Method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium

A lithium carbonate, brine technology, applied in separation methods, chemical instruments and methods, lithium carbonate;/acid carbonate, etc., can solve problems such as limitations, no breakthrough changes in solvent extraction technology, etc. Enhanced extraction ability, improved lithium-magnesium separation ability, and high metal ion extraction rate

Active Publication Date: 2015-12-16
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current solvent extraction method is limited to the liquid-liquid extraction

Method used

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  • Method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium
  • Method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium
  • Method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Li in the old brine of a salt lake in Qaidam Basin, Qinghai + , Mg 2+ and The contents are 2.24, 118.00 and 39.87g / L respectively, and the mass ratio of magnesium to lithium is equal to 52.58. Take 350mL of the old brine in a 1000mL beaker, heat and concentrate it on a temperature-adjusting electric furnace, and evaporate the water accounting for 25% of the total mass of the old brine. After cooling, all the liquid will be precipitated and transformed into a brine salt containing crystal water. Transfer to a mechanically stirred container, add 354.5mL trihexyl phosphate to it, the solid-liquid mass volume ratio is equal to 1:1 (g / mL), and carry out solid-liquid extraction at room temperature for 30min. Subsequently, the solid-liquid mixture was moved into a sand core funnel for suction filtration under reduced pressure to obtain the organic extract phase of the filtrate and the remaining halogen salt. Heat the remaining brine salt until it is completely dissolved, a...

Embodiment 2

[0036] Get 350mL of the old brine from the salt lake in Example 1 in a 1000mL beaker, and add therein the LiCl H with an analytically pure content of 97%. 2 O11.49g, the mass ratio of magnesium to lithium in the mixture is equal to 20.00. Heating and concentrating on a temperature-adjusting electric furnace evaporates 25% of the water that accounts for the total mass of the initial old brine, and after cooling, all the liquid is precipitated and transformed into a brine salt containing crystal water. Transfer to a mechanically stirred container, add 366.8mL trihexyl phosphate to it, the solid-liquid mass volume ratio is equal to 1:1 (g / mL), and carry out solid-liquid extraction at room temperature for 30min. Subsequently, the solid-liquid mixture was moved into a sand core funnel for suction filtration under reduced pressure to obtain the organic extract phase of the filtrate and the remaining halogen salt. Heat the remaining brine salt until it is completely dissolved, and t...

Embodiment 3

[0042] Take 350 mL of the old brine from the salt lake in Example 1 in a 1000 mL beaker, and the mass ratio of magnesium to lithium is equal to 52.58. Heating and concentrating on a temperature-adjusting electric furnace evaporates the water accounting for 25% of the total mass of the old brine, and after cooling, all the liquid is precipitated and transformed into a brine salt containing crystal water. Transfer to a mechanically stirred container, add 354.7mL tributyl phosphate to it, the solid-liquid mass volume ratio is equal to 1:1 (g / mL), and carry out solid-liquid extraction at room temperature for 30min. Subsequently, the solid-liquid mixture was moved into a sand core funnel for suction filtration under reduced pressure to obtain the organic extract phase of the filtrate and the remaining halogen salt. Heat the remaining brine salt until it is completely dissolved, and then cool it to precipitate out, and obtain the brine salt containing crystal water for the second ti...

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Abstract

The invention discloses a method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium. The method includes the steps of converting salt lake bittern serving as raw materials into halide salt through evaporation dehydration and crystallization separation, directly extracting halide salt through trixylyl phosphate alkane ester or a mixture of trixylyl phosphate alkane ester and monohydric alcohol, obtaining an organic extraction phase and the rest of halide salt after solid-liquid separation, conducting back extraction on the organic extraction phase through water to obtain a low-magnesium-lithium-ratio lithium-rich solution, and obtaining lithium carbonate through condensation and alkalization magnesium removal. The method has the advantages that processes related to the solid-liquid extraction method are simple, co-extraction agents are not needed, the solute distribution drive force is large, and the method is not influenced by bittern extractant two-phase balance; multiple stages of extraction processes are conducted on halide salt, the extraction rate of Li+ is larger than 90%, and the mass ratio of magnesium to lithium in the extraction phase is remarkably decreased; phase splitting is easy due to liquid-liquid back extraction, and the back extraction rates of Li+ and Mg2+ are both larger than 90%; the extraction process is operated under the neutral or weak-acid condition, the production cost is low, and the method is particularly suitable for producing lithium carbonate after separating magnesium out of bittern with the magnesium-lithium mass ratio of 120 or lower.

Description

technical field [0001] The invention belongs to the field of inorganic chemical industry and relates to a core technology for extracting lithium from salt lake brine, in particular to an important method for separating magnesium from brine with a high magnesium-to-lithium ratio and enriching lithium to produce lithium carbonate. Background technique [0002] Lithium resources in nature mainly exist in the form of spodumene, lepidolite and petalite and other pegmatite deposits and salt lake liquid and solid deposits. The production cost of extracting lithium from rock minerals is high. Since the 1990s, it has been gradually replaced by the process of extracting lithium from salt lake brine. In the "Lithium Triangle" at the junction of Chile, Argentina, and Bolivia, Mg in the brines of Atacama Salt Lake, Homebreto Salt Lake and Uyuni Salt Lake 2+ With low content, it is a high-quality resource with a low magnesium-lithium ratio, and the production process is economical and si...

Claims

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Application Information

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IPC IPC(8): C01D15/08
CPCC01D15/08B01D11/04B01D12/00C01F5/22C01F5/24C07B63/00C07F9/11
Inventor 杨立新王益付蜜齐红玉徐俞刘亚丽桂亚林何靖
Owner GUANGZHOU TINCI MATERIALS TECH
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