JPS63216986A - High-speed pickling method for low cr steel - Google Patents
High-speed pickling method for low cr steelInfo
- Publication number
- JPS63216986A JPS63216986A JP4856387A JP4856387A JPS63216986A JP S63216986 A JPS63216986 A JP S63216986A JP 4856387 A JP4856387 A JP 4856387A JP 4856387 A JP4856387 A JP 4856387A JP S63216986 A JPS63216986 A JP S63216986A
- Authority
- JP
- Japan
- Prior art keywords
- pickling
- hydrochloric acid
- soln
- steel
- low
- 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.)
- Pending
Links
- 238000005554 pickling Methods 0.000 title claims abstract description 42
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 18
- 239000010959 steel Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 46
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001447 ferric ion Inorganic materials 0.000 claims abstract description 9
- 238000007664 blowing Methods 0.000 claims abstract description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001448 ferrous ion Inorganic materials 0.000 claims abstract 2
- 239000002699 waste material Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 4
- 229910000975 Carbon steel Inorganic materials 0.000 description 3
- 239000010962 carbon steel Substances 0.000 description 3
- 238000012733 comparative method Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 241001669680 Dormitator maculatus Species 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229960002050 hydrofluoric acid Drugs 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
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
- C23G1/36—Regeneration of waste pickling liquors
Landscapes
- 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
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、Ｃｒ：ｓ〜１３重量％を含有する低Ｃｒ鋼
、特にその熱間圧延材の表面《：発生した酸化スケール
を、効率的（＝、かつ高速で除去する方法に関するもの
である。Detailed Description of the Invention [Industrial Application Field] The present invention is directed to an efficient method for removing oxidized scale generated on the surface of a low Cr steel containing Cr:s to 13% by weight, especially a hot rolled material thereof. (=, and relates to a method for removing it at high speed.
従来、一般《；、上記の低Ｃｒ鋼の脱スケールは、既存
のステンレス鋼の酸洗設備を用い、ソルト処理後硝酸電
解あるいは硝酸浸漬を行なうソルトバス法や、主として
Ｎａ ２ ＳＯ４溶液を使用する中性塩電解処理後、硝
弗酸処理を行なう中性塩法などの代表的方法によって行
なわれている。Conventionally, descaling of the above-mentioned low Cr steel has been carried out using existing stainless steel pickling equipment, using the salt bath method in which nitric acid electrolysis or nitric acid immersion is performed after salt treatment, or mainly using Na 2 SO 4 solution. This is carried out by typical methods such as the neutral salt method in which nitric-fluoric acid treatment is performed after neutral salt electrolytic treatment.
しかし、上記の従来酸洗方法は、低Ｃｒ鋼に対しては、
その酸洗時間が、ステンレス鋼を対象としているため相
対的に長くならざるを得す、この結果マトリックスの異
常腐食、すなわち過酸洗となることがしばしば発生して
おり、また一方で、炭素鋼の酸洗設備しかもたない場合
には、炭素鋼の酸洗速度は相対的に高速であるために、
低Ｃｒ鋼の酸洗を行なうことができないのが現状である
。However, the above conventional pickling method does not work well for low Cr steel.
Since the pickling time is targeted at stainless steel, it has to be relatively long, which often results in abnormal corrosion of the matrix, that is, over-pickling, and on the other hand, carbon steel If you only have pickling equipment, the pickling speed of carbon steel is relatively high, so
At present, it is not possible to pickle low Cr steel.
そこで、本発明者等は、上述のような観点から、炭素鋼
の酸洗速度に相当する高速の酸洗速度で低Ｃｒｆ１４の
脱スケールを可能とすべく研究を行なった注目し、これ
に空気を吹込んだり、あるいは過酸化水素（Ｈ２Ｏ。）
を注入したりして、前記Ｆｅ２＋を第２鉄イオン（Ｆｅ
）に酸化し、さらに塩酸（ＨＣＪ）を添加して調製した
、温度＝５０〜１００℃、Ｈ（Ｊ濃度ニア−１５％、Ｆ
ｅ 濃度：０．５〜１０％の調製溶液な酸洗溶液とし
て用いると、この再生塩酸酸洗液中のＦｅ によって
Ｃｒ鋼の脱スケニルが著しく促進されるよう（ニなって
、高速での酸洗が可能となり、しかもこの結果発生した
塩酸酸洗廃液は、再び酸化とＨＣＩ！添加の調製によっ
て再生循環使用が可能となるばかりでなく、これらの調
製は脱スケールと連続して行なえるので効率的、合理的
であるなどの知見を得たのである。Therefore, from the above-mentioned viewpoint, the present inventors conducted research to enable descaling of low Crf14 at a high pickling speed equivalent to that of carbon steel, and focused on this by or hydrogen peroxide (H2O.)
