CN109321759A - A kind of baking inphases extract titanium in high titanium slag, iron, aluminium, magnesium component method - Google Patents
A kind of baking inphases extract titanium in high titanium slag, iron, aluminium, magnesium component method Download PDFInfo
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- CN109321759A CN109321759A CN201811349762.7A CN201811349762A CN109321759A CN 109321759 A CN109321759 A CN 109321759A CN 201811349762 A CN201811349762 A CN 201811349762A CN 109321759 A CN109321759 A CN 109321759A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
- C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
- C04B7/17—Mixtures thereof with other inorganic cementitious materials or other activators with calcium oxide containing activators
- C04B7/19—Portland cements
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B21/00—Obtaining aluminium
- C22B21/0007—Preliminary treatment of ores or scrap or any other metal source
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B21/00—Obtaining aluminium
- C22B21/0015—Obtaining aluminium by wet processes
- C22B21/0023—Obtaining aluminium by wet processes from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1209—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by dry processes, e.g. with selective chlorination of iron or with formation of a titanium bearing slag
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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Abstract
The present invention provides a kind of baking inphases extract titanium in high titanium slag, iron, aluminium, magnesium component method, which comprises grinding after mixing high titanium slag with auxiliary agent is classified, and obtains material to be roasted；Material to be roasted is subjected to low-temperature bake, obtains iron, titanium component enriched gas and the first material containing aluminium, magnesium component；Temperature control is carried out to iron, titanium component enriched gas and sublimates processing to obtain iron content solid and titaniferous gas, and titaniferous gas is hydrolyzed for iron component and titanium component separation, completes the extraction to iron component and titanium component in high titanium slag；High-temperature roasting is carried out to the first material containing aluminium, magnesium component, obtains fired slags；To fired slags Soaking treatment, it is separated by solid-liquid separation, obtains the first filtrate and filter residue；Precipitating reagent is added in the first filtrate, control pH completes the extraction to aluminium component and titanium component in high titanium slag so that aluminium component and magnesium component fractional precipitation.Method and process of the invention is simple, process is short, extraction efficiency is high, is conducive to commercial introduction.
Description
Technical field
The present invention relates to field of metallurgy and chemical engineering, more particularly, be related to a kind of baking inphases extract titanium in high titanium slag, iron,
It is high to be particularly suitable for the high titanium of the solid waste water quenching generated in vanadium titano-magnetite blast furnace ironmaking process for the method for aluminium, magnesium component
The extraction of titanium, iron, aluminium, magnesium component in clinker.
Background technique
For Panzhihua steel plant year output of steel up to 10,000,000 tons, the amount of generated high-titanium blast furnace slag is up to 3,600,000 tons.Mesh
Before, the accumulating amount of high-titanium blast furnace slag is 60,000,000 tons existing.The bulk deposition of high-titanium blast furnace slag not only land occupation, but also its diafiltration
Liquid enters surface water and groundwater, causes water pollution, and percolate has certain toxicity, and being diffused into Soil Surrounding leads to the farmland village
Family's damage, forms " barren land ".Wind blows tiny slag particle and causes fugitive dust, pollutes to local and lower air port area air.And
And the high-titanium blast furnace slag for being deposited in Jinsha jiang River two sides be easy to cause landslide under rainwash, is a kind of uncontrollable peace
Full hidden danger, the bulk deposition of high-titanium blast furnace slag have become on influencing huge pollution sources on local environment and geology.
Summary of the invention
It is above-mentioned existing in the prior art it is an object of the present invention to solving for the deficiencies in the prior art
One or more problems.For example, one of the objects of the present invention is to provide a kind of simple process, process is short, high-efficient extraction
Titanium in high titanium slag, iron, aluminium, magnesium component method.
