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WO2002014221A1 - Procede et dispositif de post-traitement d'oxyde de fer - Google Patents

Procede et dispositif de post-traitement d'oxyde de fer Download PDF

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Publication number
WO2002014221A1
WO2002014221A1 PCT/US2001/025533 US0125533W WO0214221A1 WO 2002014221 A1 WO2002014221 A1 WO 2002014221A1 US 0125533 W US0125533 W US 0125533W WO 0214221 A1 WO0214221 A1 WO 0214221A1
Authority
WO
WIPO (PCT)
Prior art keywords
iron oxide
reactor
chlorine content
fluid bed
weight
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/US2001/025533
Other languages
English (en)
Inventor
Edgar J. Robert
Donald F. Kuschel
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.)
INTERNATIONAL STEEL SERVICES Inc
Original Assignee
INTERNATIONAL STEEL SERVICES Inc
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 INTERNATIONAL STEEL SERVICES Inc filed Critical INTERNATIONAL STEEL SERVICES Inc
Priority to AU2001286487A priority Critical patent/AU2001286487A1/en
Publication of WO2002014221A1 publication Critical patent/WO2002014221A1/fr
Anticipated expiration legal-status Critical
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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/02—Apparatus therefor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • 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
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • 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

Definitions

  • the present invention relates to processes and apparatus for treating iron oxide, and more particularly to such processes and apparatus, which are used to reduce chlorine concentrations.
  • a typical process to produce iron oxide from waste steel pickle liquor is spray roasting. This process produces hydrochloric acid in the off gas stream and particles of iron oxide.
  • Iron oxide powder produced from waste pickle liquor in conventional steel making operations has residual chloride compounds.
  • the chloride content of the iron oxide may vary from 0.10-0.50%. Some applications require low chloride content.
  • Some special operating practices leads to very low chlorides, however, they lead to low surface areas. It is not difficult to obtain 0.08% Cl, but in those cases, the surface area is below 3.4 m 2 /g, which severely limits its application.
  • Another process described in the U. S. Patent No. 5,597,547 is based on mixing the iron oxide with about 3-25% by weight of yellow iron oxide containing crystalline water and adding water. The mixture formed is heated up to 800°C above the decomposition temperature of the yellow iron oxide for times up to 10 hours. Another method similar to the above is based on the addition of sulfuric acid followed by drying and calcining.
  • This process takes advantage of the heat content of the iron oxide to obtain temperature compounds by controlling the atmosphere surrounding the iron oxide particles during cooling.
  • the process of this invention involves in situ post treatment of the iron oxide to change its chemistry and properties to meet a wide range of specifications.
  • the apparatus used to carry out this method consists of a vertical vessel attached to the primary source of iron oxide, which may be a roaster and which has the means to fluidize the iron oxide, by injection of a gas through a fiuidizing media. The mass of gas injected is small compared to the mass of iron oxide, thus the temperature of the iron oxide is not substantially affected by the injection of the fiuidizing gas.
  • the fiuidizing gas has also the function of producing chemical changes and/or preventing chemical reactions with the iron oxide.
  • the level of iron oxide in the vessel is set to the desired residence time to achieve the desired properties.
  • the chlorine content of the iron oxide before the process will be about 0.15% by weight or greater and, more typically, in the range of about 0.16% by weight to about 0.17% by weight.
  • the chlorine content of the iron oxide will preferably be reduced to about 0.12% by weight or less and typically to a range of from about .012% by weight or less and typically to a range of from about 0.10% by weight to about 0.11% by weight.
  • Fig. 1 is a schematic drawing of a preferred embodiment of the apparatus of the present invention.
  • the apparatus of the present invention includes an iron oxide roaster 10, which is superimposed over a reactor 12.
  • the reactor 12 includes temperature probes 14 and 16.
  • the reactor 12 also includes fluid inlet lines 18 and 20, which are positioned respectively on aeration pads 22 and 24.
  • Iron oxide 26 from the iron oxide roaster 10 is positioned in the reactor 12.
  • Inside the reactor 12 there is a sloped screen 28 interposed between the iron oxide roaster 10 and the iron oxide 26 which separate large pieces of iron oxide.
  • the iron oxide 26 is preferably in a powder having a specific surface area in the range of 4.5m 2 /g to 5.5m 2 /g, in the reactor 12.
  • the screen 28 sloped slops downwardly and laterally to a terminal lateral pocket 30. Beneath the reactor 10, there is an outlet rotary valve 32, which unloads treated iron oxide to a final product conveyor 34.
  • the system consists of a reaction vessel 12 that is attached to the iron oxide 26, which is usually a roaster 10.
  • the reaction vessel 12 is thermally insulated to limit heat losses, and maintain the temperature of the iron oxide 26 as high as possible, generally above 450°C.
  • the screen 28 separates large pieces from the iron oxide 26. Large pieces of material, which may be refractory or other undesirable pieces, are separated by the screen 28 from the iron oxide 26 are collected in the pocket 30 and removed from time to time.
  • the iron oxide 26 is maintained at the desired level in the reactor 12 by controlling the feed rate of the rotary valve 32.
  • the temperature probes 16 and 18 provide the information to control the level of the iron oxide 26 by controlling the feed rate of the rotary valve through a programmable logic controller fluidization/reaction gas through fluid inlet lines 18 and 20, which give rise to the fluid bed.
  • the velocity of the gas in the reaction vessel 12 is maintained above the critical velocity to obtain a fluid bed.
  • the fluidized iron oxide 26 is removed from the bottom of the reaction vessel 12, after a suitable residence time is achieved.
  • the final product which will preferably have a chlorine content of 12% by weight or less is screened and removed in conveyor 34.
  • the volume of the reaction vessel as well as the level depends on the objective of the treatment. Typically, the iron oxide being treated will have residence times, up to 60 minutes.
  • the gases that can be used to produce the fluid bed and react with the iron oxide are natural gas, nitrogen, air, ammonia, steam, synthesis gas, combustion gases and other chemical compounds that may suit the application.
  • the temperature of these gases may vary from room temperature up to 590°C, depending upon the specific application.
  • the mechanical effects of the fluid bed will prevent the agglomeration of the iron oxide. This effect leads to powders with desired physical characteristics, such as surface area and particle size.
  • Waste pickle liquor used for roasting has a concentration of FeCI 2 between 18 and 26%, and a concentration of HCI between 0 and 10%.
  • the process can treat the iron oxide produced from waste pickle liquor with the above concentration.
  • a number of metallic chlorides will form at temperatures between 200°C and 800°C.
  • the present invention proposes to control the environment surrounding the iron oxide during the cooling phase, preventing the presence of chlorinated gases and consequently the formation of low temperature chlorides.
  • the above table shows that there is a family of chlorides that will form at low temperature, such as Mn, Ni, Mg and Zn.
  • the present invention prevents the formation of these and similar chlorides.
  • the injection of air as a fiuidizing gas at a rate of 1.2SCF/lb. of iron oxide leads to the formation of a fluid bed.
  • the fluidization of the iron oxide particles will prevent the agglomeration of the iron oxide resulting on a larger specific surface area. Applying this process, a surface area as high as 5.5m 2 /g may be obtained with a net chloride reduction of 0.06%. Additional reduction in the chloride level may be expected with the injection of steam as a fiuidizing gas.
  • a quality of iron oxide is produced in a roaster at a rate of 700kg/h to a temperature of 470°C.
  • the iron oxide is in particles having an average major dimension of about 0.52um. Specific surface area is 5.4m 2 /g.
  • the iron oxide has a chlorine content of 0.16% by weight.
  • the iron oxide is screened to remove particles having a major dimension of 12mm and is removed to a reactor having internal dimensions of 910mmX910mmX760mm. Inside the reactor, the iron oxide is maintained at a temperature of 430°C and a fluid bed is established by injecting air into the base of the reactor at a rate of 2.8Nm 3 /min. After having a residence time of about 17 minutes in the reactor, the iron oxide is removed from the reactor through a rotary valve at a rate of
  • the final product iron oxide is removed and cooled to a temperature of 130°C over a period of 3 minutes and was found to have a chlorine content of 0.10% by weight.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Metallurgy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Iron (AREA)

