CN107287430A - A kind of method for extracting manganese in electrolytic manganese residues and the method for handling electrolytic manganese residues - Google Patents
A kind of method for extracting manganese in electrolytic manganese residues and the method for handling electrolytic manganese residues Download PDFInfo
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- CN107287430A CN107287430A CN201710755519.4A CN201710755519A CN107287430A CN 107287430 A CN107287430 A CN 107287430A CN 201710755519 A CN201710755519 A CN 201710755519A CN 107287430 A CN107287430 A CN 107287430A
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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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- 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 extracting manganese in electrolytic manganese residues and the method for handling electrolytic manganese residues, are related to solid waste and utilize field.A kind of method for extracting manganese in electrolytic manganese residues, step 1：Electrolytic manganese residues are pressed into liquid-solid ratio 1~8:1mL/g sizes mixing with sulfuric acid solution, is placed in microwave ultrasonic wave reactor, and stirring, leaching, are isolated to leachate containing manganese and leached mud under conditions of air, temperature is blasted for 25~60 DEG C.Step 2：Dry powder is added to adjust solution ph to 57, the separation of solid and liquid after stirring, 10~60min of precipitation under conditions of temperature is 25~50 DEG C in the leachate containing manganese that step 1 is obtained.This method technique is simple, and using microwave and ultrasound collective effect in slurry, the leaching rate of manganese in electrolytic manganese residues is high.A kind of method for handling electrolytic manganese residues, includes the method for above-mentioned extraction manganese in electrolytic manganese residues.This method can carry out effective recycling to electrolytic manganese residues.
Description
Technical field
Field, and more particularly to a kind of method for extracting manganese in electrolytic manganese residues and place are utilized the present invention relates to solid waste
The method for managing electrolytic manganese residues.
Background technology
Electrolytic manganese industry, as typical hydrometallurgy industry, is typical high energy consumption, high pollution, a maximum discharge
" three high " industry, it has also triggered the serious environment such as waste water, waste residue dirty while various regions rapid economic development is promoted
A large amount of stackings of dye problem, wherein electrolytic manganese residues are especially prominent with polluting.China is produced with disappearing as manganese metal the biggest in the world
It is about 3% to remain total manganese amount in Fei Guo, national electrolytic manganese industry manganese slag newly-increased 10,000,000 tons or so every year, manganese slag.Therefore, it is
Waste of resource to the manganese of electrolytic manganese residues, it is necessary to do not recycle.
But, electrolytic manganese residues particle in long-term stacking process gradually condenses into hard bulk, soluble bivalent manganese by
Value Mn is gradually oxidized to, thing containing manganese is wrapped up by gangue minerals such as silica, calcium sulphate dihydrates, causes traditional leaching method
It is difficult to which the manganese element in electrolytic manganese residues is leached.
Some auxiliary agents are added in the method that also some manganese in electrolytic manganese residues are reclaimed so that cost increase, and to subsequent treatment
It is unfavorable, it additionally there are the relatively low shortcoming of complex process, leaching rate.
The content of the invention
It is an object of the invention to provide a kind of method for extracting manganese in electrolytic manganese residues, this method technique is simple, electrolytic manganese
The leaching rate of manganese is high in slag.
Another object of the present invention is to provide a kind of method for handling electrolytic manganese residues, this method can be entered to electrolytic manganese residues
Row is effective to be recycled.
The present invention is solved its technical problem and realized using following technical scheme.
A kind of method for extracting manganese in electrolytic manganese residues, including：
Step 1：Electrolytic manganese residues are pressed into liquid-solid ratio 1~8:1mL/g sizes mixing with sulfuric acid solution, is placed in microwave-ultrasonic reaction
In kettle, stirring, leaching, are isolated to leachate containing manganese and leached mud under conditions of air, temperature is blasted for 25~60 DEG C；
Step 2：In the leachate containing manganese that step 1 is obtained plus dry powder adjusts solution ph to 5-7, temperature be 25~
Stirred under conditions of 50 DEG C, precipitate separation of solid and liquid after 10~60min.
A kind of method for handling electrolytic manganese residues, includes the method for above-mentioned extraction manganese in electrolytic manganese residues.
The beneficial effect of the embodiment of the present invention is：Present invention introduces microwave technology, selectivity of the manganese-bearing mineral by microwave
And quick heating, larger temperature difference is produced between gangue and thermal stress is formed, small split is produced at the edge of mineral therewith
Seam, causes the surface nature of mineral, internal structure to be changed, so as to improve leaching performance.
The present invention utilizes the cavitation of ultrasonic wave under conditions of air is blasted, and can make the solid floated on a liquid
Surface is enhanced Leach reaction process, improves leaching effect by destruction drastically, while leaching process can be made by being passed through air
The Fe of generation2+It is oxidized to Fe3+, reach the effect killed two birds with one stone.
