KR0135347B1 - Acid pickling solution for the drawn sheet of electric steel - Google Patents
Acid pickling solution for the drawn sheet of electric steelInfo
- Publication number
- KR0135347B1 KR0135347B1 KR1019940034863A KR19940034863A KR0135347B1 KR 0135347 B1 KR0135347 B1 KR 0135347B1 KR 1019940034863 A KR1019940034863 A KR 1019940034863A KR 19940034863 A KR19940034863 A KR 19940034863A KR 0135347 B1 KR0135347 B1 KR 0135347B1
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- South Korea
- Prior art keywords
- pickling
- hydrochloric acid
- acid solution
- solution
- added
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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
- 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
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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
- 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
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
- C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
- C23G1/061—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors nitrogen-containing compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
- B21B45/04—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for de-scaling, e.g. by brushing
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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
본 발명은 산세용액중에 산세척촉진제를 적절히 첨가하여 산세척효과의 극대화로 색상편차의 발생을 방지할 수 있는 전기강판용 압연재의 산세액을 제공하기 위하여 농도 12∼15%의 염산 용액(HCl+H2O)과, 이 염산용액에 염산용액의 0.1∼0.2%로 첨가되는 산세촉진제(RSH2)와, 순수염산의 0.2∼0.4%로 상기 염산용액에 첨가되는 산세억제제(RNH2)로 조성됨을 특징으로 한다.The present invention is a hydrochloric acid solution (HCl +) having a concentration of 12 to 15% in order to provide a pickling solution of a rolled material for electrical steel sheet which can prevent the occurrence of color deviation by maximizing the pickling effect by properly adding a pickling accelerator to the pickling solution. H 2 O), a pickling accelerator (RSH 2 ) added to the hydrochloric acid solution at 0.1 to 0.2% of hydrochloric acid solution, and a pickling inhibitor (RNH 2 ) added to the hydrochloric acid solution at 0.2 to 0.4% of pure hydrochloric acid solution. It is characterized by.
Description
제1도는 압연강판의 표면에 발생되는 일반적인 스케일의 구성을 도시한 도면,1 is a view showing the configuration of a general scale generated on the surface of the rolled steel sheet,
제2도는 산세촉진제가 첨가된 산세액의 산세척면 상태를 나타내는 사진이며,2 is a photograph showing the pickling state of the pickling solution to which the pickling accelerator is added.
제3도는 산세촉진제와 산세억제제가 첨가된 산세액의 산세척면 상태를 나타내는 사진이다.3 is a photograph showing the pickling state of the pickling solution to which the pickling accelerator and the pickling inhibitor are added.
＊도면의 주요부분에 대한 부호의 설명＊ Explanation of symbols for main parts of drawing
2:Fe 층4:FeSiO4화합물층2: Fe layer 4: FeSiO 4 compound layer
6:FeO 층8:Fe3O4층6: FeO layer 8: Fe 3 O 4 layer
10:Fe2O3층10: Fe 2 O 3 layer
본 발명은 전기강판용 압연재의 산세액에 관한 것으로, 보다 상세하게는 전기강판의 제조 공정에서 산세척 효과를 극대화하여 전기강판용 압연재의 색상 편차를 제거할 수 있는 전기강판용 압연재의 산세액에 관한 것이다.The present invention relates to a pickling liquid of a rolled sheet for electrical steel, and more particularly, to a pickling liquid of a rolled sheet for rolled electrical steel that can remove color variations of the rolled sheet for electrical steel by maximizing the pickling effect in the manufacturing process of the electrical steel sheet. It is about.
일반적으로 변압기와 회전기기등과 같은 전기기기의 철심재로 사용되는 전기강판은 제강 및 열간압연을 거쳐 판재로 압연되고 압연재를 예비 소둔과 산세 공정, 그리고 탈탄 소둔 공정과 절연 피막의 코팅 공정 등을 통해 제조된다.In general, electric steel sheets used as iron cores of electrical equipment such as transformers and rotary machines are rolled into sheet materials through steelmaking and hot rolling, and the rolled materials are preannealed and pickled, decarburized annealing and coating of insulating film, etc. It is manufactured through.
이와 같은 제조 공정중의 전기강판은 보통 고온에서 철 성분이 공기중의 산소 및 기타 가스와 반응하여 그 표면에 산화물 스케일이 생성된다.In such manufacturing processes, electrical steel sheets usually react with oxygen and other gases in the air at high temperatures to produce oxide scale on their surfaces.
