CN110002889A - A kind of Ti (C, N) base refractory material and the method for producing Ti (C, N) base refractory material using 50 titanium slags - Google Patents
A kind of Ti (C, N) base refractory material and the method for producing Ti (C, N) base refractory material using 50 titanium slags Download PDFInfo
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- CN110002889A CN110002889A CN201910417245.7A CN201910417245A CN110002889A CN 110002889 A CN110002889 A CN 110002889A CN 201910417245 A CN201910417245 A CN 201910417245A CN 110002889 A CN110002889 A CN 110002889A
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/138—Waste materials; Refuse; Residues from metallurgical processes, e.g. slag, furnace dust, galvanic waste
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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Abstract
The present invention provides a kind of Ti (C, N) base refractory material and 50 titanium slags of use produce Ti (C, N) the method for base refractory material, belong to secondary resource technical field of comprehensive utilization, the present invention produces Ti (C using 50 titanium slags, N) method of base refractory material obtains mixture the following steps are included: by 50 titanium slag powder and the mixing of carbonaceous reducing agent powder;The mixture is subjected to pelletizing, obtains pelletizing;Under a nitrogen atmosphere, the pelletizing is roasted, nitridation and carburizing reagent occurs, obtains Ti (C, N) base refractory material.The present invention prepares Ti (C using 50 titanium slags and carbonaceous reducing agent as raw material, N) base refractory material, the ingredient in 50 titanium slags is not only set to be utilized effectively, and preparation process equipment is simple, raw material is cheap and easy to get, production cost is low, refractory material high temperature resistance obtained is preferable, refractoriness >=2000 DEG C.
Description
Technical field
The present invention relates to secondary resource technical field of comprehensive utilization more particularly to a kind of Ti (C, N) base refractory material and
The method for producing Ti (C, N) base refractory material using 50 titanium slags.
Background technique
Sichuan, China be famous vanadium titanium all, possess a large amount of vanadium and titanium resources.50 titanium slags refer to TiO2Content
The titanium slag obtained for 45~55%, sefstromite concentrate by non-blast furnace process.
50 titanium slags are a kind of secondary resources, and in the process of development, existing main problem is that utilization rate is not high, also, mesh
Preceding processing and application to 50 titanium slags still not no mature techniqueflow, leads to the useful member such as Ti, Mg, Si, Ca in 50 titanium slags
Element is not fully utilized.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for producing Ti (C, N) base refractory material using 50 titanium slags, make 50 titaniums
Slag is utilized effectively, and preparation method is simple, at low cost, and obtained Ti (C, N) base refractory material fire resistance is good.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of methods for producing Ti (C, N) base refractory material using 50 titanium slags, comprising the following steps:
50 titanium slag powder and carbonaceous reducing agent powder are mixed, mixture is obtained;
The mixture is subjected to pelletizing, obtains pelletizing;
Under a nitrogen atmosphere, the pelletizing is roasted, nitridation and carburizing reagent occurs, obtains Ti (C, N) base fire resisting
Material.
Preferably, the partial size of the 50 titanium slag powder and carbonaceous reducing agent powder independently is 100~325 mesh.
Preferably, the mass ratio of the 50 titanium slag powder and carbonaceous reducing agent powder is 1:(0.4~0.7).
Preferably, the chemical composition of the 50 titanium slag powder is TiO2: 45~55wt.%;SiO2: 10~15wt.%;
CaO:3~9wt.%;MgO:10~15wt.%;Al2O3: 14~16wt.% and FeO:1~3wt.%.
Preferably, the carbonaceous reducing agent powder is coke, semi-coke, the one or more of coal dust and petroleum coke.
Preferably, the temperature of the roasting is 1500~1900 DEG C, and the time is 20~60min.
Preferably, the diameter of the pelletizing is 8~15mm.
Preferably, the amount ratio of the nitrogen and 50 titanium slag powder is 32~36L:1kg.
Ti (C, N) the base refractory material being prepared the present invention also provides above-mentioned technical proposal the method, the Ti
(C, N) base refractory material includes TiN:24~28wt.%;TiC:23~27wt.%;SiC:15~19wt.%;CaC2:7~
10wt.%;MgC2:17~21wt.% and Fe3C:1~3wt.%.
