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A kind of preparation method of low energy consumption imidazoles ionic liquid

An ionic liquid and imidazole-consuming technology, which is applied in the field of preparation of low-energy imidazole-based ionic liquids, can solve problems such as product yield, purity decline, energy use, slowdown, etc., to simplify circuits and processes, reduce energy waste, and process Conditional control for simple effects

Active Publication Date: 2018-11-06
LINZHOU KENENG MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the heating is stopped or the heating is insufficient, the temperature will automatically drop due to the endothermic reaction, and the reaction will automatically stop or slow down, resulting in a sharp drop in product yield and purity
[0015] At present, in the production process, one of the steps of heat absorption or heat release is mostly selected for production, so in the process of large-scale production, a large amount of energy consumption and waste will be caused

Method used

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  • A kind of preparation method of low energy consumption imidazoles ionic liquid
  • A kind of preparation method of low energy consumption imidazoles ionic liquid
  • A kind of preparation method of low energy consumption imidazoles ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0033] A preparation method of low energy consumption imidazole ionic liquid, comprising the following steps:

[0034] (1) Under stirring, take the raw material halogenated product R 1 x a with halide R 1 x b Mix according to a certain ratio to obtain the mixed solution A; raw material R 1 x a with R 1 x b The molar ratio is 1: (0.2~3); R 1 for C 2 ~C 8 One of the alkyl, allyl and ethyl acetate groups; X a for Cl - , X b for Br - or I - ;

[0035] (2) Under stirring, the mixed solution A and N-alkylimidazole are mixed and stirred according to the molar ratio of (1~2): 1, and the reaction is carried out at a temperature of 25~70°C for 4~8 hours, and the static After placing, use a solvent to wash excess raw materials, and then after vacuum distillation, obtain solid product B;

[0036] The structural formula of N-alkylimidazole is as follows: , where R 2 for C 1 ~C 4 the alkyl group;

[0037] (3) Perform anion exchange reaction on the solid product B obtai...

Embodiment 2

[0041] (1) Mix 46.25g of chlorobutane and 205.5g of bromobutane thoroughly and place in a constant pressure dropping funnel;

[0042](2) Add 164.2g of N-methylimidazole into the three-necked flask, and use magnetic stirring inside the three-necked flask;

[0043] (3) Place the constant-pressure dropping funnel at the mouth of the three-necked flask, and control the dropping rate to 1 drop per 2 seconds. The temperature in the flask will automatically rise to keep the temperature in the flask at 65-70°C, and the dropping will be completed in 2 hours;

[0044] (4) Continue to stir and react for 6 hours after the dropwise addition. During this process, the temperature is automatically maintained at 60~70°C, washed with ethyl acetate and rotary evaporated to obtain 391.0g of white solid product with a total yield of 94.0%. According to ion chromatography analysis, it contains 15.98g of chloride ions and 113.93g of bromide ions;

[0045] (5) The obtained white solid product was io...

Embodiment 3

[0049] (1) Fully mix 78.54g of chloropropane and 123.0g of bromopropane and place in a constant pressure dropping funnel;

[0050] (2) Add 192.26g of N-ethylimidazole into the three-necked flask, and use magnetic stirring inside the three-necked flask;

[0051] (3) Place the constant pressure dropping funnel at the mouth of the three-necked flask, control the dropping rate to 1 drop per 2 seconds, keep the temperature in the flask at 45~55°C, and complete the dropping within 2 hours;

[0052] (4) Continue to stir and react for 4 hours after the dropwise addition. During this process, the temperature is automatically maintained at 40~45°C, washed with ethyl acetate and rotary evaporated to obtain 375.29g of a light yellow liquid product with a total yield of 95.3%. According to ion chromatography analysis, it contains 32.66g of chloride ions and 78.24g of bromide ions;

[0053] (5) The obtained white solid product was ion-exchanged with 368.12 g of potassium hexafluorophosphat...

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Abstract

The invention relates to a method for preparing low-energy consumption imidazoles ionic liquid. The method comprises the following steps: 1) under stirring, taking a raw material halogenated object R1Xa and a halogenated object R1Xb to mix according to a certain ratio to obtain mixed liquor A; 2) under stirring, mixing the mixed liquor A and N-alkyl imidazole and stirring the materials for a reaction for 4-8 h at the temperature of 25-70 DEG C, standing, recovering the superfluous raw materials to obtain a solid product B; 3) performing an anion exchange reaction on the obtained solid product B and salts MY containing target anions to obtain a solution of target ionic liquid; and 4) separating the solution of the target ionic liquid and purifying the solution, and performing vacuum drying to obtain the product. Under prerequisite that the quality of the products in two steps are not decreased, by adjusting the ratio of the raw materials, and the method effectively uses one-step heat release / heat-absorbing reaction so as to reduce energy consumption and reaches a purpose of cleaning production.

Description

technical field [0001] The invention belongs to the technical field of ionic liquid production, and in particular relates to a preparation method of low energy consumption imidazole ionic liquid. Background technique [0002] Ionic liquid is a salt that exists in liquid form at room temperature or near room temperature. It has both the physical fluidity of liquid and the chemical reaction characteristics of salts, so it has many unique properties, such as structure can be designed, liquid range range Wide, close to zero vapor pressure, non-flammable, high thermal and chemical stability, etc. [0003] The synthesis of imidazole ionic liquids all adopts the following steps at present: [0004] Step 1 (see reaction formula I): [0005] [0006] The reaction process of step 1 is an organic addition reaction, and by steps such as heating, stirring, cleaning, R 1 The cycloaddition of X with N-alkylimidazoles is a one-step product. where R 1 for C 2 ~C 8 One of the alkyl ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58C07D233/56
CPCC07D233/56C07D233/58
Inventor 李凯明方金法刘艾军王存江郑勇张君芳
Owner LINZHOU KENENG MATERIAL TECH