CN106853985A - Method of the treatment containing vanadium mud - Google Patents
Method of the treatment containing vanadium mud Download PDFInfo
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- CN106853985A CN106853985A CN201510894924.5A CN201510894924A CN106853985A CN 106853985 A CN106853985 A CN 106853985A CN 201510894924 A CN201510894924 A CN 201510894924A CN 106853985 A CN106853985 A CN 106853985A
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- Prior art keywords
- containing vanadium
- mud
- titanium tetrachloride
- vanadium
- solid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The method containing vanadium mud is processed the invention discloses a kind of, titanium tetrachloride is contained in the mud containing vanadium, methods described includes:(1) vanadium mud will be contained to be supplied to the chlorination furnace from chlorination furnace top, so that the mud containing vanadium is contacted with the heat smoke produced in the chlorination furnace, the mixed gas containing gaseous titanium tetrachloride and containing vanadium solid will be obtained;(2) mixed gas containing gaseous titanium tetrachloride and containing vanadium solid are carried out into gas solid separation treatment in dust-precipitator, to respectively obtain titanium tetrachloride and solid containing vanadium.The method can be realized to the continuous processing containing vanadium mud, and titanium tetrachloride is high with the separative efficiency of solid containing vanadium in mud containing vanadium, such that it is able to fully reclaim titanium tetrachloride.
Description
Technical field
The invention belongs to chloridising production titanium dioxide technical field, specifically, vanadium mud is contained the present invention relates to a kind for the treatment of
Method.
Background technology
Fluidizing chlorination method production rutile type titanium white technique mainly includes chlorination, crude titanic chloride condensation, crude titanic chloride essence
System, oxidation, the several parts of post processing of base-material, wherein crude titanic chloride are continuously removed during vanadium using mineral oil, per hour
Solid content is discharged in 15wt% or so mud containing vanadium 7-10t, the continuous and steady operation of technique is just can guarantee that, if not into
Ripe technology is processed the mud discharged in time, it will the carrying out of serious obstruction production, is evaporated for existing mud
Technique, the treatment to mud not only needs newly-increased processing unit, in addition it is also necessary to heat energy is additionally provided, so as to significantly increase fortune
Row cost, while titanium tetrachloride and being completely separated containing vanadium mud can't completely be realized.
Therefore, technology of the treatment containing vanadium mud is further improved in existing titanic chloride production process.
The content of the invention
It is contemplated that at least solving one of technical problem in correlation technique to a certain extent.Therefore, one of the invention
Purpose is to propose a kind of method for processing and containing vanadium mud, and the method can be realized to the continuous processing containing vanadium mud, and is contained
Titanium tetrachloride is high with the separative efficiency of solid containing vanadium in vanadium mud, such that it is able to fully reclaim titanium tetrachloride.
In one aspect of the invention, the present invention proposes a kind of method for processing and containing vanadium mud.Embodiments in accordance with the present invention,
Contain titanium tetrachloride in the mud containing vanadium.According to a particular embodiment of the invention, methods described includes:
(1) vanadium mud will be contained to be supplied to the chlorination furnace from chlorination furnace top, so that the mud containing vanadium and the chlorine
Change the heat smoke contact produced in stove, obtain the mixed gas containing gaseous titanium tetrachloride and containing vanadium solid;
(2) mixed gas containing gaseous titanium tetrachloride and containing vanadium solid are carried out into gas solid separation treatment in dust-precipitator,
To respectively obtain titanium tetrachloride and solid containing vanadium.
Thus, method of the treatment containing vanadium mud according to embodiments of the present invention can be realized to the continuous processing containing vanadium mud, and
And titanium tetrachloride is high with the separative efficiency of solid containing vanadium in mud containing vanadium, such that it is able to fully reclaim titanium tetrachloride.
In addition, method of the treatment containing vanadium mud according to the above embodiment of the present invention can also have following additional technical characteristic:
In some embodiments of the invention, the mud containing vanadium is crude titanic chloride to be carried out using mineral oil refining except vanadium mistake
Journey.
