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A kind of ionic liquid with adjustable polarity and its preparation method and application

An ionic liquid, polar technology, applied in extraction purification/separation, organic chemistry, etc., can solve the problems of strong volatility and high viscosity of single-component polar adjustable solvents, achieve good economic benefits, good repeatability, synthesis The effect of simple process

Active Publication Date: 2019-03-08
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reported two-component polarity-adjustable solvents are sensitive to moisture and require a rigorous drying pretreatment process; the one-component polarity-adjustable solvents are highly volatile or have high viscosity

Method used

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  • A kind of ionic liquid with adjustable polarity and its preparation method and application
  • A kind of ionic liquid with adjustable polarity and its preparation method and application
  • A kind of ionic liquid with adjustable polarity and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The synthesis device of the ionic liquid is a three-necked flask equipped with a stirring paddle and a dropping funnel. Weigh a certain amount of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), add it into a three-necked flask and stir. Accurately weigh TFE according to the ratio of DBU to 2,2,2-trifluoroethanol (TFE) molar ratio of 1:1 and add it to the dropping funnel. Control the reaction temperature to 0°C, open the dropping funnel, and slowly drop TFE into the kettle. After the dropwise addition, continue to stir in the kettle for 0.5h. Afterwards, the solution was rotated and evaporated under reduced pressure at 30 °C for 2 h to remove excess TFE, and the polarity-tunable ionic liquid [DBUH + ][TFE - ]. The experimental raw materials did not require any drying treatment.

Embodiment 2

[0052] The synthesis device of the ionic liquid is a three-necked flask equipped with a stirring paddle and a dropping funnel. Weigh a certain amount of tetramethylguanidine (TMG), add it into a three-neck flask and stir. Accurately weigh TFE according to the ratio of TMG to 2,2,2-trifluoroethanol (TFE) molar ratio of 1:0.5 and add it to the dropping funnel. The reaction temperature was controlled at 5°C, the dropping funnel was opened, and TFE was slowly added dropwise into the kettle. After the dropwise addition, continue to stir in the kettle for 2h. Afterwards, the solution was rotary evaporated under reduced pressure at 50 °C for 3 h to remove excess TMG, and the polarity-tunable ionic liquid [TMGH + ][TFE - ]. The experimental raw materials did not require any drying treatment.

[0053] Carry out to the ionic liquid of embodiment 1, embodiment 2 1 H. 13 C NMR analysis is compared with DBU, TMG, TFE standard spectra, and the analysis data is recorded in the followi...

Embodiment 3

[0058] The synthesis device of the ionic liquid is a three-necked flask equipped with a stirring paddle and a dropping funnel. Weigh a certain amount of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), add it into a three-necked flask and stir. Accurately weigh TFP according to the ratio of DBU to 2,2,3,3-tetrafluoropropanol (TFP) molar ratio of 1:1.1 and add it to the dropping funnel. Control the reaction temperature to 10°C, open the dropping funnel, and slowly drop TFP into the kettle. After the dropwise addition, continue to stir in the kettle for 2.5h. Afterwards, the solution was rotated and evaporated under reduced pressure at 55 °C for 4 h to remove excess TFP, and the polarity-tunable ionic liquid [DBUH + ][TFP - ]. The experimental raw materials did not require any drying treatment.

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Abstract

The invention provides a polarity-adjustable ionic liquid, and a preparation method and application thereof. Especially, the polarity-adjustable ionic liquid is not sensitive to water molecules, the polarity of the system can be adjusted by taking CO2 as a molecular switch, and the ionic liquid is applied to circulate and separate low-polarity organic compounds. The polarity-adjustable ionic liquid is prepared by taking an organic alkali and a fluorine-substituted alcohol as raw materials and performing proton transfer reaction, and the ionic liquid is an ionic liquid before and after absorbing CO2. The polarity-adjustable ionic liquid is low in cost and simple in preparation method. The polarity-adjustable ionic liquid absorbing CO2 is increased in polarity, and is capable of separating out low-polarity organic compounds dissolving in the polarity-adjustable ionic liquid. Then CO2 is released through slightly heating, and low polarity of the polarity-adjustable ionic liquid is recovered. The polarity-adjustable ionic liquid is capable of repeatedly dissolving low-polarity organic compounds from mixtures and reaction systems, then helps to separate out low-polarity organic compounds by utilizing CO2 and is good in repeatability.

Description

technical field [0001] The invention relates to an ionic liquid with adjustable polarity and its preparation method and application, belonging to the field of organic chemical industry. Background technique [0002] In chemical production, multi-step reactions and separation processes are often involved, and the optimal solvent required for each step may be different. The physical properties of traditional solvents are relatively fixed. After each reaction step, the solvent needs to be removed or replaced, which not only increases the economic cost but also brings pollution to the environment. Supercritical fluids and gas-expandable liquids can change their physical properties through temperature and pressure, and can be used for extraction and separation, but the required pressure is high and the operation is complicated. Therefore, it is of great significance to develop a new type of solvent to simplify the tedious chemical separation steps. [0003] Ionic liquids are sa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04C07C279/04C07C31/38C07C7/10C07C9/15C07C9/21C07C15/107C07C11/02C07C13/18C07C13/20
CPCC07C7/10C07C31/38C07C279/04C07C2601/14C07C2601/16C07D487/04C07C9/15C07C9/21C07C15/107C07C11/02C07C13/18C07C13/20
Inventor 刘植昌胡鹏程孟祥海张睿徐春明
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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