Preparation method of double-pyridine type ironic liquid

A technology of ionic liquid and bipyridine, which is applied in the field of preparation of bipyridine ionic liquid, can solve the problems of restricting the large-scale production of ionic liquid, difficult to remove impurity ions, long reaction time, etc., achieve good application prospects and high product yield , the effect of compact equipment

Active Publication Date: 2018-12-25
ANQING NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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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  • Preparation method of double-pyridine type ironic liquid
  • Preparation method of double-pyridine type ironic liquid
  • Preparation method of double-pyridine type ironic liquid

Examples

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Embodiment 1

[0031] A kind of preparation method of bipyridine ionic liquid, is provided with at least one layer of cation exchange membrane in electrolyzer, described cation exchange membrane divides electrolyzer into cathode room and anode room, adopts PbO 2 As the anode, graphite as the cathode, the concentration of 2.5mol / L 2,2-bis-(4-alkylpyridine)methyl-1,3-propanediol aqueous solution is added in the anode chamber of the electrolytic cell as the anolyte, and the content Acetonitrile mixed aqueous solution that is 10wt% KBr is added in the cathode compartment of the electrolytic cell as the catholyte, the power is turned on, the electrolysis temperature is 50°C, and the current density is 0.75A / dm 2 Under the conditions of constant current electrolysis for 2h, the catholyte was taken out after the electrolysis was completed, separated and purified to obtain the bis[pyrrolo(1,2-A)-4-picoline] dibromide of the bispyridine ionic liquid, the purity 90wt%.

Embodiment 2

[0033] A kind of preparation method of bispyridine ionic liquid, in two storage tanks respectively filled with 3.5mol / L 2,2-bis-(4-alkylpyridine)methyl-1,3-propanediol aqueous solution as anode Electrolyte, the mixed aqueous solution of acetonitrile of 10wt% KBr is the catholyte, the said anolyte of 1500mL and the said catholyte of 1500mL are respectively added in two storage tanks, and respectively by two circulating pump Connected with one liquid storage tank, the cathode chamber of the electrolyzer communicates with another liquid storage tank. Turn on the circulation pump, and turn on the DC power supply at the same time, and use the Nafion 902 cation exchange membrane as the diaphragm to divide the electrolytic cell into a cathode chamber and an anode chamber, PbO 2 The anode is used as the anode, and the graphite is used as the cathode. The cathode and anode liquids pass through the cathode chamber and the anode chamber respectively at a flow rate of 300L / h to form a clo...

Embodiment 3

[0035] A kind of preparation method of bipyridine ionic liquid, in two liquid storage tanks respectively filled with 2,2-bis-(4-alkylpyridine)methyl-1,3-propanediol aqueous solution as anode electrolysis Liquid, the acetonitrile mixed aqueous solution of 13wt% KBr is the catholyte, the anolyte and the catholyte are respectively added in two liquid storage tanks, and the anode chamber of the electrolytic cell is connected to a storage tank by two circulation pumps respectively. The liquid tank, the cathode chamber of the electrolytic cell communicates with another liquid storage tank. Turn on the circulation pump, and turn on the DC power supply at the same time, and use the Nafion 902 cation exchange membrane as the diaphragm to divide the electrolytic cell into a cathode chamber and an anode chamber, PbO 2 The anode is used as the anode, and the graphite is used as the cathode. Both the cathode and anode electrolytes pass through the cathode chamber and the anode chamber resp...

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Abstract

The invention discloses a preparation method of double-pyridine type ironic liquid. The preparation method comprises the following steps of: arranging at least one layer of cation exchange membrane inan electrolytic bath; adopting PbO2 as an anode and graphite as a cathode; taking a 2,2-bi-(4-alkyl pyridine)methyl-1,3-propylene glycol water solution of which the concentration is 2-4 mol/L as anolyte; taking an acetonitrile and water mixed solution of KBr of which the content is 8-13 wt% as catholyte; switching on the power; carrying out constant-current electrolysis for 1-5 hours under the conditions that the electrolysis temperature is 40-65 DEG C and the current density is 0.5-2 A/dm<2>; and taking out the catholyte after the electrolysis is ended so as to obtain the double-pyridine type ironic liquid. The preparation method disclosed by the invention is simple in preparation and purification processes and is also relatively high in yield; and meanwhile the prepared double-pyridinetype ironic liquid realizes good application prospects in the aspects such as catalysis and electrochemistry.

Description

technical field [0001] The invention relates to the technical field of preparation of ionic liquids, in particular to a method for preparing bispyridine-based ionic liquids. Background technique [0002] As a new type of green solvent, ionic liquid has many excellent characteristics that traditional organic reagents cannot match, and has broad application prospects in the fields of chemical reaction and separation engineering, especially in separation engineering technologies such as rectification, extraction and gas absorption. field. 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. Therefore, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00C07D471/22
CPCC07D471/22C25B3/00
Inventor 杜荣斌刘涛吴夏周峰胡春潮
Owner ANQING NORMAL UNIV
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