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WO2006097569A1 - Procede et equipement pour le traitement thermique de solides contenant du titane - Google Patents

Procede et equipement pour le traitement thermique de solides contenant du titane Download PDF

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Publication number
WO2006097569A1
WO2006097569A1 PCT/FI2006/000086 FI2006000086W WO2006097569A1 WO 2006097569 A1 WO2006097569 A1 WO 2006097569A1 FI 2006000086 W FI2006000086 W FI 2006000086W WO 2006097569 A1 WO2006097569 A1 WO 2006097569A1
Authority
WO
WIPO (PCT)
Prior art keywords
reactor
solids
separator
gas
cooler
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/FI2006/000086
Other languages
English (en)
Inventor
Ali-Naghi Beyzavi
Lothar Formanek
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Outokumpu Oyj
Metso Corp
Original Assignee
Outotec Oyj
Outokumpu Oyj
Outokumpu Technology Oyj
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Outotec Oyj, Outokumpu Oyj, Outokumpu Technology Oyj filed Critical Outotec Oyj
Priority to AU2006224490A priority Critical patent/AU2006224490B2/en
Priority to CA2599564A priority patent/CA2599564C/fr
Publication of WO2006097569A1 publication Critical patent/WO2006097569A1/fr
Anticipated expiration legal-status Critical
Priority to NO20075289A priority patent/NO20075289L/no
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • C22B1/10—Roasting processes in fluidised form
    • 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
    • C22B34/1227—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 using an oxygen containing agent
    • 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
    • C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
    • C22B5/14—Dry methods smelting of sulfides or formation of mattes by gases fluidised material

