CN107098386A - The system and method for preparing synthetic rutile - Google Patents
The system and method for preparing synthetic rutile Download PDFInfo
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- CN107098386A CN107098386A CN201710461320.0A CN201710461320A CN107098386A CN 107098386 A CN107098386 A CN 107098386A CN 201710461320 A CN201710461320 A CN 201710461320A CN 107098386 A CN107098386 A CN 107098386A
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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
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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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
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses the system and method for preparing synthetic rutile, system includes：Cinder ladle；Reaction unit；Injection tube, its port of export is extended in reaction zone, and injection tube includes oxidizing gas conveyance conduit, nitrogen gas delivery-line and crystal seed conveyance conduit, wherein, oxidizing gas conveyance conduit is made up of the first segment pipe and second segment pipeline, is enclosed on outside nitrogen delivery pipe on second segment pipeline；Crystal seed entrance and the control valve positioned at crystal seed entrance downstream are provided with crystal seed conveyance conduit, crystal seed conveyance conduit is set up in parallel with the first segment pipe and the entrance of crystal seed conveyance conduit is connected with the entrance of the first segment pipe, and the outlet of crystal seed conveyance conduit is connected with the outlet of the first segment pipe；Breaker；Ore-dressing plant；Acid dip pickle and filter.The system, to oxidizing gas is blown inside titanium-containing molten and separated slag material, can significantly improve in titanium-containing molten and separated slag titanium compound to TiO using injection tube2Conversion ratio, so as to improve the titanium grade in the synthetic rutile prepared.
Description
Technical field
The present invention relates to field of metallurgy, specifically, the present invention relates to the system and method for preparing synthetic rutile.
Background technology
China's v-ti magnetite ore reserves extremely enriches, but traditional blast furnace-converter flow and rotary kiln-electric furnace route are all
Wherein most iron and most of vanadium can only be reclaimed, titanium resource therein can not realize recycling, cause huge resource
Waste and environmental problem.Compared to traditional blast furnace process, reduction shaft furnace-electric furnace, which melts split flow, can obtain vanadium-bearing hot metal and titaniferous
Melting slag, for realize iron, vanadium, titanium resource comprehensive utilization there is significant advantage.However, vanadium titano-magnetite reduction shaft furnace-
Electric furnace melts a point technology and remains in conceptual phase at present, has no industrialization report.Vanadium titano-magnetite reduction shaft furnace-electric furnace is molten to be got
To melting slag in TiO2Grade is relatively low, and only 50% or so, the content of calcium al-mg-si impurity is again higher, reaches 30~40%.
Over cure acid system titanium white route is had at present and reclaims the report of low-grade titanium-containing molten and separated slag, but is due to that impurity content therein is high,
Cause the acidolysis rate of melting slag relatively low, titanium concentration is low and hydrolyzes difficult, it is difficult to produce qualified titanium dioxide, and due to life
Produce high expensive, it is also difficult to realize industrialized production.On the other hand, the requirement of chloride process titanium dioxide and titanium sponge to rich-titanium material will show
Write and be higher than acid extracting titanium white, thus this low titanium grade richness titanium melting slag can not more meet chloride process titanium dioxide or titanium sponge will
Ask.From above angle analysis, the melting slag of low titanium grade reaches synthetic rutile or high-quality titanium slag firstly the need of upgrading is passed through
Titanium grade requirement could be directly as titanium white chloride and the raw material of titanium sponge production.
However, the existing means for preparing synthetic rutile still have much room for improvement.
The content of the invention
It is contemplated that at least solving one of technical problem in correlation technique to a certain extent.Therefore, the present invention
One purpose is the system and method that proposition prepares synthetic rutile.The system is using injection tube into titanium-containing molten and separated slag material
Portion is blown oxidizing gas, can significantly improve in titanium-containing molten and separated slag titanium compound to TiO2Conversion ratio, so as to improve preparation
Titanium grade in obtained synthetic rutile.
In the first aspect of the present invention, the present invention proposes a kind of system for preparing synthetic rutile.According to the present invention's
Embodiment, the system includes：
Electrode is provided with cinder ladle, the cinder ladle, the cinder ladle has high temperature titanium-containing molten and separated slag entrance, silica entrance and mixed
Close material outlet；
Defined in reaction unit, the reaction unit reaction zone and the mixed material entrance connected with the reaction zone and
Oxidation material is exported, and the mixed material entrance is connected with mixed material outlet；
Injection tube, the port of export of the injection tube is extended in the reaction zone, and the injection tube includes oxidizing gas
Conveyance conduit, nitrogen gas delivery-line and crystal seed conveyance conduit, wherein, the oxidizing gas conveyance conduit by the first segment pipe and
Second segment pipeline is constituted, and is enclosed on second segment pipe outside the nitrogen delivery pipe, the nitrogen delivery pipe have perpendicular to
The nitrogen inlet that the nitrogen delivery pipe is set；Crystal seed entrance is provided with the crystal seed conveyance conduit and is entered positioned at the crystal seed
The control valve in mouthful downstream, the crystal seed conveyance conduit is set up in parallel with first segment pipe and the crystal seed conveyance conduit enters
Mouth is connected with the entrance of first segment pipe, the outlet of the crystal seed conveyance conduit and the outlet phase of first segment pipe
Connection；
Breaker, the breaker has oxidation material entrance and material powders outlet, the oxidation material entrance
It is connected with oxidation material outlet；
There is ore-dressing plant, the ore-dressing plant material powders entrance, the outlet of thick titanium dioxide, chats outlet and mine tailing to go out
Mouthful, the material powders entrance is connected with material powders outlet, and the chats outlet is connected with the mixed material entrance；
Acid dip pickle, the acid dip pickle has thick titanium dioxide entrance, hydrochloric acid entrance and slurry outlet, the thick dioxy
Change titanium entrance with the thick titanium dioxide outlet to be connected；
Filter, the filter has slurry inlet, waste liquid outlet and synthetic rutile outlet, and the slurry enters
Mouth is connected with the slurry outlet.
The system for preparing synthetic rutile according to embodiments of the present invention is by the way that titanium-containing molten and separated slag and silica are supplied to slag
Batch mixing and insulation are carried out in bag, to obtain mixed material, and then mixed material is transferred in reaction unit, and using injection
Pipe is blown oxidizing gas into mixed material, so as to which the titanium compound in mixed material is oxidized into TiO2, obtain oxide
Material, completes to be blown crystal seeds of rutile in the backward material of injection, further to promote growing up for Rutile Type；Wherein, injection tube
The port of export extend to the inside of mixed material in reaction zone, so as to substantially improve the dynamic conditions of oxidation reaction, contracting
The short injection time, low price titanium compound is improved to TiO2Conversion ratio；And then, oxidation material is supplied into breaker progress
Break process, and obtained material powders are supplied into ore-dressing plant carry out ore dressing processing, so as to by rutile monomer and arteries and veins
Stone is separated, and obtains thick titanium dioxide, chats and mine tailing, is subsequently supplied into acid dip pickle thick titanium dioxide and is carried out at pickling
Reason, and the slurry that pickling processes are obtained is supplied into filter carry out filtration treatment, to obtain synthetic rutile product.
