CN107287430B - 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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- CN107287430B CN107287430B CN201710755519.4A CN201710755519A CN107287430B CN 107287430 B CN107287430 B CN 107287430B CN 201710755519 A CN201710755519 A CN 201710755519A CN 107287430 B CN107287430 B CN 107287430B
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- manganese
- electrolytic manganese
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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
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 method of extraction 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 reaction kettle, and stirring, leaching, are isolated to leachate containing manganese and leached mud under conditions of blasting air, temperature is 25~60 DEG C.Step 2：In the leachate containing manganese that step 1 obtains plus dry powder adjusts solution ph to 57, is separated by solid-liquid separation after stirring, 10~60min of precipitation under conditions of temperature is 25~50 DEG C.This method is simple for process, and using microwave and ultrasound collective effect in slurry, the leaching rate of manganese in electrolytic manganese residues is high.A method of processing electrolytic manganese residues include the method for above-mentioned extraction manganese in electrolytic manganese residues.This method can effectively recycle electrolytic manganese residues.
Description
Technical field
The present invention relates to solid waste to utilize field, and the method for more particularly to a kind of extraction manganese in electrolytic manganese residues and place
The method for managing electrolytic manganese residues.
Background technology
Electrolytic manganese industry is typical high energy consumption, high pollution, a maximum discharge as typical hydrometallurgy industry
" three high " industry, it is dirty that it has also caused the serious environment such as waste water, waste residue while promoting various regions rapid economic development
Dye problem, a large amount of stackings and pollution of wherein electrolytic manganese residues are especially prominent.China produces and disappears as the world's largest manganese metal
Fei Guo, national electrolytic manganese industry increase 10,000,000 tons or so of manganese slag newly every year, and it is about 3% to remain total manganese amount in manganese slag.Therefore, it is
Not waste of resource, needs to be recycled the manganese of electrolytic manganese residues.
But electrolytic manganese residues particle in long-term stacking process gradually condenses into hard bulk, soluble bivalent manganese by
It is gradually oxidized to value Mn, object containing manganese is mutually wrapped up by gangue minerals such as silica, calcium sulphate dihydrates, causes traditional leaching method
It is difficult to leach the manganese element in electrolytic manganese residues.
Also adding some auxiliary agents in the method for some manganese in electrolytic manganese residues recycling makes cost increase, and to subsequent processing
Unfavorable, additionally there are the relatively low disadvantages of complex process, leaching rate.
Invention content
The purpose of the present invention is to provide a kind of methods of extraction manganese in electrolytic manganese residues, and this method is simple for process, electrolytic manganese
The leaching rate of manganese is high in slag.
Another object of the present invention is to provide it is a kind of processing electrolytic manganese residues method, this method can to electrolytic manganese residues into
Row is effective to be recycled.
The present invention solves its technical problem using following technical scheme to realize.
A method of extraction 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 blasting air, temperature is 25~60 DEG C；
Step 2：In the leachate containing manganese that step 1 obtains plus dry powder adjusts solution ph to 5-7, temperature be 25~
It stirs under conditions of 50 DEG C, be separated by solid-liquid separation after 10~60min of precipitation.
A method of processing electrolytic manganese residues include the method for above-mentioned extraction manganese in electrolytic manganese residues.
The advantageous effect of the embodiment of the present invention is：Present invention introduces microwave technology, manganese-bearing mineral by microwave selectivity
And quickly heating, larger temperature difference is generated between gangue and forms thermal stress, generates small split at the edge of mineral therewith
Seam, causes the surface nature of mineral, internal structure to be changed, to improve leaching performance.
The present invention utilizes the cavitation of ultrasonic wave under conditions of blasting air, can make the solid to float on a liquid
Surface is enhanced Leach reaction process by destruction drastically, improves leaching effect, while being passed through air and can make leaching process
The Fe of generation2+It is oxidized to Fe3+, achieve the effect that kill two birds with one stone.
The present invention does not add nitration mixture and other auxiliary agents, advantageously reduces production cost and simplifies subsequent processing process.
The technology of present invention combination ultrasonic wave and two kinds of efficient greens of microwave creates more favorable heat for Leach reaction
Mechanics and dynamic conditions realize the efficient Rapid Leaching of manganese in manganese slag, have leaching velocity it is fast, it is environmental-friendly, processing when
Between short, low power consumption and other advantages.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the process flow chart of the specific embodiment of the invention.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below the method to a kind of extraction manganese in electrolytic manganese residues of the embodiment of the present invention and handle electrolytic manganese residues method into
Row illustrates.
