EP3760748B1 - Process for preparing optimized calcined, iron- and chrome-containing pellets - Google Patents

Process for preparing optimized calcined, iron- and chrome-containing pellets Download PDF

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Publication number
EP3760748B1
EP3760748B1 EP19183799.6A EP19183799A EP3760748B1 EP 3760748 B1 EP3760748 B1 EP 3760748B1 EP 19183799 A EP19183799 A EP 19183799A EP 3760748 B1 EP3760748 B1 EP 3760748B1
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Prior art keywords
pellets
chrome
iron
copr
calcined
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EP19183799.6A
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German (de)
English (en)
French (fr)
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EP3760748A1 (en
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Matthias Boll
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Brother Group Hong Kong Ltd
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Brother Group Hong Kong Ltd
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Priority to PL19183799.6T priority patent/PL3760748T3/pl
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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
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/2406—Binding; Briquetting ; Granulating pelletizing
    • 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
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/242—Binding; Briquetting ; Granulating with binders
    • C22B1/244—Binding; Briquetting ; Granulating with binders organic

Definitions

  • the invention relates to a process for preparing calcined, iron- and chrome-containing pellets, to calcined, iron- and chrome-containing pellets and their use for the preparation of Ferrochrome as well as to a process for the preparation of Ferrochrome using the calcined, iron- and chrome-containing pellets.
  • Ferrochrome A widely used iron- and chrome-containing alloy is the so called Ferrochrome.
  • Ferrochrome is used in the stainless-steel industry to increase the resistivity of steel against water and air to prevent the formation of rust.
  • the iron and chrome source for the Ferrochrome production is usually chromite, a chrome ore, which is found in some parts of the world, like in South Africa.
  • the production of Ferrochrome is usually carried out in huge electrically heated arc furnaces or blast furnaces at high temperatures, using a carbon based reductant which can be part of the electrode or which is mixed in the chrome ore, or both.
  • the consumption of electricity is significant and determines the cost effectiveness of a process using electrically heated furnaces.
  • the process results in a liquid, molten alloy which is casted in casts, and a layer of partially molten residue floating on top of the liquid metal, the slag.
  • fines fine chrome ore material
  • fines fine chrome ore material
  • a strong stream of hot gas is formed which results in an upstream.
  • the particles of the fines are too small to be dropped into the furnace: they would not reach the hottest zones (melt) for reduction. Most of this material will be blown out of the furnace with the off-gas stream.
  • pellets were formed out of the fines as disclosed in ZA 2004-03429 A .
  • Minerals Engineering (2012), 34, 55-62 a detailed description of the used binders and their properties and effects on the pellet strength and other properties are given.
  • the pellets produced according to the process of ZA 2004-03429 A and according to Minerals Engineering (2012), 34, 55-62 are made of chrome ore, a carbonaceous reductant and a so-called unconverted or non-activated binding agent.
  • the binding agent is a mainly silica based clay, like Bentonite. Bentonite comprises ca. 24 wt% of silicon.
  • organic binders e.g. Carboxy-methylcellulose.
  • the usage is limited to strength improvement in low temperature regimes as "wet green pellets" at room temperature as discussed in O. Sivrikaya, A. I. Arol (2013) Method to improve preheated and fired strengths of haematite pellets using boron compounds with organic binders, Ironmaking & Steelmaking, 40:1, 1-8, DOI: 10.1179/1743281212Y.0000000016 .
  • the binding agent Bentonite contains neither iron nor chrome and thus, cannot contribute to the formation of Ferrochrome afterwards. Instead, the silica contained in Bentonite increases the amount of useless and costly slag. Slag is not only an undesired by-product in the process for the production of Ferrochrome but furthermore its formation requires additional electrical energy (e.g. for heating and for the reduced throughput of the furnace).
  • Another disadvantage of the process is the effect of Bentonite on the density of the wet pellets fed into a tunnel furnace for pre-calcining step.