To achieve the goals above, an aspect of of the present present invention provide a kind of baking inphases extract titanium in high titanium slag, iron,
The method of aluminium, magnesium component, the method may include following steps: grinding after high titanium slag is mixed with auxiliary agent, classification, obtain to
Roast material；The material to be roasted is subjected to low-temperature bake, obtains iron content, titanium component enriched gas and containing aluminium, magnesium component
First material；Temperature control is carried out to the iron content, titanium component enriched gas and sublimates processing to obtain iron component and titanium component separation
It is hydrolyzed to iron content solid and titaniferous gas, and by the titaniferous gas, completes the separation to iron component and titanium component in high titanium slag
It extracts；High-temperature roasting is carried out to the first material containing aluminium, magnesium component, obtains fired slags；To the fired slags Soaking treatment,
It is separated by solid-liquid separation, obtains filter residue and the first filtrate comprising aluminium ion, magnesium ion；
Precipitating reagent is added in first filtrate, control pH is completed so that aluminium component and magnesium component fractional precipitation to height
The separation and Extraction of aluminium component and magnesium component in titanium slag, wherein the auxiliary agent is the mixture of chlorate and sulfate, low-temperature bake
Temperature is 100 DEG C~400 DEG C, and high-temperature roasting temperature is 400 DEG C~800 DEG C.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method may comprise steps of:
Grinding, classification, obtain material to be roasted after high titanium slag is mixed with chlorination salt assitant；The material to be roasted is subjected to low temperature roasting
It burns, obtains iron content, titanium component enriched gas and the first material containing aluminium, magnesium component；To the iron, titanium component enriched gas into
Row temperature control sublimates processing to obtain iron content solid and titaniferous gas for iron component and titanium component separation, and by the titaniferous gas
The separation and Extraction to iron component and titanium component in high titanium slag is completed in hydrolysis；By described containing aluminium, the first material of magnesium component and sulfuric acid
After salt assitant mixing, high-temperature roasting obtains fired slags；To the fired slags Soaking treatment, be separated by solid-liquid separation, obtain filter residue and comprising
First filtrate of aluminium ion, magnesium ion；Precipitating reagent is added in first filtrate, control pH is so that aluminium component and magnesium component point
Step precipitating, completes the separation and Extraction to aluminium component and magnesium component in high titanium slag, wherein low-temperature bake temperature is 100 DEG C~400
DEG C, high-temperature roasting temperature is 400 DEG C~800 DEG C.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, the heating rate of the low-temperature bake can be 1 DEG C/min~10 DEG C/min, and the heating rate of the high-temperature roasting can be
1 DEG C/min~10 DEG C/min.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, the high titanium slag is water quenching type high-titanium blast furnace slag, and the component of the water quenching type high-titanium blast furnace slag includes, by mass percentage
Meter, Fe2O3Content is 2%~8%, TiO2Content is 10%~25%, Al2O3Content be 8%~15%, content of MgO be 5%~
12%.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, 80% or more grain diameter of the material to be roasted is 30 μm~200 μm.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, the method also includes the water quenching type high-titanium blast furnace slag is dried, it is broken after mix again with the auxiliary agent, it is described to do
Dry temperature is 60 DEG C~120 DEG C.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, the high titanium slag is titanium-containing blast furnace slag obtained by vanadium titano-magnetite blast furnace process through the resulting tailings of high temperature cabonization-low temperature chlorination.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, the mass ratio of chlorate and sulfuric acid salt assitant quality sum and the high titanium slag is 0.1~10:1.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, the temperature control is sublimated including condensing to iron, titanium component enriched gas, and iron component gas recrystallization is completed to high titanium slag
The extraction of middle iron component；Titanium component gas is collected using liquid-absorbant, obtains aqua oxidation titanium solution, is completed to high titanium
The extraction of titanium component in slag.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, the Soaking treatment carries out Soaking treatment, the infusion to the fired slags in whipping process including the use of infusion
Volume mass ratio with the fired slags is 0.5~100:1, and the temperature of the Soaking treatment is 20 DEG C~100 DEG C.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, the fractional precipitation may include: that the first precipitating reagent is added into first filtrate, at 25 DEG C~70 DEG C adjust pH to
4.0~6.0, it is filtered after stirring, obtains the second filtrate of aluminium hydroxide powder and rich magnesium component, wherein the first precipitating reagent is hydrogen
The combination of one or both of aluminium oxide and ammonium hydroxide；The second precipitating reagent is added into the second filtrate of the rich magnesium component, 25
DEG C~70 DEG C at adjust pH to 9.0~12.0, filtered after stirring, obtain magnesium hydrate powder, wherein second precipitating reagent is
The combination of one or both of magnesium hydroxide and ammonium hydroxide.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment
In, auxiliary agent gas is contained in the iron content, titanium component enriched gas, the auxiliary agent gas contained can return after pervaporation recrystallizes
It receives and recycles, enter the auxiliary agent of infusion in the infusion containing dissolution, the auxiliary agent into infusion is through pervaporation
It can be recycled and recycle after recrystallization.
Another party of the invention provides a kind of portland cement, and the portland cement includes segmentation roasting from the above mentioned
Burn extract titanium in blast furnace slag, iron, aluminium, magnesium component method in the fired slags Soaking treatment, the filter that is obtained after separation of solid and liquid
Slag.
Compared with prior art, the beneficial effect comprise that
(1) present invention extracts titanium, iron, aluminium and the magnesium in high titanium slag using the method for baking inphases, low-temperature bake
Stage realizes the extraction of titanium, iron component under chlorination salt action, and the high-temperature roasting stage realizes aluminium, magnesium component under sulfuric acid salt action
Extraction, simple process, process be short, it is high-efficient, be more advantageous to commercial introduction；
(2) present invention is few using amount of auxiliary used in the method extraction titanium of roasting, iron, aluminium, magnesium component process, relative to
Traditional acid hydrolyzation extracts valuable component, avoids because the wasting of resources caused by using a large amount of sulfuric acid and sulfuric acid mist are formed to environment
Caused by adverse effect；
(3) auxiliary agent is roasted in method of the invention to continue to be back to firing stage after recrystallizing, improve the benefit of auxiliary agent
With rate, process costs are reduced；
(4) method of the invention is to TiO2、Fe2O3、Al2O3, MgO recovery rate can reach 50%~98%, be prepared
Product be all satisfied or be higher than national (industry) standard；
(5) requirement that Silicon-rich Calcium compounds tailings meets portland cement is remained in method of the invention after the reaction was completed, it can
It is directly used in production of construction materials, is generated without the big residue of environmental pollution, it is environmentally protective.
