EP2918688A1 - Entschwefelungsverfahren eines flüssigen Gusseisens, und Seelendraht für seine Umsetzung - Google Patents

Entschwefelungsverfahren eines flüssigen Gusseisens, und Seelendraht für seine Umsetzung Download PDF

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Publication number
EP2918688A1
EP2918688A1 EP15155616.4A EP15155616A EP2918688A1 EP 2918688 A1 EP2918688 A1 EP 2918688A1 EP 15155616 A EP15155616 A EP 15155616A EP 2918688 A1 EP2918688 A1 EP 2918688A1
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EP
European Patent Office
Prior art keywords
iron
lining
wire
calcium
liquid
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.)
Granted
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EP15155616.4A
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English (en)
French (fr)
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EP2918688B1 (de
Inventor
Sébastien GERARDIN
Olivier BAHUON
Alain Markwitz
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Affival SA
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Affival SA
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Priority to PL15155616T priority Critical patent/PL2918688T3/pl
Publication of EP2918688A1 publication Critical patent/EP2918688A1/de
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Publication of EP2918688B1 publication Critical patent/EP2918688B1/de
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C1/00—Refining of pig-iron; Cast iron
    • C21C1/02—Dephosphorising or desulfurising
    • C21C1/025—Agents used for dephosphorising or desulfurising
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/0056—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00 using cored wires
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04—Removing impurities by adding a treating agent
    • C21C7/064—Dephosphorising; Desulfurising
    • C21C7/0645—Agents used for dephosphorising or desulfurising

