Method for recovering high-purity lithium carbonate by causticizing and freezing lithium precipitation mother liquor to remove mirabilite

A technology for sinking lithium mother liquor and lithium carbonate, applied in chemical instruments and methods, lithium carbonate;/acid carbonate, inorganic chemistry, etc., can solve the problems of large evaporation, high cost, and high processing cost, and achieve The effect of cheap raw materials, low cost and less raw materials

Pending Publication Date: 2022-01-11
FUZHOU UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing recovery process route generally adds acid to destroy the carbonate, then concentrates to remove sodium sulfate and then adds sodium carbonate to precipitate lithium. In the whole process, the consumption of sulfuric acid and sodium carbonate is large, the cost is high, and the recovery rate of lithium is low.
[0004] The invention patent (ZL201110122564.9) discloses a treatment method for battery-grade lithium carbonate lithium precipitation mother liquor. First, sulfuric acid is used to acidify the lithium precipitation mother liquor, evaporate and concentrate, and then adopt steps such as sodium analysis, lithium precipitation, and cycle mother liquor to recover battery-grade lithium carbonate. Mother liquor is used to prepare battery-grade lithium carbonate. This process has a large amount of evaporation, high evaporation energy consumption, and low recovery rate of lithium precipitation.
The process technology is complex and cumbersome, the lithium recovery rate is not high, and the treatment cost is also high

Method used

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  • Method for recovering high-purity lithium carbonate by causticizing and freezing lithium precipitation mother liquor to remove mirabilite

Examples

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Embodiment 1

[0028] A method for recovering high-purity lithium carbonate by causticizing, freezing, and removing Glauber's salt from lithium-precipitating mother liquor, comprising the following steps: S1. The content is 2.3g / L, the carbonate ion content is 13g / L, the sodium ion content is 70g / L, and the sulfate ion content is 150g / L. Add calcium oxide containing 1.1-1.3 times the molar amount of carbonate ions. The specific amount of lithium sinking mother liquor is 5L, and the amount of calcium oxide added is 73g. After calcium oxide is added, the pH of the solution is 12.2, causticizing and stirring for 2.5 hours, and the temperature is 50 ℃, calcium carbonate precipitate and causticizing solution are obtained after filtration. S2. Concentration by evaporation: Evaporate and concentrate the causticizing solution obtained in step S1 to a solution specific gravity of 1.2, and then perform solid-liquid separation to obtain a concentrated solution (lithium ion concentration of 6.5 g / L) and...

Embodiment 2

[0030] A method for recovering high-purity lithium carbonate by causticizing, freezing, and removing Glauber's salt from lithium-precipitating mother liquor, comprising the following steps: S1. The content is 2.5g / L, the content of carbonate ion is 15g / L, the content of sodium ion is 75g / L, and the content of sulfate ion is 160g / L. Add calcium oxide containing 1.1-1.3 times the molar amount of carbonate ions. The specific amount of lithium sinking mother liquor is 5L, and the amount of calcium oxide added is 91g. After calcium oxide is added, the pH of the solution is 12.5 and the reaction is causticized and stirred for 3 hours. Calcium carbonate precipitate and causticizing solution are obtained after filtration. S2. Evaporation and concentration: the causticizing solution obtained in step S1 was evaporated and concentrated to a specific gravity of 1.23, followed by solid-liquid separation to obtain a concentrated solution (lithium ion concentration of 6.6 g / L) and sodium sul...

Embodiment 3

[0032]A method for recovering high-purity lithium carbonate by causticizing, freezing, and removing Glauber's salt from lithium-precipitating mother liquor, comprising the following steps: S1. The content is 2.7g / L, the carbonate ion content is 20g / L, the sodium ion content is 80g / L, and the sulfate ion content is 170g / L. Add calcium oxide containing 1.1-1.3 times the molar amount of carbonate ions. The specific amount of lithium sinking mother liquor is 5L, and the amount of calcium oxide added is 116g. After calcium oxide is added, the pH of the solution is 12.7, causticizing and stirring for 3 hours, and the temperature is 70°C , After filtration, calcium carbonate precipitate and causticizing solution are obtained. S2. Evaporation and concentration: the causticizing solution obtained in step S1 was evaporated and concentrated to a specific gravity of 1.25, followed by solid-liquid separation to obtain a concentrated solution (lithium ion concentration of 6.8 g / L) and sodiu...

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Abstract

The invention discloses a method for causticizing and freezing lithium precipitation mother liquor to remove mirabilite and recycle high-purity lithium carbonate. The method comprises the following steps of 1, lime causticizing, 2, evaporation concentration, 3, freezing crystallization and 4, carbonization lithium precipitation. The method has the beneficial effects that calcium oxide is added to remove the influence of carbonate ions in the lithium precipitation mother liquor, sodium sulfate decahydrate formed by sodium sulfate under a low-temperature condition is utilized to remove sulfate ions and sodium ions after concentration, and then carbon dioxide is absorbed and carbonized to obtain high-purity lithium carbonate. Therefore, the carbonate ions are removed through causticization of cheap quick lime, so that the complex route that in a traditional route, sulfuric acid is added for acidification to remove the carbonate ions, and sodium carbonate needs to be continuously supplemented for lithium precipitation after follow-up concentration is avoided. Besides, the added raw materials are few and cheap, and the cost is low. The high-purity lithium carbonate is finally recycled and prepared, and compared with industrial-grade and battery-grade lithium carbonate, the high-purity lithium carbonate is better in application effect and higher in value.

Description

technical field [0001] The invention relates to the field of recovering and preparing high-purity lithium carbonate from lithium-precipitating mother liquor, in particular to a method for recovering high-purity lithium carbonate from lithium-precipitating mother liquor by causticizing, freezing and removing Glauber's salt. Background technique [0002] In industrial production, the mother liquor after lithium sulfate is added to sodium carbonate for lithium precipitation also contains a certain amount of lithium ions, which can be recycled. The process for producing lithium carbonate from the existing lithium precipitation mother liquor is complicated and costly, and the recovered lithium carbonate is generally only Reach industrial grade (lithium carbonate concentration ≥ 99.2%) and battery grade (lithium carbonate concentration ≥ 99.5%), so how to efficiently use the lithium sinking mother liquor to recover and prepare high-purity lithium carbonate is of great significance....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08C01D5/00C01D5/16
CPCC01D15/08C01D5/004C01D5/16C01P2006/80
Inventor 旷戈李延鹤刘粤郑芳妍姜昀刘慧勇
Owner FUZHOU UNIV
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