CN109136551A - A method of extracting vanadium from high calcium bone coal - Google Patents
A method of extracting vanadium from high calcium bone coal Download PDFInfo
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- CN109136551A CN109136551A CN201811269333.9A CN201811269333A CN109136551A CN 109136551 A CN109136551 A CN 109136551A CN 201811269333 A CN201811269333 A CN 201811269333A CN 109136551 A CN109136551 A CN 109136551A
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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
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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
- C22B3/02—Apparatus therefor
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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Abstract
The present invention discloses a kind of method that vanadium is extracted from high calcium bone coal, it is delivered directly in closed pond the following steps are included: raw ore is carried out the ore pulp that wet milling obtains in ball mill, and directly mixed with the concentrated sulfuric acid, maturation process is carried out to high calcium bone coal by the heat of dilution and chemical reaction heat of the concentrated sulfuric acid;Then in closed pond plus water, air-blowing agitation is obtained the leaching vanadium solution of blue after separation of solid and liquid, is used to prepare V with leaching vanadium2O5Product.The present invention uses wet milling, directly carries out ore grinding without mine is dried, ore grinding yield is high, noise is small, without dust;Curing slag is sposh shape without crushing, and can directly add water extraction vanadium;Curing step uses the closed pond of insulation, is conducive to cure efficiency;Aerobic fermentation tank is combined with eluting column, effectively prevents pollution of the exhaust gas to environment when curing.The present invention preferably overcomes the problem of cumbersome technique present in existing concentrated sulfuric acid curing vanadium extraction technology, at high cost, environmental pollution.
Description
Technical field
The invention belongs to technical field of wet metallurgy, more particularly, to a kind of method for extracting vanadium from high calcium bone coal.
Background technique
High calcium bone coal is one of Rock coal containing alum mine, and CaO content usually 5% or more, is important vanadium extraction resource
One of.But high calcium bone coal is due to being rich in a large amount of dolomites, calcite, lime stone class mineral, is difficult to deal in vanadium extraction industry
A kind of ore.Traditional roasting-acid-hatching of young eggs is such as used, can generate calcium vanadate in leaching process causes the extraction rate of vanadium low, is
The extraction rate of vanadium is improved, many patents of invention disclose the mineral that floatation removes calcic.Published Chinese invention patent
(publication number CN103706465A, CN102274795A, CN103484667A, CN105032598A) proposes a kind of flotation beneficiation
Method handles high calcium bone coal, and technical solution is low-temperature bake decarburization-medicament flotation deliming-high-temperature roasting oxidizing lower vanadium, water
The technique of leaching and vanadium extraction, the extraction rate of vanadium is 65~80%.
It is a kind of more environmentally friendly method with concentrated sulfuric acid curing vanadium extraction technology, this many aspect has been disclosed
Patent of invention.But there is many deficiencies for existing concentrated sulfuric acid curing method: as there is ore grinding yield in dry powder crushing process
The problem of low, noise is big, dust from flying;Dry powder and the concentrated sulfuric acid can damage motor when being mixed, with mixture when belt transport
When concentrated sulfuric acid belt easy to damage;When matured mixture is outdoor or unlimited stacking, the SO that is released when the concentrated sulfuric acid is reacted with mineral2、
CO2, there is the hidden danger of environmental pollution for the exhaust gas such as HCl;Curing slag easily agglomerates and becomes hard, is needed before with water extraction vanadium
Increase to crush together and breaks up process, it is comparatively laborious in this way.Therefore, it is necessary to improve to existing concentrated sulfuric acid curing method.
Summary of the invention
The present invention for existing sulfuric acid curing method deficiency, it is intended to solve it is existing carried out from vanadium slag curing vanadium extraction technology
Present in ore grinding low output, process is tedious, blender is easy to damage, the problem of environmental pollution etc..
To achieve the goals above, the present invention provides a kind of method that vanadium is extracted from high calcium bone coal, and this method is using such as
The lower system, the system include:
Closed pond, sulphuric acid tank, ball mill;
The closed pond is connect with the sulphuric acid tank and the ball mill respectively;
This method comprises:
Step S1: high calcium bone coal and water are input in ball mill and carry out wet milling, obtains the ore pulp of mobility;
Step S2: the ore pulp of mobility is input in closed pond, while by sulphuric acid tank being input to the concentrated sulfuric acid closed
Chi Zhong carries out high calcium bone coal to obtain the Curing material of sposh shape from thermal maturation;
Step S3: add water into closed pond, and air-blowing is stirred, and to carry out the leaching of vanadium, obtains solidliquid mixture;
Step S4: the solidliquid mixture in closed pond being extracted out, is separated by solid-liquid separation, and obtains leaching vanadium solution.
As a preferred embodiment of the present invention, before implementation steps S1, first by high calcium bone coal lump ore Vibration Screen
Part of the choosing less than 10cm is input in ball mill.
As a preferred embodiment of the present invention, the system also includes eluting column and lye pond, the closed pond tops
It is provided with gas vent, the eluting column is connect with the gas vent by exhaust pipe;The lye pond by high-pressure pump with it is described
Injection spray pipe connection in eluting column, the injection spray pipe is for spraying NaOH/H2O2Mix aqueous alkali;The method also includes will
The exhaust gas generated in self-heating maturing process in step S2, which is transported in eluting column, carries out absorption processing.