The system, to oxidizing gas is blown inside titanium-containing molten and separated slag material, is significantly improved in titanium-containing molten and separated slag by using injection tube
Titanium compound is to TiO2Conversion ratio, so as to improve the titanium grade in the synthetic rutile prepared.
In addition, the system according to the above embodiment of the present invention for preparing synthetic rutile can also have skill additional as follows
Art feature：
In some embodiments of the invention, the crystalline substance suitable for storage crystal seeds of rutile is defined in the crystal seed conveyance conduit
Plant storehouse.Thus, it is possible to by being blown crystal seeds of rutile into mixed material, further promote growing up for Rutile Type in material,
The particle diameter of Rutile Type is improved, more convenience is provided for follow-up ore dressing processing.
In some embodiments of the invention, the internal diameter of the oxidizing gas conveyance conduit is 10~15mm, the nitrogen
The internal diameter in letter shoot road is 28~35mm, and the internal diameter of the nitrogen inlet is 3~8mm, the oxidizing gas conveyance conduit
Thickness with the nitrogen gas delivery-line is 2~4mm.
In some embodiments of the invention, the axis of the crystal seed conveyance conduit discharging section and the oxidizing gas
The opening formed between conveyance conduit axis towards the angle of first segment pipe be 30~90 degree.
In some embodiments of the invention, the ore-dressing plant is shaking table, and the acid dip pickle is sealing leaching kettle.
In the second aspect of the present invention, the present invention propose a kind of use above-described embodiment prepare synthetic rutile be
Controlling for synthetic rutile method.Embodiments in accordance with the present invention, this method includes：By titanium-containing molten and separated slag and silica supply to
Batch mixing and insulation are carried out in cinder ladle, to obtain mixed material；The mixed material is transferred in reaction unit, and using spray
Blowpipe is blown oxidizing gas, nitrogen and crystal seeds of rutile into the mixed material, to carry out oxygen to the mixed material
Change and be modified, obtain oxidation material；The oxidation material is supplied into breaker and carries out break process, to obtain material powder
End；The material powders are supplied into ore-dressing plant and carry out ore dressing processing, to obtain thick titanium dioxide, chats and mine tailing；
The thick titanium dioxide and hydrochloric acid are supplied into acid dip pickle and carry out pickling processes, to obtain slurry；And by the slurry
Material supply carries out filtration treatment into filter, to obtain synthetic rutile.
Thus, the method for preparing synthetic rutile according to embodiments of the present invention is by the way that titanium-containing molten and separated slag and silica are supplied
Batch mixing and insulation are carried out into cinder ladle, to obtain mixed material, and then mixed material is transferred in reaction unit, and use
Injection tube is blown oxidizing gas into mixed material, so as to which the titanium compound in mixed material is oxidized into TiO2, obtain oxygen
Compound material, completes to be blown crystal seeds of rutile in the backward material of injection, further to promote growing up for Rutile Type；Wherein, spray
The port of export of blowpipe extends to the inside of mixed material in reaction zone, so as to substantially improve the dynamics bar of oxidation reaction
Part, shortens the injection time, improves low price titanium compound to TiO2Conversion ratio；And then, oxidation material is supplied to breaker
Middle carry out break process, and obtained material powders are supplied into ore-dressing plant carry out ore dressing processing, so as to by rutile list
Body is separated with gangue, obtains thick titanium dioxide, chats and mine tailing, is subsequently supplied into acid dip pickle thick titanium dioxide and is carried out acid
Processing is washed, and the slurry that pickling processes are obtained is supplied into filter carries out filtration treatment, to obtain synthetic rutile
Product.This method, to oxidizing gas is blown inside titanium-containing molten and separated slag material, significantly improves titaniferous and melted by using injection tube
Titanium compound is to TiO in point slag2Conversion ratio, so as to improve the titanium grade in the synthetic rutile prepared.
In addition, the method according to the above embodiment of the present invention for preparing synthetic rutile can also have skill additional as follows
Art feature：
In some embodiments of the invention, the mixed material is incubated to 40 under 1550~1600 degrees Celsius~
It is transferred to after 60min in the reaction unit.Thus, it is possible to further improve the titanium product in the synthetic rutile prepared
Position.
In some embodiments of the invention, the SiO in the silica2Content is not less than 90wt%, the silica plus
It is the 30~40% of the titanium-containing molten and separated slag quality to enter amount.Thus, it is possible to further improve in the synthetic rutile prepared
Titanium grade.
In some embodiments of the invention, CaO and SiO in the mixed material2Mass ratio be not higher than 0.8, SiO2With
TiO2Mass ratio be not higher than 1.6.Thus, it is possible to further improve the titanium grade in the synthetic rutile prepared.
In some embodiments of the invention, the oxidizing gas is oxygen or oxygen-nitrogen mixture, the oxygen nitrogen mixing
The volume fraction of oxygen is 20~90v% in gas.Thus, it is possible to further improve the titanium product in the synthetic rutile prepared
Position.
In some embodiments of the invention, the injection time is 10~30min, and the injection complete it is preceding 3~
5min, crystal seeds of rutile is blown until the injection is completed into the mixed material.Thus, it is possible to by into mixed material
Crystal seeds of rutile is blown, further promotes Rutile Type in material to grow up, improves the particle diameter of Rutile Type, be at follow-up ore dressing
Reason provides more convenience.
In some embodiments of the invention, the average grain diameter of the material powders is 74~150 microns.Thus, it is possible to
Further improve the ore dressing effect in follow-up ore dressing processing.
In some embodiments of the invention, the ore dressing processing is carried out using shaking table, the jig frequency of the shaking table for 300~
360 times/min, stroke is 8~12mm, and feed ore concentration is 20~40%, and wherein feed ore concentration refers to that material powders account for the matter of ore pulp
Fraction is measured, wherein ore pulp refers to the mixture of water and material powders.Preferably, jig frequency be 320~360 times/min, stroke be 8~
10mm, feed ore concentration is 30~35%.Thus, it is possible to further improve the titanium grade in the synthetic rutile prepared.
In some embodiments of the invention, the concentration of the hydrochloric acid is 10~20wt%, the hydrochloric acid and the material
The liquid-solid ratio of powder is 3~5:1, the pickling processes are to carry out 30~120min under 25~90 degrees Celsius to complete.It is preferred that
Ground, the concentration of the hydrochloric acid is 15~20wt%, and the liquid-solid ratio of the hydrochloric acid and the material powders is 2~4:1, the pickling
Processing is to carry out 60~90min under 70~90 degrees Celsius to complete.Thus, it is possible to further improve the artificial gold prepared
Titanium grade in red stone.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Brief description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become from description of the accompanying drawings below to embodiment is combined
Substantially and be readily appreciated that, wherein：
Fig. 1 is the system structure diagram according to an embodiment of the invention for preparing synthetic rutile；
Fig. 2 is blowing pipe structure schematic diagram according to an embodiment of the invention；
Fig. 3 is the method flow schematic diagram according to an embodiment of the invention for preparing synthetic rutile.
Embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein from beginning to end
Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached
The embodiment of figure description 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 ", " under ", "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outer ", " up time
The orientation or position relationship of the instruction such as pin ", " counterclockwise ", " axial direction ", " radial direction ", " circumference " be based on orientation shown in the drawings or
Position relationship, is for only for ease of the description present invention and simplifies description, rather than indicate or imply that the device or element of meaning must
There must be specific orientation, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are only used for describing purpose, and it is not intended that indicating or implying relative importance
Or the implicit quantity for indicating indicated technical characteristic.Thus, define " first ", the feature of " second " can express or
Implicitly include at least one this feature.
In the present invention, unless otherwise clearly defined and limited, term " connected " should be interpreted broadly, for example, can be with
It is to be fixedly connected or be detachably connected, or integrally；Can be mechanical connection or electrical connection；Can be straight
Connect connected, can also be indirectly connected to by intermediary, can be connection or the phase interaction of two elements of two element internals
With relation, unless otherwise clear and definite restriction.For the ordinary skill in the art, on can understanding as the case may be
State the concrete meaning of term in the present invention.
In the present invention, unless otherwise clearly defined and limited, fisrt feature can be with "above" or "below" second feature
It is that the first and second features are directly contacted, or the first and second features pass through intermediary mediate contact.Moreover, fisrt feature exists
Second feature " on ", " top " and " above " but fisrt feature are directly over second feature or oblique upper, or be merely representative of
Fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " lower section " and " below " can be
One feature is immediately below second feature or obliquely downward, or is merely representative of fisrt feature level height less than second feature.
In the first aspect of the present invention, the present invention proposes a kind of system for preparing synthetic rutile.According to the present invention's
Embodiment, with reference to Fig. 1~2, the system includes：Cinder ladle 100, reaction unit 200, injection tube 300, breaker 400, ore dressing dress
Put 500, acid dip pickle 600 and filter 700.
Electrode 110 is provided with embodiments in accordance with the present invention, cinder ladle 100, there is cinder ladle 100 high temperature titanium-containing molten and separated slag to enter
Mouth 101, silica entrance 102 and mixed material outlet 103, cinder ladle 100 are suitable to titanium-containing molten and separated slag and silica carrying out batch mixing and guarantor
Temperature, to obtain mixed material.Specifically, vanadium titano-magnetite is through the TiO in reduction-molten titanium-containing molten and separated slag got2Grade
About 50wt%, calcium magnalium impurity levels are up to 30~40wt%, titanium-containing molten and separated slag by molten separating device tapping temperature 1500~
1600 DEG C, it is directly entered after slagging tap in cinder ladle, and is incorporated into cinder ladle SiO2Content is not less than 90wt% silica, while using
The mode of heated by electrodes adjusts temperature of charge in cinder ladle to 1500~1600 DEG C, to obtain mixed material.
According to a particular embodiment of the invention, can be by mixed material at 1550~1600 DEG C after mixed material is obtained
It is transferred to after 40~60min of lower insulation in subsequent reactions device, inventor has found, by the way that mixed material progress insulation can be promoted
Enter the forming core of Rutile Type in modified slag with growing up, while viscosity coefficient of dross is relatively low at the temperature disclosed above, beneficial to rutile
Diffusion mass transfer of the component in slag, so that rutile agglomeration.
Embodiments in accordance with the present invention, the particle diameter of silica is not particularly restricted, and those skilled in the art can be according to reality
Border needs to be selected, according to a particular embodiment of the invention, and silica can be not higher than 2mm Cab-O-sil using average grain diameter,
And the content of powder in Cab-O-sil is not less than 90wt%.
Embodiments in accordance with the present invention, the addition of silica 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 addition of silica can be the 30 of titanium-containing molten and separated slag quality
~40%, specifically, silica can be combined the stable calcium silicates of generation with the CaO in slag, so that rutile separate out,
Reach the purpose for preparing synthetic rutile.If being not added with silica, the TiO in slag2Stable perovskite is easily combined into CaO
CaTiO3, cause the reduction of synthetic rutile yield.The monomer dissociation of rutile can be effectively facilitated using the amount of allocating, simultaneously
Slag can be made to keep suitable fusing point and mobility to be easy to follow-up operation again.If silica amount of allocating is excessive, can make slag
Fusing point rise, viscosity increase, are unfavorable for the diffusion mass transfer of slag composition homogenization and Rutile Type in forming core and growth process
Effect；Silica amount of allocating very little, then it cannot be guaranteed that the abundant dissociation of rutile.
According to a particular embodiment of the invention, CaO and SiO in mixed material2Mass ratio be not higher than 0.8, SiO2With TiO2
Mass ratio be not higher than 1.6, it is preferable that can be further by CaO in mixed material and SiO2Mass ratio be optimized for mass ratio
CaO:SiO2=0.6~0.75, SiO2:TiO2=1.4~1.55, thus, it is possible to further improve the yield of synthetic rutile.
Reaction zone 210 is defined in embodiments in accordance with the present invention, reaction unit 200 and connected with reaction zone 210 it is mixed
Material inlet 201 and oxidation material outlet 202 are closed, mixed material entrance 201 is connected with mixed material outlet 103, reaction unit
200 are suitable to hold the mixed material in cinder ladle, and are aoxidized mixed material using the oxidizing gas being blown in injection tube
It is modified, to obtain oxidation material.According to the specific embodiment of the present invention, reaction unit can be melt pit.
Embodiments in accordance with the present invention, with reference to Fig. 2, the port of export of injection tube 300 is extended in reaction zone 310, injection tube
300 include oxidizing gas conveyance conduit 310, nitrogen gas delivery-line 320 and crystal seed conveyance conduit 330, wherein, oxidizing gas
The road of delivery pipe 310 is made up of the first segment pipe 311 and the second segment pipe 312, and second segment pipeline is enclosed on outside nitrogen delivery pipe 320
On 312, nitrogen delivery pipe 320 has the nitrogen inlet 321 set perpendicular to nitrogen delivery pipe 320；On crystal seed conveyance conduit 330
It is provided with crystal seed entrance 331 and the control valve 332 positioned at the downstream of crystal seed entrance 331, the segment pipe of crystal seed conveyance conduit 330 and first
311 are set up in parallel and the entrance of crystal seed conveyance conduit 330 is connected with the entrance of the first segment pipe 311, crystal seed conveyance conduit 330
Outlet be connected with the outlet of the first segment pipe 311, injection tube 300 be suitable into mixed material be blown oxidizing gas, nitrogen
Gas and crystal seeds of rutile, to carry out oxidation modification to mixed material, obtain oxidation material.Specifically, mixed material enters anti-
, can be by mixed material by using the injection tube to oxidizing gas is blown inside mixed material after the reaction zone for answering device
The fully oxidized titanium compound such as middle or low price titanium oxide and titanium carbonitride is TiO2, and by being blown gold into mixed material
Red stone crystal seed, further promotes Rutile Type in material to grow up, improves the particle diameter of Rutile Type, provided for follow-up ore dressing processing
More convenience.
