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Ionic liquid bis-ammonium acetate and catalytic synthesis process therefor

A technology of ionic liquid and synthesis method, applied in the fields of organic chemistry, carboxylate preparation, etc., can solve the problems of pollution, lack of raw materials, and high cost, and achieve the effects of huge application prospects, simple process flow, and high safety.

Inactive Publication Date: 2005-01-26
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are several shortcomings in the preparation of existing ionic liquids: lack of raw materials, high cost, generally more than twice that of common solvents; more steps in preparation, difficult, difficult product purification, not suitable for large-scale industrial production and application ;Usually the combination of quaternary ammonium salt and aluminum trichloride is likely to cause pollution and affect its application in green chemical industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the first step, in a reactor equipped with electric stirring, add 100 g of glacial acetic acid, 80.2 g of acetone, and then add 1.27 g of SO 4 2- / ZrO 2 . In the second step, react at 40°C for 2 hours under stirring. The third step is cooling, neutralizing with concentrated ammonia water in an ice-water bath to pH = 7-8, filtering to remove the precipitate, and the filtrate is distilled at atmospheric pressure to recover the low-boiling fraction, and then distilled under reduced pressure at 1.47Kpa to collect 71-72 ℃ fraction, at room temperature, 95.9g of white solid was obtained, which was ammonium diacetate, and the productive rate was: 70%. 1 HNMR, 13 CNMR and elemental analysis confirmed the resulting product.

Embodiment 2

[0027] In the first step, in a reactor equipped with electric stirring, add 100 g of glacial acetic acid, 89.3 g of benzene, and then add 2.54 g of SO 4 2- / ZrO 2 . In the second step, react at 50°C for 2 hours under stirring. The third step is the same as that of Example 1 and will not be repeated here.

Embodiment 3

[0029] In the first step, in a reactor equipped with electric stirring, add 100 g of glacial acetic acid, 88.3 g of toluene, and then add 3.81 g of SO 4 2- / ZrO 2 . In the second step, react at 50°C for 2 hours under stirring. The third step is the same as that of Example 1 and will not be repeated here.

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Abstract

The invention discloses an ionic liquid bis-ammonium acetate and catalytic synthesis process, wherein the acetate comprises small cationic inorganic ammonium NH4++ and rather big anion double acetate radical (CH#-[3]COO)#-[2]H#+[-], the catalytic method for synthesizing the ionic liquid consists of mixing acetic acid, mixing the solid acid catalyst and solvent, heating and stirring, reacting, neutralizing with acid and alkali, separating, decompression distilling.

Description

technical field [0001] The invention relates to an ionic liquid ammonium diacetate and a catalytic synthesis method thereof, belonging to the technical field of new chemical materials and their preparation. Background technique [0002] Ionic liquids refer to substances composed of anions and cations with a melting point lower than 100°C. Because this kind of substance has a wide temperature range in liquid state, which can reach 300°C; low vapor pressure, low volatility, high density, and good thermal stability; its physical and chemical properties can be adjusted by changing anions and cations; the electrochemical window is wide, about 4V It is widely used as solvent and catalyst in organic synthesis, solvent and extractant in chemical separation, electrolyte and medium in electrochemistry, and has shown excellent performance. In recent years, the deteriorating environmental quality has increasingly demanded the greening of the chemical producti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C55/07
Inventor 单永奎蔡清海张达崴孔爱国戴立益
Owner EAST CHINA NORMAL UNIV
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