Functionalized ionic liquid containing a phosphorus and oxygen structure, and preparation method and application thereof

A technology of ionic liquid and anion, which is applied in the preparation of the aforementioned ionic liquid, the application of uranium in the extraction of uranium-containing water system, and the field of functionalized ionic liquid, which can solve the problems that hinder the smooth progress of the extraction process.

Inactive Publication Date: 2010-09-22
BEIJING RES INST OF CHEM ENG & METALLURGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With conventional alkylimidazole hydrophobic room temperature ionic liquids such as [C 8 mim][PF 6 ] or [C 4 mim][PF 6 ] as a diluent, compounded with uranium extractant tributyl phosphate (TBP) to extract uranium in uranium-containing water system, which can obtain higher extrac

Method used

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  • Functionalized ionic liquid containing a phosphorus and oxygen structure, and preparation method and application thereof
  • Functionalized ionic liquid containing a phosphorus and oxygen structure, and preparation method and application thereof
  • Functionalized ionic liquid containing a phosphorus and oxygen structure, and preparation method and application thereof

Examples

Experimental program
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Example Embodiment

In a 250mL four-necked flask equipped with a stirrer, a constant pressure dropping funnel, a thermometer and an airway tube, add 25wt% NaOH aqueous solution (30mL), 2-bromoethanol (12.5g, 0.1mol), carbon tetrachloride ( 25mL), dichloromethane (25mL) and tetrabutylammonium bromide (0.36g, 1.12mmol), stirred to mix, ice-water bath to control the temperature of the mixed system at 10 ~ 15 ℃; di-n-butyl phosphite ( 24.3g, 0.125mol) and carbon tetrachloride (30mL) were mixed uniformly in the constant pressure dropping funnel, and then dropped dropwise into the above-mentioned 2-bromoethanol mixed system. The reaction was continued for 3 hours. After the reaction, the system was diluted with dichloromethane (20mL), filtered, and the obtained filtrate was washed three times with 2wt% dilute hydrochloric acid (20mL) and deionized water (20mL) three times, then dried with anhydrous sodium sulfate, and rotary evaporated After removal of carbon tetrachloride and dichloromethane, 2-bromo...

Example Embodiment

Embodiment 2: Preparation of 1-(di-n-butyl-n-propyl phosphate)-3-methylimidazolium bromide

In a 250mL four-necked flask equipped with a stirrer, a constant pressure dropping funnel, a thermometer and an airway tube, add 25wt% NaOH aqueous solution (30mL), 2-bromoethanol (12.5g, 0.1mol), carbon tetrachloride ( 25mL), dichloromethane (25mL) and tetrabutylammonium bromide (0.36g, 1.12mmol), stirred to mix, ice-water bath to control the temperature of the mixed system at 10 ~ 15 ℃; di-n-butyl phosphite ( 24.3g, 0.125mol) and carbon tetrachloride (30mL) were mixed uniformly in the constant pressure dropping funnel, and then dropped dropwise into the above-mentioned 2-bromoethanol mixed system. The reaction was continued for 3 hours. After the reaction, the system was diluted with dichloromethane (20mL), filtered, and the obtained filtrate was washed three times with 2wt% dilute hydrochloric acid (20mL) and deionized water (20mL) three times, then dried with anhydrous sodium sulfate...

Example Embodiment

Example 3: Preparation of 1-(di-n-butyl-n-propyl phosphate)-3-methylimidazolium hexafluorophosphate

Weigh 4.13g (0.01mol) of 1-(di-n-butyl-n-propyl phosphate)-3-methylimidazolium bromide, dissolve it in 30mL absolute ethanol, weigh 1.09g (0.01mol) of sodium tetrafluoroborate mol), was added to the aforementioned solution, and stirred and reacted at room temperature for 24 hours. The upper aqueous phase was poured off, and the lower oil phase was repeatedly washed with deionized water until no bromide ion (silver nitrate test) was present, and vacuum-dried for 24 hours to obtain a colorless viscous liquid. The obtained product was confirmed to be the compound described in the title by infrared spectrum and nuclear magnetic resonance spectrum analysis, and the yield was 50%. FTIR (cm -1 ): 3159, 3119, 2964, 2877, 1576, 1471, 1396, 1370, 1338, 1259, 1171, 1027, 877, 763, 623. 1 H NMR (D 2 O): δ=8.59(s, 1H), 7.34(d, 2H), 4.17-4.21(m, 4H), 3.97-4.01(m, 4H), 3.69-3.72(s, 3H), 3....

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Abstract

The invention relates to functionalized ionic liquid containing a phosphorus and oxygen structure with a general formula of A+ B-, which is characterized in that A+ is shown in a formula (I), and R 1 and R 2 are defined in the specification; and B- is Cl-, Br-, I -, BF4-, PF6-, NO3-, CF3SO3-, [(CF3SO2) 2N] - or CH3CO2-. The invention also relates to a method for preparing ionic liquid with the formula of A + B-, which comprises the following steps: a compound in a formula (III) is reacted with a compound in a formula (II ') to obtain a compound in a formula (II'') , and then a compound in a formula (II'') is reacted with a compound in a formula (IV) to obtain a halide ionic liquid A + B-, wherein B- is Cl-, Br-or I-, and ionic liquids with the other anions can be obtained by carrying out the ion exchange of the halide ionic liquid. The invention also relates to application of the ionic liquids in extraction of uranium from uranium-containing water systems. HO-(CH2) nCH2-X (III).

Description

technical field The invention relates to an imidazole-type ionic liquid, in particular to a functionalized ionic liquid (TSILs, Task Specific Ionic Liquids or FILs, Functionalized Ionic Liquids) containing phosphorus and oxygen structures. The present invention also relates to the preparation method of the aforementioned ionic liquid and the application of the ionic liquid, especially the application of extracting uranium in the uranium-containing water system. Background technique Compared with traditional organic solvents and electrolytes, ionic liquids have a series of outstanding advantages: (1) almost no vapor pressure, non-volatile, colorless, and odorless; (2) have a larger stable temperature range and better chemical stability (3) The solubility of inorganic substances, organic substances and polymers can be adjusted through the design of anions and cations. Due to the above excellent properties, it is regarded as a "green" solvent, which can replace the conventiona...

Claims

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Application Information

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IPC IPC(8): C07F9/6506C22B3/38C22B60/02
Inventor 李宏宇刘浩窦军彦刘正平
Owner BEIJING RES INST OF CHEM ENG & METALLURGY
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