EP3231537B1 - Production de poudre de fer élémentaire à partir de solutions de décapage - Google Patents

Production de poudre de fer élémentaire à partir de solutions de décapage Download PDF

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Publication number
EP3231537B1
EP3231537B1 EP17162167.5A EP17162167A EP3231537B1 EP 3231537 B1 EP3231537 B1 EP 3231537B1 EP 17162167 A EP17162167 A EP 17162167A EP 3231537 B1 EP3231537 B1 EP 3231537B1
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EP
European Patent Office
Prior art keywords
iron
reduction
process according
compounds
thermal decomposition
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EP17162167.5A
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German (de)
English (en)
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EP3231537A1 (fr
Inventor
Mesut Rifat GÜNEY
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Borcelik Celik San Tic AS
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Borcelik Celik San Tic AS
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/36—Regeneration of waste pickling liquors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention relates to a method for producing elemental iron powder from acidic solutions formed as a result of acidic pickling which is performed during surface treatment of iron-containing materials. More particularly, the invention relates to a method for the recovery of iron compounds from acidic solutions formed after the pickling procedure, treatment of the same in a specific process, and obtaining of elemental iron with high metalization ratio.
  • the flat steel products which are used in automotive, white goods, electricity pylons, barriers etc. are usually surface cleaned acidically prior to coating with different metals (zinc, nickel, chromium, etc.), so called galvanization, in order to provide a longer service life.
  • different metals zinc, nickel, chromium, etc.
  • galvanization so called galvanization
  • an acidic bath HCl, H 2 SO 4
  • sulfuric acid baths were used commonly for the purpose of pickling in iron & steel industry, but as from 1960s, hydrochloric acid (HCl)-containing baths have started to become widespread with the aim of obtaining the product with more quality and more homogenized surface.
  • Hydrochloric acid (HCl) is a particularly preferred acid bath due to the fact that it provides obtaining of a faster result, consuming low amount of acid and its pyrometallurgical regeneration is easier and more economic. 0.30 kg HCl is being used for 1 ton of steel during pickling.
  • the waste solution which is also called spent acid, formed following the pickling applied for the surface cleaning of steel sheets is an iron rich solution. Beside this, said solution may contain hydrochloric acid, metal ions which are present in steel composition and soluble in HCl as well as certain amounts of zinc ions if an incorrect recovery is carried out.
  • the pickling solutions formed as a result of the reactions with hydrochloric acid vary in very wide ranges in composition, and establishing the method to be applied for recovering of these solutions is quite difficult.
  • the methods of recovering the acidic cleaning solutions are gathered in two groups. The first one is the recovery of acid and the second one is the recovery of the metal formed in the acid.
  • the methods that are used for the acid recovery or regeneration are electrodialysis, diffusion dialysis, membrane distillation, evaporation and spray drying. For the recovery of metal, methods such as extraction, retardation, ion exchange and crystallization are used.
  • GB 1,219,674 discloses the reduction of iron oxide compounds (Aman oxide) by way of treating them with hydrogen by heating at high temperatures up to 1200 °C, preferably between 860-1200 °C, followed by sintering.
  • sintering is a major problem in obtaining pure iron and flow paths can easily be clogged in dynamic systems such as fluidized bed.
  • sintered product is not preferred and it needs to be grinded.
  • GB 1137525 A discloses a process for producing pure iron powder and product thereof and US 2005/191231 A1 discloses a synthesis of magnetite nanoparticles and the process of forming Fe-based nanaomaterials.
  • elemental iron should have high purity (>%99). Since the kinetics of reduction reactions depend on the diffusion of the reductive substance, elemental iron is hard to obtain at high ratio, or long term treatment is essential, when the reaction occurs within the fixed bed reactors or other conventional equipments.
  • a decomposition step is carried out at the first stage in a fluidized bed for the recovery of the acid in the spent acid composition while pure iron oxide (Fe x O y ) is obtained from the iron-containing compounds (FeCl 2 and low amount of FeCl 3 ) formed in the spent acid, and HCl is obtained as the spent product.
  • the second process step within the scope of the method is based on reduction of pure iron oxide (Fe x O y ) compounds in a fludized bed system with hydrogen and/or CO-like reductant gas.
  • the present invention provides a process for obtaining elemental iron from the acidic solution of a pickling process wherein an iron-containing material, particularly steel is surface treated.
