JPH05320959A - Rust preventing method for electrolytic iron - Google Patents

Rust preventing method for electrolytic iron

Info

Publication number
JPH05320959A
JPH05320959A JP12639492A JP12639492A JPH05320959A JP H05320959 A JPH05320959 A JP H05320959A JP 12639492 A JP12639492 A JP 12639492A JP 12639492 A JP12639492 A JP 12639492A JP H05320959 A JPH05320959 A JP H05320959A
Authority
JP
Japan
Prior art keywords
electrolytic iron
phosphate
rust
pieces
nitrite
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
Application number
JP12639492A
Other languages
Japanese (ja)
Inventor
Yoshito Takano
義人 高野
Satoshi Negishi
悟史 根岸
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Resonac Holdings Corp
Original Assignee
Showa Denko KK
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 Showa Denko KK filed Critical Showa Denko KK
Priority to JP12639492A priority Critical patent/JPH05320959A/en
Publication of JPH05320959A publication Critical patent/JPH05320959A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/18Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using inorganic inhibitors
    • C23F11/187Mixtures of inorganic inhibitors
    • C23F11/188Mixtures of inorganic inhibitors containing phosphates

Landscapes

  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)

Abstract

PURPOSE:To obtain an easy method for rust prevention of high-purity electrolytic iron by subjecting pieces of electrolytic iron to wet barrel polishing with a soln. containing nitrite, phosphate, and carbonate, dipping the pieces in a rust preventing liquid containing nitrite and phosphate, and drying. CONSTITUTION:An electrolytic iron is crushed into about 3-100mm pieces and subjected to wet barrel polishing with a soln. containing nitrite (e.g. NaNO3 with 4-8wt.% concn.), phosphate (e.g. Na4P2O7 with 4-8wt.% concn.), and carbonate (e.g. Na2CO3 with 5-9wt.% concn.) and washed with water. Then the pieces are dipped in a rust preventing liquid containing nitrite (about 0.5-1.2g/l concn.) and phosphate (about 0.6-1.3g/l canon.) and dried. By this method, rust prevention is effectively and easily performed for high-purity electrolytic iron.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は工業用純鉄として有用な
高純度電解鉄の防錆方法に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a rust preventive method for high purity electrolytic iron useful as industrial pure iron.

【0002】[0002]

【従来の技術】電解鉄は通常の軟鋼に比べ各種不純物が
格段に少ないため、磁性材料、電子材料、特殊合金材料
等高品位を要求される分野で多用されている。電解鉄は
通常軟鉄を陽極、ステンレス鋼などを陰極として、塩酸
塩浴または硫酸塩浴を使用して電解し、陰極上に高純度
鉄を電着させて得ている。
2. Description of the Related Art Electrolytic iron is remarkably less in various impurities than ordinary mild steel, and is therefore widely used in fields requiring high quality such as magnetic materials, electronic materials and special alloy materials. Electrolytic iron is usually obtained by electrolyzing soft iron as an anode and stainless steel as a cathode using a hydrochloride or sulfate bath, and electrodepositing high-purity iron on the cathode.

【0003】電解鉄は高純度であるため、表面に極く薄
い酸化膜が生じると内部を保護する性質がある。このた
め電着で得られた電解鉄を充分きれいに洗浄し、乾燥雰
囲気中に保管すれば、かなりの程度錆の発生を防止する
ことができる。このほか、電解鉄表面に油脂類を塗布し
て防錆する方法も考えられるが、油脂類を塗布すること
は使用段階で炭素、酸素等の不純物が混入する原因とな
るので好ましくない。
Since electrolytic iron has a high degree of purity, it has the property of protecting the inside if an extremely thin oxide film is formed on the surface. Therefore, if the electrolytic iron obtained by electrodeposition is thoroughly cleaned and stored in a dry atmosphere, rust can be prevented to a considerable extent. In addition, a method of applying oils and fats to the surface of electrolytic iron to prevent rust can be considered, but applying oils and fats is not preferable because it causes impurities such as carbon and oxygen to be mixed in at the use stage.

