CN112678880A - Method for recycling manganese slag - Google Patents
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- CN112678880A CN112678880A CN202011542600.2A CN202011542600A CN112678880A CN 112678880 A CN112678880 A CN 112678880A CN 202011542600 A CN202011542600 A CN 202011542600A CN 112678880 A CN112678880 A CN 112678880A
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Abstract
The invention discloses a recycling method of manganese slag, belonging to the technical field of manganese slag recycling, and the method comprises the steps of adding compound ingredients into a mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate after impurity removal to prepare a solution with a qualified ratio; and then sequentially carrying out alkalization, washing and drying treatment on the solution with qualified mixture ratio to obtain a nickel-cobalt-manganese ternary hydroxide product with a preset mixture ratio. The method can effectively recover nickel, cobalt and manganese elements in the manganese sulfide slag, effectively treat and recycle the manganese sulfide slag, solve the problem of environmental pollution of the manganese sulfide slag and prepare the battery-grade nickel-cobalt-manganese ternary hydroxide product.
Description
Technical Field
The invention belongs to the technical field of manganese slag recovery, and relates to a method for recycling manganese slag.
Background
China is the biggest world manganese production, consumption and export, and accounts for more than 90% of the total global manganese production. Manganese slag in the wet manganese industry is a general term for manganese slag leached in the production of electrolytic manganese metal, electrolytic manganese dioxide and manganese sulfate products and manganese sulfide slag generated in the solution purification process, and the yield of manganese slag in China in 2019 is reported to exceed 2000 million tons.
The manganese sulfide slag refers to sulfide slag generated in a vulcanizing agent impurity removal process in a wet production process of manganese products (including electrolytic manganese metal, manganese sulfate, electrolytic manganese dioxide, manganese carbonate and the like).
At present, about 40 million tons of manganese sulfide slag are newly added in China every year, the manganese sulfide slag is mainly distributed in provinces and cities such as Ningxia, Guizhou, Guangxi, Hunan, Chongqing and Hubei at present, enterprises do not find a method for properly treating the manganese sulfide slag, and the manganese sulfide slag is generally transported to a storage yard for damming and stacking. The domestic manganese sulfide slag tailing dam occupies a large area, has low safety factor, and not only pollutes large cultivated land and underground water source and causes serious damage to the ecological environment, but also wastes heavy metal elements (nickel, cobalt, manganese and the like) in the manganese sulfide slag under the effect of weathering eluviation for a long time.
Disclosure of Invention
The invention aims to provide a method for recycling manganese slag, which can effectively recycle nickel, cobalt and manganese elements in manganese sulfide slag to obtain a battery-grade nickel-cobalt-manganese ternary hydroxide product.
The manganese slag recycling method provided by the invention comprises the following steps:
(1) adding a vulcanizing agent into the manganese ore leaching solution, and carrying out solid-liquid separation to obtain a pure manganese sulfate solution as filtrate and manganese sulfide residue as filter residue;
(2) adding sulfuric acid and an oxidant into the manganese sulfide slag obtained in the step (1), and carrying out oxidation leaching to obtain sulfate slurry containing nickel, cobalt, manganese and zinc;
(3) carrying out filter pressing on the sulfate slurry containing nickel, cobalt, manganese and zinc obtained in the step (2) to obtain a sulfate solution and leaching residues;
(4) extracting and removing zinc in the sulfate solution obtained in the step (3) by adopting an organic system with phosphate as an extracting agent and sulfonated kerosene as a solvent to obtain a mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate;
(5) adding a compound ingredient into the mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate obtained in the step (4), namely preparing a solution with a qualified ratio by using nickel sulfate, cobalt sulfate and manganese sulfate in a set proportion;
(6) and (4) sequentially carrying out alkalization, washing and drying treatment on the solution with the qualified mixture ratio obtained in the step (5) to obtain a nickel-cobalt-manganese ternary hydroxide product with a preset mixture ratio.
Preferably, in the step (1), the vulcanizing agent is one or more of sodium sulfide, barium sulfide and sodium dimethyldithiocarbamate, so that nickel, cobalt, zinc and part of manganese in the solution are converted into the vulcanizing slag.