As a preferred embodiment of the present invention, content >=8.14wt% of the CaO in the high calcium bone coal.
As a preferred embodiment of the present invention, V in the high calcium bone coal2O5Mass fraction be 0.8~2.1%.
As a preferred embodiment of the present invention, the blocky thickness of the high calcium bone coal be less than 10cm, water content be 3~
9wt%.
As a preferred embodiment of the present invention, in step S1, relative to high calcium bone coal, the additional amount of water is 28~
38wt%.The amount of water is bigger than the amount of water after dry curing, and general dry curing amount of water is 8-12%.Water of the invention is
It is added when crushing, wet milling can be completed in this way, while ore pulp can be formed, be flowed in mixture pipeline, is transported to close
It closes in pond.Advantage first is that the recirculated water of this range is added after can be carried out wet milling, no dust, noiseless generation, and yield
Greatly.Second is that there is mobility, mixed automatically in closed pond with the concentrated sulfuric acid, when curing is sposh shape, is also sposh shape after curing, no
Agglomeration, can directly fill the water leaching vanadium into pond.
As a preferred embodiment of the present invention, in step S2, relative to the high calcium bone coal in step S1, the concentrated sulfuric acid adds
Entering amount is 38~45wt%.The consumption of the concentrated sulfuric acid is big in the present invention, but is conducive to diluting concentrated sulfuric acid fever, which can keep
Curing temperature is 135~165 DEG C, and the high calcium bone coal in closed pond is cured by the self-heating that sulfuric acid dilution generates, entire ripe
Change process does not carry out external heat, can also generate sulphur with other valuable metal element reactions in ore without the reacted concentrated sulfuric acid
Hydrochlorate dissolution.If sulphuric acid is lower than 38%, curing temperature is with regard to low, and not exclusively, vanadium extraction rate is with regard to low for the curing of high calcium bone coal.
If sulphuric acid is more than 50%, just high to cause to waste, the sodium hydroxide being added when adjusting pH value in next step needs just more,
Increase production cost.So the additional amount of the concentrated sulfuric acid is the most appropriate in above range.
As a preferred embodiment of the present invention, in step S3, relative to the high calcium bone coal in 1kg step S1, water adds
Entering amount is 2~3L.
As a preferred embodiment of the present invention, in step S1, the time of wet milling is 10~20min, obtained stream
The partial size of the ore pulp of dynamic property is 80~120 mesh.The partial size of the ore pulp for the mobility that the time of above-mentioned wet milling ensure that
For 80~120 mesh.Wherein, the yield of ball mill ore grinding is 25 ton/hours, and this wet milling eliminates the dirt of noise and dust
Dye, while increasing ore grinding amount.
As a preferred embodiment of the present invention, in step S2, the time of curing is 24~32h, and the temperature of curing is 135
~165 DEG C, pressure when curing is 0.12~0.18MPa.The above numberical range ensure that the abundant of high calcium bone coal and the concentrated sulfuric acid
Reaction, temperature height are conducive to the chemical reaction of sulfuric acid dissolution vanadium metal, and temperature low reaction is with regard to slow, and vanadium extraction rate is with regard to low.Temperature is too
Height, it is excessive to will cause closed pond pressure, and closed pond is caused to be cracked, and through inventor's experimental verification, above-mentioned pressure limit is most suitable
Pressure limit.
According to the present invention, in step S2, specifically, stopping when high calcium bone coal reaches 105~120 ton hours into closed pond
Ore pulp is inputted, mixture pipeline is moved into second closed pond;Gas exhausting valve, feed inlet, extraction opening are simultaneously closed off, it is close at this time
It closes in pond and generates 135~165 DEG C of high-temperature steam, insertion thermocouple observes temperature change, and connection pressure gauge is observed in closed pond
Steam pressure, allow high calcium bone coal to be cured in closed pond, obtain sposh shape Curing material, air-blowing steel pipe can directly be inserted into close
The bottom for closing pond illustrates Curing material without agglomeration.
As a preferred embodiment of the present invention, in step S3, the time of air-blowing stirring is 1~2.5h, and air-blowing stirring is adopted
With air compressor, pressure is 6~10MPa.
According to the present invention, specifically, in step S4, the solidliquid mixture in closed pond is extracted out with acid-proof pump, is delivered to
Filter press is separated by solid-liquid separation and is collected leaching vanadium solution, and it is the solution of tetravalence vanadium that leaching vanadium solution, which is dark blue solution, this leaching vanadium
Ammonium metavanadate can be made by adjusting pH value plus hydrogen peroxide oxidation, resin adsorption, highly basic elution, ammonium chloride precipitation processing in solution
Or vanadic anhydride product.
As a preferred embodiment of the present invention, the water used in the above method is each production process for industrial circulating water
The industrial water centralized collection given off successively uses the purified water of precipitatings, filtration treatment such as lime, liquid alkaline, sodium sulfide solution,
Recirculated water avoids waste water and discharges outward, causes environmental pollution.
As a preferred embodiment of the present invention, multiple extraction openings, multiple feed inlets are provided on the closed pond.
As a preferred embodiment of the present invention, the sulphuric acid tank is connect by sulfuric acid efferent duct with the closed pond, institute
It states sulfuric acid efferent duct and connects the one end in closed pond and be directly protruding into the feed inlet on closed pond.
