Method for recovering lithium and potassium from high-lithium-potassium anode carbon residues or high-lithium-potassium electrolytes

A potassium electrolyte and anode carbon technology, which is applied in the field of lithium and potassium recovery, can solve the problems of limited research on the recovery and extraction of lithium and potassium, and achieve good economic benefits, high product purity, and easy operation

Active Publication Date: 2020-06-23
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 content in high-lithium and high-potassium electrolytes for aluminum electrolysis is 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 , the excess of 8% by mass percentage; the calculation formula of the amount of the part of NaF is = 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 ...

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 ; Filtration and separation of precipitated lithium carbonate at a temperature of 98°C; adding Na 2 CO 3 is based...

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Abstract

The invention discloses a method for recovering lithium and potassium from high-lithium-potassium anode carbon residues or high-lithium-potassium electrolytes. The method comprises the following stepsthat (1) the high-lithium-potassium anode carbon residues or the high-lithium-potassium electrolytes are finely ground as raw materials, mixed with a concentrated sulfuric acid solution, and heated to 280-500 DEG C for reacting; (2) water is added into the reacted materials for leaching, and primary filtrate is filtered and separated out; (3) the pH value is adjusted to be equal to 6-8 when the temperature of the primary filtrate is less than or equal to 30 DEG C, and secondary filtrate is obtained through filtering and separating; (4) the secondary filtrate is cooled to minus 5 DEG C to-minus 10 DEG C, and Na2SO4 is separated out; third filtrate is filtered and separated out; (5) after the third filtrate is heated to 90-100 DEG C or boiled, Na2CO3 is added and Li2CO3 is precipitated andseparated out, and the Li2CO3 and fourth filtrate are filtered and separated out; and (6) the fourth filtrate is cooled to minus 5 DEG C to-minus 10 DEG C, and Na2SO4 is precipitated out, a K2SO4 solution is filtered to separated out, and a K2SO4.xH2O product or a K2SO4 product is obtained by concentrating or dehydrating. The method is low in process flow cost and convenient to operate, almost does not generate new pollution while the waste is fully recovered, and has a good popularization prospect.

Description

technical field [0001] The technical field of aluminum electrolysis and waste recycling of the present invention, in particular relates to a method for reclaiming 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 electrolysis cell uses carbon anode made of petroleum coke. In the aluminum electrolysis 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...

Claims

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Application Information

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Patent Type & Authority Applications(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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