Method for extracting lithium salt from high magnesium-lithium ratio salt lake brine

A technology of salt lake brine and high magnesium-lithium ratio, applied in the direction of lithium carbonate;/acid carbonate, process efficiency improvement, etc., can solve the problem of large water-soluble loss of organic phase, difficult digestion of by-product hydrochloric acid, and complicated process flow and other issues, to achieve the effects of reducing energy consumption, improving purity, and high process economy

Active Publication Date: 2019-01-11
湖南中大技术创业孵化器有限公司
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Problems solved by technology

However, the high-concentration tributyl phosphate in this system has disadvantages such as strong corrosion to extraction equipment, large water-soluble loss of the organic phase, and easy degradation in acidic media, making it difficult for large-scale industrial application
In 2012, the Chinese invention patent 201210055323.1 applied by the Qinghai Salt Lake Institute of the Chinese Academy of Sciences proposes to use alkali metal chlorides, alkaline earth metal chlorides or their mixtures to replace all-acid and all-alkali phase inversion in the extraction process of Chinese invention patent 87103431 to reduce acid-base costs And reduce the corrosion of the equipment. In 2012, the Chinese invention patent 201210164150.7 applied by the Qinghai Salt Lake Institute of the Chinese Academy of Sciences proposed an extraction system using a mixture of amides and neutral phosphorus and oxygen compounds as the extraction agent. Compared with a single extraction agent, the extraction system Tributyl phosphate can reduce the corrosion of equipment. The above improvements can partially improve the equipment corrosion problems in the tributyl phosphate extraction system. However, the existing salt lake brine extraction method for lithium still has complex process flow, high extraction reagent prices, and poor extraction equipment. High anti-corrosion requirements, large investment, and high overall production costs
The main problem of this method is that the high-temperature calcination process consumes a lot of energy, produces a large amount of by-product hydrochloric acid that is difficult to digest and severely corrodes equipment, and the production cost is high

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

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Experimental program
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specific Embodiment 1

[0027] Lithium-containing original salt lake brine is exposed to the sun in a solar salt field to obtain lithium-rich brine saturated with magnesium chloride. The brine composition (g / l): Li + 1.85, Na + 0.82,K + 0.65, Mg 2+ 106,B 2 o 3 3.64, SO 4 2- 32.63; the lithium-rich brine is spray-dried, the feed temperature of the spray-drying is room temperature, the air-in temperature of the spray-drying is 360°C, and the air-out temperature is 150°C, and a dry dehydrated solid product containing lithium chloride is produced; Dry and dehydrate the solid product at 150~300°C for 1~60min with ammonia gas flow to generate an ammonified solid product containing magnesium chloride ammonium compound and lithium chloride; use 50~100% ammonia saturated ethanol for the ammoniated solid product Solution 5-stage countercurrent extraction, extraction liquid-solid ratio 5:1, extraction time 80min, extraction temperature 20~30°C; after extraction, the slurry was centrifuged to obtain lithiu...

specific Embodiment 2

[0029] Such as figure 1 As shown, the lithium-rich brine saturated with magnesium chloride is evaporated and concentrated—acidified to extract boron—extracted to extract boron—removed from sulfate to obtain refined brine, and the composition of refined brine (g / l): Li + 9.88, Na + 0.35,K + 0.24, Mg 2+ 106,B 2 o 3 0.12, SO 4 2- 0.46; the refined brine is spray-dried, the feed temperature of the spray drying is 120°C, the air inlet temperature of the spray drying is 400°C, and the air outlet temperature is 180°C, and a dry dehydrated solid product containing lithium chloride is produced; the Dry and dehydrate the solid product at 150~300°C through ammonia gas flow for 1~60min to generate an ammoniated solid product containing magnesium chloride ammonium compound and lithium chloride; use 80~100% ammonia saturated ethanol for the ammoniated solid product 5-stage countercurrent extraction of the solution, the extraction liquid-solid ratio is 10:1, the extraction time is 120...

specific Embodiment 3

[0031] Lithium-rich brine saturated with magnesium chloride is concentrated by evaporation—acidification to extract boron—extraction to extract boron—removal of sulfate to obtain refined brine. The composition of refined brine (g / l): Li + 9.88, Na + 0.35,K + 0.24, Mg 2+ 106,B2 o 3 0.12, SO 4 2- 0.46; the refined brine is spray-dried, the feed temperature of the spray drying is 120°C, the air inlet temperature of the spray drying is 400°C, and the air outlet temperature is 180°C, and a dry dehydrated solid product containing lithium chloride is produced; the Dry and dehydrate the solid product at 150~300°C through ammonia gas flow for 1~60min to generate an ammoniated solid product containing magnesium chloride ammonium compound and lithium chloride; use 80~100% ammonia saturated ethanol for the ammoniated solid product 5-stage countercurrent extraction of the solution, the extraction liquid-solid ratio is 10:1, the extraction time is 120min, and the extraction temperature...

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Abstract

The invention discloses a method for extracting lithium salt from salt lake brine with a high ratio of magnesium to lithium. The method comprises steps as follows: organic alcohol with ammonia gas dissolved is taken as an extraction agent and used for extracting a solid phase obtained after spray drying-ammoniation transformation processing of the salt lake brine with the high ratio of magnesium to lithium, and anhydrous lithium chloride is obtained from an extraction liquid through reduced-pressure distillation or lithium carbonate is obtained through carbonization treatment. Compared with the prior art, the method has the advantages that neither high-temperature calcination nor a complicated extraction system is required, reagents used in the method have low corrosiveness and are inexpensive and available, most of the reagents can be recycled, the production cost is low, and engineering implementation is easy.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for extracting lithium salt from brine of a salt lake with a high magnesium-lithium ratio. Background technique [0002] Salt lake brine is an important resource of lithium. my country has abundant lithium resources of salt lake brine, and its reserves rank among the top in the world. Lithium ions coexist with a large amount of alkali metals and alkaline earth metals in salt lake brine. The economical recovery of lithium from salt lake brine, a natural multi-water salt system, depends not only on the concentration of lithium but also on the concentration of magnesium and calcium ions. Lithium extraction from brine produced abroad is limited to brine with low magnesium concentration, and the ratio of magnesium to lithium is less than 6:1. For the so-called "high-magnesium-lithium" salt lakes containing high-concentration magnesium and low-concentration lithium, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B26/12C01D15/08
CPCC01D15/08Y02P10/20
Inventor 欧阳红勇郭永兴
Owner 湖南中大技术创业孵化器有限公司
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