CN108910958A - A method of manganese sulfate is produced using aniline reduction electrolytic manganese anode mud - Google Patents
A method of manganese sulfate is produced using aniline reduction electrolytic manganese anode mud Download PDFInfo
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- CN108910958A CN108910958A CN201810783452.XA CN201810783452A CN108910958A CN 108910958 A CN108910958 A CN 108910958A CN 201810783452 A CN201810783452 A CN 201810783452A CN 108910958 A CN108910958 A CN 108910958A
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- manganese
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- manganese sulfate
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- aniline
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C50/00—Quinones
- C07C50/02—Quinones with monocyclic quinoid structure
- C07C50/04—Benzoquinones, i.e. C6H4O2
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin by wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/06—Obtaining tin from scrap, especially tin scrap
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B47/00—Obtaining manganese
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses a kind of methods using aniline reduction electrolytic manganese anode mud production manganese sulfate, include the following steps：S1 adds the broken slurrying of water mill in Manganese anode slime；S2 imports manganese slurry in the reaction kettle with cooling device；Aniline is added in manganese slurry in S3；Manganese slurry is heated to 90~130 degrees Celsius, the benzoquinone after collecting vaporization by S4；S5 obtains slicker solder slag and manganese sulfate solution by manganese slurry by filter press separating and filtering；Ammonium sulfide is added in manganese sulfate solution obtained after separation by S6, is removed the heavy metals such as the lead in manganese sulfate solution, is obtained the higher manganese sulfate solution of purity；S7 by the heated concentration of purified manganese sulfate solution, Crystallization Separation, dries to obtain finished solid manganese sulfate.Elements and a small amount of manganese such as lead, tin, the antimony in the former earth of positive pole are only remained after benzoquinone of the present invention, manganese are recovered, in slag, because the quantity of slag significantly tails off, therefore in slag slicker solder antimony content significantly increase and by enriching and recovering.
Description
Technical field
The present invention relates to a kind of methods using aniline reduction electrolytic manganese anode mud production manganese sulfate, belong to the life of manganese sulfate
Produce preparation technical field.
Background technique
When being electrolysed manganese sulfate, there is a manganese metal and the earth of positive pole, manganese metal is used as the deep processing of manganese, and the earth of positive pole its mainly
Ingredient is MnO2, and containing valuable metals such as lead, tin, antimony, it is generally industrially regarded into pyrolusite raw material, using iron powder reducing
Method, ferrous sulfate reduction leaching process, two mines roasting water seaoning or two mine One-step production manganese sulfates.But no matter which kind of side used
Method, because solid reductant is added, the leaching quantity of slag after soaking manganese is larger, causes the tenors such as lead, tin, the antimony in slag lower, returns
It is big to receive difficulty, cost recovery is high, and without economic significance, therefore current domestic production producer is substantially by the way of landfill
Reason, leads to the wasting of resources and environmental pollution.