In a preferable scheme, in the step (2), the oxidant is one or more of hydrogen peroxide, manganese dioxide and nitric acid;
adding manganese sulfide slag into a chemical combination barrel for water distribution and slurrying, adding sulfuric acid and an oxidant, and reacting metal sulfides NiS, CoS, MnS and ZnS in the manganese sulfide slag with the oxidant to generate NiSO-containing slurry4、CoSO4、MnSO4、ZnSO4The slurry of (4);
a small amount of Fe in the manganese sulfide slag2+Is oxidized into Fe3+，Fe3+Immediate hydrolysis to Fe (OH)3The precipitate was then removed by pressure filtration.
In the preferable scheme, in the step (3), the leached slag is subjected to harmless treatment and then is transported to a slag yard for storage.
In the preferable scheme, in the step (5), the manganese sulfate in the compound materials is the pure manganese sulfate solution obtained in the step (1), so that manganese sulfate resources are recycled.
According to the preferable scheme, in the step (5), the compound materials (including nickel sulfate, cobalt sulfate and manganese sulfate) are put into the mixed solution, deionized water is added, and the mixture is heated and stirred by steam to completely dissolve the compound materials, so that the solution with a qualified ratio is prepared.
Preferably, in the step (6), the alkalization treatment is specifically:
respectively adding the solution with qualified ratio, ammonia water and sodium hydroxide solution into a reaction kettle, and respectively controlling the flow rates of the three solutions through a quantitative pump and a flowmeter; the pH value of a reaction system is controlled by adjusting the flow of a sodium hydroxide solution, ammonia water is used as a pH value regulator and a pH value buffer, and the reaction temperature is controlled by adopting steam heating, so that the nickel-cobalt-manganese hydroxide intermediate product is continuously produced.
Preferably, in step (6), the washing treatment specifically comprises:
conveying the nickel-cobalt-manganese hydroxide intermediate product to a washer through a pump and a pipeline, washing for three times in a reverse washing mode, wherein the washing water for the third time is deionized water, the washing wastewater for the third time enters a second washing procedure to serve as the washing water for the second time, the washing wastewater for the second time enters a first washing procedure to serve as the washing water for the first time, continuously washing in a reverse order, finally, enabling the washing wastewater to flow out of the lower part of the first washer to enter a wastewater storage tank, and performing filter pressing after the intermediate product is washed to be qualified to obtain a pressed and dried intermediate product.
Preferably, in step (6), the drying treatment specifically comprises:
the dried intermediate product is sent into a vacuum drier for drying, and the moisture content of the intermediate product reaches the corresponding product standard by controlling the drying temperature and time; cooling, mixing and packaging to obtain the nickel-cobalt-manganese ternary hydroxide product with a preset ratio.
Compared with the prior art, the invention has the beneficial technical effects that:
the invention provides a method for recycling manganese slag, which can effectively recycle nickel, cobalt and manganese elements in manganese sulfide slag, effectively treat and recycle the manganese sulfide slag, solve the problem of environmental pollution of the manganese sulfide slag and prepare a battery-grade nickel-cobalt-manganese ternary hydroxide product.
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 manganese sulfide slag comprises the following main components in percentage by mass: mn (8-20%), S (3-8%), Zn (0.5-3%), Co (0.1-3%), Ni (0.1-3%) and Fe (0.3-3%).