In some embodiments of the invention, in step (1), by the mud containing vanadium through the urgency on chlorination furnace top
Shower nozzle in cold tower is injected in the chlorination furnace.Thus, it is possible to so that mud containing vanadium fully connects with the heat smoke in chlorination furnace
Touch, so as to further improve the organic efficiency of titanium tetrachloride.
In some embodiments of the invention, in step (1), the temperature of the heat smoke is 500~700 degrees Celsius.By
This, can further improve the organic efficiency of titanium tetrachloride.
In some embodiments of the invention, in step (2), into the dust-precipitator is containing gaseous titanium tetrachloride and contains
The temperature of the mixed gas of vanadium solid is 200~350 degrees Celsius.Thus, it is possible to heat balance in guarantee system, so as to ensure
The stability of system.
In some embodiments of the invention, the addition containing vanadium mud is by the temperature on the dust-precipitator suction line
Regulating valve on meter and the shower nozzle is controlled.Thus, it is possible to the Automated condtrol in realizing whole process, so as to improve
Treatment effeciency containing vanadium mud.
In some embodiments of the invention, when the mud containing vanadium is not enough, to supplying crude titanic chloride in the chlorination furnace
Or refined titanic chloride.Thus, it is possible to system entirety heat and material balance are maintained, so as to further improve the stability of a system.
Additional aspect of the invention and advantage will be set forth in part in the description, and partly will from the following description become bright
It is aobvious, or recognized by practice of the invention.
Brief description of the drawings
Of the invention above-mentioned and/or additional aspect and advantage will be apparent from description of the accompanying drawings below to embodiment is combined
Be readily appreciated that, wherein:
Fig. 1 is method flow schematic diagram of the treatment containing vanadium mud according to an embodiment of the invention;
Fig. 2 is method flow schematic diagram of the treatment containing vanadium mud according to further embodiment of the present invention.
Specific embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein identical from start to finish
Or similar label represents same or similar element or the element with same or like function.Retouched below with reference to accompanying drawing
The embodiment stated is exemplary, it is intended to for explaining the present invention, and be not considered as limiting the invention.
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", " on ", D score, "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outward ",
The orientation or position relationship of the instruction such as " clockwise ", " counterclockwise ", " axial direction ", " radial direction ", " circumference " are based on shown in the drawings
Orientation or position relationship, are for only for ease of the description present invention and simplify and describe, rather than indicate or imply signified device or
Element with specific orientation, with specific azimuth configuration and operation, therefore must be not considered as limiting the invention.
Additionally, term " first ", " second " be only used for describe purpose, and it is not intended that indicate or imply relative importance or
Person implies the quantity of the technical characteristic for indicating indicated.Thus, define " first ", the feature of " second " can express or
Implicitly include at least one this feature.In the description of the invention, " multiple " is meant that at least two, such as two,
Three etc., unless otherwise expressly limited specifically.
In the present invention, unless otherwise clearly defined and limited, the art such as term " installation ", " connected ", " connection ", " fixation "
Language should be interpreted broadly, for example, it may be fixedly connected, or be detachably connected, or integrally;Can be machinery
Connection, or electrical connection;Can be joined directly together, it is also possible to be indirectly connected to by intermediary, can be two units
Connection or two interaction relationships of element inside part, unless otherwise clearly restriction.For the ordinary skill of this area
For personnel, above-mentioned term concrete meaning in the present invention can be as the case may be understood.
In the present invention, unless otherwise clearly defined and limited, fisrt feature second feature " on " or D score can be
One and second feature directly contact, or the first and second features pass through intermediary mediate contact.And, fisrt feature is
Two features " on ", " top " and " above " but fisrt feature are directly over second feature or oblique upper, or are merely representative of first
Characteristic level is highly higher than second feature.Fisrt feature second feature " under ", " lower section " and " below " can be fisrt feature
Immediately below second feature or obliquely downward, or fisrt feature level height is merely representative of less than second feature.
