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A method for preparing trivalent pyridinium ionic liquid by electrolysis

A pyridinium ion and electrolysis technology, applied in the field of ionic liquid preparation, can solve the problems of restricting the large-scale production of ionic liquids, unable to meet actual needs, few types of ionic liquids, etc., and achieves good application prospects, huge industrial application potential, and preparation process. Easy-to-control effects

Active Publication Date: 2020-05-01
ANQING NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few types of existing ionic liquids, which cannot meet the actual needs.
The synthesis method of traditional ionic liquid generally adopts two-step method, that is: the first step is to synthesize quaternary ammonium halide by reaction of tertiary amine and alkyl halide; This method often has disadvantages such as long reaction time, excessive use of organic solvents, difficulty in removing impurity ions, and high production costs, which seriously restrict the large-scale production of ionic liquids.

Method used

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  • A method for preparing trivalent pyridinium ionic liquid by electrolysis
  • A method for preparing trivalent pyridinium ionic liquid by electrolysis
  • A method for preparing trivalent pyridinium ionic liquid by electrolysis

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Embodiment 1

[0024] A method for preparing trivalent pyridinium ionic liquid by electrolysis. Electrolysis is carried out in an electrolytic cell including a cathode chamber and an anode chamber. A layer of perfluorinated cation exchange membrane is also arranged between the cathode chamber and the anode chamber, and a DSA shape-stable anode is used. As the anode and Pt as the cathode, add the acetonitrile solution of 4-picoline with a concentration of 1.6mol / L into the cathode chamber, add the acetonitrile solution of 0.5mol / L s-tribromobenzyl into the anode chamber, and connect the silicon Rectified power supply, the electrolysis temperature is 65°C, the current density is 2A / dm 2 Under the conditions of electrolysis for 4.5h, the catholyte was taken out after the electrolysis was completed, separated and purified to obtain 1,3,5-tris[(4-methylpyridyl)-N-methylene)]phenyl bromide salt with a purity of 90wt %.

Embodiment 2

[0026] A method for preparing trivalent pyridinium ionic liquid by electrolysis. Electrolysis is carried out in an electrolytic cell including a cathode chamber and an anode chamber. A layer of perfluorinated cation exchange membrane is also arranged between the cathode chamber and the anode chamber, and a DSA shape-stable anode is used. , Pt is the cathode, the acetonitrile solution of 4-picoline with a concentration of 1mol / L is added as the catholyte in the cathode chamber of the electrolyzer, and the acetonitrile solution of 0.6mol / L s-tribromobenzyl is used as the anolyte Put it into the anode chamber of the electrolytic cell, turn on the silicon rectifier power supply, the electrolysis temperature is 60°C, and the current density is 6A / dm 2 Under the conditions of electrolysis for 4h, the current efficiency is 46%. After the electrolysis is completed, take out the catholyte, extract it with diethyl ether, put it into a rotary evaporator after obtaining the extract, and sp...

Embodiment 3

[0029] A method for preparing trivalent pyridinium ionic liquid by electrolysis. Electrolysis is carried out in an electrolytic cell including a cathode chamber and an anode chamber. A layer of perfluorinated cation exchange membrane is also arranged between the cathode chamber and the anode chamber, and Ti-based PbO is used. 2 is the anode, Pt is the cathode, the acetonitrile solution of 4-picoline with a concentration of 2mol / L is added to the cathode chamber of the electrolytic cell as the catholyte, and the acetonitrile solution of 0.3mol / L s-tribromobenzyl is used as the anode The electrolyte is added to the anode chamber of the electrolytic cell, and the silicon rectifier power supply is connected, and the electrolysis temperature is 85°C, and the current density is 1A / dm 2 Under the conditions of electrolysis for 8 hours, the current efficiency is 35%. After the electrolysis is completed, take out the catholyte, extract it with ether, put it into a rotary evaporator to d...

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Abstract

The invention discloses a method for preparing trivalent pyridine ion liquid through an electrolytic process. At least one perfluor cation exchange film is arranged in an electrolytic cell, and divides the electrolytic cell into a cathode chamber and an anode chamber, DSA or Ti-based PbO2 serves as an anode, Pt serves as a cathode, 4-methylpyridine acetonitrile solution with the concentration being 1-2mol / L is added into the cathode chamber, a trisbenzene acetonitrile solution with the concentration being 0.3 to 0.6 mol / L is added into the cathode chamber, a silicon rectifier power source is turned on, electrolysis is carried out for 4 to 8 h under the condition that the electrolyzing temperature ranges from 60 to 85 DEG C and the current density ranges from 1 to 6 A / dm<2>, after electrolyzing is finished, cathode liquid is taken out, a solvent is removed, and the trivalent pyridine ion liquid is obtained. According to the method, the preparing program of ion liquid can be effectivelysimplified, the prepared ion liquid has the three-core structure characteristic, and the method has the good application prospect in the aspects of catalysis, electrochemistry and the like.

Description

technical field [0001] The invention relates to the technical field of ionic liquid preparation, in particular to a method for preparing trivalent pyridine ionic liquid by electrolysis. Background technique [0002] As a new type of green solvent, ionic liquids have many excellent characteristics that traditional organic reagents cannot match, and are widely used in catalytic reactions, extraction and separation, gasoline desulfurization and other applications. In the prior art, the synthesized ionic liquids are mainly monovalent and a small amount of divalent. However, there are few types of ionic liquids available, which cannot meet the actual needs. The synthesis method of traditional ionic liquid generally adopts two-step method, that is: the first step is to synthesize quaternary ammonium halide by reaction of tertiary amine and alkyl halide; This method often has disadvantages such as long reaction time, excessive use of organic solvents, difficulty in removing impur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/00
CPCC25B3/00
Inventor 杜荣斌刘涛周峰胡春潮符成华黄裕安
Owner ANQING NORMAL UNIV