Example 1
The invention relates to a method for recycling manganese slag, which comprises the following steps:
(1) grinding manganese ores (including manganese carbonate ores and manganese oxide ores), then carrying out redox reaction on high-valence manganese to obtain bivalent manganese, adding sulfuric acid to dissolve and leach to generate manganese sulfate, wherein filter residues are leaching residues, removing iron from filtrate, adding barium sulfide under a neutral condition to further remove impurities, carrying out solid-liquid separation at the stage, wherein the filter residues are manganese sulfide residues, and the filtrate is a pure manganese sulfate solution;
(2) adding sulfuric acid and hydrogen peroxide into the manganese sulfide slag, and carrying out oxidation leaching to obtain sulfate slurry containing nickel, cobalt, manganese and zinc;
(3) carrying out filter pressing on sulfate slurry containing nickel, cobalt, manganese and zinc to obtain sulfate solution and leaching residues, and carrying out harmless treatment on the leaching residues to a residue field for stockpiling;
(4) extracting and removing zinc in the sulfate solution obtained in the step (3) by adopting an organic system with phosphate as an extracting agent and sulfonated kerosene as a solvent to obtain a mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate;
(5) adding a compound material into the mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate obtained in the step (4) according to Ni0.5Mn0.3Co0.2(OH)2Proportioning, adding deionized water, heating by adopting steam, stirring, and completely dissolving the compound material to prepare a solution with qualified proportioning;
(6) respectively adding the solution with qualified ratio, ammonia water and sodium hydroxide solution into a reaction kettle, and respectively controlling the flow rates of the three solutions through a quantitative pump and a flowmeter; controlling the pH value of a reaction system by adjusting the flow of a sodium hydroxide solution, taking ammonia water as a pH value regulator and a pH value buffer, and continuously producing a nickel-cobalt-manganese hydroxide intermediate product by adopting steam heating to control the reaction temperature;
(7) conveying the nickel-cobalt-manganese hydroxide intermediate product to a washer through a pump and a pipeline, washing for three times in a reverse washing mode, wherein the washing water for the third time is deionized water, the washing wastewater for the third time enters a second washing procedure as the washing water for the second time, the washing wastewater for the second time enters a first washing procedure as the washing water for the first time, washing in the reverse sequence continuously in such a way, finally, the washing wastewater flows out of the lower part of the first washer and enters a wastewater storage tank, and after the intermediate product is qualified by washing, performing pressure filtration to obtain a dried intermediate product;
(8) the dried intermediate product is sent into a vacuum drier for drying, and the moisture content of the intermediate product reaches the corresponding product standard by controlling the drying temperature and time; cooling, mixing and packaging to obtain the battery-grade Ni0.5Mn0.3Co0.2(OH)2And (5) producing the product.
In the nickel-cobalt-manganese ternary hydroxide product obtained in example 1, the content of Fe was 0.004 wt%, the content of Ca was 0.008 wt%, the content of Cu was 0.001 wt%, and the content of Zn was 0.003 wt%.
Example 2
The invention relates to a method for recycling manganese slag, which comprises the following steps:
(1) grinding manganese ores (including manganese carbonate ores and manganese oxide ores), then carrying out redox reaction on high-valence manganese to obtain bivalent manganese, adding sulfuric acid to dissolve and leach to generate manganese sulfate, wherein filter residues are leaching residues, removing iron from filtrate, adding sodium sulfide under a neutral condition to further remove impurities, carrying out solid-liquid separation at the stage, wherein the filter residues are manganese sulfide residues, and the filtrate is a pure manganese sulfate solution;
(2) adding sulfuric acid and manganese dioxide into the manganese sulfide slag, and carrying out oxidation leaching to obtain sulfate slurry containing nickel, cobalt, manganese and zinc;
(3) carrying out filter pressing on sulfate slurry containing nickel, cobalt, manganese and zinc to obtain sulfate solution and leaching residues, and carrying out harmless treatment on the leaching residues to a residue field for stockpiling;
(4) extracting and removing zinc in the sulfate solution obtained in the step (3) by adopting an organic system with phosphate as an extracting agent and sulfonated kerosene as a solvent to obtain a mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate;
(5) adding a compound material into the mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate obtained in the step (4) according to Ni0.6Mn0.2Co0.2(OH)2Proportioning, adding deionized water, heating by adopting steam, stirring, and completely dissolving the compound material to prepare a solution with qualified proportioning;
(6) respectively adding the solution with qualified ratio, ammonia water and sodium hydroxide solution into a reaction kettle, and respectively controlling the flow rates of the three solutions through a quantitative pump and a flowmeter; controlling the pH value of a reaction system by adjusting the flow of a sodium hydroxide solution, taking ammonia water as a pH value regulator and a pH value buffer, and continuously producing a nickel-cobalt-manganese hydroxide intermediate product by adopting steam heating to control the reaction temperature;
(7) conveying the nickel-cobalt-manganese hydroxide intermediate product to a washer through a pump and a pipeline, washing for three times in a reverse washing mode, wherein the washing water for the third time is deionized water, the washing wastewater for the third time enters a second washing procedure as the washing water for the second time, the washing wastewater for the second time enters a first washing procedure as the washing water for the first time, washing in the reverse sequence continuously in such a way, finally, the washing wastewater flows out of the lower part of the first washer and enters a wastewater storage tank, and after the intermediate product is qualified by washing, performing pressure filtration to obtain a dried intermediate product;
(8) feeding the dried intermediate product into vacuumDrying by a dryer, and controlling the drying temperature and time to enable the moisture content of the intermediate to reach the corresponding product standard; cooling, mixing and packaging to obtain the battery-grade Ni0.6Mn0.2Co0.2(OH)2And (5) producing the product.