According to a particular embodiment of the invention, the total length of double-deck injection tube can be 4~8m, using heat-resistance stainless steel system
Into the internal diameter of the oxidizing gas conveyance conduit on the inside of it can be 10~15mm, the oxidisability of oxidizing gas conveyance conduit
Gas access can be 10~15mm, and the nitrogen gas delivery-line internal diameter in outside can be 28~35mm, and the internal diameter of nitrogen inlet can
Think 3~8mm, the thickness of oxidizing gas conveyance conduit and nitrogen gas delivery-line can be 2~4mm, thus, it is possible to enter one
Step improves injection effect, and using double-deck injection tube design, can also effectively mitigate mixed material and the strong of injection tube is invaded
Erosion.
Embodiments in accordance with the present invention, the species of oxidizing gas is not particularly restricted, and those skilled in the art can be with
Selected according to actual needs, according to a particular embodiment of the invention, oxidizing gas can be oxygen or oxygen-nitrogen mixture,
When using oxygen-nitrogen mixture, the volume fraction of the oxygen in oxygen-nitrogen mixture can be 20~90v%, thus, it is possible to enter one
Step improves TiO in obtained mixed material2Yield.
According to a particular embodiment of the invention, during oxidizing gas conveyance conduit injection oxidizing gas, oxidizing gas
Pressure can be 0.15~0.4MPa, and when oxidizing gas uses oxygen, oxygen flow can be 15~60L/ (minkg
Slag)；When oxidizing gas uses nitrogen oxygen atmosphere, oxidizing gas flowrate Q can be by " Q=(15~60/ nitrogen oxygen atmospheres
Middle oxygen purity " is calculated, and unit is L/ (minkg slags).
According to a particular embodiment of the invention, during nitrogen gas delivery-line nitrogen-blow, nitrogen pressure can for 0.2~
0.4MPa, the flow of nitrogen can be 2~30L/ (minkg slags).
The crystal seed storehouse suitable for storage crystal seeds of rutile is defined in embodiments in accordance with the present invention, crystal seed conveyance conduit, can
, can by being blown crystal seeds of rutile into mixed material to add crystal seeds of rutile into crystal seed storehouse in advance before being blown
Further to promote growing up for Rutile Type in material, the particle diameter of Rutile Type is improved, provides and more defecates for follow-up ore dressing processing
Profit.
According to the specific embodiment of the present invention, crystal seed conveyance conduit may further include isometrical section and reducer,
Above-mentioned crystal seed storehouse is limited to isometrical section of crystal seed conveyance conduit, and isometrical section of diameter can be 30~45mm.
According to a particular embodiment of the invention, the axis of crystal seed conveyance conduit discharging section and oxidizing gas conveyance conduit
The opening formed between axis can be with 30~90 degree, it is possible thereby to which it is brilliant to be further beneficial to injection towards the angle of the first segment pipe
Kind.
According to a particular embodiment of the invention, the time of injection can be 10~30min, and mixing should be controlled during injection
Temperature of charge is maintained between 1500~1600 DEG C, and completes preceding 3~5min in injection, can be opened positioned at crystal seed entrance downstream
Control valve, into mixed material be blown crystal seeds of rutile until injection complete.
Embodiments in accordance with the present invention, can obtain more preferably oxidation using the injection tube processing mixed material of the present invention and change
The effect that property and rutile are grown up, and by being blown to mixed material depths, the power of oxidation reaction can be substantially improved
Condition, while having Gas Stirring effect concurrently；On the other hand, crystal seeds of rutile is blown into by mixing as carrier gas using blowing gas
Act on inside material and by Gas Stirring, Dispersed precipitate of the crystal seed powder in mixed material can be realized to greatest extent,
Material is avoided to reunite, so as to promote growing up for Rutile Type in mixed material.
According to the specific embodiment of the present invention, after injection is completed, mixed material can naturally be delayed in atmosphere
It is cooled to room temperature, it is possible thereby to using High temperature diffusion effect of mass transmitting, further promote growing up for Rutile Type.After testing, by inciting somebody to action
Mixed material slow cooling can make rutile particles of the particle diameter more than 100 microns in material account for total rutile particles quantity to room temperature
More than 80%, be significantly better than prior art.
Embodiments in accordance with the present invention, breaker 400 has oxidation material entrance 401 and material powders outlet 402, oxygen
Change material inlet 401 with oxidation material outlet 202 to be connected, breaker 400 is suitable to oxidation material carrying out break process, so as to
Obtain material powders.
Embodiments in accordance with the present invention, the particle diameter of material powders is not particularly restricted, and those skilled in the art can root
Selected according to being actually needed, according to a particular embodiment of the invention, the average grain diameter of material powders can be micro- for 74~150
Rice, thus, it is possible to further improve the ore dressing effect in follow-up ore dressing processing.
Embodiments in accordance with the present invention, ore-dressing plant 500 have material powders entrance 501, thick titanium dioxide outlet 502,
Chats outlet 503 and mine tailing outlet 504, material powders entrance 501 are connected with material powders outlet 402, and chats exports 503 and mixed
Close material inlet 201 be connected, ore-dressing plant 500 be suitable to by material powders carry out ore dressing processing, so as to obtain thick carbon dioxide, in
Ore deposit and mine tailing.
According to a particular embodiment of the invention, ore-dressing plant can be shaking table, and ore dressing processing is carried out by using shaking table, can
Effectively to separate the rutile monomer in mixed material with gangue, TiO is obtained2Thick rutile of the content in 45~70wt%
Product.
According to the specific embodiment of the present invention, ore dressing can be handled in obtained middling recurrence reaction unit and carried out
Oxidation modification, so as to further improve TiO2The rate of recovery.
Embodiments in accordance with the present invention, the condition of ore dressing processing is not particularly restricted, and those skilled in the art can root
Selected according to being actually needed, according to a particular embodiment of the invention, ore dressing processing can be carried out using shaking table, and shaking table is rushed
Secondary is 300~360 times/min, and stroke is 8~12mm, and feed ore concentration is 20~40%, it is preferable that jig frequency is 320~360 times/
Min, stroke is 8~10mm, and feed ore concentration is 30~35%.Thus, it is possible to further improve thick rutile in material, chats and
The separating effect of mine tailing.
Embodiments in accordance with the present invention, acid dip pickle 600 has thick titanium dioxide entrance 601, hydrochloric acid entrance 602 and slurry
Outlet 603, thick titanium dioxide entrance 601 is connected with thick titanium dioxide outlet 502, and acid dip pickle 600 is suitable to will be thick using hydrochloric acid
Titanium dioxide carries out pickling processes, to obtain slurry.Specifically, by pickling processes can by the MgO in thick titanium dioxide,
The acid soluble impurities such as CaO are fully removed, after testing, and MgO can be met in the slurry that acidic treatment is obtained and CaO total content is not high
In 3wt%.
According to a particular embodiment of the invention, acid device can be provided with to seal in leaching kettle, and sealing leaching kettle
Agitator, calandria and thermometer, and by control system control control agitator and heating body running, to adjust sealing leaching
Go out the temperature of material in kettle.
Embodiments in accordance with the present invention, the condition of pickling processes is not particularly restricted, and those skilled in the art can root
Selected according to being actually needed, according to a particular embodiment of the invention, in pickling processes the concentration of hydrochloric acid can for 10~
The liquid-solid ratio of 20wt%, hydrochloric acid and material powders can be 3~5:1, pickling processes can carry out 30 under 25~90 degrees Celsius
~120min is completed；Preferably, the concentration of hydrochloric acid can be 15~20wt% in pickling processes, and the liquid of hydrochloric acid and material powders is consolidated
Than that can be 2~4:1, pickling processes can carry out 60~90min completions under 70~90 degrees Celsius.Thus, it is possible to further
Improve the titanium grade in the synthetic rutile prepared.
