CN109022788A - A method of preparing ferro-titanium - Google Patents
A method of preparing ferro-titanium Download PDFInfo
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- CN109022788A CN109022788A CN201811013331.3A CN201811013331A CN109022788A CN 109022788 A CN109022788 A CN 109022788A CN 201811013331 A CN201811013331 A CN 201811013331A CN 109022788 A CN109022788 A CN 109022788A
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- titanium
- ilmenite
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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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
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C35/00—Master alloys for iron or steel
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Abstract
The present invention relates to a kind of method for preparing ferro-titanium, this method carries out gas-based reduction after pelletizing is made in ilmenite first, then using the ilmenite of gas-based reduction as raw material, produces ferro-titanium using self- propagating mode.The method of the present invention this method can not only reduce the quantity of slag caused by the usage amount of reducing agent metallic aluminium and self-propagating reaction needed for self-propagating reaction, but also improve ferro-titanium titanium grade and reduce oxygen content in alloy.
Description
Technical field
The present invention relates to a kind of methods for preparing ferro-titanium, specifically use self- propagating by raw material of gas-based reduction ilmenite
Technique prepares ferro-titanium, belongs to metallurgical technology field.
Background technique
Ferrotitanium ferroalloy has important application as a kind of important metal material, in industrial aspect.In terms of steel,
Ferro-titanium can be used as deoxidier, degasifier and alloying constituent, the intensity and wear-resisting property for reducing ingotism, improving steel.In addition,
In terms of chemical industry and the energy, it or a kind of important electrode coating and hydrogen storage material.Currently, its main production is remelting
Method and aluminothermic process.
Ilmenite has many advantages, such as rich reserves as a kind of titaniferous materials, cheap, is often used to production high titanium slag
And titanium white.But in ferrotianium separation process, electric arc furnaces, which prepares high titanium slag, can consume big energy, and production of titanium dioxide by sulfuric acid method can produce
Raw a large amount of waste liquids.Ilmenite directly produces ferro-titanium and avoids ferrotianium separation problem, reduces process procedure and reduces life
Produce cost.But shortcoming is that thermit reaction production ferro-titanium can consume a large amount of metallic aluminiums and generate a large amount of waste residues, same with this
When due to Al in alloy2O3It is mingled with and TiO2The factors such as incomplete are restored, so that ferro-titanium oxygen content is higher, reach 5-10%, no
Meet exported product requirement.
Summary of the invention
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of method for preparing ferro-titanium.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include:
A method of preparing ferro-titanium comprising following steps:
S1, it after acid pellet is made in ilmenite, puts it into reduction in 800~1300 DEG C of reducing atmosphere and obtains gas
Base reduced ilmenite, grinds, spare:
S2, gas-based reduction ilmenite metallic aluminium, sodium chlorate, titanium dioxide, calcium oxide and the calcirm-fluoride for obtaining step S1
It is uniformly mixed；
S3, it is lighted a fire using top, it is cooling after fully reacting, slag is separated, ferro-titanium is obtained.
Method as described above, it is preferable that in step sl, the pelletizing that is made includes the following steps: to add to ilmenite
Add its mass fraction be 1~3% bentonite, 2~4h of mixing, be gradually added into later water carry out mixing, then shelving 30~
40min, pelletizing obtain 5~8mm pelletizing；After pelletizing drying, it is put into blowing air in Muffle furnace and is pre-oxidized.
Method as described above, it is preferable that the amount that water is added is the 5~7% of ilmenite weight, and water is added and is mixed
The time of material is 30-60min.
Method as described above, it is preferable that Pre oxidation is 800~1200 DEG C in the Muffle furnace, preoxidation time
For 1~3h.
Method as described above, it is preferable that in step sl, the reducing atmosphere is CO, H2、CH4In at least one
Kind or CO, H2、CH4At least one of gaseous mixture with inert gas.
That is reducing atmosphere can be CO, H2、CH4In any one or any two or three of any ratio
The mixed gas of example, or can be CO, H2、CH4In any one or any two kinds of mixtures with inert gas, indifferent gas
Body is N2, Ar etc..
Preparation method as described above, it is preferable that in step sl, the time of the reduction is 1~5h, after grinding
Cross 200 meshes.
