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Method for preparing lithium salt through recycling lithium fluoride-containing waste material material

A technology containing lithium fluoride and lithium fluoride, applied in the direction of lithium halide, etc., can solve problems such as environmental pollution and waste of lithium resources, and achieve the effect of reducing pollution

Active Publication Date: 2015-07-22
GANFENG LITHIUM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the process of industrial production or use, lithium fluoride-containing waste will be produced. The existing technology cannot recycle the lithium fluoride-containing waste. It can only be buried, which not only wastes limited lithium resources, but also causes environmental pollution.

Method used

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  • Method for preparing lithium salt through recycling lithium fluoride-containing waste material material
  • Method for preparing lithium salt through recycling lithium fluoride-containing waste material material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) add 420kg lithium fluoride waste material and 4m 3 Pure water, stirred evenly to form a slurry, heated up to 20°C; (2) adding 280kg of HCl solution with a concentration of 31% to the slurry, adjusting the pH of the slurry to 0, and stirring for 10 minutes of acidification reaction; (3) to the reaction Add 35% CaCl to the kettle 2 The solution was 2440kg, stirred for 30 minutes, and the CaCl was added within 10 minutes. 2 solution, stirring and reacting for 1h; (4) adding CaCO to the mixed solution obtained in step (3) 3Adjust the pH of the solution to be 6; (5) add NaOH with a concentration of 32% to the mixed solution to adjust the pH of the solution to 10; (6) filter the mixed solution and wash the filter residue 2 times; (7) according to step (6) Calcium in the filtrate that obtains, sulfate ion content adds the Na of calculated amount according to excess 1%. 2 CO 3 and BaCl 2 .8H 2 O, obtained after filtration about 5.5m 3 Purification solution; (8) the p...

Embodiment 2

[0048] (1) Add 420kg lithium fluoride waste and 2.1m 3 The lotion is evenly stirred to form a slurry, and the temperature is raised to 95° C.; (2) adding 280 kg of HCl solution with a concentration of 31% to the slurry, adjusting the pH of the slurry to 0, stirring and acidifying for 60 minutes; (3) going to the reaction Add 10% CaCl to the kettle 2 The solution was 7840kg, stirred for 60 minutes, and the CaCl was added within 60 minutes. 2 solution; (4) add CaCO to the mixed solution that step (3) obtains 3 The pH of the adjusting solution is 7; (5) adding concentration to the mixed solution is 32% KOH, adjusting the pH of the solution to 12; (6) filtering the mixed solution, washing the filter residue 4 times; (7) according to step (6) In the filtrate obtained by adding Na in excess of 2% 2 CO 3 and BaCl 2 .8H 2 O, 8.5m obtained after filtration 3 Purification solution; (8) the purification solution is concentrated to Li + The content is 55g / L, and the lithium chlori...

Embodiment 3

[0050] (1) add 420kg lithium fluoride waste material and 3m 3 The lotion is stirred evenly to form a slurry, and the temperature is raised to 60° C.; (2) adding 150 kg of HNO with a concentration of 65% to the slurry 3 solution, adjust the pH of the slurry to be 0, stir and acidify for 35min; (3) add a concentration of 35% Ca(NO 3 ) 2 Solution 4250kg, stirring reaction 45min, control to add Ca(NO 3 ) 2 solution; (4) add Ca(OH) to the mixed solution that step (3) obtains 2 The pH of the adjustment solution is 6.5; (5) adding concentration to the mixed solution is 32% liquid caustic soda, and adjusts the pH of the solution to 12; (6) the mixed solution is filtered, and the filter residue is washed 3 times; (7) according to calcium, sulfuric acid Radical ion content adds Na in the filtrate that obtains in step (6) by excessive 3%. 2 CO 3 and BaCl 2。 8H 2 O, obtained after filtration about 6.5m 3 Purification solution; (8) the purification solution is concentrated to Li ...

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Abstract

The invention relates to a method for preparing a lithium salt through recycling a lithium fluoride-containing waste material, wherein the method comprises the following steps: (1) ingredient preparation: putting the lithium fluoride-containing waste material and pure water or washing water into a reaction kettle to prepare a slurry; (2) acidification: adding an inorganic acid into the reaction kettle, and regulating the pH of the slurry; (3) transformation: adding a calcium salt into the reaction kettle, and transforming; (4) neutralization: adding calcium carbonate or calcium hydroxide to neutralize excess inorganic acid; (5) pH adjustment: adding an alkali, and regulating the pH of the solution; (6) filter pressing and washing; (7) purification and impurity removal: adding soluble carbonate and BaCl2 into the filtrate, and removing Ca<2+> and SO4<2->; and (8) evaporation concentration and sodium potassium precipitation to obtain a pure lithium salt solution. The treatment problem of the lithium fluoride-containing waste material is solved, environmental pollution is reduced, lithium resources are efficiently recycled to prepare the lithium salt, the recovery rate of lithium is high, and the lithium salt production costs are low.

Description

technical field [0001] The invention belongs to a treatment method of waste materials, in particular to a method for preparing lithium salt by recycling waste materials containing lithium fluoride. Background technique [0002] Lithium fluoride is a white non-hygroscopic cubic crystal, insoluble in water, alcohol and other organic solvents. Lithium fluoride is widely used in glass, ceramics and other fields as an additive to reduce the firing temperature and improve the heat resistance, wear resistance and acid resistance of the product. High-purity lithium fluoride is also used in the production of fluorinated glass and in the synthesis of electrolytes for secondary lithium-ion batteries. [0003] Lithium fluoride-containing waste will be generated during industrial production or use. The existing technology cannot recycle the lithium fluoride-containing waste, but can only be buried. This wastes limited lithium resources and causes environmental pollution. Contents of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/04
Inventor 李良彬章小明付晓春符龙廖萃何新田陈玲
Owner GANFENG LITHIUM CO LTD
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