WO2021058044A1 - Sélection automatique de durée de décapage - Google Patents

Sélection automatique de durée de décapage Download PDF

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Publication number
WO2021058044A1
WO2021058044A1 PCT/DE2019/100853 DE2019100853W WO2021058044A1 WO 2021058044 A1 WO2021058044 A1 WO 2021058044A1 DE 2019100853 W DE2019100853 W DE 2019100853W WO 2021058044 A1 WO2021058044 A1 WO 2021058044A1
Authority
WO
WIPO (PCT)
Prior art keywords
pickling
workpieces
temperature
time
pickled
Prior art date
Application number
PCT/DE2019/100853
Other languages
German (de)
English (en)
Inventor
Martin PEESEL
Friedrich-Werner Siedentop
Original Assignee
Siedentop Gmbh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Siedentop Gmbh filed Critical Siedentop Gmbh
Priority to EP19791167.0A priority Critical patent/EP4034873A1/fr
Priority to PCT/DE2019/100853 priority patent/WO2021058044A1/fr
Publication of WO2021058044A1 publication Critical patent/WO2021058044A1/fr

Links

Classifications

    • 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
    • C23G1/086—Iron or steel solutions containing HF
    • 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
    • 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

Definitions

  • the invention relates to a pickling process for pickling workpieces made of steel, in particular stainless steel, in batch operation, in which a pickling agent containing hydrofluoric acid is sprayed from a pickling agent tank onto the workpieces held in a pickling cabin, with a desired
  • the invention also relates to a pickling system for pickling workpieces made of steel, in particular stainless steel, in batch operation, in which a pickling agent containing hydrofluoric acid is sprayed from a pickling agent tank onto the workpieces held in a pickling cabin, with for
  • a suitable pickling time must be selected to achieve a desired pickling effect on the surfaces of the workpieces to be pickled.
  • Pickling processes and systems in which the workpieces to be pickled are placed in a pickling cabin in batch operation and are sprayed with a pickling agent containing hydrofluoric acid with the pickling cabin closed, are known, for example, from EP 1 477583 B1.
  • the pickling agent containing hydrofluoric acid is fed from the pickling agent tank to the spray nozzles in the pickling booth by means of a controllable pump.
  • the pickling agent is then sprayed onto the workpieces to be pickled and runs down the workpieces due to gravity, where a corresponding collecting basin for returning the pickling agent to the pickling agent tank is arranged in the pickling cabin.
  • Pickling is known when processing metals, especially precious metals, such as so-called VA steel (stainless steel), since a metal oxide layer or scale layer is often formed on its surface, which affects both the appearance and the possible further processing of the material . In the case of stainless steel, this undesirable layer adheres very firmly to the surface, so that aggressive acids are used for pickling.
  • a common pickling acid mixture is nitric acid and hydrofluoric acid, which is used in aqueous solution. In this so-called spray pickling process, the amount of acid used can be significantly reduced by fine spraying, so that the necessary permits for such systems can be obtained more easily. It is also known from EP 1 477 583 B1 to use pickling agents made solely from hydrofluoric acid in aqueous solution, that is to say to dispense with the addition of nitric acid. This makes it easier to comply with environmental protection regulations.
  • the pickling time that is to say the exposure time of the pickling agent sprayed on during the pickling time. So far, the pickling time for such spray pickling processes has been selected by the plant operator based on empirical values. It is important that the oxides are completely removed during the pickling process in order to remove all discoloration of the edge zones and tarnishing from the workpiece surface. A material removal of approx. 1 to 3 pm is achieved. After a successful pickling process, the stainless steel surface is completely bare and no longer shows any discoloration or residue. This pure surface is then protected again in the atmosphere by oxidizing the chromium particles on the surface of the stainless steel.
  • a pickling time that is too short is selected, unwanted discoloration of the edge zones and tarnishing or other residues can remain on the surface, so that the finished workpiece does not have the desired surface quality and purity. If, on the other hand, the pickling time is chosen too long, there is likely to be an undesirably high material removal and, in addition, too long a process time and thus a reduced material throughput at the pickling plant.
  • the object of the invention is therefore to design a known pickling process or such a pickling plant in such a way that a suitable pickling time is selected automatically. This object is achieved with a pickling process according to claim 1 and a pickling plant according to claim 11.
  • a direct, automated assignment of the suitable pickling time is determined from the most important parameter for the pickling time to be selected, namely the temperature of the pickling agent to be sprayed on. For example, a fixed pickling time is assigned to each pickling temperature or to each pickling temperature range, for example in degree increments. This can be done via an evaluation and control unit in which suitable pickling times are stored for the temperature ranges or a corresponding algorithm is available from which the suitable pickling time is determined.
  • the temperature of the workpieces to be pickled is preferably measured when they are placed in the pickling cabin and the suitable pickling time is derived from this. This makes it possible for a correction value to be added to or subtracted from the pickling time in the event of greater temperature differences between the workpieces to be pickled in the pickling booth and the temperature of the pickling agent.
  • the temperature of the ambient air in the pickling cabin is measured and the suitable pickling time is derived from this. Since the pickling booth also contains a considerable volume of air, especially for large, bulky workpieces, this should also be taken into account when calculating the pickling time. If there are major differences between the temperature of the ambient air and the temperature of the pickling agent, corresponding correction amounts must be added to or deducted from the pickling time.
