EP2302102B1 - Procédé de décapage pour des tôles d'acier - Google Patents

Procédé de décapage pour des tôles d'acier Download PDF

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Publication number
EP2302102B1
EP2302102B1 EP09754861.4A EP09754861A EP2302102B1 EP 2302102 B1 EP2302102 B1 EP 2302102B1 EP 09754861 A EP09754861 A EP 09754861A EP 2302102 B1 EP2302102 B1 EP 2302102B1
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EP
European Patent Office
Prior art keywords
steel sheet
pickling
gas
blowing
oxide scale
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EP09754861.4A
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German (de)
English (en)
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EP2302102A4 (fr
EP2302102A1 (fr
Inventor
Kenichi Uemura
Daisuke Sawada
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Nippon Steel Corp
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Nippon Steel and Sumitomo Metal Corp
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    • 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
    • C23G3/00—Apparatus for cleaning or pickling metallic material
    • C23G3/02—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously
    • C23G3/027—Associated apparatus, e.g. for pretreating or after-treating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • 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
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • 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
    • C23G3/00—Apparatus for cleaning or pickling metallic material
    • C23G3/02—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously
    • C23G3/021—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously by dipping

Definitions

  • the present invention relates to a pickling method of steel sheet for removing oxide scale from the surface of the steel sheet.
  • the surface of the steel sheet is cleaned for various purposes. For example, cleaning of the steel sheet before plating or coating, pickling for removing oxide scale from hot rolled steel sheet, etc. may be mentioned.
  • oxide scale is formed on the surface of the steel sheet. This oxide scale is caught up at the rolling rolls at the time of the next step of cold rolling and often becomes a cause of damage to the surface of the steel sheet, so removal of oxide scale is becoming an essential step.
  • the steel sheet is immersed in a plurality of acid solutions and continuously run through them to pickle it.
  • a plurality of acid solutions For example, as described in " Nobuhiro Shibatomi et al., Mitsubishi Heavy Industries Technical Review, Vol. 129, No. 1, 24-29 (1992 )", there is the method of removing oxide scale by providing a weir in a box-shaped pickling tank, placing a spray nozzle in it, and spraying acid on the steel sheet.
  • Si oxides once dissolved simultaneously with oxide scale have a small solubility in the pickling solution, so while Fe ions from the oxide scale can be present in the solution, sometimes only Si oxides are redeposited. Sometimes too, the concentration of the Si ions in the pickling solution causes a change to a gel state in the solution. The deposition of this gel on the surface of the steel sheet has also been observed.
  • the present invention was made so as to solve the above problem and has as its object the provision of a continuous pickling method of steel sheet according to claim 1 able to effectively remove Si oxides contained in oxide scale for steel sheet containing Si and to greatly improve the speed of dissolution of the oxide scale.
  • the inventors engaged in intensive studies on means for solving the above problems and as a result discovered that in the process of dissolution of oxide scale of steel sheet by pickling, by temporarily taking the steel sheet out from the pickling solution and blowing gas to at least part of the surfaces of the steel sheet in the air, part of the acid solution deposited on the surface of the steel sheet is made to evaporate and the acid concentration is locally raised. They confirmed that due to this, even stubborn Si oxides contained in the oxide scale can be efficiently removed. Further, they discovered that by later repeating the pickiling, the speed of dissolution of the oxide scale is remarkably improved.
  • the inventors discovered that by blowing the gas in a direction facing the direction of movement of the steel sheet, the effect becomes more remarkable. Furthermore, they discovered that by blowing the gas from a direction facing the direction of movement of the steel sheet and at a slant from the surface of the steel sheet, the effect becomes even more remarkable.
  • the present invention was made based on these discoveries and the object above can be achieved by the features defined in the claims.
