CN107805720A - A kind of method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag carries titanium - Google Patents
A kind of method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag carries titanium Download PDFInfo
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- CN107805720A CN107805720A CN201711241777.7A CN201711241777A CN107805720A CN 107805720 A CN107805720 A CN 107805720A CN 201711241777 A CN201711241777 A CN 201711241777A CN 107805720 A CN107805720 A CN 107805720A
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- titanium
- blast furnace
- furnace slag
- containing blast
- vacuum decompression
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Classifications
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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
-
- 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
- C22B1/2406—Binding; Briquetting ; Granulating pelletizing
-
- 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
- C22B34/1218—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 obtaining titanium or titanium compounds from ores or scrap by dry processes
-
- 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
- C22B7/001—Dry processes
-
- 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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag carries titanium, belongs to titanium-containing blast furnace slag comprehensive utilization and titanium extraction field of smelting.A kind of method that the technical problems to be solved by the invention are to provide high efficiency, low energy consumption, the titanium-containing blast furnace slag of low cost carry titanium.Solid titaniferous blast furnace slag, coke powder and coal dust are well mixed, pelletizing, dry to obtain material a；Liquid titanium-containing blast furnace slag, coke powder and coal dust are well mixed, obtain material b；Material a, material b are put into vacuum reduction reaction unit, carry out vacuum decompression carbonizing reduction metallurgical reaction；Reaction product is cooled down, crushed, ball milling, magnetic separation, obtain be carbonized ilmenite concentrate product.The inventive method carries out carrying titanium using the reaction of vacuum decompression carbonizing reduction to titanium-containing blast furnace slag, reduction temperature is significantly reduced, so as to greatly reduce energy resource consumption, achievable economy carries titanium, titanium recovery rate considerably reduces the waste of titanium-containing blast furnace slag titanium resource up to 55~85%.
Description
Technical field
The invention belongs to titanium-containing blast furnace slag comprehensive utilization and titanium extraction field of smelting, and in particular to a kind of vacuum decompression carbonization
The method that reduction titanium-containing blast furnace slag carries titanium.
Background technology
Removed in high-titanium blast furnace slag rich in substantial amounts of calcium oxide, magnesia, silica, aluminum oxide, iron oxide, metal
It is valuable strategic resource and secondary resource also rich in substantial amounts of titanium dioxide resource outside the resources such as iron, physical sensible heat.Climb branch
Flower titanium resource accounts for the 90% of national titanium resource, and the titanium resource in Panzhihua high-titanium blast furnace slag accounts for the 50% of titanium resource in Panzhihua
Left and right.Therefore, it is necessary to Panzhihua high-titanium blast furnace slag is comprehensively utilized as much as possible.Panzhihua high-titanium blast furnace slag primary chemical into
Divide and be shown in Table 1.
The Panzhihua high-titanium blast furnace slag composition of table 1
At this stage, have 50% or so high-titanium blast furnace slag factory as construction ceramic, floor tile, cement admixture, manufacture cast stone, ore deposit
Cotton, insulation material, light wall plate for building, the sand of mixed mud, rubble, paveio(u)r etc.；But it is not substantially high using high titanium
Titanium resource in clinker.In addition, petroleum fracturing propping agent is also served as, but its dosage is very limited.Remainder high-titanium blast furnace slag,
For its build specialty slag field carry out stacking storage, or be arbitrarily to abandon, be discharged into Jinsha jiang River, cause land wastage,
Environmental pollution, cause a large amount of losses of the strategic resource titanium of preciousness to waste, regeneration can not be enriched with later.
At present, the method for titanium resource has hydrometallurgy and the major class of pyrometallurgy two in research and utilization titanium-containing blast furnace slag.Wet method
Metallurgical process is to leach to carry titanium using acid, alkali, but the rate of recovery of this method titanium is low, and cost is high, and caused waste liquid can not be handled, ring
Border pollution is big；Pyrogenic process carries titanium and high temperature cabonization titaniferous blast furnace is mainly carried out under 1600~1800 DEG C, condition of normal pressure using mineral hot furnace
Slag, the progress magnetic separation extraction titanium carbide to be cooled such as then, but its energy consumption is very big, operational hazards.Therefore, either firing method process,
Or wet process fails to realize the titanium resource in economic, commercialized extraction titanium-containing blast furnace slag.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of high efficiency, low energy consumption, the titanium-containing blast furnace slag of low cost carry
The method of titanium.
