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A method of purifying cryolite

A technology of cryolite and filter cake, applied in the field of purification

Active Publication Date: 2018-09-04
INNER MONGOLIA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no relevant report on the purification process of crude cryolite synthesized by complexation leaching solution. This patent is aimed at the purification of this newly synthesized crude cryolite.

Method used

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  • A method of purifying cryolite
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  • A method of purifying cryolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 20g of crude cryolite raw material synthesized by complexation leachate, mix it with water at a solid-to-liquid ratio of 1:10 to make slurry, add it to the reactor, heat to 100°C, and slowly adjust the pH value of the solution to 8 with sodium carbonate solution. Control the speed of the agitator to be 500rpm, filter after reacting for 30 minutes, wash the filter cake three times with sodium carbonate solution, mix the filter cake and water at a liquid-solid ratio of 1:50, add the mixed acid of HF-HCl to the slurry, The concentration ratio of HF:HCl is 1:0.1, the mass ratio of solid to mixed acid is 1:0.25, heat up to 60°C, stir at 300rpm stirring speed for 45min, filter, wash and dry with clean water to obtain 19.56g of pure cryolite , The recovery rate was 97.8%, and the impurity content in the product was analyzed, and the results are shown in Table 2.

[0016]

Embodiment 2

[0018] Weigh 20g of crude cryolite raw material synthesized by complex leachate, mix it with water at a solid-to-liquid ratio of 1:20 to make slurry, add it to the reactor, heat to 80°C, and slowly adjust the pH value of the solution to 9 with sodium bicarbonate solution. , control the speed of the agitator to be 600rpm, filter after 60 minutes of reaction, wash the filter cake three times with sodium bicarbonate solution, mix the filter cake and water at a liquid-solid ratio of 1:60, and add a mixture of HF-HCl to the slurry acid, the concentration ratio of HF:HCl is 1:0.2, the mass ratio of solid to mixed acid is 1:0.4, heat up to 80°C, stir at 500rpm stirring speed for 60min, filter and wash and dry with clean water to obtain pure cryolite 19.71g, the recovery rate is 98.55%, the impurity content in the analysis product, the results are shown in Table 3.

[0019]

Embodiment 3

[0021] Weigh 20g of the crude cryolite raw material synthesized by the complex leach solution, mix it with water at a solid-to-liquid ratio of 1:30 to make slurry, add it to the reactor, heat it to 70°C, and slowly adjust the pH value of the solution to 10 with ammonium carbonate solution. Control the speed of the agitator to be 800rpm, filter after reacting for 120 minutes, wash the filter cake three times with ammonium carbonate solution, mix the filter cake and water according to the liquid-solid ratio of 1:40, add the mixed acid of HF-HCl to the slurry, The concentration ratio of HF:HCl is 1:1, the mass ratio of solid to mixed acid is 1:0.5, heat up to 70°C, stir at 400rpm stirring speed for 100min, filter and wash and dry with clean water to obtain 19.85g of pure cryolite , the recovery rate was 99.25%, and the impurity content in the product was analyzed, and the results are shown in Table 4.

[0022]

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Abstract

The invention relates to a method for purifying cryolite, in particular to cryolite synthesized for waste liquid obtained after Baotou mixed rear earth concentrate complexation leaching is conducted, and a method for purifying the cryolite is developed. The method comprises the steps that coarse cryolite and water are mixed in proportion for pulping and heated, soluble carbonate is added to regulate the pH value of slurry, reacting is conducted for a certain time at a constant stirring speed, then filtering and washing are conducted, filter cake and water are mixed for secondary pulping, then mixed acid of HF and HCl is added, the mixture is heated to a certain temperature and stirred at a constant speed, reacting is conducted for a certain time, filtering and washing are conducted, and pure cryolite is obtained. The cryolite synthesized through F<-> and Al<3+> waste liquid obtained after Baotou mixed rear earth concentrate complexation leaching is conducted is purified; the technology is easy to operate, high efficiency and energy conservation are achieved, the cryolite recovery rate can reach 97% or above, all indexes of the cryolite can reach the national standard of industrial ordinary cryolite.

Description

technical field [0001] The method for purifying cryolite involved in the present invention, more specifically, is a purification method developed for cryolite synthesized from Baotou mixed rare earth concentrate complexation leaching waste liquid. Background technique [0002] Cryolite, also known as sodium hexafluoroaluminate or sodium aluminum fluoride, has a molecular formula of Na 3 AlF 6 , white fine crystals. Cryolite is mainly used as a flux for aluminum electrolysis, a wear-resistant filler, an opacifying agent, an opacifying agent, a metal flux, and an insecticide for crops. The content of cryolite in nature is rare, so the cryolite used in industry is artificially manufactured. Cryolite production processes at home and abroad include: fluorite method, phosphate fertilizer by-product method, ammonium fluoroaluminate method, fluorine-containing waste gas method and recycled cryolite recovery method. The most commonly used method is the fluorite method, but due to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/54
CPCC01F7/54C01P2006/80
Inventor 李梅张晓伟胡家利胡艳宏王觅堂柳召刚
Owner INNER MONGOLIA UNIV OF SCI & TECH