Embodiments in accordance with the present invention, filter 700 has slurry inlet 701, waste liquid outlet 702 and synthetic rutile
Outlet 703, slurry inlet 701 is connected with slurry outlet 603, and the slurry that filter 700 is suitable to obtain pickling processes is carried out
Filtration treatment, to obtain synthetic rutile product.
Thus, the system for preparing synthetic rutile according to embodiments of the present invention is by the way that titanium-containing molten and separated slag and silica are supplied
Batch mixing and insulation are carried out into cinder ladle, to obtain mixed material, and then mixed material is transferred in reaction unit, and use
Injection tube is blown oxidizing gas into mixed material, so as to which the titanium compound in mixed material is oxidized into TiO2, obtain oxygen
Compound material, completes to be blown crystal seeds of rutile in the backward material of injection, further to promote growing up for Rutile Type；Wherein, spray
The port of export of blowpipe extends to the inside of mixed material in reaction zone, so as to substantially improve the dynamics bar of oxidation reaction
Part, shortens the injection time, improves low price titanium compound to TiO2Conversion ratio；And then, oxidation material is supplied to breaker
Middle carry out break process, and obtained material powders are supplied into ore-dressing plant carry out ore dressing processing, so as to by rutile list
Body is separated with gangue, obtains thick titanium dioxide, chats and mine tailing, and wherein chats, which can be returned in reaction unit, proceeds oxidation
It is modified, subsequently thick titanium dioxide is supplied into acid dip pickle and carries out pickling processes, and the slurry that pickling processes are obtained is supplied
Filtration treatment is carried out into filter, to obtain synthetic rutile product.The system is molten to titaniferous by using injection tube
Injection oxidizing gas inside point slag material, significantly improves in titanium-containing molten and separated slag titanium compound to TiO2Conversion ratio so that
Improve the titanium grade in the synthetic rutile prepared.
In the second aspect of the present invention, the present invention propose a kind of use above-described embodiment prepare synthetic rutile be
Controlling for synthetic rutile method.Embodiments in accordance with the present invention, this method includes：By titanium-containing molten and separated slag and silica supply to
Batch mixing and insulation are carried out in cinder ladle, to obtain mixed material；Mixed material is transferred in reaction unit, and uses injection tube
Oxidizing gas, nitrogen and crystal seeds of rutile are blown into mixed material, to carry out oxidation modification to mixed material, oxygen is obtained
Compound material；Oxidation material is supplied into breaker and carries out break process, to obtain material powders；Material powders are supplied
Ore dressing processing is carried out into ore-dressing plant, to obtain thick titanium dioxide, chats and mine tailing；Thick titanium dioxide and hydrochloric acid are supplied
Pickling processes are carried out into acid dip pickle, to obtain slurry；And slurry is supplied into filter carry out filtration treatment,
To obtain synthetic rutile.
The method for preparing synthetic rutile according to embodiments of the present invention is described in detail below with reference to Fig. 3.According to
Embodiments of the invention, this method includes：
S100：Batch mixing and insulation
In the step, titanium-containing molten and separated slag and silica are supplied into cinder ladle and carry out batch mixing and insulation, to obtain mixture
Material.Specifically, vanadium titano-magnetite is through the TiO in reduction-molten titanium-containing molten and separated slag got2Grade about 50wt%, calcium al-mg-si
Impurity content is up to 30~40wt%, and titanium-containing molten and separated slag is by melting separating device tapping temperature at 1500~1600 DEG C, after slagging tap directly
Into in cinder ladle, and it is incorporated into cinder ladle SiO2Content is not less than 90wt% silica, while will by the way of heated by electrodes
Temperature of charge is adjusted to 1500~1600 DEG C, to obtain mixed material in cinder ladle.
According to a particular embodiment of the invention, can be by mixed material at 1550~1600 DEG C after mixed material is obtained
It is transferred to after 40~60min of lower insulation in subsequent reactions device, inventor has found, by the way that mixed material progress insulation can be promoted
Enter the forming core of Rutile Type in modified slag with growing up, while viscosity coefficient of dross is relatively low at the temperature disclosed above, beneficial to rutile
Diffusion mass transfer of the component in slag, so that rutile agglomeration.
Embodiments in accordance with the present invention, the particle diameter of silica is not particularly restricted, and those skilled in the art can be according to reality
Border needs to be selected, according to a particular embodiment of the invention, and silica can be not higher than 2mm Cab-O-sil using average grain diameter,
And the content of powder in Cab-O-sil is not less than 90wt%.
Embodiments in accordance with the present invention, the addition of silica 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 addition of silica can be the 30 of titanium-containing molten and separated slag quality
~40%, specifically, silica can be combined the stable calcium silicates of generation with the CaO in slag, so that rutile separate out,
Reach the purpose for preparing synthetic rutile.If being not added with silica, the TiO in slag2Stable perovskite is easily combined into CaO
CaTiO3, cause the reduction of synthetic rutile yield.The monomer dissociation of rutile can be effectively facilitated using the amount of allocating, simultaneously
Slag can be made to keep suitable fusing point and mobility to be easy to follow-up operation again.If silica amount of allocating is excessive, can make slag
Fusing point rise, viscosity increase, are unfavorable for the diffusion mass transfer of slag composition homogenization and Rutile Type in forming core and growth process
Effect；Silica amount of allocating very little, then it cannot be guaranteed that the abundant dissociation of rutile.
According to a particular embodiment of the invention, CaO and SiO in mixed material2Mass ratio be not higher than 0.8, SiO2With TiO2
Mass ratio be not higher than 1.6, it is preferable that can be further by CaO in mixed material and SiO2Mass ratio be optimized for mass ratio
CaO:SiO2=0.6~0.75, SiO2:TiO2=1.4~1.55, thus, it is possible to further improve the yield of synthetic rutile.
S200：Shift mixed material
In the step, mixed material is transferred in reaction unit, and oxidation is blown into mixed material using injection tube
Property gas, nitrogen and crystal seeds of rutile, so as to mixed material carry out oxidation modification, obtain oxidation material.
The mixed material entrance that reaction zone is defined in embodiments in accordance with the present invention, reaction unit and is connected with reaction zone
With oxidation material outlet, mixed material entrance is connected with mixed material outlet, and reaction unit is suitable to hold the mixture in cinder ladle
Material, and mixed material is subjected to oxidation modification using the oxidizing gas being blown in injection tube, to obtain oxidation material.According to
The specific embodiment of the present invention, reaction unit can be melt pit.