이와 같은 스케일은 보통 FeO, Fe2O3, Fe3O4등의 3종이 강판 표면에 FeO -Fe3O4-Fe2O3등의 순서로 형성되며, 온도에 따라 그 생성 비율이 달라지는데, 약 580℃에서 생성되는 스케일은 대부분 FeO 층으로 구성된다.Such scale is usually formed in the order of FeO, Fe 2 O 3 , Fe 3 O 4 , etc. in the order of FeO -Fe 3 O 4 -Fe 2 O 3 on the surface of the steel sheet, the production rate varies depending on the temperature, The scale produced at about 580 ° C. consists mostly of FeO layers.
또, 0.4∼3.5 중량% 전기강판에 함유된 실리콘(Si) 성분은 산소와 반응하여 FeSiO4(Fayalite) 화합물인 스케일이 생성되는데, 이러한 FeSiO4화합물은 모재의 산화 속도를 저하시키지만 융점이 1170℃로 비교적 낮기 때문에 열처리 도중에 용융되어 오히려 모재의 산화 분위기를 형성한다.In addition, 0.4 to 3.5 silicon (Si) component contained in the electrical steel is by weight%, there is a scale of FeSiO 4 (Fayalite) compound by reaction with oxygen to produce, such FeSiO 4 compounds having a melting point of 1170 ℃ but decreases the rate of oxidation of the base material As it is relatively low, it melts during heat treatment and rather forms an oxidizing atmosphere of the base material.
한편, 산세 공정을 통해 열간압연 또는 냉간압연된 압연재의 표면에 생성되는 스케일을 제거하고 있는데, 이러한 산세 공정은 쇼트 블라스터(Shot Blastor)에 의해 일차적으로 기계적인 스케일을 제거한후, 산세액의 종류와 온도 및 농도 등에 따라 압연재의 산세 특성과 표면 색상에 영향을 미친다.On the other hand, the pickling process is removing the scale generated on the surface of the hot-rolled or cold-rolled rolled material, this pickling process after removing the mechanical scale primarily by Shot Blastor, the type of pickling liquid Pickling properties and surface color of rolled materials are affected by temperature and concentration.
상기 설명한 산세액으로는 산화촉진제를 첨가한 염산을 주로 사용하는데, 이와 같은 염산은 스케일의 틈새로 침투하여 스케일 하층에 존재하는 산용해도가 높은 FeO와 반응하여 염화철을 생성하고, 그리고 Fe와 반응하여 수소 가스를 생성함으로써 스케일의 박리를 촉진한다.As the pickling solution described above, hydrochloric acid added with an oxidation promoter is mainly used. Such hydrochloric acid penetrates into the gaps of the scale to react with high acid solubility FeO present in the lower layer of the scale to produce iron chloride, and react with Fe. By generating hydrogen gas, peeling off of the scale is promoted.
이때의 반응식은 다음과 같다.The reaction scheme at this time is as follows.
Fe2O3+ 4HCl → 2FeCl2+ 2H2O + ½O2↑,Fe 2 O 3 + 4HCl → 2FeCl 2 + 2H 2 O + ½O 2 ↑,
Fe3O4+ 6HCl → 2FeCl2+ 3H2O + ½O2↑,Fe 3 O 4 + 6HCl → 2FeCl 2 + 3H 2 O + ½O 2 ↑,
FeO + 2HCl → FeCl2+ H2O,FeO + 2HCl → FeCl 2 + H 2 O,
Fe + 2HCl → FeCl2+ H2↑Fe + 2HCl → FeCl 2 + H 2 ↑
이와 같은 염산의 스케일 박리 작용은 스케일의 다소에 영향을 받게 되며, 염산에 첨가되어 FeO, Fe2O3, Fe3O4로 존재하는 스케일중의 O-2와 산세 용액중의 수소 이온과 반응하는 산세촉진제(RSH)에 의해 그 반응 속도가 가속되면서 스케일의 제거가 이루어진다.The scale peeling effect of hydrochloric acid is affected by the scale somewhat, and reacts with O -2 in the scale which is added to hydrochloric acid and is present as FeO, Fe 2 O 3 , Fe 3 O 4 and hydrogen ions in the pickling solution. The pickling accelerator (RSH) is accelerated by the reaction rate to remove the scale.
이때, 산세촉진제(RSH)에 의한 스케일 제거 반응은 다음과 같이 일어난다.At this time, the descaling reaction by the pickling accelerator (RSH) occurs as follows.