In one aspect of the invention, the present invention proposes a kind of method for processing and containing vanadium mud.Embodiments in accordance with the present invention,
The mud containing vanadium contains titanium tetrachloride.According to a particular embodiment of the invention, the method includes:(1) will contain vanadium mud from
In chlorination furnace top supply to the chlorination furnace, so that the mud containing vanadium connects with the heat smoke of generation in the chlorination furnace
Touch, obtain the mixed gas containing gaseous titanium tetrachloride and containing vanadium solid;(2) will be described containing gaseous titanium tetrachloride and containing vanadium
The mixed gas of solid carry out gas solid separation treatment in dust-precipitator, to respectively obtain titanium tetrachloride and solid containing vanadium.Invention
People has found, is supplied to chlorination furnace by that will contain vanadium mud so that mud containing vanadium inversely connects with the heat smoke of generation in chlorination furnace
Touch, it is gaseous titanium tetrachloride that the titanium tetrachloride in mud containing vanadium is gasified, so as to be again to be capable of achieving tetrachloro through follow-up dust-precipitator
Change titanium and efficiently separating containing vanadium solid, and the rate of recovery of gained titanium tetrachloride is (rate of recovery reaches 99%) high, more existing skill
The evaporation technology that cardia mud containing vanadium is used is compared, and the application need not increase processing unit newly, but ingenious utilization chlorination
In stove occur chlorination reaction produced by heat smoke waste heat mud containing vanadium is processed, so as to significantly improve titanium tetrachloride with
Processing cost is reduced while the separative efficiency of solid containing vanadium.
The method of the treatment containing vanadium mud of the embodiment of the present invention is described in detail below with reference to Fig. 1-2.It is of the invention
Embodiment, the method includes:
S100:Vanadium mud will be contained to be supplied to the chlorination furnace from chlorination furnace top
Embodiments in accordance with the present invention, will contain vanadium mud and be supplied to chlorination furnace from chlorination furnace top so that mud containing vanadium and chlorine
Change the heat smoke contact produced in stove, such that it is able to obtain the mixed gas containing gaseous titanium tetrachloride and containing vanadium solid.Invention
People has found, is supplied to chlorination furnace by that will contain vanadium mud so that mud containing vanadium inversely connects with the heat smoke of generation in chlorination furnace
Touch, it is gaseous titanium tetrachloride that the titanium tetrachloride in mud containing vanadium is gasified, so as to be again to be capable of achieving tetrachloro through follow-up dust-precipitator
Change titanium and efficiently separating containing vanadium solid, and the rate of recovery of gained titanium tetrachloride is (rate of recovery reaches 99%) high, more existing skill
The evaporation technology that cardia mud containing vanadium is used is compared, and the application need not increase processing unit newly, but ingenious utilization system
There is the heat smoke waste heat produced by chlorination reaction in internal chlorination furnace to process mud containing vanadium, so as to significantly improve four
Processing cost is reduced while titanium chloride is with the separative efficiency of solid containing vanadium.It should be noted that, " chlorination furnace " herein is existing
There is the boiling chloridizing furnace for being used of production titanium dioxide in technology.
Specifically, the production of heat smoke be mainly to continuously added in chlorination furnace titanium ore (high titanium slag or rutile), also
Immunogenic substance (petroleum coke), and continuously to being passed through oxygen, compressed air, Cl in reactor2;And temperature reaches chlorine
When changing reaction temperature, titanium ore (high titanium slag or rutile) and chlorine recur reaction and are continuously generated TiCl4Gas, reaction side
Formula is:2TiO2+3C+4Cl2=2TiCl4+2CO+CO2, i.e. heat smoke is titanium tetrachloride, carbon monoxide and carbon dioxide
Admixture of gas.
