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Phosphate ionic liquid and preparation method of phosphate ionic liquid, application and extraction method

An ionic liquid and phosphate ester technology, applied in the field of lithium extraction, can solve the problems of ionic liquid loss, low extraction efficiency, etc., and achieve the effects of reducing the use ratio, improving extraction performance, and solving low extraction efficiency.

Active Publication Date: 2021-01-26
QINGHAI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the above-mentioned deficiencies in the prior art, the present invention provides a phosphate-based ionic liquid and its preparation method, application and extraction method, in which a phosphate group having a strong extraction performance for lithium is introduced into the cation of the ionic liquid, and at the same time Select hexafluorophosphate or bistrifluoromethylsulfonimide as anion to prepare phosphate ionic liquid, use this phosphate ionic liquid as extraction agent to extract and separate lithium ions in salt lake brine, effectively solve the problem of Solved the problems of low extraction efficiency and loss of ionic liquid in the prior art

Method used

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  • Phosphate ionic liquid and preparation method of phosphate ionic liquid, application and extraction method
  • Phosphate ionic liquid and preparation method of phosphate ionic liquid, application and extraction method
  • Phosphate ionic liquid and preparation method of phosphate ionic liquid, application and extraction method

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Embodiment 1

[0032]A phosphate ionic liquid, the preparation method thereof includes the following steps:

[0033](1) Into a four-necked flask equipped with a stirrer, a constant pressure dropping funnel, a thermometer, and a gas tube, sequentially add 25wt% sodium hydroxide aqueous solution (35mL), 3-bromopropanol (20.85g), carbon tetrachloride (30mL), dichloromethane (30mL), and tetrabutylammonium bromide (TBAB, 0.39g). Combine di-n-butyl phosphite (36.38g) with carbon tetrachloride at 10-15°C in an ice-water bath. The mixed solution (35mL) was slowly dropped into the above system through a constant pressure dropping funnel, the ice-water bath was removed, and the reaction was carried out at room temperature for 4h, diluted and filtered with dichloromethane (25mL), and then successively used 2vt% dilute hydrochloric acid (25mL) Washed 3 times, deionized water (25mL) washed 3 times, and then dried over anhydrous sodium sulfate, carbon tetrachloride and dichloromethane were removed under reduced pr...

Embodiment 2

[0044]A phosphate ionic liquid, the preparation method thereof includes the following steps:

[0045](1) Into a four-necked flask equipped with a stirrer, a constant pressure dropping funnel, a thermometer, and a gas tube, sequentially add 25wt% sodium hydroxide aqueous solution (35mL), 4-bromobutanol (22.95g), carbon tetrachloride (30mL), dichloromethane (30mL) and tetrabutylammonium bromide (TBAB, 0.39g), and diisoamyl phosphate (44.44g) and carbon tetrachloride (35mL The mixed solution of) was slowly dropped into the above system through a constant pressure dropping funnel, the ice-water bath was removed, and the reaction was carried out at room temperature for 4 hours, diluted and filtered with dichloromethane (25mL), and then washed with 2vt% dilute hydrochloric acid (25mL) 3 After washing three times with deionized water (25 mL), drying with anhydrous sodium sulfate, removing carbon tetrachloride and dichloromethane under reduced pressure, to obtain compound I (phosphoric acid-br...

Embodiment 3

[0056]A phosphate ionic liquid, the preparation method thereof includes the following steps:

[0057](1) Into a four-necked flask equipped with a stirrer, a constant pressure dropping funnel, a thermometer, and a gas tube, sequentially add 25wt% sodium hydroxide aqueous solution (35mL), 4-bromobutanol (22.95g), carbon tetrachloride (30mL), dichloromethane (30mL) and tetrabutylammonium bromide (TBAB, 0.39g), and dibutyl phosphite (36.38g) and carbon tetrachloride (35mL The mixed solution of) was slowly dropped into the above system through a constant pressure dropping funnel, the ice-water bath was removed and the reaction was carried out at room temperature for 4 hours, diluted and filtered with dichloromethane (25mL), and then washed with 2vt% dilute hydrochloric acid (25mL) 3 After washing three times with deionized water (25 mL), drying with anhydrous sodium sulfate, removing carbon tetrachloride and dichloromethane under reduced pressure, to obtain compound I (phosphoric acid-bromo...

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Abstract

The invention discloses phosphate ionic liquid and a preparation method of the phosphate ionic liquid, application and an extraction method. The preparation method of the ionic liquid comprises the following steps that dialkyl phosphate is dropwise added into bromo-alkyl alcohol for reaction, and then diluting, filtering, washing, drying and decompressing are conducted to obtain a compound I; thecompound I is mixed with alkyl imidazole, washing and drying in vacuum are conducted to obtain a compound II; and the compound II is mixed with hexafluorophosphate or bis trifluoromethyl sulfonyl salt, leaving the mixture to stand, separating, washing and drying in vacuum are conducted to obtain the phosphate ionic liquid. The invention further comprises the ionic liquid prepared by the method, application and an extraction method of the ionic liquid in lithium extraction. According to the phosphate ionic liquid and preparation method of the phosphate ionic liquid, the application and the extraction method, phosphate groups are introduced into cations of the ionic liquid, hexafluorophosphate or bis trifluoromethyl sulfonyl sulfimide is selected as anions to prepare the ionic liquid, and lithium ions are extracted and separated, so that the problems of low extraction efficiency, ionic liquid loss and the like in the prior art are effectively solved.

Description

Technical field[0001]The invention relates to the technical field of lithium extraction, in particular to a phosphate ester type ionic liquid, its preparation method, application and extraction method.Background technique[0002]Lithium, known as "white gold" in the 21st century, is the alkali metal with the smallest atomic radius and the lightest mass. Because of its unique physical and chemical properties, it is used in aerospace, lithium batteries, aluminum-lithium alloys, high-speed rail, aircraft, military and marine Widely used in other fields, lithium and lithium salts have been regarded as important new energy and strategic resources. Lithium exists in nature in the form of solid lithium ore and lithium-rich natural water. Lithium in salt lake brine is an important source of all economic lithium products. my country has abundant salt lake lithium resources, mainly distributed in Qinghai Lake District and Tibet Lake District. Compared with foreign salt lakes, my country's salt ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B26/12C22B3/38
CPCC22B26/12C22B3/387Y02P10/20
Inventor 石成龙秦亚茹李宏霞卢娜娜
Owner QINGHAI UNIV FOR NATITIES
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