As a preferred embodiment of the present invention, the ball mill is connected by mixture conveyance conduit and the closed pond
It connects, one end that the mixture pipeline connects closed pond is directly protruding into the feed inlet on closed pond.
As a preferred embodiment of the present invention, the mixture conveyance conduit is pvc pipe, PE pipe, steel pipe or cast iron pipe.
As a preferred embodiment of the present invention, the bottom surface in the closed pond and the angle of horizontal direction are 8~12 °.
As a preferred embodiment of the present invention, multiple gas exhausting valves are provided on the exhaust pipe, are arranged for exhaust gas
The control put.
As a preferred embodiment of the present invention, exhaust fan I is additionally provided between the eluting column and the exhaust pipe.
As a preferred embodiment of the present invention, gas outlet is provided on the eluting column.
According to the present invention, the NaOH/H of the injection spray pipe spray2O2Aqueous alkali is mixed, to absorb the SO in exhaust gas2、
CO2, HCl gas;It is furthermore preferred that the NaOH/H2O2It mixes in aqueous alkali, NaOH and H2O2Mass fraction be respectively 4~
6% and 2~4%.As a preferred embodiment of the present invention, the injection spray pipe is more preferably multilayer.
As a preferred embodiment of the present invention, sulfuric acid metering pump is provided on the sulfuric acid efferent duct.
As a preferred embodiment of the present invention, sulfuric acid input pipe is also connected on the sulphuric acid tank.
As a preferred embodiment of the present invention, the height of the sulphuric acid tank with respect to the horizontal plane is higher than closed pond.It utilizes
Drop can be such that ore pulp automatically flows into closed pond, and the ore pulp that such wet milling generates does not need to be stirred with the concentrated sulfuric acid mixed
It closes.
As a preferred embodiment of the present invention, the ball mill is also connected with hopper, and it is defeated to be provided with recirculated water on hopper
Enter pipe.
As a preferred embodiment of the present invention, ore pulp control valve is provided on the mixture pipeline.
As a preferred embodiment of the present invention, sulfuric acid control valve is provided on the sulfuric acid efferent duct.
As a preferred embodiment of the present invention, it is 260~400m that the closed pond, which is a volume,3Cement works object,
It is rectangle, inner wall carries out acidproof processing;The closed pond is whole in depth 2.5~3.5 meters lower, and bottom of pond is a domatic, to
8~12o of top rake is used to collect the solidliquid mixture of bottom, and is conducive to acid-proof pump and is fully drawn out solidliquid mixture.
As a preferred embodiment of the present invention, the feed inlet is located at the middle part in closed pond, to input the ore pulp
And the concentrated sulfuric acid;The extraction opening is located at closed pond front, to add water from closed pond and extract solidliquid mixture;The row
Stomata is located at the rear portion in closed pond, the exhaust gas and extra water vapour that generate in the closed pond is discharged.
Compared with existing curing technology, the present invention has the advantages that
In technical solution provided by the invention, the raw material of high calcium bone coal be by wet process carry out ore grinding, without preparatory
Drying, is directly inputted in ball mill plus water carries out wet milling, its advantage is that wet milling yield is high, noise is small, without dust
It generates, high efficiency, noiseless, without dust pollution production environment can be provided;By the resulting ore pulp of wet milling, pass through pvc pipe
Road is directly inputted in closed pond to be mixed with the concentrated sulfuric acid, is mixed it is not necessary that ore pulp to be stirred with the concentrated sulfuric acid, is simplified production work
Sequence has saved cost;Then directly add water, air-blowing agitation leacs vanadium, it is not necessary that Curing material is taken out crushing, slurrying in closed pond
Carry out leaching vanadium, also greatly simplifies production process, saved the time.The present invention also focuses on environmental protection and energy saving,
The closed pond proposed has the function of that insulation, a pond are dual-purpose, and external heat need not be carried out in curing, leans on itself slaking reaction
The thermal energy of generation can maintain the curing temperature of high calcium bone coal at 135~165 DEG C, curing pressure in 0.12~0.18MP range,
Great advantage is to collect the SO generated in maturing process2、CO2, the exhaust gas such as HCl, and processing absorbed by eluting column these is useless
Gas realizes zero waste gas emission, reaches the requirement of environmental protection.Technical solution provided by the invention is a kind of environmentally friendly ripe
Change extraction vanadium method, solves the problems, such as that process is tedious, at high cost, exhaust emission present in existing curing vanadium extraction technology.
Therefore, the present invention has the characteristics that vanadium extraction is high-efficient and pollutes low.After measured, the leaching rate of vanadium up to 92.26~
99.61%, it can be achieved that pollution-free carry out vanadium extraction to high calcium bone coal.
Other features and advantages of the present invention will then part of the detailed description can be specified.
Detailed description of the invention
Exemplary embodiment of the invention is described in more detail in conjunction with the accompanying drawings, it is of the invention above-mentioned and its
Its purpose, feature and advantage will be apparent, wherein in exemplary embodiment of the invention, identical reference label
Typically represent same parts.
Fig. 1 shows flow diagram according to an embodiment of the invention.
Fig. 2 shows the signals of the closed curing vanadium extraction system of the wet milling-used according to one embodiment of present invention
Property structure chart.