Detailed description of the invention
By the description carried out with reference to the accompanying drawing, above and other purpose of the invention and feature will become more clear
Chu, in which:
The baking inphases that Fig. 1 shows one exemplary embodiment of the present invention extract titanium, iron, aluminium, magnesium group in high titanium slag
Divide the flow diagram of method.
Fig. 2 shows the baking inphases of another exemplary embodiment of the invention to extract titanium, iron, aluminium, magnesium in high titanium slag
The flow diagram of multi-component approach.
Specific embodiment
Hereinafter, baking inphases according to the present invention will be described in detail in conjunction with attached drawing and exemplary embodiment and extract height
Titanium in titanium slag, iron, aluminium, magnesium component method.
Specifically, the present invention is mixed with high titanium slag using chlorate, sulfate and carries out baking inphases, low-temperature bake process
It is middle that titanium, iron component in high titanium slag are enriched in flue dust gas phase, iron, titanium component are separated and recovered by condensation-water-soluble mode；It rises
Temperature converts soluble sulphate for aluminium, magnesium component in high titanium slag to high temperature firing stage, further passes through water logging-precipitating side
Formula separates and recovers aluminium, magnesium component.Have neither part nor lot in the auxiliary agent of reaction, a part is fired decomposition and/or after distillation is gas, through condensing
It is recycled after recrystallization；Another part is dissolved into filtrate during water logging, is recycled, is recycled after evaporation recrystallization
Auxiliary agent can be recycled in firing stage.
The baking inphases that Fig. 1 shows one exemplary embodiment of the present invention extract titanium, iron, aluminium, magnesium group in high titanium slag
Divide the flow diagram of method.Fig. 2 shows the baking inphases of another exemplary embodiment of the invention to extract in high titanium slag
Titanium, iron, aluminium, magnesium multi-component approach flow diagram.
An aspect of of the present present invention provide a kind of baking inphases extract titanium in high titanium slag, iron, aluminium, magnesium component method.?
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method an exemplary embodiment in, such as Fig. 1 institute
Show, the method may include:
High titanium slag is carried out weighing and proportioning with auxiliary agent and mixed by step S01, and grinding, classification obtains material to be roasted.
In the present embodiment, the high titanium slag can be the high-titanium blast furnace slag of water quenching type, for example, it is preferable to, it can be vanadium
The solid waste water quenching high-titanium blast furnace slag generated in titanomagnetite blast furnace ironmaking process.Wherein, the high titanium blast furnace of the water quenching type
The ingredient of slag may include, by mass percentage, Fe2O3Content is 2%~8%, TiO2Content is 10%~25%, Al2O3
Content is 8%~15%, and content of MgO is 5%~12%.Preferably, by mass percentage, the water quenching type high-titanium blast furnace slag
Ingredient may include Fe2O3Content is 2%~8%, TiO2Content is 10%~25%, Al2O3Content is 8%~15%,
Content of MgO is 5%~12%.When using water quenching type high-titanium blast furnace slag as raw material, since the humidity of the raw material is higher, it is auxiliary agent
It needs that the water quenching type high-titanium blast furnace slag is dried before mixing, be crushed.Broken purpose is to mix more with auxiliary agent
Uniformly.For example, dry temperature can be 60 DEG C~90 DEG C, it is preferred that dry temperature can be 67 DEG C~84 DEG C.Dry
Time can be confirmed according to the drying actual effect at scene, for example, drying time can be 6h~12h.Certainly, of the invention
Drying time it is without being limited thereto.For method of the invention be suitable for containing titanium, iron, aluminium, magnesium component any high titanium slag.
In the present embodiment, the high titanium slag can be titanium-containing blast furnace slag obtained by vanadium titano-magnetite blast furnace process through pyrocarbon
The resulting tailings of change-low temperature chlorination.Using the tailings as raw material, if it is the tailings of fresh baked, due to what is come out after low temperature chlorination
Tailings self-temperature is higher, does not need that tailings is dried.If it is the tailings after placement a period of time, due to the tail of titaniferous
Slag easily absorbs water, it is necessary to the tailings after placement is dried, likewise, the temperature of the drying can for 60 DEG C~