The present invention provides a kind of methods for producing Ti (C, N) base refractory material using 50 titanium slags, comprising the following steps: will
50 titanium slag powder and the mixing of carbonaceous reducing agent powder, obtain mixture;The mixture is subjected to pelletizing, obtains pelletizing;In nitrogen
Under the conditions of gas, pelletizing is roasted, nitridation and carburizing reagent occurs, obtains Ti (C, N) base refractory material.The present invention is with 50 titaniums
Slag is raw material, TiO when roasting in 50 titanium slags2It reacts with nitrogen and generates TiN and carbonaceous reducing agent reaction generation TiC;
SiO2It is reacted with carbonaceous reducing agent and generates SiC;CaO and carbonaceous reducing agent react, and generate CaC2;MgO and carbonaceous reducing agent hair
Raw reaction, generates MgC2;FeO and carbonaceous reducing agent react, and generate Fe3C is obtained containing TiN, TiC, SiC, CaC2、MgC2
And Fe3Ti (C, N) base refractory material of C.
When the present invention prepares Ti (C, N) base refractory material, using 50 titanium slags and carbonaceous reducing agent as raw material, process equipment letter
List, raw material is cheap and easy to get, production cost is low, and Ti (C, N) base refractory material obtained is mainly formed by titanium carbide and titanium nitride
Solid solution, there are high-melting-point, corrosion-resistant, the high temperature resistance characteristics such as preferably, refractoriness >=2000 DEG C.
Specific embodiment
The present invention provides a kind of methods for producing Ti (C, N) base refractory material using 50 titanium slags, comprising the following steps:
50 titanium slag powder and carbonaceous reducing agent powder are mixed, mixture is obtained;
The mixture is subjected to pelletizing, obtains pelletizing;
Under a nitrogen atmosphere, pelletizing is roasted, nitridation and carburizing reagent occurs, obtains Ti (C, N) base fire proofed wood
Material.
The present invention mixes 50 titanium slag powder and carbonaceous reducing agent powder, obtains mixture.
In the present invention, the mass ratio of the 50 titanium slag powder and carbonaceous reducing agent powder is preferably 1:(0.4~0.7),
Further preferably 1:(0.5~0.6).The present invention controls the mass ratio of 50 titanium slag powder and carbonaceous reducing agent powder above-mentioned
Range is conducive to generate the good Ti of fire resistance (C, N) base refractory material.
In the present invention, the partial size of the 50 titanium slag powder and carbonaceous reducing agent powder is independently preferably 100~325
Mesh, more preferably 200~325 mesh.The present invention is to the preparation method of the 50 titanium slag powder and carbonaceous reducing agent powder without spy
It is different to require, using preparation method well known to those skilled in the art, specifically such as broken, grinding.
In the present invention, the chemical composition of the 50 titanium slag powder is preferred are as follows: TiO2: 45~55wt.%; SiO2: 10~
15wt.%;CaO:3~9wt.%;MgO:10~15wt.%;Al2O3: 14~16wt.% and FeO:1~3wt.%.
50 titanium slag powder of the present invention preferably includes the TiO of 45~55wt.%2, more preferably 47~53wt.%;This
Invent the SiO that the 50 titanium slag powder preferably includes 10~15wt.%2, more preferably 11~14wt.%;Of the present invention 50
Titanium slag powder preferably includes the CaO of 3~9wt.%, more preferably 4~9wt.%;50 titanium slag powder of the present invention preferably wraps
Include the MgO of 10~15wt.%, more preferably 11~14wt.%;50 titanium slag powder of the present invention preferably includes 14~
The Al of 16wt.%2O3, more preferably 14~15wt.%;50 titanium slag powder of the present invention preferably includes the FeO of 1~3wt.%,
More preferably 2~3wt.%.
50 titanium slags that the present invention preferentially handles above-mentioned composition are conducive to improve the heat-resisting quantity of Ti (C, N) base refractory material
Energy.In the present invention, the carbonaceous reducing agent powder is preferably one or more of coke, semi-coke, coal dust and petroleum coke.
In the present invention, the mixing is preferably ball milling mixing;The revolution of the ball milling mixing is preferably 100~200r/
Min, more a step are preferably 150~200r/min;The time of the ball milling mixing is preferably 20min~60min, further excellent
It is selected as 30~50min.The partial size of the mixture obtained after ball milling mixing of the present invention is preferably 200~325 mesh.
