CN112645387A - Method for preparing battery-grade manganese dioxide by using anode slag - Google Patents
Method for preparing battery-grade manganese dioxide by using anode slag Download PDFInfo
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- CN112645387A CN112645387A CN202011542559.9A CN202011542559A CN112645387A CN 112645387 A CN112645387 A CN 112645387A CN 202011542559 A CN202011542559 A CN 202011542559A CN 112645387 A CN112645387 A CN 112645387A
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
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- C22B13/025—Recovery from waste materials
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Abstract
The invention discloses a method for preparing battery-grade manganese dioxide by using anode slag, which comprises the steps of introducing hydrogen prepared by decomposing ammonia, carrying out reduction reaction, reducing manganese dioxide in manganese slag into manganese monoxide, evaporating lead in the manganese slag into gas at high temperature, and recovering lead in the gas and manganese element in the reduced manganese slag; the method can effectively recover manganese and lead elements in the electrolytic manganese anode slag, effectively treat and recycle the anode slag, solve the problem of environmental pollution of the anode slag, realize the recovery of valuable resources and finally obtain the battery-grade manganese dioxide and lead concentrate sand products.
Description
Technical Field
The invention relates to a method for preparing battery-grade manganese dioxide by using anode slag.
Background
China is the biggest world manganese production, consumption and export, and accounts for more than 90% of the total global manganese production. The manganese slag of the wet manganese industry is a general name for leached manganese slag, manganese sulfide slag and anode slag. The manganese slag yield in China in 2019 is reported to exceed 2000 ten thousand tons.
When the metal manganese is electrolyzed to produce, in a diaphragm electrolytic cell, a manganese sulfate aqueous solution containing ammonium sulfate is taken as electrolyte, direct current is introduced, the metal manganese is deposited on a cathode, hydrogen is separated out, and other metal ions are also separated out in a trace amount at the cathode and mixed in a manganese sheet; oxygen is separated out on the anode, and a small amount of manganese dioxide sediment is formed, namely the anode slag. In industrial production, lead, antimony, tin, silver and other multi-element alloys are generally selected as anode materials, and stainless steel plates are selected as cathode materials. The anode slag generally contains about 40% of manganese which mainly exists in the form of manganese dioxide and 1.5% -6% of valuable metals such as lead and the like.
At present, most of domestic enterprises transport anode slag to a storage yard for damming and stacking, and not only seriously damage the ecological environment but also waste heavy metal elements in the anode slag under the effect of weathering leaching for a long time.
Disclosure of Invention
The invention aims to provide a method for preparing battery-grade manganese dioxide by using anode slag, which can effectively recover manganese and lead elements in electrolytic manganese anode slag to obtain battery-grade manganese dioxide and lead concentrate sand products.
The invention provides a method for preparing battery-grade manganese dioxide by using anode slag, which comprises the following steps:
(1) grinding the anode slag to obtain powder with preset fineness;
(2) adding the powder obtained in the step (1) into a reduction furnace, introducing hydrogen gas prepared by ammonia decomposition, carrying out reduction reaction, reducing manganese dioxide in manganese slag into manganese monoxide, evaporating lead in the manganese slag into gas at high temperature, and taking the residue in the reduction furnace as reduced manganese slag;
(3) cooling the gas obtained in the step (2) by water, and cooling lead steam in the gas into solid lead to obtain a lead concentrate product;
(4) adding the reduced manganese slag obtained in the step (2) into a dilute sulfuric acid solution for reaction to generate manganese sulfate mixed slurry;
(5) performing filter pressing on the manganese sulfate mixed slurry obtained in the step (4), wherein the obtained filter residue is leaching residue, and the filtrate is manganese sulfate solution;
(6) adding an oxidant into the manganese sulfate solution obtained in the step (5), performing oxidation iron removal, and filtering to obtain a pure manganese sulfate solution;
(7) adding sodium chlorate into the pure manganese sulfate solution obtained in the step (6), and carrying out solid-liquid separation after reaction to obtain a manganese dioxide primary product;
(8) sequentially carrying out multistage rinsing, neutralization and re-rinsing on the manganese dioxide primary product to obtain manganese dioxide slurry;
(9) carrying out solid-liquid separation on the manganese dioxide slurry in a filter press to obtain a manganese dioxide semi-finished product;
(10) and drying the semi-finished manganese dioxide product, controlling the drying temperature and time to enable the moisture content of the intermediate to reach the corresponding product standard, and cooling, mixing and packaging to obtain the battery-grade manganese dioxide product.
