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1-butyl-3-methylimidazole-tri(hexafluoroacetylacetone) cobalt (II) complex magnetic ionic liquid, and preparation method and application thereof

A technology of hexafluoroacetylacetone and magnetic ionic liquid, applied in the field of preparation, 1-butyl-3-methylimidazolium triple cobalt magnetic ionic liquid, can solve separation difficulties, low recovery rate, unsuitable for liquid chromatography, etc. problems, to achieve the effect of expanding the scope of application, simple preparation method, and safe operation

Inactive Publication Date: 2019-09-20
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many problems in most magnetic ionic liquids, such as the hydrolysis of Fe in the solvent, which affects the extraction effect; the magnetic ionic liquid based on Mn is colorless, and the recovery rate is not high, which makes separation difficult and is not suitable for liquid chromatography; Ni High viscosity, easy to adsorb on the container wall; cumbersome synthesis of organic matter
Most of the Co-based magnetic ionic liquids currently reported are long-chain phosphine salts and nitrogen salts, and their solubility is not very good. There are problems in coupling with chromatographic instruments (mobile phase matching, etc.), and most of the current magnetic properties based on Co element Ionic liquids are in the laboratory stage, have not been widely used, and there are few types, and the design and development of new magnetic ionic liquids has broad prospects

Method used

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  • 1-butyl-3-methylimidazole-tri(hexafluoroacetylacetone) cobalt (II) complex magnetic ionic liquid, and preparation method and application thereof
  • 1-butyl-3-methylimidazole-tri(hexafluoroacetylacetone) cobalt (II) complex magnetic ionic liquid, and preparation method and application thereof
  • 1-butyl-3-methylimidazole-tri(hexafluoroacetylacetone) cobalt (II) complex magnetic ionic liquid, and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The first step, the preparation of anion

[0039] Add 1.5ml of ammonia water to 30mL of absolute ethanol, then seal the flask with plastic wrap, and add 1.3ml of hexafluoroacetylacetone dropwise into the flask through a syringe at a rate of about 1mL / min, white vapor appears. After the white vapor settled, 0.8 g of cobalt chloride was added. Cobalt chloride gradually dissolved, the solution was dark red, stirred at room temperature for 5h. Ethanol was rotary evaporated at 40 °C, the crude product was redissolved in 20 mL of ethyl acetate and washed several times with 5 mL aliquots of deionized water until the aqueous fraction was loaded with AgNO 3No precipitation occurs. Ethyl acetate was evaporated by rotary evaporation at 40°C, and vacuum-dried at 40°C for 8 hours to finally obtain a red solid powder.

[0040] The second step, the preparation of cations

[0041] 20ml of N-methylimidazole and 20ml of n-bromobutane were stirred and reacted overnight at 50°C to obta...

Embodiment 2

[0046] The first step, the preparation of anion

[0047] Add 1.5ml of ammonia water to 30mL of absolute ethanol, then seal the flask with plastic wrap, and add 1.3ml of hexafluoroacetylacetone dropwise into the flask through a syringe at a rate of about 1mL / min, white vapor appears. After the white vapor settled, 0.8 g of cobalt chloride was added. Cobalt chloride gradually dissolved, the solution was dark red, stirred at room temperature for 7h. Ethanol was rotary evaporated at 50 °C, the crude product was redissolved in 20 mL of ethyl acetate and washed several times with 5 mL aliquots of deionized water until the aqueous fraction was loaded with AgNO 3 No precipitation occurs. Ethyl acetate was evaporated by rotary evaporation at 50°C, and vacuum-dried at 50°C for 9h to finally obtain a red solid powder.

[0048] The second step, the preparation of cations

[0049] 20ml of N-methylimidazole and 20ml of n-bromobutane were stirred and reacted overnight at 75°C to obtain a...

Embodiment 3

[0054] The first step, the preparation of anion

[0055] Add 1.5ml of ammonia water to 30mL of absolute ethanol, then seal the flask with plastic wrap, and add 1.3ml of hexafluoroacetylacetone dropwise into the flask through a syringe at a rate of about 1mL / min, white vapor appears. After the white vapor settled, 0.8 g of cobalt chloride was added. Cobalt chloride gradually dissolved, the solution was dark red, stirred at room temperature for 8h. Ethanol was rotary evaporated at 60 °C, the crude product was redissolved in 20 mL of ethyl acetate and washed several times with 5 mL aliquots of deionized water until the aqueous fraction was loaded with AgNO 3 No precipitation occurs. Ethyl acetate was evaporated by rotary evaporation at 60°C, and vacuum-dried at 60°C for 10 h to finally obtain a red solid powder.

[0056] The second step, the preparation of cations

[0057] 20ml of N-methylimidazole and 20ml of n-bromobutane were stirred and reacted overnight at 100°C to obtai...

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Abstract

The invention discloses a 1-butyl-3-methylimidazole-tri(hexafluoroacetylacetone) cobalt (II) complex magnetic ionic liquid as well as a preparation method and application thereof. According to the method, 1-butyl-3-methylimidazole bromide and tri(hexafluoroacetylacetone) amine cobaltate complex are employed as monomers, and the 1-butyl-3-methylimidazole-tri(hexafluoroacetylacetone) cobalt (II) complex magnetic ionic liquid is prepared by using an ion exchange. The 1-butyl-3-methylimidazole-tri(hexafluoroacetylacetone) cobalt (II) magnetic ionic liquid is in a solid state at normal temperature, can be dissolved in methanol and acetonitrile, can keep a certain viscosity, and is insoluble in water. By using dispersion liquid-liquid micro-extraction technology, the liquid can directly enter a liquid chromatograph and can be simply and conveniently used for analysis and testing. Compared with common magnetic ionic liquid, the process for preparing the magnetic ionic liquid has the advantages of being simple in synthesis step, low in viscosity, obvious in color, high in thermal stability, safe, stable, good in machinability and the like. Besides, the prepared magnetic ionic liquid is easy to process, has paramagnetism, and is matched with a liquid chromatogram mobile phase, so that the application range of the magnetic ionic liquid can be expanded.

Description

technical field [0001] The invention belongs to the technical field of magnetic ionic liquids and preparation thereof, and relates to a Co-based magnetic ionic liquid and a preparation method thereof, in particular to 1-butyl-3-methylimidazole tris(hexafluoroacetylacetonate)cobalt(II) magnetic Ionic liquid, preparation method and application. Background technique [0002] Due to its excellent characteristics, ionic liquids have received extensive attention in recent years, and ionic liquids with magnetism, namely magnetic ionic liquids, have attracted more attention because they have a certain magnetization ability in addition to the excellent characteristics of ionic liquids. shows great potential for development. This magnetization ability makes magnetic ionic liquids have their unique advantages in the analytical chemical pretreatment process. Using their magnetism, they can achieve rapid separation, and can complete extraction, enrichment, and centrifugation in one step...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58C07C45/77C07C49/92H01F1/44G01N30/06
CPCC07D233/58H01F1/44G01N30/06
Inventor 乔利珍郑可欣于春梅
Owner DALIAN UNIV OF TECH
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