CN1036228A - Preparation method of reduced ilmenite powder and uses thereof - Google Patents
Preparation method of reduced ilmenite powder and uses thereof Download PDFInfo
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- CN1036228A CN1036228A CN 88103956 CN88103956A CN1036228A CN 1036228 A CN1036228 A CN 1036228A CN 88103956 CN88103956 CN 88103956 CN 88103956 A CN88103956 A CN 88103956A CN 1036228 A CN1036228 A CN 1036228A
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- ilmenite
- reduction
- reductive agent
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Abstract
The invention discloses preparation method of a kind of reduced ilmenite powder and uses thereof, belong to ilmenite concentrate and produce the alloying technology field with the reduction of solid carbon reductive agent dry method.Employing is carried out two steps of two-stage reductive with the solid carbon reductive agent after with the roasting of ilmenite concentrate raw material initial oxidation again.Ca in the raw material, Mg, the content height of impurity elements such as Al, the oxide compound of these impurity elements has no adverse effects to its end product, can fully utilize iron, titanium resource, and the product of reduzate is used to make chemical coating of welding electrode coating.
Description
The invention belongs to ilmenite concentrate and produce the alloying technology field with the reduction of solid carbonaceous reducing agent dry method.
The multiple ilmenite concentrate treatment process that is adopted in the world at present is the back to be handled in the ilmenite concentrate reduction adopt forms such as magnetic separation separation, leaching, and iron, titanium are separated, and obtains products such as rich titanium material, iron powder, ferro-titanium, TiO 2 pigment.
United States Patent (USP) No. 3875286, No. 4019898 and No. 1431480 proposes ilmenite reduction is handled, and makes the iron in the mineral become metallic iron or iron protoxide, taps a blast furnace with rare mineral acid dipping dissolving, titanium, iron is separated, to obtain high-grade rich titanium material.
No. 3765868, United States Patent (USP) proposes to handle ilmenite with electric furnace smelting process, to obtain iron and titanium slag.
No. 4288417, United States Patent (USP) proposes to allow ilmenite powder and diluted acid react, and makes the oxyhydroxide of titanium after the hydrolysis, obtains TiO 2 pigment after roasting.
No. 3966455, United States Patent (USP), proposition directly utilizes the particulate state ilmenite powder and does not remove oxide compound in advance, produces the high-grade ferro-titanium.
English Patent No. 754453, No. 791366, proposition use the reduction magnetic method to handle ilmenite, with ilmenite levigate magnetic separation separation behind the direct solid state reduction in electric furnace, rotary kiln, obtain TiO
2Higher rich titanium material and iron content 93%, TiO
25% metal iron powder is used Electric furnace steel making behind the sintering.
No. 3850615, United States Patent (USP) proposes use the fluid bed reduction titaniferous ore, and the ferriferous oxide that reduces in the mineral with thicker relatively solid carbon reductive agent is a metallic state, and thin relatively reductive agent is suspended in the fluidized-bed and provides heat energy for reaction.In this technological process, titaniferous ore will mix with reductive agent in reactor 950 ℃ of following preheatings, again by reformed gas (as CO+H
2) deliver to and carry out reduction reaction in the fluidized-bed reactor, and then deliver to and isolate the reduction mineral in the cyclone separator.Therefore, this complex technical process, operation is various.In addition, this technology also requires:
(1) titaniferous ore is had granularity requirements, the main particle size range of used titaniferous ore 20～60% is greatly about 80～100 orders, and above-mentioned ore will be preheating to 900～1100 ℃, and institute's iron content occurs with ferrous form;
(2) solid carbon reductive agent size-grade distribution is had requirement, basic size composition is 20～150 orders, and 40～80% of reductive agent weight percentage must be through preheating.Above-mentioned reductive agent grain graininess is that 20～40 purposes account for 25% at least, and about 80～150 purpose fine particles are no less than 25%.
Above-mentioned various technology generally can not be utilized the iron resources in the mineral.Although the reduction magnetic method can fully utilize titanium, iron resources, for containing the high mineral of Mg, reduce easy ring formation, sticking kiln with rotary kiln, make process be difficult to carry out.And above-mentioned polytechnic end product such as titanium alloy, iron powder, titanium white etc., all do not allow more impurity element and exist.Therefore, contain S with above-mentioned the whole bag of tricks processing, Ca, Mg, Al is high and also contains some other impurity elements, and compact structure, FeO/Fe
2O
3The granular ilmenite that ratio is big, for example the Flos Bombacis Malabarici ilmenite concentrate is very inappropriate.
The objective of the invention is, according to containing S, Ca, Mg, the characteristics of the ilmenite concentrate that Al is high, Ca in the raw material, Mg, the oxide compound of impurity elements such as Al has no adverse effects to its end product, with fairly simple method, make the reduced ilmenite powder that chemical coating of welding electrode coating is used, the comprehensive utilization natural resources, iron, titanium are also used.