90 DEG C, it is preferred that dry temperature can be 67 DEG C~84 DEG C.
In the present embodiment, the mixed aid that the auxiliary agent can form for chlorate and sulfate.The chlorate can
To be ammonium chloride (NH4Cl), sodium chloride (NaCl), calcium chloride (CaCl2) and aluminium chloride (AlCl3One or more of)
Combination.The sulfate can be ammonium sulfate ((NH4)2SO4), ammonium hydrogen sulfate (NH4HSO4) and sulfuric acid (H2SO4) one of or
Two kinds of combinations, wherein H2SO4Mass fraction can be 20%~98%.The mixed aid formed for chlorate and sulfate
For, chlorate mainly acts on the low-temperature bake stage, generates the chloride of iron and the chloride of titanium.Sulfate mainly acts on
The high-temperature roasting stage generates the sulfate of aluminium and the sulfate of magnesium.For between the chlorate and sulfate in mixed aid
Quality proportioning can guarantee that the titanium in raw material, iron, aluminium, magnesium component have enough chlorates and sulfuric acid there is no strict requirements
Reactant salt.In the present invention, it can choose the salt other than above-mentioned enumerate for chlorate and sulfate.For example, chlorination
Salt can be potassium chloride etc., and sulfate can be potassium sulfate etc..But since the auxiliary agent for being added different will affect in process of the present invention
The constituent of the filter residue of generation, for prepared with filter residue portland cement be it is unfavorable, can be destroyed containing other elements
The performance of portland cement.It is preferred, therefore, that the chlorate of the invention can be ammonium chloride (NH4Cl), sodium chloride
(NaCl), calcium chloride (CaCl2) and aluminium chloride (AlCl3) one or more of combination.The sulfate can be sulfuric acid
Ammonium ((NH4)2SO4), ammonium hydrogen sulfate (NH4HSO4) and sulfuric acid (H2SO4) one or both of combination, wherein H2SO4Quality
Score can be 20%~98%.
In the present embodiment, the mass ratio of the high titanium slag and chlorate and sulfate mixed aid can be 1:0.1~
10.Preferably, mass ratio can be 1:1~8.
In the present embodiment, the material particular diameter to be roasted can meet 30 μm~200 μm for 80% or more particle.It is excellent
Choosing, 80% or more particle meets 50 μm~160 μm.Above-mentioned particle size, which is arranged, uniformly to mix convenient for raw material with auxiliary agent
It closes, is conducive to the abundant progress of calcination.
Step S02 carries out low-temperature bake to the material to be roasted that the step S01 is obtained, obtains iron, titanium component enriched gas
Body and first material containing aluminium, magnesium component.
In this example, material to be roasted can be delivered to calcining kiln and carries out segmentally heating roasting.What is carried out first is
Low-temperature bake.During roasting, a part of auxiliary agent is decomposed and/or is distilled due to maturing temperature, in gaseous state with
Iron, the mixing of titanium component enriched gas.Another part of auxiliary agent is reacted with high titanium slag to be obtained iron content, titanium component enriched gas and contains
There is the first material of aluminium, magnesium component.The first material containing aluminium, magnesium component does not contain iron, titanium component.It is described containing aluminium,
The first material of magnesium component can form fired slags after high-temperature roasting.
In the present embodiment, the heating rate of the low-temperature bake can be 1 DEG C/min~10 DEG C/min, low-temperature bake temperature
Degree can be 100 DEG C~400 DEG C.Preferably, heating rate can be 3 DEG C/min~8 DEG C/min, and low-temperature bake temperature can be
180 DEG C~340 DEG C.The soaking time of low-temperature bake can be confirmed according to practical roasting amount or phenomenon, for example, when heat preservation
Between can be 0.1h~5h, certainly, soaking time of the invention is without being limited thereto.
In the present embodiment, as shown in Figure 1, since the chlorate of addition of the invention mainly acts on low-temperature bake rank
Section.Therefore, for titanium, iron component, corresponding titanium tetrachloride and ferric trichloride can be generated contained in the high titanium slag.Described
Iron, titanium component enriched gas can be with the mixed gas for titanium tetrachloride and ferric trichloride, and in titanium tetrachloride and tri-chlorination
In the mixed gas of iron, it is mingled with the auxiliary agent gas of auxiliary agent distillation and/or decomposition.
Step S03 carries out temperature control to the iron, titanium component enriched gas and sublimates processing to divide iron component and titanium component
From obtaining iron content solid and titaniferous gas, and the titaniferous gas is hydrolyzed, complete to iron component in high titanium slag and titanium component
It extracts.
In the present embodiment, it is sublimated by temperature control, i.e. the condensation of control temperature separates iron component and titanium component.It is solidifying
China is that substance skips the phenomenon that liquid directly becomes solid-state from gaseous state, and condensation is to reduce the temperature of hot object and undergoing phase transition
Process, condensation in the present invention is to realize the mode of operation sublimated.In condensation process, condenser can be used to iron, titanium group
Separating/enriching gas is condensed.Since iron, titanium component enriched gas are mingled with the distillation of auxiliary agent and/or decompose gas, condensing
The auxiliary agent gas and iron component (iron chloride) gas for distilling and/or decomposing in the process carry out at the different location of condenser tube wall
It recrystallizes, the iron component recrystallized can be scraped, obtain iron-containing fixation (iron chloride solid), completion proposes iron component
It takes.It can continue cycling through after the auxiliary agent recycling of recrystallization for firing stage.For example, as shown in Figure 1, obtaining sulfuric acid after recrystallization
Then salt and chlorate are re-applied in firing stage of the invention.