  • the Bentonite is absorbing water and decreases the density of the pellets, which leads to a lower throughput of material through the tunnel furnace, as this is limited by volume per time unit, but the producer get paid by mass of pellets produced.
  • the pore volume of the pellets is important, as the reducing gases formed in the arc furnace process need to reach the oxides in the pellets. So, a higher Chrome content and an increased density of the raw, dried pellets is desired with only small changes in the porosity of the indurated, calcined pellets. This results in lower slag production, higher throughput through the (tunnel-) furnace.
  • WO 2018/172284 A1 discloses a method for producing pre-reduced calcined, iron- and chrome-containing pellets, wherein chromite ore material and COPR are mixed with large amounts of a reductant component and subsequently reduced at temperatures of 1250 °C to 1600 °C in an inert or reducing atmosphere.
  • chromite ore material and COPR are mixed with large amounts of a reductant component and subsequently reduced at temperatures of 1250 °C to 1600 °C in an inert or reducing atmosphere.
  • the process according to said process yields calcined pellets with a higher cold crush strength compared to pellets obtained by using bentonite binder, they have a lower density than the latter.
  • CN 106 086 402 A discloses a method for producing ferrochrome.
  • the method comprises the steps of grinding ferrochrome ore and reducing agents separately into particles more than 70% of which has a particle size of 200 mesh; mixing; and forming to obtain pellets.
  • the method uses a binder which is one or more selected from bentonite and starch solution.
  • Organic binders are expected to have no large impact on the cold crush strength after firing, as they burn off at low temperatures below 500 °C.
  • the invention therefore provides a process for preparing calcined, iron- and chrome-containing pellets comprising the steps:
  • the chrome ore material used in step a) contains:
  • the worldwide largest chrome ores deposits are located in South Africa, countries, Turkey and the Philippines and in some other countries.
  • the chrome ore is divided into two categories: The metallurgical grade with ⁇ 45 wt% of Cr 2 O 3 and the chemical grade with ⁇ 45 wt% and ⁇ 40 wt% of Cr 2 O 3 .
  • the largest known deposit of chrome ore is found in clouds with over 300 million tons.
  • Chrome Ore Process Residue sometimes also named chromite ore processing residue is known to person skilled in the art as a waste stream comprising chrome and other metal oxides from the industrial production of chromate.
  • the Chrome Ore Process Residue (COPR) used in step a) is preferably a by-product from the sodium monochromate production process. Therein, chrome ore is mixed with soda ash and heated to a temperature of about 1200 °C under oxidizing condition. The reaction mixture is leached with water, and the dried solid residue is the so-called Chrome Ore Process Residue (COPR).
  • the COPR is obtained in the process for producing sodium monochromate from chromite via an oxidative alkaline digestion with sodium carbonate (no lime process, CaO content of ⁇ 5wt%).
  • COPR contains metal oxides such as chromium(III) oxide (Cr 2 O 3 ), aluminum oxide (Al 2 O 3 ), iron(III) oxide (Fe 2 O 3 ), iron(II) oxide (FeO), magnesium oxide (MgO), calcium oxide (CaO), silicon oxide (SiO 2 ), vanadium oxide (V 2 O 5 ), sodium oxide (Na 2 O) and sodium monochromate (Na 2 CrO 4 ).
  • metal oxides such as chromium(III) oxide (Cr 2 O 3 ), aluminum oxide (Al 2 O 3 ), iron(III) oxide (Fe 2 O 3 ), iron(II) oxide (FeO), magnesium oxide (MgO), calcium oxide (CaO), silicon oxide (SiO 2 ), vanadium oxide (V 2 O 5 ), sodium oxide (Na 2 O) and sodium monochromate (Na 2 CrO 4 ).
  • the Cr(VI) is preferably present as sodium monochromate (Na 2 CrO 4 ) in the COPR.
  • the CaO content of the COPR is preferably less than 15wt%, particularly preferably less than 10wt%, most preferably less than 5wt%.
