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A kind of preparation method of imidazole ionic liquid and single crystal thereof

A technology of ionic liquids and imidazoles, which is applied in the field of preparation of imidazole ionic liquids and their single crystals, can solve the problems of a large number of solvents, long heating and reflux time, energy consumption, etc., and achieve the effect of simple operation and low cost

Inactive Publication Date: 2015-08-12
CHANGAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, such ionic liquids cannot be synthesized in one step by a direct method. Usually, the halide substitution method is used to replace the halide salt containing the target cation with the target anion.

Method used

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  • A kind of preparation method of imidazole ionic liquid and single crystal thereof
  • A kind of preparation method of imidazole ionic liquid and single crystal thereof
  • A kind of preparation method of imidazole ionic liquid and single crystal thereof

Examples

Experimental program
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Effect test

experiment example 1

[0023] Weigh bromide-1-ethyl-3-methylimidazole (2.62mmol, 0.5g) and CdCl 2 2.5H 2 O (0.074g, 0.4mmol) was mixed in a 25mL stainless steel reaction vessel lined with tetrafluoroethylene. The reaction kettle was placed in a programmed temperature-controlled oven, kept at 160°C for 3 days, then cooled down to room temperature at a cooling rate of 10°C / h, filtered, and dried to obtain 0.15 g of colorless transparent columnar crystal particles with a yield of 57.25%.

experiment example 2

[0025] Weigh bromide-1-ethyl-3-methylimidazole (2.62mmol, 0.5g) and CdCl 2 2.5H 2 O (0.092g, 0.5mmol) was mixed in a 25mL stainless steel reaction vessel lined with tetrafluoroethylene. The reaction kettle was placed in a programmed temperature-controlled oven, and after being kept at 160°C for 3 days, the temperature was lowered to room temperature at a rate of 10°C / h, filtered, and dried. Obtained 0.26g of colorless transparent columnar crystal particles with a yield of 78.79%.

experiment example 3

[0027] Weigh bromide-1-ethyl-3-methylimidazole (2.62mmol, 0.5g) and CdCl 2 2.5H 2 O (0.110g, 0.6mmol) was mixed in a 25mL stainless steel reaction vessel lined with tetrafluoroethylene. The reaction kettle was placed in a programmed temperature-controlled oven, and after being kept at 160°C for 5 days, the temperature was lowered to room temperature at a rate of 5°C / h, filtered, and dried. Obtained 0.382g of colorless transparent columnar crystal particles with a yield of 97.21%.

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Abstract

The invention relates to the field of ionic liquids and preparation thereof and discloses an imidazolium ionic liquid [EMIM]2[CdBr4] and a preparation method for a single crystal thereof. The preparation method comprises the following steps: mixing (CdC12).(2.5H2O) with brominated-1-ethyl-3-methylimidazole in a mol ratio of 1: 2 to 1: 7 at room temperature and adding an obtained mixture into a reaction vessel with a tetrafluoroethylene lining; then, heating the reaction vessel to a temperature of 110 to 180 DEG C in a baking oven with program controlled temperature and carrying out thermal insulation and a reaction for 2 to 7 d; and finally, cooling the baking oven with program controlled temperature to room temperature at a cooling rate of 5 to 10 DEG C / h and filtering and drying a resultant to obtain a colorless transparent cylindrical crystal particle. The imidazolium ionic liquid [EMIM]2[CdBr4] provided by the invention can be used as a solvent for an organic reaction and polymerization and in the fields of chemical separation and electrochemistry.

Description

technical field [0001] The invention relates to the field of ionic liquids and preparation thereof, in particular to an imidazole ionic liquid and a method for preparing single crystals thereof. Background technique [0002] Ionic liquids are substances composed of specific cations and anions that are liquid at or near room temperature. Ionic liquids often exhibit unique physical and chemical properties and unique functions, and are a new type of "soft" function worthy of research and development. material or medium. Compared with traditional organic solvents, ionic liquids have properties such as wide liquid range, wide dissolution range, low vapor pressure, good stability, adjustable acid-base, and recyclability. Another class of green solvents. [0003] The research on ionic liquids can be traced back to 1914. After Sugden reacted ethylamine with 20% nitric acid, the water was removed under reduced pressure, and the organic salt ethylamine nitrate [C] that was liquid at...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58
Inventor 苟蕾郝丽敏马洁
Owner CHANGAN UNIV