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Method used for separating rare earth from bastnaesite sulphuric acid leach solution and preparing ice stone

A bastnasite and leaching solution technology, applied in aluminum fluoride, process efficiency improvement, aluminum halide and other directions, to achieve the effect of reducing recycling, reducing pollution and reducing waste

Inactive Publication Date: 2012-09-05
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005]The above methods all achieve Ce4+, RE3+, F- The separation of , due to the strong coordination ability of fluorine, increases the difficulty of subsequent separation and treatment of rare earths. A lot of research work is needed to realize industrial application, and fluorine is treated as a useless element, and fluorine is not really treated. Resource utilization as a resource also causes a great waste of fluorine resources. If the fluorine / rare earth can be separated by adding a fluorine complexing agent before or during the extraction process, the impact of fluorine on the subsequent treatment process can be eliminated. Then leaching and separation of rare earths can be carried out, and the resource utilization of fluorine can be carried out, so as to finally realize the clean production of rare earth smelting and the comprehensive utilization of resources

Method used

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  • Method used for separating rare earth from bastnaesite sulphuric acid leach solution and preparing ice stone
  • Method used for separating rare earth from bastnaesite sulphuric acid leach solution and preparing ice stone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Bastnaesite was oxidized and roasted in the air at 400°C for 4 hours, and the concentration of bastnaesite was added to 1.0mol L -1 sulfuric acid, leached at 30°C for 4h, the liquid-solid weight ratio of sulfuric acid to bastnaesite was 5:1, to obtain bastnaesite sulfuric acid leaching solution, wherein Ce 4+ The concentration is 0.02 mol·L -1 , F - The concentration is 0.03mol·L -1 , RE 3+ The concentration is 0.35 mol·L -1 , the acidity of the solution is 0.2mol L -1 ;

[0029] (2) Add NaAlO to bastnaesite sulfuric acid leaching solution 2 , the molar ratio of fluorine to aluminum is 2:1, and the F in the sulfuric acid leaching solution - with NaAlO 2 Complexation, separation from cerium and trivalent rare earth elements;

[0030] (3) Mix P204 and sulfonated kerosene to obtain an organic phase, the concentration of the extractant is 0.1 mol / L, mix the organic phase with the above-mentioned bastnaesite sulfuric acid leaching solution at a volume ratio of 1:...

Embodiment 2

[0033] (1) The bastnaesite was oxidized and roasted in the air at 600°C for 2 hours, and the bastnaesite was added to the concentration of 0.5mol L after the oxidation roasting -1 Sulfuric acid, at 50 ℃ leaching time 2h, the liquid-solid weight ratio of sulfuric acid and bastnaesite is 10:1, obtain bastnaesite sulfuric acid leaching solution, wherein Ce 4+ The concentration is 0.015 mol·L -1 , F - The concentration is 0.03mol·L -1 , RE 3+ The concentration is 0.02mol·L -1 , the acidity of the solution is 1mol L -1 ;

[0034] (2) Add AlCl to the bastnaesite sulfuric acid leaching solution 3 , the molar ratio of fluorine to aluminum is 1:1, and the F in the sulfuric acid leaching solution - with AlCl 3 Complexation, separation from cerium and trivalent rare earth elements;

[0035] (3) Mix P507-P204 and sulfonated kerosene to obtain the organic phase, the mass fraction of P204 is 60%, the concentration of the extractant is 1mol / L, and the organic phase is mixed with the...

Embodiment 3

[0038] (1) Bastnaesite was oxidized and roasted in air at 800°C for 1 hour, and the concentration of bastnaesite was added to 2.0mol L after oxidation roasting -1 Sulfuric acid, leaching time 0.5h at 100°C, the liquid-solid weight ratio of sulfuric acid to bastnaesite is 1:1, to obtain bastnaesite sulfuric acid leaching solution, wherein Ce 4+ The concentration is 0.23mol L -1 , F - The concentration is 0.35mol L -1 , RE 3+ The concentration is 0.28 mol·L -1 ,, the acidity of the solution is 0.2mol L -1 ;

[0039] (2) Adding Al to bastnaesite sulfuric acid leaching solution 2 (SO 4 ) 3 , the molar ratio of fluorine to aluminum is 6:1, and the F in the sulfuric acid leaching solution - with Al 2 (SO 4 ) 3 Complexation, separation from cerium and trivalent rare earth elements;

[0040] (3) Mix P507 and sulfonated kerosene to obtain an organic phase, the concentration of the extractant is 3 mol / L, mix the organic phase with the above-mentioned bastnaesite sulfuric a...

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Abstract

The invention belongs to the technical field of rare earth hydrometallurgy, and specifically relates to a method used for separating rare earth from a bastnaesite sulphuric acid leach solution and preparing an ice stone. The method comprises the following steps of: adding aluminium salt as a fluorine complexing agent in a bastnaesite sulphuric acid leach solution, mixing an extraction agent and a diluting agent to obtain an organic phase, mixing the organic phase and the bastnaesite sulphuric acid leach solution according to the volume ratio of (1-10):1, vibrating for 5-60 minutes, and splitting phase after standing for 10-60 minutes; and obtaining the organic phase of loading cerium and an extractive surplus phase containing fluorine and trivalence rare earth, adding a sodium compound in the extractive surplus phase, adjusting pH to 2-5, obtaining Na3AlF6 precipitation, namely the ice stone, carrying out solid-liquid separation, and obtaining the trivalence rare earth solution after defluorination. Compared with the prior art, the method provided by the invention reduces the generation of three wastes containing fluorine due to fluorine recovery, greatly lightens the environmental pollution from a flow, can carry out reclamation utilization on fluorine in a water phase, and reduces the waste of a fluorine resource.

Description

technical field [0001] The invention belongs to the technical field of rare earth hydrometallurgy, and in particular relates to a method for separating rare earth from bastnaesite sulfuric acid leaching solution and preparing cryolite. Background technique [0002] Bastnaesite is the world's largest reserve, and is currently the largest amount of rare earth mineral resources mined and used. Its composition is mainly light rare earth elements, and it is also associated with valuable resources of 0.1~0.2wt.% thorium and 7~9wt.% of fluorine. [0003] At present, there are more than 10 kinds of techniques used in the decomposition of bastnaesite and the extraction of rare earths. In summary, there are mainly acid methods and alkali methods. Among them, the acid methods mainly use hydrochloric acid or sulfuric acid, such as concentrated sulfuric acid roasting method. , so that HF ​​gas and sulfuric acid mist are easy to be generated in the process, which not only pollutes the e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/08C22B3/26C22B59/00C22B1/02C01F7/54
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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