CN110157904A - A kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution - Google Patents
A kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution Download PDFInfo
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- CN110157904A CN110157904A CN201910465472.7A CN201910465472A CN110157904A CN 110157904 A CN110157904 A CN 110157904A CN 201910465472 A CN201910465472 A CN 201910465472A CN 110157904 A CN110157904 A CN 110157904A
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- manganese
- sulfate solution
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- sulfuric acid
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- 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
- C22B47/0018—Treating ocean floor nodules
- C22B47/0027—Preliminary treatment
-
- 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
- C22B47/0018—Treating ocean floor nodules
- C22B47/0045—Treating ocean floor nodules by wet processes
- C22B47/0054—Treating ocean floor nodules by wet processes leaching processes
- C22B47/0063—Treating ocean floor nodules by wet processes leaching processes with acids or salt solutions
Abstract
The invention discloses a kind of methods that manganese nodule reduction roasting-leaching prepares manganese sulfate solution.It is prepared in the steps below；A, manganese nodule is crushed, obtains A product；B, newborn carbon mixing is added into A product, obtains composite ore, composite ore is added in sulfuric acid solution and is stirred, B product are obtained；C, water is added into B product, stirs evenly, obtain C product；D, C product are sent into roaster, carry out calcination, obtains D product；E, D product are transferred in batch extractor, after sulfuric acid solution or waste electrolyte is added, adds water adjusting liquid and consolidate mass ratio, be stirred to react, obtain E product；F, E product are subjected to solid-liquor separation, can be obtained manganese sulfate solution, manganese sulfate solution can be used for electrolytic manganese production, it can also be used to the preparation of the product of high purity manganese sulfate.The present invention has process equipment simple, and processing cost is low, and investment operating cost is lower, and manganese recovery ratio is high, provides the beneficial effect of reference to the development and utilization of manganese nodule.
Description
Technical field
The present invention relates to a kind of method for preparing manganese sulfate solution, especially a kind of manganese nodule reduction roasting-leaching preparation
The method of manganese sulfate solution.
Background technique
Manganese nodule is a kind of lumps seabed ore containing a variety of non-ferrous metals such as manganese, nickel, cobalt, copper, also known as mostly golden
Belong to tuberculosis.Deepwater station is widely distributed in the seabed of 4000-6000m.There are about manganese nodules for every square kilometre of deep seafloor
4400t, the estimation of seabed gross reserves reach trillion t of 3-3.5.Only Pacific manganese nodule reserves just have 1.7 trillion t, and they are also
In the rate growth with ten thousand t of about 1000-1600 every year.Contain 70 multiple elements in tuberculosis, wherein manganese content reaches 17.4%-
28.07%, manganese content is up to 57% in most rich manganese nodule, and China is that maximum manganese product consumes state in the world, due to China
Manganese ore lean ore is more, rich ore critical shortage, has theoretical and realistic meaning to the development and utilization of manganese nodule.
Ocean manganese nodule belongs to difficult and utilizes manganese resource, and manganese is mainly with δ-MnO2Form exists, and crystal structure is stablized, and is insoluble in
In acid & alkali liquid, it is typically led to reducing agent and is reduced into Mn2+After dissolve out.Common method has fire reduction, wet reducing now
And Bioleaching.Not only process multipotency consumption is high for fire reduction manganese, but also serious pollution can be generated to environment.Although Bioleaching gram
The some shortcomings of fire reduction are taken, but the period is longer.Wet reducing leaching of manganese mild condition, it is now that low energy pollution is small
The important channel of Smelting Plant.The critical problem of wet reducing leaching manganese is the reducing agent for finding a kind of economy, actual effect, has been reported
Reducing agent have SO2, waste paper, biomass etc..The dynamics research of organic matter wet method reducing pyrolusite concentrates on small-molecule substance
And biomass, as VEGLIO et al. has studied lactose, sucrose, caramel colorant, oat straw with spheric granules shrinking-core model respectively
The dynamics of the reducing leached pyrolusite ores such as stalk.
