Method for recovering lithium and potassium from high-lithium-potassium anode carbon slag or high-lithium-potassium electrolyte

A technology of potassium electrolyte and anode carbon, which is applied in the field of lithium and potassium recovery, can solve the problem that there is not much research on recovering and extracting lithium and potassium, and achieves the effects of good economic benefits, easy operation and high product purity

Active Publication Date: 2021-12-21
SHENYANG BEIYE METALLURGIGAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although the lithium and potassium contained in the high-lithium and high-potassium electrolyte of aluminum electrolysis are as high as 7-10% or even higher, there are not many studies on the recovery and extraction of lithium and potassium from high-lithium and high-potassium electrolytes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Grind the high-lithium potassium electrolyte to a particle size of -0.075mm as the raw material, then mix the raw material with the concentrated sulfuric acid solution in the reactor, and heat it to 380°C for reaction; the mass concentration of the concentrated sulfuric acid solution is 98%, and the concentration of the concentrated sulfuric acid solution Dosage according to H 2 SO 4 With LiF, KF, CaF 2 React with part of NaF to generate Li 2 SO 4 、K 2 SO 4 , CaSO4 and Na 2 SO 4 On the basis of 8% excess by mass percentage; the amount of the part of NaF The calculation formula is W=a-0.83bx;

[0035] In the formula: a is the total mass of NaF in the high lithium potassium electrolyte; x is the AlF in the high lithium potassium electrolyte 3 The total mass of b, the value of b is 0.3; the HF generated by the reaction and the unreacted H 2 SO 4 Exhausted from the reactor in gaseous form;

[0036] Take out the reacted material, add water to leaching to make Na...

Embodiment 2

[0044] Method is the same as embodiment 1, the difference is

[0045] (1) Grinding high-lithium-potassium anode carbon slag (anode carbon slag containing high-lithium-potassium electrolyte) as a raw material, mixing the raw material with concentrated sulfuric acid solution and heating to 450°C for reaction; the excess of concentrated sulfuric acid solution is 6%; the value of b is 0.35 ;

[0046] (2) When adding water for leaching, the amount of water added is based on the amount of Na in the filtrate 2 SO 4 The mass concentration is 25%; the main component of primary slag is Na 5 al 3 f 14 , AlF 3 , CaSO 4 , C and Al 2 o 3 ; The primary slag is heated to 1050°C to make Na 5 al 3 f 14 and AlF 3 evaporative separation;

[0047] (3) NaOH solution is added to the primary filtrate to adjust the pH value=7.5, and the mass concentration of NaOH solution is 30%;

[0048] (4) The secondary filtrate is cooled to -9°C, Na 2 SO 4 Take Na 2 SO 4 10H 2 Precipitation of O...

Embodiment 3

[0052] Method is the same as embodiment 1, the difference is

[0053] (1) The raw material is mixed with the concentrated sulfuric acid solution and heated to 280°C for reaction; the concentrated sulfuric acid solution is over 10%; the value of b is 0.35;

[0054] (2) When adding water for leaching, the amount of water added is based on the amount of Na in the filtrate 2 SO 4 The mass concentration is 15%; the primary slag is heated to 1000°C to make Na 5 Al 3 f 14 and AlF 3 evaporative separation;

[0055] (3) NaOH solution is added to the primary filtrate to adjust the pH value=7, and the mass concentration of NaOH solution is 30%;

[0056] (4) The secondary filtrate is cooled to -8°C, Na 2 SO 4 Take Na 2 SO 4 10H 2 Precipitation of O form; separation by filtration at -8°C;

[0057] (5) Heating the filtrate three times to 98°C and adding Na 2 CO 3 ; Filtrate and separate the precipitated lithium carbonate at a temperature of 98°C; add Na 2 CO 3 is based on Na...

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Abstract

The method for reclaiming lithium and potassium from high-lithium-potassium anode carbon slag or high-lithium-potassium electrolyte is carried out in the following steps: (1) grinding high-lithium-potassium anode carbon slag or high-lithium-potassium electrolyte as raw material and mixing with concentrated sulfuric acid solution Heating to 280-500°C for reaction; (2) add water to leach the reacted material, filter and separate the primary filtrate; (3) adjust the pH value to 6-8 when the temperature of the primary filtrate is ≤30°C, and obtain the secondary filtrate by filtering and separating (4) cooled to -5~-10°C, Na 2 SO 4 Precipitate; filter and separate the filtrate three times; (5) add Na after heating to 90-100°C or boiling 2 CO 3 , Li 2 CO 3 Precipitated and separated Li by filtration 2 CO 3 and four times of filtrate; (6) four times of filtrate is cooled to -5~-10°C, Na 2 SO 4 Precipitate; filter and separate K 2 SO 4 solution, concentrated or dehydrated to obtain K 2 SO 4 ·xH 2 O or K 2 SO 4 product. The process flow of the method of the invention has low cost, is easy to operate, hardly produces new pollution while fully recovering waste materials, and has good promotion prospects.

Description

technical field [0001] The invention relates to the technical field of aluminum electrolysis and waste recycling, in particular to a method for recovering lithium and potassium from high-lithium-potassium anode carbon slag or high-lithium-potassium electrolyte. Background technique [0002] In the process of industrial aluminum electrolysis production, Al 2 o 3 It is the raw material for aluminum electrolysis. The electrolytic cell uses a carbon anode made of petroleum coke. In the aluminum electrolytic cell, aluminum electrolysis Al 2 o 3 The chemical reaction for producing metal aluminum is: [0003] 2Al 2 o 3 +3C→4Al+3CO 2 . [0004] In the aluminum electrolytic production process, when the raw material Al used 2 o 3 Contains CaO, when Al is produced, these impurities are transformed into CaF2 and enter the electrolyte; therefore, the CaF in the electrolyte 2 It is usually not artificially added; in my country, some electrolytic aluminum plants also use Li 2 O ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B7/04C22B26/10C22B26/12
CPCC22B7/04C22B7/006C22B26/12C22B26/10Y02P10/20
Inventor 冯乃祥杨超
Owner SHENYANG BEIYE METALLURGIGAL TECH CO LTD
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