The Fe2+ is converted into ferric ions (Fe
) and further added hydrochloric acid (HCJ), temperature = 50 to 100 °C, H (J concentration near-15%, F
e When used as a prepared pickling solution with a concentration of 0.5 to 10%, the Fe in this regenerated hydrochloric acid pickling solution will significantly accelerate the deskenylation of Cr steel (in turn, the deskenylation of Cr steel will be accelerated). In addition, the hydrochloric acid pickling waste generated as a result can not only be recycled and used again by oxidation and addition of HCI!, but also efficient as these preparations can be performed continuously with descaling. They obtained knowledge that it is accurate and rational.
この発明は、上記知見Ｃ二もとづいてなされたものであ
るが、その実施に際して、特にＦｅ２＋からＦｅ３＋へ
の酸化は、反応速度を促進させるためにできるだけ高い
温度、実際には５０〜１００℃の温度で行なうのがよく
、またこれを空気の吹込み（＝より行なう場合には、空
気の吹込み量を、廃液＝１１当り５０ＣＣ／Ｊｌ１８以
上とし、かつ吹込み器具の先端にグラスフィルターなど
を取付けて細かい泡状とするのが望ましく、さらに廃液
中に、活性炭を酢加し、その触媒作用を利用したり、あ
るいはＮａＣＡを添加したりして、酸化反応の加速をは
かるのもよく、一方、Ｈ２Ｏ２の添加による酸化は、廃
液中への注入により簡単に行なえるが、コスト高となる
欠点がある。This invention was made based on the above-mentioned knowledge C2, but in carrying out the oxidation from Fe2+ to Fe3+, the temperature is as high as possible, in fact, at a temperature of 50 to 100°C, in order to accelerate the reaction rate. It is best to carry out this by blowing air (=), the amount of air blowing should be 50CC/Jl18 or more per waste liquid=11, and a glass filter etc. should be attached to the tip of the blowing device. It is desirable to make the oxidation reaction into a fine foam, and it is also good to accelerate the oxidation reaction by adding activated carbon to the waste liquid to utilize its catalytic action, or by adding NaCA. Oxidation by addition of H2O2 can be easily carried out by injection into the waste liquid, but has the disadvantage of high cost.
つぎに、この発明の方法において、再生塩酸酸洗液の温
度、ＨＣ７濃度、およびＦｅ 濃度を上記の通りに限
定した理由を説明する。Next, the reason why the temperature, HC7 concentration, and Fe2 concentration of the regenerated hydrochloric acid pickling solution are limited as described above in the method of the present invention will be explained.
（ａ） 温度
温度は高いほど脱スケール性は向上するが、その温度が
５０℃未満では脱スケール性が劣り、一方その温度が１
００’Ｃ’に越えると、Ｈ（Ｊ ミストの発生量が増大
して、環境悪化を招くようになることから、その温度を
５０〜１００℃と定めた。(a) Temperature The higher the temperature, the better the descaling property is, but if the temperature is less than 50°C, the descaling property is poor;
If the temperature exceeds 00'C', the amount of H(J mist generated increases, leading to environmental deterioration. Therefore, the temperature was set at 50 to 100C.
（ｂｌ ＨＣ７濃度
そのＨ（Ｊ濃度が７％未満では、所望の脱スケール性を
確保することができず、一方そのＨ（Ｊ濃度が１５％を
越えると、脱スケール性は増すものの、ＨＣＪ ミスト
の発生量が多くなって、作業環境の悪化を招くばかりで
なく、酸洗後の表面肌の凹凸が大となることから、その
ＨＣ７濃度を７〜１５％と定めたつこの範囲内ではＨ（
Ｊ濃度の高い方が脱スケールは加速される。(bl) If the HC7 concentration and H(J concentration is less than 7%, the desired descaling property cannot be ensured. On the other hand, if the H(J concentration exceeds 15%), although the descaling property increases, HCJ mist Not only does this increase the amount of H(
Descaling is accelerated when the J concentration is high.
（ｃｌ Ｆｅ 濃度
そのＦｅ 濃度が０．５％未満では、所望の酸洗高速
化をはかることができず、一方そのＦｅ３＋濃度が１０
％を越えると、酸洗後の表面に孔食が発生し易くなるこ
とから、そのＦｅ 濃度？０，５〜１０％と定めた。(cl Fe concentration If the Fe concentration is less than 0.5%, the desired pickling speed cannot be achieved; on the other hand, if the Fe3+ concentration is less than 10%,
If the Fe concentration exceeds %, pitting corrosion tends to occur on the surface after pickling. It was set at 0.5-10%.