Method as described above, it is preferable that in step s 2, the gas-based reduction ilmenite and metallic aluminium, sodium chlorate, two
The proportion of titanium oxide, calcium oxide and calcirm-fluoride be in mass ratio 100:127~146:37~78:164~190:18~36:6~
22 carry out ingredient.
Method as described above, it is preferable that in step s 2, account for 90% or more under 100 mesh of metallic aluminium, the chlorine
95% or more is accounted under 200 mesh of sour sodium and titanium dioxide.
Method as described above, it is preferable that in step s 2, the titanium dioxide can be replaced with rutile or high titanium slag,
The sodium chlorate can be replaced with potassium chlorate.
(3) beneficial effect
The beneficial effects of the present invention are:
The present invention provides one kind using gas-based reduction ilmenite as raw material, and the side of ferro-titanium is produced using self- propagating mode
Method.This method can not only reduce slag caused by the usage amount of reducing agent metallic aluminium and self-propagating reaction needed for self-propagating reaction
Amount, but also ferro-titanium titanium grade can be improved and reduce oxygen content in alloy.
Detailed description of the invention
Fig. 1 is the object phasor of the gas-based reduction ilmenite prepared in embodiment 1.
Specific embodiment
Using pellet is first prepared in the present invention, reduction treatment is carried out later, adds metallic aluminium, sodium chlorate, titanium dioxide
It is smelted after titanium, calcium oxide and calcirm-fluoride mixing and obtains ferro-titanium.Main reaction are as follows: 3Fe+NaClO3+6Al+3TiO2=
3Al2O3+ 3FeTi+NaCl, 6Fe+NaClO3+6Al+3TiO2=3Al2O3+3Fe2Ti+NaCl, 4Al+3TiO2=3Ti+
2Al2O3, wherein metallic aluminium is reducing agent, and sodium chlorate exothermic mixture, titanium dioxide is then the titanium grade in order to improve ferro-titanium.
And calcium oxide and calcirm-fluoride are then to promote the reduction rate of titanium and improve the mobility of slag respectively.
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
Embodiment 1
A method of preparing ferro-titanium comprising following steps:
1, prepared by gas-based reduction ilmenite:
The bentonite that its mass fraction is 2% is added to ilmenite, mixing 3h is gradually added into accounts for raw material ilmenite weight later
5% water mixing 4h of amount, then shelving 30min, pelletizing obtain 5-8mm pelletizing.After pelletizing is dried, it is put into 1000 DEG C
Blowing air pre-oxidizes 2h in Muffle furnace.Later, 800 DEG C, 30%N are put it into2CO reducing atmosphere in reductase 12 h.It is gone back
Former ilmenite is milled to through 200 meshes, spare.Its reduced ilmenite object phasor, as shown in Figure 1, illustrating ilmenite acid pellet
It can be reduced under this reducing condition, and there are a large amount of metallic irons to generate.
2, ferro-titanium raw material is prepared:
It is according to mass ratio by gas-based reduction ilmenite, metallic aluminium, sodium chlorate, titanium dioxide, calcium oxide and calcirm-fluoride
100:134.4:51.7:174.5:26.9:13.5 carrying out ingredient, wherein account for 90% or more under 100 mesh of metallic aluminium, sodium chlorate and
95% or more is accounted under 200 mesh of titanium dioxide.
3, prepared by ferro-titanium:
Raw material is uniformly mixed, is lighted a fire using top, it is cooling after fully reacting, slag is separated, ferro-titanium is obtained, wherein
Ti content is 48.2%, iron content 25.6%, aluminium content 8.47%, oxygen content 1.97%.
Embodiment 2
The present embodiment is real, and difference is on the basis of embodiment 1, adds 1% bentonite, mixing 4h, and addition water is
6% mixing 3h, the shelving 35min of ilmenite weight obtain 5-8mm pelletizing, and 800 DEG C of pre-oxidation 2 in Muffle furnace is put into after drying
Hour ilmenite pelletizing restore 5 hours in 1100 DEG C, the atmosphere of 100%CO, acquisition reduced ilmenite is milled to by 200
Mesh, it is spare.