A method of extraction 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 at the same time in microwave, ultrasonication, blast air, temperature is 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.It needs to illustrate
It is that in other embodiments, microwave frequency is alternatively other ranges.In addition, in the present embodiment, microwave-ultrasonic reaction kettle
Microwave and ultrasound generating means is as installed in a kettle, microwave can be carried out at the same time in microwave-ultrasonic reaction kettle
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 is conducive to valuable mineral and is dissociated with gangue so that sulfuric acid solution and useful mine under the action of microwave and ultrasonic wave
Reaction between object 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, blasting air using intermittent in step 1, ventilatory capacity is 0.5~5m3/h。
Step 2：In the leachate containing manganese that step 1 obtains plus dry powder adjusts solution ph to 5-7, temperature be 25~
50 DEG C, mixing speed be 10~50rmp under the conditions of, be separated by solid-liquid separation after 10~60min of precipitation after obtain more pure soaking containing manganese
Go out liquid.Leaching rate >=90% of the manganese finally obtained.
A method of processing electrolytic manganese residues include 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 first Si 14.2%, S 10.3%, Ca 12.6%, Al 3.8%, Fe4.1%, Mn 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
5% sulfuric acid solution of concentration is sized mixing, and is placed in microwave-ultrasonic reaction kettle.In microwave frequency 2.45GHz, microwave power 400W, surpass
Frequency of sound wave 20kHz, ultrasonic power 60W, it is 0.5m to blast air mass flow3/ h, temperature be 25 DEG C, mixing speed 100rpm
Under the conditions of leach 30min, be isolated to leachate containing manganese and leached mud.
Then dry powder is added to adjust solution ph to 5 in leachate containing manganese, temperature is 25 DEG C, mechanical agitation speed is
10rpm is separated by solid-liquid separation after precipitating 10min, obtains more pure leachate containing manganese.
Embodiment 2
It is first Si 14.8%, S 10.2%, Ca 9.8%, Al 4.4%, Fe4.6%, Mn 2.9% by main component
Electrolytic manganese residues through grind screening obtain≤150 μm of granulated slag, 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 reaction kettle.In microwave frequency 2.45GHz, microwave power 100W, ultrasound
Wave frequency rate 20kHz, ultrasonic power 150W, it is 5m to blast air mass flow3/ h, temperature are 25 DEG C, mixing speed is 600rpm items
5min is leached under part, is isolated to leachate containing manganese and leached mud.
Then dry powder is added to adjust solution ph to 7 in leachate containing manganese, temperature is 25 DEG C, mechanical agitation speed is
50rpm is separated by solid-liquid separation after precipitating 60min, obtains more pure leachate containing manganese.
Embodiment 3
It is first Si 16.1%, S 13.2%, Ca 8.5%, Al 4.5%, Fe4.9%, Mn 2.6% by main component
Electrolytic manganese residues through grind screening obtain≤150 μm of granulated slag, 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 reaction kettle.In microwave frequency 2.45GHz, microwave power 200W, ultrasound
Wave frequency rate 40kHz, ultrasonic power 100W, it is 2m to blast air mass flow3/ h, temperature are 60 DEG C, mixing speed is 300rpm items
15min is leached under part, is isolated to leachate containing manganese and leached mud.
Then dry powder is added to adjust solution ph to 6 in leachate containing manganese, temperature is 25 DEG C, mechanical agitation speed is
20rpm is separated by solid-liquid separation after precipitating 30min, obtains more pure leachate containing manganese.
Embodiment 4
It is first Si 15.3wt%, S 12.5wt%, Ca 8.9wt%, Al3.2wt%, Fe by main component
The electrolytic manganese residues of 3.4wt% and Mn 3.6wt% obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid
Admittedly than 2:1mL/g sizes mixing with 10% sulfuric acid solution of volumetric concentration, is placed in microwave-ultrasonic reaction kettle.In microwave frequency
2.45GHz, microwave power 60W, ultrasonic frequency 30kHz, ultrasonic power 75W, it is 1m to blast air mass flow3/ 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 dry powder is added to adjust solution ph to 6 in leachate containing manganese, temperature is 30 DEG C, mechanical agitation speed is
20rpm is separated by solid-liquid separation after precipitating 30min, obtains more pure leachate containing manganese.
Embodiment 5
It is first Si 12.5wt%, S 11.6wt%, Ca 7.8wt%, Al5.8wt%, Fe by main component
The electrolytic manganese residues of 4.2wt% and Mn 2.9wt% obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid
Admittedly than 3:1mL/g sizes mixing with 10% sulfuric acid solution of volumetric concentration, is placed in microwave-ultrasonic reaction kettle.In microwave frequency
2.45GHz, microwave power 150W, ultrasonic frequency 30kHz, ultrasonic power 200W, it is 4m to blast air mass flow3/ h, temperature
20min is leached under the conditions of being 200rpm for 30 DEG C, mixing speed, is isolated to leachate containing manganese and leached mud.
Then dry powder is added to adjust solution ph to 5 in leachate containing manganese, temperature is 50 DEG C, mechanical agitation speed is
20rpm is separated by solid-liquid separation after precipitating 20min, obtains more pure leachate containing manganese.