Preferably, in the step (1), the fineness of the powder with the predetermined fineness is-0.075 mm and accounts for more than 80%.
Preferably, in the step (2), the temperature of the reduction reaction is 700 ℃ to 1200 ℃.
More preferably, in the step (2), the temperature of the reduction reaction is 800 to 1000 ℃.
Preferably, in the step (5), the leached slag is subjected to harmless treatment and then is transported to a slag yard for storage.
Preferably, in the step (6), the oxidant is one or a combination of more of oxygen, hydrogen peroxide and manganese dioxide.
Preferably, in the step (6), the iron-removed slag obtained by filtering is calcined at low temperature to obtain the cement admixture which can be sold to cement factories.
More preferably, the low-temperature calcination temperature is 300 ℃ to 520 ℃.
In the step (7), sodium chlorate is added into the manganese sulfate solution, and the reaction synthesis process is as follows:
5MnSO4+2NaClO3+4H2O＝4MnO2+Na2SO4+4H2SO4+Cl2↑
the manganese dioxide generated by the reaction nucleates and grows on manganese dioxide seed crystals which are placed in a reactor in advance, and the apparent specific gravity and the crystal structure of a reaction product are regulated and controlled by controlling the temperature and the reaction speed, so that the optimal electrochemical activity is achieved.
Preferably, in the step (7), solid-liquid separation is carried out in a filter press, and the filtrate is recycled to the reaction synthesis process because the filtrate contains sulfuric acid and unreacted manganese sulfate.
In the step (8), the specific surface area of the manganese dioxide primary product is large, a large amount of acid and impurities can be adsorbed on the surfaces of microscopic particles of the manganese dioxide primary product, and multi-stage rinsing is required firstly.
Preferably, in the step (8), when the manganese dioxide primary product is rinsed in multiple stages until the pH value is greater than 3, adding a neutralizing agent for neutralization, and adjusting the pH value to 6-8.
More preferably, the neutralizing agent is one or two of sodium hydroxide and ammonium bicarbonate.
Preferably, in step (8), after neutralization, the manganese dioxide is rinsed again with purified water to remove residual neutralizing agent and other impurities.
Compared with the prior art, the invention has the beneficial technical effects that:
the invention provides a method for preparing battery-grade manganese dioxide by using anode slag, which can effectively recover manganese and lead elements in electrolytic manganese anode slag, effectively treat and recycle the anode slag, solve the problem of environmental pollution caused by the anode slag, realize the recovery of valuable resources and finally obtain battery-grade manganese dioxide and lead concentrate sand products.
Drawings
FIG. 1 is a process flow diagram of example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
In this example, unless otherwise specified, all reagents used were common commercial products or prepared by conventional means, and the equipment used was conventional in the art, and the following are some examples of the inventors in the experiment:
in the embodiment of the invention, the anode slag comprises the following main components in percentage by mass: mn (30-50%), Pb (1.5-6%), S (3-8%) and Fe (0.1-1%).
