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A kind of method of high-pressure complexation leaching bastnaesite

A bastnasite and complexing technology, which is applied in the field of high-pressure complexation and leaching of bastnaestite, can solve the problems of large fluorine-containing wastewater, long reaction time, complicated operation, etc., and achieves low equipment requirements, low cost, and mineral decomposition. high rate effect

Active Publication Date: 2018-05-15
INNER MONGOLIA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the alkaline method has high requirements on mineral grades, strict requirements on equipment corrosion resistance, high alkali consumption, and produces a large amount of fluorine-containing wastewater. If it is not treated, it will also pollute the environment.
[0005] In addition to the above methods, Li Mei of Inner Mongolia University of Science and Technology has also developed a complex leaching process to decompose bastnaesite. For example, the patent CN 201210434070.9 discloses a complex leaching of bastnaesite-containing rare earth concentrate and a cryolite preparation method. This method is to use hydrochloric acid and aluminum chloride complex to leach bastnaesite under normal pressure, and finally prepare cryolite. This method can effectively leach bastnaesite, but requires high acidity and high liquid-solid ratio. Long response time and complicated operation
The pressure leaching process has been used in many other mineral leaching, but no one has ever studied it in the field of bastnaesite leaching, especially the complex leaching of bastnaesite. For bastnaesite, we have developed a short process , easy to operate, economical and environmentally friendly, and high decomposition efficiency pressure leaching process has important practical significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 1 kg of Sichuan Mianning bastnaesite concentrate containing 52.3% of rare earth oxides above 200 mesh, the fluorine content of the bastnaesite concentrate is 7.8%, and AlCl 3 ·6H 2 O is a complexing agent, fluorine and AlCl in bastnaesite concentrate 3 ·6H 2 The total molar ratio of aluminum in O is 2, put into the autoclave together with bastnaesite concentrate, then add 25L of 0.5mol / L HCl solution, and finally raise the temperature of the autoclave to 140°C and keep it warm for 30 min. The pressure is 1.0MPa, and at the same time, constant stirring is maintained. After vacuum filtration, the filter residue is washed with boiling water for 3 times, and the final dissolution rate of bastnaesite in the concentrate reaches 99.6%.

Embodiment 2

[0020] Weigh 1 kg of Baotou Baiyanebo bastnaesite concentrate containing 58.5% of rare earth oxides above 200 mesh, the fluorine content of the bastnaesite concentrate is 7.6%, and AlCl 3 ·6H 2 O and Al(NO 3 ) 3 9H 2 O is a complexing agent. The total molar ratio of the fluorine element in the bastnaesite concentrate to the aluminum element in the aluminum salt is 0.5. Add the bastnaesite concentrate to the high-pressure reactor, and then add 2.0mol / L HCl solution 20L , and finally, the high-pressure reactor was rapidly heated to 160°C and kept warm for 50 minutes, the pressure was 1.2MPa, and at the same time, it was kept stirring at a constant speed. After filtration under reduced pressure, the filter residue was washed with boiling water for 3 times, and the final dissolution rate of bastnaesite in the concentrate reached 99.8%. .

Embodiment 3

[0022] Weigh 1 kg of American Manyan Pass bastnaesite concentrate with a rare earth oxide content of 66.1% above 200 mesh, the fluorine content of this bastnaesite concentrate is 7.5%, select Al(NO 3 ) 3 9H 2 O is a complexing agent, and the fluorine element in bastnaesite concentrate and Al(NO 3 ) 3 9H 2 The total molar ratio of aluminum in O is 1.0, and it is added to the autoclave together with bastnaesite concentrate, and then 2mol / L of HNO is added 3 The mixed solution with HCl was 15L. Finally, the autoclave was rapidly heated to 180°C and kept for 25 minutes, the pressure was 2.0MPa, and at the same time, stirring was maintained at a constant speed. The dissolution rate of ore reaches 99.7%.

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Abstract

The invention relates to a method for leaching bastnaesite through high-pressure complexing and belongs to the technical field of rare earth hydrometallurgy. According to the method for leaching the bastnaesite through high-pressure complexing, firstly, bastnaesite concentrate is mixed with a certain concentration of inorganic acid and a certain amount of easily-soluble aluminum slat; secondly, the mixture is added to a high-pressure reactor for pressure leaching, wherein the control conditions comprise that the particle size of the bastnaesite is 200 meshes or above, the molar concentration of hydrogen ions of the added inorganic acid is 0.5-2 mol / L, the total molar ratio of the fluorine element in the added bastnaesite concentrate to the aluminum element in the aluminum slat is 0.5-2, the liquid-solid ratio is (10-25):1, after the temperature is rapidly raised to 110-150 DEG C, the temperature is kept for 25-50 minutes, and the pressure is 0.5-4 MPa; and the bastnaesite is fully decomposed and dissolved in the solution, and fluorine and aluminum exist in the solution in a complex form. By the adoption of the method for leaching the bastnaesite through high-pressure complexing, operation is conducted in a high-pressure sealed environment, the environmental pollution is less, the acidity and the concentration of the aluminum are low, the reaction speed is high, the energy consumption is greatly lowered, and the economic benefits are high.

Description

technical field [0001] The invention relates to a method for high-pressure complexation leaching bastnaesite, which belongs to the technical field of rare earth hydrometallurgy. Background technique [0002] Bastnaesia rare earth concentrate is a composite compound of rare earth carbonate and rare earth fluoride, and its chemical formula can be expressed as REFCO 3 or REF 3 ·RE 2 (CO 3 ) 3 . This mineral is mainly distributed in California in the United States, Baiyun Obo in Inner Mongolia, Mianning County in Sichuan, Weishan County in Shandong and other places. Bastnaesite is thermally decomposed into rare earth oxides and oxyfluorides, and then rare earths are extracted by acid leaching, alkaline leaching or acid-base progressive leaching. [0003] At present, the various decomposition methods for single-type bastnaesite are mainly acid method and alkali method. The acid method mainly uses hydrochloric acid or sulfuric acid, such as concentrated sulfuric acid roastin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/06C22B59/00
CPCC22B3/065C22B3/08C22B3/10C22B59/00Y02P10/20
Inventor 张晓伟李梅柳召刚王觅堂胡艳宏胡家利
Owner INNER MONGOLIA UNIV OF SCI & TECH