Definitions

  • the present invention relates to a process for the heat treatment of solids containing titanium, in which fine-grained solids are heated to a temperature of 700 to 1000 0 C in a reactor with circulating fluidized bed and are discharged from the reactor together with waste gases into a downstream separator, in which the solids are separated from the waste gases and are recirculated to the reactor at least partly and/or phase by phase. Furthermore, the invention relates to a corresponding plant.
  • Such processes and plants are used for instance for the magnetizing calcination of ilmenite (X*Ti ⁇ 2 Y*FeOZ*Fe 2 O 3 ).
  • a reactor with stationary fluidized bed was used for the magnetizing calcination of ilmenite, which reactor has, however, only a small control range and a low reaction density.
  • a reactor with stationary fluidized bed only a comparatively low flow rate is possible with respect to the container volume.
  • the temperature and retention time control also frequently is unfavorable in the case of such reactors with stationary fluidized bed.
  • this object substantially is solved in that the ilmenite is calcined under reducing conditions.
  • a cooling apparatus which allows for a relatively rapid cooling of the product.
  • This may be effected by indirect cooling in an irrigation or shower cooler or by direct cooling by means of water injection.
  • an injection cooler is provided, in which the solids are cooled to below 250 0 C by injecting a coolant and possibly are cooled further in another cooler, for instance a fluidized-bed cooler, downstream of the injection cooler, fluidizing gas being introduced into the injection cooler with such a gas velocity that the Particle-Froude-Number in the fluidized bed is between 0.01 and 10, in particular between 0.1 and 1.
  • the Particle-Froude-Number at the bottom of the fluidized-bed cooler is between 0.1 and 0.25, in particular about 0.17.
  • the Particle-Froude-Number preferably is between 0.35 and 0.55, in particular about 0.47.
  • the Particle-Froude-Numbers are each defined by the following equation:
  • u effective velocity of the gas flow in m/s
  • Pt effective density of the fluidizing gas in kg/m 3
  • p s density of a solid particle in kg/m 3 (apparent density)
  • dp mean diameter in m of the particles of the reactor inventory (or the secondary agglomerates formed) during operation of the reactor
  • g gravitational constant in m/s 2 .
  • dp does not designate the mean diameter (d_50) of the material used, but the mean diameter of the reactor inventory formed during operation of the reactor, which can differ significantly from the mean diameter of the material used (primary particles).
  • the product withdrawn from the reactor or the separator first of all is cooled very much in the cooling apparatus to e.g. about 100 to 200 0 C within a very short time. Changes in the magnetizingly calcined ilmenite during the cooling period largely can be avoided in this way. Due to the rapid cooling, a particularly high product quality of the magnetizingly calcined ilmenite thus can be achieved. This high product quality ensures a high degree of separation during a subsequent magnetic separation.
  • the gas velocity of the fluidizing gas in the injection cooler therefore is chosen such that a comparatively dense fluidized bed is obtained.
  • the fluidized bed is denser at the bottom of the injection cooler than at the top of the injection cooler, as the coolant injected is evaporated there.
  • the product heat no longer usable in the process is dissipated.
  • water is injected into the injection cooler as coolant.
  • the gas content in the fluidized bed of the injection cooler then can include between 50 and 70%, in particular about 60 % steam.
  • the process in accordance with the invention can be heat- treated effectively.
  • the process is suited for the magnetizing calcination of ilmenite.
  • the mean particle size (d_50) of the solids supplied to the reactor preferably is between 75 and 350 ⁇ m, in particular between about 100 and 150 um.
  • the maximum grain size of the solids supplied to the reactor is about 2 mm, preferably less than 250 ⁇ m.
  • the grain size of the ilmenite magnetizingly calcined in the reactor preferably lies in the same ranges indicated above.
  • the generation of the amount of heat necessary for the operation of the reactor can be effected in any way known to the expert for this purpose.
  • it is provided to cover the required amount of heat by supplying hot gases or preheated solids.
  • a gaseous reducing agent e.g. molecular hydrogen, gas mixtures containing molecular hydrogen, carbon monoxide or gas mixtures containing carbon monoxide, e.g. reformer gas
  • it is also possible to produce the above mentioned reducing gas in the reactor, e.g. by the awakestoichiometrical burning of fuels such as natural gas, oil or coal.
  • a particularly high product quality can be achieved when the retention time of the solids in the reactor is between 10 and 50 minutes, in particular about 30 minutes.
  • the Particle- Froude-Number in the reactor can lie in a range from about 0.3 to 30, in particular between 0.5 and 15.
  • the energy consumption of the process can be reduced in that in the separator at least part of the waste gas of the reactor is separated from solids and supplied to a preheating stage upstream of the reactor.
  • the preheating stage can, for instance, comprise a heat exchanger such as a Venturi preheater, and a separator such as a cyclone or the like. In this way, the solids supplied to the reactor are dried and preheated, whereby the heat treatment in the reactor is facilitated.
  • a multi-stage preheating of solids is also possible, the waste gas of the reactor being cooled step by step.
  • the waste gases of the reactor together with the e.g. steam-loaded waste gases of the injection cooler are cleaned in a waste gas cleaning stage downstream of the preheating stage.
  • the gases then can possibly be recirculated to the process.
  • the recirculation of solids from the separator into the reactor is effected in a self- regulating manner. In this way, an intensive internal and external re-mixing of the solids treated in the reactor can be effected, so that a uniform temperature and reaction profile is achieved in the reactor.
  • a plant in accordance with the invention which is in particular suited for performing the process described above, includes a reactor with circulating fluidized bed, downstream of which a separator is provided. Downstream of the reactor and/or the separator there is furthermore provided a cooling apparatus formed as an injection cooler and downstream of the same a separate fluidized- bed cooler.
  • the product can be cooled quickly, i.e. within few seconds, to temperatures between e.g. 100 and 200 0 C by injecting for instance water.
  • This rapid first cooling is decisive for the product quality, as for instance during the magnetizing calcination of ilmenite changes in the product are possible during a too long cooling time.
  • the final cooling of the product then is effected in the separate fluidized-bed cooler, which is provided downstream of the injection cooler.
  • cooling coils are provided in the fluidized-bed cooler, through which a coolant is passed countercurrently. These cooling coils can for instance be combined to form cooling bundles.
  • the product heat no longer usable in the process can be dissipated particularly effectively, when the same has two or more chambers through whose bottom fluidizing gas is introduced by means of a blower.
  • the fluidizing gas on the one hand is used for cooling the product and at the same time effects an intensive intermixing of the solids to be cooled.