Example 1
The invention relates to a method for preparing battery-grade manganese dioxide by using anode slag, which comprises the following steps:
(1) feeding the anode slag into a flour mill for dry milling, and returning coarse materials to the flour mill for regrinding through a particle classifier to obtain powder with the fineness of-0.075 mm accounting for more than 80%;
(2) adding the powder obtained in the step (1) into a reduction furnace, controlling the temperature to be 1200 ℃, introducing hydrogen gas prepared by ammonia decomposition, carrying out reduction reaction, reducing manganese dioxide in manganese slag into manganese monoxide, and evaporating lead in the manganese slag into gas at high temperature to obtain reduced manganese slag;
(3) cooling the gas obtained in the step (2) by water, and cooling lead steam in the gas into solid lead to obtain a lead concentrate product;
(4) adding the reduced manganese slag into a dilute sulfuric acid solution for reaction to generate manganese sulfate mixed slurry;
(5) carrying out filter pressing on the manganese sulfate mixed slurry to obtain filter residues, namely leaching residues, wherein the filtrate is a manganese sulfate solution;
(6) adding hydrogen peroxide into a manganese sulfate solution, carrying out oxidation iron removal, filtering to obtain a pure manganese sulfate solution which can be directly used as an electrolytic manganese raw material, filtering to obtain iron-removed slag, and calcining at 300 ℃ to obtain a cement blending material;
(7) adding sodium chlorate into the pure manganese sulfate solution, carrying out solid-liquid separation after reaction to obtain a manganese dioxide primary product, wherein the reaction is as follows:
5MnSO4+2NaClO3+4H2O＝4MnO2+Na2SO4+4H2SO4+Cl2↑
the chemical manganese dioxide generated by the reaction nucleates and grows on manganese dioxide seed crystals which are placed in a reactor in advance, and the apparent specific gravity and the crystal structure of a reaction product are regulated and controlled by controlling the temperature and the reaction speed, so that the optimal electrochemical activity is achieved;
(8) sequentially carrying out multistage rinsing, neutralization and re-rinsing on the manganese dioxide primary product to obtain manganese dioxide slurry;
the specific surface area of the manganese dioxide primary product is large, a large amount of acid and impurities can be adsorbed on the surfaces of microscopic particles of the manganese dioxide primary product, and multi-stage rinsing is required firstly;
when the pH value is higher than 3 after rinsing, adding a neutralizing agent for neutralization, and adjusting the pH value to be about 7, wherein the neutralizing agent is ammonium bicarbonate;
after neutralization, rinsing again by using purified water to remove residual neutralizer and other impurities;
(9) carrying out solid-liquid separation on the manganese dioxide slurry in a filter press to obtain a manganese dioxide semi-finished product;
(10) and drying the semi-finished manganese dioxide product, controlling the drying temperature and time to enable the moisture content of the intermediate to reach the corresponding product standard, and cooling, mixing and packaging to obtain the battery-grade manganese dioxide product.
Example 2
The invention relates to a method for preparing battery-grade manganese dioxide by using anode slag, which comprises the following steps:
(1) feeding the anode slag into a flour mill for dry milling, and returning coarse materials to the flour mill for regrinding through a particle classifier to obtain powder with the fineness of-0.075 mm accounting for more than 80%;
(2) adding the powder obtained in the step (1) into a reduction furnace, controlling the temperature to be 700 ℃, introducing hydrogen gas prepared by ammonia decomposition, carrying out reduction reaction, reducing manganese dioxide in manganese slag into manganese monoxide, and evaporating lead in the manganese slag into gas at high temperature to obtain reduced manganese slag;
(3) cooling the gas obtained in the step (2) by water, and cooling lead steam in the gas into solid lead to obtain a lead concentrate product;
(4) adding the reduced manganese slag into a dilute sulfuric acid solution for reaction to generate manganese sulfate mixed slurry;
(5) carrying out filter pressing on the manganese sulfate mixed slurry to obtain filter residues, namely leaching residues, wherein the filtrate is a manganese sulfate solution;
(6) adding oxygen into the manganese sulfate solution, carrying out oxidation iron removal, filtering to obtain a pure manganese sulfate solution which can be directly used as an electrolytic manganese raw material, filtering to obtain iron-removed slag, and calcining at 520 ℃ to obtain a cement blending material;
(7) adding sodium chlorate into the pure manganese sulfate solution, carrying out solid-liquid separation after reaction to obtain a manganese dioxide primary product, wherein the reaction is as follows:
5MnSO4+2NaClO3+4H2O＝4MnO2+Na2SO4+4H2SO4+Cl2↑
the chemical manganese dioxide generated by the reaction nucleates and grows on manganese dioxide seed crystals which are placed in a reactor in advance, and the apparent specific gravity and the crystal structure of a reaction product are regulated and controlled by controlling the temperature and the reaction speed, so that the optimal electrochemical activity is achieved;
(8) sequentially carrying out multistage rinsing, neutralization and re-rinsing on the manganese dioxide primary product to obtain manganese dioxide slurry;
the specific surface area of the manganese dioxide primary product is large, a large amount of acid and impurities can be adsorbed on the surfaces of microscopic particles of the manganese dioxide primary product, and multi-stage rinsing is required firstly;
rinsing until the pH value is more than 3, adding a neutralizing agent for neutralization, and adjusting the pH value to about 7, wherein the neutralizing agent is sodium hydroxide;
after neutralization, rinsing again by using purified water to remove residual neutralizer and other impurities;
(9) carrying out solid-liquid separation on the manganese dioxide slurry in a filter press to obtain a manganese dioxide semi-finished product;
(10) and drying the semi-finished manganese dioxide product, controlling the drying temperature and time to enable the moisture content of the intermediate to reach the corresponding product standard, and cooling, mixing and packaging to obtain the battery-grade manganese dioxide product.