RSH + (FeO, Fe2O3, Fe3O4) → (RS)2Fe + H2ORSH + (FeO, Fe 2 O 3 , Fe 3 O 4 ) → (RS) 2 Fe + H 2 O
(R : 알킬기, C1∼C10)(R: alkyl group, C 1 to C 10 )
즉, 스케일의 수소 이온과 반응하는 반응 촉진 인자는 RS-2의 활동도(Activity)에 영향을 받고, 산소 이온은 RS-2+ H+의 활성화와 별도로 염산의 수소 이온을 활성화시켜 스케일의 박리를 촉진시킨다.That is, the reaction facilitating factor that reacts with the hydrogen ions of the scale is affected by the activity of RS -2 , and the oxygen ions activate the hydrogen ions of hydrochloric acid separately from the activation of RS -2 + H + to exfoliate the scale. To promote.
그런데 이와 같이 염산에 산세촉진제를 첨가하여 스케일의 박리를 촉진하는 종래의 전기강판용 압연재의 산세액은 스케일 제거 효과는 높일 수 있으나 산세촉진제가 과량 첨가되었을 때 전기강판 표면에 탄소 석출물을 생성하여 전기강판의 표면을 검은색으로 얼룩지게 하는 원인이 되기 때문에 염산중에 적량의 산세촉진제를 조정 상태로 첨가한 전기강판용 압연재의 산세액이 요구되는 상황이다.However, the pickling solution of the conventional rolled roll for electrical steel, which promotes peeling off the scale by adding a pickling accelerator to hydrochloric acid, can increase the scale removing effect, but when an excessive amount of pickling accelerator is added, carbon precipitates are generated on the surface of the steel sheet. Since the surface of the steel sheet is stained black, the pickling liquid of the rolled material for rolled electrical steel sheet in which hydrochloric acid is added with an appropriate amount of a pickling accelerator in an adjusted state is required.
본 발명은 상기와 같은 종래 기술의 문제점을 해결하기 위하여 이루어진 것으로, 산세촉진제를 농도를 조절하여 첨가하여 산세촉진제의 과다 첨가를 방지하고, 염산의 농도를 적절히 유지하여 전기강판용 압연재의 제조시 산세척 효과를 극대화함으로써 압연재의 색상 편차를 방지할 수 있는 전기강판용 압연재의 산세액을 제공하는데 그 목적이 있다.The present invention has been made to solve the problems of the prior art as described above, by adding a pickling accelerator by adjusting the concentration to prevent excessive addition of pickling accelerator, and maintain the concentration of hydrochloric acid properly to produce acid in the production of rolled material for electrical steel sheet The purpose of the present invention is to provide a pickling solution for rolling materials for electrical steel sheet which can prevent color variation of the rolling material by maximizing the cleaning effect.
상기 목적을 달성하기 위한 본 발명의 전기강판용 압연재의 산세액은, 농도 12∼15%의 염산 용액(HCl+H2O)과, 이 염산 용액에 염산 용액의 0.1∼0.2% 첨가되는 산세촉진제(RSH)와, 상기 염산 용액에 순수 염산의 0.2∼0.4%로 첨가되는 산세억제제(RNH2)로 조성됨을 특징으로 하는 구성이다.Pickling liquid of the rolled material for electrical steel sheet of the present invention for achieving the above object is a pickling accelerator which is added to the hydrochloric acid solution (HCl + H 2 O) with a concentration of 12 to 15%, and 0.1 to 0.2% of the hydrochloric acid solution to the hydrochloric acid solution (RSH) and a pickling inhibitor (RNH 2 ) added to the hydrochloric acid solution at 0.2 to 0.4% of pure hydrochloric acid.
이하에서는 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail.
전기강판용 압연재의 표면에 생성되는 스케일은 보통 제1도에 도시한 바와 같이 Fe층(2) 표면에 생성되는 FeSiO4화합물층(4)과 FeO층(6), 그리고 Fe3O4층(8)과 Fe2O3층(10)으로 구분되는데, 온도에 따라 그 생성 비율이 달라지게 되며, 약 580℃에서 생성되는 스케일은 대부분 FeO로 구성된다.The scale formed on the surface of the rolled sheet for electrical steel sheet is usually a FeSiO 4 compound layer (4), a FeO layer (6), and a Fe 3 O 4 layer (8) formed on the surface of the Fe layer (2) as shown in FIG. ) And Fe 2 O 3 layer (10), the production rate varies depending on the temperature, the scale produced at about 580 ℃ is mostly composed of FeO.