The present invention solves the technical scheme that above-mentioned technical problem uses and there is provided a kind of vacuum decompression carbonizing reduction titaniferous
The method that blast furnace slag carries titanium, this method comprise the following steps：
A, when titanium-containing blast furnace slag is solid-state, solid titaniferous blast furnace slag, coke powder and coal dust are well mixed, through pelletizing, dried
It is dry, obtain material a；When titanium-containing blast furnace slag is liquid, liquid titanium-containing blast furnace slag, coke powder and coal dust are well mixed, obtain material b；
B, at least one of step A resulting materials a or material b are put into vacuum reduction reaction unit, carry out vacuum
Depressurize carbonizing reduction metallurgical reaction；
C, reaction finishes, and after reaction product is cooled into room temperature, through broken, ball milling, magnetic separation, obtains the ilmenite concentrate production that is carbonized
Thing.
Wherein, in the above method, in step A, the mass ratio of the titanium-containing blast furnace slag, coke powder and coal dust is 1：0.1~
0.2：0.25~0.45；The titanium-containing blast furnace slag is solid-state or liquid.
Wherein, in the above method, in step A, granularity≤0.5mm of the solid titaniferous blast furnace slag.
Wherein, in the above method, in step A, granularity≤0.5mm of the coke powder.
Wherein, in the above method, in step A, granularity≤0.5mm of the coal dust.
Wherein, in the above method, in step A, when titanium-containing blast furnace slag is solid-state, the well mixed mixing degree >=
98.5%.
Wherein, in the above method, in step B, the reaction temperature of the vacuum decompression carbonizing reduction metallurgical reaction is 1300
~1400 DEG C；The vacuum of the vacuum decompression carbonizing reduction metallurgical reaction is 1~100Pa.
Wherein, in the above method, in step B, reaction time of the vacuum decompression carbonizing reduction metallurgical reaction for 0.5~
2h。
Wherein, in the above method, in step C, the broken ball milling is milled to granularity≤0.1mm to be broken.
Wherein, in the above method, in step C, the magnetic field intensity of the magnetic separation is 0.5~1.5T.
Wherein, it is described to be cooled to completely cut off air slow cooling or water quenching chilling in step C in the above method.
Beneficial effects of the present invention：
The inventive method carries out carrying titanium using the reaction of vacuum decompression carbonizing reduction to titanium-containing blast furnace slag, is reduced compared with prior art
300~400 DEG C of reduction reaction temperature, significantly reduces reduction temperature, and so as to greatly reduce energy resource consumption, achievable economy carries
Titanium；Under vacuum decompression and high temperature reduction precondition, by the TiO in blast furnace slag2And CaTiO3Being reduced into Deng titaniferous materials has
The TiC and Ti (C, N) of magnetic, so as to using high intensity magnetic separation method will have magnetic TiC, Ti (C, N) with it is other non-magnetic
Material efficiently separates；The inventive method need not introduce other relative titaniferous materials for being easier to carry out carburizing reagent, titanium recovery rate
I.e. up to 55~85%, cost is not reduced closely, also considerably reduces the waste of titanium-containing blast furnace slag titanium resource, the tail through magnetic separation
Ore deposit can still be used as construction material etc. to be used, and improve the value of titanium-containing blast furnace slag；The reducing agent of the inventive method
Raw material coke powder, coal dust are cheap and easy to get, simple to operate, safety, it is easy to accomplish industrialization, reduce further and put forward titanium cost；This hair
The grade height of bright method preparation carbonization ilmenite concentrate product, cost are low, thus can be widely used for such as Chemical Leaching, chlorination processing and obtain
To higher purity titanium products TiC or titanium other products TiCl4, and titanium intermediate products etc..