After obtaining mixture, the mixture is carried out pelletizing by the present invention, obtains pelletizing.Work of the present invention to the pelletizing
Skill does not have particular/special requirement, using conventional rolling moulding process or pressure molding well known to those skilled in the art.
In a specific embodiment of the present invention, it is preferred to use disc balling machine carries out pelletizing.In the present invention, the diameter of the pelletizing is excellent
It is selected as 8~15mm, more preferably 10~12mm.The present invention roasts again after mixture is carried out pelletizing, compared to the mixing of powder shaped
Material or block-like mixture are roasted, and the gas permeability of pelletizing is more preferable after pelletizing.The present invention is by pelletizing diameter control above-mentioned
Range is conducive to shorten calcining time, while guaranteeing the intensity of sample after roasting.
After obtaining pelletizing, the present invention under a nitrogen atmosphere, is roasted the pelletizing, and nitridation and carburizing reagent occurs,
Obtain Ti (C, N) base refractory material.
In the present invention, the temperature of the roasting is preferably 1500~1900 DEG C, and more preferably 1700~1900 DEG C;Institute
The time for stating roasting is preferably 20~60min, more preferably 30~60min.The present invention controls maturing temperature in above range,
Be conducive to improve the fire resistance of Ti (C, N) base refractory material.When temperature is increased to 2000 DEG C, the Al in titanium slag2O3Also with carbonaceous
Former agent reacts, and generates Al4C3, and Al4C3It is easily decomposed into methane and aluminium hydroxide, aluminium hydroxide fusing point is 300 DEG C, is influenced
The performance of refractory material.
In the present invention, the amount ratio of the nitrogen and 50 titanium slag powder is preferably 34~36L:1kg.Nitrogen of the present invention
Gas preferentially with the TiO in raw material2Nitridation reaction occurs, generates TiN, nitrogen use level is excessive, and the TiN of generation is more, consumed
TiO2Also more, it reacts with carbonaceous reducing agent less, the TiC of generation is also just few.The present invention is by the dosage control of nitrogen
System can balance the TiO in 50 titanium slags in above range2It is reacted with nitrogen, carbonaceous reducing agent, it is ensured that the Ti (C, N) of generation
The content of TiN is 24~28wt.% in base refractory material, and the content of TiC is 23~27wt.%, and then ensure that Ti (C, N)
The fire resistance of base refractory material.
TiO in roasting process of the present invention, in 50 titanium slags2It reacts with nitrogen and generates TiN and carbonaceous reducing agent
Reaction generates TiC;SiO2It is reacted with carbonaceous reducing agent and generates SiC;CaO and carbonaceous reducing agent react, and generate CaC2;MgO and
Carbonaceous reducing agent reacts, and generates MgC2;FeO and carbonaceous reducing agent react, and generate Fe3C, obtain containing TiN, TiC,
SiC、CaC2、 MgC2And Fe3Ti (C, N) base refractory material of C, efficiently uses each ingredient in 50 titanium slags, while by
Carburizing reagent occurs in 50 titanium slags and carbonaceous reducing agent, generates TiC and CO, CO is reducing atmosphere, can guarantee the Ti generated
(C, N) is not oxidized.
Ti (C, N) the base refractory material being prepared the present invention also provides preparation method described in above-mentioned technical proposal, institute
Stating Ti (C, N) base refractory material includes TiN:24~28wt.%;TiC:23~27wt.%;SiC:15~19wt.%;CaC2:
7~10wt.%;MgC2: 17~21wt.% and Fe3C:1~3%.
In the present invention, Ti (C, N) the base refractory material includes the TiN of 24~28wt.%, preferably 25~
27wt.%.
In the present invention, Ti (C, N) the base refractory material includes the TiC of 23~27wt.%, preferably 24~
26wt.%.
Ti (C, N) base refractory material of the present invention includes the SiC, preferably 16~18wt.% of 15~19wt.%.
Ti (C, N) base refractory material of the present invention includes the CaC of 7~10wt.%2, preferably 8~10wt.%.
Ti (C, N) base refractory material of the present invention includes the MgC of 17~21wt.%2, preferably 17~20wt.%.
Ti (C, N) base refractory material of the present invention includes 1~3% Fe3C, preferably 1~2wt.%.