본 발명은 압연재 스트립을 염산에 적량의 산세촉진제가 첨가된 산세액으로 산세하여 압연재 스트립 표면의 스케일을 제거하는 경우 표면에 탄소석출물을 형성시켜 검은 얼룩이 발생하는 것을 방지하도록 소량의 산세억제제(Inhibitor)를 첨가함에 특징이 있다.The present invention is a small amount of pickling inhibitors to prevent the formation of black stains by forming a carbon precipitate on the surface when pickling the roll strip with a pickling solution with a suitable pickling accelerator added to hydrochloric acid to remove the scale of the roll strip surface ( Inhibitor).
본 발명에서는, 압연재 표면에 발생하는 얼룩 등의 색상 편차를 방지하도록 농도 12∼15%의 염산 용액(HCl+H2O)에 염산 용액의 0.1∼0.2% 범위로 산세촉진제(RSH)가 첨가된 산세액에 다시 순수염산의 0.2∼0.4% 범위로 산세억제제를 첨가하여 산세액을 조성함에 특징이 있다.In the present invention, pickling accelerators (RSH) are added to the hydrochloric acid solution (HCl + H 2 O) at a concentration of 12 to 15% in the range of 0.1 to 0.2% of the hydrochloric acid solution to prevent color variations such as stains occurring on the surface of the rolled material. The pickling solution is characterized in that the pickling solution is added by adding an acid pickling inhibitor in the range of 0.2 to 0.4% of pure hydrochloric acid.
산세촉진제의 반응에 의해 스케일이 제거된 압연재 표면에 발생된 얼룩 등의 색상 편차가 일종의 과산세에 기인함을 알아내고, 이를 방지하기 위해 산세액에 산세억제제를 첨가하는데, 산세억제제의 첨가에 의해 그 극성기인 아미노기(-NH2)가 압연재의 소지 금속인 철(Fe)과 결합하여 강한 흡착력을 발생하여 압연재 표면의 얼룩 등의 색상 편차 및 부식을 방지하는 것이다.It was found that the color variation such as unevenness generated on the surface of the rolled material descaled by the reaction of the pickling accelerator was caused by a kind of over pickling, and to prevent this, a pickling inhibitor was added to the pickling solution. As a result, the amino group (-NH 2 ), which is a polar group thereof, is combined with iron (Fe), which is the base metal of the rolled material, to generate a strong adsorption force, thereby preventing color variation and corrosion of the surface of the rolled material.
압연재의 산세 공정에서 이와 같은 스케일은 쇼트 블라스터에서 기계적으로 일차 제거된후, 산세탱크에서 염산 용액과 반응하여 미제거된 스케일을 산세 공정을 통해 제거하고 있는데, 염산용액에 산세촉진제 및 산세억제제를 본 발명에서와 같이 소정량 첨가한 산세액에 의하면 압연재 표면의 스케일 제거 및 우수한 표면 색상 확보가 가능하다.In the pickling process of the rolled material, such scale is first mechanically removed from the shot blaster and then reacted with the hydrochloric acid solution in the pickling tank to remove the unremoved scale through the pickling process.The pickling accelerator and the pickling inhibitor are removed from the hydrochloric acid solution. According to the pickling liquid added in a predetermined amount as in the present invention it is possible to remove the scale of the surface of the rolled material and ensure excellent surface color.
이하, 실시예와 관련하여 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.
[종래예][Prior example]
종래 산세 공정에 사용되는 산세액은 농도 12∼15%의 염산 용액(HCl+H2O)을 80∼85℃로 유지하고 이러한 염산 용액에 염산 용액의 0.1∼0.2%의 산세촉진제(RSH)를 첨가한 것이다.The pickling solution used in the conventional pickling process maintains a hydrochloric acid solution (HCl + H 2 O) at a concentration of 12 to 15% at 80 to 85 ° C and adds 0.1 to 0.2% pickling accelerator (RSH) of hydrochloric acid solution to the hydrochloric acid solution. It is added.
이 산세촉진제를 표 1과 같이 농도를 달리하여 첨가후 스케일 제거 효과와 압연재의 표면 색상에 미치는 변화를 조사하였다.The pickling accelerators were changed at different concentrations as shown in Table 1 to investigate the effect of descaling effect and the surface color of the rolled material.
