CN108118156B - A kind of method that electrolytic manganese anode mud separation produces electrolytic manganese metal and recycles lead - Google Patents
A kind of method that electrolytic manganese anode mud separation produces electrolytic manganese metal and recycles lead Download PDFInfo
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- CN108118156B CN108118156B CN201810023327.9A CN201810023327A CN108118156B CN 108118156 B CN108118156 B CN 108118156B CN 201810023327 A CN201810023327 A CN 201810023327A CN 108118156 B CN108118156 B CN 108118156B
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/10—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of chromium or manganese
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- 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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Abstract
A kind of method for separating production electrolytic manganese metal the invention discloses electrolytic manganese anode mud and recycling lead, the following steps are included: S1. electrolytic manganese anode mud and sulfuric acid solution, blackstrap aqueous solution are mixed, then iron powder is added, separates leachate and leached mud after the reaction was completed；S2. H is added in leachate2O2, the leachate of COD must be removed；S3. ammonium sulfide or Sodium Dimethyldithiocarbamate is added in the leachate for removing COD, and ammonium hydroxide is added, obtain purification of manganese sulfate liquid, the electrolysis of purification of manganese sulfate liquid obtains metal manganese product.The present invention can also recycle the lead concentrate of 50% or more lead tolerance while producing Electrolytic Manganese Product, to realize that the clean and effective of electrolytic manganese anode mud utilizes.
Description
Technical field
The present invention relates to electrolytic manganese anode mud processing technology field more particularly to a kind of electrolytic manganese anode mud separation production electricity
Solution manganese metal and the method for recycling lead.
Background technique
Manganese has highly important strategic position as a kind of important metallurgy, chemical raw material in national economy.I
State's iron and steel output accounts for about 3/4ths of Gross World Product, " no manganese not Cheng Gang ", in smelting iron and steel, manganese and oxygen, sulphur it is affine
Power is all bigger, is the desulfurizing agent and deoxidier of molten steel.Electrolytic manganese metal is production stainless steel, height since purity is high, impurity are few
The important alloying element and welding rod of strength low alloy steel, alumal, cupromanganese etc., ferrite, permanent-magnet alloy member
Element and many medication chemistries with manganese salt produce in indispensable raw material.With the rise of technological progress and new industry, electrolysis
Manganese metal is increasingly extensive in the application of metallurgy, electronics, functional material and fine manganese salt arts.
Electrolytic manganese anode mud refers to use manganese sulfate solution in a cell electrolysis production manganese metal during, in anode
Room is inevitably formed with manganese dioxide (MnO2) or the hydrous oxide precipitating of manganese based on substance, black easily agglomerates,
Wherein manganese content is up to 40% ~ 50%, contains sardinianite, cesarolite (PbMn simultaneously3O7·nH2O), the multiple elements such as tin, selenium and
Compound, structure is complicated.
1 t electrolytic manganese metal of every production just generates 50 ~ 100 kg electrolytic manganese anode muds, by China's electrolytic manganese metal
Yield is converted into the quantum of output of electrolytic manganese anode mud up to 100,000 tons/year or more.Mineral composition and knot due to electrolytic manganese anode mud
Structure is complicated, and the hydrous oxide symbiosis of lead and manganese therein is very close, most of manganese oxide jelly with gluey annulus
Construction, therefore manganese and recycling lead cannot be purified using simple mechanical sorting method.It is used on a small quantity currently, electrolytic manganese anode mud removes
Than iron, the overwhelming majority is as industrial solid wastes by stockpiling disposition or cheap selling to smelting for the leaching manganese ore liquid of electrolytic manganese factory
Ingredient of the refinery as refining manganeisen raw material, however the substances such as lead, selenium in Manganese anode slime are volatile at high temperature, it is per ton
Manganese anode slime will volatilize nearly 50 kg of lead metal, not only waste lead resource, it is often more important that causes serious environmental pollution, damages
The life and health of the victimization people.
In recent years, researcher finds different processing methods for the characteristic of electrolytic manganese anode mud, mainly studies
Using Manganese anode slime as production manganese sulfate, manganese carbonate, the pure manganese dioxide of chemistry or battery, oxidation manganese systems product and LiMn2O4 etc.
