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A method for extracting lithium from high magnesium-lithium ratio salt lake brine

A technology of salt lake brine and high magnesium-lithium ratio, applied in the direction of improving process efficiency, etc., can solve the problems of strong corrosion of equipment and low product purity, achieve high reaction yield, easy access to reaction raw materials, and improve water-in-oil The effect of the phenomenon

Active Publication Date: 2019-05-03
金昆仑锂业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the shortcomings of the existing solvent extraction method for extracting lithium salts from high-magnesium-lithium ratio salt lake brine, the equipment is highly corrosive, the stripping solution is directly evaporated, and the product produced by crystallization is not high in purity, the present invention provides a method that can reduce Corrosive to equipment and can improve the method of product purity, suitable for industrial production

Method used

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  • A method for extracting lithium from high magnesium-lithium ratio salt lake brine
  • A method for extracting lithium from high magnesium-lithium ratio salt lake brine
  • A method for extracting lithium from high magnesium-lithium ratio salt lake brine

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Experimental program
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Effect test

Embodiment 1

[0019] The extractant is TBP and sulfonamide compound N,N-bis-(2-ethylhexyl)ethylsulfonamide, whose structural formula is as follows:

[0020]

[0021] The synthesis method of the above-mentioned N,N-bis-(2-ethylhexyl)ethylsulfonamide: add 0.3mol of N,N-bis-(2-ethylhexyl)amine into a 1000ml three-necked flask, add 0.33mol of Ethylsulfonyl chloride, 200ml dichloromethane, stir to cool down to -5°C~0°C, add dropwise 0.3mol ethylsulfonyl chloride / 150ml methylene chloride solution, keep the system temperature below 5°C during the dropwise addition, and complete the dropwise addition , react at 0°C for 2h, add 220ml of water, extract and keep the organic phase. The organic phase was washed with alkali and acid respectively, dried with anhydrous sodium sulfate, and spin-dried to obtain the target product.

[0022] Add 1 volume of salt lake brine shown in Table 1 into a separatory funnel, add a certain amount of FeCl 3 (FeCl 3 Li in brine + The molar ratio is 1:1) as a co-extr...

Embodiment 2

[0026] The extractant is TBP and sulfonamide compound N-methyl-N-phenylethyl ethyl sulfonamide, and its structural formula is as follows:

[0027]

[0028] Add 1 volume of salt lake brine shown in Table 1 into a separatory funnel, add a certain amount of FeCl 3 (FeCl 3 Li in brine + The molar ratio is 1:1.5) as a co-extraction agent, shake to dissolve it. Add 5 volumes of the organic phase (compared to O / A=5), wherein the volume ratio of N-methyl-N-phenylethylethylsulfonamide, TBP and 200# solvent naphtha is 4:3:3, shake for 10 After 10 minutes rest layered. Determination of Li in the equilibrium aqueous phase + , Calculate the extraction rate of lithium to be 90.96%. After washing, stripping, evaporation, decolorization, cooling, crystallization and drying, the Na in the product is measured + 、K + , Mg 2+ , Ca 2+ , SO 4 2- , B 2 O 3 The percentage contents are 0.0030%, 0.0008%, 0.0016%, 0.0005%, 0.0012%, 0.028%, respectively.

Embodiment 3

[0030] The extractant is TBP and sulfonamide compound N-methyl-N-(2-pyridine) ethyl isopropyl sulfonamide, its structural formula is as follows:

[0031]

[0032] Add 1 volume of salt lake brine shown in Table 1 into a separatory funnel, add a certain amount of FeCl 3 (FeCl 3 Li in brine + The molar ratio is 1:1.3) as a co-extraction agent, shake to dissolve it. Add 2 volumes of organic phase (compared to O / A = 2) with N-methyl-N-(2-pyridine)ethylisopropylsulfonamide, TBP and sulfonated kerosene in a volume ratio of 1:3: 6. After shaking for 10 minutes, rest and stratify. Determination of Li in the equilibrium aqueous phase + , Calculate the extraction rate of lithium to be 81.17%. After washing, stripping, evaporation, decolorization, cooling, crystallization and drying, the Na in the product is measured + 、K + , Mg 2+ , Ca 2+ , SO 4 2- , B 2 O3 The percentage contents are 0.0026%, 0.0007%, 0.0014%, 0.0005%, 0.0010%, 0.024%, respectively.

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Abstract

The invention provides a method for extracting lithium chloride from high-magnesium-lithium ratio salt lake brine by solvent extraction. The extraction system includes an extraction agent, a co-extraction agent and a diluent, and the extraction agent is a sulfonamide compound and tributyl phosphate A mixture of esters, the co-extraction agent is ferric chloride, and the diluent is solvent gasoline or sulfonated kerosene. The present invention reduces the concentration of tributyl phosphate, thereby reducing the amount of brine dissolved in tributyl phosphate, improving the water-in-oil phenomenon, improving product purity, and the acidity of such substances in the stripping process Its hydrolysis ability is reduced, the loss of the oil phase in multiple extraction processes is reduced, and the yield of lithium extraction in the prior art is achieved at the same time. The extraction process is simple to operate and easy to industrialized production.

Description

technical field [0001] The invention relates to a method for extracting lithium salt from brine of a high-magnesium-lithium ratio salt lake by using a solvent extraction method. Background technique [0002] my country is a country with a large amount of lithium resources, and its proven reserves of lithium resources rank second in the world, second only to Bolivia. The salt lake lithium resources in the Qaidam Basin in Qinghai are very rich, ranking first in the country. The main feature of the lithium-rich salt lake in Qinghai is the high content of associated magnesium, and the magnesium / lithium ratio in the brine is as high as 40-1200. Because the chemical properties of magnesium and lithium are very similar, it is very difficult to separate and extract lithium, which has long restricted the development of lithium extraction industry in Qinghai brine. [0003] Solvent extraction is a lithium extraction technology that has been studied more in China. It has the advantag...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B26/12C22B3/40
CPCC22B26/12C22B3/409Y02P10/20
Inventor 赵朋龙邱旭勇魏廷祥
Owner 金昆仑锂业有限公司
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