CN113104897A - Method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder - Google Patents
Method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder Download PDFInfo
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Abstract
The invention relates to a method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder, which comprises the following steps: 1) pulping battery black powder, adding concentrated sulfuric acid to carry out first-stage agitation leaching, controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃, and adding a reducing agent; 2) performing filter pressing on the first-stage leachate, adjusting the pH value of the filtrate to remove iron and aluminum, and performing extraction treatment to separate manganese, cobalt, nickel and lithium; the filter residue is used as a raw material for the second-stage leaching; 3) carrying out second-stage reduction leaching on filter residue produced by first-stage filter pressing, adding a reducing agent, and controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃; 4) carrying out filter pressing on the leaching solution, and washing filter residues to obtain graphite residues; 5) adding barium sulfide into the filtrate of the second-stage pressure filtration, controlling the temperature to be 55-70 ℃, the pH value to be 3.5-4.5, and reacting for 1-3 hours; 6) carrying out filter pressing on the solution after nickel and cobalt removal, wherein the filtrate is a manganese sulfate solution; 7) and adding sodium ferbamate and sodium fluoride into the manganese sulfate solution, and performing filter pressing to obtain a solution, namely the battery-grade manganese sulfate solution.
Description
Technical Field
The invention belongs to the technical field of waste lithium battery recovery and treatment, and particularly relates to a method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder.
Background
China is the biggest world for producing lithium ion batteries, and the lithium ion battery industry has become one of high and new technology industries which are mainly supported by the country. The high-manganese ternary lithium ion battery is applied to two-wheel and three-wheel electric vehicles in large quantity, so that the scrapped quantity is more considerable. The treatment of waste products and production waste materials in the lithium ion battery industry becomes a difficult problem which is urgently needed to be solved in the clean production of the lithium ion battery industry. The waste lithium ion battery belongs to typical solid waste, and the resource utilization of the waste lithium ion battery not only can solve the environmental problem caused by the waste lithium ion battery, but also can relieve the situation of strategic metal resource shortage in China and promote the sustainable development of the battery industry in China.
At present, the recovery method of the anode material of the waste lithium ion battery mainly adopts a hydrometallurgical process of sulfuric acid leaching, and the basic process is as follows: the method comprises the steps of leaching metal elements in the waste lithium ion positive electrode material at one time by using sulfuric acid, separating by hydrometallurgy, recycling in the form of nickel, cobalt and manganese salts, enriching the lithium elements into raffinate, removing oil and impurities from the raffinate, and precipitating lithium ions in solution by using sodium carbonate to form lithium carbonate precipitate. Because a large amount of reducing agents are added in the sulfuric acid leaching process, metals such as aluminum, copper, iron, nickel, cobalt, manganese and the like in the anode material are synchronously leached, and then the metals such as nickel, cobalt, manganese and the like are separated and recovered by an extraction method. This aspect consumes large amounts of reducing agent; on the other hand, a large amount of manganese is separated from nickel and cobalt by an extraction method, the production cost is high, and the production processing capacity of an extraction line is greatly weakened.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention aims to provide a method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder, and aims to solve the problems of poor economy, small processing capacity, high production cost and the like in the existing high-manganese ternary black powder processing technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder comprises the following steps:
1) first-stage leaching: pulping the anode powder and the cathode powder of the waste high-manganese ternary lithium ion battery, adding concentrated sulfuric acid to carry out primary stirring leaching, controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃, and adding a reducing agent;
2) first-stage filter pressing: filter-pressing the first-stage leachate, wherein the content of nickel and cobalt in the filtrate is high, the content of manganese is low, the leaching rate of lithium at the stage can reach more than 98%, and extracting and separating manganese, cobalt, nickel and lithium after removing iron and aluminum by adjusting the Ph value; the manganese content in the filter residue is higher and is used as a raw material for second-stage leaching; leaching most of nickel, cobalt and lithium into a solution through first-stage leaching and first-stage filter pressing treatment, controlling the leaching of manganese as little as possible, and enriching the manganese in slag;
3) secondary leaching: carrying out two-stage reduction leaching on filter residue produced by first-stage filter pressing, wherein the molar weight of the added reducing agent is 1.5-1.8 times of the manganese content in the filter residue, and controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃;
4) second-stage filter pressing: carrying out filter pressing on the leaching solution, and washing filter residues to obtain graphite residues; the filtrate contains a small amount of nickel and cobalt, and the manganese content is high;
5) precipitating nickel and cobalt: adding barium sulfide into the filtrate of the second-stage pressure filtration, controlling the temperature to be 55-70 ℃, the pH value to be 3.5-4.5, and reacting for 1-3 hours;
6) and (3) filter pressing: carrying out filter pressing on the solution after nickel and cobalt removal, wherein filter residues are nickel cobalt sulfide materials and can be used as raw materials for oxygen pressure leaching; the filtrate is manganese sulfate solution;
7) removing impurities: sodium ferbamate and sodium fluoride are added into the manganese sulfate solution to remove trace heavy metals and metal calcium and magnesium ions, and the solution obtained through filter pressing is the battery-grade manganese sulfate solution.