Brief description of the drawings
Fig. 1 is vacuum reduction reaction unit schematic diagram used by the embodiment of the present invention 1；
Fig. 2 is vacuum reduction reaction unit schematic diagram used by the embodiment of the present invention 2；
Wherein, 1 is charge pipe, and 2 be heating electrode, and 3 be reactor, and 4 is can open confined space, and 5 be base, and 6 be liquid
State blast furnace slag dress fills.
Embodiment
Specifically, a kind of method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag carries titanium, this method comprise the following steps：
A, when titanium-containing blast furnace slag is solid-state, solid titaniferous blast furnace slag, coke powder and coal dust are well mixed, through pelletizing, dried
It is dry, obtain material a；When titanium-containing blast furnace slag is liquid, liquid titanium-containing blast furnace slag, coke powder and coal dust are well mixed, obtain material b；
B, at least one of step A resulting materials a or material b are put into vacuum reduction reaction unit, carry out vacuum
Depressurize carbonizing reduction metallurgical reaction；
C, reaction finishes, and after reaction product is cooled into room temperature, through broken, ball milling, magnetic separation, obtains the ilmenite concentrate production that is carbonized
Thing.
Titanium-containing blast furnace slag is the slag that v-ti magnetite concentrate obtains after blast furnace process separation is tapped a blast furnace, and it is liquid to be come out from blast furnace
Slag, but be just solid-state after supercooling.Therefore, the blast furnace slag of history accumulation is solid-state normal-temperature titanium-containing blast furnace slag, is now then needed
Solid titaniferous blast furnace slag, coke powder and coal dust are well mixed, through pelletizing, drying, obtain pelletizing material (i.e. material a)；Brand new is
Liquid high temperature sludge, liquid blast furnace are not required to pelletizing, only need to uniformly be mixed it with reducing agent coke powder, coal dust, save energy consumption,
It can specifically use penetrating or mechanical agitation to add and be well mixed, obtain material b.
In the inventive method, no matter titanium-containing blast furnace slag is solid-state or liquid, the titanium-containing blast furnace slag, coke powder and coal dust
Mass ratio is 1：0.1~0.2：0.25~0.45.
In order to increase titanium-containing blast furnace slag and reducing agent (coke powder, coal dust) contact area, reduction reaction efficiency is improved, works as titaniferous
When blast furnace slag is solid-state, granularity≤0.5mm of titanium-containing blast furnace slag；No matter titanium-containing blast furnace slag is solid-state or liquid, used Jiao
Granularity≤0.5mm of powder, granularity≤0.5mm of coal dust.
When titanium-containing blast furnace slag is solid-state, well mixed mixing degree >=98.5% in the inventive method rate-determining steps A, from
And reduction reaction is set fully to carry out.
When reducing metallurgical, pressure is lower, and temperature is lower needed for reaction；Pressure is higher, and required reaction temperature is corresponding higher,
Inventor is according to reaction equation C+TiO2=CO+TiC, with reference to actual experiment effect, from energy-conservation and reaction efficiency, present invention side
It is 1300~1400 DEG C that method, which controls the reaction temperature of vacuum decompression carbonizing reduction metallurgical reaction, and vacuum is 1~100Pa, now
Reaction time is 0.5~2h.
Reaction product, using nature Slow cooling, also can rapidly be cooled down in the case where completely cutting off air using water quenching；For
It is easily operated, while improve follow-up efficiency of magnetic separation, granularity≤0.1mm can be milled to by the reaction product after cooling is broken.
In the inventive method step C, obtained carbonization ilmenite concentrate product is the mixture of titanium carbide and titanium carbonitride.True
Under sky decompression and high temperature reduction precondition, by the TiO in blast furnace slag2And CaTiO3Deng titaniferous materials be reduced into tool it is magnetic
TiC and Ti (C, N), have so as to have magnetic TiC, Ti (C, N) and other non-magnetic materials using the method for high intensity magnetic separation
Effect separation；The magnetic field intensity of the magnetic separation is 0.5~1.5T；It is described to be cooled to completely cut off air slow cooling or water quenching chilling.