The present invention is for No. 3850615 a documents with United States Patent (USP), and the method that this patent proposes is, the ferriferous oxide that reduces in the titaniferous ore with the solid carbon reductive agent in fluidized-bed is a metallic state.The weak point of this technology is, not only complex process, and reductive agent is mixed with breeze, and the reaction back is separated by swirler, still contains carbon in the reduction mineral, and the Fe granularity after the reduction is very thin, can not be used to make chemical coating of welding electrode coating.
Method of the present invention is to adopt to contain TiO
247～50%, compact structure, FeO/Fe
2O
3The ilmenite concentrate of the granular ilmenite type of ratio 〉=5 carries out oxidizing roasting on electric furnace or sinter machine, maturing temperature is 790～890 ℃, and roasting time is with S content height and FeO/Fe in the raw material
2O
3Ratio size and decide Fe in the product of roasting
2O
3Content and take off S and lead with the time and be directly proportional is generally with S content in the product＜0.03% degree of being.Ilmenite after the oxidizing roasting adds the lid layer reductive agent above with in the fire proofed wood batch can of packing between powdered form and reductant layer.Reductive agent can be used high-carbon fuel such as charcoal, coke breeze, low-sulfur hard coal, bituminous coal, graphite, refinery coke, and its granularity is generally 0～15mm, is good with 1～5mm, and granularity is little, and specific surface is big, and active good, reducing power is good.The 120%(weight of the theoretical mixed carbon comtent of the ilmenite concentrate of the add-on of reductive agent after) greater than oxidizing roasting.Fire-resistant can after installing is sent into and is carried out two-stage reduction in tunnel furnace or the electric furnace, and the first stage of reduction temperature is 1140 ± 25 ℃, soaking time 〉=4 hour.After reduction ratio reaches more than 90%, be warmed up to 1240 ± 25 ℃, insulation again, soaking time 〉=30 minute are continued reduction and also being allowed the metal abrasive grit assemble to grow up, and soaking time is according to the requirement of product granularity is decided.Cooling is come out of the stove when temperature drops to 750 ℃ then, adopts protection to be quickly cooled to room temperature, to avoid the oxidation again of as-reduced iron.Subsequently thing in the fire-resistant can is poured on the screen cloth in 15mm aperture and sieved, make the reduzate and remaining reductive agent, ash separation of caking.The reduzate Universal ball grinding machine of packing into after the surface-conditioning dedust carries out fragmentation, crosses 40 mesh sieves, just obtains reduced ilmenite powder product.The chemical ingredients of product is compared as shown in table 1 with GB GB5688-85 welding electrode with reduced ilmenite powder FTH9.20.
The chemical ingredients of table 1 product (wt%) compares with GB
The size-grade distribution of product is compared as shown in table 2 with GB GB5688-85 welding electrode with ilmenite powder FTH9.20.
The size-grade distribution of table 2 product and GB are relatively
Product of the present invention meets the requirement that the GB GB5688-85 welding electrode of making chemical coating of welding electrode coating is used reduced ilmenite powder FTH9.20 fully.
Advantage of the present invention is:
(1) can fully utilize titanium, iron resources in the ilmenite concentrate, technical process is short, simple, the easily control of equipment.
(2) employing oxidizing roasting both can have been removed the S in the mineral, had changed the raw ore structure again, made ferriferous oxide become Fe with the ilmenite that titanium dioxide is solid-solubilized in
2O
3TiO
2Form, help the carrying out of reduction process.
(3) reductive agent and ilmenite concentrate interlayer are packed into and are reduced in the fire-resistant can, and its residual reductive agent and product separate easily are clean, and the reduzate carbon content is low.In addition, the interlayer tinning is a reductive agent around the ore, does not directly contact with jar, so can not glue jar.
(4) the two-stage reduction both can obtain bigger reduction rate, can obtain the iron particle thicker than the abrasive grit in the general reducing process again.Iron and TiO
2Be monomer separation, mechanically mixing, abrasive grit is spherical in shape, is suitable for doing very much chemical coating of welding electrode coating.
(5) oxide compound of impurities element such as Ca, Mg.Al etc. need not removed in the ilmenite, and these oxide compounds there is no harm to doing chemical coating of welding electrode coating, because usually add some mineral in the chemical coating of welding electrode formulation for coating material, (mainly contain TiO as rutile
2); Granite, feldspar (all mainly contain SiO
2And Al
2O
3), white clay, mica, talcum, kaolin (all mainly contain Al
2O
3And SiO
2), asbestos (mainly contain SiO
2, MgO, Al
2O
3And CaO) etc.So, the product that reduzate of the present invention can directly be used as chemical coating of welding electrode coating.
Technical process of the present invention such as accompanying drawing.
