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Method for preparing quaternary amine dual-functional ionic liquid

An ionic liquid, dual-function technology, applied in chemical instruments and methods, preparation of carboxylates, preparation of amino compounds from amines, etc., to achieve the effects of low cost of raw materials, simple synthesis route, and simple equipment

Inactive Publication Date: 2010-06-09
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the patent for the synthesis of quaternary ammonium bifunctional ionic liquids has not been reported yet.

Method used

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  • Method for preparing quaternary amine dual-functional ionic liquid
  • Method for preparing quaternary amine dual-functional ionic liquid
  • Method for preparing quaternary amine dual-functional ionic liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: Ion exchange method prepares [A336][NO 3 ]

[0037] According to the steps described in the synthesis route of the ion exchange method in the technical background, 8.5 g of sodium nitrate (0.1 mol) was dissolved in 20 mL of deionized water. Then 40.457 g (0.1 mol) of Aliquat336 was dissolved in 50 mL of acetone. Under magnetic stirring, the acetone solution containing Aliquat336 was added dropwise to the sodium nitrate aqueous solution, the acetone-water solution was stirred at room temperature for 1 h, the layers were left to stand, and the upper phase was taken out. Rotate the upper phase with a rotary evaporator at 80°C for 50 minutes to spin out the isopropanol and water contained in it to obtain [A336][NO 3 ]. The above [A336][NO 3 ] was dissolved in 50 mL of acetone and the sodium chloride was filtered off with a 4.5 micron filter. Spinning for another hour removes the acetone to give [A336][NO 3 ] (structure as shown in formula 1). Income[A33...

Embodiment 2

[0038] Embodiment 2: the influence of methanol, ethanol, propanol, isopropanol on preparation [A336][OH]

[0039] Dissolve 112.36 grams of Aliquat 336 in 500 mL of distilled methanol, ethanol, propanol, and isopropanol, and dissolve them completely. Add 6.39 g of metallic sodium to 5 plastic bottles, then add 125 mL of distilled methanol, ethanol, propanol, and isopropanol, and react at room temperature for 3 hours to prepare sodium alkoxide. The above solutions were mixed and stirred at 50°C for 4 hours to prepare [A336][OR]. The resulting solution was centrifuged at 8000 rpm for 10 minutes to remove the sodium chloride precipitate. Add 500 ml of deionized water to the filtrate, shake for 30 minutes, and perform hydrolysis to prepare [A336][OH]. Take 1 ml of the above-mentioned [A336][OH], respectively, and use bromothymol blue as an indicator to titrate with hydrochloric acid with a concentration of 0.132 mol / L. It is measured that the yields of [A336][OH] prepared by met...

Embodiment 3

[0040] In order to determine the influence of different types and concentrations of acids on [A336][OH] titration, take 1 ml of the above-mentioned [A336][OH] respectively, use bromothymol blue as indicator, and use hydrochloric acid with a concentration of 0.132mol / l Titration was carried out and the result was 0.121 mol / l. Under the same conditions, titrate with nitric acid with a concentration of 0.298 mol / l, and the result is 0.123 mol / l. The results showed that different types and concentrations of acids had little effect on the titration results.

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Abstract

The invention relates to a method for preparing quaternary amine dual-functional ionic liquid. The quaternary amine dual-functional ionic liquid is prepared by sequentially adopting an anion exchange reaction, a hydrolysis reaction and an acid-alkali neutralizing reaction; a synthetic route is simple; the reaction can be completed at the normal temperature and under the normal pressure with moderate reaction conditions; an apparatus is simple; in the process of preparing the quaternary amine dual-functional ionic liquid by quaternary ammonium hydroxide and acid through the acid-alkali neutralizing reaction, the reaction is sufficient; through ICP-MS and ionic chromatographic detection, the content of sodion and chloridion in the methyl trioctylphosphine ammonium nitric acid ionic liquid prepared by the acid-alkali neutralizing reaction is obviously lower than that of the methyl trioctylphosphine ammonium nitric acid ionic liquid prepared by the anion exchange reaction. In the invention, superficial characteristics on the decomposition temperature, the density, the moisture content of the prepared dual-functional ionic liquid and the intersolubility of normal organic solvents are carried out.

Description

technical field [0001] The invention relates to a preparation method of a quaternary ammonium bifunctional ionic liquid. technical background [0002] Ionic liquids are a class of "designable" liquid functional materials. They have the characteristics of wide liquid temperature range, low vapor pressure, low volatility, high density, good solubility for some organic and inorganic substances, wide electrochemical window, and strong solubility. Due to these properties of ionic liquids, their applications in catalysis, electrochemistry, synthesis, separation and other fields have attracted increasing attention [N.V.Plechkova and K.R.Seddon.Chem.Soc.Rev., 2008, 1, 123-150]. In related industrial processes, the application of ionic liquids has been widely carried out. In recent years, ionic liquids have been used in nuclear waste treatment [W.R.Pitner, D.Hebditch, J.Hatter D.W.Rooney, K.R.Seddon and R.C.Thied, World Pat., WO 01 / 13379, 2001 (British Nuclear Fuels Plc)], solar ce...

Claims

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Application Information

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IPC IPC(8): C07F9/40C07F9/30C07C211/63C07C209/68C07C59/70C07C51/41
Inventor 陈继孙晓琦纪杨刘郁
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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