The present invention is described in further detail below by embodiment, but therefore not limited the scope of the present invention
Among described scope of embodiments.
Embodiment 1
The method that the present embodiment titanium-containing blast furnace slag carries titanium comprises the following steps：
A, it is 0.5mm solid titaniferous blast furnace slag, coke powder and coal dust to be crushed into granularity respectively；By solid titaniferous blast furnace slag
50g, coke powder 7.5g and coal dust 17.5g are well mixed to mixing degree >=98.5%, through pelletizing, drying, obtain pelletizing feed；By pelletizing feed
It is put into vacuum reduction reaction unit (Fig. 1), under the conditions of temperature is 1350 DEG C, vacuum is 50Pa, carries out vacuum decompression carbon
Change reduction metallurgical reaction 2h；
B, reaction is finished, and after reaction product isolation air is cooled into room temperature, the reaction product after cooling is crushed
Granularity≤0.1mm is milled to, is put into the intensity magnetic separator that magnetic field intensity is 0.8T and carries out magnetic separation, obtain the ilmenite concentrate product that is carbonized,
Its Ti (C, N) content is 34.32/%, titanium recovery rate 65.3%.
Embodiment 2
The method that the present embodiment titanium-containing blast furnace slag carries titanium comprises the following steps：
A, it is 0.5mm coke powder and coal dust to be crushed into granularity respectively；By liquid titanium-containing blast furnace slag 50g, coke powder 7.5g and coal
Powder 17.5g is well mixed, and is put into vacuum reduction reaction unit (Fig. 1), temperature be 1350 DEG C, vacuum be 50Pa conditions
Under, carry out vacuum decompression carbonizing reduction metallurgical reaction 2h；
B, reaction is finished, and after reaction product isolation air is cooled into room temperature, the reaction product after cooling is crushed
Granularity≤0.1mm is milled to, is put into the intensity magnetic separator that magnetic field intensity is 1T and carries out magnetic separation, obtain the ilmenite concentrate product that is carbonized, its
Ti (C, N) content is 38.36/%, titanium recovery rate 70.7%.
Claims (9)
1. the method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag carries titanium, it is characterised in that：Comprise the following steps：
A, when titanium-containing blast furnace slag is solid-state, solid titaniferous blast furnace slag, coke powder and coal dust are well mixed, through pelletizing, drying, obtained
Material a；When titanium-containing blast furnace slag is liquid, liquid titanium-containing blast furnace slag, coke powder and coal dust are well mixed, obtain material b；
B, at least one of step A resulting materials a or material b are put into vacuum reduction reaction unit, carry out vacuum decompression
Carbonizing reduction metallurgical reaction；
C, reaction finishes, and after reaction product is cooled into room temperature, through broken, ball milling, magnetic separation, obtains the ilmenite concentrate product that is carbonized.
2. the method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag according to claim 1 carries titanium, it is characterised in that：Step
In A, the mass ratio of the titanium-containing blast furnace slag, coke powder and coal dust is 1：0.1~0.2：0.25~0.45；The titanium-containing blast furnace slag is
Solid-state or liquid.
3. the method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag according to claim 1 carries titanium, it is characterised in that：Step
In A, granularity≤0.5mm of the solid titaniferous blast furnace slag；Granularity≤0.5mm of the coke powder；The granularity of the coal dust≤
0.5mm。
4. the method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag according to claim 1 carries titanium, it is characterised in that：Step
In A, when titanium-containing blast furnace slag is solid-state, well mixed mixing degree >=98.5%.
5. the method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag according to claim 1 carries titanium, it is characterised in that：Step
In B, the reaction temperature of the vacuum decompression carbonizing reduction metallurgical reaction is 1300~1400 DEG C；The vacuum decompression carbonizing reduction
The vacuum of metallurgical reaction is 1~100Pa.
6. the method that the vacuum decompression carbonizing reduction titanium-containing blast furnace slag according to any one of Claims 1 to 5 carries titanium, its feature
It is：In step B, the reaction time of the vacuum decompression carbonizing reduction metallurgical reaction is 0.5~2h.