Embodiments of the invention adopt two kinds of technologies to carry out as a comparison respectively.It is raw material that two embodiment all adopt the milltailings ilmenite concentrate (belonging to granular ilmenite powder) of Flos Bombacis Malabarici vanadium titano-magnetite, and its ore compact structure contains TiO
247～50%, FeO/Fe
2O
3Ratio 〉=5.The chemical ingredients of ilmenite concentrate raw material is as shown in table 3.Make reductive agent with coke breeze, its chemical ingredients and granularity are as shown in table 4.
The chemical ingredients of table 3 ilmenite concentrate (wt%)
| TiO | MgO | Al 2O 3 | CaO | FeO | Fe 2O 3 | S | P |
| 47.68 | 6.00 | 1.40 | 1.20 | 34.22 | 5.72 | 0.12 | 0.01 |
The chemical ingredients (wt%) of table 4 reductive agent coke breeze and granularity (mm)
| Fixed carbon | Volatile matter | Ash content | Moisture | Granularity |
| 72.61 | 23.43 | 3.96 | 0.83 | 0～5 |
Embodiment 1:
Ilmenite powder claims 100 unit weights, reductive agent claims 25 unit weights, make fire-resistant can with alumina crucible, charging (is tank skin and central part packing reductive agent between the employing annular layer, adorn ilmenite powder between the two-layer reductive agent), simulation tunnel kiln reduction process is carried out the two-stage reduction: be incubated 4 hours down at 1140 ± 5 ℃, be warmed up to 1240 ℃ of insulations 30 minutes then, outage subsequently, furnace cooling to 750 ℃ is come out of the stove, and the sealing air cooling is to room temperature, tank switching, surface blowing cleaning is with crossing 40 eye mesh screens after the fragmentation of Universal ball grinding machine.The chemical ingredients of the reduced ilmenite powder product that is obtained is as shown in table 5, and its size-grade distribution is as shown in table 6.
The chemical ingredients (wt%) of table 5 embodiment 1 product
| TiO 2 | FeO | C | S | P |
| 49.09 | 34.99 | 0.057 | 0.085 | 0.0069 |
The size-grade distribution of table 6 embodiment 1 product, %
Embodiment 2:
Ilmenite powder claims 100 unit weights, and reductive agent claims 25 unit weights.With ilmenite powder in cabinet-type electric furnace with 860 ± 5 ℃ of oxidizing roastings 90 minutes under still air, packing into the charging method identical with embodiment 1 then, fire-resistant can carries out two-stage reduction, tank switching, surface-conditioning, fragmentation, (technology and various parameter and embodiment 1 are just the same) sieves.The chemical ingredients that adopts embodiment 2 initial oxidation roastings to carry out the reduced ilmenite powder that two-stage reductive technology obtained again sees Table 7, and its size-grade distribution sees Table 8.
The chemical ingredients (wt%) of table 7 embodiment 2 products
| TiO 2 | FeO | M.Fe | C | S | P |
| 52.40 | 8.62 | 26.3 | 0.17 | 0.026 | <0.01 |
The size-grade distribution of table 8 embodiment 2 products, %
Abrasive grit electron probe microanalysis in the product, iron level are 97.333%.
The contrast of chemical ingredients and size-grade distribution by two embodiment obtained products, can obviously find out, carry out two-stage reductive technology again after adopting embodiment 2 initial oxidation roastings, every index of its reduced ilmenite powder product all meets the GB GB5688-85 welding electrode reduced ilmenite powder FTH9.20 standard-required of chemical coating of welding electrode coating.And embodiment 1 with embodiment 2 identical reducing process conditions under, because do not carry out this process of oxidizing roasting, its sweetening effectiveness is very poor, the ferrous content height, the metallic iron reduction ratio is low, and the chemical ingredients of product and granularity all do not meet GB5688-85 welding electrode reduced ilmenite powder FTH9.20 standard.
Claims (2)
1, a kind of preparation method of reduced ilmenite powder comprising being raw material with the ilmenite concentrate, adopts oxidation, two steps of reduction, it is characterized in that:
A. will contain TiO
247～50% ilmenite concentrate carries out oxidizing roasting in air under 790～890 ℃, to remove S and to make FeO change Fe into
2O
3
B. add the solid carbon reductive agent, its granularity is 0～15mm, 120% (weight) of the theoretical mixed carbon comtent of the ilmenite concentrate of add-on after greater than oxidizing roasting, to be incubated down at 1140 ± 25 ℃ behind the adding of the ilmenite concentrate after the oxidizing roasting reductive agent, first stage of reduction is carried out in soaking time 〉=4 hour, makes Fe
2O
3Be reduced into Fe, insulation again under 1240 ± 25 ℃ then, the subordinate phase reduction is carried out in soaking time 〉=30 minute, and the Fe particle is grown up, and is cooled to 750 ℃ and comes out of the stove, and protection is quickly cooled to room temperature.