  • both the workpieces to be pickled by spraying with the possibly heated pickling agent and those in the pickling cabin during loading with the to be bitten Workpieces exchanged and cooled ambient air must be warmed up. Accordingly, the sprayed pickling agent cools down considerably, so that a significant increase in the pickling time is necessary.
  • the total heat capacity of the workpieces to be pickled in the pickling booth can also be used when calculating the pickling time to be selected, especially in connection with the correspondingly measured Temperatures for the workpieces to be pickled and the pickling agent used can be determined.
  • the hydrofluoric acid concentration of the pickling agent is measured and taken into account when calculating the pickling time, an increase in the concentration of the pickling agent can occur when the pickling agent is diluted, for example due to the entry of moisture from wet workpieces to be pickled or particularly moist ambient air (precipitation) or with partial evaporation be taken into account when calculating the pickling time.
  • the pickling time is automatically reduced, while with a lower hydrofluoric acid concentration the pickling time is extended.
  • the material of the workpieces to be pickled is determined when it is placed in the pickling booth and taken into account when calculating the pickling time, the material of the workpieces to be pickled can be checked using measurements, thus ensuring a quality control of the respective pickling order and an adjustment of the pickling time to the respective material can be automated .
  • a stainless steel with the material number 1.4301 can be processed with a shorter pickling time than, for example, a material 1.4429.
  • material analysis devices are known which are designed, for example, as laser pistols and which determine the material using optical evaluation methods.
  • the pickling time can also be adapted to the material thickness of the workpieces to be pickled, since thin-walled workpieces are very large in relation to their weight
  • the surface will quickly adapt to the ambient temperature and the temperature of the pickling agent and very massive workpieces, in which the temperature of the workpiece on its surface will only slowly adapt to the temperature of the environment and the temperature of the pickling agent, are taken into account.
  • model calculations or analytical equations for temperature adjustment on the surface can be derived and used to calculate the pickling time.
  • a pickling factor is determined and taken into account when calculating the pickling time so that the individual wishes of the respective customer can also be taken into account when selecting the automatic pickling time.
  • the pickling factor indicates, as it were, whether normal pickling, strong pickling or removal pickling is desired by the customer.
  • the automatically determined pickling time is adjusted accordingly, taking into account the selected pickling factor.
  • V 2 with a conventional pickling time of 30 min
  • V 8 with a conventional pickling time of 120 min;
  • T w temperature of the workpieces to be pickled
  • T R temperature of the ambient air in the pickling cabin
  • T B temperature of the pickling
  • the pickling time is based on the measured values for the material thickness of the workpiece to be pickled, the measured temperatures of the pickling agent, the ambient air in the pickling cabin and the pickling agent temperature with the corresponding factors derived from the measured values are calculated as the pickling time to be applied in hours.
  • extrapolation is made for intermediate values.
  • the pickling system contains at least three temperature sensors, namely a first temperature sensor for determining the temperature of the pickling agent in the pickling agent tank or in a feed line to the spray nozzles in the pickling cabin, a second temperature sensor for determining the temperature of the workpieces to be pickled and a third temperature sensor for determining the temperature the ambient air in the pickling booth, the first, second and third temperature sensors being operatively connected to an evaluation and control unit in order to determine or calculate the suitable pickling time.
  • the essential temperature-related influences on the pickling result can be taken into account using a relatively simple sensor system with a connected evaluation and control unit, and the appropriate pickling time can be determined from this.
  • a scale is provided in the feed of the workpieces to be pickled.
  • the workpieces to be pickled can for example be hung on or on mobile racks, in which case these mobile racks, which remain in the pickling booth, also have to be measured accordingly.
  • an analysis device for measuring the hydrofluoric acid concentration of the pickling agent is arranged in the pickling agent tank or in a feed line to spray nozzles in the pickling cabin.
  • a stainless steel workpiece made of 2 mm stainless steel sheet of the quality 1.4301 is processed with a hydrofluoric acid pickle in a pickling cabin by spray pickling.
  • the pickling time required for this workpiece is calculated according to the invention using the formula according to claim 9.
  • a pickling time of 30 minutes is usually used according to a conventional choice based on experience with pickling agents. Accordingly, the quality factor has to be assigned 2.
  • the temperature is automatically recorded with an infrared surface temperature measuring device when the workpiece to be pickled is placed in the pickling cabin.
  • a total pickling time of t B 3.24 h is thus calculated.
  • the workpiece to be pickled is hooked into the pickling cabin and pickled for 3% hours under the aforementioned conditions. Due to the values measured and transferred to the system control, the pickling result always corresponds to the desired degree of pickling and is also below different boundary conditions, in particular other temperatures, a slightly lower or higher hydrofluoric acid concentration in the pickling agent and the like are always comparable. Due to the measured boundary conditions and the correspondingly assigned factors, the correct pickling time can always be used. It is preferred that the measured values are transmitted directly to a control unit in which the calculation mode and the associated factors are stored, so that the correct pickling time is always carried out automatically on the pickling device.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