According to one embodiment of present invention, the temperature of heat smoke is not particularly restricted, and those skilled in the art can basis
It is actually needed and is selected, according to a particular embodiment of the invention, the temperature of heat smoke can be 500~700 degrees Celsius.By
This, it is ensured that titanium tetrachloride high-efficiency gasification in mud containing vanadium, so as to significantly improve the organic efficiency of titanium tetrachloride.
According to still a further embodiment, the source containing vanadium mud is not particularly restricted, as long as wherein containing four chlorinations
Titanium, according to a particular embodiment of the invention, mud containing vanadium can be that refined removing is carried out to crude titanic chloride using mineral oil
During vanadium.Specifically, liquid crude titanic chloride is carried out except vanadium treatment using mineral oil in evaporator, can be by wherein
Lower boiling VOCl2It is converted into high boiling VOCl3, be then evaporated treatment, refined titanic chloride in the form of a vapor from
Rectifying column at the top of evaporator enters into the condensed refined titanic chloride to liquid of condenser system of postorder, remaining after evaporation liquid
Body is mud containing vanadium.
According to still another embodiment of the invention, mud containing vanadium can be sprayed into through the shower nozzle in the chilling tower on chlorination furnace top
To in chlorination furnace.Inventor has found, is inversely connect with heat smoke to chlorination furnace by that will be contained vanadium mud and be supplied using shower nozzle
Touch, can cause that mud containing vanadium is fully contacted heat exchange with heat smoke, such that it is able to improve the gasification efficiency of titanium tetrachloride, and then
Improve the rate of recovery of titanium tetrachloride.
S200:Mixed gas containing gaseous titanium tetrachloride and containing vanadium solid are carried out into gas solid separation treatment in dust-precipitator
Embodiments in accordance with the present invention, the mixed gas containing gaseous titanium tetrachloride and containing vanadium solid obtained above are being gathered dust
Gas solid separation treatment is carried out in device, such that it is able to respectively obtain titanium tetrachloride and solid containing vanadium.Specifically, isolated gas
State titanium tetrachloride is refined into subsequent condensation operation to titanium tetrachloride, and is contained vanadium solid and settled in the presence of gravity gathers dust
To dust-precipitator bottom, will be contained vanadium solid and be supplied by the opening and closing of valve of bottom two carries out harmless treatment to pulping tank slurrying.
According to one embodiment of present invention, into the gaseous mixture containing gaseous titanium tetrachloride and containing vanadium solid of the dust-precipitator
The temperature of body is not particularly restricted, and those skilled in the art can be selected according to actual needs, tool of the invention
Body embodiment, the temperature into the mixed gas containing gaseous titanium tetrachloride and containing vanadium solid of the dust-precipitator can be
200~350 degrees Celsius.Inventor find, if into the mixed gas of dust-precipitator temperature it is low when may cause titanium tetrachloride liquid
Change causes the blocking of dust collecting system, and the temperature of the mixed gas into dust-precipitator it is high when can increase the pressure of postorder condenser system,
And can also cause the change of whole system temperature and pressure while production capacity is reduced.Thus, containing for dust-precipitator will be entered
The temperature of gaseous titanium tetrachloride and the mixed gas containing vanadium solid is maintained at 200~350 degrees Celsius and can not only avoid dust collecting system
Blocking, and the pressure of follow-up postorder condenser system can be reduced.
According to still a further embodiment, the addition containing vanadium mud is by the thermometer on the dust-precipitator suction line
It is controlled with the regulating valve on the shower nozzle.Specifically, temperature monitor is provided with the inlet duct of dust-precipitator, the temperature
Degree detector be connected with the regulating valve of chilling tower upper nozzle, control entrance dust-precipitator gas-solid mixture temperature 200-350 DEG C it
Between, valve can automatically adjust aperture until closing, valve opening can gradually be held greatly when temperature is high when temperature is low, and set
Shower nozzle is multiple, and closing and opening is adjusted successively according to the change of temperature, such that it is able to keep system internal heat
Balance, it is ensured that system continuous and steady operation, and it is possible to prevente effectively from the blocking of dust-precipitator tremie pipe is to chlorination furnace ebullated bed
Influence, while in order to keep system overall thermal amount and material balance, when mud containing vanadium is not enough, can be supplied in chlorination furnace
Crude titanic chloride or refined titanic chloride are fed.