  • the reactor preferably has a separate upstream burning chamber, in which the hot gas is produced. It, however, is equally possible to provide a lance assembly and/or bottom tuyeres opening into the same, e.g. disposed laterally, which are connected with a supply conduit for especially gaseous reducing agents, so that the fuel is burnt inside the reactor.
  • a self-regulating U- shaped seal is provided between the reactor and the separator, by means of which the supply of solids from the separator into the reactor is controlled.
  • An expensive control system for instance by using an L-valve known from the prior art, thus can be omitted.
  • a preheating stage can be provided upstream of the reactor, in which the solids are dried and preheated.
  • the preheating stage includes e.g. a drier, which is connected with the waste gas conduit of the separator downstream of the reactor, so that the heat present in the waste gas stream can be utilized for predrying/ preheating the solids.
  • moist solids are introduced into a preheating stage via a screw conveyor 1.
  • This preheating stage comprises a Venturi drier 2, in which the raw material is suspended, dried and preheated, and a separator 3, e.g. a cyclone, downstream of the Venturi drier 2.
  • the solids separated from waste gases in the separator 3 are charged into a reactor 4.
  • the reactor 4 constitutes a fluidized-bed reactor with a circulating fluidized bed.
  • bottom tuyeres are provided in the reactor 4, through which gas, e.g. air or mixtures with air, is introduced by means of a blower 5.
  • gas e.g. air or mixtures with air
  • a blower 5 Via lateral lances 6, natural gas is supplied to the reactor 4, which is burnt inside the reactor together with the fluidizing gas.
  • fuel can be introduced into the reactor 4 via a conduit 7 by means of bottom tuyeres.
  • the gas composition e.g. the content of CO and CO 2
  • the reducing potential of the gas depends on the relation CO:CO 2 .
  • the solids are carried upwards by the fluidizing gas. Part of the solids separate out in the reactor and are thereby recirculated to the circulating fluidized bed, in order to be carried upwards again by the fluidizing gas. Together with a waste gas stream from the reactor 4, the other part of the solids is discharged upwards through a conduit 8 and in a downstream separator 9, for instance a cyclone, separated from the gas stream for the most part. Through a conduit 10, the solids from the separator 9 are recirculated to the fluidized-bed reactor 4. By means of this intensive internal and external remixing a particularly uniform temperature and reaction profile is achieved inside the fluidized-bed reactor 4.
  • the control of the amount of solids recirculated from the separator 9 into the fluidizedbed reactor 4 is effected via a self-regulating U-shaped seal 11 which is provided in the conduit 10.
  • a control and regulating unit for metering the amount of solids recirculated into the fluidized-bed reactor 4 can be omitted.
  • the gas stream separated from the solids in the separator 9 is supplied to the Venturi drier 2, so that the heat content of the gas stream leaving the separator 9 is utilized for drying and preheating the solids.
  • hot solids are withdrawn and supplied to an injection cooler 13 via conduits 12a and 12b, respectively.
  • the hot solids are fluidized in a stationary fluidized bed.
  • air is introduced into the injection cooler 13 as fluidizing air via a blower 14.
  • the gas velocity of the fluidizing gas is chosen such that the fluidization in the injection cooler 13 is low, so that the stationary fluidized bed expands only little.
  • water is injected into the injection cooler 13 as coolant via conduit 15.
  • the water is evaporated in the injection cooler 13, so that the stationary fluidized bed in the upper region of the injection cooler 13 expands more than in the bottom region of the injection cooler.
  • the fluidized-bed cooler Downstream of the injection cooler 13 a separate fluidized-bed cooler 16 is provided, in which the product heat no longer usable in the process is dissipated.
  • the fluidized-bed cooler has two chambers 16a and 16b, into which e.g. water is countercurrently introduced as coolant through schematically illustrated cooling coils 17, whereby the product is further cooled to the temperature necessary for the further processing, such as the magnetic separation.
  • a blower 18 air is introduced into the two chambers i6a and 16b of the fluidized-bed cooler 16, in order to fluidize and cool the product.
  • the cooled product then is supplied to the further processing via a conduit 19.
  • the separator 3 of the preheating stage, the injection cooler 13 as well as the fluidized-bed cooler 16 are connected with a waste gas cleaning stage 20, which for instance has a bag filter.
  • the gas streams partly containing solids and/or steam are cleaned.
  • the solids can be charged from the waste gas cleaning stage 20 into the fluidized-bed cooler 16.
  • the waste gas of the cyclone 3 was supplied to the waste gas cleaning stage 20, partly recirculated and oxidized and supplied to a chimney.
  • the dry ilmenite dust separated in the waste gas cleaning stage 20 was passed through a conduit directly into the product stream 19.
  • the injection cooler 13 was operated as stationary fiuidized bed by supplying about 6300 Nm 3 /h of recircuiated waste gas as fluidizing gas into the injection cooler 13 via the blower 14. At the same time, about 8 m'lh of water were introduced into the injection cooler 13 via conduit 15, so that the hot ilmenite was cooled to about 150 0 C within few seconds. Due to the evaporating water, the steam was about 60% of the total amount of gas in the fluidized bed of the injection cooler 13. The gas velocity of the fluidizing gas introduced via the blower 14 was chosen such that the Particle-Froude-Number at the bottom of the injection cooler 13 was about 0.17 and at the top of the injection cooler about 0.47.
  • the final cooling of the product was effected in the two chambers 16a and 16b of the fluidized-bed cooler 16.
  • about 6000 Nm 3 /h of recirculated waste gas were introduced into the fluidized-bed cooler 16 via the blower 18.
  • cooling water was countercurrently passed through the chambers 16a and 16b via conduit 17.
  • the conduit 17 had cooling bundles. In this way, a reducing magnetizing calcination of ilmenite could be effected, and due to the rapid cooling no changes were detected during the cooling period, so that the calcined ilmenite had a high product quality.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Crucibles And Fluidized-Bed Furnaces (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L’invention concerne un procédé et un équipement pour le traitement thermique de solides contenant du titane. Selon ce procédé, des solides à grains fins sont chauffés à une température de 700 à 1000°C dans un réacteur (4) avec lit fluidisé circulant puis sont en partie évacués du réacteur (4) avec des effluents gazeux vers un séparateur en aval (9). Dans ce même séparateur, les solides sont séparés des effluents gazeux et remis en circulation vers le réacteur (4) au moins en partie et/ou phase par phase. Le traitement thermique selon l’invention est effectué en conditions oxydantes.
PCT/FI2006/000086 2005-03-16 2006-03-14 Procede et equipement pour le traitement thermique de solides contenant du titane Ceased WO2006097569A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
AU2006224490A AU2006224490B2 (en) 2005-03-16 2006-03-14 Process and plant for the heat treatment of solids containing titanium
CA2599564A CA2599564C (fr) 2005-03-16 2006-03-14 Procede et equipement pour le traitement thermique de solides contenant du titane
NO20075289A NO20075289L (no) 2005-03-16 2007-10-16 Fremgangsmate og anlegg for varmebehandling av faststoffer som inneholder titanium

