Extractant and preparation method and application thereof

An extraction agent and an unsubstituted technology, applied in the field of extraction agent and its preparation, can solve the problems of difficult solid-liquid separation, large consumption of chemical reagents, and small size of rare earth particles, so as to achieve large rare earth precipitation size, easy solid-liquid separation, The effect of good selectivity

Active Publication Date: 2019-07-23
XIAMEN INST OF RARE EARTH MATERIALS
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  • Abstract
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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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  • Extractant and preparation method and application thereof
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  • Extractant and preparation method and application thereof

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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 a preparation method and application thereof. A phenoxy dicarboxylic acid extractant is synthesized by reacting a diphenol compound and halogenated alkyl carboxylic ester in a solvent and then acidifying; and the saponification extractant is used for beneficiating trace rare earth in an MgSO4 leaching solution of ionic adsorption type rare earth mineral. Compared with an existing extractant, the saponification extractant has higher precipitation capacity, better rare earth selectivity, and high precipitation efficiency; as the rare earth precipitates are large in size, a rare earth extraction complex can be separated from a water phase more conveniently, and the production efficiency is improved; and moreover, no volatile diluent is used in the beneficiation process, the COD value of raffinate meets the national wastewater discharge standard in China, and the raffinate and the carboxylic acid extractant can be 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 Applications(China)
IPC IPC(8): C22B3/32C22B59/00
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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