CN106319246A - Granulation method of fine-fraction titanium-rich material - Google Patents
Granulation method of fine-fraction titanium-rich material Download PDFInfo
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- CN106319246A CN106319246A CN201610712820.2A CN201610712820A CN106319246A CN 106319246 A CN106319246 A CN 106319246A CN 201610712820 A CN201610712820 A CN 201610712820A CN 106319246 A CN106319246 A CN 106319246A
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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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- 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
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/242—Binding; Briquetting ; Granulating with binders
- C22B1/243—Binding; Briquetting ; Granulating with binders inorganic
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Abstract
The invention provides a granulation method of a fine-grained titanium-rich material, which belongs to the technical field of titanium-rich material production, and specifically comprises the steps of preparing a proper amount of sodium hydroxide or potassium hydroxide into a binder with a proper amount of water, adding the fine-grained titanium-rich material into an agglomeration granulation or fluidization granulator, uniformly spraying the prepared binder into the titanium-rich material for granulation, drying the granulated product at 50-100 ℃, and calcining and curing at 500-1200 ℃ to obtain a granular titanium-rich material product meeting the requirement of the boiling chlorination process. The granulation method has the advantages of easily available binder source, low granulation cost, moderate granularity of the obtained titanium-rich material, good compression strength and heat resistance of the particles and high chlorination reaction activity, is suitable for granulating the fine-grained titanium-rich material obtained by leaching and removing impurities from ilmenite, titanium concentrate or titanium slag, and is particularly suitable for producing the high-quality titanium-rich material suitable for the boiling chlorination process by utilizing the titanium concentrate containing high calcium and magnesium.
Description
Technical field
The invention belongs to rich-titanium material production technical field, be specifically related to fine fraction rich-titanium material prilling process.
Background technology
Rich-titanium material includes high titanium slag and synthetic rutile.Along with titanium sponge and the fast development of chloride process titanium dioxide, to Gao Pin
The demand of position rich-titanium material increases rapidly, especially because environmental requirement is increasingly stricter, the grade requirement of rich-titanium material is tended to height
Shelvesization.The rich-titanium material production method of application divides pyrogenic process and wet method at present, and pyrogenic process is that electro-smelting produces, and wet method mainly includes reduction
Bubble method, the salt acid-hatching of young eggs etc..
Electric furnace smelting process because production technology is simple, " three wastes " less, the feature such as the recyclable pig iron, be that current rich-titanium material produces
Main method.But electric furnace smelting process power consumption is big, typically in the area use that electric power is more sufficient.It addition, smelting process is to calcium, magnesium etc.
The removing ability of non-ferrous impurities, for the ilmenite high to content of calcium and magnesium, the titanium slag grade that electro-smelting produces is low, and calcium,
Content of magnesium is high, is not suitable for fluidizing chlorination requirement.
For the ilmenite that content of calcium and magnesium is high, hydrochloric acid leaching process is a kind of effective method, and its leaching velocity is fast, remove impurity
Ability is strong, synthetic rutile of high grade, but leaching process efflorescence is serious.The reason of hydrochloric acid leaching process rutile efflorescence includes
Physics efflorescence and chemical pulverization.When physics efflorescence is due to leaching, touching between granule or between granule and other materials
Hit, friction etc. makes the efflorescence that grain breakage produces.Chemical pulverization is then due to salt Ore Leaching early stage, part TiO2Hydrochloric acid can be dissolved in
In, along with reaction is carried out, acid concentration reduces, the titanium that early stage the is dissolved TiO that hydrolysis precipitation is fine from solution again2, chemical pulverization
Being the main cause of synthetic rutile efflorescence, during ilmenite raw ore direct salt Ore Leaching, the pulverization rate of synthetic rutile reaches
About 30%.Fine powder is unfavorable to fluidizing chlorination operation, and thinner material easily forms channel in fluidization process, causes gas
Utilization rate reduces；Fine powder easily escapes with going out furnace gases when fluidizing chlorination simultaneously, causes significant loss, reduces yield.Cause
This, during as fluidizing chlorination raw material, it is desirable to the fine powder of below particle diameter 0.1mm is less than 25%.Although ilmenite is through peroxidating, reduction
Salt Ore Leaching again after pretreatment, can alleviate pulverization rate, but still can not be fully solved its pulverizing problem.Especially because domestic 90%
Ilmenite belong to calcium-magnesium-containing Gao Yan ore deposit, mostly ilmenite concentrate is to flotate in the mine tailing choose iron ore concentrate, often granularity
Relatively thin (the accounting for more than 70% of-74 μm), even if increasing operation to sub-elect the product of+74 μm from ilmenite concentrate product, but owing to solving
Low from degree and that Si, Ca and Mg amount is high problem, gained synthetic rutile product granularity can not be directly used in existing boiling chlorine
Metallization processes.Therefore, the granulation how solving fine fraction rich-titanium material is most important to producing fluidizing chlorination rich-titanium material.