Embodiment 6
It is first Si 11.5wt%, S 10.6wt%, Ca 8.5wt%, Al5.2wt%, Fe by main component
The electrolytic manganese residues of 3.4wt% and Mn 4.2wt% obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid
Admittedly than 5:1mL/g sizes mixing with 18% sulfuric acid solution of volumetric concentration, is placed in microwave-ultrasonic reaction kettle.In microwave frequency
2.45GHz, microwave power 240W, ultrasonic frequency 30kHz, ultrasonic power 300W, it is 4m to blast air mass flow3/ h, temperature
20min is leached under the conditions of being 200rpm for 30 DEG C, mixing speed, is isolated to leachate containing manganese and leached mud.
Then dry powder is added to adjust solution ph to 7 in leachate containing manganese, temperature is 40 DEG C, mechanical agitation speed is
30rpm is separated by solid-liquid separation after precipitating 50min, obtains more pure leachate containing manganese.
Embodiment 7
It is first Si 15.3wt%, S 9.7wt%, Ca 7.9wt%, Al3.6wt%, Fe 4.1wt% by main component
And the electrolytic manganese residues of Mn 3.2wt% obtain≤150 μm of granulated slag through grinding screening, 500g samples are weighed, by liquid-solid ratio 6:
1mL/g sizes mixing with 15% sulfuric acid solution of volumetric concentration, is placed in microwave-ultrasonic reaction kettle.It is micro- in microwave frequency 2.45GHz
Wave power 230W, ultrasonic frequency 30kHz, ultrasonic power 200W, it is 2.5m to blast air mass flow3/ h, temperature are 50 DEG C, stir
It mixes under the conditions of speed is 600rpm and leaches 15min, be isolated to leachate containing manganese and leached mud.
Then dry powder is added to adjust solution ph to 7 in leachate containing manganese, temperature is 30 DEG C, mechanical agitation speed is
40rpm is separated by solid-liquid separation after precipitating 40min, obtains more pure leachate containing manganese.
Test example
Manganese leaching rate is tested：It is soaked containing manganese to being extracted in the extracting method step 2 of the manganese in electrolytic manganese residues of embodiment 1-7
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,The manganese leaching rate of embodiment 1-7 is recorded in table 1.
The manganese leaching rate of 1 embodiment 1-7 of table
It can be seen from the result of table 1 embodiment 1-7 manganese leaching rate >=90%.It illustrates to implement through the invention
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 the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of method of extraction manganese in electrolytic manganese residues, which is characterized 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 reaction kettle,
Stirring, leaching, are isolated to leachate containing manganese and leached mud under conditions of blasting air, temperature is 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~
It stirs under conditions of 50 DEG C, be separated by solid-liquid separation after 10~60min of precipitation.
2. the method for extraction manganese in electrolytic manganese residues according to claim 1, which is characterized in that the volume of the sulfuric acid solution
A concentration of 5~20%.
3. the method for extraction manganese in electrolytic manganese residues according to claim 1, which is characterized in that the ultrasound in the step 1
Wave working frequency is 20~40kHz, and ultrasonic power is 50~250Wh of per kilogram slurry.
4. the method for extraction manganese in electrolytic manganese residues according to claim 1, which is characterized in that microwave frequency 2.45GHz,
Microwave power is 40~200Wh of per kilogram slurry.
5. the method for extraction manganese in electrolytic manganese residues according to claim 1, which is characterized in that between being used in the step 1
The formula of having a rest blasts air, and ventilatory capacity is 0.5~5m3/h。
6. the method for extraction manganese in electrolytic manganese residues according to claim 1, which is characterized in that the stirring in the step 1
Speed is 100-600rpm, and extraction time is 5~30min.
7. the method for extraction manganese in electrolytic manganese residues according to claim 1, which is characterized in that the stirring in the step 2
Speed is 10~50rmp.
8. the method for extraction manganese in electrolytic manganese residues according to claim 1, it is characterised in that the grain of the electrolytic manganese residues
≤ 150 μm of degree.
9. the method for extraction manganese in electrolytic manganese residues according to claim 1, it is characterised in that：Solid-liquid point in the step 2
Leaching rate >=90% of manganese from after.
10. a kind of method of processing electrolytic manganese residues, which is characterized in that extract and be electrolysed including claim 1-9 any one of them
The method of manganese in manganese slag.
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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 |
| CN111111854B (en) * | 2019-12-30 | 2021-02-12 | 铜仁学院 | Manganese ore industrialization wet ball milling method based on electrolytic manganese metal system backwater |
| CN113121127B (en) * | 2021-04-21 | 2022-01-11 | 昆明学院 | Manganese slag solid waste recycling treatment method and application thereof |
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| CN102424424A (en) * | 2011-09-15 | 2012-04-25 | 陈昆先 | Production method for manganese sulfate by using biological cellulose and low-grade manganese ores |
| CN102618728A (en) * | 2011-10-10 | 2012-08-01 | 云南建水锰矿有限责任公司 | Method for producing manganese sulfate by leaching manganese alloy slag under normal pressure |
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