7. the method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag according to claim 1 carries titanium, it is characterised in that：Step
In C, the broken ball milling is milled to granularity≤0.1mm to be broken.
8. the method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag according to claim 1 carries titanium, it is characterised in that：Step
In C, the magnetic field intensity of the magnetic separation is 0.5~1.5T.
9. the method that the vacuum decompression carbonizing reduction titanium-containing blast furnace slag according to any one of claim 1~8 carries titanium, its feature
It is：It is described to be cooled to completely cut off air slow cooling or water quenching chilling in step C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711241777.7A CN107805720A (en) | 2017-11-30 | 2017-11-30 | A kind of method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag carries titanium |
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| CN201711241777.7A CN107805720A (en) | 2017-11-30 | 2017-11-30 | A kind of method that vacuum decompression carbonizing reduction titanium-containing blast furnace slag carries titanium |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943151A (en) * | 2020-08-18 | 2020-11-17 | 重庆大学 | Method for improving carbonitriding efficiency of titanium-containing blast furnace slag and preparing titanium carbonitride |
| CN113233500A (en) * | 2021-06-25 | 2021-08-10 | 中国恩菲工程技术有限公司 | Method and system for producing titanium tetrachloride by smelting titanium-containing slag |
| CN115010170A (en) * | 2022-07-04 | 2022-09-06 | 重庆大学 | TiCl preparation by utilizing titanium-containing blast furnace slag 4 Method (2) |
| CN116411194A (en) * | 2023-04-17 | 2023-07-11 | 攀枝花学院 | Method for preparing titanium-silicon alloy from titanium-containing blast furnace slag by combining carbonaceous material and biomass material in one step |
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| CN104498734A (en) * | 2015-01-09 | 2015-04-08 | 重庆大学 | Titanium recovery treatment method for titanium-bearing blast furnace slag based on vacuum carbothermal reduction |
| CN106044771A (en) * | 2016-06-01 | 2016-10-26 | 重庆大学 | Titanium carbide preparation method based on carbonization titanium extraction treatment of titanium-bearing blast furnace slag |
| CN106987725A (en) * | 2017-03-27 | 2017-07-28 | 北京科技大学 | A kind of titanium-containing blast furnace slag ferrosilicon process titanium extracting technology method |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104498734A (en) * | 2015-01-09 | 2015-04-08 | 重庆大学 | Titanium recovery treatment method for titanium-bearing blast furnace slag based on vacuum carbothermal reduction |
| CN106044771A (en) * | 2016-06-01 | 2016-10-26 | 重庆大学 | Titanium carbide preparation method based on carbonization titanium extraction treatment of titanium-bearing blast furnace slag |
| CN106987725A (en) * | 2017-03-27 | 2017-07-28 | 北京科技大学 | A kind of titanium-containing blast furnace slag ferrosilicon process titanium extracting technology method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943151A (en) * | 2020-08-18 | 2020-11-17 | 重庆大学 | Method for improving carbonitriding efficiency of titanium-containing blast furnace slag and preparing titanium carbonitride |
| CN111943151B (en) * | 2020-08-18 | 2023-06-13 | 重庆大学 | Method for improving titanium-containing blast furnace slag carbonitride efficiency and preparing titanium carbonitride |
| CN113233500A (en) * | 2021-06-25 | 2021-08-10 | 中国恩菲工程技术有限公司 | Method and system for producing titanium tetrachloride by smelting titanium-containing slag |
| CN115010170A (en) * | 2022-07-04 | 2022-09-06 | 重庆大学 | TiCl preparation by utilizing titanium-containing blast furnace slag 4 Method (2) |
| CN115010170B (en) * | 2022-07-04 | 2023-09-22 | 重庆大学 | TiCl preparation by using titanium-containing blast furnace slag 4 Is a method of (2) |
| CN116411194A (en) * | 2023-04-17 | 2023-07-11 | 攀枝花学院 | Method for preparing titanium-silicon alloy from titanium-containing blast furnace slag by combining carbonaceous material and biomass material in one step |
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Application publication date: 20180316 |