Summary of the invention
Present invention aims to existing rich-titanium material produce present in pulverization rate is high, fine fraction rich-titanium material is difficult to full
The problems such as foot fluidizing chlorination production requirement, propose a kind of fine fraction rich-titanium material prilling process, thus realize fine fraction rich-titanium material
Low cost pelletize, it is thus achieved that the rich-titanium material that granularity is moderate, comprcssive strength is high, heat resistance is good, chlorization activity is good.The purpose of the present invention
It is achieved through the following technical solutions.
Fine fraction rich-titanium material prilling process, using caustic alkali or caustic solution is binding agent, by rich-titanium material and binding agent
Through Granulation Equipments pelletize after mixing, then solidification obtains meeting the granule rich-titanium material product of fluidizing chlorination process grain size requirement.Institute
State the mixture that caustic alkali is the one or both in sodium hydroxide, potassium hydroxide.
Further, described Granulation Equipments is Squeezinggranulator, extruding granulator, sponging granulator, granulating disc, stream
Change the one in comminutor.
Further, described solidification is to calcine granulation product after drying to obtain granule rich-titanium material, calcining heat be 500～
1200 DEG C, preferable temperature is 700～1000 DEG C.
Further, described meets the granule rich-titanium material product that fluidizing chlorination process grain size requires, its granularity is whole
By 0.5mm sieve aperture, wherein siftage≤25% of below 0.1mm.
Further, described rich-titanium material is mixed with binding agent after through Granulation Equipments pelletize be: by rich-titanium material with quantitatively viscous
Knot agent mix homogeneously, then uses Squeezinggranulator or extruding granulator pelletize.Or rich-titanium material is entered disk after drying make
In grain machine or fluidisation granulator, then quantitative binding agent is sprayed in rich-titanium material equably and carries out pelletize.Described quantitative bonding
Agent is the sodium hydroxide solution quantitative sodium hydroxide and quantitative water being mixed to get, and sodium hydroxide concentration therein is rich titanium
The 0.2～2.5% of material quality, water consumption is the 5～20% of rich-titanium material quality.
Further, described rich-titanium material is mixed with binding agent after through Granulation Equipments pelletize it may also is that be 50 by concentration
～the sodium hydroxide solution of 200g/L mixes 1～4h by liquid-solid mass ratio 2:1～5:1 with rich-titanium material at temperature 40～100 DEG C,
Filtering, filter cake is washed with water to Na in filter cake2O mass content 0.2～2%, then by the filtration cakes torrefaction after washing to aqueous 1～
Carry out disk pelletizing after 20% or roll-in is pelletized, calcining solidification obtains granule rich-titanium material, or by solid for the filter cake calcining after washing
Crush after change, classification obtains granule rich-titanium material.
Further, siftage >=30% that granularity is 0.1mm of described fine fraction rich-titanium material, TiO2Mass content >=
85%.
Further, described fine fraction rich-titanium material is the mixture of one or more in ilmenite, ilmenite concentrate, titanium slag
Obtain through leaching remove impurity, the artificial golden red that preferably ilmenite or ilmenite concentrate hydrochloric acid leaching process obtain after removing calcium, magnesium, ferrum
Stone powder.
The present invention uses sodium hydroxide or potassium hydroxide solution to do the adhesive for granulating of fine fraction rich-titanium material, is suitably adapted for squeezing
The multiple prillings such as pressure comminutor, extruding granulator, sponging granulator, granulating disc, fluidisation granulator, have and are a granulated into
This is the lowest, it is thus achieved that rich-titanium material granularity moderate, grain compressive strength is good with heat resistance, the active height of chlorination reaction.
Detailed description of the invention
Fine fraction rich-titanium material adhesive for granulating and prilling process, by appropriate sodium hydroxide or potassium hydroxide with appropriate water
Being modulated into binding agent standby, wherein the consumption of sodium hydroxide or potassium hydroxide is the 0.2～2.5% of rich-titanium material quality, the use of water
Amount is the 5～20% of rich-titanium material quality；Then fine fraction rich-titanium material is added in agglomeration granulation or fluidisation granulator, then will adjust
The binding agent of system is sprayed at uniformly in rich-titanium material and carries out pelletize, and granulation product is dried again 500～1200 in 50～100 DEG C
DEG C calcining solidification obtain the granule rich-titanium material that granularity is moderate.