Definitions

  • the invention relates to the field of processes for the production in the liquid state of cast iron for the production of molded parts. It concerns mainly, but not exclusively, cast irons whose carbon is in the form of graphite, both vermicular graphite cast irons, and flake graphite cast irons, and spheroidal graphite cast irons known as GS fonts or ductile cast irons.
  • a cast iron is an alloy of iron and carbon containing from 2 to 7% by weight of carbon approximately, and containing various other elements as alloying elements or impurities.
  • the carbon content of a cast iron whose carbon is in the form of graphite is in most cases around 3.0 to 3.8% by weight. All percentages that will be given later will be percentages by weight.
  • Cast irons are commonly developed using facilities called "cupolas". They are vertical furnaces fed with scrap and coke. The melting takes place at high temperature and produces a carbon-rich liquid metal. At the end of these cupolas, the cast also contains elements such as silicon (from 0.5 to 2.5%), manganese (from 0.4% to 1.0%) and sulfur whose content can be as high as 0.12%. This sulfur comes from the use of coke, which contains it as an impurity.
  • the calcium sulphides thus created form a slag on the surface of the liquid iron which is enclosed in a container called a "pocket". It is then necessary to "unravel” it, that is to say to remove it by means of tools such as a plane, controlled manually or by a machine.
  • the use of CaC 2 results in the formation of a dry, solid slag, supernatant on the surface of the cast iron. This is therefore regularly cleaned by the operator to avoid irreparable deterioration of the refractory lining the inside of the pocket and with which the liquid iron and slag are in contact.
  • This energetic stirring can also be obtained, in addition to or in place of the use of Ca carbonate, by an injection of neutral gas (generally nitrogen) by means of a porous plug disposed in the bottom of the pocket.
  • neutral gas generally nitrogen
  • An electromagnetic stirring technique described in the patent US-A-4,412,801 , also allows such a brewing of the cast iron.
  • Magnesium can also be used in admixture with other products for the desulfurization of cast iron. So the document EP-A-0 514 294 describes a product comprising a mixture of calcium carbide and magnesium grains: the magnesium is coated with calcium carbide. The mixture may further contain a slag of composition 2CaO.SiO 2 . Again, the desulfurization process requires the use of CaC 2 .
  • the object of the invention is to completely prevent the use of calcium carbide for the desulphurization of cast iron, in particular cast irons whose carbon is in the form of graphite, for economic and ecological reasons, while maintaining an effective less comparable to desulphurization compared to processes using calcium carbide.
  • the subject of the invention is a continuous desulphurization process for a liquid iron, in which a flux-cored wire comprising an envelope is injected into the liquid iron flowing continuously in a liquid-iron processing plant. and a lining, said lining comprising a desulfurizing product, characterized in that said desulfurizing product is metallic calcium, in that the lining also comprises at least one neutral element with respect to the melt, and in that the content the metal calcium of the packing is such that the content of metallic calcium of the cored wire is between 30 and 120 g / m of cored wire.
  • Said neutral element present in the lining may be iron.
  • Said lining may also contain aluminum, representing up to 2% by weight of the lining.
  • Said cast iron may be a cast iron whose carbon is in the form of graphite.
  • the invention also relates to a cored wire for the metallurgical treatment of liquid metals, comprising a lining of a product intended to dissolve and react optionally with the liquid metal and a casing surrounding said lining, characterized in that said lining comprises calcium and at least one neutral element with respect to a cast iron, said content of the metallic calcium thread in the assembly formed by the packing and the casing being between 30 and 120 g / m of cored wire .
  • Said neutral element may be iron.
  • Said lining may also contain aluminum, representing up to 2% by weight of the lining.
  • Said lining may be in powder form.
  • Said packing may be in the form of an extruded bar.
  • the invention consists in carrying out the desulphurization of a cast iron, in particular of a graphitic cast iron, by a continuous process in which is added by means of a cored wire, as a desulfurizing product, a mixture of calcium base, a neutral element for cast iron such as iron, and possibly aluminum.
  • Calcium is a widely used element in the iron and steel industry for the pocket treatment performed before pouring. It makes it possible to modify the chemical composition of the inclusions, and consequently their morphology and their properties, for example in order to improve the flowability of the steels by transforming the solid alumina inclusions into inclusions of calcium aluminates (CaO, Al 2 O 3 ), liquids at usual casting temperatures, or making inclusions of plastic oxides during rolling.
  • CaO calcium aluminates
  • the most relevant criterion to be respected as regards the composition and morphology of the cored wire is its metric weight of metallic calcium. This takes into account not only the Ca content in the desulphurizing product, but also the diameter and compactness of the wire lining, to determine how much Ca, and therefore what length of wire, must be added to obtain the desulfurization depending on the sulfur content of the initial melt.
  • the advantages of the cored wire 10 containing the material to be added to the liquid metal with respect to an addition of the same material in the form of bulk powder or pieces are well known, including in the field of foundry: addition of a quantity of well controllable material and a depth certainly adequate, all this being achieved by adjusting the speed of injection of the wire, and the thickness of the metal shell which determines its melting speed.