2, a kind of purposes of reduced ilmenite powder, its raw material ilmenite concentrate compact structure, FeO/Fe
2O
3Ratio 〉=5 is characterized in that, S in the raw material, Ca, Mg, Al content height, product make chemical coating of welding electrode coating and use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88103956 CN1022579C (en) | 1988-06-24 | 1988-06-24 | Process for preparing reduced titanite ore powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88103956 CN1022579C (en) | 1988-06-24 | 1988-06-24 | Process for preparing reduced titanite ore powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1036228A true CN1036228A (en) | 1989-10-11 |
| CN1022579C CN1022579C (en) | 1993-10-27 |
Family
ID=4832827
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88103956 Expired - Fee Related CN1022579C (en) | 1988-06-24 | 1988-06-24 | Process for preparing reduced titanite ore powder |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085737C (en) * | 1999-08-10 | 2002-05-29 | 中南工业大学 | Process for preparing Ti-enriched material from ilmenite concentrate |
| WO2011080253A1 (en) * | 2009-12-28 | 2011-07-07 | Crenox Gmbh | Method for recovering titanium-containing byproducts |
| CN101925427B (en) * | 2008-01-23 | 2014-06-18 | 特拉迪姆有限公司 | Phlegmatized metal powder or alloy powder and method and reaction vessel for production thereof |
| CN103937960A (en) * | 2014-04-08 | 2014-07-23 | 东北大学 | Staged reduction method of boron-containing iron ore concentrate |
| CN106367586A (en) * | 2016-11-22 | 2017-02-01 | 江苏省冶金设计院有限公司 | System and method for treating titanium concentrate |
| CN106399666A (en) * | 2016-11-22 | 2017-02-15 | 江苏省冶金设计院有限公司 | System and method for treating titanium concentrate by combining rotary hearth furnace and electric furnace |
| CN106801181A (en) * | 2016-12-10 | 2017-06-06 | 包钢集团矿山研究院（有限责任公司） | A kind of method that ferro-titanium is smelted in carbon thermal reduction |
| CN107743567A (en) * | 2015-06-15 | 2018-02-27 | 因姆普朗伯德公司 | Application of the ilmenite of pre-oxidation in fluidized-bed combustion boiler |
| CN107760870A (en) * | 2017-10-18 | 2018-03-06 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of welding reduced ilmenite |
| CN112410539A (en) * | 2020-10-30 | 2021-02-26 | 河南佰利联新材料有限公司 | Method for sorting titanium middlings containing weak magnetic gangue minerals |
-
1988
- 1988-06-24 CN CN 88103956 patent/CN1022579C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085737C (en) * | 1999-08-10 | 2002-05-29 | 中南工业大学 | Process for preparing Ti-enriched material from ilmenite concentrate |
| CN101925427B (en) * | 2008-01-23 | 2014-06-18 | 特拉迪姆有限公司 | Phlegmatized metal powder or alloy powder and method and reaction vessel for production thereof |
| WO2011080253A1 (en) * | 2009-12-28 | 2011-07-07 | Crenox Gmbh | Method for recovering titanium-containing byproducts |
| CN102753301A (en) * | 2009-12-28 | 2012-10-24 | 克利诺克斯股份有限公司 | Method for recovering titanium-containing byproducts |
| CN103937960A (en) * | 2014-04-08 | 2014-07-23 | 东北大学 | Staged reduction method of boron-containing iron ore concentrate |
| CN107743567A (en) * | 2015-06-15 | 2018-02-27 | 因姆普朗伯德公司 | Application of the ilmenite of pre-oxidation in fluidized-bed combustion boiler |
| CN106367586A (en) * | 2016-11-22 | 2017-02-01 | 江苏省冶金设计院有限公司 | System and method for treating titanium concentrate |
| CN106399666A (en) * | 2016-11-22 | 2017-02-15 | 江苏省冶金设计院有限公司 | System and method for treating titanium concentrate by combining rotary hearth furnace and electric furnace |
| CN106801181A (en) * | 2016-12-10 | 2017-06-06 | 包钢集团矿山研究院（有限责任公司） | A kind of method that ferro-titanium is smelted in carbon thermal reduction |
| CN106801181B (en) * | 2016-12-10 | 2019-01-29 | 包钢集团矿山研究院（有限责任公司） | A kind of method that ferro-titanium is smelted in carbon thermal reduction |
| CN107760870A (en) * | 2017-10-18 | 2018-03-06 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of welding reduced ilmenite |
| CN112410539A (en) * | 2020-10-30 | 2021-02-26 | 河南佰利联新材料有限公司 | Method for sorting titanium middlings containing weak magnetic gangue minerals |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1022579C (en) | 1993-10-27 |
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