Description of symbols: the closed pond 1-;2- extraction opening;3- feed inlet;4- gas vent;5- exhaust pipe;501- exhaust control
Valve processed;6- exhaust fan I;7- eluting column;701- injection spray pipe;The gas outlet 8-;9- high-pressure pump;10- lye pond;The metering of 11- sulfuric acid
Pump;1101- sulfuric acid efferent duct;12- sulfuric acid input pipe;13- sulphuric acid tank;14- recycles water inlet pipe;16- hopper;17- ball milling
Machine;1701- mixture conveyance conduit;301- ore pulp control valve;302- sulfuric acid control valve.
Specific embodiment
The preferred embodiment of the present invention is described in more detail below.Although the following describe preferred implementations of the invention
Mode, however, it is to be appreciated that may be realized in various forms the present invention without that should be limited by the embodiments set forth herein.Phase
Instead, these embodiments are provided so that the present invention is more thorough and complete, and can be by the scope of the present invention completely
It is communicated to those skilled in the art.
In the embodiment of the present invention, the flow diagram that the method for vanadium is extracted from high calcium bone coal is as shown in Figure 1;What is used mentions
Vanadium system is vanadium extraction system as described below:
As shown in Fig. 2, being equipped with exhaust pipe 5 at the top of closed pond 1, one end of exhaust pipe 5 is connect with gas vent 4, the exhaust
The other end of pipeline 5 is connect with exhaust fan I 6, and the outlet of the exhaust fan I 6 passes through pipeline and eluting column 7 (a height of 6m is arranged)
Connection, the exhaust gas generated in the closed pond 1 is delivered in eluting column 7, three layers of injection spray pipe are provided in the eluting column 7
701 (identifying in Fig. 2, illustrate only one layer of injection spray pipe 701), the injection spray pipe 701 is for spraying NaOH/H2O2Mixing
Aqueous alkali, to absorb the SO in exhaust gas2Gas carries out absorption cleaning processing to exhaust gas;The top of the eluting column 7 is also set
There is gas outlet 8, is discharged by purified gas by gas outlet 8;Wherein, the NaOH/H2O2It mixes in aqueous alkali,
NaOH and H2O2Mass fraction be respectively 5% and 3%.It is arranged in the upstream of the eluting column 7 for storing the NaOH/
H2O2The lye pond 10 of aqueous alkali is mixed, the aqueous alkali in lye pond 10 is delivered to the spray in eluting column 7 by high-pressure pump 9
It is sprayed in mist pipe 701.Ball mill 17, PVC pipeline 1701, sulphuric acid tank 13 is arranged in the upstream in closed pond 1;Mix material conveying tube
1701 one end of road is connected with ball mill 17, and the other end is directly protruding into the feed inlet 3 in closed pond;13 exit of sulphuric acid tank is provided with
One sulfuric acid metering pump 11, sulfuric acid efferent duct 1101 are directly protruding into the feed inlet in closed pond 1;When closed 1 Rock coal containing alum amount of pond
Reach 100~130 ton hours, close the ore pulp control valve 301 and gas exhausting valve 501, keeps the closed pond 1
After the completion of the pretreatment from thermal maturation, gas exhausting valve is opened to pre-process from thermal maturation for closed environment
501 extract the exhaust gas in closed pond 1 out, are transported to eluting column 7 and carry out absorption processing, when no exhaust gas, close gas exhausting valve
501, it opens extraction opening 2 and adds water, and air-blowing agitation leacs vanadium into closed pond 1;Leaching finishes, and is mixed solid-liquid by extraction opening 2
Object extraction is closed, is separated by solid-liquid separation.In addition, the top cement pre-fabricated panel in the closed pond 1 is closed, be provided with extraction opening 2, into
Material mouth 3, gas vent 4.
Embodiment 1
(1) bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 1.28%, CaO are 8.14%) 105 tons, and 29.4 tons of progress wet millings of recirculated water are added into ball mill 17
10min, the ore grinding yield of high calcium bone coal are 25 ton/hours, obtain the ore pulp that granularity is 80 mesh.
(2) ore pulp control valve 301 is opened, ore pulp is continuously flowed into closed pond 1 by PVC mixture conveyance conduit 1701
In, while opening sulfuric acid control valve 302 and 42 tons of concentrated sulfuric acids (being checked and approved with sulfuric acid metering pump 11) is added into closed pond 1, the two is certainly
Row mixing, obtains sposh shape mixture;When inputting ore pulp and the concentrated sulfuric acid, closes the extraction opening 2 in closed pond 1, opens exhaust control
Valve 501 and exhaust fan I 6 processed, are transported to eluting column 7 for the exhaust gas in closed pond 1 and carry out absorption processing.
(3) when in closed pond 1 high calcium bone coal reach 105 ton hours, continue in maturing process close extraction opening 2, close simultaneously
Ore pulp control valve 301 and gas exhausting valve 501 are closed, stops exhaust fan I 6 and operates, keeping entire closed pond 1 is closed state, dimension
165 DEG C of curing temperature are held, pressure 0.18MP range is cured, high calcium bone coal curing time in closed pond 1 remains 32h.
(4) when curing finishes, opening gas exhausting valve 501 simultaneously opens exhaust fan I 6, and the mixture in closed pond 1 is existed
The gas generated in stacking process, which is transported in eluting column 7, carries out purified treatment, and purified gas is discharged by gas outlet 8;
When exhaust gas is completely exhausted out, extraction opening 2 is opened.
