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A kind of preparation method of high-purity imidazole acetate ionic liquid

The technology of imidazole acetate and methylimidazole acetate is applied in the field of preparation of high-purity ionic liquid, can solve the problems of high raw material alkoxide price, serious environmental pollution, harsh reaction conditions, etc. The effect of high product purity and moderate reaction speed

Active Publication Date: 2022-05-24
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method not only has a huge number of by-products and seriously pollutes the environment, but also has a large amount of lead ions remaining in the form of complexation in the product.
[0009] Disclosed in CN1914181A are two preparation methods of imidazole acetate ionic liquid, the preparation process of the two methods is relatively complicated, and the raw material alkoxide used is expensive, flammable, and the reactants are extremely sensitive to water, the cost is high, and it is not conducive to control , it is also easy to introduce impurities such as sulfur and barium
But the conversion rate of this reaction is low (up to 91.5%), and a lot of residues of 1-substituent imidazole raw materials remain in the product
And in the synthetic process, the C of No. 2 position of 1-substituent imidazole will react with dimethyl carbonate to generate some carbonyl by-products, resulting in impure product
[0014] All in all, the current preparation methods of acetic acid ionic liquids more or less have the following problems: the raw materials contain heavy metals or other pollution; the raw materials are expensive; the reaction is not complete or prone to disproportionation; the reaction process is slow; Halogen and metal ions remain more

Method used

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  • A kind of preparation method of high-purity imidazole acetate ionic liquid
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  • A kind of preparation method of high-purity imidazole acetate ionic liquid

Examples

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Effect test

Embodiment 1

[0043] Preparation of 1-ethyl-3-methylimidazolium acetate ionic liquid:

[0044] Dissolve 1.0 mol of 1-ethyl-3-methylimidazolium chloride in 48 g of water to obtain solution A, and dissolve 1.2 mol of lithium perchlorate in 254 g of water to obtain solution B; mix solution A and solution B, 575g of dichloromethane was added, and the reaction was mechanically stirred for 12 hours; the liquid was separated, and the water phase was separated into a waste liquid, which was recovered, and the organic phase was washed with 260g of pure water each time, and washed 5 times, using AgNO 3 No precipitation was detected in the solution; the organic phase was vacuum rotary evaporated at 80 °C to obtain 193 g of 1-ethyl-3-methylimidazolium perchlorate ionic liquid intermediate in a yield of 91.9%; 579 g of ethanol was added, and under vigorous stirring, Slowly add a total of 90.1g of potassium acetate in 4 batches. During the addition process, solids are dissolved and separated out, and the...

Embodiment 2

[0046] Preparation of 1-butyl-3-methylimidazolium acetate ionic liquid:

[0047] Dissolve 1.0 mol of 1-butyl-3-methylimidazolium bromide in 58 g of water to obtain solution A, and dissolve 0.8 mol of lithium perchlorate in 170 g of water to obtain solution B; mix solution A and solution B, 531g of dichloromethane was added, and the reaction was mechanically stirred for 12 hours; the liquid was separated, and the organic phase was washed with 278g of pure water each time, and washed 3 times with AgNO 3 No precipitation was detected in the solution; the organic phase was vacuum rotary evaporated at 80°C to obtain 178.4g of 1-butyl-3-methylimidazolium perchlorate ionic liquid intermediate, the yield was 93.7%; 446g of ethanol was added, and under vigorous stirring, A total of 79.8 g of potassium acetate was slowly added in 4 batches. During the addition, solids were dissolved and precipitated continuously, and the reaction was continued for 12 hours; the stirring was stopped, fro...

Embodiment 3

[0049] Preparation of 1-octyl-3-methylimidazolium acetate ionic liquid:

[0050] Dissolve 1.0 mol of 1-octyl-3-methylimidazolium chloride in 78 g of water to obtain solution A, and dissolve 2.0 mol of lithium perchlorate in 426 g of water to obtain solution B; mix solution A and solution B, 841g of dichloromethane was added, and the reaction was mechanically stirred for 12 hours; the liquid was separated, and the water phase was separated into a waste liquid, which was recovered, and the organic phase was washed with 256g of pure water each time, and washed 3 times, using AgNO 3 No precipitation was detected in the solution; the organic phase was vacuum rotary-evaporated at 80°C to obtain 193 g of 1-octyl-3-methylimidazolium perchlorate ionic liquid intermediate with a yield of 91.9%; 965 g of ethanol was added, and under vigorous stirring, the A total of 90.1g of potassium acetate was slowly added in 4 batches. During the addition process, solids were dissolved and precipitat...

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Abstract

The invention belongs to the technical field of ionic liquid synthesis, and in particular relates to a preparation method of a high-purity imidazole acetate ionic liquid, in which a 1-alkyl-3-methylimidazole halogenated product is reacted with lithium perchlorate to obtain a high-purity Pure 1-alkyl-3-methylimidazolium perchlorate ionic liquid intermediate; the intermediate is then subjected to metathesis reaction with potassium acetate or ammonium acetate to obtain 1-alkyl-3-methylimidazolium acetate ion Liquid, raw materials are cheap and easy to obtain, raw materials or intermediate by-products have no heavy metals or other pollution, the reaction is thorough, the reaction yield is higher than 90.0%, the product purity is higher than 99.0%, the halogen residue in the product is less than 5ppm, and the K ion or ammonium in the product Root content is less than 200ppm.

Description

technical field [0001] The invention belongs to the field of ionic liquid synthesis, in particular to a method for preparing a class of high-purity ionic liquids in which the cation is imidazole (ring) and the anion is acetate. Background technique [0002] Ionic liquid is an emerging functional material with many advantages such as extremely low vapor pressure, high electrical conductivity, stable chemical properties, and flowable physical form. Hot spots with development prospects. In addition to the above advantages, ionic liquids also have a wide variety of characteristics. Both anionic and cationic structures can be molecularly grafted according to needs, so ionic liquids are a universal chemical material in the future; on the other hand, ionic liquids have the largest The advantage is that it is green and environmentally friendly, and there is no volatile loss during use. The concept of green is very suitable for the current concept of environmental protection. At pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58
CPCC07D233/58
Inventor 陈辉李凯明王晓航林孟昌
Owner SHANDONG UNIV OF SCI & TECH
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