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A kind of purification method of imidazoles ionic liquid

A technology of ionic liquid and purification method, which is applied in the field of ionic liquid production, can solve problems such as product yield reduction, achieve the effects of improving product quality, reducing extraction times, and reducing insoluble flocculent impurities

Active Publication Date: 2019-05-10
LINZHOU KENENG MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The raw materials used in most MY salts and one-step products will inevitably introduce a small amount of flocculent insoluble impurities that are visible or invisible to the naked eye. The salt density in it is relatively high, and it is deposited on the layered interface and the bottom of the separatory tank. In this case The lower liquid separation will cause the impurities to be distributed between the product and the organic phase, or below the layered interface, resulting in the product needing multiple cleanings to meet the required requirements, and multiple cleanings will eventually lead to a decrease in product yield

Method used

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  • A kind of purification method of imidazoles ionic liquid
  • A kind of purification method of imidazoles ionic liquid
  • A kind of purification method of imidazoles ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0036] A kind of purification method of imidazoles ionic liquid, comprises the following steps:

[0037] (1) Under stirring, the crude product [R 1 R 2 IM]X performs anion exchange reaction with the salt MY containing the target anion in aqueous medium to obtain [R 1 R 2 IM] Mixed solution A of Y and MX; R 1 for C 2 ~C 8 One of the alkyl, allyl and ethyl acetate groups; R 2 for C 1 ~C 4 Alkyl; X is halogen or ester; M is H or alkali metal element; Y is BF 4 - 、PF 6 - , SbF 6 - , N(CF 3 SO 2 ) - , N(C 2 f 5 SO 2 ) - , N(FSO 2 ) 2 - or CF 3 SO 3 - ;

[0038] (2) Add an organic extractant to the mixed solution A in step (1), mix evenly and let it stand, the mixed solution will automatically stratify, containing ionic liquid [R 1 R 2 The organic phase of IM] Y is in the lower floor, and the aqueous phase containing MX is in the upper floor; the organic extractant is at least one of methylene chloride, chloroform, carbon tetrachloride and ether;

[0...

Embodiment 2

[0045] Purification of 1-butyl-3-methylimidazolium tetrafluoroborate

[0046] 1.0 mol of 1-butyl-3-methylimidazolium bromide was dissolved in 500 mL of water, 1.0 mol of ammonium tetrafluoroborate was added with stirring, and the reaction was stirred at room temperature for 24 hours.

[0047] Add 400mL of dichloromethane to the resulting mixed solution, transfer it to a separatory funnel, add 100g of sodium nitrate, shake it, let it stand, and layer into the organic phase in the upper layer, and the water phase in the lower layer; drain the lower water phase, and add the organic phase again 500mL of water and 150g of sodium nitrate, shake, stand still, separate layers, discharge the lower aqueous phase, and repeat this cleaning operation once again; at this time, it is detected that the organic phase is free of bromide ions and ammonium ions, and a colorless transparent liquid is obtained by vacuum rotary evaporation Product, yield 92.0%.

[0048]

Embodiment 3

[0050] Purification of 1-allyl-3-butylimidazolium hexafluorophosphate

[0051] Dissolve 1.0 mol of 1-allyl-3-butylimidazolium chloride in 500 mL of water, add 1.0 mol of potassium hexafluorophosphate under stirring, and react with stirring at room temperature for 12 hours.

[0052] Add 400mL of dichloromethane to the resulting mixed solution, transfer to a separatory funnel, add 110g of potassium carbonate, oscillate, let stand, and layer into the organic phase in the upper layer, and the water phase in the lower layer; the lower water phase is discharged, and the organic phase is added again. 500mL of water and 180g of potassium carbonate, shake, stand still, separate layers, discharge the lower aqueous phase, and repeat this cleaning operation twice; at this time, the organic phase is detected to be free of bromide ions and ammonium ions, and a light yellow transparent liquid is obtained by vacuum rotary evaporation Product, yield 93.0%.

[0053]

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Abstract

The invention relates to a purification method of an imidazole ionic liquid. The purification method comprises the following steps: adding a coarse product of [R1R2IM]X and MY into a water medium to carry out anion exchange reactions; then adding an organic extracting agent into the mixed solution, evenly mixing, allowing the system to stand still to carry out automatic layering; then adding salt D into the mixed solution, evenly mixing, allowing the system to stand still to carry out automatic layering, wherein the upper layer is an organic phase, and the lower layer is an water phase containing MX; discharging the water phase containing MX; then adding purified water and salt D into the organic phase, vibrating the system to carry out layering, discharging the lower layer (water phase); and repeating the steps of adding purified water and salt D for 2 to 3 times until no MX impurity is detected in the organic phase. By selecting a proper solvent and adding proper salt, the water phase density is increased, thus the extraction frequency is reduced, and the product quality is improved.

Description

technical field [0001] The invention belongs to the technical field of ionic liquid production, and in particular relates to a purification method of imidazole ionic liquid. Background technique [0002] Ionic liquids have unique physical and chemical properties, and room temperature ionic liquids have become a key subject that scientists are concerned about today. With the increase in the types of ionic liquids, the synthesis methods of imidazole ionic liquids have also made rapid progress. At present, the synthesis of ionic liquids mostly adopts a two-step method, wherein the first step is an organic addition reaction to synthesize intermediates containing halogen anions, such as 1-butyl-3-methylimidazolium chloride salt, 1-ethyl-3- Methylimidazolium Bromide. The second step is the metathesis reaction, the purpose of which is to obtain a specifically designed product containing the target anion through ionic liquid exchange. [0003] Wherein the second step reaction can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58
CPCC07D233/58
Inventor 方金法李凯明王存江李义伟付涛
Owner LINZHOU KENENG MATERIAL TECH
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