The present invention advantageously reduces production cost and simplifies subsequent treatment process without nitration mixture and other auxiliary agents.
The present invention combines the technology of ultrasonic wave and two kinds of efficient greens of microwave, is that Leach reaction creates more favorable heat
Mechanics and dynamic conditions, realize the efficient Rapid Leaching of manganese in manganese slag, with leaching velocity it is fast, environment-friendly, processing when
Between short, low power consumption and other advantages.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be attached to what is used required in embodiment
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, therefore is not construed as pair
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 is the process chart of the specific embodiment of the invention.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional production that can be obtained by commercially available purchase
Product.
A kind of method of extraction manganese in electrolytic manganese residues and the method for processing electrolytic manganese residues to the embodiment of the present invention are entered below
Row is illustrated.
A kind of method for extracting manganese in electrolytic manganese residues, including：
Step 1：Electrolytic manganese residues are pressed into liquid-solid ratio 1~8:1mL/g sizes mixing with sulfuric acid solution, is placed in microwave-ultrasonic reaction
Kettle is carried out in microwave, ultrasonication simultaneously, to blast air, temperature be 25~60 DEG C, mixing speed is 100-600rpm's
Under the conditions of, leach 5~30min, be isolated to leachate containing manganese and leached mud.
Wherein, the main component of electrolytic manganese residues includes：Si 9-17wt%, S 8-14wt%, Ca6-11wt%, Al 3-
8wt%, Fe 2-6wt% and Mn 1-5wt%.
In an embodiment of the present invention, the ultrasound working frequency in step 1 is 20~40kHz, and ultrasonic power is every
Kilogram 50~250Wh of slurry.Microwave frequency is 2.45GHz, and microwave power is 40~200Wh of per kilogram slurry.Need explanation
It is that in other embodiments, microwave frequency is alternatively other scopes.In addition, in the present embodiment, microwave-ultrasonic reactor
Microwave and ultrasound generating means is as installed in a kettle., microwave can be carried out simultaneously in microwave-ultrasonic reactor
And ultrasonication.
Further, granularity≤150 μm of electrolytic manganese residues.The electrolytic manganese residues of this particle size range have larger with sulfuric acid solution
Contact area, in the presence of microwave and ultrasonic wave, is conducive to valuable mineral to be dissociated with gangue so that sulfuric acid solution and useful ore deposit
Reaction between thing is more abundant, improves the leaching rate of manganese in electrolytic manganese residues.
Further, the volumetric concentration of sulfuric acid solution is 5~20%.
In addition, in an embodiment of the present invention, air is blasted using batch (-type) in step 1, throughput is 0.5~5m3/h。
Step 2：In the leachate containing manganese that step 1 is obtained plus dry powder adjusts solution ph to 5-7, temperature be 25~
50 DEG C, mixing speed be 10~50rmp under the conditions of, obtain more pure containing manganese leaching after 10~60min of precipitation after separation of solid and liquid
Go out liquid.Leaching rate >=90% of the manganese finally obtained.
A kind of method for handling electrolytic manganese residues, includes the method for above-mentioned extraction manganese in electrolytic manganese residues.This method can be right
Electrolytic manganese residues are effectively recycled.
With reference to embodiment, the invention will be further described.
Embodiment 1
It is Si 14.2%, S 10.3%, Ca 12.6%, Al 3.8%, Fe4.1%, Mn first by main component
4.9% electrolytic manganese residues obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid-solid ratio 8:1mL/g and volume
The sulfuric acid solution of concentration 5% is sized mixing, and is placed in microwave-ultrasonic reactor.In microwave frequency 2.45GHz, microwave power 400W, surpass
Frequency of sound wave 20kHz, ultrasonic power 60W, blast air mass flow for 0.5m3/ h, temperature are 25 DEG C, mixing speed is 100rpm
Under the conditions of leach 30min, be isolated to leachate containing manganese and leached mud.
Then in leachate containing manganese plus dry powder adjusts solution ph to 5, temperature is 25 DEG C, mechanical agitation speed is
Separation of solid and liquid after 10rpm, precipitation 10min, obtains more pure leachate containing manganese.
Embodiment 2
It is Si 14.8%, S 10.2%, Ca 9.8%, Al 4.4%, Fe4.6%, Mn 2.9% first by main component
Electrolytic manganese residues obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid-solid ratio 1:1mL/g and volumetric concentration
20% sulfuric acid solution is sized mixing, and is placed in microwave-ultrasonic reactor.In microwave frequency 2.45GHz, microwave power 100W, ultrasound
Wave frequency rate 20kHz, ultrasonic power 150W, blast air mass flow for 5m3/ h, temperature are 25 DEG C, mixing speed is 600rpm bars
5min is leached under part, leachate containing manganese and leached mud is isolated to.
