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Homogeneous catalyst and heterogeneous catalyst based on ionic liquid, and preparation methods and application thereof

A heterogeneous catalyst, homogeneous catalyst technology, applied in the synthesis of new strong basic ionic liquid, new ionic liquid riveting field, can solve the problem of weak alkalinity, poor nucleophilicity, poor stability of strong basic ionic liquid, etc. question

Inactive Publication Date: 2020-10-23
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purpose of the present invention is to develop a new type of strong base with special structure, high temperature resistance and high stability, aiming at the problems of weak alkalinity, poor nucleophilicity or poor stability and easy deactivation of ionic liquids reported in literature or patents. sexual ionic liquid

Method used

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  • Homogeneous catalyst and heterogeneous catalyst based on ionic liquid, and preparation methods and application thereof
  • Homogeneous catalyst and heterogeneous catalyst based on ionic liquid, and preparation methods and application thereof
  • Homogeneous catalyst and heterogeneous catalyst based on ionic liquid, and preparation methods and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0127] The specific preparation method of 1-ethyl-3-methylimidazolium imidazolium salt: dissolve 0.5mol imidazole in 60mL ethanol solvent, add equimolar potassium ethoxide to a three-necked flask, stir vigorously at 60°C for 6h, and the reaction is over Finally, under the condition of 65°C in an oil bath, the solvent ethanol and the product ethanol were removed by rotary evaporation under reduced pressure for 2 hours, and dried in a vacuum drying oven for 12 hours to constant weight to prepare imidazole potassium salt. 0.5 mol of commercially purchased [EmIm]Br was added into a three-necked flask, and potassium imidazole was added in an equimolar ratio under the condition of ethanol with water as a solvent, and the reaction was stirred at room temperature for 24 hours. After the reaction was completed, the resulting white solid KBr was removed by filtration, and the solvent was removed by rotary evaporation under reduced pressure for 2 hours in an oil bath at 65°C, and dried in...

Embodiment 2

[0130] Table 1 is a comparison of the activities of commercially purchased ionic liquids and ionic liquids synthesized in the laboratory for the transesterification of dimethyl carbonate and ethanol. Catalyst evaluation conditions are as follows: 46g ethanol and 90g dimethyl carbonate reaction raw materials (molar ratio: 1:1) are uniformly mixed in a 250mL flask, magnetically stirred, the reaction system is heated to 76-78°C, and about 2.72g of ion is added after the reflux is stable. The mass of the liquid and the ionic liquid accounts for 2% of the mass of the reaction raw materials, and the reaction time is 30-240min. The commercially purchased ionic liquids are: 1-ethyl-3-methylimidazolium acetate, 1-ethyl-3-methylimidazolium chloride, 1-ethyl-3-methylimidazolium bromide, 1- Ethyl-3-methylimidazolium iodide, 1-butyl-3-methylimidazolium fluoroborate, 1-butyl-3-methylimidazolium chloride, 1-butyl-3-methylimidazolium bromide salt, 1-butyl-3-methylimidazolium iodide salt, 1,3...

Embodiment 3

[0137] With 1-butyl-3-methylimidazolium pyrrole salt as catalyst, the initial state of the catalyst is as follows Figure 5 As shown, the color of the prepared ionic liquid is transparent light yellow.

[0138] 1-butyl-3-methylimidazolium pyrrole salt catalyst reuse evaluation conditions are, 46g ethanol and 90g dimethyl carbonate reaction raw materials (molar ratio is 1:1) are uniformly mixed in a 250mL flask, magnetically stirred, and the temperature of the reaction system is raised to 76-78°C, after the reflux is stable, add about 2.72g of 1-butyl-3-methylimidazolium pyrrole salt ionic liquid, the mass of the ionic liquid accounts for 2% of the mass of the reaction raw materials, and the reaction time is 30min. After the reaction, the reaction raw materials, products and ionic liquid were rotary evaporated at 110° C. for 30 minutes under reduced pressure. The remaining liquid in the rotary evaporator is the 1-butyl-3-methylimidazole pyrrole salt catalyst, which is directly...

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Abstract

The invention discloses a homogeneous catalyst. The homogeneous catalyst comprises ionic liquid, wherein the ionic liquid comprises anions and cations; both the anions and the cations contain nitrogenheterocyclic rings; the cations have structures as shown in a formula I or a formula II; and the anions have a structure as shown in a formula III, a formula IV or a formula V. The invention also discloses a heterogeneous catalyst containing the homogeneous catalyst. The invention also relates to preparation methods and application of the homogeneous catalyst and the heterogeneous catalyst. The homogeneous catalyst and the heterogeneous catalyst are used for transesterification of dimethyl carbonate and ethanol, transesterification of dimethyl carbonate and diethyl carbonate, and transesterification of methanol and diethyl carbonate to synthesize high-purity ethyl methyl carbonate products. The catalysts show extremely high reaction activity, reaction equilibrium can be achieved after a reaction is conducted for 5 min at 76-78 DEG C, and the catalysts show high catalytic activity even under the condition of near room temperature (30 DEG C). The synthesized ionic liquid can be repeatedly used for 20 times, the catalytic activity of the ionic liquid is basically unchanged, and the ionic liquid shows high stability.

Description

technical field [0001] This application belongs to chemistry and chemical engineering, high-purity lithium battery electrolyte synthesis, specifically, it relates to a synthesis method of a new type of strong alkaline ionic liquid and a riveting-type immobilization method of the new type of ionic liquid, and the prepared heterogeneous catalyst For the catalytic synthesis of ethyl methyl carbonate. Background technique [0002] Ethyl methyl carbonate (EMC) is a linear carbonate compound with an asymmetric structure. It has both the characteristics of dimethyl carbonate (DMC) and diethyl carbonate (DEC). It is compatible with alcohols, ethers, and ketones. Miscible with almost all organic solvents, it can be used as carbonylation or alkylation reagent for organic synthesis. EMC has high oxygen content, low toxicity, low bio-persistence, and low solubility in water. It is considered as an environmentally friendly chemical and is a promising gasoline additive that can increase ...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C68/06C07C69/96
CPCB01J31/0282B01J31/0284B01J31/0292C07C68/06C07C69/96B01J2231/49B01J31/0298B01J31/0279
Inventor 石磊郭建军李新刘铭玉
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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