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Method for efficiently extracting lithium from lithium-rich aluminum electrolyte waste residues and preparing anhydrous aluminum fluoride

A technology of aluminum electrolyte and water aluminum fluoride, applied in aluminum fluoride, chemical instruments and methods, aluminum halide, etc., can solve the problem of ineffective utilization and other problems, and achieve the effect of thorough removal, efficient recovery and high purity

Active Publication Date: 2021-11-30
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic and foreign reports can be used to produce aluminophosphate cement, but the valuable elements lithium, fluorine, and aluminum cannot be efficiently utilized

Method used

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  • Method for efficiently extracting lithium from lithium-rich aluminum electrolyte waste residues and preparing anhydrous aluminum fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] Take 100g of lithium-rich aluminum electrolyte waste residue, 136.23g of 98% concentrated sulfuric acid, mix and mature for 10min, and then heat at 275°C for 1.5h to obtain defluorinated material and hydrogen fluoride gas. The fluorine removal rate is 99.51%.

[0086] Mix the obtained defluorinated material with water, the ratio of defluorinated material to water is 1g:5mL, then stir at 80°C at 500rpm for 2h; after stirring, filter and separate to obtain primary filtrate and primary filter residue, Li, Na , the leaching rate of K is greater than 99.50%, the leaching rate of Al is 98.46%, and the leaching residue is mainly C, SiO 2 , CaSO 4 .

[0087] Prepare the extraction phase, the extraction agent is diethylhexyl phosphate, the diluent is sulfonated kerosene, the volume ratio of the extraction agent and the extraction phase is 0.2; the primary filtrate and the extraction phase are mixed according to the volume of 1:1, and the pH value is adjusted to 4.3 Carry out e...

Embodiment 2

[0095] Take 100g of lithium-rich aluminum electrolyte waste residue, 142.71g of 98% concentrated sulfuric acid, mix and mature for 30min, and then heat at 250°C for 2h to obtain defluorinated material and hydrogen fluoride gas. The fluorine removal rate is 99.23%.

[0096] Mix the obtained defluorinated material with water, the ratio of defluorinated material to water is 1g:7mL, then stir at 60°C at 450rpm for 3h; after stirring, filter and separate to obtain primary filtrate and primary filter residue, Li, Na , the leaching rate of K is greater than 99.12%, the leaching rate of Al is 98.18%, and the leaching residue is mainly C, SiO 2 , CaSO 4 .

[0097] Prepare the extraction phase, the extraction agent is dioctylphenyl phosphate, the diluent is sulfonated kerosene, the volume ratio of the extraction agent and the extraction phase is 0.25; the primary filtrate and the extraction phase are mixed according to the volume of 2:1, and the pH value is adjusted Extraction was car...

Embodiment 3

[0104] Take 100g of lithium-rich aluminum electrolyte waste residue, 149.2g of 98% concentrated sulfuric acid, mix and mature for 60min, and then heat at 200°C for 3h to obtain defluorinated material and hydrogen fluoride gas. The fluorine removal rate is 99.83%.

[0105] Mix the obtained defluorinated material with water, the ratio of defluorinated material to water is 1g:9mL, then stir at 80°C at 550rpm for 4h; after stirring, filter and separate to obtain the primary filtrate and primary filter residue, Li, Na , the leaching rate of K is greater than 99.75%, the leaching rate of Al is 99.31%, and the leaching residue is mainly C, SiO 2 , CaSO 4 .

[0106] Prepare the extraction phase, the extraction agent is diethylhexyl phosphate, the diluent is sulfonated kerosene, the volume ratio of the extraction agent and the extraction phase is 0.3; the primary filtrate and the extraction phase are mixed according to the volume of 3:1, and the pH value is adjusted to 3.2 Carry out ...

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Abstract

The invention belongs to the technical field of nonferrous metal extraction. The invention provides a method for efficiently extracting lithium from lithium-rich aluminum electrolyte waste residues and preparing anhydrous aluminum fluoride. According to the method, HF gas generated by curing and volatilizing concentrated sulfuric acid is subjected to dust removal and impurity removal and then directly makes contact with an aluminum-loaded organic phase to prepare anhydrous AlF3, the purity of the synthesized anhydrous AlF3 is high, the prepared anhydrous AlF3 can be returned to the aluminum electrolysis process to serve as a cosolvent, and cyclic utilization of aluminum and fluorine is achieved. According to the method, the lithium resource in the lithium-rich aluminum electrolyte waste residues is recycled in the form of Li2CO3, the recycling rate is high, the product purity is high, and high economic benefits are achieved. According to the method, sodium dimethyl dithiocarbamate solution is used as a precipitator to deeply purify and remove calcium, magnesium and aluminum, the impurity element removal effect is thorough, and raw materials are prepared for the step of precipitating lithium in sodium carbonate. In the treatment process of the lithium-rich aluminum electrolyte waste residues, various components can be efficiently recycled, and new pollution is not generated while waste materials are fully recycled.

Description

technical field [0001] The invention relates to the technical field of extraction of nonferrous metals, in particular to a method for efficiently extracting lithium and preparing anhydrous aluminum fluoride from lithium-rich aluminum electrolyte waste residue. Background technique [0002] The proven reserves of lithium resources in the world are 21 million tons. At present, the raw materials for extracting lithium resources at home and abroad mainly come from salt lake brine and spodumene. The high Li content in alumina leads to long-term accumulation of Li in the electrolyte of aluminum electrolytic cells using this type of alumina raw material, and its concentration can reach 1.0-2.7% (based on Li + ), resulting in a decrease in the dissolving capacity of alumina in the electrolytic cell, a decrease in current efficiency, and an increase in energy consumption. At the same time, compared with traditional lithium ore resources (Li in lepidolite 2 O 3.2%–6.45%), aluminum e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B21/00C22B26/12C22B3/38C01F7/50C01D15/08C01B25/30C01D5/00
CPCC22B7/007C22B26/12C22B21/0023C01F7/50C01D15/08C01B25/308C01D5/00C01P2006/82Y02P10/20
Inventor 赖延清李帅杨声海陈永明田忠良金胜明莫才宣
Owner CENT SOUTH UNIV
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