  • This technique is well known to those skilled in the art, it is not necessary to describe it further.
  • the invention is based not on the use of the technique of addition of substances to liquid flux cored wire, known in itself, but on the nature of the substances thus added for the desulfurization of the liquid iron continuously.
  • the desulphurized liquid cast iron 14 flows continuously out of the siphon bag 1 by overflow over the side wall of the second compartment 7 and flows into a container (not shown) which will transport it to the site where it will be poured, while that the excess slag flows continuously, also by overflow through a scrubber opening 16 formed in the side wall of the pocket 1, and, if necessary, also using a plane controlled manually or automated, out the first compartment 5 of the siphon pocket 1 to pour into a container where it solidifies.
  • E d represents the amount of desulphurizer required per tonne of liquid iron to reduce the sulfur content of the liquid metal by 1 ppm.
  • This example is representative of the known prior art for the desulfurization of cast iron flowing continuously in a siphon pocket.
  • the contents of the cupola pour into a siphon pocket identical to that shown schematically in FIG. figure 1 .
  • the sulfur content obtained in the pocket during the calcium carbide treatment is particularly low (0.015%) with a powder consumption of 3.9 kg of product per tonne of processed iron, ie a desulphurization efficiency E d of 8.7 g ./t.ppm.
  • the slag formed is characterized by dry dross that can be removed from the siphon pocket without particular difficulties.
  • the quantity produced is on average between 10 and 20 kg of slag per tonne of processed iron.
  • this slag contains about 4.5% by weight of unprocessed calcium carbide, which makes it imperative to reprocess it to remove calcium carbide, or to store it in a special landfill to meet current environmental standards or, presumably, to come into the different country.
  • the overall cost of the desulfurization process is therefore not satisfactory, which is mainly the source of the problem that the invention aims to solve.
  • Reference Example 2 cored wire of CaC 2 and lime
  • Tests were conducted on the plant described in Example 1, and under comparable operating conditions relating to the flow of liquid iron, its temperature and its initial sulfur content.
  • the desulfurization efficiency E d for the reference wire is 7.1 g./t.ppm if only the addition of material due to the powder is taken into account. But it is preferable, because more rigorous, to also take into account the mass of iron brought by the envelope of the wire for the calculation of E d . In this case, E d is 13.0 g./t.ppm The powder consumption is lower than the reference method of Example 1, and the desulfurization efficiency E d is therefore better.
  • This wire was introduced into the siphon bag under the same conditions as those of the reference example 2.
  • the initial sulfur content at the start of the test was 0.085% with a flow rate of 20 tonnes per hour.
  • the injection speed of the cored wire was 4.2 m / min, ie a consumption of 2.4 kg of powder per ton of processed iron.
  • the sulfur content of the pig iron in the bag during the treatment was 0.038%, ie a desulphurization efficiency E d of 5.1 g./t.ppm, or 9.0 g./t.ppm if the intake is taken into account. in iron from the wrap of the wire. This result was therefore at this stage better than that of the reference example 2.
  • the sulfur content in the iron contained in the pocket 1 has risen to 0.065% despite an increase in the injection speed to 5 m / min (with a flow rate of iron and an initial sulfur content unchanged).
  • the desulfurization efficiency E d has thus deteriorated 14.3 g./t.ppm, or 25.4 g./t.ppm if the iron content of the wire casing is taken into account, and the test was discontinued since it was clearly Inconclusive.
  • Neutral element means an element which does not adversely affect the desulphurisation, in particular in that it does not have a negative impact on the composition and the physical properties of the slag, and the dissolution of which in the Liquid iron, in the amount present in the desulphurization product, would be tolerable with respect to future uses of the pig iron.
  • iron is such a neutral element since it constitutes the basic element of all melting and the casing of the cored wire, and an additional addition of iron to the liquid bath accompanying that of the desulfurization product would not have been possible. no chemical consequences, positive or negative.
  • the desulphurization could also constitute all or part of the operation of addition of an element that one would like to find at a minimum level in the final cast iron, and this would make it possible to benefit from the reliability linked to the addition of an element by cored wire, of which we previously spoke.
  • the inventors have thus first tested a mixture of metal calcium and iron powders, in proportions of about 30% / 70% by weight, respectively. Another 40% / 60% ratio was also tested. Considering the dimensions of the wire and the compactness of the mixture, the metric weight of Ca was respectively 81 and 102 g / m.
  • a deoxidizing element in this case aluminum.
  • the cast iron is not deoxidized at the outlet of the cupola.
  • the dissolved oxygen content is certainly not very high, due to the presence typically of between 3.50% and 3.70% of carbon, but it is not zero. Measurements carried out show dissolved oxygen contents of about 20 to 40 ppm at the outlet of the cupola.
  • the addition of aluminum in the cast iron reduces the oxidation of the bath according to the reaction: (3) 2 Al + 3 O ⁇ Al 2 O 3
  • the person responsible for making the cast iron may therefore plan to use flux cored wires of various aluminum contents. , so useful, to systematically add an effective amount but not excessive aluminum in the melt.
  • the aluminum content in the filling of the cored wire can vary from 0 to 2% by weight.
