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A method for extracting and separating rare earth yttrium by using pyridine carboxylic acid ionic liquid

A pyridine carboxylic acid, ionic liquid technology, applied in the direction of improving process efficiency, can solve the problems of difficult to achieve high-efficiency separation and purification of yttrium, low separation coefficient, easy volatility, etc., achieves no saponification in operation, good separation performance, and improved selection. sexual effect

Active Publication Date: 2022-02-11
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the low separation coefficient of yttrium, holmium and erbium in the industry, it is difficult to realize the efficient separation and purification of yttrium, and the traditional organic solvents used in the daily extraction and separation process are volatile and toxic. The method for extracting and separating the rare earth element yttrium by pyridine carboxylic acid ionic liquid, the pyridine carboxylic acid ionic liquid used has stable chemical properties and is non-volatile, and the carboxylic acid functional group can significantly improve the extraction and separation performance of yttrium, the extraction time is short, the operation is simple, and the ion liquid recyclable

Method used

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  • A method for extracting and separating rare earth yttrium by using pyridine carboxylic acid ionic liquid
  • A method for extracting and separating rare earth yttrium by using pyridine carboxylic acid ionic liquid
  • A method for extracting and separating rare earth yttrium by using pyridine carboxylic acid ionic liquid

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Experimental program
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Effect test

Embodiment 1

[0033] Ionic liquid [(CH 2 ) n Preparation of COOHpyr][Br], n=3,4,5,6,7

[0034] Dissolve 0.2mol of 4-bromobutyric acid, 5-bromopentanoic acid, 6-bromohexanoic acid, 7-bromoheptanoic acid, and 8-bromooctanoic acid in 50ml of ethanol, and then add them dropwise to a three-necked flask containing equimolar pyridine , stirred magnetically at 70°C for 48h, condensed and refluxed. After the reaction, a precipitate was produced, and the excess ethanol was removed by rotary evaporation. The product was washed more than 10 times with ethyl acetate, and dried under vacuum at 65 °C for 48 h to obtain 5 powdery solids [(CH 2 ) n COOHpyr][Br], n=3, 4, 5, 6, 7, the yields were 88.4%, 89.6.7%, 93.1%, 95.7%, 95.8%, respectively.

Embodiment 2

[0036] Ionic liquid [(CH 2 ) n COOHpyr][NTf 2 ], the preparation of n=3,4,5,6,7

[0037] LiNTf 2 Respectively with the [(CH 2 ) n COOHpyr] [Br], n = 3, 4, 5, 6, 7, ion exchange reaction was performed in deionized water, magnetically stirred at room temperature for 12 hours, left to stand and separated, and the lower layer was the reaction product. The product was washed several times with deionized water until no white precipitate was detected by saturated silver bromide solution, and then the P 2 o 5 As a desiccant, vacuum-dried at 65°C for 24 hours to obtain five viscous ionic liquids [(CH2 ) n COOHpyr][NTf 2 ], n=3, 4, 5, 6, 7, the yields were 89.3%, 92.7%, 93.8%, 95.7%, 96.5%, respectively.

Embodiment 3

[0039] Pyridine carboxylic acid ionic liquid [(CH 2 ) 3 COOHpyr][NTf 2 ] to the extraction and separation of yttrium

[0040] 1) The rare earth hydrochloric acid solution containing yttrium is used as the raw material liquid, the concentration of yttrium in the raw material liquid is 0.015mol / L, and the pH value is 2.51.

[0041] 2) configure the ionic liquid phase, select pyridine carboxylic acid ionic liquid [(CH 2 ) 3 COOHpyr][NTf 2 ] is the extractant, select [C 4 mim][NTf 2 ] As a diluent, the concentration of the extractant in the ionic liquid phase is 0.2mol / L.

[0042] 3) The raw material liquid and the ionic liquid phase were mixed and extracted in a constant temperature water bath oscillator, the extraction time was 5 min, the temperature was 25° C., and the rotation speed during the extraction and stripping process was 200 r / min. The concentration of rare earth elements in raffinate was measured by ICP method, and the results showed that the extraction rate ...

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Abstract

The invention relates to a method for extracting and separating rare earth element yttrium by using pyridine carboxylic acid ionic liquid, and belongs to the field of ionic liquid extraction and separation of rare earth. Using the hydrochloric acid aqueous solution containing rare earth elements yttrium, holmium, and erbium as the raw material solution, the ionic liquid phase and the rare earth raw material solution are mixed and extracted, and the raffinate and the ionic liquid phase loaded with rare earth are obtained after centrifugation. The ionic liquid phase is back-extracted, and the pure rare earth solution and the regenerated ionic liquid phase are obtained after centrifugation. The ionic liquid phase of the present invention consists of pyridine carboxylic acid ionic liquid extractant ([(CH 2 ) n COOHpyr][NTf 2 ], n=3,4,5,6,7) and ionic liquid [C 4 mim][NTf 2 ] diluent composition, replacing the traditional organic solvents such as naphthenic acid, toluene, etc., and the separation performance of yttrium / erbium, yttrium / holmium, the extraction process is short extraction time, simple operation, ionic liquid can be recycled.

Description

technical field [0001] The invention relates to a method for extracting and separating rare earth element yttrium by using pyridine carboxylic acid ionic liquid, and belongs to the field of ionic liquid extraction and separation of rare earth. Background technique [0002] Rare earth elements are composed of scandium (Sc), yttrium (Y) and 15 kinds of lanthanide rare earth elements, which can be divided into light rare earth elements lanthanum (La), cerium (Ce), and praseodymium according to the atomic electron layer structure and physical and chemical properties of rare earth elements. (Pr), neodymium (Nd), promethium (Po), samarium (Sc), europium (Eu) and heavy rare earth elements gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er) ), thulium (Th), ytterbium (Yb), lutetium (Lu), scandium (Sc), yttrium (Y)). Rare earth elements have unique optical, electrical, and magnetic properties, and are widely used in various functional materials, such as rare ea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B59/00C22B3/36
CPCC22B59/00Y02P10/20
Inventor 高红帅胡凯博张香平聂毅董海峰张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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