Binary eutectic ionic liquid and preparation method thereof

An ionic liquid and eutectic technology, applied in organic chemistry and other directions, can solve the problems of complex preparation process, high viscosity and high cost, and achieve the effects of simple preparation process, low material density and energy density, and good electrical conductivity.

Inactive Publication Date: 2009-10-21
EAST CHINA NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the traditional ionic liquids are prepared by replacement, ion exchange or neutralization reaction, the preparation

Method used

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  • Binary eutectic ionic liquid and preparation method thereof
  • Binary eutectic ionic liquid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Preparation of Tetrabutylammonium Bromide / Imidazolium Ionic Liquid

[0018] In the first step, imidazole and tetrabutylammonium bromide were purified by recrystallization from toluene, and dried under vacuum at 60°C to obtain pure imidazole and tetrabutylammonium bromide.

[0019] In the second step, weigh 9.67g (0.03mol) of tetrabutylammonium bromide and 4.77g (0.07mol) of imidazole respectively, mix well, and heat at 100°C under stirring to obtain a homogeneous colorless liquid, and then vacuum After drying, the binary deep eutectic ionic liquid tetrabutylammonium bromide / imidazole is obtained. According to the DSC test, the eutectic temperature of this ionic liquid is 21°C; the viscosity at 70°C is 27.8cp. The conductivity at 130°C is 1.9×10 -2 Scm -1 ; Stable electrochemical window is 3.4V.

Embodiment 2

[0021] Preparation of Choline Chloride / Imidazolium Ionic Liquid

[0022] In the first step, imidazole is purified by recrystallization from toluene, choline chloride is purified by recrystallization from acetone, and vacuum-dried at 60°C to obtain pure imidazole and choline chloride.

[0023] In the second step, choline chloride 4.19g (0.03mol) and imidazole 4.77g (0.07mol) were weighed respectively, mixed uniformly, and heated at 100°C under stirring to obtain a homogeneous colorless liquid, and then vacuum-dried at 60°C, That is, the binary deep eutectic ionic liquid choline chloride / imidazole is obtained. According to the DSC test, the eutectic temperature of this ionic liquid is 56° C.; the viscosity at 70° C. is 15.0 cp. Conductivity at 130°C 5.2×10 -2 Scm -1 ; Stable electrochemical window is 3.0V.

Embodiment 3

[0025] Preparation of 1-ethyl-3-butylbenzotriazole hexafluorophosphate / imidazole ionic liquid

[0026] The first step, the purification of raw materials and the synthesis of 1-ethyl-3-butylbenzotriazole hexafluorophosphate

[0027] ①Imidazole was purified by recrystallization from toluene, and vacuum-dried at 60°C to obtain pure imidazole.

[0028] ②Synthesis and purification of 1-ethyl-3-butylbenzotriazole hexafluorophosphate

[0029] 20g of benzotriazole and 20ml of bromobutane were dissolved in 30% NaOH aqueous solution, then 1g of tetrabutylammonium bromide was added, stirred at 50°C for 10h, left to stand, and the upper layer was rotary evaporated at 70°C to obtain 1-butyl Benzotriazole. Pour 30g of 1-butylbenzotriazole and 13ml of bromoethane into a 100ml three-neck flask at 70°C and stir and reflux for 48-72h, the product is washed three times with ethyl acetate, and rotary evaporated at 70°C for 3h to obtain 1-ethyl- 3-Butylbenzotriazole bromide. Disperse 25g of 1-...

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Abstract

The invention discloses a binary eutectic ionic liquid and a preparation method thereof. The ionic liquid contains imidazole molecules and has a structure formula as shown on the right, wherein MX is tetrabutyl ammonium bromide, choline chloride or 1-ethyl-3-butyl-benzotriazole hexafluorophosphate. The preparation method comprises the following steps: mixing the tetrabutyl ammonium bromide, the choline chloride or the 1-ethyl-3-butyl-benzotriazole hexafluorophosphate with imidazole; heating the mixture to obtain a homogeneous phase colorless liquid; and vacuum-drying the colorless liquid to obtain the ionic liquid. The ionic liquid has good viscosity, electrical conductivity and stable electrochemical window, wherein the viscosity can reach 11.0 cp minimally at a temperature of 70 DEG C; the electrical conductivity can reach 5.2*10Scm maximally at a temperature of 130 DEG C; the stable electrochemical window can reach 3.4V maximally; besides, the preparation method is simple and environmentally-friendly.

Description

technical field [0001] The invention relates to the preparation of chemical materials, in particular to a binary deep eutectic ionic liquid and a preparation method thereof. technical background [0002] Ionic liquids have become one of the hotspots in green chemistry research and are known as green solvents in the 21st century. The advantages of ionic liquids as solvents or catalysts and their applications in chemical reactions, separation processes, electrochemistry and other fields have achieved many good experimental results. In addition, ionic liquids are promising in electrochemical applications such as solar cells and electric double layer capacitors, and can also be used in the preparation of high ion-conducting polymers, universal lubricants, and the dissolution of cellulose. However, most of the traditional ionic liquids are prepared by replacement, ion exchange or neutralization reaction, the preparation process is relatively complicated, and there are still prob...

Claims

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Application Information

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IPC IPC(8): C07D233/58C07C211/63C07C215/40C07D249/18
Inventor 单永奎张新华侯亚伟单冲冲王平
Owner EAST CHINA NORMAL UNIV
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