  • the steel sheet after pickling process obtained by the present invention has a clean surface free of pickling scars.
  • FIG. 1 shows an example of blowing gas to the surface of the steel sheet in a single pickling tank during pickling and performing the subsequent pickling in the same pickling tank as the above,
  • the inventors discovered that when removing oxide scale formed on the surface of steel sheet, if temporarily blowing gas to at least part of the surfaces of the steel sheet in the air in the process of dissolving the oxide scale by a pickling solution, the pickling efficiency (efficiency of removal of oxide scale) is improved.
  • the deposited pickling solution becomes locally higher in acid concentration, so the adhered part of the oxide scale layer and steel sheet is selectively dissolved.
  • the oxide scale is easily removed.
  • the blowing of the gas if blowing the gas at a slant with respect to the surface of the steel sheet, the effect is obtained more remarkably.
  • JP S62-243788A also discloses a method of blowing air on to a steel strip.
  • this method is aimed at the removal of the layer of acid solution (boundary film layer) deposited on the steel strip. Therefore, this requires using air to blow away the acid solution and bringing an end of a partition plate having elasticity into contact with the steel strip to wipe away the remaining the acid solution. Allowing the deposited pickling solution to remain at the surface of the steel sheet to be concentrated as explained above is neither described nor suggested. Therefore, even if using the method or system of JP S62-243788A , the deposited pickling solution ends up being removed, so it is not possible to concentrate the deposited pickling solution to raise the acid concentration as explained above and an effect like the present invention cannot be obtained. Rather, the pickling solution ends up being removed, so new spot like patterns (patterns formed at surface of steel sheet due to uneven acid solution) are liable to form.
  • the surface of the steel sheet may mean one surface of the steel sheet, both (front and back) surfaces, the side surfaces, or all surfaces.
  • the surfaces are not particularly limited so long as surfaces on the steel sheet.
  • the dissolved and freed gel-like Si oxides and the oxide scale having the layer where Si oxides concentrate can be removed by blowing a gas.
  • a gas for removal of Si oxides and oxide scale, while the dynamic action of blowing the gas also is effective in removal, above and beyond that, as explained above, it is believed that these are efficiently removed by the superposed chemical effect due to the concentration of the pickling solution deposited at the surface.
  • the concentrated pickling solution concentrates at the interface of the steel sheet and oxide scale due to the surface tension to selectively dissolve it the more the solution evaporates. This is believed because there is a concentrated layer of Si oxides at the interface of the steel sheet and oxide scale, so removal of the Si oxides is promoted and, accordingly, the efficiency of removal of the oxide scale is increasingly improved.
  • the gel-like Si oxides and the interface of the oxide scale and the surface of the steel sheet are selectively dissolved whereby removal of Si oxides is promoted.
  • the Si oxides interfering with the removal of the oxide scale are efficiently removed as explained above, so if the steel sheet is again immersed in the pickling solution, the oxide scale is also efficiently removed. That is, the dissolution speed of the oxide scale is improved. This has a large effect when the Si oxides are gel-like.
  • the effect of improvement of the pickling efficiency is remarkable in steel sheet with a content of Si of 0.1 to 3.5 mass%. If the content of Si contained in the steel sheet becomes 0.1 mass% or more, a layer where Si oxides concentrate is easily formed, so a remarkable effect of improvement of the pickling efficiency is obtained. If the content of Si increases, the effect of improvement of the pickling efficiency becomes greater, but if the content of Si contained in the steel sheet exceeds 3.5 mass%, no further improvement in the pickling efficiency is seen any longer and the efficiency remains constant.
  • FIG. 3 schematically shows an enlarged view of blowing gas to the surface of the steel sheet (only one surface shown).
  • FIG. 3 schematically shows the case where the surface of the steel sheet has an oxide scale layer 6 and where, between the oxide scale layer 6 and the steel sheet 2, there is a layer 7 where Si oxides are concentrated.