In some implementations, it is also possible to be that sodium hydroxide is configured to sodium hydroxide that concentration is 50～200g/L in advance is molten
Liquid is standby, and the consumption of sodium hydroxide and water is not by rich-titanium material matter quantitative limitation, and then sodium hydroxide solution and rich-titanium material are by liquid-solid
Mass ratio 2:1～5:1 stirs mixing 1～4h at temperature 40～100 DEG C, filters, and filtrate can be recycled, and filter cake washes with water
Na to dry filter cake2O mass content 0.2～2%, then carries out disk by the filtration cakes torrefaction after washing after aqueous 5～20%
Pelletize or extruder grain, then calcining solidification obtains granule rich-titanium material.The naoh concentration of described sodium hydroxide solution is.
The present invention can be used for being obtained through leaching remove impurity by the mixture of one or more in ilmenite, ilmenite concentrate, titanium slag
Fine fraction rich-titanium material, siftage >=30% that granularity is 0.1mm of described fine fraction rich-titanium material, TiO2Mass content >=
85%.It is particularly well-suited to the fine fraction synthetic rutile powder obtained after hydrochloric acid leaching process removes calcium, magnesium, ferrum by ilmenite concentrate.
During enforcement, Granulation Equipments section selects Squeezinggranulator, extruding granulator, sponging granulator, agglomeration granulation machine, fluidisation
The Granulation Equipments of the routine such as comminutor and technique, preferably granulating disc.
With following nonlimiting examples, the method for the present invention is further described, to contribute to understanding the present invention's
Content and advantage thereof, and not as limiting the scope of the present invention, protection scope of the present invention is determined by claims.
Embodiment 1
1kg sodium hydroxide 10kg water dissolution is obtained caustic alkali binding agent standby, will be obtained through salt Ore Leaching by ilmenite concentrate
To all by 0.1mm sieve aperture, containing TiO2The synthetic rutile powder 100kg of 94.2% at the uniform velocity adds granulating disc on one side, and one
While pelletize in the synthetic rutile powder surface being sprayed onto in disk pelletizing at the uniform velocity, uniformly by the binding agent of modulation, comminutor
Product out is dried at 80 DEG C, calcines 1h in 1000 DEG C, i.e. obtained the sieve of 0.45mm sieve aperture, wherein below 0.1mm
Lower thing accounts for the granule rich-titanium material of 5%.
Embodiment 2
By by ilmenite concentrate through salt Ore Leaching obtain whole by 0.1mm sieve aperture, containing TiO2The artificial golden red of 94.2%
Stone, mixes 1h with the sodium hydroxide solution that concentration is 200g/L according to liquid-solid mass ratio 3:1 at 70 DEG C, then filters, filter cake
It is washed with water to Na in dry meter filter cake2O mass content 0.5%, after drying in 900 DEG C of solidifications, then broken, classification obtained
0.45mm sieves, and the granule rich-titanium material product that 0.1mm siftage is less than 20%.
Embodiment 3
By by ilmenite concentrate through salt Ore Leaching obtain whole by 0.1mm sieve aperture, containing TiO2The artificial golden red of 94.2%
Stone, mixes 1h with the sodium hydroxide solution that concentration is 200g/L according to liquid-solid mass ratio 3:1 at 70 DEG C, then filters, filter cake
Be washed with water to pH value 9～11, then filter, filtration cakes torrefaction to the most aqueous be less than 5% after add disk pelletizing machine, simultaneously uniformly spray
Spilling suitable quantity of water to pelletize, granulator product out is dried at 80 DEG C, calcines 1h in 900 DEG C, i.e. obtained 0.45mm
The siftage of sieve aperture, wherein below 0.1mm accounts for the granule richness titanium of 5%.
Embodiment 4
1kg sodium hydroxide 15kg water dissolution is obtained caustic alkali binding agent, then with 100kg by ilmenite concentrate through salt acidleach
Go out obtain whole by 0.1mm sieve aperture, containing TiO2The synthetic rutile powder mix homogeneously of 94.2%, then mixes gained
Expecting to pelletize through roll squeezer, then calcining solidification obtains meeting the rich-titanium material of fluidizing chlorination particle requirement.
Claims (10)
1. fine fraction rich-titanium material prilling process, it is characterised in that using caustic alkali or caustic solution is binding agent, by rich-titanium material
Through Granulation Equipments pelletize after mixing with binding agent, then solidification obtains meeting the granule rich-titanium material of fluidizing chlorination process grain size requirement
Product, described caustic alkali is the mixture of the one or both in sodium hydroxide, potassium hydroxide.
Prilling process the most according to claim 1, it is characterised in that described Granulation Equipments is agglomeration granulation machine, fluidizes and make
One in grain machine, Squeezinggranulator, extruding granulator, sponging granulator.
Prilling process the most according to claim 1, it is characterised in that described solidification is in 50～100 DEG C by granulation product
Being dried, then calcining obtains granule rich-titanium material product, and calcining heat is 500～1200 DEG C, preferably 700～1000 DEG C.
Prilling process the most according to claim 3, it is characterised in that described meets what fluidizing chlorination process grain size required
Granule rich-titanium material product, its granularity is all by 0.5mm sieve aperture, wherein siftage≤25% of below 0.1mm.