Although having carried out the studies above, rarely has the report of industrial application at present.Therefore, the invention proposes a kind of manganese knots
The method that core low-temperature reduction roasting-leaching prepares manganese sulfate solution lays the foundation for the development and utilization of manganese nodule.
Summary of the invention
The object of the present invention is to provide a kind of methods that manganese nodule reduction roasting-leaching prepares manganese sulfate solution.This hair
Bright to have process equipment simple, processing cost is low, and investment operating cost is lower, and manganese recovery ratio is high, the development and utilization to manganese nodule
The characteristics of reference is provided.
Technical solution of the present invention: a kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution, by following steps
Suddenly it is prepared；
A, manganese nodule is crushed, obtains A product；
B, newborn carbon mixing is added into A product, obtains composite ore, composite ore is added in sulfuric acid solution and is stirred, B product are obtained；
C, water is added into B product, stirs evenly, obtain C product；
D, C product are sent into roaster, carry out calcination, obtains D product；
E, D product are transferred in batch extractor, after sulfuric acid solution or waste electrolyte is added, adds water adjusting liquid and consolidate mass ratio, stir
Reaction is mixed, E product are obtained；
F, E product are subjected to solid-liquor separation, can be obtained manganese sulfate solution.
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, in the step a, to manganese nodule
It carries out being crushed to 300-400 mesh.
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, in the step b, the new life
Carbon is that glucose or white sugar are added strong sulfuric acid response and obtain solid.
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, in the step b, by following ratios
The mixing of 5-15g new life carbon is added into 100gA product, obtains composite ore for example.
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, in the step b, by following ratios
100g composite ore is added in the sulfuric acid solution of 40-80ml and is stirred, obtains B product by example；The volume fraction of the sulfuric acid solution is
40-60%。
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, and in the step c, the liquid of C product is solid
Mass ratio is 0.5-0.7.
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, in the step d, calcination
Temperature be 400-800 DEG C, time of reaction is 90-180min.
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, in the step e, by following ratios
, in 100gD product, 5-10ml sulfuric acid solution or waste electrolyte is added, the mass fraction of sulfuric acid in sulfuric acid solution or waste electrolyte
For 40-60%.
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, in the step e, adds water
Adjusting liquid to consolidate mass ratio is 3-5.
Manganese nodule reduction roasting-leaching above-mentioned is prepared in the method for manganese sulfate solution, in the step e, reaction temperature
It is 80-95 DEG C, the reaction time is 7-10 hours.
Compared with prior art, the present invention is by having the advantages that
1, for the present invention for the manganese dioxide in manganese nodule than relatively inert, the not high status of utilization rate proposes a kind of manganese knot
The method that core low-temperature reduction roasting-leaching prepares manganese sulfate solution, this method mainly include the low-temperature bake of manganese nodule, leach two
A key step, can be obtained manganese sulfate solution, and the leaching rate > 85% of manganese can be used as making after carrying out different degrees of removal of impurities
The raw material of standby different manganese systems materials, and manganese sulfate solution can be used for electrolytic manganese production, it can also be used to the product of high purity manganese sulfate
Preparation.
2, the temperature of calcination of the present invention is 400-800 DEG C, and the time of reaction is 90-180min, is restored than conventional carbon
The maturing temperature of (800 DEG C or so) is low, and corresponding equipment investment operating cost reduces；Reaction principle of the invention are as follows: 2MnO2 +
C + 2H2SO4 = 2MnSO4 + CO2(g) + 2H2Traditional leaching process is advanceed to calcining process by O, by traditional reduction
Roasting becomes sulfating roasting.