Preferably, in step 1), the reducing agent is added in a molar amount of 0.8 to 1.2 times the cobalt content.
Preferably, in the step 1), the reducing agent is one or a mixture of more than two of hydrogen peroxide, sodium thiosulfate, sodium sulfite and sodium metabisulfite.
Preferably, the addition amount of barium sulfide in the step 5) is 1.1-1.4 times of the theoretical total amount of nickel, cobalt and copper.
The leaching process adopts a leaching mode combining primary leaching and secondary strong reduction leaching, the addition of a reducing agent is controlled in a sectional manner, so that nickel and cobalt are leached as far as possible to obtain a solution during primary leaching, manganese is leached as little as possible and is enriched in slag, the high manganese slag can also be sold as manganese-rich slag, the high nickel and cobalt solution produced by filter pressing can be merged into a high nickel and cobalt ternary black powder (such as 523, 622 and 811 black powder) leaching solution system, and the high nickel and cobalt solution is used as a raw material solution of an extraction line after the pH value is adjusted to remove impurities; and (3) carrying out secondary strong reduction leaching on filter residues obtained after the first-stage leaching and filter pressing, dissolving and leaching residual nickel, cobalt and most of manganese, wherein the leached residues can be sold as graphite materials, removing nickel, cobalt, copper and iron from the solution by barium sulfide, removing heavy metals by sodium ferometalate, and removing calcium and magnesium from manganese fluoride to prepare battery-grade manganese sulfate.
The beneficial technical effects are as follows:
according to the invention, high-manganese ternary black powder or positive and negative electrode black powder is subjected to selective leaching of first-stage leaching and second-stage complete leaching to realize separation of most manganese from nickel, cobalt and lithium, so that the problems of high extraction production cost, overlarge production load of a manganese extraction stage and the like caused by extraction procedures of one-time complete leaching of the high-manganese ternary powder are solved; the recovery rate of the lithium element in the whole process is not influenced, the consumption of acid and alkali in the high manganese nickel cobalt solution extraction process is greatly reduced, and the production efficiency of the extraction process is improved.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Example 1
A method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder comprises the following steps: 1) pulping the anode and cathode powder of the waste high-manganese ternary lithium ion battery, adding concentrated sulfuric acid to carry out first-stage stirring leaching, controlling the pH value to be 1.4 and the temperature to be 85 ℃, and adding hydrogen peroxide according to the molar weight of 0.8 time of the cobalt content in the process; filter-pressing the leachate, wherein the content of nickel and cobalt in the filtrate is high, the content of manganese is low, the leaching rate of lithium at the stage can reach more than 98%, and the leachate enters an extraction production line for extraction treatment after iron and aluminum are removed by adjusting the pH value to separate manganese, cobalt, nickel and lithium; the filter residue is used as a raw material for the second-stage leaching; carrying out two-stage reduction leaching on the filter residue produced in the first stage, wherein the molar weight of the hydrogen peroxide added at this time is 1.5 times of the manganese content in the residue, and the pH value is controlled to be less than 1.5 in the process and the temperature is 85-95 ℃; carrying out filter pressing on the leaching solution, and washing filter residues to obtain graphite residues; the filtrate contains a small amount of nickel and cobalt, and the manganese content is high; adding barium sulfide into the filtrate, controlling the temperature to be 55-70 ℃, the pH value to be 3.5, reacting for 1 hour, and simultaneously controlling the addition of the barium sulfide to be 1.1 times of the total amount of theoretical nickel, cobalt and copper; carrying out filter pressing on the solution after nickel and cobalt removal, wherein filter residues are nickel cobalt sulfide materials and can be used as raw materials for oxygen pressure leaching; the filtrate is manganese sulfate solution; and adding sodium ferbamate and sodium fluoride into the manganese sulfate solution to remove trace heavy metals, metal calcium and magnesium ions respectively, and performing filter pressing to obtain a solution, namely the battery-grade manganese sulfate solution. The extraction production line is not described in detail in the present application as the prior art in the field, and the technical scheme thereof is not an innovative point in the present application.
