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Preparation method of battery-grade lithium carbonate

A lithium carbonate, battery-grade technology, applied in the direction of lithium carbonate; The same problem, to achieve the effect of improving lithium deposition rate, high recovery rate, and simple operation

Inactive Publication Date: 2018-07-17
SHANDONG LUBEI ENTERPRISE GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, by improving the roasting, leaching and purification conditions, the yield of lithium in lepidolite can be increased to 85%. The quality of lithium carbonate is difficult to meet the battery level requirements, and the loss of lithium in the sodium analysis process is also relatively large, resulting in a low total recovery rate of lepidolite
Due to the difference in lithium content and impurity content in lithium in spodumene and spodumene, the concentrations of sodium and potassium salts in the concentrated purification solution are very different. Therefore, spodumene cannot be completely used to prepare lithium carbonate during lithium precipitation. condition

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) First, Li 2 After the lepidolite ore with an O content of 3.9 is ground, it is mixed evenly according to the mass ratio of ore: sodium sulfate: limestone=0.5:0.4:0.1, and roasted at 950℃ for 90 minutes. After the roasting material is ground, the liquid-solid ratio is 2 :1, temperature 90℃, leaching for 90min, adding sodium carbonate and sodium hydroxide to the leaching solution to adjust the pH 11 to obtain the purified liquid, and then evaporate and concentrate the purified liquid to Li 2 The concentration of O is 39 g / l, and 30 ppm EDTA solution is added.

[0025] (2) Slowly add the lithium sulfate solution after purifying the concentrated solution to a certain amount of 300g / l sodium carbonate solution for a lithium precipitation. Sodium carbonate and Li in concentrate 2 The molar ratio of O is 1.2:1, the lithium sinking time is 40 minutes, and the lithium sinking temperature is 90°C. The primary lithium rate is 65.2%, the product Li 2 CO 3 The content is 99.52%.

[...

Embodiment 2

[0030] (1) First, Li 2 After the lepidolite ore with an O content of 3.8 is ground, it is mixed uniformly according to the mass ratio of ore: sodium sulfate: limestone = 0.5: 0.4: 0.1, and roasted at 960 ℃ for 90 min. After the roasting material is ground, the liquid-solid ratio is 3 :1, temperature 90℃, leaching for 90min, adding sodium carbonate and sodium hydroxide to the leaching solution to adjust the pH 11 to obtain the purified liquid, and then evaporate and concentrate the purified liquid to Li 2 The concentration of O is 36g / l, and 35ppm EDTA solution is added.

[0031] (2) Slowly add the lithium sulfate solution after purifying the concentrated solution to a certain amount of 300g / l sodium carbonate solution for a lithium precipitation. Sodium carbonate and Li in concentrate 2 The molar ratio of O is 1.3:1, the lithium sinking time is 40 minutes, and the lithium sinking temperature is 88°C. The primary lithium rate is 63.83%, the product Li 2 CO 3 The content is 99.54%....

Embodiment 3

[0036] (1) First, Li 2 After grinding the lepidolite ore with an O content of 4.0, mix it evenly according to the mass ratio of ore: sodium sulfate: limestone = 0.5: 0.3: 0.1, and roast it at 900 ℃ for 120 minutes. After the roasting material is ground, the liquid-solid ratio is 4 :1, temperature 85℃, leaching for 120min, adding sodium carbonate and sodium hydroxide to the leaching solution to adjust the pH 11 to obtain the purified liquid, and then evaporate and concentrate the purified liquid to Li 2 The concentration of O is 40g / l, and 30ppm EDTA solution is added.

[0037] (2) Slowly add the lithium sulfate solution after purifying the concentrated solution to a certain amount of 250g / l sodium carbonate solution for a lithium precipitation. Sodium carbonate and Li in concentrate 2 The molar ratio of O is 1.2:1, the lithium sinking time is 40 minutes, and the lithium sinking temperature is 90°C. The primary lithium rate is 65.61%, the product Li 2 CO 3 The content is 99.55%.

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Abstract

The invention provides a preparation method of battery-grade lithium carbonate. The preparation method comprises the steps: roasting lithionite, sodium sulfate and limestone by using a sulfate method,evaporating and concentrating a leachate, adding sodium carbonate, carrying out primary lithium sedimentation, and then, carrying out cooling to separate out sodium; and then, carrying out secondarylithium sedimentation. After a purified liquid is subjected to the primary lithium sedimentation and the secondary lithium sedimentation, the total recovery rate of lithium is high, and the requirement of battery-grade lithium carbonate is met. The method provided by the invention is capable of not only increasing the lithium sedimentation efficiency, but also reducing the loss of lithium in a sodium separation process during lithium sedimentation and sodium separation, simple in operation and high in safety.

Description

Technical field [0001] The present invention is a preparation method of battery-grade lithium carbonate, specifically a preparation method of producing battery-grade lithium carbonate from lepidolite by adopting a sulfate method. Background technique [0002] As the basic raw material for most other lithium products, lithium carbonate is widely used in glass, ceramics, metallurgy, chemicals, electronics, medicine, batteries and other fields. In recent years, in the context of national energy-saving emission reduction and sustainable development strategies, the lithium-ion battery industry has developed rapidly, and battery-grade lithium carbonate as a cathode material and electrolyte material for lithium batteries has become the focus of attention. With the rapid development of lithium batteries, the demand for battery-grade lithium carbonate is bound to increase. Currently, the preparation of lithium carbonate generally uses spodumene as a raw material, and some also use the sa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08
CPCC01D15/08C01P2006/80
Inventor 冯祥义冯怡利鲍树涛吕金辉马辉
Owner SHANDONG LUBEI ENTERPRISE GROUP
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