By gas-based reduction ilmenite, metallic aluminium, potassium chlorate, titanium dioxide, calcium oxide and calcirm-fluoride according to mass ratio 100:
138.5:74:189:34.6:11.1 carrying out ingredient, 90% or more is wherein accounted under 100 mesh of metallic aluminium, potassium chlorate and titanium dioxide
95% or more is accounted under 200 meshes.
Raw material is uniformly mixed, is lighted a fire using top, it is cooling after fully reacting, slag is separated, ferro-titanium is obtained, wherein
Ti content is 49.6%, iron content 26.0%, aluminium content 8.12%, oxygen content 3.10%.
Embodiment 3
The present embodiment is real, and difference is on the basis of embodiment 1, adds 3% bentonite, and addition water is 7%, shelving
40min obtains 5-8mm pelletizing, be put into after drying in Muffle furnace the ilmenite pelletizing of 1200 DEG C of pre-oxidation 1 hour 1200 DEG C,
100%H2Atmosphere in restore 3 hours, obtain reduced ilmenite, be milled to through 200 meshes, it is spare.
By gas-based reduction ilmenite, metallic aluminium, sodium chlorate, titanium dioxide, calcium oxide and calcirm-fluoride according to mass ratio 100:
136:58:187:20.8:13.9 carrying out ingredient, 90% or more is wherein accounted under 100 mesh of metallic aluminium, sodium chlorate and titanium dioxide
95% or more is accounted under 200 sieves.
Raw material is uniformly mixed, is lighted a fire using top, it is cooling after fully reacting, slag is separated, ferro-titanium is obtained, wherein
Ti content is 50.8%, iron content 25.3%, aluminium content 8.23%, oxygen content 3.27%.
Embodiment 4
The present embodiment is real, and difference is on the basis of embodiment 1, adds 2.5% bentonite, addition water is 6%, bored
Expect 35min, obtain 5-8mm pelletizing, is put into after drying in Muffle furnace and pre-oxidizes 3 hours ilmenite pelletizings 1100 for 900 DEG C
DEG C, 70%CH4It is restored 3 hours in the atmosphere of 30%Ar, obtains reduced ilmenite, be milled to through 200 meshes, it is spare.
By gas-based reduction ilmenite, metallic aluminium, potassium chlorate, titanium dioxide, calcium oxide and calcirm-fluoride according to mass ratio 100:
137:65:184:27.7:11.1 carrying out ingredient, 90% or more is wherein accounted under 100 mesh of metallic aluminium, potassium chlorate and titanium dioxide
95% or more is accounted under 200 sieves.
Raw material is uniformly mixed, is lighted a fire using top, it is cooling after fully reacting, slag is separated, ferro-titanium is obtained, wherein
Ti content is 49.3%, iron content 26.1%, aluminium content 7.83%, oxygen content 4.11%.
By calculating it is found that preparing ferro-titanium as raw material using gas-based reduction ilmenite of the invention, can save about
16% metallic aluminium and the ferro-titanium slag of reduction about 14%.If to prepare ferro-titanium raw material carry out certain preheating or
Certain reaction heat is provided by electric energy, then effect is more significant.
Comparative example 1
By ilmenite powder in 600 DEG C of roasting 2h, moisture removal and organic matter are removed.
By ilmenite powder, metallic aluminium, sodium chlorate, titanium dioxide, calcium oxide and calcirm-fluoride according to mass ratio be 100:133:
49:171:27:13 carries out ingredient.
Ferro-titanium is finally obtained, wherein Ti content is 47.7%, iron content 25.1%, aluminium content 6.83%, oxygen
Content 6.17%.
Comparative example 2
By ilmenite powder in 1000 DEG C of roasting 2h, moisture removal and organic matter are removed.
By ilmenite powder, metallic aluminium, sodium chlorate, titanium dioxide, calcium oxide and calcirm-fluoride according to mass ratio be 100:130:
43:65:33:10 carries out ingredient.
Ferro-titanium is finally obtained, wherein Ti content is 47.0%, iron content 23.8%, aluminium content 6.92%, oxygen
Content 6.39%.
It can be seen that from above, after the present invention is using gas-based reduction pretreatment, not doing pretreated method than comparative example can be effective
Ferro-titanium titanium grade is improved, and oxygen content substantially reduces, the waste residue amount of generation is greatly reduced.