【0004】[0004]

【発明が解決しようとする課題】電解鉄表面が平滑な場
合は付着不純物も少なく、錆も発生しにくいが、一般に
電着して得られた電解鉄表面は、細かな突起部分やへこ
み部分があり、良好な平滑性を保っているわけではな
い。表面が平滑でない電解鉄は突起部分およびくぼみ部
分から錆が発生し易く、塩酸塩浴を用いて得られたもの
は特に顕著であり、通常の缶内密封保管では発錆を防止
するのは困難である。
When the surface of the electrolytic iron is smooth, less impurities are attached and rust is less likely to occur. Generally, however, the electrolytic iron surface obtained by electrodeposition has fine protrusions and dents. However, it does not maintain good smoothness. Electrolytic iron with a non-smooth surface is prone to rust from protrusions and dents, and the one obtained using a hydrochloric acid salt bath is particularly prominent, and it is difficult to prevent rusting in ordinary canned storage. Is.

【0005】また、表面が汚れている場合も汚染部分か
ら発錆するので、通常は乾式バレル研磨等で汚染部分を
研磨除去しているが、それでも有効に発錆を防止するこ
とはできない。
Further, even if the surface is dirty, rust is generated from the contaminated part. Therefore, although the contaminated part is usually polished and removed by dry barrel polishing or the like, the rust cannot be effectively prevented.

【0006】[0006]

【課題を解決するための手段】本発明では電解鉄を適当
な大きさに破砕し、亜硝酸塩、リン酸塩および炭酸塩を
溶解した液中で湿式バレル研磨し水洗したのち、亜硝酸
塩とリン酸塩を含有する防錆液中に浸漬したのち、乾燥
する手段を採用した。本発明の対象となる電解鉄は塩酸
塩浴を使用したものでも硫酸塩浴を使用したものでも良
いが、前者のものに対する効果が顕著である。通常電解
鉄は厚さ5〜10mmの板状に電着しているが、これを
3〜100mmの小片に破砕し、ミル中でバレル研磨す
る。バレル研磨はアルミナ等のバレル研削材を使用して
も良いが、特に研削材を使用しなくても電解鉄同志の研
磨力だけでも充分である。バレル研磨に際しては亜硝酸
塩、リン酸塩および炭酸塩を含む水溶液を共存させて湿
式研磨し、バレル研磨によって生じたきれいな表面を洗
浄すると同時に極く薄く表面を酸化させて防錆効果を持
たせるようにする。
In the present invention, electrolytic iron is crushed to an appropriate size, wet barrel polished in a liquid in which nitrite, phosphate and carbonate are dissolved and washed with water, and then nitrite and phosphorus are added. A means of drying after immersing in an anticorrosive solution containing an acid salt was adopted. The electrolytic iron to which the present invention is applied may use either a hydrochloride bath or a sulfate bath, but the effect of the former is remarkable. Usually, electrolytic iron is electrodeposited in a plate shape having a thickness of 5 to 10 mm, which is crushed into small pieces of 3 to 100 mm and barrel-polished in a mill. For barrel polishing, a barrel abrasive such as alumina may be used, but it is sufficient to use only the polishing power of electrolytic iron without using any abrasive. When barrel-polishing, wet polishing with an aqueous solution containing nitrite, phosphate and carbonate to clean the surface produced by barrel-polishing and at the same time oxidize the surface to a very thin level for rust prevention To

【0007】湿式バレル研磨に使用する亜硝酸塩として
は亜硝酸ナトリウム(NaNO3 )、亜硝酸カリウム
(KNO3 )等が利用できる。リン酸塩としてはピロポ
リリン酸ナトリウム(Na427 )、トリポリリン
酸ナトリウム(Na5310)、テトラポリリン酸ナ
トリウム(Na6413)等が利用できる。また、炭
酸塩としては炭酸ナトリウム(Na2 CO3 )、炭酸カ
リウム(K2 CO3 )、炭酸リチウム(Li2 CO3
等が利用できる。
Sodium nitrite (NaNO 3 ), potassium nitrite (KNO 3 ), etc. can be used as the nitrite used for the wet barrel polishing. As the phosphate, sodium pyropolyphosphate (Na 4 P 2 O 7 ), sodium tripolyphosphate (Na 5 P 3 O 10 ), sodium tetrapolyphosphate (Na 6 P 4 O 13 ) and the like can be used. The carbonates include sodium carbonate (Na 2 CO 3 ), potassium carbonate (K 2 CO 3 ), lithium carbonate (Li 2 CO 3 ).
Etc. are available.