Summary of the invention
The object of the present invention is to provide a kind of methods using aniline reduction electrolytic manganese anode mud production manganese sulfate, adopt
Manganese, benzoquinone have not only been recycled with this method, but also has recycled the valuable elements such as the lead in the earth of positive pole to the greatest extent, together
When perfectly solve the Manganese anode slime bring wasting of resources of electrolytic manganese manufacturer and problem of environmental pollution.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A method of manganese sulfate being produced using aniline reduction electrolytic manganese anode mud, is included the following steps：
S1 adds water slurrying in Manganese anode slime；Below levigate extremely -120 mesh of Manganese anode slime；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, detection manganese slurry
Solid-to-liquid ratio (guaranteeing the initial acid concentrations being added in 400~500g/l) and manganese dioxide content, are added according to manganese dioxide content
Sulfuric acid solution (dosage of sulfuric acid be theoretical amount 1~2 times)；
S3, by reactor temperature control at 30 degrees Celsius hereinafter, manganese slurry in aniline is added, after having added aniline,
It is reacted 2~10 hours under normal temperature state；
MnO2+C6H7N+H2SO4→MnSO4+C6H4O2+H2O
Manganese slurry is heated to 90~130 degrees Celsius by S4, and the benzoquinone after collecting vaporization, temperature is too low, and benzoquinone is not
It can vaporize completely, the excessively high benzoquinone of temperature will appear coking phenomenon, both will affect the rate of recovery of benzoquinone, using this
The rate of recovery of method benzoquinone is up to 97% or more；
S5, by manganese slurry be cooled to 55 degrees Celsius or less (temperature is excessively high, in ammonium hydroxide with when ammonium hydroxide volatilization loss it is larger),
Ammonium hydroxide is added in manganese slurry, the pH value that manganese is starched is adjusted to 5~7, and (under this pH condition, the impurity other than manganese is deposited in solid form
), by manganese slurry by filter press separating and filtering, obtain slicker solder slag (lead, tin the rate of recovery can achieve 99% or more) and sulfuric acid
Manganese solution；
Appropriate ammonium sulfide will be added in S6 in manganese sulfate solution, further purification removes the heavy metals such as lead；
MeSO4+(NH4)2S→MeS+(NH4)2SO4, Me indicates the heavy metals such as lead in this chemical formula.
Purified manganese sulfate solution is obtained finished solid sulfuric acid by heating evaporation concentration, Crystallization Separation, drying by S7
Manganese.
In a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate above-mentioned, the step S6 further includes
Following methods：The manganese sulfate solution is collected, ammonium sulfide solution is added in manganese sulfate solution, removes the lead in manganese sulfate solution
Equal heavy metals.
In a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate above-mentioned, the step S1 further includes
Following methods：Manganese anode slime particle is milled to -120 mesh hereinafter, then adding water slurrying.
In a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate above-mentioned, the Manganese anode slime is electricity
The Manganese anode slime generated when solving manganese.
In a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate above-mentioned, aniline is no more than anti-
Answer in kettle controlled at controlling value, aniline is added in manganese slurry.
Compared with prior art, lead, the tin, antimony in the former earth of positive pole are only remained after benzoquinone of the present invention, manganese are recovered, in slag
Equal elements and a small amount of manganese, because the quantity of slag significantly tails off, therefore in slag slicker solder antimony content significantly increase and by enriching and recovering.The technique one
It lifts three to obtain, has not only recycled manganese, benzoquinones, but also recycled the valuable elements such as the lead in the earth of positive pole to the greatest extent, while complete
Beauty solves the Manganese anode slime bring wasting of resources of electrolytic manganese manufacturer and problem of environmental pollution.
The present invention is further illustrated With reference to embodiment.
Specific embodiment
The embodiment of the present invention 1：A method of manganese sulfate being produced using aniline reduction electrolytic manganese anode mud, including following
Step：
S1 adds water slurrying in Manganese anode slime, and Manganese anode slime is levigate to -120 mesh；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, detection manganese slurry
Sulfuric acid solution is added according to manganese dioxide content in solid-to-liquid ratio and manganese dioxide content；Guarantee the initial acid concentrations being added in 400g/
L, the dosage of sulfuric acid are 1 times of theoretical amount；
Reactor temperature is controlled at 30 degrees Celsius, aniline is added in manganese slurry, after having added aniline, in room temperature by S3
Reacted 2 hours under state, by aniline be no more than in reaction kettle controlled at controlling value, aniline is added in manganese slurry；
Manganese slurry is heated to 90 degrees Celsius, the benzoquinone after collecting vaporization by S4；
Manganese slurry is cooled to 55 degrees Celsius, ammonium hydroxide is added in manganese slurry, the pH value that manganese is starched is adjusted to 5, manganese slurry is passed through by S5
Filter press separating and filtering obtains slicker solder slag and manganese sulfate solution；
Ammonium sulfide is added in manganese sulfate solution obtained after separation by S6, removes the heavy metals such as the lead in manganese sulfate solution,
The higher manganese sulfate solution of purity is obtained, the manganese sulfate solution is collected, ammonium sulfide solution is added in manganese sulfate solution, go sulphur removal
Heavy metal in sour manganese solution；
S7 by the heated concentration of purified manganese sulfate solution, Crystallization Separation, dries to obtain finished solid manganese sulfate.