In the nickel-cobalt-manganese ternary hydroxide product obtained in example 2, the content of Fe was 0.003 wt%, the content of Ca was 0.006 wt%, the content of Cu was 0.002 wt%, and the content of Zn was 0.004 wt%.
Example 3
The invention relates to a method for recycling manganese slag, which comprises the following steps:
(1) grinding manganese ores (including manganese carbonate ores and manganese oxide ores), then carrying out redox reaction on high-valence manganese to obtain bivalent manganese, adding sulfuric acid to dissolve and leach to generate manganese sulfate, wherein filter residues are leaching residues, removing iron from filtrate, adding sodium dimethyldithiocarbamate (SDD) under a neutral condition to further remove impurities, carrying out solid-liquid separation at the stage, wherein the filter residues are manganese sulfide residues, and the filtrate is a pure manganese sulfate solution;
(2) adding sulfuric acid and nitric acid into the manganese sulfide slag, and carrying out oxidation leaching to obtain sulfate slurry containing nickel, cobalt, manganese and zinc;
(3) carrying out filter pressing on sulfate slurry containing nickel, cobalt, manganese and zinc to obtain sulfate solution and leaching residues, and carrying out harmless treatment on the leaching residues to a residue field for stockpiling;
(4) extracting and removing zinc in the sulfate solution obtained in the step (3) by adopting an organic system with phosphate as an extracting agent and sulfonated kerosene as a solvent to obtain a mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate;
(5) adding a compound material into the mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate obtained in the step (4) according to Ni0.8Mn0.1Co0.1(OH)2Proportioning, adding deionized water, heating by adopting steam, stirring, and completely dissolving the compound material to prepare a solution with qualified proportioning;
(6) respectively adding the solution with qualified ratio, ammonia water and sodium hydroxide solution into a reaction kettle, and respectively controlling the flow rates of the three solutions through a quantitative pump and a flowmeter; controlling the pH value of a reaction system by adjusting the flow of a sodium hydroxide solution, taking ammonia water as a pH value regulator and a pH value buffer, and continuously producing a nickel-cobalt-manganese hydroxide intermediate product by adopting steam heating to control the reaction temperature;
(7) conveying the nickel-cobalt-manganese hydroxide intermediate product to a washer through a pump and a pipeline, washing for three times in a reverse washing mode, wherein the washing water for the third time is deionized water, the washing wastewater for the third time enters a second washing procedure as the washing water for the second time, the washing wastewater for the second time enters a first washing procedure as the washing water for the first time, washing in the reverse sequence continuously in such a way, finally, the washing wastewater flows out of the lower part of the first washer and enters a wastewater storage tank, and after the intermediate product is qualified by washing, performing pressure filtration to obtain a dried intermediate product;
(8) the dried intermediate product is sent into a vacuum drier for drying, and the moisture content of the intermediate product reaches the corresponding product standard by controlling the drying temperature and time; cooling, mixing and packaging to obtain the battery-grade Ni0.8Mn0.1Co0.1(OH)2And (5) producing the product.
