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The synthetic method of tetrafluoroborate ionic liquid

A technology of tetrafluoroborate and synthesis method, which is applied in the field of synthesis of tetrafluoroborate ionic liquid, can solve the problems of incomplete reaction and slow reaction, and achieve fast reaction rate, high yield and high refractive index Effect

Active Publication Date: 2020-06-23
杭州华樾新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It should be noted that in the two-step synthesis method, the step in which the target anion replaces the halide ion is the step that determines the reaction rate, and the reaction is generally slow and incomplete.

Method used

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  • The synthetic method of tetrafluoroborate ionic liquid
  • The synthetic method of tetrafluoroborate ionic liquid
  • The synthetic method of tetrafluoroborate ionic liquid

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preparation example Construction

[0027]

[0028] Disperse the quaternized ammonium substrate and alkyl halide with a molar ratio of 1:1~7 in the solvent, and irradiate with ultraviolet light at 30~50°C, and the light intensity is 10~1000W / m 2 , and the irradiation time is 8-12 hours to obtain a quaternary ammonium salt solution.

[0029] The quaternization substrate in the present invention is selected from tertiary amines shown in formula (a), N-substituted imidazoles shown in formula (b) or N-substituted pyridines shown in formula (c), preferably as shown in N-substituted imidazoles represented by formula (b),

[0030]

[0031] Among them, R1~R4 are the same or different, and are independently selected from C1-C6 alkyl, C2-C6 heteroalkyl, C3-C6 cycloalkyl, C1-C6 alkoxy, C1-C6 alkylthio or aryl . Selecting the above electron-rich groups can facilitate the reaction of the quaternized ammonium substrate with the alkyl halide to form a quaternary ammonium salt.

[0032] In the present invention, the C1-...

Embodiment approach

[0053] According to a preferred embodiment of the present invention, the synthetic method of tetrafluoroborate ionic liquid comprises the steps:

[0054] (1) Disperse the quaternized substrate and the alkyl halide in a solvent, the molar ratio of the quaternized substrate to the alkyl halide is 1:1-4; at 30-35°C, the light intensity is 50-800W / m 2 The ultraviolet light is irradiated, and the irradiation time is 9 to 11 hours to obtain a quaternary ammonium salt solution;

[0055] (2) Mix the quaternary ammonium salt solution obtained in step (1) with sodium tetrafluoroborate evenly, and the molar ratio of the quaternized substrate to the sodium tetrafluoroborate is 1:1~4, and at 38~43 At ℃, the light intensity is 50~800W / m 2 The ultraviolet light is irradiated, and the irradiation time is 17 to 19 hours to obtain a mixed solution containing tetrafluoroborate ionic liquid;

[0056] (3) Filtrating the mixed liquid obtained in step (2) to obtain a filtrate, concentrating the ...

specific Embodiment approach

[0057] According to a specific embodiment of the present invention, the synthetic method of tetrafluoroborate ionic liquid comprises the steps:

[0058] (1) Evenly disperse 1-methylimidazole and ethyl chloride with a molar ratio of 1:1 in ethanol, heat it to 35°C with a circulating heating device, and use a light intensity of 75W / m 2 or 600W / m 2 The ultraviolet light is irradiated, and the irradiation time is 10h, obtains the quaternary ammonium salt solution of 1-ethyl-3-methylimidazole chloride;

[0059] (2) Mix the quaternary ammonium salt solution obtained in step (1) with sodium tetrafluoroborate evenly, the molar ratio of the 1-methylimidazole to the sodium tetrafluoroborate is 1:1, and heat up to 40°C After that, the light intensity is 75W / m 2 or 600W / m 2 The ultraviolet light is irradiated, the irradiation time is 18h, and the mixed solution containing tetrafluoroborate ionic liquid;

[0060] (3) Filtrate the mixed solution obtained in step (2) to obtain a filtrate...

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Abstract

The invention discloses a synthetic method of tetrafluoroborate ionic liquid. The method comprises the following steps: enabling a quaternized substrate and alkyl halide to be dispersed in a solvent in a molar ratio of 1 to (1-7), adopting ultraviolet irradiation at 30-50 DEG C, enabling illumination intensity to be 10-1,000W / m<2> and irradiating for 8-12h to obtain a quaternary ammonium salt solution; enabling the quaternary ammonium salt solution and tetrafluoroborate to be uniformly mixed, adopting the ultraviolet irradiation at 35-45 DEG C, enabling the illumination intensity to be 10-1,000W / m<2> and irradiating for 16-20h to obtain mixed liquor; enabling the mixed liquor to be filtered to obtain filtrate, enabling the filtrate to be heated and concentrated, and removing the solvent toobtain the tetrafluoroborate ionic liquid. The method adopts the modes of ultraviolet irradiation and heating to synthesize the tetrafluoroborate ionic liquid, and the yield and reaction rate are high.

Description

technical field [0001] The invention relates to a method for synthesizing tetrafluoroborate ionic liquid, in particular to a method for synthesizing tetrafluoroborate ionic liquid whose cation is N,N'-disubstituted imidazolium cation. Background technique [0002] Ionic liquids have made great breakthroughs as environmentally friendly solvents, known as "green solvents", generally composed of larger organic cations and smaller inorganic or organic anions, and are in a molten state at room temperature or low temperature. Compared with traditional organic solvents and electrolytes, ionic liquids have the following advantages: almost no vapor pressure, which solves the problem of environmental pollution caused by the easy volatilization of organic substances; it has a larger stable temperature range, better chemical stability and wider Electrochemical stable potential window; low melting point and high polarity, good solubility for various organic substances, water and inorgani...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58
Inventor 戴秀萍赵张刚
Owner 杭州华樾新材料有限公司