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005012524A DE102005012524A1 (de) 2005-03-16 2005-03-16 Verfahren und Anlage zur Wärmebehandlung titanhaltiger Feststoffe
DE102005012524.7 2005-03-16

Publications (1)

Publication Number Publication Date
WO2006097569A1 true WO2006097569A1 (fr) 2006-09-21

Family

ID=36926902

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/FI2006/000086 Ceased WO2006097569A1 (fr) 2005-03-16 2006-03-14 Procede et equipement pour le traitement thermique de solides contenant du titane

Country Status (8)

Country Link
CN (1) CN101142329A (fr)
AU (1) AU2006224490B2 (fr)
CA (1) CA2599564C (fr)
DE (1) DE102005012524A1 (fr)
NO (1) NO20075289L (fr)
UA (1) UA91354C2 (fr)
WO (1) WO2006097569A1 (fr)
ZA (1) ZA200503457B (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105567933A (zh) * 2015-12-16 2016-05-11 宁波高新区世代能源科技有限公司 高效节能环保的不锈钢热处理机

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103031433B (zh) * 2011-09-30 2014-07-30 中国科学院过程工程研究所 一种钛铁精矿流态化氧化焙烧-流态化还原焙烧系统及焙烧工艺
CN103031432B (zh) * 2011-09-30 2014-09-24 中国科学院过程工程研究所 钛铁精矿流态化氧化-还原焙烧改性的系统及焙烧工艺
CN102410706A (zh) * 2011-11-03 2012-04-11 云南新立有色金属有限公司 一种钛铁矿粉流化床干燥方法
EP3153775A1 (fr) 2015-10-08 2017-04-12 Improbed AB Procédé permettant de faire fonctionner une chaudière à lit fluidisé
EP3153776A1 (fr) 2015-10-08 2017-04-12 Improbed AB Cycle de gestion de lit pour une chaudière à lit fluidisé et dispositif correspondant
DE102016103349A1 (de) * 2016-02-25 2017-08-31 Outotec (Finland) Oy Verfahren und Vorrichtung zur thermischen Behandlung eines verunreinigten Feststoffes
US20230131508A1 (en) * 2020-01-09 2023-04-27 Thyssenkrupp Industrial Solutions Ag Apparatus and process for thermal treatment of mineral solids

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4076796A (en) * 1975-06-03 1978-02-28 Metallgesellschaft Aktiengesellschaft Carrying out endothermic processes in fast fluidized reactor with conventionally fluidized holding reactor
AU765620B2 (en) * 1998-11-23 2003-09-25 Outotec Oyj Process of reducing ilmenite
WO2004057040A1 (fr) * 2002-12-23 2004-07-08 Outokumpu Technology Oy Procede et installation mettant en oeuvre un lit fluidise pour le traitement thermique de solides contenant du titane

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4076796A (en) * 1975-06-03 1978-02-28 Metallgesellschaft Aktiengesellschaft Carrying out endothermic processes in fast fluidized reactor with conventionally fluidized holding reactor
AU765620B2 (en) * 1998-11-23 2003-09-25 Outotec Oyj Process of reducing ilmenite
WO2004057040A1 (fr) * 2002-12-23 2004-07-08 Outokumpu Technology Oy Procede et installation mettant en oeuvre un lit fluidise pour le traitement thermique de solides contenant du titane

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105567933A (zh) * 2015-12-16 2016-05-11 宁波高新区世代能源科技有限公司 高效节能环保的不锈钢热处理机

Also Published As

Publication number Publication date
AU2006224490A1 (en) 2006-09-21
AU2006224490B2 (en) 2010-07-22
ZA200503457B (en) 2006-02-22
CA2599564A1 (fr) 2006-09-21
CA2599564C (fr) 2016-05-24
DE102005012524A1 (de) 2006-09-21
NO20075289L (no) 2007-12-10
CN101142329A (zh) 2008-03-12
UA91354C2 (ru) 2010-07-26

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