(5) after the completion of gas purification processing, the extraction opening 2 in closed pond 1 is opened, 210 tons of recirculated waters are added, use air compressor machine
The leaching that 2.5h carries out vanadium is stirred in air-blowing, then extracts solidliquid mixture out from the acid-proof pump of extraction opening 2, and be transported to plate compression
Machine is separated by solid-liquid separation, and is obtained the leaching vanadium liquid of blue, is used to prepare vanadium product.
Using V in iron ammonium sulfate oxidation reduction titration measurement high calcium bone coal and filter residue2O5Content, obtain high calcium stone
V in coal2O5Extraction rate be 99.57%, and in the gas after eluting column purified treatment be free of SO2、CO2, the exhaust gas such as HCl, it is full
Sufficient gas discharge standard.
In this embodiment, it keeps step (2), (3), (4), (5) constant, changes the step the recirculated water additional amount in (1)
It is 30.5,31.5,33.6,35.7,37.8,39.9 tons, the extraction rate of vanadium is 93.76-99.43%, and CaO content is low in leachate
In 1.1 μ g/mL, most of CaO is coexisted in leaching slag with calcium sulfate slag.
Embodiment 2
(1) bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 1.57%, CaO are 10.46%) 110 tons, and 41.8 tons of progress wet millings of recirculated water are added into ball mill 17
10min, the ore grinding yield of high calcium bone coal are 25 ton/hours, obtain the ore pulp that granularity is 100 mesh.
(2) ore pulp control valve 301 is opened, ore pulp is continuously flowed into closed pond 1 by PVC mixture conveyance conduit 1701
In, while opening sulfuric acid control valve 302 and 49.5 tons of concentrated sulfuric acids (being checked and approved with sulfuric acid metering pump 11), the two are added into closed pond 1
It voluntarily mixes, obtains sposh shape mixture;When inputting ore pulp and the concentrated sulfuric acid, closes the extraction opening 2 in closed pond 1, opens exhaust
Exhaust gas in closed pond 1 is transported to eluting column 7 and carries out absorption processing by control valve 501 and exhaust fan I 6.
(3) when in closed pond 1 high calcium bone coal reach 110 ton hours, continue in maturing process close extraction opening 2, close simultaneously
Ore pulp control valve 301 and gas exhausting valve 501 are closed, stops exhaust fan I 6 and operates, keeping entire closed pond 1 is closed state, dimension
135 DEG C of curing temperature are held, pressure 0.18MP range is cured, high calcium bone coal cures for 24 hours in closed pond 1.
(4) when curing finishes, opening gas exhausting valve 501 simultaneously opens exhaust fan I 6, and the mixture in closed pond 1 is existed
The gas generated in stacking process, which is transported in eluting column 7, carries out purified treatment, and purified gas is discharged by gas outlet 8;
When exhaust gas is completely exhausted out, extraction opening 2 is opened.
(5) after the completion of gas purification processing, the extraction opening in closed pond 1 is opened, 275 tons of recirculated waters are added, use air compressor machine
The leaching that 1.5h carries out vanadium is stirred in air-blowing, then extracts solidliquid mixture out from the acid-proof pump of extraction opening 2, and be transported to plate compression
Machine is separated by solid-liquid separation, and is obtained the leaching vanadium liquid of blue, is used to prepare vanadium product.
Using V in iron ammonium sulfate oxidation reduction titration measurement high calcium bone coal and filter residue2O5Content, obtain high calcium stone
V in coal2O5Extraction rate be 97.14%, and in the gas after eluting column purified treatment be free of SO2、CO2, the exhaust gas such as HCl, it is full
Sufficient gas discharge standard.
In this embodiment, it keeps step (1), (3), (4), (5) constant, changes the step the additional amount of the concentrated sulfuric acid in (2)
It is 41.8,42.9,44,45.1,46.2,47.3,48.4 tons, the extraction rate of vanadium is 93.26-98.89%, and CaO contains in leachate
Amount is present in leaching slag lower than 1.1 μ g/mL, most of CaO with calcium sulfate slag.
Embodiment 3
(1) bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 1.18%, CaO are 9.47%) 115 tons, and 38.5 tons of progress wet millings of recirculated water are added into ball mill 17
10min, the ore grinding yield of high calcium bone coal are 25 ton/hours, obtain the ore pulp that granularity is 120 mesh.
(2) ore pulp control valve 301 is opened, ore pulp is continuously flowed into closed pond 1 by PVC mixture conveyance conduit 1701
In, while opening sulfuric acid control valve 302 and 48.3 tons of concentrated sulfuric acids (being checked and approved with sulfuric acid metering pump 11), the two are added into closed pond 1
It voluntarily mixes, obtains sposh shape mixture;When inputting ore pulp and the concentrated sulfuric acid, closes the extraction opening 2 in closed pond 1, opens exhaust
Exhaust gas in closed pond 1 is transported to eluting column 7 and carries out absorption processing by control valve 501 and exhaust fan I 6.
(3) when in closed pond high calcium bone coal reach 115 ton hours, continue in maturing process close extraction opening 2, simultaneously close off
Ore pulp control valve 301 and gas exhausting valve 501 stop exhaust fan I 6 and operate, and keeping entire closed pond 1 is closed state, maintain
150 DEG C of curing temperature, pressure 0.18MP range is cured, high calcium bone coal cures 26h in closed pond 1.
(4) when curing finishes, opening gas exhausting valve 501 simultaneously opens exhaust fan I 6, and the mixture in closed pond 1 is existed
The gas generated in stacking process, which is transported in eluting column 7, carries out purified treatment, and purified gas is discharged by gas outlet 8;
When exhaust gas is completely exhausted out, extraction opening 2 is opened.