  • the process basically comprises the following steps:
  • Said thermal decomposition can be carried out preferably in a fluidized bed and at a temperature between 500 °C and 1000 °C.
  • H 2 or CO preferably H 2 or CO
  • H 2 is used as a reductant.
  • removal of the water occurring in this step is particularly preferred.
  • Said reduction can be carried out at a temperature above 500 °C as mentioned above.
  • the reduction can be carried out at temperatures of between 600-800 °C, more preferably about 650 °C.
  • the reductant used herein may comprise H 2/ N 2 gas mixture having a volumetric ratio of higher than 1:1, more preferably 2:1 or more.
  • Fe x O y particles by way of seeding during formation of Fe x O y compounds in thermal decomposition has certain advantages. Ultimately, due to this reason, elemental iron is obtained in a layered structure. Said Fe x O y particles treated with reduction have the preferred particle size of between 300 ⁇ m and 1000 ⁇ m, more preferably between 300 ⁇ m and 600 ⁇ m. Thus, the additional operations affecting quality of the material in the negative way such as grinding are eliminated.
  • a process for the production of elemental iron powder from the waste acidic solutions formed at the end of the acidic (HCl) pickling treatment which is applied during surface treatments of iron-containing materials, particularly steel materials is disclosed.
  • Said process optionally comprises the steps of regeneration and recovery of the spent acid used in the process.
  • the oxides on the surface of steel or iron-containing material treated with a pickling procedure are eventually cleaned and the material is prepared for subsequent surface treatments.
  • the process bath there exist usually the used HCl, iron ions, zinc ions and iron chloride compounds.
  • metal chlorides coming from the steel structure which can be soluble in acid.
  • HCl and iron chloride-containing dirty acid solution decomposes, and as a result, HCl is obtained along with Fe x O y compounds as the side product.
  • the invention in another aspect, may comprise an additional process step besides obtaining of emental iron which allows the recovery of gaseous HCl occurring after thermal decomposion in order to use it again in the pickling bath.
  • the regenerated gaseous acid can be removed from the medium, cooled and stored by way of conventional techniques, or it can be fed back to the pickling procedure. It has been observed that gaseous regenerated acid can be recovered more easily and efficiently if the thermal decomposition is carried out in a fluidized bed.
  • the regenerated acid for instance, can be seperated from iron oxide particles by way of drawing it into a cyclone by means of a fan. Afterwards, acid vapor comes to a venturi and its temperature can be decreased till 100 °C.
  • a ready-to-use acidic solution can be formed by spraying water onto the regenerated acid which can be taken into absorbers.
  • the inventors have found that the abovementioned diffusion limitation can be eliminated by using fluidizied bed at the reduction step. Since the contact surface of iron oxide particles with the reductant gas has been increased, a considerable increase in the efficiency has been observed. However, even though it has positive effect, it has been observed that the desired ratio of metalization could not be achieved and sintering is still a problem. To overcome these problems, the inventors have carried out a seeding procedure in thermal decomposition step and obtained the layered iron oxide compounds as shown in Figure 1 . The seeding can be carried out by addition of iron oxide seeds to the decomposition reaction medium. It has been unexpectedly observed that this layered structure has eliminated particularly the diffusion barrier problem, enhanced the reduction kinetics of Fe x O y compounds and it plays a significant role in obtaining the metalization at a higher ratio (>%99 Fe).
  • the iron oxide (Fe x O y ) compounds which are formed via seeding at the end of the decomposition, are being contacted with a reductant in a fluidized bed and elemental iron powder (Fe) is eventually obtained.
  • Said reductant is preferably H 2 or CO, more preferably H 2 gas.
  • reductant gases which are known in the prior art like CH 4 can also be used.
  • H 2 usage as a reductant the reduction of Fe x O y compounds in the fluidized bed is basically carried out in three steps.
  • reaction steps are as follows: 3Fe 2 O 3 + H 2 ⁇ 2Fe 3 O 4 + H 2 O 2Fe 3 O 4 + 2H 2 ⁇ 6FeO + 2H 2 O 6FeO + 6H 2 ⁇ 6Fe + 6H 2 O
  • Figure 4a presents the SEM image of the resultant iron particles obtained through the reduction procedure which has been carried out for 60 minutes wherein the volumetric ratio of H 2/ N 2 was 2:1 at 500 °C. In this experiment, 46% metalization was achieved.
  • Figure 4b presents the SEM image of the resultant iron particles obtained through the reduction procedure which has been carried out for 60 minutes wherein the volumetric ratio of H 2/ N 2 was 2:1 at 1000 °C. In this experiment, %99.98 metalization was achieved.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Chemically Coating (AREA)