Example 3
The invention relates to a method for preparing battery-grade manganese dioxide by using anode slag, which comprises the following steps:
(1) feeding the anode slag into a flour mill for dry milling, and returning coarse materials to the flour mill for regrinding through a particle classifier to obtain powder with the fineness of-0.075 mm accounting for more than 80%;
(2) adding the powder obtained in the step (1) into a reduction furnace, controlling the temperature to be 900 ℃, introducing hydrogen gas prepared by ammonia decomposition, carrying out reduction reaction, reducing manganese dioxide in manganese slag into manganese monoxide, and evaporating lead in the manganese slag into gas at high temperature to obtain reduced manganese slag;
(3) cooling the gas obtained in the step (2) by water, and cooling lead steam in the gas into solid lead to obtain a lead concentrate product;
(4) adding the reduced manganese slag into a dilute sulfuric acid solution for reaction to generate manganese sulfate mixed slurry;
(5) carrying out filter pressing on the manganese sulfate mixed slurry to obtain filter residues, namely leaching residues, wherein the filtrate is a manganese sulfate solution;
(6) adding manganese dioxide into a manganese sulfate solution, carrying out oxidation iron removal, filtering to obtain a pure manganese sulfate solution which can be directly used as an electrolytic manganese raw material, filtering to obtain iron-removed slag, and calcining at 400 ℃ to obtain a cement blending material;
(7) adding sodium chlorate into the pure manganese sulfate solution, carrying out solid-liquid separation after reaction to obtain a manganese dioxide primary product, wherein the reaction is as follows:
5MnSO4+2NaClO3+4H2O＝4MnO2+Na2SO4+4H2SO4+Cl2↑
the chemical manganese dioxide generated by the reaction nucleates and grows on manganese dioxide seed crystals which are placed in a reactor in advance, and the apparent specific gravity and the crystal structure of a reaction product are regulated and controlled by controlling the temperature and the reaction speed, so that the optimal electrochemical activity is achieved;
(8) sequentially carrying out multistage rinsing, neutralization and re-rinsing on the manganese dioxide primary product to obtain manganese dioxide slurry;
the specific surface area of the manganese dioxide primary product is large, a large amount of acid and impurities can be adsorbed on the surfaces of microscopic particles of the manganese dioxide primary product, and multi-stage rinsing is required firstly;
when the pH value is higher than 3 after rinsing, adding a neutralizing agent for neutralization, adjusting the pH value to be about 7, wherein the neutralizing agent is a mixture of sodium hydroxide and ammonium bicarbonate (the mass ratio is 1: 1);
after neutralization, rinsing again by using purified water to remove residual neutralizer and other impurities;
(9) carrying out solid-liquid separation on the manganese dioxide slurry in a filter press to obtain a manganese dioxide semi-finished product;
(10) and drying the semi-finished manganese dioxide product, controlling the drying temperature and time to enable the moisture content of the intermediate to reach the corresponding product standard, and cooling, mixing and packaging to obtain the battery-grade manganese dioxide product.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A method for preparing battery-grade manganese dioxide by using anode slag is characterized by comprising the following steps:
(1) grinding the anode slag to obtain powder with preset fineness;
(2) adding the powder obtained in the step (1) into a reduction furnace, introducing hydrogen gas prepared by ammonia decomposition, carrying out reduction reaction, reducing manganese dioxide in manganese slag into manganese monoxide, evaporating lead in the manganese slag into gas at high temperature, and taking the residue in the reduction furnace as reduced manganese slag;
(3) cooling the gas obtained in the step (2) by water, and cooling lead steam in the gas into solid lead to obtain a lead concentrate product;
(4) adding the reduced manganese slag obtained in the step (2) into a dilute sulfuric acid solution for reaction to generate manganese sulfate mixed slurry;
(5) performing filter pressing on the manganese sulfate mixed slurry obtained in the step (4), wherein the obtained filter residue is leaching residue, and the filtrate is manganese sulfate solution;
(6) adding an oxidant into the manganese sulfate solution obtained in the step (5), performing oxidation iron removal, and filtering to obtain a pure manganese sulfate solution;
(7) adding sodium chlorate into the pure manganese sulfate solution obtained in the step (6), and carrying out solid-liquid separation after reaction to obtain a manganese dioxide primary product;
(8) sequentially carrying out multistage rinsing, neutralization and re-rinsing on the manganese dioxide primary product to obtain manganese dioxide slurry;
(9) carrying out solid-liquid separation on the manganese dioxide slurry in a filter press to obtain a manganese dioxide semi-finished product;
(10) and drying the semi-finished manganese dioxide product, controlling the drying temperature and time to enable the moisture content of the intermediate to reach the corresponding product standard, and cooling, mixing and packaging to obtain the battery-grade manganese dioxide product.