つぎに、この発明の方法を実施例により具体的に説明す
るっ
ＨＣｌｊ ： ０．０２ ％ 、 Ｆｅ”” ： １３
．５％＋Ｆｅ −０，２％ｙ含有する塩酸酸洗廃液を用
い、これ（二温度＝８０℃にて溶液：ＩＩｌ当り２００
ｃｃ／ｍの流量で、吹込み時間を変えながら空気を吹込
み、ついで各種割合でＨ（Ｊ ４添加することにより、
それぞれ第１表に示される各種の再生塩酸酸洗液を調製
し、これらの各種の再生塩酸酸洗液のそれぞれに、幅：
５０Ｉ×長さ：１００ｍ×厚さ：３Ｈの寸法をもった８
ＵＳ４１０Ｌ （Ｃｒ：１１％含有の低Ｃｒ鋼）の熱延
鋼板を２５秒間浸漬（この浸漬時間は連続焼鈍酸洗ライ
ンにおける長さ：２５ｍの酸洗槽でライン速度：５Ｑｍ
／ｍｍで酸洗を行なう場合を想定して定めた）して、そ
の表面の脱スケールを行なうことによって本発明法１〜
１３および比較法１〜５？：それぞれ実施し、脱スケー
ル状況と表面状況乞観察した。Next, the method of the present invention will be specifically explained with reference to Examples.HClj: 0.02%, Fe"": 13
．． Using a hydrochloric acid pickling waste solution containing 5% + Fe -0.2%y, this (solution at two temperatures = 80°C: 200
By blowing air at a flow rate of cc/m while changing the blowing time, and then adding H (J4) in various proportions,
Various regenerated hydrochloric acid pickling solutions shown in Table 1 are prepared, and each of these various regenerated hydrochloric acid pickling solutions has a width:
8 with dimensions of 50I x length: 100m x thickness: 3H
A hot rolled steel plate of US410L (low Cr steel containing 11% Cr) is immersed for 25 seconds (this immersion time is a pickling tank with a length of 25 m in a continuous annealing pickling line and a line speed of 5 Qm).
/mm), and by descaling the surface, methods 1 to 1 of the present invention
13 and Comparative Methods 1-5? : Each was carried out and the descaling situation and surface situation were carefully observed.
なお、比較法１〜５は、再生塩酸酸洗液のＦｅ３＋濃度
または温度がこの発明の範囲から外れたものである。In Comparative Methods 1 to 5, the Fe3+ concentration or temperature of the regenerated hydrochloric acid pickling solution was outside the scope of the present invention.
本発明法１〜１３においては、いずれも２５秒の短かい
酸洗時間で税スケールが完全に行なわれており、このこ
とは高速酸洗が可能であることを示し、かつ表面肌もき
わめて良好であるのに対して、比較法１〜５においては
、税スケールが不十分なものや、表面凹凸の激しいもの
が観察され、良好な脱スケールを行なうことができない
ものであったＯ
上述のよう（：、この発明の方法によれば、低Ｃｒ鋼の
高速での酸洗を効率的）：、かつ合理的に、コスト安く
行なうことができるのである。In Methods 1 to 13 of the present invention, the tax scale was completely removed in a short pickling time of 25 seconds, which indicates that high-speed pickling is possible, and the surface texture is also extremely good. On the other hand, in Comparative Methods 1 to 5, insufficient scale and severe surface unevenness were observed, making it impossible to perform good descaling. (According to the method of the present invention, low Cr steel can be pickled efficiently at high speed): and can be carried out rationally and at low cost.
Claims (3)
吹込み、あるいは過酸化水素の注入により第２鉄イオン
に酸化し、かつこれに塩酸を添加して調製した、温度：
５０〜１００℃、塩酸濃度：７〜１５％、第２鉄イオン
濃度：０．５〜１０％の再生塩酸酸洗液中にて、低Ｃｒ
鋼の脱スケールを高速で行なうことを特徴とする再生塩
酸酸洗液使用による低Ｃｒ鋼の高速酸洗方法。(1) Ferrous ions contained in the hydrochloric acid pickling waste liquid are oxidized to ferric ions by blowing air or injecting hydrogen peroxide, and then hydrochloric acid is added to the ferric ions. Temperature:
Low Cr in a regenerated hydrochloric acid pickling solution at 50-100°C, hydrochloric acid concentration: 7-15%, ferric ion concentration: 0.5-10%.
A high-speed pickling method for low Cr steel using a recycled hydrochloric acid pickling solution, which is characterized by descaling steel at a high speed.
ことを特徴とする上記特許請求の範囲第（１）項記載の
低Ｃｒ鋼の高速酸洗方法。(2) The high-speed pickling method for low Cr steel according to claim (1), characterized in that the recycled hydrochloric acid pickling solution is further reused and recycled.
