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Method of extracting lithium chloride from sulfate-type salt lake brine

A kind of salt lake brine and sulfate type technology, applied in the direction of lithium halide, etc., can solve the problem of high price of extraction agent, and achieve the effect of simple reaction route, high reaction yield and high industrial production value

Active Publication Date: 2016-10-26
青海柴达木兴华锂盐有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most suitable crown ether ring for extracting lithium is 14 crown-4. Due to the high price of this type of extractant, there is no report on its industrial application.

Method used

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  • Method of extracting lithium chloride from sulfate-type salt lake brine
  • Method of extracting lithium chloride from sulfate-type salt lake brine
  • Method of extracting lithium chloride from sulfate-type salt lake brine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The extractant is TBP and amide compound N,N-bis(2-ethylhexyl)acrylamide, whose structural formula is as follows:

[0022]

[0023] Its synthesis method is as follows: Add N,N-di-(2-ethylhexyl)amine into a three-necked flask, then add 1.1 equivalents of triethylamine, add dichloromethane as a solvent, and drop the system temperature to -5 ℃~0℃, dropwise add acryloyl chloride / dichloromethane solution, control the system temperature at 0℃, react for 2h, add water solution, collect the organic phase, and spin dry to obtain the target product.

[0024] 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), where the volume ratio of N,N-di(2-ethylhexyl)acrylamide, TBP and 200# solvent naphtha is 3:2:5, shake for 5 After 10 minutes rest layered. Determination of Li in the ...

Embodiment 2

[0028] The extractant is TBP and amide compound N-(1-methylbutyl)-N-cyclohexamethylene-3-methyl-2-butenamide, and its structural formula is as follows:

[0029]

[0030] 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 organic phase (compared to O / A = 5) with N-(1-methylbutyl)-N-cyclohexamethylene-3-methyl-2-butenamide, TBP and sulfo The volume ratio of kerosene is 2:1:2, and after shaking for 10 minutes, the layers are still separated. Determination of Li in the equilibrium aqueous phase + concentration, the single extraction rate of lithium was calculated to be 88.01%, and the yield reached 98.67% after three countercurrent extractions.

[0031] Comparison results: The amide compound extractant shown in the following structural formula was synthesized. Using the same method as above, the yield reache...

Embodiment 3

[0034] The extractant is TBP and amide compound N,N-dibutyl-2-methyl-2-butenamide, and its structural formula is as follows:

[0035]

[0036] 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-extraction agent, shake to dissolve it. Add 2 volumes of organic phase (compared to O / A = 0.8) with N,N-dibutyl-2-methyl-2-butenamide, TBP and sulfonated kerosene in a volume ratio of 1:1:2 , shake for 10 minutes and then rest for stratification. Determination of Li in the equilibrium aqueous phase + concentration, the calculated lithium extraction rate was 82.15%, and the yield reached 96.70% after three countercurrent extractions.

[0037] Comparison results: The amide compound extractant shown in the following structural formula was synthesized. Using the same method as above, the yield reached 81.28% after three countercurrent extractions.

[0038]

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Abstract

The invention provides a method of extracting lithium chloride from sulfate-type salt lake brine. An extraction system comprises an extractor, a co-extractor and a diluent, and the extractor is a mixture of an unsaturated hydrocarbon amide compound and tributyl phosphate. The extractor used in the method contains unsaturated hydrocarbon, and a 1, 4-conjugated system is formed between carbon-carbon double bond and carbon-oxygen double bond when double bonds of are directly connected with carbonyl; electric charge density on carbonyl oxygen is increased under action that carbonyl absorbs electrons, so that capability, in coordination with metal ions, of carbonyl is enhanced, and yield of extracted lithium is increased.

Description

technical field [0001] The invention relates to a method for extracting lithium chloride from sulfate type salt lake brine by solvent extraction. Background technique [0002] Lithium chloride is also widely used in the fields of biology and medicine. In addition, lithium chloride is also a raw material for producing lithium metal, a welding agent for aluminum, a dehumidifier for air conditioners, and a raw material for nonlinear optical materials in optical communications. As a result, the production of lithium chloride shows unprecedented good prospects. At present, the production method of lithium chloride is mainly the reaction of lithium carbonate or lithium hydroxide with hydrochloric acid. With the rapid rise of lithium carbonate and lithium hydroxide prices, it is no economic benefit to produce lithium chloride by this method. The invention adopts the extraction method to extract lithium chloride, the process is simple, the operation is convenient, the cost is low, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/04
CPCC01D15/04
Inventor 赵朋龙邱旭勇陈念
Owner 青海柴达木兴华锂盐有限公司
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