Prilling process the most according to claim 1, it is characterised in that described granulation process is particularly as follows: be dried rich-titanium material
In rear addition agglomeration granulation machine or fluidisation granulator, then quantitative binding agent is sprayed in rich-titanium material equably and carries out pelletize；
Described quantitative binding agent is the caustic solution quantitative sodium hydroxide or potassium hydroxide being mixed to get with quantitative water, wherein
Sodium hydroxide or consumption is rich-titanium material quality the 0.2～2.5% of potassium hydroxide, water consumption be rich-titanium material quality 5～
20%.
Prilling process the most according to claim 1, it is characterised in that described granulation process is particularly as follows: molten by sodium hydroxide
Liquid and rich-titanium material are stirred at temperature 40～100 DEG C by liquid-solid mass ratio 2:1～5:1 and mix 1～4h, filter, and filtrate returns and follows
Ring uses, and filter cake is washed with water in filter cake dry meter containing Na2O mass 0.2～2%, then by the filtration cakes torrefaction after washing to containing
Carrying out disc granulation or extruder grain after water 1～20%, the concentration of described sodium hydroxide solution is 50～200g/L.
Prilling process the most according to claim 6, it is characterised in that by solid for dinectly bruning after the filtration cakes torrefaction after washing
Changing, then broken, classification obtains granule rich-titanium material.
Prilling process the most according to claim 1, it is characterised in that described fine fraction rich-titanium material is ilmenite, titanium essence
The mixture of one or more in ore deposit, titanium slag obtains through leaching remove impurity.
Prilling process the most according to claim 8, it is characterised in that the granularity of described fine fraction rich-titanium material is 0.1mm
Siftage >=30%, TiO2Mass content >=85%.
Prilling process the most according to claim 8, it is characterised in that described fine fraction rich-titanium material is ilmenite or titanium
The synthetic rutile powder that concentrate hydrochloric acid leaching process obtains after removing calcium, magnesium, ferrum.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109761271A (en) * | 2019-03-29 | 2019-05-17 | 河南佰利联新材料有限公司 | A method of recycling titaniferous fines |
| CN110563034A (en) * | 2019-09-29 | 2019-12-13 | 河南佰利联新材料有限公司 | Preparation of chlorination-process TiO by using titanium-rich fine powder2Method for preparing raw material |
| CN110627119A (en) * | 2019-09-29 | 2019-12-31 | 河南佰利联新材料有限公司 | Preparation of chlorination method TiO by using titanium-containing fine powder2Method for preparing raw material |
| CN113215396A (en) * | 2020-01-21 | 2021-08-06 | 有研工程技术研究院有限公司 | Method for granulating fine-particle titanium concentrate or titanium-rich material |
| CN114702062A (en) * | 2022-04-02 | 2022-07-05 | 中南大学 | Method for granulating fine titanium-rich material |
| CN114702063A (en) * | 2022-04-02 | 2022-07-05 | 中南大学 | Method for preparing fluidized chlorination furnace charge by granulating fine titanium-rich material |
| CN114702061A (en) * | 2022-04-02 | 2022-07-05 | 中南大学 | Granulation method of fine-particle titanium-rich material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110563034A (en) * | 2019-09-29 | 2019-12-13 | 河南佰利联新材料有限公司 | Preparation of chlorination-process TiO by using titanium-rich fine powder2Method for preparing raw material |
| CN110627119A (en) * | 2019-09-29 | 2019-12-31 | 河南佰利联新材料有限公司 | Preparation of chlorination method TiO by using titanium-containing fine powder2Method for preparing raw material |
| CN110627119B (en) * | 2019-09-29 | 2022-05-13 | 河南佰利联新材料有限公司 | Preparation of chlorination-process TiO by using titanium-containing fine powder2Method for preparing raw material |
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| CN113215396A (en) * | 2020-01-21 | 2021-08-06 | 有研工程技术研究院有限公司 | Method for granulating fine-particle titanium concentrate or titanium-rich material |
| CN114702062A (en) * | 2022-04-02 | 2022-07-05 | 中南大学 | Method for granulating fine titanium-rich material |
| CN114702063A (en) * | 2022-04-02 | 2022-07-05 | 中南大学 | Method for preparing fluidized chlorination furnace charge by granulating fine titanium-rich material |
| CN114702061A (en) * | 2022-04-02 | 2022-07-05 | 中南大学 | Granulation method of fine-particle titanium-rich material |
| CN114702062B (en) * | 2022-04-02 | 2024-02-23 | 中南大学 | Method for granulating fine-grain titanium-rich material |
| CN114702061B (en) * | 2022-04-02 | 2024-03-26 | 中南大学 | Granulating method of fine-grain titanium-rich material |
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