Example 2
A method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder comprises the following steps: 1) pulping the anode and cathode powder of the waste high-manganese ternary lithium ion battery, adding concentrated sulfuric acid to carry out first-stage stirring leaching, controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃, and adding sodium sulfite according to the molar weight 1.2 times of the cobalt content in the process; filter-pressing the leachate, wherein the leachate has high nickel and cobalt contents and low manganese contents, the leaching rate of lithium at the stage can reach more than 98%, and the leachate enters an extraction production line for extraction treatment after iron and aluminum are removed by adjusting the pH value to separate manganese, cobalt, nickel and lithium; the filter residue is used as a raw material for the second-stage leaching; carrying out two-stage reduction leaching on the filter residue produced in the first stage, wherein the molar weight of the reducing agent added at this time is 1.8 times of the manganese content in the residue, and the pH value is controlled to be less than 1.5 in the process, and the temperature is 85-95 ℃; carrying out filter pressing on the leaching solution, and washing filter residues to obtain graphite residues; the filtrate contains a small amount of nickel and cobalt, and the manganese content is high; adding barium sulfide into the filtrate, controlling the temperature to be 55-70 ℃, the pH value to be 4.5, reacting for 3 hours, and simultaneously controlling the addition of the barium sulfide to be 1.4 times of the theoretical total amount of nickel, cobalt and copper; carrying out filter pressing on the solution after nickel and cobalt removal, wherein filter residues are nickel cobalt sulfide materials and can be used as raw materials for oxygen pressure leaching; the filtrate is manganese sulfate solution; and adding sodium ferbamate and sodium fluoride into the manganese sulfate solution to remove trace heavy metals, metal calcium and magnesium ions respectively, and performing filter pressing to obtain a solution, namely the battery-grade manganese sulfate solution.
Example 3
A method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder comprises the following steps: 1) pulping the anode and cathode powder of the waste high-manganese ternary lithium ion battery, adding concentrated sulfuric acid to carry out first-stage stirring leaching, controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃, and adding sodium thiosulfate according to the molar weight 0.8-1.2 times of the cobalt content in the process; filter-pressing the leachate, wherein the leachate has high nickel and cobalt contents and low manganese contents, the leaching rate of lithium at the stage can reach more than 98%, and the leachate enters an extraction production line for extraction treatment after iron and aluminum are removed by adjusting the pH value to separate manganese, cobalt, nickel and lithium; the filter residue is used as a raw material for the second-stage leaching; carrying out two-stage reduction leaching on the filter residue produced in the first stage, wherein the molar weight of the added reducing agent is 1.5 times of the manganese content in the residue, the pH value is controlled to be less than 1.5 in the process, and the temperature is 85-95 ℃; carrying out filter pressing on the leaching solution, and washing filter residues to obtain graphite residues; the filtrate contains a small amount of nickel and cobalt, and the manganese content is high; adding barium sulfide into the filtrate, controlling the temperature to be 55-70 ℃, the pH value to be 3.5-4.5, reacting for 1-3 hours, and simultaneously controlling the adding amount of the barium sulfide to be 1.4 times of the theoretical total amount of nickel, cobalt and copper; carrying out filter pressing on the solution after nickel and cobalt removal, wherein filter residues are nickel cobalt sulfide materials and can be used as raw materials for oxygen pressure leaching; the filtrate is manganese sulfate solution; and adding sodium ferbamate and sodium fluoride into the manganese sulfate solution to remove trace heavy metals, metal calcium and magnesium ions respectively, and performing filter pressing to obtain a solution, namely the battery-grade manganese sulfate solution.