る脱スケールと連続させて行なうことを特徴とする上記
特許請求の範囲第（１）項記載の低Ｃｒ鋼の高速酸洗方
法。(3) A high-speed pickling method for low Cr steel according to claim (1), characterized in that the preparation of the hydrochloric acid pickling waste liquid is carried out in succession with descaling using the recycled hydrochloric acid pickling liquid. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4856387A JPS63216986A (en) | 1987-03-03 | 1987-03-03 | High-speed pickling method for low cr steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4856387A JPS63216986A (en) | 1987-03-03 | 1987-03-03 | High-speed pickling method for low cr steel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63216986A true JPS63216986A (en) | 1988-09-09 |
Family
ID=12806856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4856387A Pending JPS63216986A (en) | 1987-03-03 | 1987-03-03 | High-speed pickling method for low cr steel |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63216986A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0776993A1 (en) * | 1995-11-28 | 1997-06-04 | Eka Chemicals AB | Method for pickling steel |
| FR2745301A1 (en) * | 1996-02-27 | 1997-08-29 | Usinor Sacilor | PROCESS FOR STRIPPING A STEEL PART AND PARTICULARLY A STAINLESS STEEL SHEET STRIP |
| WO1999027162A1 (en) * | 1997-11-24 | 1999-06-03 | Acciai Speciali Terni S.P.A. | Method for pickling steel products |
| EP0949354A1 (en) * | 1998-04-06 | 1999-10-13 | SOLVAY (Société Anonyme) | Pickling process |
| US6398876B1 (en) * | 1998-12-22 | 2002-06-04 | Andritz—Patentverwaltungs-Gesellschaft m.b.H. | Process for pickling steel |
| KR100460174B1 (en) * | 2002-03-14 | 2004-12-04 | 동인산업(주) | Fe(+3) preparation method and preparation machine |
| JP2007107045A (en) * | 2005-10-13 | 2007-04-26 | Jfe Steel Kk | Method for pickling stainless steel material and method for producing the same |
| JP2007107044A (en) * | 2005-10-13 | 2007-04-26 | Jfe Steel Kk | Method for pickling stainless hot rolled steel material and method for producing the same |
| JP2013124394A (en) * | 2011-12-15 | 2013-06-24 | Parker Corp | Surface treatment agent for stainless steel, and method for treatment and management thereof |
| CN105696009A (en) * | 2014-11-27 | 2016-06-22 | 宝钢工程技术集团有限公司 | Treatment device of stainless steel pickling solution and use method thereof |
-
1987
- 1987-03-03 JP JP4856387A patent/JPS63216986A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0776993A1 (en) * | 1995-11-28 | 1997-06-04 | Eka Chemicals AB | Method for pickling steel |
| FR2745301A1 (en) * | 1996-02-27 | 1997-08-29 | Usinor Sacilor | PROCESS FOR STRIPPING A STEEL PART AND PARTICULARLY A STAINLESS STEEL SHEET STRIP |
| EP0792949A1 (en) * | 1996-02-27 | 1997-09-03 | USINOR SACILOR Société Anonyme | Process for pickling a steel workpiece, in particular stainless steel sheet strip |
| CN1084801C (en) * | 1996-02-27 | 2002-05-15 | 尤吉纳股份有限公司 | Process for pickling piece of steel and in particular sheet strip of stainless steel |
| US6500328B1 (en) * | 1997-11-24 | 2002-12-31 | Acciai Speciali Terni S.P.A. | Method for pickling steel products |
| WO1999027162A1 (en) * | 1997-11-24 | 1999-06-03 | Acciai Speciali Terni S.P.A. | Method for pickling steel products |
| EP0949354A1 (en) * | 1998-04-06 | 1999-10-13 | SOLVAY (Société Anonyme) | Pickling process |
| US6398876B1 (en) * | 1998-12-22 | 2002-06-04 | Andritz—Patentverwaltungs-Gesellschaft m.b.H. | Process for pickling steel |
| KR100460174B1 (en) * | 2002-03-14 | 2004-12-04 | 동인산업(주) | Fe(+3) preparation method and preparation machine |
| JP2007107045A (en) * | 2005-10-13 | 2007-04-26 | Jfe Steel Kk | Method for pickling stainless steel material and method for producing the same |
| JP2007107044A (en) * | 2005-10-13 | 2007-04-26 | Jfe Steel Kk | Method for pickling stainless hot rolled steel material and method for producing the same |
| JP2013124394A (en) * | 2011-12-15 | 2013-06-24 | Parker Corp | Surface treatment agent for stainless steel, and method for treatment and management thereof |
| CN105696009A (en) * | 2014-11-27 | 2016-06-22 | 宝钢工程技术集团有限公司 | Treatment device of stainless steel pickling solution and use method thereof |
| CN105696009B (en) * | 2014-11-27 | 2017-12-29 | 宝钢工程技术集团有限公司 | The processing unit and its application method of acid washing liquid for stainless steel |
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