Method for electrochemical synthesis of cyclic carbonate and application of method

A cyclic carbonate, electrochemical technology, applied in the electrolysis process, electrolysis components, electrolysis organic production and other directions, can solve the problem of harsh reaction conditions and so on

Active Publication Date: 2020-12-22
HUNAN INSTITUTE OF ENGINEERING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although the development and use of traditional synthesis methods and catalysts have been developed to a certain extent, the reaction conditions are harsh.

Method used

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  • Method for electrochemical synthesis of cyclic carbonate and application of method
  • Method for electrochemical synthesis of cyclic carbonate and application of method
  • Method for electrochemical synthesis of cyclic carbonate and application of method

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preparation example Construction

[0024] The invention provides a kind of preparation method of cyclic carbonate, comprises the following steps:

[0025] The method uses a graphite rod as a working electrode, a Pt ring as an auxiliary electrode, a silver wire as a reference electrode, tetrabutylammonium perchlorate as a supporting electrolyte, and dimethylformamide as an electrolyte. The second catalyst is obtained by catalyzing the electrochemical addition of carbon dioxide and alkylene oxide. The reaction is carried out at normal temperature and pressure. The obtained product is extracted three times by adding water and dimethyl ether, and then evaporated to obtain a cyclic carbonate;

[0026] Preparation of reference electrode: Weigh 0.0169g of nitrate (AgNO3) and dissolve it in 10mL of dimethylamide (DMF), stir to dissolve it completely, and then transfer it to the reference electrode fixed with silver wire, soak the electrode in Stay overnight in the solution configured above to stabilize the reference el...

Embodiment 1

[0064] Product preparation: Weigh 1g of tetrabutylammonium perchlorate (TBAP) and dissolve it in dimethylformamide (DMF), transfer it to a 50mL volumetric flask and constant volume, add the above electrolyte solution into the H-type electrolytic cell with a pipette gun There are two chambers, Yin and Yang, and the volume of each chamber is 10mL. The working electrode and reference electrode are placed in the cathode chamber, and the auxiliary electrode is placed in the anode chamber. High-purity nitrogen gas is introduced into the two chambers of the electrolytic cell for 15 minutes to remove dissolved oxygen. Add 50mg of complex 1 and 50mg of complex 3 to the cathode chamber of the H-type electrolytic cell, respectively, and epichlorohydrin with a molar ratio of 1:5000 to the first catalyst, feed 0.1MPa carbon dioxide for 20min, and set the electrolysis voltage -2V, Electrolysis time 2h.

[0065] Product extraction: transfer the above electrolysis product into a separatory fu...

Embodiment 2

[0070] Product preparation: Weigh 2g of tetrabutylammonium perchlorate (TBAP) and dissolve it in dimethylformamide (DMF), transfer it to a 50mL volumetric flask and constant volume, add the above electrolyte solution into the H-type electrolytic cell with a pipette gun There are two chambers, Yin and Yang, and the volume of each chamber is 10mL. The working electrode and reference electrode are placed in the cathode chamber, and the auxiliary electrode is placed in the anode chamber. High-purity nitrogen gas is introduced into the two chambers of the electrolytic cell for 15 minutes to remove dissolved oxygen. Add 100mg of complex 1 and 100mg of complex 4 to the cathode chamber of the H-type electrolytic cell, and epoxycyclopentane with a molar ratio of 1:50000 to the first catalyst, feed 8MPa carbon dioxide for 20min, and set the electrolysis voltage to -2.5V , Electrolysis time 2h.

[0071] Product extraction: transfer the above electrolysis product into a separatory funnel,...

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Abstract

The invention provides a method for electrochemical synthesis of cyclic carbonate and application of the method. According to the method, a graphite rod is used as a working electrode, a Pt ring is used as an auxiliary electrode, a silver wire is used as a reference electrode, tetrabutylammonium perchlorate is used as a supporting electrolyte, and dimethylformamide is used as an electrolyte. Electrochemical addition is conducted on carbon dioxide and alkylene oxide under the catalysis of a first catalyst and a second catalyst, water and dimethyl ether are added into the obtained product afterthe reaction is completed, and extracting and evaporating are conducted to obtain cyclic carbonate. The first catalyst is 3,7,12,17-tetramethyl-8,13-divinyl-2,18-porphinediformic acid, and the secondcatalyst is 5,10,15,20-tetraphenylporphyrin. By changing a metal center and a porphyrin ring ligand and combining an electrochemical synthesis reaction, a carbon dioxide cycloaddition reaction is efficiently catalyzed under mild conditions, so that the efficiency of the carbon dioxide cycloaddition reaction is improved; and the method has the characteristics of high conversion efficiency and mildreaction conditions.

Description

technical field [0001] The present invention relates to a method for synthesizing organic compounds and its application, in particular to a method for electrochemically synthesizing cyclic carbonate and its reference. Background technique [0002] Carbon dioxide, the main emission from fossil fuel combustion, is one of the greenhouse gases that contribute to global warming. With the development of the industrial revolution and the extensive use of fossil fuels, the concentration of carbon dioxide in the atmosphere is increasing. In 2019, the global carbon dioxide level is close to the highest level on record. At the same time, carbon dioxide can also be used as a renewable carbon resource that is ubiquitous in nature, non-toxic, cheap, and inexhaustible. In recent years, carbon dioxide has been increasingly regarded as an important raw material in a chemical process. Through chemical fixation and conversion into chemical products, it can not only meet human needs for raw ma...

Claims

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Application Information

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IPC IPC(8): C25B3/00
CPCC25B3/00
Inventor 沈静周亮方正军兰东辉王佳胡伟肖恒肖甘罗刘文皓
Owner HUNAN INSTITUTE OF ENGINEERING
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