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, alkylphenoxycar

Method used

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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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Example Embodiment

[0039] The present invention also provides a method of preparing a dialkyl amino phenoxyacetic acid extractant, comprising the steps of:

[0040] A) Reaction the nitrophenol, sodium haloaceous acetate, base, alcohol and water, and heat reflow, to obtain a nitrobenzoxoate salt;

[0041] b) Hydrogenation of the nitrobenzoxicarboxylate to obtain an aminophenoxic acid salt;

[0042] C) The alkylation reaction of the amino phenoxycarboxylate and the halogenated hydrocarbon reaction was completed, and the reaction was completed, and the dialkyl amino acetic acid extractant of the structure shown in the formula (I) was obtained.

[0043]

[0044] Among them, R1 and R2 are independently selected from C 1 ~ C 10 The alkyl group, more specifically 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 present invention, a mixture of nitrophenol, sodium halo acetate, alkali, alcohol,...

Example Embodiment

[0069] Example 1

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

[0071]

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

[0073] A mixed solvent of 0.1 mol of nitrophenol, 100 ml volume ratio of 1: 1 is placed in three flasks, and 0.1 mol of sodium hydroxide, stirred dissolved. Add 0.15 mol sodium chloroacetate and 0.2 g of Ki, heated to 110 ° C, and the condensation reflux reaction was 0.5 h. After the reaction was completed, cooled to room temperature, evaporated to the solvent, and the nitrobenzoxide salt was obtained.

[0074] Then, the nitrobenzoxyacetate, 5 mg commercially available 10 wt.% PD / C catalyst and 100 ml of ethanol solvent were mixed, the control reaction temperature was 70 ° C, circulated into hydrogen gas, cooled to room temperature after 4 h, and solid-liquid separation The etha...

Example Embodiment

[0077] Example 2

[0078] The extractant is 4-N, N-dimethyl amino acetic acid, i.e., R1 in the formula (I) is heptyl, R2 is heptyl, and its chemical structure is specifically shown in formula (I-2):

[0079]

[0080] Preparation method of 4-N, N-Diheeheheee amoxyethoxoic acid Refer to Example 1, the alkylation reagent used in the use of 1-bromophenic alkane.

[0081] It was titrated and a nuclear magnetic resonance character, and the results showed that the purity of the extractant of 4-N, N-diheptamine oxoacetic acid prepared in the present embodiment was greater than 95%, and the total yield was 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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