Ti (C, N) base refractory material each component mating reaction of the present invention has Ti (C, N) base refractory material good
High temperature resistance, refractoriness >=2000 DEG C.
Below with reference to embodiment to Ti provided by the invention (C, N) base refractory material and using 50 titanium slags produce Ti (C,
N) method of base refractory material is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) raw material is broken
50 titanium slags and carbonaceous reducing agent coke are distinguished into crushing grinding, obtaining granularity is 200 mesh powders;
(2) mixing
50 titanium slag powder 1000g (71wt.%) are weighed, carbonaceous reducing agent coke powder 400g (29wt.%) is placed in ball milling
In tank, ball milling revolution is 150r/min, and Ball-milling Time 30min obtains mixture;
(3) pelletizing
Mixed material is used into disc balling machine pelletizing, causing diameter is the pelletizing of 10mm;
(4) Ti (C, N) base refractory material is prepared
Pelletizing is put into Muffle furnace, 1200 DEG C are warming up to by room temperature with 10 DEG C/min rate, when temperature is warming up to 1200
DEG C when, be continually fed into nitrogen and amount to 36L, being passed through rate is 0.6L/min, while continuing to heat up, and is heated up with the rate of 5 DEG C/min
It to 1800 DEG C, is roasted when temperature reaches 1800 DEG C, keeps the temperature 30min, material and carbonaceous reducing agent occur carburizing reagent, generate
TiC and CO, CO are reducing atmosphere, guarantee that the Ti (C, N) generated is not oxidized, then take out crucible and be air-cooled to room temperature, obtain
Ti (C, N) base refractory material.
It is obtained by detecting chemical component: the TiN:27.8wt.% wherein generated;TiC:24.9wt.%;SiC:
18.9wt.%;CaC2: 7.5wt.%;MgC2: 19.1wt.% and Fe3C:1.8wt.%.
Refractoriness test method: obtained Ti (C, N) base refractory material after roasting is put into 2000 DEG C of temperature or more
It is kept the temperature in stove, Ti (C, N) base refractory material does not occur obviously to deform, and illustrates refractoriness >=2000 DEG C of high-temperature refractory.
Embodiment 2
(1) raw material is broken
50 titanium slags and carbonaceous reducing agent coal dust are distinguished into crushing grinding, obtaining granularity is 300 mesh powders;
(2) mixing
50 titanium slag powder 1000g (66wt.%) are weighed, carbonaceous reducing agent coal dust powder 500g (34wt.%) is placed in ball milling
In tank, ball milling revolution is 200r/min, and Ball-milling Time 30min obtains mixture;
(3) pelletizing
Mixed material is used into disc balling machine pelletizing, causing diameter is the pelletizing of 12mm;
(4) Ti (C, N) base refractory material is prepared
Pelletizing is put into Muffle furnace, 1200 DEG C are warming up to by room temperature with 10 DEG C/min rate, when temperature is warming up to 1200
DEG C when, be continually fed into nitrogen and amount to 34L, being passed through rate is 0.6L/min, while continuing to heat up, and is heated up with the rate of 5 DEG C/min
It to 1900 DEG C, is roasted when temperature reaches 1900 DEG C, keeps the temperature 40min, carburizing reagent occurs for material and carbonaceous reducing agent, raw
It is reducing atmosphere at TiC and CO, CO, guarantees that the Ti (C, N) generated is not oxidized, then take out crucible and be air-cooled to room temperature, obtain
To Ti (C, N) base refractory material.
Detection obtains: the TiN:26.9wt.% wherein generated;TiC:25.4wt.%;SiC:16.8wt.%; CaC2:
9.4wt.%;MgC2: 19.4wt.% and Fe3C:2.1wt.%, refractoriness >=2000 DEG C of high-temperature refractory.