표 1에 나타낸 바와 같이, 산세촉진제(RSH)는 첨가량 0.1% 미만에서는 스케일의 제거 효과가 미흡함과 아울러 줄무늬의 발생 원인이 되고, 0.2%를 초과하는 경우 얼룩 무늬의 발생을 초래하기 때문에 그 첨가량을 0.1∼0.2%로 하는 것이 바람직하며, 이러한 범위의 산세촉진제가 첨가된 산세액에서의 압연재 표면의 산세효과를 제2도 사진이 보이고 있다.As shown in Table 1, the pickling accelerator (RSH) is less than 0.1% of the addition amount is insufficient effect of removing the scale and cause the generation of streaks, if exceeding 0.2%, the addition amount is increased because It is preferable to set it as 0.1 to 0.2%, and the photograph of FIG. 2 shows the pickling effect of the rolling material surface in the pickling liquid to which the pickling accelerator of this range was added.
[실시예]EXAMPLE
종래와 같이, 염산 용액에 산세촉진제를 상기와 같이 첨가한 산세액으로 압연재 표면을 산세시 얼룩이 존재하는 것을 해결하기 위하여, 상기 염산 용액에 순수 염산의 0.2∼0.4%의 산세억제제(RNH)를 각각 첨가하여 산세액을 조성하였으며, 시험 결과를 표 2에 나타내었다.As in the prior art, in order to solve the presence of stains when pickling the surface of the rolled material with the pickling solution in which the pickling accelerator is added to the hydrochloric acid solution as described above, 0.2 to 0.4% of the pickling inhibitor (RNH) of pure hydrochloric acid is added to the hydrochloric acid solution. Each was added to form a pickling solution, the test results are shown in Table 2.
표 2로부터 알 수 있는 바와 같이, 산세억제제를 0.2% 미만 첨가시 부식 방지 효과가 미약하며, 0.4%를 초과하여 첨가시는 비용 상승을 초래하므로 산세억제제는 0.2∼0.4% 첨가하는 것이 양호하다.As can be seen from Table 2, the addition of less than 0.2% of the pickling inhibitor is a corrosion protection effect is weak, the addition of more than 0.4% causes an increase in the cost of the pickling inhibitor is preferred to add 0.2 to 0.4%.
이와 같이, 적정량의 산세촉진제 및 산세억제제를 염산 용액에 혼합하여 조성한 본 발명에 따른 전기강판용 압연재의 산세액을 사용하여 압연재를 산세한후 얻어진 압연재 표면을 제3도에 사진으로 나타내었다.Thus, the surface of the rolled material obtained after pickling the rolled material using the pickling solution of the rolled material for electrical steel sheet according to the present invention formed by mixing an appropriate amount of the pickling accelerator and the pickling inhibitor in a hydrochloric acid solution is shown in the photograph in FIG. .
제3도로부터 알 수 있는 바와 같이, 본 발명의 산세액으로 산세한 압연재 표면에서는 검은 얼룩의 발생이 없으며, 표면 색상도 우수하였다.As can be seen from FIG. 3, black spots were not generated on the surface of the rolled material pickled with the pickling solution of the present invention, and the surface color was also excellent.
따라서, 상기 설명한 바와 같이, 본 발명의 전기강판용 압연재의 산세액을 사용하여 산세하면 압연재 표면의 산세 효과를 극대화할 수 있고, 압연재 표면의 색상 편차의 발생을 방지할 수 있다.Therefore, as described above, when pickling using the pickling liquid of the rolled material for electrical steel sheet of the present invention, it is possible to maximize the pickling effect on the surface of the rolled material and to prevent the occurrence of color variation on the surface of the rolled material.
Claims (1)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019940034863A KR0135347B1 (en) | 1994-12-17 | 1994-12-17 | Acid pickling solution for the drawn sheet of electric steel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019940034863A KR0135347B1 (en) | 1994-12-17 | 1994-12-17 | Acid pickling solution for the drawn sheet of electric steel |
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| KR960023254A KR960023254A (en) | 1996-07-18 |
| KR0135347B1 true KR0135347B1 (en) | 1998-07-01 |
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| KR20210078167A (en) * | 2019-12-18 | 2021-06-28 | 주식회사 포스코 | Electrical steel sheet and manufacturing method of the same |
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| KR20210078167A (en) * | 2019-12-18 | 2021-06-28 | 주식회사 포스코 | Electrical steel sheet and manufacturing method of the same |
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