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A kind of extractant and its preparation method and application

An extractant and rare earth technology, applied in the field of extractant and its preparation, can solve the problems of difficult solid-liquid separation, large consumption of chemical reagents, small particle size of rare earth, etc., and achieves large size of rare earth precipitate, easy and good solid-liquid separation The effect of sedimentation rate

Active Publication Date: 2021-08-03
XIAMEN INST OF RARE EARTH MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, ammonium bicarbonate or oxalic acid precipitation is often used to enrich and recover rare earths, but the recovery rate of rare earths in this process is low, and a large amount of chemical reagents are required to produce a large amount of ammonia nitrogen wastewater or oxalic acid wastewater, which is easy to cause water pollution. environmental pollution
It is reported that when one ton of rare earth elements is mined, 3.5 tons of ammonium bicarbonate is consumed, and 1,000-1,200 cubic meters of ammonia nitrogen wastewater is produced, while the precipitated oxalic acid wastewater is difficult to treat due to its toxicity and water solubility, which has a considerable impact on the environment harm
In addition, the size of rare earth particles obtained by using ammonium bicarbonate or oxalic acid is extremely small, making it difficult to separate solids and liquids

Method used

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  • A kind of extractant and its preparation method and application
  • A kind of extractant and its preparation method and application
  • A kind of extractant and its preparation method and application

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preparation example Construction

[0046] The present invention provides the preparation method of above-mentioned extractant, comprises the steps:

[0047] (1) Hydroquinone compound and halogenated alkyl carboxylate react in solvent to obtain crude ester;

[0048] (2) dissolving the crude ester in absolute ethanol and tetrahydrofuran, adding an ethanol solution containing hydroxide to obtain a reaction mixture;

[0049] (3) After removing the solvent of the reaction mixture, the residue was dissolved in water and acidified to obtain an extractant.

[0050]In the above method for preparing the extractant provided by the present invention, firstly, the diphenol compound and the halogenated alkyl carboxylate are mixed in a solvent. Wherein, the alkyl group in the halogenated alkyl carboxylate can be independently selected from substituted straight-chain alkyl groups with 3-12 carbon atoms, unsubstituted straight-chain alkyl groups with 3-12 carbon atoms, substituted branched chain alkyl groups with 3 to 12 carb...

Embodiment 1

[0070] 1. The preparation method of extractant 2,2'-(1,4-phenylene bis(oxy))dioctanoic acid (PPBOA)

[0071] (1) Add 1.80 g (0.045 mol) of sodium hydride and 20 ml of N,N-dimethylformamide (DMF) into the reaction vessel. Stir at room temperature, and slowly add a solution of hydroquinone (0.02mol, 2.20g of hydroquinone in 20ml of DMF) under argon (or nitrogen) protection to obtain a sodium phenoxide solution; slowly add 2-bromooctanoic acid A solution of methyl ester (0.05mol, 11.9g) was stirred at 60°C for 6 hours; after extraction with cyclohexane, the organic phase was concentrated under reduced pressure to finally obtain the corresponding crude ester.

[0072] Wherein, the reagents selected above can also be replaced by similar reagents to realize the preparation of the extractant, for example: sodium hydride can also be replaced by other alkalis, and N,N-dimethylformamide can also be replaced by N,N-dimethylacetamide ; Methyl 2-bromooctanoate can also be replaced by othe...

Embodiment 2

[0085] 1. The preparation method of extractant 2,2'-(1,2-phenylene bis(oxy))dioctanoic acid (OPBOA)

[0086] Add 1.80g (0.045mol) of sodium hydride and 20ml of N,N-dimethylformamide (DMF) into a reaction vessel equipped with a condensation and stirring device, stir at room temperature, and slowly add o-benzene under the protection of argon A solution of diphenol was obtained to obtain a sodium phenoxide solution, a solution of methyl 2-bromooctanoate (0.05mol, 11.9g) was slowly added, and stirred at 75°C for 6 hours; after extraction with cyclohexane, the organic phase was concentrated under reduced pressure, and finally The corresponding crude ester was obtained.

[0087] (2) Dimethyl 2,2'-(1,2-phenylenebis(oxy))dioctanoate, absolute ethanol (C 2 h 5 OH) (60ml) and tetrahydrofuran (THF) (V C2H5OH :V THF , 1:1) was added to the reaction vessel; after complete dissolution, 60ml ethanol solution containing KOH (0.08mol, 4.6448g) was added dropwise at room temperature, and he...

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Abstract

The invention provides an extractant and its preparation method and application. The phenoxydicarboxylic acid extractant is synthesized by reacting a quinone compound and a halogenated alkyl carboxylate in a solvent, followed by acidification; and then through saponification The Extractant Enrichment MgSO of Ion Adsorption Rare Earth Minerals 4 Trace rare earths in the leaching solution, compared with existing extractants, has higher precipitation capacity and better rare earth selectivity, high precipitation efficiency, and larger size of rare earth precipitates, which is beneficial to the extraction of rare earth complexes and The separation of the water phase improves the production efficiency, and the enrichment process of the present invention has no volatile diluent, the COD value of the raffinate meets the national wastewater discharge standard of China, and both the raffinate and the carboxylic acid extractant can be recovered and recycled.

Description

technical field [0001] The invention belongs to the field of rare earth enrichment, and in particular relates to an extractant and its preparation method and application. Background technique [0002] Due to the unique properties of rare earths and their applications in high-tech fields such as luminescence, electronics and magnetism, the rare earth industry has developed rapidly in the past few decades. China is rich in rare earth resources, and its annual output accounts for more than 90% of the world's total output, especially ion-adsorption rare earth ores, which are mainly distributed in Jiangxi, Guangdong, Hunan, Guangxi, Fujian and other places in my country. Studies have found that in ion-adsorption rare earth minerals The medium and heavy rare earths found in the minerals are more than ten times more than other light rare earth rich minerals. In the prior art, ammonium sulfate is usually used as a leaching solution to recover rare earths from ion-adsorbed minerals; ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/00C07C51/00C22B3/32C22B59/00
CPCC22B59/00C22B3/32Y02P10/20
Inventor 孙晓琦苏祥王艳良苏佳
Owner XIAMEN INST OF RARE EARTH MATERIALS
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