Then in leachate containing manganese plus dry powder adjusts solution ph to 7, temperature is 25 DEG C, mechanical agitation speed is
Separation of solid and liquid after 50rpm, precipitation 60min, obtains more pure leachate containing manganese.
Embodiment 3
It is Si 16.1%, S 13.2%, Ca 8.5%, Al 4.5%, Fe4.9%, Mn 2.6% first by main component
Electrolytic manganese residues obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid-solid ratio 4:1mL/g and volumetric concentration
10% sulfuric acid solution is sized mixing, and is placed in microwave-ultrasonic reactor.In microwave frequency 2.45GHz, microwave power 200W, ultrasound
Wave frequency rate 40kHz, ultrasonic power 100W, blast air mass flow for 2m3/ h, temperature are 60 DEG C, mixing speed is 300rpm bars
15min is leached under part, leachate containing manganese and leached mud is isolated to.
Then in leachate containing manganese plus dry powder adjusts solution ph to 6, temperature is 25 DEG C, mechanical agitation speed is
Separation of solid and liquid after 20rpm, precipitation 30min, obtains more pure leachate containing manganese.
Embodiment 4
It is Si 15.3wt%, S 12.5wt%, Ca 8.9wt%, Al3.2wt%, Fe first by main component
3.4wt% and Mn 3.6wt% electrolytic manganese residues obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid
Admittedly than 2:1mL/g sizes mixing with the sulfuric acid solution of volumetric concentration 10%, is placed in microwave-ultrasonic reactor.In microwave frequency
2.45GHz, microwave power 60W, ultrasonic frequency 30kHz, ultrasonic power 75W, blast air mass flow for 1m3/ h, temperature are
45 DEG C, mixing speed be 500rpm under the conditions of leach 10min, be isolated to leachate containing manganese and leached mud.
Then in leachate containing manganese plus dry powder adjusts solution ph to 6, temperature is 30 DEG C, mechanical agitation speed is
Separation of solid and liquid after 20rpm, precipitation 30min, obtains more pure leachate containing manganese.
Embodiment 5
It is Si 12.5wt%, S 11.6wt%, Ca 7.8wt%, Al5.8wt%, Fe first by main component
4.2wt% and Mn 2.9wt% electrolytic manganese residues obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid
Admittedly than 3:1mL/g sizes mixing with the sulfuric acid solution of volumetric concentration 10%, is placed in microwave-ultrasonic reactor.In microwave frequency
2.45GHz, microwave power 150W, ultrasonic frequency 30kHz, ultrasonic power 200W, blast air mass flow for 4m3/ h, temperature
It is to leach 20min under the conditions of 200rpm for 30 DEG C, mixing speed, is isolated to leachate containing manganese and leached mud.
Then in leachate containing manganese plus dry powder adjusts solution ph to 5, temperature is 50 DEG C, mechanical agitation speed is
Separation of solid and liquid after 20rpm, precipitation 20min, obtains more pure leachate containing manganese.
Embodiment 6
It is Si 11.5wt%, S 10.6wt%, Ca 8.5wt%, Al5.2wt%, Fe first by main component
3.4wt% and Mn 4.2wt% electrolytic manganese residues obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid
Admittedly than 5:1mL/g sizes mixing with the sulfuric acid solution of volumetric concentration 18%, is placed in microwave-ultrasonic reactor.In microwave frequency
2.45GHz, microwave power 240W, ultrasonic frequency 30kHz, ultrasonic power 300W, blast air mass flow for 4m3/ h, temperature
It is to leach 20min under the conditions of 200rpm for 30 DEG C, mixing speed, is isolated to leachate containing manganese and leached mud.
Then in leachate containing manganese plus dry powder adjusts solution ph to 7, temperature is 40 DEG C, mechanical agitation speed is
Separation of solid and liquid after 30rpm, precipitation 50min, obtains more pure leachate containing manganese.
Embodiment 7
It is Si 15.3wt%, S 9.7wt%, Ca 7.9wt%, Al3.6wt%, Fe 4.1wt% first by main component
And Mn 3.2wt% electrolytic manganese residues obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid-solid ratio 6:
1mL/g sizes mixing with the sulfuric acid solution of volumetric concentration 15%, is placed in microwave-ultrasonic reactor.It is micro- in microwave frequency 2.45GHz
Wave power 230W, ultrasonic frequency 30kHz, ultrasonic power 200W, blast air mass flow for 2.5m3/ h, temperature are 50 DEG C, stirred
Speed is mixed to leach 15min under the conditions of 600rpm, leachate containing manganese and leached mud is isolated to.