L'invention concerne un procédé de décapage conçu pour décaper des pièces en acier, en particulier en acier inoxydable, lors d'un processus discontinu, un agent décapant comportant de l'acide flurohydrique étant prélevé d'un réservoir d'agent décapant et pulvérisé sur les pièces maintenues dans une cabine de décapage, une durée de décapage (tB) adaptée étant sélectionnée pour obtenir un effet décapant souhaité à la surface de la pièce à décaper. Ce procédé est caractérisée en ce que la température de l'agent décapant (TB) est mesurée et la durée de décapage (tB) adaptée est déterminée à partir du résultat de mesure. L'invention concerne en outre une installation de décapage servant à décaper des pièces en acier, en particulier en acier inoxydable, lors d'un processus discontinu, un agent décapant comportant de l'acide flurohydrique étant prélevé d'un réservoir d'agent décapant et pulvérisé sur les pièces maintenues dans une cabine de décapage, une durée de décapage adaptée étant sélectionnée pour obtenir un effet décapant souhaité à la surface de la pièce à décaper. Cette installation est caractérisée en ce qu'un premier capteur de température conçu pour déterminer la température de l'agent décapant dans le réservoir d'agent décapant ou dans une conduite vers des buses de pulvérisation dans la cabine de décapage, un deuxième capteur de température conçu pour déterminer la température des pièces à décaper et un troisième capteur de température conçu pour déterminer la température de l'air ambiant dans la cabine de décapage sont prévus, le premier, le deuxième et le troisième capteur de température étant reliés de manière fonctionnelle à une unité d'évaluation et de commande pour déterminer ou calculer le temps de décapage adapté.
PCT/DE2019/100853 2019-09-26 2019-09-26 Sélection automatique de durée de décapage WO2021058044A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP19791167.0A EP4034873A1 (fr) 2019-09-26 2019-09-26 Sélection automatique de durée de décapage
PCT/DE2019/100853 WO2021058044A1 (fr) 2019-09-26 2019-09-26 Sélection automatique de durée de décapage

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/DE2019/100853 WO2021058044A1 (fr) 2019-09-26 2019-09-26 Sélection automatique de durée de décapage

Publications (1)

Publication Number Publication Date
WO2021058044A1 true WO2021058044A1 (fr) 2021-04-01

Family

ID=68318755

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE2019/100853 WO2021058044A1 (fr) 2019-09-26 2019-09-26 Sélection automatique de durée de décapage

Country Status (2)

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EP (1) EP4034873A1 (fr)
WO (1) WO2021058044A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115044917A (zh) * 2022-06-21 2022-09-13 北京首钢冷轧薄板有限公司 热轧带钢酸洗速度确定方法及装置

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0776993A1 (fr) * 1995-11-28 1997-06-04 Eka Chemicals AB Procédé de décapage d'acier
EP1106713A2 (fr) * 1999-12-08 2001-06-13 Siemens Aktiengesellschaft Méthode pour déterminer le temps de décapage d'une bande métallique couvert de calamine
US6396280B1 (en) * 1997-11-06 2002-05-28 Sumitomo Metal Industries, Ltd. Method and apparatus for measurement and automatic control of acid concentration
EP1477583B1 (fr) 2003-05-13 2007-10-17 Siedentop GmbH Appareil et procédé pour le décapage des matériaux en acier

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0776993A1 (fr) * 1995-11-28 1997-06-04 Eka Chemicals AB Procédé de décapage d'acier
US6396280B1 (en) * 1997-11-06 2002-05-28 Sumitomo Metal Industries, Ltd. Method and apparatus for measurement and automatic control of acid concentration
EP1106713A2 (fr) * 1999-12-08 2001-06-13 Siemens Aktiengesellschaft Méthode pour déterminer le temps de décapage d'une bande métallique couvert de calamine
EP1477583B1 (fr) 2003-05-13 2007-10-17 Siedentop GmbH Appareil et procédé pour le décapage des matériaux en acier

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115044917A (zh) * 2022-06-21 2022-09-13 北京首钢冷轧薄板有限公司 热轧带钢酸洗速度确定方法及装置
CN115044917B (zh) * 2022-06-21 2023-10-03 北京首钢冷轧薄板有限公司 热轧带钢酸洗速度确定方法及装置

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Publication number Publication date
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