A kind of preparation method of imidazole polyionic liquid

An ionic liquid and imidazole technology, applied in the field of preparation of imidazole polyionic liquids, can solve the problems of limited types and quantities of imidazole polyionic liquids, and achieve the effect of enriching types and quantities

Active Publication Date: 2022-05-27
河南纳宇新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the types and quantities of imidazole-based polyionic liquids are relatively limited.

Method used

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  • A kind of preparation method of imidazole polyionic liquid
  • A kind of preparation method of imidazole polyionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Accurately weigh (10 g, 1 mmol) hydroxy-terminated polyepichlorohydrin, add it to a 250 mL round-bottomed flask, pass argon into the round-bottomed flask for 10 min, and add methylimidazole (0.2 g, 2.8 mmol) , seal the round-bottomed flask and place it in an oil bath at 80°C for 12 hours of reaction. After the reaction is stopped, settle it in ether solution, collect the precipitate by centrifugation, wash it with ether for many times, and dissolve it in ethanol. Continue to use Diethyl ether precipitation treatment, centrifugal washing for several times to completely wash small molecular impurities, and drying in a vacuum drying oven at 60 °C for 24 hours to obtain side chains containing Cl - The imidazole polyionic liquids 1.

Embodiment 2

[0017] Accurately weigh the side chain containing Cl prepared in 1 - The imidazole-based polyionic liquid 1 (1.9 g, 10 mmol) was added to a 250 mL round-bottomed flask, 30 mL of distilled water was added to dissolve it to form a polyionic liquid 1 solution, and the bistrifluoromethanesulfonimide lithium LiNTf was weighed. 2 (1.43g, 5mmol) was dissolved in 20mL of distilled water, then added dropwise to the polyionic liquid 1 solution, stirred at room temperature for 4h, stopped stirring, placed in an oil bath at 80°C for 1h, and removed the upper layer of water Then, add 60 mL of distilled water to the round-bottomed flask and stir for 20 min. After standing for 30 min, remove the upper water phase. Use silver nitrate solution to detect whether there are chloride ions in the upper water phase. If so, continue to repeat the above experimental steps until the upper water is Until there is no chloride ion in the phase, rotary-evaporated to remove part of the aqueous solution, and...

Embodiment 3

[0019] Accurately weigh the side chain containing Cl prepared in 1 - The imidazole-based polyionic liquid 1 (1.9 g, 10 mmol) was added to a 250 mL round-bottomed flask, 30 mL of distilled water was added to dissolve it to form a polyionic liquid 1 solution, and the bistrifluoromethanesulfonimide lithium LiNTf was weighed. 2 (0.71 g, 2.5 mmol) was dissolved in 20 mL of distilled water, and then added dropwise to the solution of polyionic liquid 1. During the dropwise addition, a light yellow oily liquid appeared, stirred at room temperature for 4 h, stopped stirring, and placed in a 80°C Let stand in an oil bath for 1 hour to remove the upper aqueous phase, then add 60 mL of distilled water to the round-bottomed flask and stir for 20 min. After standing for 30 min, remove the upper aqueous phase and use silver nitrate solution to detect whether there is still chloride ion in the upper aqueous phase. If there is, continue to repeat the above experimental steps until there is no ...

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Abstract

The invention discloses a preparation method of an imidazole polyionic liquid, belonging to the technical field of polyionic liquid synthesis. The key points of the technical scheme of the present invention are as follows: firstly, react the polyepichlorohydrin containing hydroxyl groups with alkylimidazoles containing different chain lengths to prepare ‑ The imidazole-based polyionic liquid 1; then react the polyionic liquid 1 with the metal salt, and adjust the amount of the metal salt so that it and the polyionic liquid 1 have only part of the Cl in the ion exchange process ‑ By anion exchange in the metal salt, the imidazole-based polyionic liquid 2 containing two different anions in the side chain is finally prepared. The imidazole-based polyionic liquid prepared by the invention can effectively adjust the different hydrophilicity and hydrophobicity of the polymer by introducing different anions into the side chain of the polymer at the same time, and at the same time enrich the types and quantities of the polyionic liquid.

Description

technical field [0001] The invention belongs to the technical field of synthesis of polyionic liquids, and in particular relates to a preparation method of imidazole polyionic liquids. Background technique [0002] Polyionic liquids are polymerized from a class of ionic liquids with a melting point near room temperature, and their structures contain inorganic anions and organic cations. Usually the cation is an organic substance containing heteroatoms such as phosphorus, sulfur and nitrogen, and the anion is usually a hexafluorophosphate ion (PF6 - ), chloride ion (Cl - ), iodide ions (I - ), bromide ion (Br - ), bistrifluoromethanesulfonimide salt ion (N(CF 3 SO 2 ) 2- ) is TFSI - , nitrate ions (NO 3 - ) and acetate ions (C 2 H 5 COO - )Wait. Compared with small molecular ionic liquids, polyionic liquids have better chemical stability, better ionic conductivity, higher thermal stability, wider electrochemical potential window and stronger mechanical strength. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/333C08G65/337
CPCC08G65/33317C08G65/337
Inventor 李新娟孙艳平贾献彬王尚月
Owner 河南纳宇新材料有限公司
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