Since titanium component gas is different from the freezing point of iron component gas, the gas of titanium component can't coagulate within the condenser
Gu.Need to collect titanium component gas after the condenser, use liquid-absorbant collect titanium component gas (titanium tetrachloride gases) with
Obtain aqua oxidation titanium solution (TiO2·nH2O), the extraction to titanium component is completed.The liquid absorption liquid can be industrial
One of water, tap water or distilled water or a variety of mixing.
Step S04 carries out high-temperature roasting to the first material containing aluminium, magnesium component, obtains fired slags；To the roasting
Slag Soaking treatment is separated by solid-liquid separation, obtains the first filtered fluid and filter residue；Precipitating reagent is added in first filtered fluid, controls
PH completes the extraction to aluminium component and magnesium component in high titanium slag so that aluminium component and magnesium component fractional precipitation.
In the present embodiment, it after the completion of low-temperature bake, needs to carry out high-temperature roasting to the first material containing aluminium, magnesium component
Processing.The heating rate of the high-temperature roasting can be 1 DEG C/min~10 DEG C/min, high-temperature roasting temperature can for 400 DEG C~
800℃.Preferably, heating rate can be 3 DEG C/min~7.8 DEG C/min, and high-temperature roasting temperature can be 420 DEG C~750 DEG C.
The soaking time of high-temperature roasting can be confirmed according to practical roasting amount or phenomenon, for example, soaking time can be 0.1h
~5h, certainly, high-temperature roasting soaking time of the invention are without being limited thereto.
More than, above-mentioned roasting process, which is arranged, to be advantageous in that, Fe, Ti group within the temperature range of low-temperature bake, in slag
Divide and chlorination salt assitant extent of reaction highest.Al, Mg component and sulfuric acid salt assitant within the temperature range of high-temperature roasting, in slag
Extent of reaction highest.It may be implemented within the scope of different temperatures by the otherness of this reactivity successively to Fe, Ti, Al, Mg
Extraction.For the heating rate of roasting, heating rate is excessively slow, and the reaction time is long, and energy consumption is excessively high, and heating rate is too fast,
It reacts insufficient, is unfavorable for the extraction of Fe, Ti, Al, Mg.
In the present embodiment, the boiling point of the chloride formed due to each element is different, after low-temperature bake, iron component and
Titanium component becomes gas, and aluminium component and magnesium component remain in first material.Sulfuric acid salt assitant mainly acts on high-temperature roasting
Stage converts soluble sulphate for aluminium, magnesium component to after first material high-temperature roasting.Therefore, the aluminium component in high titanium slag
It is enriched in the fired slags with magnesium component.And the components such as calcium, silicon contained in high titanium slag are equally enriched in because of higher boiling
In fired slags.Therefore, calcium, silicon, magnesium and aluminium component are contained in fired slags.
In the present embodiment, the water logging process of fired slags carries out in lasting stirring.Preferably, infusion can be work
One of industry water, tap water or distilled water or a variety of mixing.Certainly, infusion used in the present invention is without being limited thereto.Institute
The volume mass ratio (proportion unit can be mL/g) for stating infusion and fired slags can be 0.5~100:1.Preferably, volume
Mass ratio can be 6~80:1.The temperature of water logging can be 20 DEG C~100 DEG C, it is preferred that can be 25 DEG C~100 DEG C.Water logging
Time can be determined according to the actual amount of fired slags, for example, the time of water logging can be 0.1h~5.0h.It is arranged above-mentioned
Volume mass ratio and water soaking temperature, which are advantageous in that, both can guarantee that fired slags water logging is complete, and the reasonable benefit of resource is also ensured
With being unlikely to waste.
In the present embodiment, the fractional precipitation may include two stages.First stage may include to described first
The first precipitating reagent is added in filtrate, pH to 4.0~6.0 is adjusted at 25 DEG C~70 DEG C, is filtered after stirring, obtains aluminium hydrate powder
Body (Al (OH)3) and rich magnesium component the second filtrate, complete extraction to aluminium component.It preferably, can be at 28 DEG C~62 DEG C
It is precipitated under the conditions of adjusting pH to 4.3~5.4.First precipitating reagent can be one of aluminium hydroxide and ammonium hydroxide or two
Kind combination.The time of mixing can be 1min~120min, and certainly, mixing time can based on experience value or scene carries out
It determines.Filtering in first stage precipitating can be using one or more of natural subsidence, suction filtration or filters pressing combination.