3, manganese nodule is deposited on deep-sea, containing Determination of multiple metal elements, wherein most have business development value is manganese, cobalt, nickel
Deng, its main component is also MnO2, and Mn content is up to 55%, develops and uses at present less, belong to the manganese ore of high-quality, but by
There is very strong inertia in manganese dioxide, soda acid is all insoluble, therefore processing difficulty is larger, and the seldom existing manganese nodule of industrial application is ground
It is less to study carefully report, in terms of concentrating research mineral associations and mineral phase structure, it is a kind of potential manganese ore money that it is few, which to leach research to it,
Source, the present invention is directed to manganese nodule, proposes a kind of method that manganese nodule low-temperature reduction roasting-leaching prepares manganese sulfate solution, right
The development and utilization of manganese nodule provide reference；
4, the preparation of existing manganese sulfate solution is generally prepared using manganese spar Ore Leaching, uses pyrolusite carbon reducting roast on a small quantity
It leaches and obtains afterwards.The former grade of ore is low, the quantity of slag is big, and the latter's grade of ore is high, and energy consumption is high, but the quantity of slag is small.But industrialization status
90% uses the former, and the manganese content for the manganese nodule that the present invention studies can match in excellence or beauty with pyrolusite, and the quantity of slag is few, and uses than soft manganese
The lower energy consumption of mine conventional method, therefore there is potential advantage.
In conclusion the present invention has process equipment simple, processing cost is low, and investment operating cost is lower, manganese recovery ratio
Height provides the beneficial effect of reference to the development and utilization of manganese nodule.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiment 1.A kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution, is made in the steps below
It is standby；
A, 100kg manganese nodule is carried out being crushed to 300 mesh, obtains A product；
B, the mixing of 5g new life carbon is added into every 100gA product, obtains composite ore, every 100g composite ore is added in 40ml sulfuric acid solution
It is stirred, obtains B product；The new life carbon is that glucose or white sugar are added strong sulfuric acid response and obtain solid；The sulfuric acid solution
Volume fraction is 40%；
C, water is added into B product, stirs evenly, obtain C product, it is 0.5 that the liquid of C product, which consolidates mass ratio,；
D, C product to be sent into roaster, carries out calcination, the temperature of calcination is 400 DEG C, and the time of reaction is 90min,
Obtain D product；
E, D product are transferred in batch extractor, in every 100gD product, after 5ml sulfuric acid solution or waste electrolyte is added, add water tune
It is 3 that section liquid, which consolidates mass ratio, is stirred to react, and reaction temperature is 80 DEG C, and the reaction time is 7 hours, obtains E product；The sulfuric acid solution or
The mass fraction of sulfuric acid is 40% in waste electrolyte；
F, E product are subjected to solid-liquor separation, can be obtained manganese sulfate solution, the leaching rate of manganese is 86%.
Embodiment 2.A kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution, is made in the steps below
It is standby；
A, 100kg manganese nodule is carried out being crushed to 350 mesh, obtains A product；
B, the mixing of 8g new life carbon is added into every 100gA product, obtains composite ore, every 100g composite ore is added in 50ml sulfuric acid solution
It is stirred, obtains B product；The new life carbon is that glucose or white sugar are added strong sulfuric acid response and obtain solid；The sulfuric acid solution
Volume fraction is 45%；
C, water is added into B product, stirs evenly, obtain C product, it is 0.6 that the liquid of C product, which consolidates mass ratio,；
D, C product are sent into roaster, carry out calcination, the temperature of calcination is 500 DEG C, and the time of reaction is
110min obtains D product；
E, D product are transferred in batch extractor, in every 100gD product, after 6ml sulfuric acid solution or waste electrolyte is added, add water tune
It is 4 that section liquid, which consolidates mass ratio, is stirred to react, and reaction temperature is 85 DEG C, and the reaction time is 8 hours, obtains E product；The sulfuric acid solution or
The mass fraction of sulfuric acid is 45% in waste electrolyte；
F, E product are subjected to solid-liquor separation, can be obtained manganese sulfate solution, the leaching rate of manganese is 90%.