  • the Si oxides pass once through the pickling tank, so are dissolving. At this time, as shown in FIG. 3 , blowing the gas slanted with respect to the surface of the steel sheet makes it directly strike the interface between the oxide scale layer and steel sheet, so a sufficient effect is obtained. If the angle ⁇ is less than 1°, even if raising the gas blowing pressure, the gas striking the surface of the steel sheet disperses, so the gas will not strike the surface of the steel sheet with a sufficiently high pressure in some cases. If the angle ⁇ exceeds 75°, the blown gas will increasingly no longer directly strike the interface of the oxide scale layer and steel sheet and the above effect will no longer be sufficiently obtained in some cases.
  • the means for blowing the gas may use any method, but for example the method of using a blower, nozzle, etc. may be mentioned. In particular, it is preferable to use a nozzle to blow the gas.
  • the angle ⁇ is preferably 10° to 60°. More preferably, to make the blown gas concentrate at the interface between the oxide scale layer and steel sheet, the angle ⁇ is preferably made 15° to 45°.
  • the width of the blowing nozzle port shown in FIG. 3 is preferably at least the width of the surface of the steel sheet.
  • the nozzle port may be a slit in the width direction or independent nozzle ports may be aligned in the width direction. Further, as shown in FIG. 6 , it is also possible to make the nozzle port swing in a plane parallel to the surface of the steel sheet.
  • FIG. 1 and FIG. 2 show one gas blowing nozzle 1 arranged at each of the two surfaces of the steel sheet, but there is no need to limit the gas blowing nozzles to one for each surface of the steel sheet.
  • FIG. 5 it is also possible to arrange two or more gas blowing nozzles in the direction of movement of the steel sheet and blow gas in multiple stages. By using multistage gas blowing nozzles, it is possible to remove the oxide scale more efficiently.
  • a gas blowing nozzle is preferably provided at each of the two surfaces of the steel sheet, but may also be provided at only one surface. Of course, there is no need to simultaneously blow the gas at the two surfaces. It is also possible to blow the gas alternately at one surface at a time.
  • the angle ⁇ formed by the nozzle gas blowing direction and the surface of the steel sheet is preferably variable. For example, when the speed of movement of the steel sheet is large, even if making the angle ⁇ large, a sufficient gas blowing effect is obtained, but when the speed of movement of the steel sheet is small, the angle ⁇ may be reduced to obtain a sufficient gas blowing effect. Therefore, it is possible to make the angle variable in accordance with the speed of movement of the steel sheet.
  • the gas is blown at the surface of the steel sheet, so, for example, as shown in FIG. 1 , it may be considered to use a single pickling tank to pickle the steel sheet, take out the pickled steel sheet once from the pickling tank and blow gas at it, and further use the same pickling tank for repeat pickling.
  • a plurality of pickling tanks may be arranged in a line to form a pickling facility ( FIG. 2 shows an example of two pickling tanks) and a steel sheet pickled between one tank and another may be taken out from the pickling tank once and gas blown at it.
  • FIG. 4 schematically shows a pickling facility used to achieve the present invention.
  • the gas used in the present invention is not particularly limited, but for example, air, nitrogen, argon, or another gas may be used. Further, mixed gases of these may also be used.
  • the pressure of the blown gas at the blowing port may be made 0.5 to 1.0 MPa or more to obtain the effect of the present invention. If less than 0.5 MPa, the pickling speed sometimes cannot be improved. Further, the reason why the upper limit is defined as 1.0 MPa is that if blowing gas over 1.0 MPa, the facilities relating to the pressurizing system become larger in size and the economic effect cannot be obtained in some cases.
  • the gas blowing nozzle port is preferably a distance of 2 cm to 80 cm from the surface of the steel sheet. Therefore, when inclining the gas blowing nozzle port, the distance becomes the shortest straight line distance between the gas blowing nozzle port and the surface of the steel sheet multiplied by 1/sin ⁇ . If less than 2 cm, vibration of the running steel sheet causes contact with the gas blowing nozzle port. If over 80 cm, the gas blown toward the surface of the steel sheet sometimes will not sufficiently reach the surface of the steel sheet. While depending on the state of the peripheral facilities etc., with a distance of 5 cm to 30 cm, a high effect can be obtained.
  • the pickling solution of the pickling tank used to achieve the present invention is a pickling solution for removing ordinary oxide scale.