The second precipitating reagent can be added into the second filtrate of the rich magnesium component in second stage, lower at 25 DEG C~70 DEG C
PH to 9.0~12.0 is saved, is filtered after stirring, obtains magnesium hydrate powder (Mg (OH)2) and third filtrate, it completes to magnesium component
Extraction.Preferably, it is carried out under the conditions of pH to 9.4~11.3 can be adjusted at 28 DEG C~63 DEG C.Second precipitating reagent can
Think that one or both of magnesium hydroxide and ammonium hydroxide combine.The time of mixing can be 1min~120min, certainly, stir
Mixing the time can based on experience value or scene is determined.Filtering in second stage precipitating can be using natural subsidence, suction filtration
Or one or more of filters pressing combination.
In the present embodiment, due to there is the presence of sulfuric acid salt assitant, contain sulfuric acid salt assitant in the third filtrate.To
Three filtrates can recycle sulfuric acid salt assitant after being recrystallized and be used in firing stage, realize the recycling and reusing of auxiliary agent.
In the present embodiment, extracting method of the invention can be to titanium dioxide, di-iron trioxide, three oxygen in high titanium slag
The recovery rate for changing two aluminium and magnesia reaches 50%~98%.
More than, it should be noted that there is no the sequencings carried out by the step S03 and step S04 of method of the invention.
Can with step S03 prior to step S04, can also with step S04 prior to step S03, also can with step S03 and step S04 simultaneously into
Row.
Baking inphases of the invention extract titanium in high titanium slag, iron, aluminium, magnesium component method another exemplary implementation
In example, as shown in Fig. 2, generating the chloride of iron component and titanium component due to chlorate main function and low-temperature bake stage.Sulphur
Hydrochlorate mainly acts on the high-temperature roasting stage, generates the sulfate of aluminium component and magnesium component.It therefore, can be by chlorate and sulfuric acid
Salt is separately added into reaction step of the invention.Before low-temperature bake, in the preparation process of material to be roasted, chlorate is helped
Agent is mixed with raw material high titanium slag.Then it after low-temperature bake, will obtain containing aluminium, the first material of magnesium component and sulfuric acid salt assitant
Mixing, by high-temperature roasting, obtains fired slags.Other technological parameters and titanium in above-mentioned section of roasting extraction high titanium slag, iron,
Aluminium, magnesium component method exemplary embodiment in technological parameter it is identical.
Another aspect provides a kind of portland cements.One in portland cement of the invention is exemplary
In embodiment, the portland cement include above-mentioned baking inphases extract titanium in high titanium slag, iron, aluminium, magnesium component method in it is right
The fired slags Soaking treatment, the filter residue obtained after separation of solid and liquid.
In the present embodiment, due to containing the components such as calcium, silicon, magnesium and aluminium in above-mentioned fired slags.Water logging completion in, magnesium and
Aluminium component enters the first filtrate, and calcium and silicon then enter filter residue.Due to the presence of the sulfate in auxiliary agent, and sulfate is main
High-temperature roasting is acted on, therefore, calcium and silicon components then mainly exist in the form of calcium sulfate and amorphous silica.Due to filter
It is rich in silico-calcium component in slag, meets the requirement of portland cement, portland cement can be directly applied to.
Exemplary embodiments mentioned above for a better understanding of the present invention carries out into one it below with reference to specific example
Walk explanation.
Example 1
1) the water quenching type high-titanium blast furnace slag for taking Sichuan area to generate after the ironmaking of " blast furnace process " technique is main
Raw material, respectively with ammonium chloride and ammonium sulfate with the ratio mix of molar ratio 1:1 and 1:1, then mixture is crushed,
Grinding to partial size meet 80% or more particle less than 30 μm, by mixture in 60 DEG C of drying indoor seasoning 6h.
2) mixture is placed in kiln, sets heat treatment process and parameter, specifically: with the heating rate of 1 DEG C/min,
200 DEG C are risen to by room temperature, keeps the temperature 30min.In temperature-rise period, the iron chloride of chlorination reaction generation, titanium chloride gas are evacuated to pipe
In road, iron chloride is attached on tube wall through condensation, can get chlorination iron powder body after collection.Titanium chloride gas, which is passed through in tap water, to be inhaled
It receives, can get hydrated titanium dioxide precipitating.Kiln is set after low-temperature bake with the heating rate of 1 DEG C/min, is risen by 200 DEG C
To 400 DEG C, 30min is kept the temperature, is then cooled to room temperature with kiln, obtains the fired slags of rich magnesium aluminium component.Wherein, low-temperature bake rank
Section chlorination auxiliary agent is back to firing stage after volatilization condensation, and during low-temperature bake, condensation temperature is successively set as 280 DEG C
With 250 DEG C.