2. The method for preparing battery grade manganese dioxide by using anode slag according to claim 1, wherein in the step (1), the fineness of the powder with the predetermined fineness is-0.075 mm and accounts for more than 80%.
3. The method for preparing battery-grade manganese dioxide by using anode slag according to claim 1, wherein the temperature of the reduction reaction in the step (2) is 700-1200 ℃.
4. The method for preparing battery-grade manganese dioxide by using anode slag according to claim 1, wherein in the step (6), the oxidant is one or more of oxygen, hydrogen peroxide and manganese dioxide.
5. The method for preparing battery-grade manganese dioxide by using anode slag according to claim 1, wherein in the step (6), the iron-removed slag obtained by filtering is calcined at low temperature to obtain a cement blending material.
6. The method for preparing battery-grade manganese dioxide by using anode slag according to claim 5, wherein the low-temperature calcination temperature is 300-520 ℃.
7. The method for preparing battery-grade manganese dioxide by using anode slag according to claim 1, wherein in the step (7), solid-liquid separation is carried out in a filter press, the filtrate contains sulfuric acid and unreacted manganese sulfate, and the filtrate is recycled to the reaction synthesis process.
8. The method for preparing battery-grade manganese dioxide by using anode slag according to claim 1, wherein in the step (8), when the manganese dioxide primary product is rinsed in multiple stages until the pH value is more than 3, a neutralizing agent is added for neutralization, and the pH value is adjusted to 6-8.
9. The method for preparing battery-grade manganese dioxide by using anode slag according to claim 8, wherein the neutralizing agent is one or both of sodium hydroxide and ammonium bicarbonate.
10. The method for preparing battery-grade manganese dioxide using anode slime as set forth in claim 1, wherein in step (8), after neutralization, the manganese dioxide is rinsed again with purified water to remove residual neutralizer and other impurities.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113772734A (en) * | 2021-11-04 | 2021-12-10 | 四川省盈达锂电新材料有限公司 | Method for recovering manganese and iron resources from manganese slag |
| CN114835167A (en) * | 2022-04-13 | 2022-08-02 | 贵州大龙汇成新材料有限公司 | Process for producing manganese sulfate by using poor manganese ore |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105886781A (en) * | 2016-06-29 | 2016-08-24 | 广西桂柳化工有限责任公司 | Method for recovering manganese dioxide from electrolytic manganese anode mud |
| CN110016562A (en) * | 2019-04-23 | 2019-07-16 | 重庆大学 | A kind of method of lead in removing electrolytic manganese anode mud |
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2020
- 2020-12-23 CN CN202011542559.9A patent/CN112645387A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105886781A (en) * | 2016-06-29 | 2016-08-24 | 广西桂柳化工有限责任公司 | Method for recovering manganese dioxide from electrolytic manganese anode mud |
| CN110016562A (en) * | 2019-04-23 | 2019-07-16 | 重庆大学 | A kind of method of lead in removing electrolytic manganese anode mud |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113772734A (en) * | 2021-11-04 | 2021-12-10 | 四川省盈达锂电新材料有限公司 | Method for recovering manganese and iron resources from manganese slag |
| CN114835167A (en) * | 2022-04-13 | 2022-08-02 | 贵州大龙汇成新材料有限公司 | Process for producing manganese sulfate by using poor manganese ore |
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