Diphenylamino oxocarboxylic acid extraction agent and preparation method and application thereof

A technology of diphenylamino oxocarboxylic acid and extractant, which is applied in the field of diphenylamino oxocarboxylic acid extractant, can solve the problems of difficult separation of heavy rare earth elements and yttrium, low separation coefficient, etc., and achieve single component, chemical The effect of stable structure and stable extraction performance

Inactive Publication Date: 2021-05-07
XIAMEN TUNGSTEN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although the molecular formula is ROCH 2 The alkylphenoxycarboxylic acid of COOH can separate yttrium from lanthanides, and the extraction performance is stable, but the separation coefficient of heavy rare earths and yttrium in the extr

Method used

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  • Diphenylamino oxocarboxylic acid extraction agent and preparation method and application thereof
  • Diphenylamino oxocarboxylic acid extraction agent and preparation method and application thereof
  • Diphenylamino oxocarboxylic acid extraction agent and preparation method and application thereof

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preparation example Construction

[0044] The present invention also provides a kind of preparation method of above-mentioned diphenylamino oxocarboxylic acid extraction agent, comprises the following steps:

[0045] A) After mixing dialkylaniline, alkyldiacid monoethyl chloride, organic solvent and organic base, react to obtain a reaction solution;

[0046] B) mixing the reaction solution with water to obtain an oil phase and a water phase;

[0047] C) Distilling the oil phase under reduced pressure to obtain monoethyl diphenylaminooxycarboxylate;

[0048] D) heating the monoethyl diphenylaminooxycarboxylate to reflux in a sodium hydroxide solution, acidifying and distilling under reduced pressure to obtain a diphenylaminooxycarboxylic acid extractant.

[0049] In some embodiments of the invention, step A) comprises:

[0050] a) mixing dialkylaniline, organic base and organic solvent to obtain a mixed solution;

[0051] b) mixing alkyldiacid monoethyl chloride with the mixed solution to react to obtain a re...

Embodiment 1

[0101] The chemical structure of 5-diphenylamino-5-oxopentanoic acid is shown in formula (I-1), namely R 1 and R 2 Both are H, and the value of n is 3;

[0102]

[0103] Its preparation steps are as follows:

[0104](1) Mix 16.9g of diphenylamine, 15.2g of triethylamine and 40mL of dichloromethane, stir evenly to obtain a mixed solution, and cool the mixed solution to 0°C with an ice-water bath.

[0105] (2) Add 17.9 g of monoethyl glutaric acid chloride to the mixed liquid, and stir and react at 0° C. for 30 min to obtain a reaction liquid.

[0106] (3) Add deionized water to the reaction solution, the reaction solution is divided into an oil phase and a water phase, and the oil phase is distilled under reduced pressure to obtain the crude product ethyl 5-diphenylamino-5-oxopentanoate.

[0107] (4) Heat ethyl 5-diphenylamino-5-oxopentanoate in 100 mL of a mixed solution containing 5 g of sodium hydroxide (solvents include ethanol and water, volume ratio 1:1) to 70° C. f...

Embodiment 2

[0113] The chemical structure of 3-(4,4'-dimethyldiphenylamino)-3-oxopropionic acid is shown in formula (I-2), ie R 1 and R 2 Both are methyl groups, and the value of n is 1;

[0114]

[0115] Its preparation steps are as follows:

[0116] (1) Mix 19.7g of 4,4'-dimethyldiphenylamine, 15.2g of triethylamine and 40mL of dichloromethane, stir evenly to obtain a mixed solution, and cool the mixed solution to 0°C with an ice-water bath.

[0117] (2) 15.0 g of monoethyl malonate chloride was added to the mixed liquid, and stirred and reacted at 0° C. for 30 min to obtain a reaction liquid.

[0118] (3) Add deionized water to the reaction solution, the reaction solution is divided into an oil phase and a water phase, and the oil phase is distilled under reduced pressure to obtain the crude product 3-(4,4'-dimethyldiphenylamino)-3 - ethyl oxopropionate.

[0119] (4) Mix ethyl 3-(4,4'-dimethyldiphenylamino)-3-oxopropanoate in 100mL containing 5g sodium hydroxide (solvents includ...

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Abstract

The invention relates to the technical field of rare earth resource recovery, in particular to a diphenylamino oxocarboxylic acid extraction agent and a preparation method and application thereof. The diphenylamino oxocarboxylic acid extraction agent has a structure shown in a formula (I); and in the formula (I), R1 and R2 are independently selected from H or C1-C9 alkyl groups, and n is a natural number from 1 to 6. The diphenylamino oxocarboxylic acid extraction agent provided by the invention can be used for effectively separating yttrium from lanthanide, and compared with an industrially applied naphthenic acid extraction agent, the extraction agent provided by the invention has the advantages of simplex component, stable chemical structure, no reduction of the concentration of an extracted organic phase and stable extraction performance; and moreover, the coefficient of the diphenylamino oxocarboxylic acid extraction agent for separating yttrium from light rare earth elements is obviously higher than that of the naphthenic acid extraction agent, the coefficient of the diphenylamino oxocarboxylic acid extraction agent for separating yttrium from heavy rare earth elements is also higher than that of the naphthenic acid extraction agent, and the diphenylamino oxocarboxylic acid extraction agent can completely replace the naphthenic acid extraction agent in the aspect of separation efficiency and has quite good application prospects.

Description

technical field [0001] The invention relates to the technical field of rare earth resource recovery, in particular to a diphenylaminooxycarboxylic acid extraction agent, a preparation method and application thereof. Background technique [0002] In the field of ion separation of rare earth elements, naphthenic acid is mainly used as an extractant to extract and separate yttrium from rare earth element mixtures in industry. Naphthenic acid is a by-product of the petrochemical industry, the source is limited, and its components are complex, and rare earths need to be extracted under high pH conditions. After long-term use, its composition is prone to change, resulting in a decrease in the concentration of the organic phase and affecting the separation. process stability. At present, researchers are urgently looking for a new type of carboxylic acid extractant to replace naphthenic acid, for example: Chinese patent CN1084574A discloses a carboxylic acid type extractant for sep...

Claims

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Application Information

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IPC IPC(8): C22B3/32C22B59/00
CPCC22B59/00Y02P10/20
Inventor 王艳良吴玉远肖文涛林锦池
Owner XIAMEN TUNGSTEN
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