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Chelate type ionic liquid and preparation and purification method thereof

A technology of ionic liquid and purification method, which is applied in the field of chelating ionic liquid and its preparation and purification, and can solve the problems of unstable decomposition of carboxylic anions

Inactive Publication Date: 2012-01-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2009, Yoshida et al. reported a dark green Co-containing room temperature ionic liquid with 4,4'-dicarboxylic acid-2,2'-bipyridine as the chelating ligand anion and an asymmetric tetradecyltri-n-hexylphosphine cation. However, it decomposes at around 75°C, which may be due to the instability caused by the decomposition of carboxylic acid anions. (Inorg.Chem.48 (2009) 9989) From the current research situation, the preparation of a stable metal-containing room temperature ionic liquid remains a major challenge

Method used

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  • Chelate type ionic liquid and preparation and purification method thereof
  • Chelate type ionic liquid and preparation and purification method thereof
  • Chelate type ionic liquid and preparation and purification method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 0.208g, 1mmol of hexafluoroacetylacetone and 15ml of acetonitrile into a 50ml round-bottom single-necked flask, put it in a water bath at 35°C, and then add ammonia water. After 24 hours of reaction, CoCl was added 2 .4H 2 O 0.33mmol, carry out again 8 hours, add trimethyl n-hexadecyl ammonium bromide 0.33mmol, react and carry out 10 hours again, filter and remove inorganic salt (NH 4 Br, NH 4 Cl), the acetonitrile was evaporated by a rotary evaporator to obtain a red liquid, which became solid after cooling.

[0041] Dissolve the obtained crude product in 10 mL of ethyl acetate, then add an equal volume of water, shake for 3 minutes, and separate into layers. The upper layer is the ionic liquid phase, and the lower layer is the water phase. Separation to remove the water layer, repeat the above steps 3 times , the rich ionic liquid phase was collected, and the solvent was removed by a rotary evaporator, and the resulting product was vacuum-dried for 24 hours to ...

Embodiment 2

[0043] Add 0.208g, 1mmol of hexafluoroacetylacetone and 15ml of acetonitrile into a 50ml round-bottom single-necked flask, put it in a water bath at 35°C, and then add ammonia water. After 24 hours of reaction, CoCl was added 2 .4H 2 O 0.33mmol, carry out again 8 hours, add tetrabutylammonium chloride 0.33mmol, react and carry out 10 hours again, filter and remove inorganic salt (NH 4 Cl), the acetonitrile was evaporated by a rotary evaporator to obtain a red liquid, which became solid after cooling.

[0044] Dissolve the obtained crude product in 10 mL of ethyl acetate, then add an equal volume of water, shake for 3 minutes, and separate into layers. The upper layer is the ionic liquid phase, and the lower layer is the water phase. Separation to remove the water layer, repeat the above steps 3 times , the rich ionic liquid phase was collected, and the solvent was removed by a rotary evaporator, and the resulting product was vacuum-dried for 24 hours to obtain purified [(C ...

Embodiment 3

[0046] Add 0.208g, 1mmol of hexafluoroacetylacetone and 15ml of acetonitrile into a 50ml round-bottom single-necked flask, put it in a water bath at 35°C, and then add ammonia water. After 24 hours of reaction, CoCl was added 2 .4H 2 O 0.33mmol, carry out 8 hours again, add triphenyl n-butyl phosphine chloride 0.33mmol, react and carry out 10 hours again, filter and remove inorganic salt (NH 4 Cl), the acetonitrile was evaporated by a rotary evaporator to obtain a red liquid, which became solid after cooling.

[0047] Dissolve the obtained crude product in 10 mL of ethyl acetate, then add an equal volume of water, shake for 3 minutes, and separate into layers. The upper layer is the ionic liquid phase, and the lower layer is the water phase. Separation to remove the water layer, repeat the above steps 3 times , the rich ionic liquid phase was collected, and the solvent was removed by a rotary evaporator, and the obtained product was vacuum-dried for 24 hours to obtain purifi...

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Abstract

The invention relates to chelate type ionic liquid prepared by using coordinating capacity of beta-diketone anions. The chelate type ionic liquid is prepared by combining different cations and different anions. The cations may be quaternary amine, quaternary phosphorus, alkyl pyridine, alkyl iminazole or the like, the anions may be different alkyls, fluorinated alkyl, phenyl or furyl substituted beta-diketone complex ions and the metal may be Cu, Ni, Co, Mn, Cr, Zn or Fe. The preparation process of the chelate type ionic liquid is simple, quick, and low in energy consumption, does not require any strict conditions and makes product purification easy; and the chelate type ionic liquid has high chemical stability and high thermodynamic stability, and the melting point is easy to regulate. The ionic liquid enriches the ionic liquid range greatly and has high potential use value.

Description

technical field [0001] The invention relates to a new method for preparing chelated ionic liquids by utilizing the coordination ability of β-diketone anions, and a new type of chelated metal-containing ionic liquid prepared by combining different cations, different anions and different metals of ionic liquids. Background technique [0002] Ionic liquids are composed of organic cations and inorganic or organic anions, and are liquid salts at room temperature or below 100°C. Since the 1990s, ionic liquids have attracted increasing research interest from scientists due to their unique properties: low vapor pressure, wide liquid range, good electrical conductivity, and designability. With the introduction of the concept of "green chemistry" and the increase of global environmental pressure, ionic liquids are used as a new reaction medium in more and more fields. [0003] Since the first generation of ionic liquids - chloroaluminate ionic liquids, metal-containing ionic liquids...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/68C07C49/92C07C45/77C07F9/54C07D233/58C07D213/20
Inventor 李浩然张鹏飞王从敏
Owner ZHEJIANG UNIV
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