The above described is only a preferred embodiment of the present invention, being not the limitation for doing other forms to the present invention, appoint
What those skilled in the art can use the equivalence enforcement that technology contents disclosed above were changed or be modified as equivalent variations
Example.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to the above embodiments
What simple modification, equivalent variations and remodeling, still falls within the protection scope of technical solution of the present invention.
Claims (9)
1. a kind of method for preparing ferro-titanium, which is characterized in that it includes the following steps:
S1, it after pelletizing is made in ilmenite, puts it into reduction in 800~1300 DEG C of reducing atmosphere and obtains gas-based reduction titanium
Iron ore is ground, spare:
S2, gas-based reduction ilmenite and metallic aluminium, sodium chlorate, titanium dioxide, calcium oxide and calcirm-fluoride that step S1 is obtained are mixed
It closes uniform；
S3, it is lighted a fire using top, it is cooling after fully reacting, slag is separated, ferro-titanium is obtained.
2. the method as described in claim 1, which is characterized in that in step sl, it is described be made pelletizing include the following steps: to
Ilmenite adds the bentonite that its mass fraction is 1~3%, and 2~4h of mixing is gradually added into water later and carries out mixing, then bored
Expect 30~40min, pelletizing obtains 5~8mm pelletizing；After pelletizing drying, it is put into blowing air in Muffle furnace and carries out pre- oxygen
Change.
3. method according to claim 2, which is characterized in that the amount that water is added is the 5~7% of ilmenite weight, is added
Enter water and carries out the time of mixing as 30-60min.
4. method according to claim 2, which is characterized in that Pre oxidation is 800~1200 DEG C in the Muffle furnace, in advance
Oxidization time is 1~3h.
5. the method as described in claim 1, which is characterized in that in step sl, the reducing atmosphere is CO, H2、CH4In
At least one, or be CO, H2、CH4At least one of gaseous mixture with inert gas.
6. the method as described in claim 1, which is characterized in that in step sl, the time of the reduction is 1~5h, grinding
Smash it through 200 meshes.
7. the method as described in claim 1, which is characterized in that in step s 2, the gas-based reduction ilmenite and metallic aluminium,
Sodium chlorate, titanium dioxide, calcium oxide and calcirm-fluoride proportion in mass ratio for 100:127~146:37~78:164~190:18~
36:6~22 carries out ingredient.
8. the method as described in claim 1, which is characterized in that in step s 2, accounted under 100 mesh of metallic aluminium 90% with
On, 95% or more is accounted under 200 mesh of the sodium chlorate and titanium dioxide.
9. the method as described in claim 1, which is characterized in that in step s 2, the titanium dioxide rutile or high titanium
Slag replacement, the sodium chlorate are replaced with potassium chlorate.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131128A (en) * | 2014-07-21 | 2014-11-05 | 东北大学 | Aluminum thermal self-propagating-injection depth reduction based method for preparing ferro-titanium |
| CN106834891A (en) * | 2017-02-14 | 2017-06-13 | 东北大学 | A kind of preparation method of ferro-titanium |
| CN106834880A (en) * | 2017-02-14 | 2017-06-13 | 东北大学 | A kind of preparation method of ferro-titanium |
| CN107099696A (en) * | 2017-06-13 | 2017-08-29 | 东北大学 | The method for preparing ferro-titanium with wash heat refining is reduced based on aluminothermy self- propagating gradient |
-
2018
- 2018-08-31 CN CN201811013331.3A patent/CN109022788B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131128A (en) * | 2014-07-21 | 2014-11-05 | 东北大学 | Aluminum thermal self-propagating-injection depth reduction based method for preparing ferro-titanium |
| CN106834891A (en) * | 2017-02-14 | 2017-06-13 | 东北大学 | A kind of preparation method of ferro-titanium |
| CN106834880A (en) * | 2017-02-14 | 2017-06-13 | 东北大学 | A kind of preparation method of ferro-titanium |
| CN107099696A (en) * | 2017-06-13 | 2017-08-29 | 东北大学 | The method for preparing ferro-titanium with wash heat refining is reduced based on aluminothermy self- propagating gradient |
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