Embodiment 2：A method of manganese sulfate being produced using aniline reduction electrolytic manganese anode mud, is included the following steps：
Then plus water slurrying S1, the Manganese anode slime particle generated when by electrolytic manganese are milled to -150 mesh,；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, detection manganese slurry
Sulfuric acid solution is added according to manganese dioxide content in solid-to-liquid ratio and manganese dioxide content；Guarantee the initial acid concentrations being added in 500g/
L, the dosage of sulfuric acid are 2 times of theoretical amount；
Reactor temperature is controlled at 20 degrees Celsius, aniline is added in manganese slurry, after having added aniline, in room temperature by S3
Reacted 10 hours under state, by aniline be no more than in reaction kettle controlled at controlling value, aniline is added in manganese slurry；
Manganese slurry is heated to 130 degrees Celsius, the benzoquinone after collecting vaporization by S4；
Manganese slurry is cooled to 45 degrees Celsius, ammonium hydroxide is added in manganese slurry, the pH value that manganese is starched is adjusted to 7, manganese slurry is passed through by S5
Filter press separating and filtering obtains slicker solder slag and manganese sulfate solution；
Ammonium sulfide is added in manganese sulfate solution obtained after separation by S6, removes the heavy metals such as the lead in manganese sulfate solution,
The higher manganese sulfate solution of purity is obtained, the manganese sulfate solution is collected, ammonium sulfide solution is added in manganese sulfate solution, go sulphur removal
Heavy metal in sour manganese solution；
S7 by the heated concentration of purified manganese sulfate solution, Crystallization Separation, dries to obtain finished solid manganese sulfate.
Embodiment 3：A method of manganese sulfate being produced using aniline reduction electrolytic manganese anode mud, is included the following steps：
Then plus water slurrying S1, the Manganese anode slime particle generated when by electrolytic manganese are milled to -160 mesh,；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, detection manganese slurry
Sulfuric acid solution is added according to manganese dioxide content in solid-to-liquid ratio and manganese dioxide content；Guarantee the initial acid concentrations being added in 430g/
L, the dosage of sulfuric acid are 1.4 times of theoretical amount；
Reactor temperature is controlled at 25 degrees Celsius, aniline is added in manganese slurry, after having added aniline, in room temperature by S3
Reacted 7 hours under state, by aniline be no more than in reaction kettle controlled at controlling value, aniline is added in manganese slurry；
Manganese slurry is heated to 110 degrees Celsius, the benzoquinone after collecting vaporization by S4；
Manganese slurry is cooled to 35 degrees Celsius, ammonium hydroxide is added in manganese slurry, the pH value that manganese is starched is adjusted to 6, manganese slurry is passed through by S5
Filter press separating and filtering obtains slicker solder slag and manganese sulfate solution；
Ammonium sulfide is added in manganese sulfate solution obtained after separation by S6, removes the heavy metals such as the lead in manganese sulfate solution,
The higher manganese sulfate solution of purity is obtained, the manganese sulfate solution is collected, ammonium sulfide solution is added in manganese sulfate solution, go sulphur removal
Heavy metal in sour manganese solution；
S7 by the heated concentration of purified manganese sulfate solution, Crystallization Separation, dries to obtain finished solid manganese sulfate.