Then in leachate containing manganese plus dry powder adjusts solution ph to 7, temperature is 30 DEG C, mechanical agitation speed is
Separation of solid and liquid after 40rpm, precipitation 40min, obtains more pure leachate containing manganese.
Test example
Manganese leaching rate is tested：To being extracted in the extracting method step 2 of embodiment 1-7 manganese in electrolytic manganese residues containing manganese leaching
The content for going out the manganese that liquid is leached using atomic absorption spectroscopy determination is M1, the manganese content in electrolytic manganese residues is M0,Embodiment 1-7 manganese leaching rate is recorded in table 1.
The embodiment 1-7 of table 1 manganese leaching rate
It can be seen from the result of table 1 embodiment 1-7 manganese leaching rate >=90%.Illustrate by present invention implementation
The extracting method of the manganese in electrolytic manganese residues of example can obtain higher manganese leaching rate.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of method for extracting manganese in electrolytic manganese residues, it is characterised in that including：
Step 1：Electrolytic manganese residues are pressed into liquid-solid ratio 1~8:1mL/g sizes mixing with sulfuric acid solution, is placed in microwave-ultrasonic reactor,
Stirring, leaching, are isolated to leachate containing manganese and leached mud under conditions of air, temperature is blasted for 25~60 DEG C；
Step 2：In leachate containing manganese described in being obtained in step 1 plus dry powder adjusts solution ph to 5-7, temperature be 25~
Stirred under conditions of 50 DEG C, precipitate separation of solid and liquid after 10~60min.
2. the method according to claim 1 for extracting manganese in electrolytic manganese residues, it is characterised in that the volume of the sulfuric acid solution
Concentration is 5~20%.
3. the method according to claim 1 for extracting manganese in electrolytic manganese residues, it is characterised in that the ultrasound in the step 1
Ripple working frequency is 20~40kHz, and ultrasonic power is 50~250Wh of per kilogram slurry.
4. the method according to claim 1 for extracting manganese in electrolytic manganese residues, it is characterised in that microwave frequency is 2.45GHz,
Microwave power is 40~200Wh of per kilogram slurry.
5. the method according to claim 1 for extracting manganese in electrolytic manganese residues, it is characterised in that between being used in the step 1
The formula of having a rest blasts air, and throughput is 0.5~5m3/h。
6. the method according to claim 1 for extracting manganese in electrolytic manganese residues, it is characterised in that the stirring in the step 1
Speed is 100-600rpm, and extraction time is 5~30min.
7. the method according to claim 1 for extracting manganese in electrolytic manganese residues, it is characterised in that the stirring in the step 2
Speed is 10~50rmp.
8. the method according to claim 1 for extracting manganese in electrolytic manganese residues, it is characterised in that the grain of described electrolytic manganese residues
≤ 150 μm of degree.
9. the method according to claim 1 for extracting manganese in electrolytic manganese residues, it is characterised in that：Solid-liquid point in the step 2
Leaching rate >=90% of manganese from after.
10. a kind of method for handling electrolytic manganese residues, it is characterised in that including the extraction electrolysis described in claim any one of 1-9
The method of manganese in manganese slag.
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Cited By (5)
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| CN108754151A (en) * | 2018-06-23 | 2018-11-06 | 铜仁学院 | A kind of leaching method of manganese in electrolytic manganese residues |
| CN109762994A (en) * | 2019-03-27 | 2019-05-17 | 贵州省过程工业技术研究中心 | A kind of processing electrolytic manganese residues dry powder and processing electrolytic manganese residues method |
| CN110479207A (en) * | 2019-07-26 | 2019-11-22 | 铜仁学院 | A kind of method that the alkali fusion activation of electrolytic manganese residues microwave prepares high adsorption value fluorite |
| CN111111854A (en) * | 2019-12-30 | 2020-05-08 | 铜仁学院 | Manganese ore industrialization wet ball milling method based on electrolytic manganese metal system backwater |
| CN113121127A (en) * | 2021-04-21 | 2021-07-16 | 昆明学院 | Manganese slag solid waste recycling treatment method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754151A (en) * | 2018-06-23 | 2018-11-06 | 铜仁学院 | A kind of leaching method of manganese in electrolytic manganese residues |
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| CN110479207A (en) * | 2019-07-26 | 2019-11-22 | 铜仁学院 | A kind of method that the alkali fusion activation of electrolytic manganese residues microwave prepares high adsorption value fluorite |
| CN111111854A (en) * | 2019-12-30 | 2020-05-08 | 铜仁学院 | Manganese ore industrialization wet ball milling method based on electrolytic manganese metal system backwater |
| CN113121127A (en) * | 2021-04-21 | 2021-07-16 | 昆明学院 | Manganese slag solid waste recycling treatment method and application thereof |
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| CN107287430B (en) | 2018-09-21 |
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