Claims (14)

  1. Procédé d'obtention de fer élémentaire à partir d'une solution acide issue d'un procédé de décapage dans lequel un matériau contenant du fer a subi un traitement de surface, lequel procédé comporte les étapes suivantes :
    - solubiliser le matériau contenant du fer, au moyen d'une solution acide comprenant de l'acide chlorhydrique,
    - faire subir une décomposition thermique aux composés de type chlorure de fer formés dans ladite solution par suite de la solubilisation,
    - ensemencer le milieu en y ajoutant de l'oxyde de fer, au cours de la décomposition thermique, et obtenir des composés de type FexOy sous forme de couches,
    - obtenir des particules d'oxyde de fer, mettre les composés de type FexOy en couches ainsi formés en contact avec un matériau réducteur, dans un lit fluidisé, et réduire les composés de fer,
    - et obtenir, comme résultat de cette réduction, du fer élémentaire en poudre.
  2. Procédé conforme à la revendication 1, dans lequel le matériau contenant du fer est un produit plat en acier.
  3. Procédé conforme à la revendication 1, dans lequel la décomposition thermique est réalisée dans un lit fluidisé ou dans un four rotatif.
  4. Procédé conforme à la revendication 1, dans lequel la température au cours de l'opération de décomposition thermique vaut entre 750 et 950 °C.
  5. Procédé conforme à la revendication 3, lequel procédé comporte en outre le fait de régénérer une solution d'HCl en extrayant du HCl gazeux du lit fluidisé et en le faisant refroidir dans l'étape de décomposition thermique.
  6. Procédé conforme à la revendication 1, dans lequel le matériau réducteur est de l'hydrogène (H2) ou du monoxyde de carbone (CO).
  7. Procédé conforme à la revendication 6, dans lequel le matériau réducteur est de l'hydrogène (H2).
  8. Procédé conforme à la revendication 1, lequel procédé comporte le fait d'éliminer l'eau qui se forme au cours de la réduction des composés de fer.
  9. Procédé conforme à la revendication 1, dans lequel la réduction est opérée à une température qui vaut entre 500 et 1000 °C.
  10. Procédé conforme à la revendication 9, dans lequel la réduction est opérée à une température qui vaut entre 600 et 800 °C.
  11. Procédé conforme à la revendication 1, dans lequel de l'hydrogène (H2) est utilisé comme réducteur et introduit conjointement avec de l'azote (N2) utilisé comme gaz vecteur, et le rapport volumique H2/N2 est supérieur à 1/1.
  12. Procédé conforme à la revendication 11, dans lequel le rapport volumique H2/N2 est supérieur à 2/1.
  13. Particules de composés de type FexOy en couches, obtenues dans l'étape de décomposition thermique d'un procédé conforme à la revendication 1.
  14. Particules de fer en couches, obtenues dans l'étape de réduction d'un procédé conforme à la revendication 1.
EP17162167.5A 2016-03-25 2017-03-21 Production de poudre de fer élémentaire à partir de solutions de décapage Active EP3231537B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
TR2016/03891A TR201603891A2 (tr) 2016-03-25 2016-03-25 Dekapaj çözelti̇leri̇nden saf demi̇r tozu üreti̇mi̇

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
TR201603891 Previously-Filed-Application 2016-03-25

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EP3231537A1 EP3231537A1 (fr) 2017-10-18
EP3231537B1 true EP3231537B1 (fr) 2020-01-01

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TR (1) TR201603891A2 (fr)

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA844536A (en) * 1970-06-16 Kudryk Val Recovery of sulfur and iron oxide from pyritic materials
GB190300423A (en) 1903-01-07 1903-12-10 Henry William Hemingway Improvements in the Treatment of Waste Pickle Liquor for the Removal or Utilisation of Free Acid Contained therein.
GB662051A (en) * 1948-01-06 1951-11-28 Davide Primavesi Improved chemical process for producing powdered iron
GB656003A (en) 1948-03-18 1951-08-08 Erzhutte Ag A process for the simultaneous recovery of base metals in powder form and of metallic salts
SE306096B (fr) * 1965-06-23 1968-11-18 Centro Speriment Metallurg
GB1219674A (en) 1968-10-07 1971-01-20 British Iron Steel Research Process for the production of iron powder from aman oxide
US4414021A (en) * 1982-05-06 1983-11-08 Welbon William W Process for the synthesis of iron powder
JPS59145707A (ja) * 1983-02-10 1984-08-21 Furukawa Mining Co Ltd 強磁性の金属粉末の製造方法
AT399516B (de) * 1993-07-21 1995-05-26 Andritz Patentverwaltung Verfahren zur regeneration von salzsäure aus beizanlagen
US6962685B2 (en) * 2002-04-17 2005-11-08 International Business Machines Corporation Synthesis of magnetite nanoparticles and the process of forming Fe-based nanomaterials

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

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EP3231537A1 (fr) 2017-10-18

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