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Method for preparing villiaumite and lithium salt by using high-lithium electrolyte

A technology of electrolyte and lithium salt, which is applied in the field of aluminum electrolyte recycling, can solve the problems of low molecular ratio of recycled cryolite, low electrolyte molecule, shrinking cryolite market demand, etc., and achieve the effect of high recovery rate and large market demand

Pending Publication Date: 2021-07-30
ZHENGZHOU JINGWEI TECH & IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Chinese patent CN108569711A discloses a method of extracting lithium salt from high-lithium electrolyte waste in aluminum electrolysis to prepare lithium carbonate. The high-lithium electrolyte is dissolved by sulfuric acid wet method. The purified electrolyte cannot be directly returned to the electrolytic cell for use due to its low molecular weight. ; Chinese patent CN105543504A discloses a method for extracting lithium salt in aluminum electrolyte by fluoridation roasting and acid leaching, using wet acidification to dissolve the electrolyte, and the regenerated cryolite and lithium carbonate obtained are also unable to directly because of the low molecular ratio of regenerated cryolite Return to the electrolyzer for use
Chinese patent CN105349786A discloses a method for comprehensive recycling of lithium-containing aluminum electrolytes to obtain cryolite and lithium carbonate, but the value of cryolite is low, and the production capacity of electrolytic aluminum is close to the ceiling, and the market demand for cryolite will gradually shrink
[0005] However, there are relatively few studies on the simultaneous preparation of aluminum fluoride-based fluoride salts and lithium salts using high-lithium electrolytes.

Method used

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  • Method for preparing villiaumite and lithium salt by using high-lithium electrolyte
  • Method for preparing villiaumite and lithium salt by using high-lithium electrolyte
  • Method for preparing villiaumite and lithium salt by using high-lithium electrolyte

Examples

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Embodiment 1

[0042] This embodiment provides a method for preparing fluorine salts and lithium salts using high-lithium electrolytes, including:

[0043] First take 100 kg of electrolyte particles with a particle size of less than 25 mm and 80 kg of aluminum sulfate in a ball mill and grind them to 300 mesh, and then mix them uniformly with 150 kg of sulfuric acid with a mass fraction of 5% to make a raw material mixed slurry, wherein the electrolyte particles including Na 3 AlF 6 Content 76%, Na 5 al 3 f 14 8% content, 8% LiF content, 2% C content, CaF 2 Content 3.2%, Al 2 o 3 content of 2.8%; the mixed slurry of the raw materials was atomized to a particle size of less than 120 μm, sprayed into a rotary furnace, calcined at 500°C for 2 h, added 320 kg of pure water after cooling, and wet-milled to less than 200 mesh. Dry at 500°C to obtain 75 kg of fluorine salt mixture; use XRD semi-quantitative analysis to detect and analyze the composition of the fluoride salt mixture, the resu...

Embodiment 2

[0047] This embodiment provides a method for preparing fluoride salts and lithium salts using high-lithium electrolytes, which includes: first taking 1000 kg of electrolyte particles with a particle size of less than 25 mm and 1500 kg of aluminum sulfate octadecahydrate into a ball mill, mixing and grinding to 400 mesh, Then it is uniformly mixed with 1200 kg of sulfuric acid with a mass fraction of 30% to make a raw material mixed slurry, wherein the electrolyte particles include Na 3 AlF 6 Content 80%, Na 5 al 3 f 14 6% content, 4% LiF content, 2.5% C content, CaF 2 Content 2.5%, Al 2 o 3 Content 5%; atomize the mixed slurry of the raw materials to a particle size of less than 150 μm, spray it into a rotary furnace, calcinate at 600°C for 5 hours, add 1600kg of pure water after cooling, wet grind to less than 200 mesh, and dry the filtered residue at 500°C , obtain 780 kg fluorine salt mixture, adopt XRD semi-quantitative analysis method to detect and analyze the compo...

Embodiment 3

[0051] This example provides a method for preparing fluoride salts and lithium salts using high-lithium electrolytes, including: first take 500 kg of electrolyte particles with a particle size of less than 25 mm, 350 kg of sodium sulfate and 350 kg of aluminum sulfate, add them to a ball mill, mix and grind to 400 mesh , and then uniformly mixed with 250 kg of sulfuric acid solution with a mass fraction of 50% to make a raw material mixed slurry, wherein the electrolyte particles include Na 3 AlF 6 Content 74%, Na 5 al 3 f 14 7% content, 10% LiF content, 2.5% C content, CaF 2 Content 3.2%, Al 2 o 3 content of 3.3%; the mixed slurry of the raw materials is atomized to a particle size of less than 150 μm, sprayed into a rotary furnace, calcined at 550°C for 1 h, cooled and then added with 1500 kg of pure water, and wet-milled to a size of less than 200 mesh. Dry at 550°C to obtain 315 kg of fluorine salt mixture. The composition of the fluoride salt mixture is detected and...

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Abstract

The invention provides a method for preparing villiaumite and lithium salt by using a high-lithium electrolyte, which comprises the following steps: uniformly mixing a high-lithium electrolyte, a sulfate and a sulfuric acid solution to obtain raw material mixed slurry; carrying out atomization treatment on the raw material mixed slurry, and then carrying out calcination treatment to prepare a calcined product; carrying out water washing treatment on the calcined product to obtain villiaumite filter residues and lithium-containing filtrate; drying the villiaumite filter residues to prepare villiaumite for electrolytic aluminum; and treating the lithium-containing filtrate to prepare the lithium salt. According to the method, fluorine and lithium in the high-lithium electrolyte can be recovered and converted into villiaumite and lithium salt with high additional values, and the recovery rate is high. In addition, the villiaumite and the lithium salt prepared by the method provided by the invention have large market demands, no waste, waste water or waste gas is discharged in the technological process, and the method is environment-friendly and pollution-free.

Description

technical field [0001] The invention relates to the technical field of recycling aluminum electrolytes, in particular to a method for preparing fluorine salts and lithium salts using high-lithium electrolytes. Background technique [0002] During the production of electrolytic aluminum, alumina and fluoride salts need to be supplemented regularly. A small amount of lithium oxide in alumina is converted into lithium fluoride or lithium cryolite in the electrolytic cell and gradually enriched. The content of lithium salts such as lithium fluoride and lithium cryolite can be as high as 4% to 12%, forming a high-lithium electrolyte. High-lithium electrolytes will reduce the solubility of alumina in it, and will increase the superheat of the electrolyte and increase energy consumption. , shorten the service life of the electrolytic cell. Usually, after the lithium salt is enriched to a certain extent, the electrolyte needs to be replaced, and the replaced high-lithium electrolyt...

Claims

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Application Information

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IPC IPC(8): C01F7/54C01F7/50C01D15/08C01D7/00C01D5/00
CPCC01F7/54C01F7/50C01D15/08C01D5/00C01D7/00C01P2002/72C01P2006/80C01P2004/80
Inventor 冯晓强于长军牛文军李伟华张敬一
Owner ZHENGZHOU JINGWEI TECH & IND
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