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A kind of preparation method of imidazole dialkyl phosphate ionic liquid

A technology of azole-type dialkyl phosphate and dialkyl phosphate, which is applied in the field of ionic liquid preparation, can solve the impossibility of ionic liquid in the chemical industry, restrict the large-scale production of ionic liquid, and difficult to remove impurity ions, etc. problems, to achieve huge industrial application potential, easy control of the preparation process, and high product yield

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

Among the most reported ionic liquid varieties, trifluoromethylsulfamide [NTf2] - , trifluoromethanesulfonic acid [OTf] - and trifluoroacetic acid [TFA] - Ionic liquids as anions are unlikely to find industrial application in the chemical industry because of their high price
The ionic liquid with dialkyl phosphate as anion is much cheaper, but its synthesis method has the disadvantages of too long reaction time, the use of a large amount of organic solvent, the difficulty of removing impurity ions, and high production costs, which seriously restrict the production of ionic liquids. mass production of

Method used

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  • A kind of preparation method of imidazole dialkyl phosphate ionic liquid
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  • A kind of preparation method of imidazole dialkyl phosphate ionic liquid

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Embodiment 1

[0024] A method for preparing an imidazole dialkyl phosphate ionic liquid. 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. The stable anode is the anode, and Pt is the cathode. The acetonitrile solution of N-ethylimidazole with a concentration of 1.2mol / L is added in the cathode chamber, and the acetonitrile solution of trimethyl phosphate with a concentration of 1.6mol / L is added in the anode chamber. Silicon-through rectifier power supply, the electrolysis temperature is 75°C, and the current density is 2.5A / dm 2 Under the conditions of electrolysis for 6.5h, the catholyte was taken out after the electrolysis was completed, separated and purified to obtain 1-ethyl-3-methylimidazolium phosphate ionic liquid with a purity of 83wt%, and its H 1 NMR: 8.706(s, 1H), 7.485(s, 1H), 7.419(s, 1H), 4.211(q, 2H), 3.8...

Embodiment 2

[0026] A preparation method of imidazole dialkyl phosphate ionic liquid, 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 graphite is used as the Anode, Pt as the cathode, the acetonitrile solution of N-ethylimidazole with a concentration of 1mol / L is added to the cathode chamber of the electrolytic cell as the catholyte, and the acetonitrile solution of triethyl phosphate with a concentration of 3mol / L 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 75°C, and the current density is 7A / dm 2 Under the conditions of electrolysis for 6 hours, the current efficiency is 30%. After the electrolysis is completed, the catholyte is taken out and put into a rotary evaporator for rotary evaporation to obtain 1-...

Embodiment 3

[0029] A preparation method of imidazole dialkyl phosphate ionic liquid, 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 Ti-based PbO 2 Is the anode, Pt is the cathode, the concentration is 1.5mol / L the acetonitrile solution of N-ethylimidazole is added in the cathode chamber of the electrolyzer as the catholyte, the concentration is the acetonitrile solution of the tributyl phosphate of 1.5mol / L as Add the anolyte into the anode chamber of the electrolytic cell, turn on the silicon rectifier power supply, and the electrolysis temperature is 80°C, and the current density is 1.5A / dm 2 Under the conditions of electrolysis for 9 hours, the current efficiency is 40%. After the electrolysis is completed, the catholyte is taken out and put into a rotary evaporator for rotary evaporation to obtain 1-butyl-3-...

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Abstract

The invention discloses a method for preparing an imidazole dialkyl phosphate ionic liquid. At least one layer of perfluorinated cation exchange membrane is arranged in an electrolytic cell, and the perfluorinated cation exchange membrane divides the electrolytic cell into a cathode chamber and an anode chamber. , by shape-stabilizing the anode with DSA, Ti-based PbO 2 Or graphite is the anode, Pt is the cathode, the N-ethylimidazole acetonitrile solution with a concentration of 1-1.5mol / L is added to the cathode chamber, and the concentration of 1.5-3mol / L trialkyl phosphate acetonitrile solution is added to the anode chamber , turn on the silicon rectifier power supply, the electrolysis temperature is 75-80 ℃, the current density is 1.5-7A / dm 2 Under the conditions of electrolysis for 6-9h, the catholyte was taken out, separated and purified to obtain the imidazole dialkyl phosphate ionic liquid. The method of the invention can not only effectively simplify the preparation procedure of the ionic liquid, but also the prepared ionic liquid has good application prospects in 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 an imidazole-based dialkyl phosphate ionic liquid. Background technique [0002] As a new type of green solvent, ionic liquid has many excellent properties that traditional organic reagents cannot match, and has broad application prospects in the fields of chemical reaction and separation engineering, especially in the field of separation technology such as rectification, extraction and gas absorption. Among the most reported ionic liquid varieties, trifluoromethylsulfamide [NTf2] - , trifluoromethanesulfonic acid [OTf] - and trifluoroacetic acid [TFA] - Ionic liquids as anions are unlikely to find commercial application in the chemical industry because of their high price. The ionic liquid with dialkyl phosphate as anion is much cheaper, but its synthesis method has the disadvantages of too long reaction time, the use of a large amount ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/04C25B3/25
CPCC25B3/25
Inventor 杜荣斌刘涛周峰胡春潮符成华黄裕安
Owner ANQING NORMAL UNIV
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