  • a pickling solution for removing ordinary oxide scale for example, an aqueous hydrochloric acid solution, aqueous sulfuric acid solution, aqueous fluoric acid solution (hydrofluoric acid), or aqueous solutions of these solutions further containing nitric acid, acetic acid, formic acid, etc. may be used.
  • the concentration of the acid of the pickling solution is not particularly limited, but is 2 mass% to 20 mass% in range. If less than 2 mass%, a sufficient speed of dissolution of the oxide scale sometimes cannot be obtained. If over 20 mass%, the pickling tank becomes remarkably corroded in some cases or the rinse tank has to be made larger in some cases.
  • the pickling solution may have Fe 2+ ions added to it.
  • the concentration of Fe 2+ ions is more preferably 30 to 150 g/L. If less than 30 g/L, stable pickling is not possible in some cases. If over 150 g/L, the pickling speed becomes slower in some cases. Further, the pickling solution may also have Fe 3+ ions added to it.
  • the temperature of the pickling solution is not particularly limited, but for the pickling efficiency, temperature control, or other reasons, ordinary temperature to 97°C is preferable.
  • the speed of movement of the steel sheet at the gas blowing part of the present invention is not particularly limited, but is preferably 50 m/min to 400 m/min. If less than 50 m/min, the productivity (pickling efficiency) becomes lower in some cases. If over 400 m/min, the effect of improvement of the pickling efficiency by the blowing of a gas sometimes can no longer be obtained.
  • the steel sheet running speed is particularly preferably 100 m/min to 200 m/min.
  • the inventors used an aqueous HCl solution as the pickling solution and adjusted and controlled it during operation to give hydrochloric acid within the range of 6 to 9 mass%. Furthermore, they added FeCl 2 so that the Fe 2+ in the solution became 80 g/L. Further, for Fe 3+ as well, in the same way, the inventors added FeCl 3 so that the Fe 3+ in the solution became 1 g/L. They warmed the pickling solution to a temperature of 70°C ( ⁇ 5°C).
  • the inventors changed the running speed (movement speed) of the steel sheet and measured the pickling time for the area ratio of removal of oxide scale to reach 90%.
  • a case where the pickling time for the area ratio of removal of oxide scale to reach 90% or more exceeded 35 seconds was evaluated as "poor", a case of 30 to 35 seconds as "fair”, a case of 25 to 30 seconds as "good”, and a case of within 25 seconds as "very good”.
  • Table 1 shows the results of evaluation. Compared with the case of not blowing gas, blowing gas to the surface of the steel sheet during the pickling process enabled the pickling time to be shortened. For the gas blowing angle, a range of 1° to 75° was more superior for improvement of the pickling efficiency. Further, with a pressure of the gas at the blowing port in the range of 0.5 to 1.0 MPa, the pickling efficiency was higher. The effect of gas blowing appeared remarkably in steel sheet containing 0.1 to 3.6 mass% of Si. Table 1 Si content of steel sheet (mass%) Type of gas Gas pressure at blowing port (MPa) Blowing angle ⁇ (°) Evaluation of pickling time Inv. Ex. 1 0.3 Argon 0.5 60 Very good Inv. Ex.
  • Example 2 In the same way as Example 1, the inventors used test steel sheets containing C, Mn, S, and Nb and containing Si shown in Table 2 and blew a gas between the two pickling tanks shown in FIG. 2 for pickling.
  • the pickling solutions of the two pickling tanks are the same as in Example 1.
  • the temperature of the pickling solution was made 75°C ( ⁇ 5°C) by warming.
  • the method of evaluation is the same as in Example 1.
  • Table 2 shows the results of evaluation. Compared with when not blowing gas, blowing gas to the surface of the steel sheet during the pickling process enabled the pickling time to be shortened. Regarding the blowing angle of the gas, a range of 1° to 75° was better for improvement of the pickling efficiency. Further, with a pressure of the gas at the blowing port of 0.5 to 1.0 MPa in range, the pickling efficiency was higher.
  • the present invention can be utilized in the iron and steel industry. According to the present invention, it becomes possible to efficiently remove oxide scale of steel sheet.
  • the steel sheet after pickling process obtained by the present invention has a clean surface free of pickling scars. Due to this, it is possible to strikingly improve the productivity of hot rolled steel sheet, in particular automobile steel sheet and other high strength steel sheet. The inventors are confident that this can contribute to the supply of good quality, low cost steel sheet.