In the nickel-cobalt-manganese ternary hydroxide product obtained in example 3, the content of Fe was 0.002 wt%, the content of Ca was 0.01 wt%, the content of Cu was 0.003 wt%, and the content of Zn was 0.004 wt%.
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 (8)
1. The method for recycling manganese slag is characterized by comprising the following steps:
(1) adding a vulcanizing agent into the manganese ore leaching solution, and carrying out solid-liquid separation to obtain a pure manganese sulfate solution as filtrate and manganese sulfide residue as filter residue;
(2) adding sulfuric acid and an oxidant into the manganese sulfide slag obtained in the step (1), and carrying out oxidation leaching to obtain sulfate slurry containing nickel, cobalt, manganese and zinc;
(3) carrying out filter pressing on the sulfate slurry containing nickel, cobalt, manganese and zinc obtained in the step (2) to obtain a sulfate solution and leaching residues;
(4) extracting and removing zinc in the sulfate solution obtained in the step (3) by adopting an organic system with phosphate as an extracting agent and sulfonated kerosene as a solvent to obtain a mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate;
(5) adding a compound ingredient into the mixed solution containing nickel sulfate, cobalt sulfate and manganese sulfate obtained in the step (4), namely preparing a solution with a qualified ratio by using nickel sulfate, cobalt sulfate and manganese sulfate in a set proportion;
(6) and (4) sequentially carrying out alkalization, washing and drying treatment on the solution with the qualified mixture ratio obtained in the step (5) to obtain a nickel-cobalt-manganese ternary hydroxide product with a preset mixture ratio.
2. The manganese slag recycling method according to claim 1, wherein in step (1), the vulcanizing agent is one or more of sodium sulfide, barium sulfide and sodium dimethyldithiocarbamate.
3. The manganese slag recycling method according to claim 1, wherein in the step (2), the oxidant is one or more of hydrogen peroxide, manganese dioxide and nitric acid.
4. The manganese slag recycling method according to claim 1, wherein in the step (5), the manganese sulfate in the compound material is the pure manganese sulfate solution obtained in the step (1) to recycle manganese sulfate resources.
5. The recycling method of manganese slag according to claim 1, wherein in the step (5), the compound material is added into the mixed solution, deionized water is added, and the mixture is heated and stirred by steam to completely dissolve the compound material, so as to prepare a solution with a qualified mixture ratio.
6. The manganese slag recycling method according to claim 1, wherein in the step (6), the alkalization treatment is specifically:
respectively adding the solution with qualified ratio, ammonia water and sodium hydroxide solution into a reaction kettle, and respectively controlling the flow rates of the three solutions through a quantitative pump and a flowmeter; the pH value of a reaction system is controlled by adjusting the flow of a sodium hydroxide solution, ammonia water is used as a pH value regulator and a pH value buffer, and the reaction temperature is controlled by adopting steam heating, so that the nickel-cobalt-manganese hydroxide intermediate product is continuously produced.
7. The manganese slag recycling method according to claim 1, wherein in the step (6), the washing treatment specifically comprises:
conveying the nickel-cobalt-manganese hydroxide intermediate product to a washer through a pump and a pipeline, washing for three times in a reverse washing mode, wherein the washing water for the third time is deionized water, the washing wastewater for the third time enters a second washing procedure to serve as the washing water for the second time, the washing wastewater for the second time enters a first washing procedure to serve as the washing water for the first time, continuously washing in a reverse order, finally, enabling the washing wastewater to flow out of the lower part of the first washer to enter a wastewater storage tank, and performing filter pressing after the intermediate product is washed to be qualified to obtain a pressed and dried intermediate product.
8. The manganese slag recycling method according to claim 1, wherein in the step (6), the drying treatment specifically comprises:
the dried intermediate product is sent into a vacuum drier for drying, and the moisture content of the intermediate product reaches the corresponding product standard by controlling the drying temperature and time; cooling, mixing and packaging to obtain the nickel-cobalt-manganese ternary hydroxide product with a preset ratio.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024060546A1 (en) * | 2022-09-23 | 2024-03-28 | 广东邦普循环科技有限公司 | Method for feeding nickel, cobalt, and manganese metal liquids |
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