  • COPR preferably contains:
  • the Cr(VI) content of the COPR is 0.01 to 1 wt%.
  • the Cr content in the COPR is 2 to 25 wt%, particularly preferably 5 to 9 wt%.
  • the Fe content in the COPR is 28 to 35 wt%, particularly preferably 29 to 34 wt%.
  • the Si content in the COPR is 0 to 1.5 wt%, particularly preferably 0.4 to 1.0 wt%.
  • the Cr(VI) content of the COPR is preferably ⁇ 0.0001 wt%.
  • COPR with a Cr(VI) content of ⁇ 0.0001 wt% is preferably obtained via a reduction process of COPR with a Cr(VI) content of 0.01 to 1 wt% in that the reduction of Cr(VI) to Cr(III) takes preferably place via polyethylene glycol (PEG) or glycerol as disclosed in WO 2014/006196 A1 or, alternatively, in an atmosphere containing less than 0.1 % by volume of an oxidizing gas as disclosed in WO 2016/074878 A1.
  • PEG polyethylene glycol
  • glycerol as disclosed in WO 2014/006196 A1
  • an atmosphere containing less than 0.1 % by volume of an oxidizing gas as disclosed in WO 2016/074878 A1.
  • the saccharide binder to be used in the present invention can be selected from monosaccharides, disaccharides, oligosaccharides, and polysaccharides or mixtures thereof, preferably from disaccharides, oligosaccharides, and polysaccharides or mixtures thereof, more preferably from oligosaccharides, and polysaccharides or mixtures thereof, and most preferably from polysaccharides and mixtures thereof.
  • Examples of monosaccharides are glucose, galactose, fructose and xylose
  • examples of disaccharides are sucrose, lactose, maltose and trehalose
  • examples for oligosaccharides include maltodextrins, raffinose, stachyose and fructo-oligosaccharides
  • examples of polysaccharides are amylose, amylopectin, starch, modified starches, arabinoxylans, chitin glycogen, cellulose, hemicellulose, pectins, hydrocolloids, agarose, dextran and guaran.
  • the saccharide binder comprises guaran, also called guar gum.
  • the amount of saccharide binder in the pellets obtained by step a) is typically below 5 wt%, preferably below 4 wt%, and most preferably in the range of 1 wt% to 3 wt% based on COPR.
  • the pellets obtained by step a) comprise the saccharide binder in an amount of 0.003 wt% to 1wt% based on the amount of chrome ore material, COPR, saccharide binder and, if present, carbonaceous reductant.
  • the pellets obtained by step a) comprise less than 3 wt%, preferably less than 2 wt%, more preferably less than 1 wt%, and most preferably 0 wt% of carbonaceous reductant based on the amount of chrome ore material, COPR, saccharide binder and carbonaceous reductant.
  • carbonaceous reductant refers to all organic substances, which are capable of reducing the Fe- or Cr oxides in the chrome ore material under the calcining conditions of step c).
  • said expression refers to the compounds anthracite, char, coke and bituminous coal.
  • carbonaceous reductant does not include saccharide binder.
  • pellets as used in the present invention refers to particular or granular material with regular or irregular shape, preferably with a spheric shape.
  • pellets refers to particles or granules having a volume equivalent to that of a sphere with a diameter of 4-30 mm, more preferably 8-20 mm, most preferably of 10-15 mm.
  • the mixing is conducted by using a dry ball mill.
  • the solid components used in step a) are preferably milled.
  • the milling can take place prior to the mixing in step a), during the mixing in step a) or after the mixing in step a).
  • the chrome ore material, COPR, saccharide binder and optionally carbonaceous reductant are milled during mixing in step a).
  • the pellets obtained by step a) comprise:
  • the mixture obtained after the mixing of the chrome ore material, COPR and optional carbonaceous reductant in step a) provides a particle size distribution (d90) of 50 to 100 ⁇ m, particularly preferably of 65 to 85 ⁇ m.