Embodiments in accordance with the present invention, with reference to Fig. 2, the port of export of injection tube 300 is extended in reaction zone 310, injection tube
300 include oxidizing gas conveyance conduit 310, nitrogen gas delivery-line 320 and crystal seed conveyance conduit 330, wherein, oxidizing gas
The road of delivery pipe 310 is made up of the first segment pipe 311 and the second segment pipe 312, and second segment pipeline is enclosed on outside nitrogen delivery pipe 320
On 312, nitrogen delivery pipe 320 has the nitrogen inlet 321 set perpendicular to nitrogen delivery pipe 320；On crystal seed conveyance conduit 330
It is provided with crystal seed entrance 331 and the control valve 332 positioned at the downstream of crystal seed entrance 331, the segment pipe of crystal seed conveyance conduit 330 and first
311 are set up in parallel and the entrance of crystal seed conveyance conduit 330 is connected with the entrance of the first segment pipe 311, crystal seed conveyance conduit 330
Outlet be connected with the outlet of the first segment pipe 311, injection tube 300 be suitable into mixed material be blown oxidizing gas, nitrogen
Gas and crystal seeds of rutile, to carry out oxidation modification to mixed material, obtain oxidation material.Specifically, mixed material enters anti-
, can be by mixed material by using the injection tube to oxidizing gas is blown inside mixed material after the reaction zone for answering device
The fully oxidized titanium compound such as middle or low price titanium oxide and titanium carbonitride is TiO2, and by being blown gold into mixed material
Red stone crystal seed, further promotes Rutile Type in material to grow up, improves the particle diameter of Rutile Type, provided for follow-up ore dressing processing
More convenience.
According to a particular embodiment of the invention, the total length of double-deck injection tube can be 4~8m, using heat-resistance stainless steel system
Into the internal diameter of the oxidizing gas conveyance conduit on the inside of it can be 10~15mm, the oxidisability of oxidizing gas conveyance conduit
Gas access can be 10~15mm, and the nitrogen gas delivery-line internal diameter in outside can be 28~35mm, and the internal diameter of nitrogen inlet can
Think 3~8mm, the thickness of oxidizing gas conveyance conduit and nitrogen gas delivery-line can be 2~4mm, thus, it is possible to enter one
Step improves injection effect, and using double-deck injection tube design, can also effectively mitigate mixed material and the strong of injection tube is invaded
Erosion.
Embodiments in accordance with the present invention, the species of oxidizing gas is not particularly restricted, and those skilled in the art can be with
Selected according to actual needs, according to a particular embodiment of the invention, oxidizing gas can be oxygen or oxygen-nitrogen mixture,
When using oxygen-nitrogen mixture, the volume fraction of the oxygen in oxygen-nitrogen mixture can be 20~90v%, thus, it is possible to enter one
Step improves TiO in obtained mixed material2Yield.
According to a particular embodiment of the invention, during oxidizing gas conveyance conduit injection oxidizing gas, oxidizing gas
Pressure can be 0.15~0.4MPa, and when oxidizing gas uses oxygen, oxygen flow can be 15~60L/ (minkg
Slag)；When oxidizing gas uses nitrogen oxygen atmosphere, oxidizing gas flowrate Q can be by " Q=(15~60/ nitrogen oxygen atmospheres
Middle oxygen purity " is calculated, and unit is L/ (minkg slags).
According to a particular embodiment of the invention, during nitrogen gas delivery-line nitrogen-blow, nitrogen pressure can for 0.2~
0.4MPa, the flow of nitrogen can be 2~30L/ (minkg slags).
The crystal seed storehouse suitable for storage crystal seeds of rutile is defined in embodiments in accordance with the present invention, crystal seed conveyance conduit, can
, can by being blown crystal seeds of rutile into mixed material to add crystal seeds of rutile into crystal seed storehouse in advance before being blown
Further to promote growing up for Rutile Type in material, the particle diameter of Rutile Type is improved, provides and more defecates for follow-up ore dressing processing
Profit.
According to the specific embodiment of the present invention, crystal seed conveyance conduit may further include isometrical section and reducer,
Above-mentioned crystal seed storehouse is limited to isometrical section of crystal seed conveyance conduit, and isometrical section of diameter can be 30~45mm.
According to a particular embodiment of the invention, the axis of crystal seed conveyance conduit discharging section and oxidizing gas conveyance conduit
The opening formed between axis can be with 30~90 degree, it is possible thereby to which it is brilliant to be further beneficial to injection towards the angle of the first segment pipe
Kind.
According to a particular embodiment of the invention, the time of injection can be 10~30min, and mixing should be controlled during injection
Temperature of charge is maintained between 1500~1600 DEG C, and completes preceding 3~5min in injection, can be opened positioned at crystal seed entrance downstream
Control valve, into mixed material be blown crystal seeds of rutile until injection complete.
Embodiments in accordance with the present invention, can obtain more preferably oxidation using the injection tube processing mixed material of the present invention and change
The effect that property and rutile are grown up, and by being blown to mixed material depths, the power of oxidation reaction can be substantially improved
Condition, while having Gas Stirring effect concurrently；On the other hand, crystal seeds of rutile is blown into by mixing as carrier gas using blowing gas
Act on inside material and by Gas Stirring, Dispersed precipitate of the crystal seed powder in mixed material can be realized to greatest extent,
Material is avoided to reunite, so as to promote growing up for Rutile Type in mixed material.
According to the specific embodiment of the present invention, after injection is completed, mixed material can naturally be delayed in atmosphere
It is cooled to room temperature, it is possible thereby to using High temperature diffusion effect of mass transmitting, further promote growing up for Rutile Type.After testing, by inciting somebody to action
Mixed material slow cooling can make rutile particles of the particle diameter more than 100 microns in material account for total rutile particles quantity to room temperature
More than 80%, be significantly better than prior art.
S300：Break process
In the step, oxidation material is supplied into breaker and carries out break process, to obtain material powders.
Embodiments in accordance with the present invention, the particle diameter of material powders is not particularly restricted, and those skilled in the art can root
Selected according to being actually needed, according to a particular embodiment of the invention, the average grain diameter of material powders can be micro- for 74~150
Rice, thus, it is possible to further improve the ore dressing effect in follow-up ore dressing processing.
S400：Ore dressing is handled
In the step, by material powders supply into ore-dressing plant carry out ore dressing processing, so as to obtain thick titanium dioxide, in
Ore deposit and mine tailing.
According to a particular embodiment of the invention, ore-dressing plant can be shaking table, and ore dressing processing is carried out by using shaking table, can
Effectively to separate the rutile monomer in mixed material with gangue, TiO is obtained2Thick rutile of the content in 45~70wt%
Product.
According to the specific embodiment of the present invention, ore dressing can be handled in obtained middling recurrence reaction unit and carried out
Oxidation modification, so as to further improve TiO2The rate of recovery.
Embodiments in accordance with the present invention, the condition of ore dressing processing is not particularly restricted, and those skilled in the art can root
Selected according to being actually needed, according to a particular embodiment of the invention, ore dressing processing can be carried out using shaking table, and shaking table is rushed
Secondary is 300~360 times/min, and stroke is 8~12mm, and feed ore concentration is 20~40%, it is preferable that jig frequency is 320~360 times/
Min, stroke is 8~10mm, and feed ore concentration is 30~35%.Thus, it is possible to further improve thick rutile in material, chats and
The separating effect of mine tailing.
S500：Pickling processes
In the step, thick titanium dioxide and hydrochloric acid are supplied into acid dip pickle and carry out pickling processes, to obtain slurry.
