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A kind of rare earth extraction agent and the method for separating rare earth yttrium

An extractant and rare earth technology, applied in the field of rare earth extraction and separation, can solve the problems of decreased extraction capacity, increased economic cost, low separation coefficient, etc., and achieves the effects of reducing the number of extraction stages, eliminating pollution, and achieving good selectivity.

Active Publication Date: 2020-12-01
厦门熙途科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Naphthenic acid will slowly undergo esterification reaction with mixed alcohol additives, resulting in a significant drop in extraction capacity, and needs to be replaced every few years, which not only wastes resources but may also pollute the environment and greatly increase economic costs
Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences designed and synthesized a carboxylic acid-type extractant code-named CA12. Chinese patent CN99118261.8 discloses a process for separating yttrium oxide based on CA12, but CA12 is sensitive to heavy rare earth Er, Tm, Yb or Lu and Y has a lower separation factor

Method used

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  • A kind of rare earth extraction agent and the method for separating rare earth yttrium
  • A kind of rare earth extraction agent and the method for separating rare earth yttrium
  • A kind of rare earth extraction agent and the method for separating rare earth yttrium

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Example 1 Preparation of 2,6-dimethylheptylphenoxy n-butyric acid

[0041] Add 50 grams of absolute ethanol and 48.4 grams of sodium 2,6-dimethylheptylphenolate into the reaction vessel, start stirring and heating, raise the temperature to 110°C, and slowly add 37.8 grams of sodium bromide-n-butyrate into the reaction vessel . After reacting for 1 hour, cool to room temperature, distill the solvent of the obtained reaction product under reduced pressure, then add 6mol / L hydrochloric acid solution for acidification, wash the acidified product three times with water, and distill under reduced pressure at 160°C to obtain 2,6- Dimethylheptylphenoxy n-butyric acid.

[0042] The 2,6-dimethylheptylphenoxy-n-butyric acid prepared in Example 1 of the present invention has been subjected to acid-base titration and NMR detection, and the purity is greater than 95%. It has the structure of formula I, and R in formula I 1 Take 2,6-dimethylheptyl.

Embodiment 2

[0043] Example 2 Preparation of 2,6-dimethylheptylphenoxyisobutyric acid

[0044] Add 100 grams of absolute ethanol and 48.4 grams of sodium 2,6-dimethylheptylphenolate into the reaction vessel, start stirring and heating, raise the temperature to 100°C, and slowly add 37.8 grams of sodium bromoisobutyrate into the reaction vessel . After reacting for 1.5 hours, cool to room temperature, distill the solvent of the obtained reaction product under reduced pressure, then add 6mol / L hydrochloric acid solution for acidification, wash the acidified product three times, and distill under reduced pressure at 160°C to obtain 2,6- Dimethylheptylphenoxyisobutyric acid.

[0045] The 2,6-dimethylheptylphenoxyisobutyric acid prepared in Example 2 of the present invention is subjected to acid-base titration and NMR detection, and the purity is greater than 97%, and has the structure of formula II. In formula II, R 2 Take 2,6-dimethylheptyl.

Embodiment 3

[0046] Example 3 Preparation of 2,6-dimethylheptylphenoxy sec-butyric acid

[0047] Add 150 grams of absolute ethanol and 48.4 grams of sodium 2,6-dimethylheptylphenolate into the reaction vessel, start stirring and heating, raise the temperature to 90°C, and slowly add 37.8 grams of sodium bromide sec-butyrate into the reaction vessel . After reacting for 2 hours, cool to room temperature, distill the solvent of the obtained reaction product under reduced pressure, then add 6mol / L hydrochloric acid solution for acidification, wash the acidified product three times with water, and distill under reduced pressure at 160°C to obtain 2,6- Dimethylheptylphenoxy-sec-butyric acid.

[0048] The 2,6-dimethylheptylphenoxy-sec-butyric acid prepared in Example 3 of the present invention has been subjected to acid-base titration and NMR detection, and the purity is greater than 98%. It has the structure of formula III. In formula III, R 3 Take 2,6-dimethylheptyl.

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Abstract

The invention provides a rare earth extractant, which includes one or more of the compounds of formula I, formula II and formula III. The invention provides a method for separating rare earth yttrium, comprising the following steps: 1) mixing a rare earth extractant and a diluent to obtain an organic phase; 2) mixing the organic phase with a yttrium-containing rare earth material liquid and then extracting to obtain an aqueous phase and organic phase, containing yttrium in the aqueous phase; 3) pickling the organic phase in step 2) to obtain aqueous phase and organic phase, containing yttrium in the aqueous phase; 4) organic phase in step 3) The phase is back-extracted to obtain an aqueous phase and an organic phase, and the aqueous phase contains rare earth elements such as neodymium. Compared with the prior art, the rare earth extractant provided by the present invention has good selectivity for separating rare earth elements, the structure of the rare earth extractant is stable, it can be recycled for more than one year, no emulsification occurs during extraction, and the synthesis of the extractant is simple and the cost is low .

Description

technical field [0001] The invention relates to the technical field of rare earth extraction and separation, in particular to a rare earth extraction agent and a method for separating rare earth yttrium. Background technique [0002] Yttrium is widely used in the fields of rare earth aluminum alloys, functional ceramics, lasers and phosphors. In the prior art, the separation of rare earth yttrium mainly adopts the extraction and separation method using naphthenic acid as the main extraction agent. Naphthenic acid will slowly undergo esterification reaction with mixed alcohol additives, resulting in a significant decline in extraction capacity, and needs to be replaced every few years, which not only wastes resources but may also pollute the environment and greatly increase economic costs. Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences designed and synthesized a carboxylic acid-type extractant code-named CA12. Chinese patent CN99118261.8 discloses a pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/32C22B59/00
CPCC22B59/00C22B3/32Y02P10/20
Inventor 孙晓琦王艳良李福建
Owner 厦门熙途科技有限公司
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