3) it is mixed after taking out fired slags with tap water with the ratio of volume mass ratio 1:1, is heated to stirring water logging at room temperature
10min obtains infusion (the first filtrate) and the water logging slag (filter residue) rich in calcium, silicon rich in magnesium, aluminium component.To rich magnesium aluminium group
Ammonium hydroxide is added in the infusion divided, adjust pH value at room temperature and is maintained in 4.0~6.0 ranges, stirs filtering point after 10min
From acquisition aluminium hydroxide powder and rich magnesium component infusion；Ammonium hydroxide is added into rich magnesium component infusion, adjusts pH at room temperature
It is worth and is maintained in 9.0~12.0 ranges, is separated by filtration acquisition magnesium hydrate powder after stirring 20min.Rich calcium silicon water logging slag at
Divide and meet portland cement, can directly be applied.
Example 2
1) the water quenching type high-titanium blast furnace slag for taking Sichuan area to generate after the ironmaking of " blast furnace process " technique is main
Raw material, respectively with ammonium chloride and ammonium sulfate with the ratio mix of molar ratio 8:1 and 8:1, then mixture is crushed,
Grinding to partial size meet 80% or more particle less than 50 μm, by mixture in 80 DEG C of drying indoor seasoning 8h.
2) mixture is placed in kiln, sets heat treatment process and parameter, specifically: with the heating speed of 10 DEG C/min
Rate rises to 400 DEG C by room temperature, keeps the temperature 180min, and in temperature-rise period, iron chloride, the titanium chloride gas that chlorination reaction is generated are taken out
Into exhaust pipe, iron chloride is attached on tube wall through condensation, can get chlorination iron powder body after collection.Titanium chloride gas is passed through certainly
It is absorbed in water, can get hydrated titanium dioxide precipitating.Kiln is set after low-temperature bake with the heating rate of 10 DEG C/min,
800 DEG C are risen to by 400 DEG C, 180min is kept the temperature, is then cooled to room temperature with kiln, obtains the fired slags of rich magnesium aluminium component.Wherein,
Low-temperature bake stage chlorination auxiliary agent is back to firing stage after volatilization condensation, and tunnel kiln is opened during low-temperature bake
Gas collection and phase condensation device, condensation temperature are successively set as 280 DEG C and 250 DEG C.
3) it is mixed after taking out fired slags with tap water with the ratio of volume mass ratio 1:100, stirs water logging at room temperature
180min obtains infusion and the water logging slag rich in calcium, silicon rich in magnesium, aluminium component.Add into the infusion of rich magnesium aluminium component
Enter ammonium hydroxide, adjust pH value at room temperature and be maintained in 4.0~6.0 ranges, is separated by filtration acquisition hydroxide after stirring 120min
Aluminium powder body and rich magnesium component infusion；Ammonium hydroxide is added into rich magnesium component infusion, adjust pH value at room temperature and is maintained at 9.0
In~12.0 ranges, acquisition magnesium hydrate powder is separated by filtration after stirring 180min.Rich calcium silicon water logging slag ingredient meets silicate
Cement can be applied directly.
In conclusion an aspect of of the present present invention carries out titanium, iron, aluminium and the magnesium in high titanium slag using the method for baking inphases
It extracts, the low-temperature bake stage realizes the extraction of titanium, iron component under chlorination salt action, and the high-temperature roasting stage is under sulfuric acid salt action
Realize the extraction of aluminium, magnesium component, simple process, process be short, it is high-efficient, be more advantageous to commercial introduction；On the other hand, the present invention makes
Amount of auxiliary is few, extracts valuable component relative to traditional acid hydrolyzation, avoids because of the wasting of resources caused by using a large amount of sulfuric acid
The adverse effect caused by environment is formed with sulfuric acid mist；And it roasts auxiliary agent in method of the invention to continue back after recrystallizing
For firing stage, the utilization rate of auxiliary agent is improved, process costs are reduced；In another aspect, method of the invention is to TiO2、
Fe2O3、Al2O3, MgO recovery rate can reach 50%~98%, the product being prepared is all satisfied or is higher than national (industry) mark
It is quasi-；In another aspect, the requirement that Silicon-rich Calcium compounds tailings meets portland cement is remained in method of the invention after the reaction was completed, it can
It is directly used in production of construction materials, the big residue of no environmental pollution generates.
Although those skilled in the art should be clear above by combining exemplary embodiment to describe the present invention
Chu can carry out exemplary embodiment of the present invention each without departing from the spirit and scope defined by the claims
Kind modifications and changes.
Claims (10)
1. a kind of baking inphases extract titanium in high titanium slag, iron, aluminium, magnesium component method, which is characterized in that the method includes with
Lower step:
Grinding, classification, obtain material to be roasted after high titanium slag is mixed with auxiliary agent；
The material to be roasted is subjected to low-temperature bake, obtain iron content, titanium component enriched gas and containing aluminium, magnesium component first
Material；
Temperature control is carried out to the iron content, titanium component enriched gas and sublimates processing to obtain iron content for iron component and titanium component separation
Solid and titaniferous gas, and the titaniferous gas is hydrolyzed, complete the separation and Extraction to iron component and titanium component in high titanium slag；
High-temperature roasting is carried out to the first material containing aluminium, magnesium component, obtains fired slags；
To the fired slags Soaking treatment, it is separated by solid-liquid separation, obtains filter residue and the first filtrate comprising aluminium ion, magnesium ion；
Precipitating reagent is added in first filtrate, control pH is completed so that aluminium ion and magnesium ion fractional precipitation to high titanium slag
The separation and Extraction of middle aluminium component and magnesium component, wherein
The auxiliary agent is the mixture of chlorate and sulfate, and low-temperature bake temperature is 100 DEG C~400 DEG C, high-temperature roasting temperature
It is 400 DEG C~800 DEG C.