Abstract

Procédé servant à traiter l'oxyde de fer généré par de la liqueur de décapage épuisée contenant du chlorure d'hydrogène libre. On sépare de l'oxyde de fer les morceaux trop fortement dimensionnés. On maintient l'oxyde de fer à température élevée pendant une durée de résidence dans la cuve d'un réacteur. On injecte ensuite un agent de fluidisation afin de créer un lit fluidisé avec l'oxyde de fer. On maintient le niveau de l'oxyde de fer fluidisé et on évacue ensuite cet oxyde de fer de la cuve de réaction. L'invention concerne également un dispositif servant à mettre ce procédé en application.
PCT/US2001/025533 2000-08-15 2001-08-15 Procede et dispositif de post-traitement d'oxyde de fer Ceased WO2002014221A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001286487A AU2001286487A1 (en) 2000-08-15 2001-08-15 Process and apparatus for post-treatment of iron oxide

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US63960800A 2000-08-15 2000-08-15
US09/639,608 2000-08-15

Publications (1)

Publication Number Publication Date
WO2002014221A1 true WO2002014221A1 (fr) 2002-02-21

Family

ID=24564825

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2001/025533 Ceased WO2002014221A1 (fr) 2000-08-15 2001-08-15 Procede et dispositif de post-traitement d'oxyde de fer

Country Status (2)

Country Link
AU (1) AU2001286487A1 (fr)
WO (1) WO2002014221A1 (fr)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3311466A (en) * 1963-11-29 1967-03-28 Int Nickel Co Reduction of metal oxides
US3896211A (en) * 1967-10-02 1975-07-22 Harle & Lechopiez Purification of iron oxides

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3311466A (en) * 1963-11-29 1967-03-28 Int Nickel Co Reduction of metal oxides
US3896211A (en) * 1967-10-02 1975-07-22 Harle & Lechopiez Purification of iron oxides

Also Published As

Publication number Publication date
AU2001286487A1 (en) 2002-02-25

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