Embodiment 3
(1) raw material is broken
50 titanium slags and carbonaceous reducing agent petroleum coke are distinguished into crushing grinding, obtaining granularity is 100 mesh powders;
(2) mixing
50 titanium slag powder 1000g (66wt.%) are weighed, carbonaceous reducing agent coal dust powder 500g (34wt.%) is placed in ball milling
In tank, ball milling revolution is 250r/min, and Ball-milling Time 40min obtains mixture;
(3) pelletizing
Mixed material is used into disc balling machine pelletizing, causing diameter is the pelletizing of 12mm;
(4) Ti (C, N) base refractory material is prepared
Pelletizing is put into Muffle furnace, 1200 DEG C are warming up to by room temperature with 10 DEG C/min rate, when temperature is warming up to 1200
DEG C when, be continually fed into nitrogen and amount to 36L, being passed through rate is 0.6L/min, while continuing to heat up, and is heated up with the rate of 5 DEG C/min
It to 1900 DEG C, is roasted when temperature reaches 1900 DEG C, keeps the temperature 40min, material and carbonaceous reducing agent occur carburizing reagent, generate
TiC and CO, CO are reducing atmosphere, guarantee that the Ti (C, N) generated is not oxidized, then take out crucible and be air-cooled to room temperature, obtain
Ti (C, N) base refractory material.
Detection obtains: the TiN:26.6wt.% wherein generated;TiC:25.7wt.%;SiC:17.1wt.%; CaC2:
9.1wt.%;MgC2: 19.6wt.%;Fe3C:1.9wt.%, refractoriness >=2000 DEG C of high-temperature refractory.
As seen from the above embodiment, it is produced the present invention provides a kind of Ti (C, N) base refractory material and using 50 titanium slags
The method of Ti (C, N) base refractory material, the present invention prepare Ti (C, N) base fire proofed wood using 50 titanium slags and carbonaceous reducing agent as raw material
Expect, Ti, Mg, Si, Ca element in 50 titanium slags are finally with TiN, TiC, SiC, CaC2, MgC2Form be present in refractory material
In, so that the ingredient in 50 titanium slags is utilized effectively, and preparation process equipment of the invention is simple, raw material is cheap and easy to get, raw
Solid solution at low cost, Ti (C, N) base refractory material obtained is mainly formed by titanium carbide and titanium nitride is produced, there is Gao Rong
Point, corrosion-resistant, high temperature resistance is preferable, refractoriness >=2000 DEG C.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of method for producing Ti (C, N) base refractory material using 50 titanium slags, comprising the following steps:
50 titanium slag powder and carbonaceous reducing agent powder are mixed, mixture is obtained;
The mixture is subjected to pelletizing, obtains pelletizing;
Under a nitrogen atmosphere, the pelletizing is roasted, nitridation and carburizing reagent occurs, obtains Ti (C, N) base refractory material.
2. the method according to claim 1, wherein the partial size of the 50 titanium slag powder and carbonaceous reducing agent powder
It independently is 100~325 mesh.
3. the method according to claim 1, wherein the quality of the 50 titanium slag powder and carbonaceous reducing agent powder
Than for 1:(0.4~0.7).
4. described in any item methods according to claim 1~3, which is characterized in that the chemical composition of the 50 titanium slag powder is
TiO2: 45~55wt.%;SiO2: 10~15wt.%;CaO:3~9wt.%;MgO:10~15wt.%;Al2O3: 14~
16wt.% and FeO:1~3wt.%.
5. the method according to claim 1, wherein the carbonaceous reducing agent powder be coke, semi-coke, coal dust and
One or more of petroleum coke.
6. the time is the method according to claim 1, wherein the temperature of the roasting is 1500~1900 DEG C
20~60min.
7. the method according to claim 1, wherein the diameter of the pelletizing is 8~15mm.
8. the method according to claim 1, wherein the amount ratio of the nitrogen and 50 titanium slag powder be 32~
36L:1kg。
9. Ti (C, N) base refractory material that any one of claim 1~8 the method is prepared, which is characterized in that the Ti
(C, N) base refractory material includes TiN:24~28wt.%;TiC:23~27wt.%;SiC:15~19wt.%;CaC2: 7~
10wt.%;MgC2: 17~21wt.% and Fe3C:1~3wt.%.
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CN106498108A (en) * | 2016-09-30 | 2017-03-15 | 江西理工大学 | DRI and nitrogen are produced with titanomagnetite concentrate(Carbon)The method for changing titanium |
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---|---|---|---|---|
CN106498108A (en) * | 2016-09-30 | 2017-03-15 | 江西理工大学 | DRI and nitrogen are produced with titanomagnetite concentrate(Carbon)The method for changing titanium |
CN108929951A (en) * | 2018-08-07 | 2018-12-04 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of utilization method of v-ti magnetite concentrate |
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Title |
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Application publication date: 20190712 |