Specifically, the acid soluble impurities such as MgO, CaO in thick titanium dioxide can fully be removed by pickling processes, after testing, acid
Property the obtained slurry of processing in can meet MgO and CaO total content not higher than 3wt%.
According to a particular embodiment of the invention, acid device can be provided with to seal in leaching kettle, and sealing leaching kettle
Agitator, calandria and thermometer, and by control system control control agitator and heating body running, to adjust sealing leaching
Go out the temperature of material in kettle.
Embodiments in accordance with the present invention, the condition of pickling processes is not particularly restricted, and those skilled in the art can root
Selected according to being actually needed, according to a particular embodiment of the invention, in pickling processes the concentration of hydrochloric acid can for 10~
The liquid-solid ratio of 20wt%, hydrochloric acid and material powders can be 3~5:1, pickling processes can carry out 30 under 25~90 degrees Celsius
~120min is completed；Preferably, the concentration of hydrochloric acid can be 15~20wt% in pickling processes, and the liquid of hydrochloric acid and material powders is consolidated
Than that can be 2~4:1, pickling processes can carry out 60~90min completions under 70~90 degrees Celsius.Thus, it is possible to further
Improve the titanium grade in the synthetic rutile prepared.
S600：Filtration treatment
In the step, slurry is supplied into filter and carries out filtration treatment, to obtain synthetic rutile.
Thus, the method for preparing synthetic rutile according to embodiments of the present invention is by the way that titanium-containing molten and separated slag and silica are supplied
Batch mixing and insulation are carried out into cinder ladle, to obtain mixed material, and then mixed material is transferred in reaction unit, and use
Injection tube is blown oxidizing gas into mixed material, so as to which the titanium compound in mixed material is oxidized into TiO2, obtain oxygen
Compound material, completes to be blown crystal seeds of rutile in the backward material of injection, further to promote growing up for Rutile Type；Wherein, spray
The port of export of blowpipe extends to the inside of mixed material in reaction zone, so as to substantially improve the dynamics bar of oxidation reaction
Part, shortens the injection time, improves low price titanium compound to TiO2Conversion ratio；And then, oxidation material is supplied to breaker
Middle carry out break process, and obtained material powders are supplied into ore-dressing plant carry out ore dressing processing, so as to by rutile list
Body is separated with gangue, obtains thick titanium dioxide, chats and mine tailing, and wherein chats, which can be returned in reaction unit, proceeds oxidation
It is modified, subsequently thick titanium dioxide is supplied into acid dip pickle and carries out pickling processes, and the slurry that pickling processes are obtained is supplied
Filtration treatment is carried out into filter, to obtain synthetic rutile product.This method is molten to titaniferous by using injection tube
Injection oxidizing gas inside point slag material, significantly improves in titanium-containing molten and separated slag titanium compound to TiO2Conversion ratio so that
Improve the titanium grade in the synthetic rutile prepared.
Below with reference to specific embodiment, present invention is described, it is necessary to which explanation, these embodiments are only description
Property, without limiting the present invention in any way.
Embodiment 1
Synthetic rutile is prepared according to the following steps：
Titanium-containing molten and separated slag and silica are supplied into cinder ladle and carry out batch mixing and insulation, to obtain mixed material；Wherein, silicon
Stone uses SiO2Content is not less than 94wt% and average grain diameter is not higher than 2mm Cab-O-sil, and the addition of Cab-O-sil is molten for titaniferous
Divide the 30% of slag amount, finally make mass ratio CaO in mixed material:SiO2=0.5, mass ratio SiO2:TiO2=1.4, batch mixing mistake
Mixed material temperature is adjusted to 1500 DEG C by the way of heated by electrodes in journey, and by obtained mixed material at 1500 DEG C
It is incubated in 40min, insulating process and suitably stirs, non-uniform components；
Mixed material is transferred in melt pit, and using injection tube be blown into mixed material oxidizing gas, nitrogen and
Crystal seeds of rutile, to carry out oxidation modification to mixed material, obtains oxidation material；Wherein, oxidizing gas uses purity oxygen,
Pressure is 0.15MPa, and flow is 15L/ (minkg slags), and nitrogen pressure is 0.2MPa, and flow is 10~30L/ (minkg
Slag), injection total time is 10min, and injection starts to open crystal seed storehouse control valve after 5min, and crystal seeds of rutile is blown into mixed material
Interior, the addition of crystal seeds of rutile is 0.5kg/t slags, is blown the natural slow cooling of material to room temperature after terminating；
Oxidation material is supplied into breaker and carries out break process, to obtain 74~150 microns of average grain diameter
Material powders；
Material powders are supplied into ore-dressing plant and carry out ore dressing processing, to obtain thick titanium dioxide, chats and mine tailing；
Wherein, shaking table jig frequency is 320 times/min, and stroke is 8mm, and feed ore concentration is 30%, TiO in obtained thick titanium dioxide2Content
For 55wt%, rutile yield reaches 82%；
Thick titanium dioxide and hydrochloric acid are supplied into acid dip pickle and carry out pickling processes, to obtain slurry；Wherein, hydrochloric acid
Concentration is 10wt%, and the liquid-solid ratio of hydrochloric acid and material powders is 3:1, pickling temperature is 25 DEG C, and the time is 30min；
Slurry is supplied into filter and carries out filtration treatment, to obtain TiO2Content is 95wt% artificial golden red
Stone.
Embodiment 2
Synthetic rutile is prepared according to the following steps：
Titanium-containing molten and separated slag and silica are supplied into cinder ladle and carry out batch mixing and insulation, to obtain mixed material；Wherein, silicon
Stone uses SiO2Content is not less than 94wt% and average grain diameter is not higher than 2mm Cab-O-sil, and the addition of Cab-O-sil is molten for titaniferous
Divide the 40% of slag amount, finally make mass ratio CaO in mixed material:SiO2=0.6, mass ratio SiO2:TiO2=1.5, batch mixing mistake
Mixed material temperature is adjusted to 1600 DEG C by the way of heated by electrodes in journey, and by obtained mixed material at 1600 DEG C
It is incubated in 40min, insulating process and suitably stirs, non-uniform components；
Mixed material is transferred in melt pit, and using injection tube be blown into mixed material oxidizing gas, nitrogen and
Crystal seeds of rutile, to carry out oxidation modification to mixed material, obtains oxidation material；Wherein, oxidizing gas uses purity oxygen,
Pressure is 0.4MPa, and flow is 60L/ (minkg slags), and nitrogen pressure is 0.4MPa, and flow is 30L/ (minkg slags), spray
Total time is blown for 30min, and injection starts to open crystal seed storehouse control valve after 25min, crystal seeds of rutile is blown into mixed material, gold
The addition of red stone crystal seed is 2kg/t slags, is blown the natural slow cooling of material to room temperature after terminating；
Oxidation material is supplied into breaker and carries out break process, to obtain 74~150 microns of average grain diameter
Material powders；
Material powders are supplied into ore-dressing plant and carry out ore dressing processing, to obtain thick titanium dioxide, chats and mine tailing；
Wherein, shaking table jig frequency is 360 times/min, and stroke is 10mm, and feed ore concentration is 35%, TiO in obtained thick titanium dioxide2Content
For 65wt%, rutile yield reaches 85%；
Thick titanium dioxide and hydrochloric acid are supplied into acid dip pickle and carry out pickling processes, to obtain slurry；Wherein, hydrochloric acid
Concentration is 20wt%, and the liquid-solid ratio of hydrochloric acid and material powders is 3:1, pickling temperature is 90 DEG C, and the time is 30min；
Slurry is supplied into filter and carries out filtration treatment, to obtain TiO2Content is 99wt% artificial golden red
Stone.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means to combine specific features, structure, material or the spy that the embodiment or example are described
Point is contained at least one embodiment of the present invention or example.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be with office
Combined in an appropriate manner in one or more embodiments or example.In addition, in the case of not conflicting, the skill of this area
Art personnel can be tied the not be the same as Example or the feature of example and non-be the same as Example or example described in this specification
Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification.