As described above, method of the treatment containing vanadium mud according to embodiments of the present invention can have the advantages that to be selected from it is following at least it
One:
Method of the treatment containing vanadium mud according to embodiments of the present invention can utilize the heat and equipment of system itself to mud containing vanadium
Processed, saved cost.
Method of the treatment containing vanadium mud according to embodiments of the present invention can make titanium tetrachloride realize thoroughly dividing with solid impurity
From, the titanium tetrachloride separated is entered Collection utilization after condenser system condensation, improve the rate of recovery of titanium tetrachloride, four
The rate of recovery of titanium chloride reaches 99%.
By the thermometer and regulating valve on dust-precipitator suction line in method of the treatment containing vanadium mud according to embodiments of the present invention
Carry out addition of the chain control containing vanadium mud, it is ensured that the heat balance of system, the dust-precipitator tremie pipe for effectively avoiding
Block and the influence to chlorination furnace ebullated bed.
Method of the treatment containing vanadium mud according to embodiments of the present invention is entirely Automated condtrol in the whole process of mud conditioning,
And do not result in secondary pollution.
Understand for convenience, the method for the treatment containing vanadium mud of the embodiment of the present invention is described in detail below with reference to Fig. 2.
First, after the crude titanic chloride that chloridization process is produced evaporates in evaporator with mineral oil, refined titanic chloride
The rectifying column from the top of evaporator enters into condensed smart four chlorination to liquid of condenser system of postorder in the form of a vapor
Titanium, the mud containing vanadium after evaporation in base of evaporator is pumped into the groove of slurry collecting containing vanadium by the mud of base of evaporator, then
The chilling tower got at the top of chlorination furnace by the groove pump of slurry collecting containing vanadium is injected in chlorination furnace by shower nozzle, in the process containing vanadium
Mud directly connects during landing from the top down under gravity with 500-700 DEG C of heat smoke of rising in boiling chloridizing furnace
Touch so that the titanium tetrachloride in mud is gasified during decline, solid containing vanadium also gathers dust with the mixed gas entrance in stove
Device, solid material containing vanadium is deposited to dust-precipitator bottom in the presence of gravity gathers dust, and is made by the opening and closing of two valves in bottom solid
Body material carries out harmless treatment after entering into pulping tank slurrying, and passes through the titanium tetrachloride gases entrance that dust-precipitator is separated
Follow-up condensation procedure is condensed, and stable to ensure the gas temperature for entering dust-precipitator, and four may be caused when temperature is low
Titanium chloride liquefaction causes the blocking of dust collecting system, the pressure of postorder condenser system can be increased when temperature is high, and reducing production capacity
While can also cause the change of whole system temperature and pressure, be that this is provided with temperature detection on the inlet duct of dust-precipitator
The valve of each shower nozzle entrance on instrument, the temperature monitor and chilling tower is chain, and control enters the gas-solid mixture temperature of dust-precipitator
Between 200-350 DEG C, valve can automatically adjust aperture until closing, valve opening can gradually be held when temperature is high to degree when temperature is low
Greatly, and set shower nozzle for multiple, close and open all be to be adjusted successively according to the change of temperature.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specific example ",
Or the description of " some examples " etc. means to combine specific features, structure, material or feature bag that the embodiment or example are described
It is contained at least one embodiment of the invention or example.In this manual, to the schematic representation of above-mentioned term necessarily
It is directed to identical embodiment or example.And, the specific features of description, structure, material or feature can be any
Combined in an appropriate manner in individual or multiple embodiments or example.Additionally, in the case of not conflicting, the skill of this area
Can be combined for the feature of the different embodiments or example described in this specification and different embodiments or example by art personnel
And combination.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment be it is exemplary,
It is not considered as limiting the invention, one of ordinary skill in the art within the scope of the invention can be to above-described embodiment
It is changed, changes, replacing and modification.