  • a d90 of 50 ⁇ m means that 90% by volume of the pellets of the mixture have a particle size of 50 ⁇ m and below.
  • the mixture obtained after the mixing of chrome ore material, COPR and an optional carbonaceous reductant is further mixed with water.
  • pelletization takes place.
  • pelletization can be effected by pressing the mixture into the desired form.
  • the weight ratio of water to the sum of the components chrome ore material, COPR and a carbonaceous reductant is preferably between 1:6 and 1: >100, particularly preferably between 1:8 and 1: >100, most preferably 1:125.
  • the pelletization may take place in either a pan or drum pelletizing unit. Thereby, composite carbon containing (so-called "green") pellets are obtained.
  • the silicon content of the pellets obtained by step a) is below 2.5 wt%, particularly preferably below 2 wt%.
  • the pellets obtained by step a) do not crack when dropped from a height of up to 0.2 m, particularly preferably of up to 0.4 m, most preferably of up to 0.5 m, on a steel plate.
  • the green wet pellets show, after drying in air, a density higher than pellets produced with a binder state-of-the-art.
  • the pellets can be pre-dried under ambient conditions, preferably at a temperature of 18 to 30 °C for 4 to 40 hours, preferably for 12 to 30 hours, but this is optional.
  • the optional drying is done by heating the pellets under atmospheric conditions, preferably. Particularly preferably, the drying takes place at a temperature above 70 °C, most preferably above 100 °C.
  • the time for the drying is preferably 2 to 50 hours, particularly preferably 6 to 30 hours, and can be performed in an oven.
  • step a) or step b), if step b) is performed may be conducted in different ways known to the skilled person. This calcining process can be performed either under ambient gas atmosphere or under an atmosphere with reduced oxygen level compared to ambient atmosphere.
  • the heating unit is preferably a rotary kiln, a muffle furnace, a tube furnace or a tunnel furnace, preferably a belt tunnel furnace.
  • the wet or optionally dry, pellets obtained by step a) or step b) are calcined at oven temperatures of 1250 °C to 1600 °C for periods of 1 minute to 8 hours, preferably of 1300 °C to 1500 °C for periods of 5 minutes to 5 hours.
  • the inert atmosphere contains less than 0.1 vol-% of oxygen.
  • the inert atmosphere is argon.
  • the heating unit is operated as a reduction unit i.e. the heating unit is operated such as to maintain sufficient reducing conditions in the immediate environment of the particle bed so as to achieve high degrees of both iron and chromium metallization and commensurately limited degrees of carbon burn-off.
  • the calcination is preferably carried out at oven temperatures of 1250 °C to 1600 °C for periods of 1 to 8 hours, preferably of 1300 °C to 1500 °C for periods of 2 to 5 hours, in an inert atmosphere.
  • the inert atmosphere contains less than 0.1 vol-% of oxygen.
  • the inert atmosphere is argon.
  • the reduction facility is preferably operated in a manner so as to ensure that the preheated pellets are maintained at a temperature of preferably 1350 °C to 1450 °C for a period of 2 to 5 hours, through the use of an oxygen enhanced coal combustion device.
  • Oxygen support of the combustion device is considered a vital part in ensuring adequate flame geometry and energy release, while enabling the maintenance of a suitably reducing environment in the particle bed to achieve the requisite degree of metallization.
  • metallized particles means that at least a part of the Fe- and Cr-ions contained in the chromite ore material and the COPR as used in step a) are reduced to chromium and iron in the oxidation state 0.
  • the degree of metallization in the metallized particles obtained by step c) is above 65%, particularly preferably above 75%, and most preferably above 85% of the weight of the Fe- and Cr-ions contained in the chromite ore material and the COPR as used in step a).
  • the degree of metallization can be determined via thermogravimetric analysis that is known to the skilled person. The loss of weight at those temperatures is directly correlated with the loss of bound oxygen consumed by the reductant component, and therewith the degree of metallization to Fe and Cr, and the loss of the reductant component itself. After the subtraction of organic compounds in the reductant component, which is determined in a separate measurement with pure reductant component, the degree of metallization can be calculated with ease.