Claims (10)
1. a kind of system for preparing synthetic rutile, it is characterised in that including：
Electrode is provided with cinder ladle, the cinder ladle, the cinder ladle has high temperature titanium-containing molten and separated slag entrance, silica entrance and mixture
Material outlet；
Reaction zone and the mixed material entrance connected with the reaction zone and oxidation are defined in reaction unit, the reaction unit
Material outlet, the mixed material entrance is connected with mixed material outlet；
Injection tube, the port of export of the injection tube is extended in the reaction zone, and the injection tube is conveyed including oxidizing gas
Pipeline, nitrogen gas delivery-line and crystal seed conveyance conduit, wherein, the oxidizing gas conveyance conduit is by the first segment pipe and second
Segment pipe is constituted, and is enclosed on outside the nitrogen delivery pipe on second segment pipe, and the nitrogen delivery pipe has perpendicular to described
The nitrogen inlet that nitrogen delivery pipe is set；Crystal seed entrance is provided with the crystal seed conveyance conduit and under the crystal seed entrance
The control valve of trip, the crystal seed conveyance conduit and first segment pipe be set up in parallel and the entrance of the crystal seed conveyance conduit with
The entrance of first segment pipe is connected, and the outlet of the crystal seed conveyance conduit is connected with the outlet of first segment pipe
It is logical；
Breaker, the breaker has oxidation material entrance and material powders outlet, the oxidation material entrance and institute
Oxidation material outlet is stated to be connected；
Ore-dressing plant, the ore-dressing plant has material powders entrance, the outlet of thick titanium dioxide, chats outlet and mine tailing outlet,
The material powders entrance is connected with material powders outlet, and the chats outlet is connected with the mixed material entrance；
Acid dip pickle, the acid dip pickle has thick titanium dioxide entrance, hydrochloric acid entrance and slurry outlet, the thick titanium dioxide
Entrance is connected with the thick titanium dioxide outlet；
Filter, the filter have slurry inlet, waste liquid outlet and synthetic rutile outlet, the slurry inlet with
The slurry outlet is connected.
2. system according to claim 1, it is characterised in that defined in the crystal seed conveyance conduit suitable for storage golden red
The crystal seed storehouse of stone crystal seed.
3. system according to claim 1, it is characterised in that the internal diameter of the oxidizing gas conveyance conduit is 10~
15mm, the internal diameter of the nitrogen gas delivery-line is 28~35mm, and the internal diameter of the nitrogen inlet is 3~8mm, the oxidisability gas
Body conveyance conduit and the thickness of the nitrogen gas delivery-line are 2~4mm.
4. system according to claim 1, it is characterised in that the axis of the crystal seed conveyance conduit discharging section with it is described
The opening formed between oxidizing gas conveyance conduit axis towards the angle of first segment pipe be 30~90 degree.
5. the system for preparing synthetic rutile described in a kind of any one of use Claims 1 to 4 prepares the side of synthetic rutile
Method, it is characterised in that including：
Titanium-containing molten and separated slag and silica are supplied into cinder ladle and carry out batch mixing and insulation, to obtain mixed material；
The mixed material is transferred in reaction unit, and oxidisability gas is blown into the mixed material using injection tube
Body, nitrogen and crystal seeds of rutile, to carry out oxidation modification to the mixed material, obtain oxidation material；
The oxidation material is supplied into breaker and carries out break process, to obtain material powders；
The material powders are supplied into ore-dressing plant and carry out ore dressing processing, to obtain thick titanium dioxide, chats and mine tailing；
The thick titanium dioxide and hydrochloric acid are supplied into acid dip pickle and carry out pickling processes, to obtain slurry；And
The slurry is supplied into filter and carries out filtration treatment, to obtain synthetic rutile.
6. method according to claim 6, it is characterised in that protect the mixed material under 1550~1600 degrees Celsius
It is transferred to after 40~60min of temperature in the reaction unit.
7. method according to claim 6, it is characterised in that the SiO in the silica2Content is not less than 90wt%, described
The addition of silica is the 30~40% of the titanium-containing molten and separated slag quality,
Optionally, CaO and SiO in the mixed material2Mass ratio be not higher than 0.8, SiO2With TiO2Mass ratio be not higher than
1.6。
8. method according to claim 6, it is characterised in that the oxidizing gas is oxygen or oxygen-nitrogen mixture, institute
The volume fraction for stating oxygen in oxygen-nitrogen mixture is 20~90v%；
Optionally, the injection time is 10~30min, and completes preceding 3~5min in the injection, into the mixed material
Crystal seeds of rutile is blown until the injection is completed.
9. method according to claim 6, it is characterised in that the ore dressing processing is carried out using shaking table, the shaking table
Jig frequency is 300~360 times/min, and stroke is 8~12mm, and feed ore concentration is 20~40%.
10. method according to claim 6, it is characterised in that the concentration of the hydrochloric acid is 10~20wt%, the hydrochloric acid
Liquid-solid ratio with the material powders is 3~5:1, the pickling processes are that 30~120min of progress is complete under 25~90 degrees Celsius
Into.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108249477A (en) * | 2018-04-20 | 2018-07-06 | 四川星明能源环保科技有限公司 | A kind of synthetic rutile and the method that rutile is made using titanium-containing blast furnace slag manufacturer |
| CN108455664A (en) * | 2018-04-20 | 2018-08-28 | 四川星明能源环保科技有限公司 | A kind of rutile template and its preparation method and application |
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| CN102154531A (en) * | 2011-03-25 | 2011-08-17 | 喀左县钒钛资源综合开发利用工程技术研究中心 | Method for producing artificial rutile from titanium-containing blast furnace slags |
| CN106048107A (en) * | 2016-07-18 | 2016-10-26 | 东北大学 | Smelting reduction production and thermal refining method for titanium-containing slag mixture |
| CN207129968U (en) * | 2017-06-14 | 2018-03-23 | 江苏省冶金设计院有限公司 | The system for preparing synthetic rutile |
Cited By (2)
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| CN108249477A (en) * | 2018-04-20 | 2018-07-06 | 四川星明能源环保科技有限公司 | A kind of synthetic rutile and the method that rutile is made using titanium-containing blast furnace slag manufacturer |
| CN108455664A (en) * | 2018-04-20 | 2018-08-28 | 四川星明能源环保科技有限公司 | A kind of rutile template and its preparation method and application |
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