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Dialkylaminophenoxy acetic acid extracting agent and preparation method and application thereof

A technology of dialkylaminophenoxyacetic acid and alkylaminophenoxyacetic acid, which is applied in the field of dialkylaminophenoxyacetic acid extraction agent and its preparation, can solve the problem of difficult separation of heavy rare earth elements, low separation coefficient, high separation coefficient, etc. problem, to achieve the effect of single component, improved separation coefficient and stable extraction process

Active Publication Date: 2021-03-30
FUJIAN CHANGJIANG GOLDEN DRAGON RARE EARTH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, during the research process, it was found that although alkylphenoxycarboxylic acid and naphthenic acid are similar and can separate yttrium from all lanthanides, there is the same problem in the actual operation process, that is, alkylphenoxycarboxylic acid The extraction agent has a high separation coefficient for light rare earth elements and yttrium, but a low separation coefficient for heavy rare earth elements and yttrium, which makes it difficult to separate heavy rare earth elements from yttrium

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  • Dialkylaminophenoxy acetic acid extracting agent and preparation method and application thereof
  • Dialkylaminophenoxy acetic acid extracting agent and preparation method and application thereof
  • Dialkylaminophenoxy acetic acid extracting agent and preparation method and application thereof

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preparation example Construction

[0039] The present invention also provides a kind of preparation method of dialkylaminophenoxyacetic acid extractant, comprising the following steps:

[0040] a) Mixing p-nitrophenol, sodium haloacetate, alkali, alcohol and water, and heating to reflux for reaction to obtain p-nitrophenoxycarboxylate;

[0041] b) hydrogenating and reducing the p-nitrophenoxycarboxylate to obtain p-aminophenoxycarboxylate;

[0042] c) reacting the p-aminophenoxycarboxylate with a halogenated hydrocarbon to carry out an alkylation reaction, and then acidifying after completion of the reaction to obtain a dialkylaminophenoxyacetic acid extractant with a structure shown in formula (I);

[0043]

[0044] Wherein, R1 and R2 are independently selected from C 1 ~C 10 The alkyl group, more specifically can be C 1 Alkyl, C 2 Alkyl, C 3 Alkyl, C 4 Alkyl, C 5 Alkyl, C 6 Alkyl, C 7 Alkyl, C 8 Alkyl, C 9 Alkyl or C 10 alkyl.

[0045]In the preparation method provided by the invention, firstl...

Embodiment 1

[0070] The extractant is 4-N,N-dimethylaminophenoxyacetic acid, that is, in the formula (I), R1 is a methyl group, and R2 is a methyl group, and its chemical structure is specifically shown in the formula (I-1):

[0071]

[0072] 4-N, the preparation method of N-dimethylaminophenoxyacetic acid is as follows:

[0073] Put 0.1 mol of p-nitrophenol, 100 mL of a mixed solvent of ethanol and water with a volume ratio of 1:1 in a three-necked flask, add 0.1 mol of sodium hydroxide, and stir to dissolve. Then add 0.15mol sodium chloroacetate and 0.2g KI, heat to 110°C, condense and reflux for 0.5h. Cool to room temperature after the reaction, evaporate the solvent, and wash with water to obtain p-nitrophenoxyacetate.

[0074] Then mix p-nitrophenoxyacetate, 5 mg of commercially available 10wt.% Pd / C catalyst and 100 mL of ethanol solvent, control the reaction temperature at 70 ° C, circulate hydrogen gas, react for 4 hours and cool to room temperature, after solid-liquid separati...

Embodiment 2

[0078] The extractant is 4-N,N-diheptylaminophenoxyacetic acid, that is, in formula (I), R1 is heptyl, R2 is heptyl, and its chemical structure is specifically shown in formula (I-2):

[0079]

[0080] The preparation method of 4-N,N-diheptylaminophenoxyacetic acid refers to Example 1, except that the alkylating agent used is 1-bromoheptane.

[0081] The results of acid-base titration and NMR characterization show that the purity of the extractant of 4-N,N-diheptylaminophenoxyacetic acid prepared in this example is greater than 95%, and the total yield of the preparation is greater than 85%.

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Abstract

The invention belongs to the field of rare earth resource recovery, and particularly relates to a dialkylaminophenoxy acetic acid extracting agent and a preparation method and application thereof. Thedialkylaminophenoxy acetic acid extracting agent has a chemical structure shown in a formula (I); and R1 and R2 are independently selected from alkyl groups of C1-C10. The dialkylaminophenoxy aceticacid extracting agent can effectively separate yttrium from other lanthanide elements, and compared with industrially-applied naphthenic acid extracting agents, the extracting agent is single in component, free of emulsification and more stable in extraction process; and compared with other alkyl-substituted phenoxy carboxylic acid extracting agents, the extracting agent keeps a high separation coefficient of light rare earth elements and yttrium, meanwhile, the separation coefficient of heavy rare earth elements and yttrium is improved, the extraction stage number can be further reduced, theprocess can be shortened, the economic cost can be saved, and the production efficiency can be improved.

Description

technical field [0001] The invention belongs to the field of recovery of rare earth resources, and in particular relates to a dialkylaminophenoxyacetic acid extractant and a preparation method and application thereof. Background technique [0002] In the field of separation of rare earth metal ions, naphthenic acid is mainly used as an extractant in industry to extract and separate yttrium from rare earth metal mixtures. Naphthenic acid is a by-product of the petrochemical industry, its source is limited, and its components are complex. It needs to be extracted under high pH conditions to extract rare earths. After long-term use, its composition is prone to change, which affects the stability of the separation process. Researchers are eager to find a new type of carboxylic acid extractant to replace naphthenic acid. For example, the patent CN1084574A discloses a carboxylic acid type extractant for separating rare earth metals. The molecular formula is ROCH 2 COOH, where R i...

Claims

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Application Information

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IPC IPC(8): C22B3/32C22B59/00
CPCC22B59/00Y02P10/20
Inventor 林锦池王艳良吴玉远肖文涛
Owner FUJIAN CHANGJIANG GOLDEN DRAGON RARE EARTH CO LTD
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