  • Examples 4.1 and 4.2 according to the invention flux-cored wire based on metallic calcium and iron
  • Table 1 shows the physical characteristics, where the thickness of the steel sheath and the calcium content vary.
  • Table 2 presents the metallurgical results for each wire in three series of tests. These results are compared with those obtained by the application of the conventional method described in the example and those obtained by the application of Example 2 (reference cored wire).
  • the cored wires 4.1 and 4.2 according to the invention give much better results than the reference cored wire of the invention.
  • Example 2 which contains CaC 2 : 30 to 40% improvement, a fortiori that the reference wire 1 (between 44 and 52% improvement). If one takes into account the iron brought by the envelope of the wire, the improvement seems smaller, but is nevertheless significant. The validity of the idea underlying the invention is therefore fully confirmed.
  • the behavior of the formed slag is perfectly adapted to the deslagging of the siphon pocket.
  • the formed slag does not adhere to the refractory walls of the ladle, unlike that of Example 3.
  • the quantity of slag generated by the desulfurization treatment is less than 5 kg per tonne of iron treated.
  • This slag does not contain, of course, any trace of calcium carbide. It can therefore be removed from the foundry in the form of ordinary waste, without danger to the environment, and be used for the same purposes, for example, of the cement works and public works, as, for example, the classic slags of high -flowers and steel mills.
  • the surface of the cast iron is loaded with very fine slag pellets. These beads will then grow in diameter over time.
  • the process was self-sustaining: the balls, which have become sufficiently large, with a diameter of the order of 10 cm, are evacuated by the scrubber orifice 16, are replaced by new ones. very small balls that will grow in turn, and so on. The scrubbing operation is thereby greatly facilitated.
  • the figure 2 shows the surface of the slag 6, with the cored wire 10 which crosses it. We can see very well that the slag is very much in the form of small and large logs.
  • These balls 17, 18 are each composed of an alternation of thick concentric layers of slag with high proportions of sulfur (approximately 1 to 4 mm) and thinner metal layers (of the order of a millimeter).
  • the mechanisms of formation of these beads 17, 18 are, for the moment, unknown, but this phenomenon is systematically observed.
  • the flux-cored wire according to the version of example 3 is to be avoided since it does not generate slags that are easily removable, which leads to very poor desulphurization once past the beginning of the treatment. It was therefore not considered useful to evaluate several of the mentioned parameters, since even if it does not use calcium carbide, it is not a satisfactory technical solution on important points.
  • Example 2 Although more expensive because of its conditioning, the reference cored wire of Example 2 (20% CaC 2 - 80% CaO) is advantageous vis-à-vis the addition of CaC 2 bulk. Indeed, the evacuated slag containing much less calcium carbide, it generates a lower environmental risk. Nevertheless, this risk exists, and one can think that the coming years will irremediably see the total prohibition of the use of the calcium carbide in foundry in all its forms. The inventors' approach is a priority in this context of respect for the environment, while taking into account, of course, the technical results to be achieved.
  • the flux-cored wire of Example 4.1 according to the invention (81 g / m of Ca) makes it possible to achieve a desulfurization efficiency of more than 40% higher than that of the CaC 2 reference flux-cored wire, with an economic balance sheet as well. favorable (8% gain). Economically more expensive by 20% compared to the bulk addition, this example 4.1 has the considerable advantage of not generating any waste containing residual calcium carbide, in addition to being more efficient from a metallurgical point of view. For all these reasons, the immediate additional cost compared to the bulk addition of CaC 2 , as long as it is legally possible, can be offset, or at least greatly reduced, by savings on recycling or storage of slag.
  • Example 4.2 (102 g / m Ca) has a desulfurization efficiency quite comparable (40%) to that of the yarn of Example 4.1. As with the latter, the waste generated contains no trace of calcium carbide.
  • the flux-cored wire according to the invention makes it possible to respond optimally technically and economically to the problem of desulfurization of the iron at the end of a cupola, while controlling the environmental constraints.
  • the cored wire according to the invention is characterized by a composition of the packing, whether in the form of a powder or in the form of an extruded bar, calculated so that, taking into account the material of the casing of the wire filled, the material introduced into the cast iron, taken as a whole, contains between 30 and 120 grams of metallic Ca per meter of cored wire, the rest of the packing and the envelope of the wire which dissolves in the molten iron being constituted by at least one element whose behavior towards the cast iron can be described as "neutral" in the sense that has been seen, and which in most cases will be iron.
  • the addition of metallic Ca varies from 1.4 to 1.7 g per tonne of melt and per ppm of sulfur to be removed.
  • This amount of sulfur to be removed is generally from 300 to 700 ppm, and thus, theoretically, 420 to 1190 g of metallic Ca per tonne of melt are required. It is considered that the optimum speed of introduction of the cored wire into the pocket, to obtain a melting of the wire at the right depth, is 2 to 5 m / min.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)
  • Treatment Of Steel In Its Molten State (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
EP15155616.4A 2014-03-11 2015-02-18 Entschwefelungsverfahren eines flüssigen gusseisens, und seelendraht für seine umsetzung Active EP2918688B1 (de)