Claims (7)
1. it is a kind of to process the method containing vanadium mud, contain titanium tetrachloride in the mud containing vanadium, it is characterised in that methods described
Including:
(1) vanadium mud will be contained to be supplied to the chlorination furnace from chlorination furnace top, so that the mud containing vanadium and the chlorine
Change the heat smoke contact produced in stove, obtain the mixed gas containing gaseous titanium tetrachloride and containing vanadium solid;
(2) mixed gas containing gaseous titanium tetrachloride and containing vanadium solid are carried out into gas solid separation treatment in dust-precipitator,
To respectively obtain titanium tetrachloride and solid containing vanadium.
2. method according to claim 1, it is characterised in that the mud containing vanadium is to thick four chlorination using mineral oil
Titanium carries out refined except vanadium process.
3. method according to claim 1 and 2, it is characterised in that in step (1), will the mud containing vanadium
It is injected in the chlorination furnace through the shower nozzle in the chilling tower on chlorination furnace top.
4. the method according to claim any one of 1-3, it is characterised in that in step (1), the heat smoke
Temperature be 500~700 degrees Celsius.
5. method according to claim 4, it is characterised in that in step (2), into containing for the dust-precipitator
The temperature for having gaseous titanium tetrachloride and the mixed gas containing vanadium solid is 200~350 degrees Celsius.
6. the method according to claim 4 or 5, it is characterised in that the addition containing vanadium mud is by the receipts
The regulating valve on thermometer and the shower nozzle on dirt device suction line is controlled.
7. method according to claim 6, it is characterised in that when the mud containing vanadium is not enough, to the chlorination furnace
Interior supply crude titanic chloride or refined titanic chloride.
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Cited By (5)
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CN107857295A (en) * | 2017-11-13 | 2018-03-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Organic matter removes vanadium mud energy saving resources Application way and device |
CN109250751A (en) * | 2018-10-26 | 2019-01-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Handle the method that titanium tetrachloride purification removes vanadium mud |
CN110871140A (en) * | 2019-10-29 | 2020-03-10 | 山东鲁北企业集团总公司 | System and method for recovering titanium tetrachloride from titanium tetrachloride suspension |
CN111533164A (en) * | 2020-01-03 | 2020-08-14 | 中信钛业股份有限公司 | Vanadium removal method for titanium tetrachloride in boiling chlorination system |
CN113666417A (en) * | 2021-09-13 | 2021-11-19 | 攀钢集团钒钛资源股份有限公司 | Vanadium-containing slurry separation method and device |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107857295A (en) * | 2017-11-13 | 2018-03-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Organic matter removes vanadium mud energy saving resources Application way and device |
CN109250751A (en) * | 2018-10-26 | 2019-01-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Handle the method that titanium tetrachloride purification removes vanadium mud |
CN110871140A (en) * | 2019-10-29 | 2020-03-10 | 山东鲁北企业集团总公司 | System and method for recovering titanium tetrachloride from titanium tetrachloride suspension |
CN110871140B (en) * | 2019-10-29 | 2021-05-07 | 山东鲁北企业集团总公司 | System and method for recovering titanium tetrachloride from titanium tetrachloride suspension |
CN111533164A (en) * | 2020-01-03 | 2020-08-14 | 中信钛业股份有限公司 | Vanadium removal method for titanium tetrachloride in boiling chlorination system |
CN111533164B (en) * | 2020-01-03 | 2023-10-10 | 中信钛业股份有限公司 | Vanadium removal method for titanium tetrachloride in boiling chlorination system |
CN113666417A (en) * | 2021-09-13 | 2021-11-19 | 攀钢集团钒钛资源股份有限公司 | Vanadium-containing slurry separation method and device |
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