Embodiment 3.A kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution, is made in the steps below
It is standby；
A, 100kg manganese nodule is carried out being crushed to 400 mesh, obtains A product；
B, the mixing of 10g new life carbon is added into every 100gA product, obtains composite ore, 60ml sulfuric acid solution is added in every 100g composite ore
In be stirred, obtain B product；The new life carbon is that glucose or white sugar are added strong sulfuric acid response and obtain solid；The sulfuric acid solution
Volume fraction be 50%；
C, water is added into B product, stirs evenly, obtain C product, it is 0.7 that the liquid of C product, which consolidates mass ratio,；
D, C product are sent into roaster, carry out calcination, the temperature of calcination is 600 DEG C, and the time of reaction is
130min obtains D product；
E, D product are transferred in batch extractor, in every 100gD product, after 7ml sulfuric acid solution or waste electrolyte is added, add water tune
It is 5 that section liquid, which consolidates mass ratio, is stirred to react, and reaction temperature is 90 DEG C, and the reaction time is 9 hours, obtains E product；The sulfuric acid solution or
The mass fraction of sulfuric acid is 55% in waste electrolyte；
F, E product are subjected to solid-liquor separation, can be obtained manganese sulfate solution, the leaching rate of manganese is 92%.
Embodiment 4.A kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution, is made in the steps below
It is standby；
A, 100kg manganese nodule is carried out being crushed to 350 mesh, obtains A product, the mixing of 13g new life carbon b, is added into every 100gA product, obtains
Every 100g composite ore is added in 70ml sulfuric acid solution and is stirred, obtains B product by composite ore；The new life carbon is glucose or white
Sugar is added strong sulfuric acid response and obtains solid；The volume fraction of the sulfuric acid solution is 55%；
C, water is added into B product, stirs evenly, obtain C product, it is 0.6 that the liquid of C product, which consolidates mass ratio,；
D, C product are sent into roaster, carry out calcination, the temperature of calcination is 700 DEG C, and the time of reaction is
160min obtains D product；
E, D product are transferred in batch extractor, in every 100gD product, after 8ml sulfuric acid solution or waste electrolyte is added, add water tune
It is 4 that section liquid, which consolidates mass ratio, is stirred to react, and reaction temperature is 95 DEG C, and the reaction time is 9 hours, obtains E product；The sulfuric acid solution or
The mass fraction of sulfuric acid is 55% in waste electrolyte；
F, E product are subjected to solid-liquor separation, can be obtained manganese sulfate solution, the leaching rate of manganese is 88%.
Embodiment 5.A kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution, is made in the steps below
It is standby；
A, 100kg manganese nodule is carried out being crushed to 400 mesh, obtains A product,
B, the mixing of 15g new life carbon is added into every 100gA product, obtains composite ore, 80ml sulfuric acid solution is added in every 100g composite ore
In be stirred, obtain B product；The new life carbon is that glucose or white sugar are added strong sulfuric acid response and obtain solid；The sulfuric acid solution
Volume fraction be 60%；
C, water is added into B product, stirs evenly, obtain C product, it is 0.7 that the liquid of C product, which consolidates mass ratio,；
D, C product are sent into roaster, carry out calcination, the temperature of calcination is 800 DEG C, and the time of reaction is
180min obtains D product；
E, D product are transferred in batch extractor, in every 100gD product, after 10ml sulfuric acid solution or waste electrolyte is added, add water tune
It is 5 that section liquid, which consolidates mass ratio, is stirred to react, and reaction temperature is 95 DEG C, and the reaction time is 10 hours, obtains E product；The sulfuric acid solution or
The mass fraction of sulfuric acid is 60% in waste electrolyte；
F, E product are subjected to solid-liquor separation, can be obtained manganese sulfate solution, the leaching rate of manganese is 95%.
