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Method for preenriching and separating lithium and boron from salt lake brine by liquid-liquid-liquid three-phase extraction

A salt lake brine and pre-concentration technology, applied in chemical instruments and methods, lithium compounds, boron compounds, etc., can solve the problems of high solubility of diisobutyl ketone, high price, insufficient selectivity of precipitation method, etc., and achieve pH of solution. The effect of wide adaptation range and easy phasing behavior

Inactive Publication Date: 2014-07-30
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem of this method is that the solubility of diisobutyl ketone in water is large and the price is expensive, which has no practical industrial application significance; the single-stage extraction rate of lithium is low, and the seven-stage cascade extraction can only reach about 80%
The precipitation method is not selective enough and is not suitable for brines with high magnesium-lithium ratio or low lithium and boron concentrations

Method used

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  • Method for preenriching and separating lithium and boron from salt lake brine by liquid-liquid-liquid three-phase extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Take 50mL of the concentrated brine solution, and the brine composition is: Li + 2.21g / L, B 2 o 3 2.85g / L, Mg 2+ 100.71g / L, Na + 5.53g / L, K + 2.85g / L, the mass ratio of magnesium to lithium is 45.6.

[0053] Add co-extractant FeCl to the above brine 3 , the molar ratio of iron to lithium was 1.2:1, and the pH of the brine was adjusted to 1.5; then 10 g of water-soluble high molecular polymer polyethylene glycol PEG (molecular weight: 2000) was added, thoroughly mixed at room temperature and then centrifuged to separate phases to obtain the above, A two-liquid phase system in which the lower two layers coexist; 25 mL of kerosene solution with a volume percentage concentration of 80% TBP is added to the two-liquid phase system, and the obtained mixture is fully mixed at room temperature and left to separate phases to obtain upper, middle, and A three-liquid phase system in which the lower three layers coexist. The upper and middle two phases of the three-liquid ph...

Embodiment 2

[0055] Take 50mL of the concentrated brine solution, and the brine composition is: Li + 0.48g / L, B 2 o 3 0.89g / L, Mg 2+ 96.21g / L, Na + 9.03g / L, K + 5.48g / L, the mass ratio of magnesium to lithium is 200.4.

[0056] Add the co-extraction agent NaClO in the above brine 4 , ClO 4 - with Li + The molar ratio of the brine is 2:1, and the pH of the brine is adjusted to 7; then 15 g of the water-soluble polymer EOPO (molecular weight: 2500) is added, mixed thoroughly at room temperature, and the phases are separated by centrifugation to obtain a two-liquid phase in which the upper and lower layers coexist. system; add 30 mL of kerosene solution with volume percent concentration of 50% TOPO to the two-liquid phase system, and the obtained mixture is fully mixed at room temperature and left to separate phases to obtain a three-phase liquid phase in which upper, middle and lower layers coexist. system. The upper and middle two phases of the three-liquid phase system were resp...

Embodiment 3

[0058] Take 50mL of the concentrated brine solution, and the brine composition is: Li + 1.80g / L, B 2 o 3 20.89g / L, Mg 2+ 90.51g / L, Na + 6.89g / L,K + 1.85g / L, SO 4 2- 28.82g / L, the mass ratio of magnesium to lithium is 50.3.

[0059] Adjust the pH of the brine to 2, then add 15 g of water-soluble polymer polyethylene glycol PEG (molecular weight: 2000), mix well at room temperature and then centrifuge to separate the phases to obtain a two-liquid phase system in which the upper and lower layers coexist; Add 1,1,2,2,3,3-fluoroheptyl-7,7-dimethyl-4,6-octyldiketone (HFDMOP) with a concentration of 30% by volume to the two-liquid phase system 25 mL of heptane solution, the resulting mixture was fully mixed at room temperature and then allowed to stand for phase separation to obtain a three-phase system in which upper, middle and lower layers coexist. The upper and middle two phases of the three-liquid phase system were respectively taken to analyze the concentration of lith...

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Abstract

The invention relates to a method for preenriching and separating lithium and boron from salt lake brine by liquid-liquid-liquid three-phase extraction, which comprises the following steps: adding water-soluble auxiliary extractant into a salt lake concentrated brine solution, regulating the pH value of the brine, adding water-soluble high molecular polymer, and thoroughly mixing at room temperature to obtain an upper / lower two-layer liquid-phase system; adding organic extractant, and mixing to obtain an upper / middle / lower three-layer liquid-phase system; and taking the upper and middle phases from the three-liquid-phase system, and respectively recovering lithium and boron in the upper and middle phases by back washing. The invention can simultaneously enrich and extract lithium and boron by one-step extraction from high-magnesium / lithium-ratio salt lake brine, and can separate the lithium and boron from abundant coexistent ions of magnesium, calcium and other impurity metals in the brine. The lithium and boron are respectively selectively enriched from the upper and middle phases in the three-liquid-phase system to implement primary separation, thereby facilitating the subsequent purification and refinement. The three-liquid-phase extraction can be carried out under neutral or weakly-acidic conditions, and has strong adaptability.

Description

technical field [0001] The invention relates to the technical field of extraction and separation of valuable metal ions in salt lake brine, in particular to a liquid-liquid-liquid three-phase extraction pre-enrichment and separation method for lithium and boron in salt lake brine. Background technique [0002] Salt lake brine is rich in valuable metal ions such as potassium, sodium, lithium, boron, and magnesium. The total proven reserves of lithium resources in my country rank second in the world, second only to Bolivia, and the lithium resources in salt lake brine account for 79% of the country's total reserves, ranking third in the world. In addition, my country's boron resources are also relatively rich, but most of them are boron mafic ores that are difficult to use. Available and easy-to-process white boron ore only accounts for 6.7% of the total domestic reserves. After decades of mining, the current reserves are less than 3 million tons B 2 o 3 , which is expected...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B26/12C01D15/00C01B35/00
Inventor 黄焜刘会洲
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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