The raw material of new material, but that there are still production costs is higher, the valuable element rate of recovery is low, or energy consumption is high, process route is long, very
To will form secondary pollution problems.Under the premise of national environmental protection energy saving policy is increasingly stringent, it can not generally be adopted by factory.
Therefore, status is utilized in the critical role in China and the processing of electrolytic manganese anode mud in view of current manganese, finds a kind of economic, environmental protection
Mode handle and had important practical significance using electrolytic manganese anode mud and urgent.
Summary of the invention
A kind of method for separating production electrolytic manganese metal the invention discloses electrolytic manganese anode mud and recycling lead, in production electricity
The lead concentrate of 50% or more lead tolerance can also be recycled while solving metal manganese product, to realize that the cleaning of electrolytic manganese anode mud is high
Effect utilizes.
To achieve the above object, the technical solution of the present invention is as follows:
A kind of method that electrolytic manganese anode mud separation produces electrolytic manganese metal and recycles lead, comprising the following steps:
S1. electrolytic manganese anode mud and 2.5 ~ 3.5molL-1Sulfuric acid solution mixing, and 65 ~ 70 gL are added-1Blackstrap
Aqueous solution stirring, the dosage of blackstrap are the 85 ~ 90% of reducing agent theoretical amount, 150 ~ 250 rmin of stirring rate-1, above-mentioned
In the mixture of electrolytic manganese anode mud, sulfuric acid solution and blackstrap aqueous solution, liquid-solid ratio is 3.8 ~ 4.2: 1, keeps mixture
Temperature is 70 ~ 80 DEG C, reacts 30 ~ 50min, and iron powder is then added, and the dosage of iron powder is greater than the theoretical amount of remaining reducing agent, instead
10 ~ 20min is answered, separates leachate and leached mud with filter press after the reaction was completed；
S2. H is added in leachate2O2, oxidizing condition are as follows: ρ (H2O2)/ρ (COD)=2.0 ~ 2.5, control reaction temperature be 48 ~
52 DEG C, the leachate of COD must be removed；
S3. ammonium sulfide or Sodium Dimethyldithiocarbamate is added in the leachate for removing COD, and the pH that ammonium hydroxide adjusting leachate is added is
5.5 ~ 6.0, removing heavy metals are removed, purification of manganese sulfate liquid is obtained, the electrolysis of purification of manganese sulfate liquid obtains metal manganese product.
Preferably, in the step S1, the concentration of sulfuric acid solution is 3.5molL-1, blackstrap concentration of aqueous solution is 70
g·L-1, liquid-solid ratio 4:1.
Preferably, 190 ~ 210 rmin of stirring rate-1。
Preferably, in the step S1, the temperature of mixture is 70 DEG C.
Preferably, in the step S2, ρ (H2O2)/ρ(COD)=2.5。
Preferably, in the step S2, reaction temperature is 50 DEG C, and the reaction time is 2 ~ 2.5h.
Preferably, in the step S3, the temperature that ammonium hydroxide reaction is added is 45 ~ 55 DEG C.
Preferably, in the step S1, leached mud takes out after cleaning in filter press to be dried, and obtains lead concentrate product.
The invention has the following advantages that
(1) electrolytic manganese anode mud is carried out manganese metal recycling directly as reactant by the present invention, and sulfuric acid is added, first with useless sugar
Honey is reducing agent, then using iron powder as reducing agent, the manganese leaching rate in the earth of positive pole can be made to reach 99% or more, and blackstrap is production
Waste can substantially reduce production cost, realize refuse reclamation, energy-saving ring by carrying out recycling and reusing to blackstrap
It protects.
(2) lead in the earth of positive pole is all stayed in filter residue and is separated and recovered through separation, and the present invention is directly to being deposited in pressure
Filter residue in filter aluminium sheet is cleaned, and treatment process is quick, and cleaning is completed to dry.
(3) present invention is handled leachate by hydrogen peroxide, organic matter therein is aoxidized, so that electrolytic manganese anode mud
Electrolyte COD concentration generated is leached between 60-160mg/L, manganese electrolytic process is caused to reduce organic substance residues
It influences, improves the efficiency and quality of electrolytic manganese metal.
