Method for extracting lithium salt from lithium ore

A lithium ore and lithium extraction technology, applied in the direction of lithium carbonate;/acid carbonate, etc., can solve the problems of reduced yield and efficiency, equipment corrosion, large amount of neutralized slag, etc., and achieve high comprehensive utilization rate , the effect of improving yield and easy washing

Active Publication Date: 2019-03-08
CHANGSHA YUANPENG CHEM TECH
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AI Technical Summary

Problems solved by technology

The main disadvantages of the sulfuric acid method are ① a large amount of sulfuric acid is required during leaching, and a large amount of aluminum elements are taken in and out, resulting in a large amount of neutralized slag and low production efficiency; ② the leaching time is long, requiring more than 8 hours, and the energy consumption is high; , hydrofluoric acid volatilizes, which is extremely corrosive to equipment and not friendly to the environment
[0008] The advantage of the sulfate method is that the roasting conversion rate is higher in the early stage, but sodium sulfate, potassium sulfate and lithium sulfate are easy to form double salts in the solution, resulting in lower yield and efficiency in the later stage

Method used

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  • Method for extracting lithium salt from lithium ore

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Weigh 5000g of spodumene with a lithium oxide content of 7.5%, add 4800g of calcium chloride, and mix evenly; roast at 1050°C for 60 minutes to obtain a roasted material; take it out, cool to room temperature, add 12000mL of water, and stir for 30 minutes. Filtration to obtain filtrate and filter residue.

[0047] Table 1 Spodumene data, %

[0048] Li / Li2O

K

Rb

Cs

3.49 / 7.50

0.35

0.10

0.035

[0049] Table 2 filtrate data, g / L

[0050] Li

Na

K

14.52

1.03

1.44

[0051] Table 3 Residue data, %

[0052]

Li

K

Rb

Cs

Lithium slag

0.07

0.03

0.0015

0.0007

Leaching rate

99.07

91.43

98.50

98.00

[0053] (2) Concentrate the filtrate obtained in step (1), and separate the obtained concentration into solid and liquid. The liquid data are as follows:

[0054] Table 4 Concentrate data, g / L

[0055] LiCl

Na

K

Rb

Cs ...

Embodiment 2

[0065] (1) Weigh 2000g of finely ground β-spodumene with a lithium oxide content of 6.0%, add 2400g of calcium chloride, 1000g of sodium chloride, and potassium chloride mixed salt, and mix evenly; roast at 920°C for 20 minutes to obtain a roasted material; Take it out, after cooling to room temperature, add 4000mL of water, stir for 30min, and filter to obtain filtrate and filter residue.

[0066] Table 6 Spodumene data, %

[0067] Li / Li2O

[0068] Table 7 filtrate data, g / L

[0069] Li

[0070] Table 8 Residue data, %

[0071] Li2CO3

[0072] (2) Concentrate the filtrate obtained in step (1), and separate the obtained concentration into solid and liquid. The liquid data are as follows:

[0073] Table 9 Concentrate data, g / L

[0074] LiCl

[0075] (3) Adjust the concentrated solution obtained in step (2) to a lithium content of 22g / L, add a slight excess of sodium carbonate and sodium hydroxide according to the residual divalent meta...

Embodiment 3

[0081] (1) Weigh 6000g of finely ground spodumene with a lithium oxide content of 5.3%, add 500g of calcium carbonate, 3600g of calcium chloride, and 2000g of sodium chloride, and mix well; roast at 990°C for 60 minutes to obtain a roasted material; take it out and cool After reaching room temperature, 15 L of water was added, stirred for 30 min, and filtered to obtain filtrate and filter residue.

[0082] Table 11 Spodumene data, %

[0083] Li / Li2O

[0084] Table 12 Filtrate data, g / L

[0085] Li

[0086] Table 13 Residue data, %

[0087]

[0088] (2) Concentrate the filtrate obtained in step (1), and separate the obtained concentration into solid and liquid. The liquid data are as follows:

[0089] Table 14 Concentrate data, g / L

[0090] LiCl

[0091] (3) Adjust the concentrated solution obtained in step (2) to a lithium content of 22g / L, add a slight excess of sodium carbonate and sodium hydroxide according to the residual divalent...

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Abstract

The invention discloses a method for extracting lithium salt from lithium ore. The method comprises the steps as follows: performing material mixing, roasting, water extraction, concentration, separation of sodium, potassium, rubidium and cesium, purification and impurity removal, lithium precipitation, washing, drying and fine grinding to obtain battery-grade lithium carbonate; performing neutralization, concentration, separation of sodium, potassium, rubidium and cesium, washing and drying on primary lithium precipitation mother liquor to obtain industrial-grade or battery-grade lithium carbonate; returning obtained secondary mother liquor to be mixed with the primary lithium precipitation mother liquor to form a closed loop. The method has better leaching effects on various content of lithium, sodium, potassium, rubidium and cesium in lithium ore, the lithium leaching rate in spodumene reaches 99%, and the leaching rates of rubidium and cesium in lepidolite are larger than 99%; recovery rate of lithium later is larger than 97% and the total yield of lithium is larger than 91%. Byproducts can be reused, and the method is environmentally friendly due to the fact that fluorine is fixed in slag, adopts a short technological process, is low in cost and has good industrial promotion value.

Description

technical field [0001] The invention relates to a process for extracting lithium salt, which is suitable for extracting and preparing lithium salt by using lithium ore as a raw material, and belongs to the technical field of rare metal extraction. Background technique [0002] Lithium salts, especially lithium carbonate, are widely used in glass, ceramics, lubricants and other fields, and are also widely used in high-tech fields such as lithium batteries, nuclear energy, aerospace and other fields. Especially in recent years, with the rapid development of the new energy automobile industry, large-scale energy storage equipment, 3C equipment, and wearable equipment, the demand for lithium carbonate in the global market is increasing year by year. [0003] The global lithium resources can be divided into ore and brine resources, among which the ore resources are mainly spodumene, lepidolite, lapidolite, and lithium feldspar. my country is mainly rich in spodumene and spodumen...

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 吕运征吕运凤徐雪梅
Owner CHANGSHA YUANPENG CHEM TECH
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