(5) after the completion of gas purification processing, the extraction opening 2 in closed pond 1 is opened, 250 tons of recirculated waters are added, use air compressor machine
The leaching that 2.0h carries out vanadium is stirred in air-blowing, then extracts solidliquid mixture out from the acid-proof pump of extraction opening 2, and be transported to plate compression
Machine is separated by solid-liquid separation, and is obtained the leaching vanadium liquid of blue, is used to prepare vanadium product.
Using V in iron ammonium sulfate oxidation reduction titration measurement high calcium bone coal and filter residue2O5Content, obtain high calcium stone
V in coal2O5Extraction rate be 96.41%, and in the gas after eluting column purified treatment be free of SO2、CO2, the exhaust gas such as HCl, it is full
Sufficient gas discharge standard.
In this embodiment, keep step (1), (2), (4), (5) constant, the curing temperature changed the step in (3) is
135,140,145,155,160,165 DEG C, the extraction rate of vanadium is 93.56-99.52%, the extraction rate of vanadium be influenced by temperature compared with
Greatly, CaO content is present in leaching slag lower than 1.1 μ g/mL, most of CaO with calcium sulfate slag in leachate.
Embodiment 4
(1) bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 0.96%, CaO are 10.74%) 120 tons, and 36 tons of progress wet millings of recirculated water are added into ball mill 17
10min, the ore grinding yield of high calcium bone coal are 25 ton/hours, obtain the ore pulp that granularity is 80 mesh.
(2) ore pulp control valve 301 is opened, ore pulp is continuously flowed into closed pond 1 by PVC mixture conveyance conduit 1701
In, while opening sulfuric acid control valve 302 and 48 tons of concentrated sulfuric acids (being checked and approved with sulfuric acid metering pump 11) is added into closed pond 1, the two is certainly
Row mixing, obtains sposh shape mixture;When inputting ore pulp and the concentrated sulfuric acid, closes the extraction opening 2 in closed pond 1, opens exhaust control
Valve 501 and exhaust fan I 6 processed, are transported to eluting column 7 for the exhaust gas in closed pond 1 and carry out absorption processing.
(3) when in closed pond 1 high calcium bone coal reach 120 ton hours, continue in maturing process close extraction opening 2, close simultaneously
Ore pulp control valve 301 and gas exhausting valve 501 are closed, stops exhaust fan I 6 and operates, keeping entire closed pond 1 is closed state, dimension
145 DEG C of curing temperature are held, cures pressure 0.18MP range, high calcium bone coal curing time in closed pond 1 is 28h.
(4) when curing finishes, opening gas exhausting valve 501 simultaneously opens exhaust fan I 6, and the mixture in closed pond 1 is existed
The gas generated in stacking process, which is transported in eluting column 7, carries out purified treatment, and purified gas is discharged by gas outlet 8;
When exhaust gas is completely exhausted out, extraction opening 2 is opened.
(5) after the completion of gas purification processing, the extraction opening 2 in closed pond 1 is opened, 300 tons of recirculated waters are added, use air compressor machine
The leaching that 2.4h carries out vanadium is stirred in air-blowing, then extracts solidliquid mixture out from the acid-proof pump of extraction opening 2, and be transported to plate compression
Machine is separated by solid-liquid separation, and is obtained the leaching vanadium liquid of blue, is used to prepare vanadium product.
Using V in iron ammonium sulfate oxidation reduction titration measurement high calcium bone coal and filter residue2O5Content, obtain high calcium stone
V in coal2O5Extraction rate be 95.48%, and in the gas after eluting column purified treatment be free of SO2、CO2, the exhaust gas such as HCl, it is full
Sufficient gas discharge standard.
In this embodiment, keep step (1), (2), (4), (5) constant, the curing time changed the step in (3) is
24,25,26,27,29,30,31,32 hours, the extraction rate of vanadium was 93.17-98.36%, and CaO content is lower than 1.1 in leachate
μ g/mL, most of CaO are present in leaching slag with calcium sulfate slag.
Embodiment 5
(1) bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 0.96%, CaO are 10.12%) 125 tons, and 45 tons of progress wet millings of recirculated water are added into ball mill 17
10min, the ore grinding yield of high calcium bone coal are 25 ton/hours, obtain the ore pulp that granularity is 120 mesh.
(2) ore pulp control valve 301 is opened, ore pulp is continuously flowed into closed pond 1 by PVC mixture conveyance conduit 1701
In, while opening sulfuric acid control valve 302 and 50 tons of concentrated sulfuric acids (being checked and approved with sulfuric acid metering pump 11) is added into closed pond 1, the two is certainly
Row mixing, obtains sposh shape mixture;When inputting ore pulp and the concentrated sulfuric acid, closes the extraction opening 2 in closed pond 1, opens exhaust control
Valve 501 and exhaust fan I 6 processed, are transported to eluting column 7 for the exhaust gas in closed pond 1 and carry out absorption processing.
