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Method for reducing ratio of magnesium to lithium in salt lake through solar-assisted salt crystallization

A magnesium-lithium ratio and salt lake technology, applied in the direction of lithium carbonate;/acid carbonate, magnesium chloride, magnesium halide, etc., can solve the problems of long production cycle, high power and water consumption of adsorption method, and high corrosion. problems, to achieve the effect of saving manpower and material resources, shortening the production cycle, and simplifying the production process

Active Publication Date: 2019-10-18
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the solvent extraction method has high requirements on the acid corrosion resistance of the equipment, the acid and alkali consumption is high, and the organic phase residue of the raffinate pollutes the surrounding environment of the salt lake; the adsorption method consumes a lot of power and water, the eluent has a low lithium content, and the production The stability is poor; the HCl gas generated by the calcination water immersion method is highly corrosive, the energy consumption is high, and the amount of by-products is too large. The total recovery yield is low, and there are still difficulties in practical application; for brine with high lithium content and low magnesium-lithium ratio, evaporation crystallization separation method and precipitation method are generally used. The precipitation method is divided into two steps: salt field evaporation concentration and precipitation separation. Evaporation concentration is The process of naturally evaporating, concentrating, and separating high-concentration lithium-containing brine through salt field sun exposure, but this process has a long production cycle (15-30 days) and is greatly affected by natural conditions, resulting in low production efficiency.

Method used

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  • Method for reducing ratio of magnesium to lithium in salt lake through solar-assisted salt crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) At room temperature, in the primary salt field of magnesium-lithium saturated brine with a magnesium-lithium ratio of 80:1, according to Mg 2+ Mg in salt and saturated brine 2+ Add Mg to the molar ratio of 1:8 2+ Salt, dry the salt in the salt field for 4 days to get clear liquid and granular precipitated crystal MgCl 2·6H 2 O.

[0029] (2) Introduce the clear liquid into the secondary salt field, collect the precipitated crystal MgCl 2 ·6H 2 O, MgCl 2 ·6H 2 O is dehydrated at 105°C to obtain MgCl 2 4H 2 O, MgCl 2 4H 2 O is heated to 150°C for dehydration to obtain MgCl 2 2H 2 O.

[0030] (3) According to Mg 2+ Mg in the supernatant solution of salt and step (2) 2+ The molar ratio is 1:8 plus Mg 2+ Salt in secondary salt pans, where Mg 2+ Salt contains all of the MgCl prepared in step (2) 2 2H 2 O, the clear liquid was sun-salted for 4 days, and the clear liquid and granular precipitated crystal MgCl were obtained again 2 ·6H 2 O.

[0031] (4) ...

Embodiment 2

[0034] (1) At room temperature, in the primary salt field of magnesium-lithium saturated brine with a magnesium-lithium ratio of 200:1, according to Mg 2+ Mg in salt and saturated brine 2+ Add Mg to the molar ratio of 1:5 2+ Salt, dry the salt in the salt field for 7 days to obtain clear liquid and granular precipitated crystal MgCl 2 ·6H 2 O.

[0035] (2) Introduce the clear liquid into the secondary salt field, collect the precipitated crystal MgCl 2 ·6H 2 O, MgCl 2 ·6H 2 O is heated to 117°C for dehydration to obtain MgCl 2 4H 2 O, MgCl 2 4H 2 O is heated to 200°C for dehydration to obtain MgCl 2 2H 2 O.

[0036] (3) According to Mg 2+ Mg in the supernatant solution of salt and step (2) 2+ The molar ratio is 1:5 plus Mg 2+ Salt in secondary salt pans, Mg 2+ Salt contains all of the MgCl prepared in step (2) 2 2H 2 O, the clear liquid was sun-salted for 7 days, and the clear liquid and granular precipitated crystal MgCl were obtained again 2 ·6H 2 O.

...

Embodiment 3

[0039] (1) At room temperature, in the primary salt field of magnesium-lithium saturated brine with a magnesium-lithium ratio of 10:1, according to Mg 2+ Mg in salt and saturated brine 2+ Add Mg to the molar ratio of 1:10 2+ Salt, dry the salt in the salt field for 1 day to get clear liquid and granular precipitated crystal MgCl 2 ·6H 2 O.

[0040] (2) Introduce the clear liquid into the secondary salt field, collect the precipitated crystal MgCl 2 ·6H 2 O, MgCl 2 ·6H 2 O is heated to 96°C and dehydrated to obtain MgCl 2 4H 2 O, MgCl 2 4H 2 O is heated to 135°C for dehydration to obtain MgCl 2 2H 2 O.

[0041] (3) According to Mg 2+ Mg in the supernatant solution of salt and step (2) 2+ The molar ratio is 1:10 plus Mg 2+ Salt in secondary salt pans, where Mg 2+ Salt contains all of the MgCl prepared in step (2) 2 2H 2 O, the clear liquid is salted for 1 day, and the clear liquid and granular precipitated crystal MgCl are obtained again 2 ·6H 2 O.

[0042]...

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Abstract

The invention relates to a method for reducing the ratio of magnesium to lithium in a salt lake through solar-assisted salt crystallization. The method comprises the following steps: (1) adding a Mg<2+> salt at a molar ratio of the added Mg<2+> salt to Mg<2+> in saturated brine at (1:5)-(1:10) to the saturated brine which has a molar ratio of magnesium to lithium at (200:1)-(10:1), and drying thesaturated brine in the sun for 1-7 days so as to obtain a clear liquid and a granular precipitated crystal MgCl2.6H2O; (2) heating the precipitated crystal MgCl2.6H2O so as to obtain MgCl2.4H2O, MgCl2.2H2O or MgCl2; (3) adding a Mg<2+> salt to the clear liquid at a molar ratio of the added Mg<2+> salt to Mg<2+> in the clear liquid in the step (1) at (1:5)-(1:10), wherein the added Mg<2+> salt comprises MgCl2.4H2O, MgCl2.2H2O or MgCl2 obtained in the step (2); and drying the clear liquid in the sun for 1-7 days so as to obtain a clear solution and a granular precipitated crystal MgCl2.6H2O again; and (4), repeating the steps of (2) and (3), and repeating the cycle 2-8 times. According to the method, the products are generated through cyclic induction of the products, the entire salt dryingcycle is shortened, the production process is simple, less equipment investment is required, and no contaminants is introduced in the production process.

Description

technical field [0001] The invention belongs to the technical field of extracting lithium from salt lake sun-dried salt, and in particular relates to a method for assisting crystallized sun-dried salt to reduce the ratio of magnesium to lithium in a salt lake. Background technique [0002] A salt lake is a saline water body, usually referring to the salinity w(NaCl eq )>3.5% (greater than the average salinity of seawater), including dry brine lakes with dried-up surface brine and composed of saline deposits and intergranular brine. The brine contains a large amount of sodium, potassium, magnesium, lithium, chlorine, and sulfur It is one of the important raw materials for extracting lithium at present. [0003] There are many salt lakes in my country. Among them, the Qinghai salt lake area is the lake area with the most abundant salt lake resources in my country. The drying conditions are good, but the magnesium-lithium ratio of the salt lake resources itself is very high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/30C01D15/08C01D3/06
CPCC01F5/30C01D15/08C01D3/06
Inventor 张勇吴云陈杰罗喆陈喆吴江渝
Owner WUHAN INSTITUTE OF TECHNOLOGY
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