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Method for removing fluorine in bastnaesite sulfuric acid leaching liquid by using zirconium-containing adsorbent

A technology of bastnaesite and adsorbent, applied in the field of rare earth hydrometallurgy

Inactive Publication Date: 2013-03-06
NORTHEASTERN UNIV LIAONING
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Problems solved by technology

[0006] Aiming at the waste of resources and environmental pollution caused by the existence of fluorine in the existing bastnaesite smelting and separation technology, the present invention provides a method using zirconium-containing adsorbent The method for removing fluorine in the bastnaesite sulfuric acid leaching solution aims to use a zirconium-containing fluorine-removing adsorbent prepared by a precipitation method to remove fluorine as a fluorine adsorbent for the sulfuric acid leach solution obtained by bastnaesite oxidation roasting-sulfuric acid leaching, so that The fluorine is separated from the rare earth, thereby eliminating the impact of fluorine on the subsequent treatment process and greatly reducing the environmental pollution of the process

Method used

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  • Method for removing fluorine in bastnaesite sulfuric acid leaching liquid by using zirconium-containing adsorbent
  • Method for removing fluorine in bastnaesite sulfuric acid leaching liquid by using zirconium-containing adsorbent
  • Method for removing fluorine in bastnaesite sulfuric acid leaching liquid by using zirconium-containing adsorbent

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Experimental program
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Effect test

Embodiment 1

[0030] (1) ZrOCl 2 Dissolve in water to prepare 0.1mol L -1 solution, add 0.1mol·L while stirring -1 NaOH solution was used as a precipitating agent, and the pH was adjusted to 9. After the white precipitate was formed, it was stirred and activated at 65°C for 4h, and then filtered with suction. The obtained solid product was washed with distilled water until it was neutral, and dried at 100°C for 4h to obtain a zirconium-containing adsorbent. hydrated zirconia;

[0031] (2) The bastnaesite was oxidized and roasted at 400°C for 4 hours, and the concentration of 0.5mol L was added to the oxidized and roasted bastnaesite -1 sulfuric acid, leached at 50°C for 4h, the liquid-solid weight ratio of sulfuric acid to bastnaesite was 5:1, to obtain bastnaesite sulfuric acid leaching solution;

[0032](3) Dilute bastnaesite sulfuric acid leaching solution with water 10 times, where F - The concentration is 4.3×10 -3 mol L -1 , Ce 4+ The concentration is 2.6×10 -3 mol L -1 , RE ...

Embodiment 2

[0036] (1) ZrO(NO 3 ) 2 Dissolve in water to make 0.05mol·L -1 solution, add 0.05mol·L while stirring -1 NaOH solution was used as a precipitating agent, and the pH was adjusted to 10. After the white precipitate was formed, it was stirred and activated at 75°C for 2h, and then filtered with suction. hydrated zirconia;

[0037] (2) The bastnaesite was oxidized and roasted at 500°C for 3 hours, and the concentration of 2.0mol L was added to the oxidized and roasted bastnaesite -1 sulfuric acid, leached at 65°C for 2h, the liquid-solid weight ratio of sulfuric acid to bastnaesite was 10:1, to obtain bastnaesite sulfuric acid leaching solution;

[0038] (3) Dilute bastnaesite sulfuric acid leaching solution with water 30 times, where F - The concentration is 7.23×10 -3 mol L -1 , Ce 4+ The concentration is 4.96×10 -3 mol L -1 , RE 3+ The concentration is 7.4×10 -3 mol L -1 , adjust the acidity to 1mol L -1 , adding 1.0 g / 50 ml of the prepared zirconium-containing ad...

Embodiment 3

[0042] (1) ZrCl 4 Dissolve in water to prepare 0.5mol L -1 solution, add 0.5mol L while stirring -1 The ammonia solution was used as a precipitating agent, and the pH was adjusted to 10. After the white precipitate was formed, it was stirred and activated at 100 ° C for 1 h, and then filtered with suction. hydrated zirconia;

[0043] (2) The bastnaesite was oxidized and roasted at 800°C for 1 hour, and the concentration of 6.0mol L was added to the oxidized and roasted bastnaesite -1 Sulfuric acid was leached at 100°C for 0.5h, the liquid-solid weight ratio of sulfuric acid to bastnaesite was 1:1, and bastnaesite sulfuric acid leach solution was obtained;

[0044] (3) Dilute bastnaesite sulfuric acid leaching solution with water 100 times, where F - The concentration is 5.2×10 -3 mol L -1 , Ce 4+ The concentration is 2.89×10 -3 mol L -1 , RE 3+ The concentration is 5.02×10 -3 mol L -1 , adjust the acidity to 1mol L -1 , adding 0.4g / 50ml of the prepared zirconium-c...

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Abstract

The invention belongs to the technical field of rare earth wet metallurgy, and particularly relates to a method for removing fluorine in bastnaesite sulfuric acid leaching liquid by using a zirconium-containing adsorbent. The method comprises the following steps of firstly, preparing zirconium salt into solution being 0.05-0.5 mol.L<-1>, stirring and activating by adding a precipitating agent, obtaining zirconium-containing adsorbent hydrated zirconium oxide by drying a solid product obtained by suction filtration, diluting bastnaesite sulfuric acid leaching liquid by 10-100 times by adding water, regulating the acidity to be 0.1-1.0 mol.L<-1>, adding 0.2-1.0g / 50ml of a prepared zirconium-containing adsorbent, oscillating for 10-40 minutes, and then carrying out solid-liquid separation, and obtaining to obtain solid zirconium-containing adsorbent loaded with fluorine and defluorination sulfuric acid leaching liquid. According to the method disclosed by the invention, the generation of three fluorine-containing waste products is reduced through fluorine removing, the environment pollution due to a procedure is greatly relieved, meanwhile, the influence for on the extraction and the separation of follow-up rare earth due to the fluorine can be removed by simultaneously removing the fluorine from sulfuric acid liquid before extraction, the zirconium adsorbent after the adsorption can be reutilized, and the cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of rare earth hydrometallurgy, and in particular relates to a method for removing fluorine in a bastnaesite sulfuric acid leaching solution by using a zirconium-containing adsorbent. Background technique [0002] Bastnaesite (REFCO 3 ) is the rare earth mineral with the largest reserves in the world, accounting for more than 70% of the total rare earth. Its composition is mainly light rare earth elements. Bastnaesite concentrate generally contains about 50wt.% of cerium and 7~9wt.% of fluorine. [0003] At present, the decomposition of bastnaesite and the extraction of rare earth mainly include acid method and alkali method. The alkali method uses concentrated NaOH to decompose the concentrate, which requires high grade concentrate and high corrosion resistance requirements for equipment. The heating problem has not been well solved so far, so it is rarely used in industry at present; the acid method mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/24C22B59/00
CPCY02P10/20
Inventor 薛向欣何金桂李勇黄小卫杨合茹红强
Owner NORTHEASTERN UNIV LIAONING
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