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Method for separating tetravalent cerium, thorium and rare earth

A rare earth and solid-state separation technology, which is applied in the field of thorium and rare earth and tetravalent cerium separation, can solve the problem that the medium can only be nitric acid, etc., and achieve the effects of strong extraction ability, elimination of influence, shortening the separation process and cost

Active Publication Date: 2016-07-06
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the P503 extractant used in this patent can only extract tetravalent cerium in the nitric acid system, resulting in the medium of the extraction and separation process can only be nitric acid

Method used

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  • Method for separating tetravalent cerium, thorium and rare earth
  • Method for separating tetravalent cerium, thorium and rare earth
  • Method for separating tetravalent cerium, thorium and rare earth

Examples

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Embodiment

[0143] In order to further illustrate the solutions of the present invention, specific examples of the present invention are provided to help those skilled in the art understand and implement the present invention, but the present invention is not limited to these examples.

[0144] Reagents and sources

[0145]Diethylhexyl phosphite, di-n-octyl phosphite, di-n-heptyl phosphite, di-isooctyl phosphite, aviation kerosene and TBP were purchased from Shanghai Laish Chemical Co., Ltd.

[0146] Paraformaldehyde, di-n-hexylamine, diisobutylamine, n-butylamine, diisooctylamine, dodecylamine, isooctylamine, dimethylamine, toluene, xylene, p-toluenesulfonic acid, and heptane purchased from Aladdin Reagent Co., Ltd.

[0147] Cyanex923 and 2-methylheptanol were purchased from Shanghai Cyanex Chemical Co., Ltd.

[0148] Feed liquid, washing liquid and stripping agent are self-made in the laboratory.

[0149] Other reagents (such as acids, etc.) are commercially available analytical reag...

preparation example 1

[0152] Preparation Example 1: Preparation of (N,N-dihexylamino)methylphosphonic acid bis(2-ethylhexyl)ester

[0153]

[0154] In a three-necked flask equipped with a mechanical stirrer, a water separator, and a condensation reflux device, add diethylhexyl phosphite (1mol), paraformaldehyde (M=30, 1.05mol), di-n-hexylamine (1.05mol) , toluene (700ml) and p-toluenesulfonic acid (2g), heated to reflux at 130°C, and the water generated by the reaction was separated. When anhydrous is produced, react for another 2 hours. 10 g of potassium carbonate was added to the reaction mixture, and heating to reflux was continued for 15 min. The reaction mixture was filtered to remove excess potassium carbonate in the reaction, washed three times with distilled water, and the toluene was removed by rotary evaporation to obtain the target product.

[0155] 1 HNMR (400MHz, CDCl 3 ,ppm): δ1.74-0.86[m,(CH 3 ) 6 ,(CH 2 ) 16 ,(CH) 2 ],2.63[m,(CH 2 )],2.95[t,CH 2 , J=8Hz], 3.96[m, (CH ...

preparation example 2

[0156] Preparation Example 2: Preparation of Dioctyl (N,N-Diisobutylamino)methylphosphonate

[0157]

[0158] Except that di-n-octyl phosphite was used to replace diethylhexyl phosphite and diisobutylamine was used to replace di-n-hexylamine, the target product was prepared by the same process as in Preparation Example 1.

[0159] 1 HNMR (400MHz, CDCl 3 ,ppm): δ1.71-0.89[m,(CH 3 ) 6 ,(CH 2 ) 12 ],2.05[m,(CH) 2 ],2.31[m,(CH 2 ) 2 ],2.95[m,(CH 2 )],4.02[m,(CH 2 ) 2 ].

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Abstract

The invention relates to a method for separating tetravalent cerium, thorium and rare earth. The method comprises following steps: feed liquid containing the tetravalent cerium, thorium and rare earth is provided; an amino-contained neutral phosphine extraction agent in the general formula I is used for performing extraction and separation on the tetravalent cerium from the feed liquid to obtain cerium-contained extraction liquid and cerium extraction tail liquid; the amino-contained neutral phosphine extraction agent in the general formula I is used for performing extraction and separation on the thorium from the cerium extraction tail liquid to obtain thorium-contained extraction liquid and thorium extraction tail liquid; and the rare earth in the thorium extraction tail liquid is recycled, and the chemical formula is shown in the specification, wherein R1 and R2 are each and independently selected from a C1-C12 alkyl group, R3 and R4 are each and independently selected from a C1-16 alkyl group and hydrogen, and n is an integer of one to eight.

Description

technical field [0001] The invention relates to a method for separating tetravalent cerium, thorium and rare earth. More specifically, it relates to a method for sequentially extracting and separating tetravalent cerium and thorium by using an amino-containing neutral phosphine extractant system, thereby realizing the separation of tetravalent cerium, thorium and rare earth. Background technique [0002] Baotou mixed rare earth ore is mainly composed of bastnaesite and monazite ore, of which cerium accounts for about 50% of the total rare earth content. In addition to rare earth elements, the concentrate also contains a large number of non-rare earth impurity elements, such as fluorine, thorium, phosphorus, silicon, iron, calcium, etc. At present, Baotou rare earth mine mainly uses concentrated sulfuric acid to strengthen high-temperature roasting technology, and thorium, fluorine, phosphorus, etc. have not been recovered, and have caused pollution to the environment. [0...

Claims

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Application Information

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IPC IPC(8): C22B3/38C22B59/00C22B60/02
CPCY02P10/20
Inventor 廖伍平卢有彩张志峰李艳玲吴国龙
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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