  • step c By the use of the calcined pellets obtained by step c) the electrical energy consumption for the complete reduction to iron metal and chrome metal in the arc furnace is reduced.
  • step c) the calcined pellets obtained by step c) are discharged, either via direct hot transfer to the smelting furnace or via controlled cooling of the calcined product, to yield cool, mechanically stable pellets.
  • the Cr(VI) content is preferably ⁇ 0.0001 wt%.
  • the calcined pellets obtained by step c) provide increased mechanical stability compared to those obtained by step a).
  • the calcined pellets can be further stored or transported, e.g. to an electric submerged arc furnace for the preparation of Ferrochrome.
  • the calcined pellets obtained by step c) have an average cold crushing strength of at least 130 kgf/pellet, preferably at least 160 kgf/pellet, and most preferably at least 200 kgf/pellet. This value is determined in consideration of DIN EN 993-5 (2016) by placing a pellet between two steel plates arranged in parallel. With an hydraulic system, the plates are constantly moved towards each other and the pellet in the gap is squeezed. The applied force is measured continuously. The measurement is stopped, as soon as the applied force decreases while the plates are still moving towards each other (pellet has cracked). The maximum force measured in the described setup is calculated as an applied weight in kgf. 1 kgf are equivalent to 9.806650 N. In the present examples, the cold crushing strength is given the as average of 100 pellets of same size.
  • the present invention further provides calcined, iron- and chrome-containing pellets that contain:
  • the calcined iron- and chrome-containing pellets have an average cold crushing strength of at least 130 kgf/pellet, preferably at least 160 kgf/pellet, and most preferably at least 200 kgf/pellet.
  • the calcined, iron- and chrome-containing pellets contain chrome as chrome(III)oxide (Cr 2 O 3 ) and as chrome metal, iron as iron(II) oxide (FeO) and iron(III) oxide (Fe 2 O 3 ) and as iron metal, and silicon as silicon oxide (SiO 2 ).
  • the ratio of iron metal to iron(II,III) in the calcined, iron- and chrome-containing pellets is preferably ⁇ 1:2, particularly preferably ⁇ 1:10.
  • the ratio of chrome metal to chrome(III) in the calcined, iron- and chrome-containing pellets is preferably ⁇ 1:2, particularly preferably ⁇ 1:10.
  • the ratio of iron and chrome metal to iron(II,III) and chrome(III) in the calcined, iron- and chrome-containing pellets is preferably ⁇ 1:2, particularly preferably ⁇ 1:10.
  • the Cr(VI) content is preferably ⁇ 0.0001 wt%.
  • the calcined, iron- and chrome-containing pellets are particularly preferably free of Cr(VI).
  • the calcined, iron- and chrome-containing pellets have a diameter of 6 to 13 mm.
  • the calcined, iron- and chrome-containing pellets according to the invention are obtained by the process for preparing calcined, iron- and chrome-containing pellets according to the invention.
  • the invention further provides the use of calcined, iron- and chrome-containing pellets according to the invention for the preparation of Ferrochrome.
  • the invention further provides a process for the preparation of Ferrochrome, wherein the calcined, iron- and chrome-containing pellets according to the invention are fed into an electric arc furnace and molten under reduction of iron- and chrome oxides.
  • the material was placed in a pelletization disc and water was sprayed on the surface while the disc was turning to produce small pellets of about 3 mm, which were screened out and used as seed pellets for the actual pelletizing process.
  • pellets with a diameter of above 11,2 mm were screened out (with 7 wt% of water) and dried.
  • the density of the dried pellets was determined using the displaced volume method.
  • the pellets were calcined in a chamber furnace. The temperature was increased rapidly (within few minutes) to 1400 °C and hold for 10 minutes. The pellets were then left to cool down to ambient temperature. The density of the indurated pellets was determined on 200 pellets by the volume of displacement method. The cold compression strength (CCS) was determined using 200 indurated pellets produced as above.