Example 4
A method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder comprises the following steps: 1) pulping the anode and cathode powder of the waste high-manganese ternary lithium ion battery, adding concentrated sulfuric acid to carry out first-stage stirring leaching, controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃, and adding sodium pyrosulfite according to the molar weight 0.8-1.2 times of the cobalt content in the process; filter-pressing the leachate, wherein the leachate has high nickel and cobalt contents and low manganese contents, the leaching rate of lithium at the stage can reach more than 98%, and the leachate enters an extraction production line for extraction treatment after iron and aluminum are removed by adjusting the pH value to separate manganese, cobalt, nickel and lithium; the filter residue is used as a raw material for the second-stage leaching; carrying out second-stage reduction leaching on the filter residue produced in the first stage, wherein the molar weight of the added reducing agent is 1.8 times of the manganese content in the residue, the pH value is controlled to be less than 1.5 in the process, and the temperature is 85-95 ℃; carrying out filter pressing on the leaching solution, and washing filter residues to obtain graphite residues; the filtrate contains a small amount of nickel and cobalt, and the manganese content is high; adding barium sulfide into the filtrate, controlling the temperature to be 55-70 ℃, the pH value to be 3.5-4.5, reacting for 1-3 hours, and simultaneously controlling the adding amount of the barium sulfide to be 1.1 times of the theoretical total amount of nickel, cobalt and copper; carrying out filter pressing on the solution after nickel and cobalt removal, wherein filter residues are nickel cobalt sulfide materials and can be used as raw materials for oxygen pressure leaching; the filtrate is manganese sulfate solution; and adding sodium ferbamate and sodium fluoride into the manganese sulfate solution to remove trace heavy metals, metal calcium and magnesium ions respectively, and performing filter pressing to obtain a solution, namely the battery-grade manganese sulfate solution.
Claims (5)
1. A method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder is characterized by comprising the following steps:
1) first-stage leaching: pulping the anode powder and the cathode powder of the waste high-manganese ternary lithium ion battery, adding concentrated sulfuric acid to carry out primary stirring leaching, controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃, and adding a reducing agent;
2) first-stage filter pressing: performing filter pressing on the first-stage leachate, adjusting the pH value of the filtrate to remove iron and aluminum, and performing extraction treatment to separate manganese, cobalt, nickel and lithium; the filter residue is used as a raw material for the second-stage leaching;
3) secondary leaching: carrying out second-stage reduction leaching on filter residue produced by first-stage filter pressing, adding a reducing agent, and controlling the pH value to be less than 1.5 and the temperature to be 85-95 ℃;
4) second-stage filter pressing: carrying out filter pressing on the leaching solution, and washing filter residues to obtain graphite residues;
5) precipitating nickel and cobalt: adding barium sulfide into the filtrate of the second-stage pressure filtration, controlling the temperature to be 55-70 ℃, the pH value to be 3.5-4.5, and reacting for 1-3 hours;
6) and (3) filter pressing: carrying out filter pressing on the solution after nickel and cobalt removal, wherein filter residues are nickel cobalt sulfide materials; the filtrate is manganese sulfate solution;
7) removing impurities: and (2) adding sodium ferometalate and sodium fluoride into the manganese sulfate solution to remove trace heavy metals and metal calcium and magnesium ions, and performing filter pressing to obtain a solution, namely the battery-grade manganese sulfate solution.
2. The method for selectively leaching and sectionally separating nickel, cobalt and manganese from the black powder of the high-manganese battery as recited in claim 1, wherein in the step 1), a reducing agent is added according to a molar amount of 0.8-1.2 times of the cobalt content.
3. The method for selectively leaching and sectionally separating nickel, cobalt and manganese from the black powder of the high-manganese battery as claimed in claim 1, wherein in the step 3), the molar amount of the reducing agent added is 1.5-1.8 times of the manganese content in the filter residue.
4. The method for selectively leaching and sectionally separating nickel, cobalt and manganese from the black powder of the high-manganese battery as claimed in claim 1, wherein in the step 1) and the step 3), the reducing agent is one or a mixture of more than two of hydrogen peroxide, sodium thiosulfate, sodium sulfite and sodium metabisulfite.
5. The method for selectively leaching and sectionally separating nickel cobalt and manganese from the black powder of the high-manganese battery according to claim 1, characterized in that: the addition amount of barium sulfide in the step 5) is 1.1-1.4 times of the theoretical total amount of nickel, cobalt and copper.
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| CN113684381A (en) * | 2021-08-27 | 2021-11-23 | 昆明理工大学 | Method for preparing high-purity manganese sulfate by microwave-flow field coupling strengthening treatment of pyrolusite |
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