Claims (6)
1. a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate, which is characterized in that include the following steps：
S1 adds water slurrying in Manganese anode slime；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, the solid-liquid of detection manganese slurry
Than with manganese dioxide content, according to manganese dioxide content be added sulfuric acid solution；
S3 controls reactor temperature at 30 degrees Celsius hereinafter, aniline is added in manganese slurry, after having added aniline, in room temperature
It is reacted 2~10 hours under state；
Manganese slurry is heated to 90~130 degrees Celsius, the benzoquinone after collecting vaporization by S4；
S5, by manganese slurry be cooled to 55 degrees Celsius hereinafter, manganese slurry in ammonium hydroxide is added, by manganese starch pH value be adjusted to 5~7, manganese is starched
By filter press separating and filtering, slicker solder slag and manganese sulfate solution are obtained；
Ammonium sulfide is added in manganese sulfate solution obtained after separation by S6, is removed the heavy metals such as the lead in manganese sulfate solution, is obtained pure
Spend higher manganese sulfate solution；
S7 by the heated concentration of purified manganese sulfate solution, Crystallization Separation, dries to obtain finished solid manganese sulfate.
2. a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate according to claim 1, feature
It is, the step S6 further includes following methods：The manganese sulfate solution is collected, it is molten that ammonium sulfide is added in manganese sulfate solution
Liquid removes the heavy metal in manganese sulfate solution.
3. a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate according to claim 1, feature
It is, the step S1 further includes following methods：Manganese anode slime particle is milled to -120 mesh hereinafter, then adding water slurrying.
4. a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate according to claim 1, feature
It is, the Manganese anode slime that the Manganese anode slime generates when being electrolytic manganese.
5. a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate according to claim 1, feature
It is, further includes following methods in the step S3：By aniline be no more than reaction kettle in controlled at controlling value, by benzene
Amine is added in manganese slurry.
6. a kind of method using aniline reduction electrolytic manganese anode mud production manganese sulfate according to claim 1, feature
It is, further includes following methods in the step S2：The solid-to-liquid ratio and manganese dioxide content for detecting manganese slurry, contain according to manganese dioxide
Sulfuric acid solution is added in amount；Guarantee the initial acid concentrations being added in 400~500g/l, the dosage of sulfuric acid is 1~2 times of theoretical amount.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387391A (en) * | 2021-07-30 | 2021-09-14 | 广西埃索凯新材料科技有限公司 | Manganese sulfate production system based on manganese oxide ore |
| CN115011799A (en) * | 2022-07-13 | 2022-09-06 | 重庆上甲电子股份有限公司 | Method for producing soft magnetic trimanganese tetroxide by using electrolytic manganese anode slime |
| CN115058600A (en) * | 2022-07-21 | 2022-09-16 | 贵州大学 | Method for preparing manganese sulfate solution and recycling lead from anode slag |
| CN115386744A (en) * | 2022-08-18 | 2022-11-25 | 铜仁学院 | Method for high-value utilization of manganese anode slime |
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| CN103789551A (en) * | 2014-02-18 | 2014-05-14 | 广西大学 | Method for preparing manganese sulfate electrolyte and recycling lead by using electrolytic manganese anode mud |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387391A (en) * | 2021-07-30 | 2021-09-14 | 广西埃索凯新材料科技有限公司 | Manganese sulfate production system based on manganese oxide ore |
| CN115011799A (en) * | 2022-07-13 | 2022-09-06 | 重庆上甲电子股份有限公司 | Method for producing soft magnetic trimanganese tetroxide by using electrolytic manganese anode slime |
| CN115058600A (en) * | 2022-07-21 | 2022-09-16 | 贵州大学 | Method for preparing manganese sulfate solution and recycling lead from anode slag |
| CN115386744A (en) * | 2022-08-18 | 2022-11-25 | 铜仁学院 | Method for high-value utilization of manganese anode slime |
| CN115386744B (en) * | 2022-08-18 | 2024-02-02 | 铜仁学院 | Method for high-value utilization of manganese anode slime |
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Inventor after: Li Shuchun Inventor after: Fu Jing Inventor after: Liao Xinren Inventor after: Ma Juncai Inventor after: Zhao Fei Inventor before: Li Shuchun Inventor before: Liao Xinren Inventor before: Ma Juncai Inventor before: Zhao Fei |
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Application publication date: 20181130 |