  • Example B comparative example according to EP 18196811.6
  • the material was placed in a pelletization disc and water was sprayed on the surface while the disc was turning to produce small pellets of about 3 mm, which were screened out and used as seed pellets for the actual pelletizing process.
  • pellets with a diameter of above 11,2 mm were screened out and dried.
  • the density of the dried pellets was determined using the displaced volume method.
  • the pellets were calcined in a chamber furnace. The temperature was increased rapidly (within few minutes) to 1400 °C and hold for 10 minutes. The pellets were then left to cool down to ambient temperature. The density of the indurated pellets was determined on 200 pellets by the volume of displacement method. The cold compression strength (CCS) was determined using 200 indurated pellets produced as above.
  • Example C (comparative example according to ZA 2004-03429 A)
  • the material was placed in a pelletization disc and water was sprayed on the surface while the disc was turning to produce small pellets of about 3 mm, which were screened out and used as seed pellets for the actual pelletizing process.
  • pellets with a diameter of above 11,2 mm were screened out and dried.
  • the density of the dried pellets was determined using the displaced volume method.
  • pellets were calcined in a chamber furnace. The temperature was increased rapidly (within few minutes) to 1400 °C and hold for 10 minutes. The pellets were then left to cool down to ambient temperature. The averaged density of the pellets was determined on 200 pellets by volumetric displacement. The cold compression strength (CCS) was determined using 200 indurated pellets produced as above.
  • Example C (comparative) Average density of dried pellets (g/cm 3 ) 3.24 3.30 3.09 Average density of calcined pellets (g/cm 3 ) 3.41 3.45 3.34 Average Cold Crush Strength (kgf/pellet) > 200 > 120 > 200

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EP19183799.6A 2019-07-02 2019-07-02 Process for preparing optimized calcined, iron- and chrome-containing pellets Active EP3760748B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP19183799.6A EP3760748B1 (en) 2019-07-02 2019-07-02 Process for preparing optimized calcined, iron- and chrome-containing pellets
PL19183799.6T PL3760748T3 (pl) 2019-07-02 2019-07-02 Sposób otrzymywania zoptymalizowanych kalcynowanych peletek zawierających żelazo i chrom

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EP19183799.6A EP3760748B1 (en) 2019-07-02 2019-07-02 Process for preparing optimized calcined, iron- and chrome-containing pellets

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EP3760748A1 EP3760748A1 (en) 2021-01-06
EP3760748B1 true EP3760748B1 (en) 2023-09-20

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IT202100000386A1 (it) * 2021-01-12 2022-07-12 Danieli Off Mecc Prodotto agglomerato solido a base di ossidi di ferro e relativo metodo di produzione
CN114196822A (zh) * 2021-12-03 2022-03-18 河南锦瀚环保科技有限公司 一种圆盘造球烧结球团矿新型粘合剂及其制备方法
CN114592123B (zh) * 2021-12-27 2024-05-10 福建通海镍业科技有限公司 一种铬矿粉球及其制备方法

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ZA200403429B (en) 2004-05-06 2005-11-30 Xstrata South Africa Pty Ltd Process.
NO2870107T3 (pl) 2012-07-06 2018-06-16
KR20160073994A (ko) * 2013-10-21 2016-06-27 케이더블유쥐 리소시즈, 인코퍼레이티드 크로마이트 광석으로부터 직접 크롬 철 합금의 제조
EP3020690A1 (de) 2014-11-13 2016-05-18 LANXESS Deutschland GmbH Verfahren zur Reduktion von sechswertigem Chrom in oxidischen Feststoffen
CN106086402A (zh) * 2016-07-20 2016-11-09 江苏省冶金设计院有限公司 一种铬铁合金的生产方法
EA201992240A1 (ru) 2017-03-21 2020-03-23 Ланксесс Дойчланд Гмбх Способ получения железо- и хромсодержащих частиц

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