Claims (10)
1. a kind of method that manganese nodule reduction roasting-leaching prepares manganese sulfate solution, it is characterised in that: made in the steps below
It is standby；
A, manganese nodule is crushed, obtains A product；
B, newborn carbon mixing is added into A product, obtains composite ore, composite ore is added in sulfuric acid solution and is stirred, B product are obtained；
C, water is added into B product, stirs evenly, obtain C product；
D, C product are sent into roaster, carry out calcination, obtains D product；
E, D product are transferred in batch extractor, after sulfuric acid solution or waste electrolyte is added, adds water adjusting liquid and consolidate mass ratio, stir
Reaction is mixed, E product are obtained；
F, E product are subjected to solid-liquor separation, can be obtained manganese sulfate solution.
2. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step a, manganese nodule is carried out to be crushed to 300-400 mesh.
3. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step b, the new life carbon is that glucose or white sugar are added strong sulfuric acid response and obtain solid.
4. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step b, in following ratios, the mixing of 5-15g new life carbon is added into 100gA product, obtains composite ore.
5. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step b, in following ratios, 100g composite ore is added in the sulfuric acid solution of 40-80ml and is stirred, obtain B product；It is described
The volume fraction of sulfuric acid solution is 40-60%.
6. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step c, it is 0.5-0.7 that the liquid of C product, which consolidates mass ratio,.
7. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step d, the temperature of calcination is 400-800 DEG C, and the time of reaction is 90-180min.
8. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step e, in following ratios, in 100gD product, 5-10ml sulfuric acid solution or waste electrolyte, sulfuric acid solution or useless electricity is added
The volume fraction for solving sulfuric acid in liquid is 40-60%.
9. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step e, adding water and adjusting liquid to consolidate mass ratio is 3-5.
10. the method that manganese nodule reduction roasting-leaching according to claim 1 prepares manganese sulfate solution, it is characterised in that:
In the step e, reaction temperature is 80-95 DEG C, and the reaction time is 7-10 hours.
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| CN111876586A (en) * | 2020-07-29 | 2020-11-03 | 北京科技大学 | Method for comprehensively recovering all elements by roasting and reducing ocean cobalt-rich crusts through biomass |
| CN114988485A (en) * | 2022-07-13 | 2022-09-02 | 重庆上甲电子股份有限公司 | Method for synchronously producing manganous-manganic oxide and ferric oxide for soft magnetism by using marine polymetallic nodule |
| CN115140777A (en) * | 2022-07-13 | 2022-10-04 | 重庆上甲电子股份有限公司 | Method for producing ferromanganese composite material for soft magnetism by using ocean manganese nodules |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111876586A (en) * | 2020-07-29 | 2020-11-03 | 北京科技大学 | Method for comprehensively recovering all elements by roasting and reducing ocean cobalt-rich crusts through biomass |
| CN114988485A (en) * | 2022-07-13 | 2022-09-02 | 重庆上甲电子股份有限公司 | Method for synchronously producing manganous-manganic oxide and ferric oxide for soft magnetism by using marine polymetallic nodule |
| CN115140777A (en) * | 2022-07-13 | 2022-10-04 | 重庆上甲电子股份有限公司 | Method for producing ferromanganese composite material for soft magnetism by using ocean manganese nodules |
| CN114988485B (en) * | 2022-07-13 | 2023-03-10 | 重庆上甲电子股份有限公司 | Method for synchronously producing manganous-manganic oxide and ferric oxide for soft magnetism by using marine polymetallic nodule |
| CN115140777B (en) * | 2022-07-13 | 2023-04-25 | 重庆上甲电子股份有限公司 | Method for producing ferromanganese composite material for soft magnetic by utilizing ocean manganese nodule |
| US11791078B1 (en) | 2022-07-13 | 2023-10-17 | Chongqing Shangjia Electronic Co., Ltd. | Method for synchronous production of manganese tetraoxide and ferric oxide for soft magnetic material by using marine polymetallic nodules |
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