(3) when in closed pond 1 high calcium bone coal reach 125 ton hours, continue in maturing process close extraction opening 2, close simultaneously
Ore pulp control valve 301 and gas exhausting valve 501 are closed, stops exhaust fan I 6 and operates, keeping entire closed pond 1 is closed state, dimension
165 DEG C of curing temperature are held, pressure 0.18MP range is cured, high calcium bone coal cures 30h in closed pond 1.
(4) when curing finishes, opening gas exhausting valve 501 simultaneously opens exhaust fan I 6, and the mixture in closed pond 1 is existed
The gas generated in stacking process, which is transported in eluting column 7, carries out purified treatment, and purified gas is discharged by gas outlet 8;
When exhaust gas is completely exhausted out, extraction opening 2 is opened.
(5) after the completion of gas purification processing, the extraction opening 2 in closed pond 1 is opened, 275 tons of recirculated waters are added, use air compressor machine
The leaching that 1.8h carries out vanadium is stirred in air-blowing, then extracts solidliquid mixture out from the acid-proof pump of extraction opening 2, and be transported to plate compression
Machine is separated by solid-liquid separation, and is obtained the leaching vanadium liquid of blue, is used to prepare vanadium product.
Using V in iron ammonium sulfate oxidation reduction titration measurement high calcium bone coal and filter residue2O5Content, obtain high calcium stone
V in coal2O5Extraction rate be 96.48%, and in the gas after eluting column purified treatment be free of SO2、CO2, the exhaust gas such as HCl, it is full
Sufficient gas discharge standard.
In this embodiment, keep step (1), (2), (3), (4) constant, change the step the solid-to-liquid ratio in (5) be 1:2,
The extraction rate of 1:2.1,1:2.4,1:2.6,1:2.8,1:3.0 (kg/L), vanadium are 93.43-96.79%, and solid-to-liquid ratio is to extraction rate
Influence it is little.CaO content is present in leaching slag lower than 1.1 μ g/mL, most of CaO with calcium sulfate slag in leachate.
Embodiment 6
(1) bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 0.96%, CaO are 9.78%) 120 tons, and 38.4 tons of progress wet millings of recirculated water are added into ball mill 17
10min, the ore grinding yield of high calcium bone coal are 25 ton/hours, obtain the ore pulp that granularity is 100 mesh.
(2) ore pulp control valve 301 is opened, ore pulp is continuously flowed into closed pond 1 by PVC mixture conveyance conduit 1701
In, while opening sulfuric acid control valve 302 and 49.2 tons of concentrated sulfuric acids (being checked and approved with sulfuric acid metering pump 11), the two are added into closed pond 1
It voluntarily mixes, obtains sposh shape mixture;When inputting ore pulp and the concentrated sulfuric acid, closes the extraction opening 2 in closed pond 1, opens exhaust
Exhaust gas in closed pond 1 is transported to eluting column 7 and carries out absorption processing by control valve 501 and exhaust fan I 6.
(3) when in closed pond 1 high calcium bone coal reach 120 ton hours, continue in maturing process close extraction opening 2, close simultaneously
Ore pulp control valve 301 and gas exhausting valve 501 are closed, stops exhaust fan I 6 and operates, keeping entire closed pond 1 is closed state, dimension
145 DEG C of curing temperature are held, pressure 0.18MP range is cured, high calcium bone coal cures 26h in closed pond 1.
(4) when curing finishes, opening gas exhausting valve 501 simultaneously opens exhaust fan I 6, and the mixture in closed pond 1 is existed
The gas generated in stacking process, which is transported in eluting column 7, carries out purified treatment, and purified gas is discharged by gas outlet 8;
When exhaust gas is completely exhausted out, extraction opening 2 is opened.
(5) after the completion of gas purification processing, the extraction opening 2 in closed pond 1 is opened, 200 tons of recirculated waters are added, use air compressor machine
The leaching that 2.2h carries out vanadium is stirred in air-blowing, then extracts solidliquid mixture out from the acid-proof pump of extraction opening 2, and be transported to plate compression
Machine is separated by solid-liquid separation, and is obtained the leaching vanadium liquid of blue, is used to prepare vanadium product.
Using V in iron ammonium sulfate oxidation reduction titration measurement high calcium bone coal and filter residue2O5Content, obtain high calcium stone
V in coal2O5Extraction rate be 97.16%, and in the gas after eluting column purified treatment be free of SO2、CO2, the exhaust gas such as HCl, it is full
Sufficient gas discharge standard.
In this embodiment, it keeps step (1), (2), (3), (4) constant, changes the step the air-blowing mixing time in (5)
For 1.5,1.8,2.1,2.3,2.4,2.5h, the extraction rate of vanadium is 93.43-97.74%.CaO content is lower than 1.1 μ in leachate
G/mL, most of CaO are present in leaching slag with calcium sulfate slag.
Embodiment 7
The bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 1.57%, CaO are 10.46%) 110 tons, 35 tons of recirculated water, 40 tons of the concentrated sulfuric acid.
Other operating procedures are 92.26-98.23% with embodiment 1, the extraction rate of vanadium.
Embodiment 8
The bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 1.57%, CaO are 10.46%) 115 tons, 40 tons of recirculated water, 45 tons of the concentrated sulfuric acid.
Other operating procedures are 94.13-99.15% with embodiment 1, the extraction rate of vanadium.
Embodiment 9
The bulk for taking vibrating screen to screen is less than the blocky high calcium bone coal (V of 10cm, water content 8%2O5Mass content be
The mass content of 1.57%, CaO are 10.46%) 120 tons, 35 tons of recirculated water, 45 tons of the concentrated sulfuric acid.
