared by the following method: the acetic acid solution of cyclohexane is placed in a membrane reactor, and an aqueous electrolyte solution (NaCl solution) is added thereto to obtain a completely miscible homogeneous transparent solution, wherein, in the reaction raw material solution, cyclohexane The volume ratio of alkane to acetic acid is 1:0.5, the concentration of electrolyte NaCl is 5.0g / L, and the concentration of cyclohexane is 0.1mol / L;

[0057] Under normal temperature and pressure, the working voltage is 3.0V, and the current density is 1.0mA / cm 2 Under certain conditions, the porous titanium-based electrocatalytic membrane loaded with titanium dioxide is used to catalyze the oxidation of cyclohexane to synthesize...

Embodiment 2

[0060] The porous titanium-based electrocatalytic membrane loaded with manganese oxide is used as the anode, and the auxiliary electrode is used as the cathode to form an electrocatalytic membrane reactor;

[0061] The reaction raw material solution is prepared by the following method: the propionic acid solution of cyclohexane is placed in a membrane reactor, and the aqueous solution (NaOH solution) of electrolyte is added thereto to obtain a completely miscible homogeneous transparent solution, wherein, in the reaction raw material solution, cyclohexane The volume ratio of hexane to propionic acid is 1:5, the concentration of electrolyte NaOH is 2.0g / L, and the concentration of cyclohexane is 0.05mol / L;

[0062] Under normal temperature and pressure, the working voltage is 4.0V, and the current density is 2.0mA / cm 2 Under certain conditions, the porous titanium-based electrocatalytic membrane loaded with manganese oxide is used to catalyze the oxidation of cyclohexane to syn...

Embodiment 3

[0065] The porous nickel-based electrocatalytic membrane loaded with vanadium oxide is used as the anode, and the auxiliary electrode is used as the cathode to form an electrocatalytic membrane reactor;

[0066] The reaction raw material solution is prepared by the following method: the acetonitrile solution of cyclohexane is placed in a membrane reactor, and the aqueous solution of the electrolyte (NaNO 3 solution) to obtain a completely miscible homogeneous transparent solution, wherein, in the reaction raw material solution, the volume ratio of cyclohexane to acetonitrile is 1:1, and the electrolyte NaNO 3 The concentration of cyclohexane is 15.0g / L, and the concentration of cyclohexane is 1.0mol / L;

[0067] Under normal pressure, the reaction temperature is 10°C, the working voltage is 4.0V, and the current density is 3.0mA / cm 2 Under the conditions, the porous nickel-based electrocatalytic membrane loaded with vanadium oxide catalyzes the oxidation of cyclohexane to synt...

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Abstract

The invention discloses a method for synthesizing cyclohexanol and cyclohexanone by electrochemically catalytically oxidizing cyclohexane and belonging to the technical field of organic electrochemical synthesis. The porous metal electrocatalytic membrane loaded with metal oxide is used as the anode, and the auxiliary electrode is used as the cathode to form an electrocatalytic membrane reactor; the reaction raw material solution is a mixed aqueous solution of cyclohexane, organic solvent and electrolyte, under certain operating voltage and current density conditions Under the conditions, cyclohexane is catalyzed and oxidized to the products cyclohexanol and cyclohexanone on the surface of the membrane and in the pores by the metal oxide supported on the membrane. It is pumped to the permeate side to achieve real-time online separation or transfer, and then the membrane permeate is separated and purified to finally obtain the products cyclohexanol and cyclohexanone. Compared with traditional techniques, the invention has the advantages of high efficiency, greenness, high selectivity, simple operation, etc., is suitable for industrial implementation, and has broad application prospects.

Description

technical field [0001] The invention belongs to the technical field of organic electrochemical synthesis, in particular to a method for synthesizing cyclohexanol and cyclohexanone by electrochemically catalyzing cyclohexane oxidation. Background technique [0002] Cyclohexanol and cyclohexanone are extremely important chemical raw materials, and are necessary intermediates for the production of caprolactam and adipic acid. The preparation of cyclohexanol / ketone by liquid-phase cyclohexane oxidation is an industrially very important and commercially valuable chemical synthesis method. At present, the methods for synthesizing and preparing cyclohexanol / ketone at home and abroad are mainly cyclohexane oxidation. The cyclohexane oxidation method is divided into non-catalytic oxidation method and catalytic oxidation method, and the catalytic oxidation method is divided into photocatalytic oxidation method, boric acid catalyst oxidation method, cobalt salt catalytic oxidation met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/02C25B3/23
Inventor 李建新王虹方肖尹振康建立
Owner TIANJIN POLYTECHNIC UNIV
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