(4) manganese electrolyte production electrolysis manganese product generated is leached with electrolytic manganese anode mud, ton product power consumption is about
6200kwh/t, energy consumption are greatly reduced, remarkable in economical benefits.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited to following reality
Apply example.
Embodiment 1
A kind of method that electrolytic manganese anode mud separation produces electrolytic manganese metal and recycles lead, comprising the following steps:
S1. electrolytic manganese anode mud and 3.5molL-1Sulfuric acid solution mixing, and 70 gL are added-1Blackstrap aqueous solution
Stirring, the dosage of blackstrap are the 90% of reducing agent theoretical amount, 200 rmin of stirring rate-1, above-mentioned electrolytic manganese anode mud,
In the mixture of sulfuric acid solution and blackstrap aqueous solution, liquid-solid ratio 4: 1, keeping the temperature of mixture is 70 DEG C, reaction
40min, is then added iron powder, and the dosage of iron powder is greater than the theoretical amount of remaining reducing agent, reacts 15min, use after the reaction was completed
Filter press separates leachate and leached mud；
S2. H is added in leachate2O2, oxidizing condition are as follows: ρ (H2O2)/ρ (COD)=2.5, control reaction temperature are 50 DEG C, instead
It is 2h between seasonable, the leachate of COD must be removed；
S3. Sodium Dimethyldithiocarbamate is added in the leachate for removing COD, and it is 5.5 ~ 6.0 that ammonium hydroxide, which is added, to adjust the pH of leachate, reaction
Temperature is 50 DEG C, removes removing heavy metals, obtains purification of manganese sulfate liquid, and the electrolysis of purification of manganese sulfate liquid obtains metal manganese product.
To recycle to lead, leached mud takes out after cleaning in filter press to be dried, and obtains lead concentrate product.
Embodiment 2
A kind of method that electrolytic manganese anode mud separation produces electrolytic manganese metal and recycles lead, comprising the following steps:
S1. electrolytic manganese anode mud and 3.5molL-1Sulfuric acid solution mixing, and 65 gL are added-1Blackstrap aqueous solution
Stirring, the dosage of blackstrap are the 90% of reducing agent theoretical amount, 150 rmin of stirring rate-1, above-mentioned electrolytic manganese anode mud,
In the mixture of sulfuric acid solution and blackstrap aqueous solution, liquid-solid ratio 4.2: 1, keeping the temperature of mixture is 75 DEG C, reaction
50min, is then added iron powder, and the dosage of iron powder is greater than the theoretical amount of remaining reducing agent, reacts 10min, use after the reaction was completed
Filter press separates leachate and leached mud；
S2. H is added in leachate2O2, oxidizing condition are as follows: ρ (H2O2)/ρ (COD)=2, control reaction temperature are 48 DEG C, reaction
Time is 2h, must remove the leachate of COD；
S3. ammonium sulfide is added in the leachate for removing COD, and it is 5.5 ~ 6.0 that ammonium hydroxide, which is added, to adjust the pH of leachate, reaction
Temperature is 45 DEG C, removes removing heavy metals, obtains purification of manganese sulfate liquid, and the electrolysis of purification of manganese sulfate liquid obtains metal manganese product.
To recycle to lead, leached mud takes out after cleaning in filter press to be dried, and obtains lead concentrate product.
Embodiment 3
A kind of method that electrolytic manganese anode mud separation produces electrolytic manganese metal and recycles lead, comprising the following steps:
S1. electrolytic manganese anode mud and 3.5molL-1Sulfuric acid solution mixing, and 70 gL are added-1Blackstrap aqueous solution
Stirring, the dosage of blackstrap are the 85% of reducing agent theoretical amount, 250 rmin of stirring rate-1, above-mentioned electrolytic manganese anode mud,
In the mixture of sulfuric acid solution and blackstrap aqueous solution, liquid-solid ratio 3.8: 1, keeping the temperature of mixture is 80 DEG C, reaction
30min, is then added iron powder, and the dosage of iron powder is greater than the theoretical amount of remaining reducing agent, reacts 20min, use after the reaction was completed
Filter press separates leachate and leached mud, and leached mud takes out after cleaning in filter press to be dried, and lead concentrate product is obtained；
S2. H is added in leachate2O2, oxidizing condition are as follows: ρ (H2O2)/ρ (COD)=2.5, control reaction temperature are 52 DEG C, instead
It is 2h between seasonable, the leachate of COD must be removed；
S3. ammonium sulfide or Sodium Dimethyldithiocarbamate is added in the leachate for removing COD, and the pH that ammonium hydroxide adjusting leachate is added is
5.5 ~ 6.0, reaction temperature is 55 DEG C, removes removing heavy metals, obtains purification of manganese sulfate liquid, and the electrolysis of purification of manganese sulfate liquid obtains manganese metal production
Product.