Other operating procedures are 95.32-97.87% with embodiment 1, the extraction rate of vanadium.
Comparative example 1
Operating method is same as Example 1, the difference is that, the high calcium bone coal in step (1) first dries 2 at 100 DEG C
It, carries out dry method ore grinding, and powder size is 80 mesh, and the yield of ball mill is 5-6 ton/hours, 105 decibels of noise, dust surpass
Mark.Baking process is increased in this comparative example 1, relatively time-consuming, mill efficiency is low, and noise is big, dust pollution is serious.
Comparative example 2
Dry method ore grinding is carried out by comparative example 1, dry powder and water 100:12 in mass ratio are stirred in blender, then
40% concentrated sulfuric acid is added by dry powder quality, is stirred, is deposited in closed pond in blender), the extraction rate of vanadium is
89.78%.In this comparative example 2, mixture is stirred in blender, causes blender to stop over and is cleared up, work
It is poor to make efficiency.One of agitating procedure is increased compared to embodiment 1-8.
Comparative example 3
Operating method is same as Example 1, the difference is that, step (2) is opened close when inputting ore pulp and the concentrated sulfuric acid
It closes the extraction opening in pond, close gas exhausting valve and exhaust fan, the exhaust gas in closed pond is handled without absorption.In step (3)
Keeping entire closed pond is open state.Curing temperature is at 90-105 DEG C in this comparative example 3, and vanadium extraction rate is in 69-76%;Simultaneously
It is diffused with a large amount of white irritating smog pollution environment above closed pond, influences entire production environment.
By above-described embodiment and comparative example, it is found that the present invention has, scale of investment is small, production cost is low, industrialized production is simple
The advantages that single, easy to operate, V leaching rate is high.It can also make full use of closed pond that there is heat-insulation and heat-preservation, collect exhaust gas, a pond two
With the characteristics of, build accumulation pond more, then kiloton high calcium bone coal in disposable maturation process carries out plus water, air-blowing agitation leacs,
Consecutive production vanadium product according to a conventional method.The high calcium bone coal raw ore that the present invention uses is not necessarily to ore dressing, decarburization, calcination process, keeps away
Exempt from that energy consumption is excessive, unfavorable factor of exhaust emission, has been a kind of environmentally protective extraction vanadium method.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes are obvious for the those of ordinary skill in art field.
Claims (10)
1. a kind of method for extracting vanadium from high calcium bone coal, which is characterized in that this method uses system as described below, the system
Include:
Closed pond (1), sulphuric acid tank (13), ball mill (17);
The closed pond (1) connect with the sulphuric acid tank (13) and the ball mill (17) respectively;
This method comprises:
Step S1: high calcium bone coal and water are input in ball mill (17) and carry out wet milling, obtains the ore pulp of mobility;
Step S2: the ore pulp of mobility is input in closed pond (1), while by sulphuric acid tank (13) being input to the concentrated sulfuric acid close
It closes in pond (1), high calcium bone coal is carried out to obtain the Curing material of sposh shape from thermal maturation;
Step S3: to closed pond (1) Zhong Jiashui, and air-blowing is stirred, and to carry out the leaching of vanadium, obtains solidliquid mixture;
Step S4: the solidliquid mixture in closed pond (1) being extracted out, is separated by solid-liquid separation, and obtains leaching vanadium solution.
2. according to the method described in claim 1, wherein,
The system also includes eluting column (7) and lye pond (10), it is provided with gas vent (4) at the top of the closed pond (1), it is described
Eluting column (7) is connect with the gas vent (4) by exhaust pipe (5);The lye pond (10) passes through high-pressure pump (9) and the leaching
Injection spray pipe (701) connection in tower (7) is washed, the injection spray pipe (701) is for spraying NaOH/H2O2Mix aqueous alkali;
The method also includes the exhaust gas generated in self-heating maturing process in step S2 is transported in eluting column (7) to absorb
Processing.
3. method according to claim 1 or 2, wherein
Content >=8.14wt% of CaO in the high calcium bone coal.
4. method according to claim 1 or 2, wherein V in the high calcium bone coal2O5Mass fraction be 0.8~
2.1%.
5. method according to claim 1 or 2, wherein in step S1, relative to high calcium bone coal, the additional amount of water is 28
~38wt%.
6. method according to claim 1 or 2, wherein in step S2, relative to the high calcium bone coal in step S1, dense sulphur
The additional amount of acid is 38~45wt%.
7. method according to claim 1 or 2, wherein in step S3, relative to the high calcium bone coal in 1kg step S1, water
Additional amount be 2~3L.
8. method according to claim 1 or 2, wherein in step S1, the time of wet milling is 10~20min, is obtained
Mobility ore pulp partial size be 80~120 mesh.
9. method according to claim 1 or 2, wherein in step S2, the time of curing is 24~32h, the temperature of curing
It is 135~165 DEG C, pressure when curing is 0.12~0.18MPa.
10. method according to claim 1 or 2, wherein in step S3, the time of air-blowing stirring is 1~2.5h, air-blowing
Stirring uses air compressor, and pressure is 6~10MPa.
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CN112921189A (en) * | 2021-02-03 | 2021-06-08 | 四川大学 | Method for extracting low-valence vanadium from vanadium-containing mineral through pressure leaching |
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