2. a kind of baking inphases extract titanium in high titanium slag, iron, aluminium, magnesium component method, which is characterized in that the method includes with
Lower step:
Grinding, classification, obtain material to be roasted after high titanium slag is mixed with chlorination salt assitant；
The material to be roasted is subjected to low-temperature bake, obtain iron content, titanium component enriched gas and containing aluminium, magnesium component first
Material；
Temperature control is carried out to the iron, titanium component enriched gas and sublimates processing so that it is solid to obtain iron content by iron component and titanium component separation
Body and titaniferous gas, and the titaniferous gas is hydrolyzed, complete the separation and Extraction to iron component and titanium component in high titanium slag；
After the first material containing aluminium, magnesium component is mixed with sulfuric acid salt assitant, high-temperature roasting obtains fired slags；
To the fired slags Soaking treatment, it is separated by solid-liquid separation, obtains filter residue and the first filtrate comprising aluminium ion, magnesium ion；
Precipitating reagent is added in first filtrate, control pH is completed so that aluminium ion and magnesium ion fractional precipitation to high titanium slag
The separation and Extraction of middle aluminium component and magnesium component, wherein
The temperature of the low-temperature bake is 100 DEG C~400 DEG C, the temperature of high-temperature roasting is 400 DEG C~800 DEG C.
3. baking inphases according to claim 1 or 2 extract titanium in high titanium slag, iron, aluminium, magnesium component method, feature
It is, the high titanium slag is water quenching type high-titanium blast furnace slag, and the component of the water quenching type high-titanium blast furnace slag includes, by mass percentage
Meter, Fe2O3Content is 2%~8%, TiO2Content is 10%~25%, Al2O3Content be 8%~15%, content of MgO be 5%~
12%.
4. baking inphases according to claim 1 or 2 extract titanium in high titanium slag, iron, aluminium, magnesium component method, feature
It is, 80% or more grain diameter of the material to be roasted is 30 μm~200 μm.
5. baking inphases according to claim 1 or 2 extract titanium in high titanium slag, iron, aluminium, magnesium component method, feature
It is, the high titanium slag is titanium-containing blast furnace slag obtained by vanadium titano-magnetite blast furnace process through the resulting tail of high temperature cabonization-low temperature chlorination
Slag.
6. baking inphases according to claim 1 or 2 extract titanium in high titanium slag, iron, aluminium, magnesium component method, feature
It is, the ratio of the chlorate and the sulfate quality sum and the high titanium slag quality is 0.1~10:1.
7. baking inphases according to claim 1 or 2 extract titanium in high titanium slag, iron, aluminium, magnesium component method, feature
It is, the temperature control is sublimated including condensing to iron, titanium component enriched gas, and iron component gas recrystallization is completed to high titanium
The extraction of iron component in slag；
Titanium component gas is collected using liquid-absorbant, obtains aqua oxidation titanium solution, is completed to titanium component in high titanium slag
Extraction.
8. baking inphases according to claim 1 or 2 extract titanium in high titanium slag, iron, aluminium, magnesium component method, feature
It is, the Soaking treatment carries out Soaking treatment, the water logging to the fired slags in whipping process including the use of infusion
The volume mass ratio of liquid and the fired slags is 0.5~100:1, and the temperature of the Soaking treatment is 20 DEG C~100 DEG C.
9. baking inphases according to claim 1 or 2 extract titanium in blast furnace slag, iron, aluminium, magnesium component method, feature
It is, the fractional precipitation includes:
The first precipitating reagent is added into first filtrate, pH to 4.0~6.0 is adjusted at 25 DEG C~70 DEG C, is filtered after stirring,
Obtain the second filtrate of aluminium hydroxide powder and rich magnesium component, wherein the first precipitating reagent is one of aluminium hydroxide and ammonium hydroxide
Or two kinds of combinations；
The second precipitating reagent is added into the second filtrate of the rich magnesium component, pH to 9.0~12.0 is adjusted at 25 DEG C~70 DEG C,
It is filtered after stirring, obtains magnesium hydrate powder, wherein second precipitating reagent is one or both of magnesium hydroxide and ammonium hydroxide
Combination.
10. a kind of portland cement, which is characterized in that the portland cement includes by claim 1 or claim 2 institute
The baking inphases stated extract titanium in blast furnace slag, iron, aluminium, magnesium component method in the fired slags Soaking treatment, be separated by solid-liquid separation
The filter residue obtained afterwards.
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