Priority Applications (1)

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PL15155616T PL2918688T3 (pl) 2014-03-11 2015-02-18 Sposób odsiarczania ciekłego żeliwa i drut rdzeniowy do jego realizacji

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR1451999A FR3018524B1 (fr) 2014-03-11 2014-03-11 Procede de desulfuration d'une fonte liquide et fil fourre pour sa mise en oeuvre

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EP2918688A1 true EP2918688A1 (de) 2015-09-16
EP2918688B1 EP2918688B1 (de) 2018-11-28

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EP (1) EP2918688B1 (de)
FR (1) FR3018524B1 (de)
PL (1) PL2918688T3 (de)
TR (1) TR201902701T4 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114606362A (zh) * 2022-03-17 2022-06-10 首钢水城钢铁（集团）有限责任公司 一种转炉渣洗脱硫的工艺

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1980002565A1 (fr) * 1979-05-15 1980-11-27 Sofrem Produit pour la desulfuration des fontes et aciers
US4412801A (en) 1980-05-02 1983-11-01 G. Siempelkamp Gmbh & Co. Pressed-board plant with multilevel press
EP0281485A1 (de) * 1987-02-03 1988-09-07 Affival Mischprodukt in einer rohrförmigen Hülle zur Behandlung von geschmolzenen Metallbädern
EP0514294A1 (de) 1991-05-16 1992-11-19 Pechiney Electrometallurgie Entschwefelungsmittel für Gusseisen, bestehend aus Magnesium mit einem Kalziumkarbidüberzug
WO2010067033A1 (fr) * 2008-12-12 2010-06-17 Affival Armature pour bobine de fil pour addition de substances dans un bain de métal liquide
DE102012013662A1 (de) * 2012-07-10 2014-01-16 Mechthilde Döring-Freißmuth Füllldraht und Verfahren zur Behandlung von Eisenschmelzen

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2997963B1 (fr) * 2012-11-09 2015-09-04 Affival Fil fourre pour traitement metallurgique d'un bain de metal en fusion et procede correspondant

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1980002565A1 (fr) * 1979-05-15 1980-11-27 Sofrem Produit pour la desulfuration des fontes et aciers
US4412801A (en) 1980-05-02 1983-11-01 G. Siempelkamp Gmbh & Co. Pressed-board plant with multilevel press
EP0281485A1 (de) * 1987-02-03 1988-09-07 Affival Mischprodukt in einer rohrförmigen Hülle zur Behandlung von geschmolzenen Metallbädern
EP0514294A1 (de) 1991-05-16 1992-11-19 Pechiney Electrometallurgie Entschwefelungsmittel für Gusseisen, bestehend aus Magnesium mit einem Kalziumkarbidüberzug
WO2010067033A1 (fr) * 2008-12-12 2010-06-17 Affival Armature pour bobine de fil pour addition de substances dans un bain de métal liquide
DE102012013662A1 (de) * 2012-07-10 2014-01-16 Mechthilde Döring-Freißmuth Füllldraht und Verfahren zur Behandlung von Eisenschmelzen

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114606362A (zh) * 2022-03-17 2022-06-10 首钢水城钢铁（集团）有限责任公司 一种转炉渣洗脱硫的工艺
CN114606362B (zh) * 2022-03-17 2023-08-11 首钢水城钢铁（集团）有限责任公司 一种转炉渣洗脱硫的工艺

Also Published As

Publication number Publication date
TR201902701T4 (tr) 2019-03-21
FR3018524B1 (fr) 2017-03-10
EP2918688B1 (de) 2018-11-28
FR3018524A1 (fr) 2015-09-18
PL2918688T3 (pl) 2019-06-28

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