Claims (4)

  1. Procédé de décapage pour éliminer la calamine d'une tôle d'acier (2) ayant une teneur en Si de 0,1 à 3,5 % en masse, caractérisé par le fait qu'il comporte une étape A de décapage de la tôle d'acier (2) à l'aide d'une solution de décapage dans un bac de décapage (3,4), une étape B consistant à retirer la tôle d'acier (2) du bac de décapage (3, 4) puis à souffler un gaz vers au moins une partie des surfaces de la tôle d'acier (2) dans l'air après ladite étape A de manière à ce que la solution de décapage déposée sur la surface de la tôle d'acier (2) au niveau de la partie ayant reçu le gaz soufflé s'évapore partiellement et à ce que sa concentration en acide devienne supérieure en laissant la solution de décapage déposée rester à la surface de la tôle d'acier pour être concentrée, et une étape C de décapage de ladite tôle d'acier (2) ensuite après ladite étape B, dans lequel un angle θ (°) formé entre une direction de soufflage dudit gaz et au moins une partie des surfaces de la tôle d'acier (2) est 1° ≤ θ ≤ 75°.
  2. Procédé de décapage d'une tôle d'acier selon la revendication 1, caractérisé par le soufflage dudit gaz à l'opposé d'une direction de mouvement de la tôle d'acier (2).
  3. Procédé de décapage d'une tôle d'acier selon la revendication 1 ou 2, caractérisé en ce qu'une pression de soufflage dudit gaz est de 0,5 à 1,0 MPa.
  4. Procédé de décapage d'une tôle d'acier selon l'une quelconque des revendications 1 à 3, caractérisé en ce que le décapage de ladite étape A est réalisé dans un premier bac de décapage (4) et le décapage de ladite étape C est réalisé dans un second bac de décapage (5).
EP09754861.4A 2008-05-30 2009-05-28 Procédé de décapage pour des tôles d'acier Active EP2302102B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2008143582 2008-05-30
PCT/JP2009/060205 WO2009145353A1 (fr) 2008-05-30 2009-05-28 Procédé de décapage pour tôles d’acier et appareil de décapage

Publications (3)

Publication Number Publication Date
EP2302102A1 EP2302102A1 (fr) 2011-03-30
EP2302102A4 EP2302102A4 (fr) 2015-07-15
EP2302102B1 true EP2302102B1 (fr) 2017-11-15

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EP09754861.4A Active EP2302102B1 (fr) 2008-05-30 2009-05-28 Procédé de décapage pour des tôles d'acier

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US (1) US20110079244A1 (fr)
EP (1) EP2302102B1 (fr)
JP (1) JP4714800B2 (fr)
KR (1) KR101249167B1 (fr)
CN (1) CN102046850B (fr)
BR (1) BRPI0913196B1 (fr)
WO (1) WO2009145353A1 (fr)

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EP2806051B1 (fr) * 2012-01-18 2016-04-06 JFE Steel Corporation Procédé pour empêcher la coloration jaune indésirée de la surface d'une feuille d'acier nettoyée par acide
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JP6979516B2 (ja) * 2018-04-16 2021-12-15 Ｐｒｉｍｅｔａｌｓ Ｔｅｃｈｎｏｌｏｇｉｅｓ Ｊａｐａｎ株式会社 酸洗設備及び酸洗設備の運転方法
CN111472009A (zh) * 2020-04-30 2020-07-31 苏州强新合金材料科技有限公司 一种钢类线材的拉拔除锈工艺
CN114101384B (zh) * 2020-08-31 2024-01-09 宝山钢铁股份有限公司 板带焊缝过平整机和张紧辊时的张紧力控制方法
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Publication number Publication date
JP4714800B2 (ja) 2011-06-29
BRPI0913196B1 (pt) 2019-04-16
JPWO2009145353A1 (ja) 2011-10-20
KR20110003556A (ko) 2011-01-12
WO2009145353A1 (fr) 2009-12-03
US20110079244A1 (en) 2011-04-07
EP2302102A4 (fr) 2015-07-15
CN102046850A (zh) 2011-05-04
EP2302102A1 (fr) 2011-03-30
CN102046850B (zh) 2014-01-29
BRPI0913196A2 (pt) 2016-01-12
KR101249167B1 (ko) 2013-03-29

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