To recycle to lead, leached mud takes out after cleaning in filter press to be dried, and obtains lead concentrate product.
Table 1
Claims (1)
1. a kind of method that electrolytic manganese anode mud separation produces electrolytic manganese metal and recycles lead, it is characterised in that including following step
It is rapid:
S1. electrolytic manganese anode mud and 3.5molL-1Sulfuric acid solution mixing, and 70 gL are added-1The stirring of blackstrap aqueous solution,
The dosage of blackstrap is the 85 ~ 90% of reducing agent theoretical amount, 190 ~ 210 rmin of stirring rate-1, above-mentioned electrolytic manganese anode
In the mixture of mud, sulfuric acid solution and blackstrap aqueous solution, liquid-solid ratio 4: 1, keeping the temperature of mixture is 70 DEG C, reaction 30
Then iron powder is added in ~ 50min, the dosage of iron powder is greater than the theoretical amount of remaining reducing agent, reacts 10 ~ 20min, and reaction is completed
Leachate and leached mud are separated with filter press afterwards；Leached mud takes out after cleaning in filter press to be dried, and lead concentrate product is obtained；
S2. H is added in leachate2O2, oxidizing condition are as follows: ρ (H2O2)/ρ (COD)=2.5, control reaction temperature are 50 DEG C, the reaction time
For 2 ~ 2.5h, the leachate of COD must be removed；
S3. ammonium sulfide or Sodium Dimethyldithiocarbamate is added in the leachate that COD will be removed, and be added ammonium hydroxide adjust the pH of leachate be 5.5 ~
6.0, the temperature of reaction is 45 ~ 55 DEG C, removes removing heavy metals, obtains purification of manganese sulfate liquid, and the electrolysis of purification of manganese sulfate liquid obtains manganese metal production
Product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023046725A1 (en) * | 2021-09-22 | 2023-03-30 | Eramet | Metallic manganese production from ore without co2 emission |
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| CN110408786A (en) * | 2019-08-29 | 2019-11-05 | 贵州大学 | A kind of method that the catalysis of electrolytic manganese anode slag prepares manganese sulfate solution and recycles lead |
| CN112795773B (en) * | 2020-12-18 | 2022-10-14 | 南方锰业集团有限责任公司大新锰矿分公司 | Method for removing Ca and Mg in electrolytic manganese metal anode mud |
| CN112553468B (en) * | 2020-12-18 | 2022-08-23 | 南方锰业集团有限责任公司 | Method for producing high-purity manganese sulfate by adopting metal manganese anode mud |
| CN112607782B (en) * | 2020-12-18 | 2022-10-14 | 南方锰业集团有限责任公司 | Method for preparing battery-grade high-purity manganese sulfate by using metal manganese anode slime |
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| CN115724470B (en) * | 2022-09-26 | 2024-05-07 | 广西科技师范学院 | Purification method of manganese sulfate solution |
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| JPS61143527A (en) * | 1984-12-14 | 1986-07-01 | Kurita Water Ind Ltd | Treatment of metal-containing water |
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| WO2023046725A1 (en) * | 2021-09-22 | 2023-03-30 | Eramet | Metallic manganese production from ore without co2 emission |
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Address after: 532200 Shilin Road, Chongzuo City, Guangxi Zhuang Autonomous Region Patentee after: Nanfang Manganese Industry Group Co.,Ltd. Address before: 532200 Shilin Road, Chongzuo City, Guangxi Zhuang Autonomous Region Patentee before: CITIC DAMENG MINING INDUSTRIES Ltd. |
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