Preparation method of ionic liquid

One kind of ionic liquid and another kind of technology, applied in the field of preparation of ionic liquid, can solve the problems of limited application of ionic liquid, difficult volatilization of ionic liquid, inability to refine, etc., and achieve the effect of reducing solvent residue, low equipment requirements and easy operation.

Active Publication Date: 2021-03-16
珠海中科先进技术研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]However, the purity of ionic liquids prepared at present is generally 99%, which severely limits the application of ionic liquids
However, it is more difficult to remove trace impurities in the crude ionic liquid, and the ionic liquid cannot be refined by distillation because it is difficult to volatilize.

Method used

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  • Preparation method of ionic liquid
  • Preparation method of ionic liquid
  • Preparation method of ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A method for preparing high-purity ionic liquid, comprising the following steps:

[0034] (1) The first recrystallization: by molar fraction, take 5 parts of 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide salt [EMlm]TFSI ionic liquid crude product, 70°C Rotary steam for 4 hours, wait for the crude product to cool down to room temperature, add the recrystallization mixed organic reagent (by mass parts, 7 parts of dichloromethane and 6 parts of ethyl acetate), shake it manually, and wait for the crude product of the ionic liquid and the recrystallization reagent to fully After mixing, refrigerate in a -80°C refrigerator, let stand for 24 hours, and precipitate transparent crystals;

[0035] (2) The second recrystallization: Pour out the solvent after the first recrystallization, and place the transparent crystal obtained after recrystallization at room temperature until the crystal dissolves, and then spin evaporate at 75°C to remove the impurity in the rec...

Embodiment 2

[0039] A method for preparing high-purity ionic liquid, comprising the following steps:

[0040] (1) The first recrystallization: by molar fraction, take 7 parts of the crude product of 1-butyl-3-methylimidazolium hexafluorophosphate [BmIm]PF6 ionic liquid, rotary steam at 60°C for 4 hours, and wait for the crude product to cool down to room temperature, add the recrystallization mixed organic reagent (according to the mass parts, 7 parts of methanol and 6 parts of acetonitrile), shake it manually, and after the crude ionic liquid is fully mixed with the recrystallization reagent, put it in a -80°C refrigerator for refrigeration. After standing for 24 hours, transparent crystals were precipitated;

[0041] (2) The second recrystallization: Pour out the solvent after the first recrystallization, and place the transparent crystal obtained after recrystallization at room temperature until the crystal dissolves, and then spin evaporate at 75°C to remove the impurity in the recryst...

Embodiment 3

[0045] A method for preparing high-purity ionic liquid, comprising the following steps:

[0046] (1) The first recrystallization: In terms of molar parts, take 4 parts of 1-methyl-1-propylpyrrole bis(fluorosulfonyl)imide salt P1,3FSI crude ionic liquid, and rotary steam at 60°C for 4h , when the crude product cools down to room temperature, add recrystallization mixed organic reagent (according to mass parts, 7 parts of isopropanol and 6 parts of acetone), shake manually, after the crude product of ionic liquid and recrystallization reagent are fully mixed, put into- Refrigerate in a refrigerator at 80°C, let it stand for 24 hours, and transparent crystals will precipitate;

[0047] (2) For the second recrystallization, pour out the solvent after the first recrystallization, and place the transparent crystal obtained after recrystallization at room temperature until the crystal dissolves, and then spin evaporate at 75°C to remove the impurity during recrystallization Recrysta...

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Abstract

The invention belongs to the technical field of preparation of chemical reagents, and discloses a preparation method of ionic liquid. The method comprises the following steps: mixing a crude product of the ionic liquid with an organic solvent mixed solution, carrying out refrigeration crystallization, separating the solvent from the ionic liquid, and repeating the crystallization process for one or more times to obtain purified ionic liquid; wherein the organic solvent mixed solution at least contains two organic solvents, at least one organic solvent can be miscible with the ionic liquid, andthe other organic solvent cannot be miscible with the ionic liquid. By adopting the method provided by the invention, the purity of the purified ionic liquid is greater than 99.9%, and the recrystallization yield is greater than 80%; the used raw materials are common reagents, so that the solvent residue can be reduced to the maximum extent, the purification cost is low, the equipment requirementis low, the operation is easy, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of chemical reagents, and in particular relates to a preparation method of an ionic liquid. Background technique [0002] Ionic liquid is a new type of environmentally friendly green solvent, which refers to a liquid composed entirely of ions. At room temperature, ionic liquids coexist as anions and cations in liquid state. Ionic liquids have attracted a lot of attention in the industry because of their wide electrochemical window, high thermal stability, good thermal and electrical conductivity, and room temperature operability, and have been applied in various fields of chemical research. Especially as a reaction solvent, it is applied to various types of reactions, such as hydrogenation reactions, Friedel-Crafts reactions, asymmetric catalytic reactions, etc. [0003] However, the purity of currently prepared ionic liquids is generally 99%, which severely limits the application of ionic l...

Claims

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Application Information

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IPC IPC(8): B01D9/02C07D233/58C07D295/037C07D295/023C07D295/088C07C303/44C07C311/50
CPCB01D9/0018C07D233/58C07D295/037C07D295/023C07D295/088C07C303/44C07C311/50Y02P20/54
Inventor 张嘉恒王嘉慧陈正件费玉清陈晓欣江俊杰
Owner 珠海中科先进技术研究院有限公司
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