【0008】これら塩類を水に溶かし、ミル中に添加す
る。塩の濃度は亜硝酸塩が4〜8wt%、リン酸塩が4〜
8wt%、炭酸塩が5〜9wt%が適当である。水溶液の量
は特に制限はなく、研磨中で電解鉄表面が濡れれば良
く、ミルの大きさにもよるが装入物に対して約50%前
後が目安となる。研磨時間は電解鉄の表面状態にもよる
が1〜5時間を必要とする。
These salts are dissolved in water and added to the mill. The concentration of salt is 4-8 wt% for nitrite and 4-for phosphate.
8 wt% and 5 to 9 wt% carbonate are suitable. The amount of the aqueous solution is not particularly limited, as long as the surface of the electrolytic iron is wet during polishing, and depending on the size of the mill, it is about 50% with respect to the charged amount as a guide. The polishing time is 1 to 5 hours depending on the surface condition of electrolytic iron.

【0009】研磨終了後水洗して研磨粉や塩類を除去し
た後、亜硝酸塩とリン酸塩を含む防錆液中に浸漬して乾
燥させ防錆処理する。防錆液中に使用する亜硝酸塩とリ
ン酸塩は前記湿式バレル研磨の際に使用するものと同じ
ものが使用できるが、各塩の濃度は1/5〜1/8に薄
めたもので良い。すなわち防錆液の亜硝酸塩濃度は0.
5〜1.2g/l、リン酸塩濃度は0.6〜1.3g/
lが適当である。さらに界面活性剤としてイソプロピル
アルコール等を0.5〜3g/l加えても良い。このよ
うに少量の塩を含む溶液中に浸漬して電解鉄表面に極く
薄い防錆皮膜を形成する。浸漬時間は数分間で良い。
After completion of polishing, the product is washed with water to remove polishing powder and salts, and then immersed in a rust preventive solution containing nitrite and phosphate to be dried for rust preventive treatment. As the nitrite and the phosphate used in the rust preventive solution, the same ones as those used in the wet barrel polishing can be used, but the concentration of each salt may be diluted to 1/5 to 1/8. .. That is, the nitrite concentration of the rust preventive solution is 0.
5-1.2 g / l, phosphate concentration 0.6-1.3 g /
l is suitable. Furthermore, 0.5 to 3 g / l of isopropyl alcohol or the like may be added as a surfactant. Thus, by dipping in a solution containing a small amount of salt, an extremely thin anticorrosive film is formed on the surface of electrolytic iron. The immersion time may be several minutes.

【0010】[0010]

【作用】本発明は、亜硝酸塩、リン酸塩および炭酸塩を
含む水溶液中で電解鉄小片を湿式バレル研磨し、電解鉄
表面に付着したくぼみに入り込んでいる不純物を研削洗
浄除去すると同時に、新しく生成した表面を直ちにリン
酸皮膜処理をほどこすものである。さらにより希薄な塩
溶液を使用して極く薄い防錆皮膜を形成する処理をほど
こすものである。
According to the present invention, electrolytic iron pieces are subjected to wet barrel polishing in an aqueous solution containing nitrite, phosphate and carbonate to remove impurities in the dents adhering to the surface of electrolytic iron by grinding, cleaning, and at the same time. The produced surface is immediately subjected to phosphoric acid film treatment. Furthermore, the treatment for forming an extremely thin rust preventive film is performed by using a more dilute salt solution.

【0011】[0011]

【実施例】塩酸塩浴を用いて製造した平均厚さ5mmの
電解鉄を7〜50mmに破砕し、ミル内に装入して湿式
バレル研磨を行った。バレル研磨条件は以下の通りであ
る。 電解鉄装入量 : 600kg 溶液装入量 : 300l 溶液成分及び濃度 : 亜硝酸ナトリウム 6g/l リン酸ナトリウム 6g/l (Na427 、Na5310、Na6413) 炭酸ナトリウム 7g/l ミル回転数 30rpm 研磨時間 4時間
[Example] Electrolytic iron having an average thickness of 5 mm produced by using a hydrochloride bath was crushed to 7 to 50 mm, charged into a mill and subjected to wet barrel polishing. Barrel polishing conditions are as follows. Electrolytic iron charging amount: 600 kg Solution charging amount: 300 l Solution component and concentration: Sodium nitrite 6 g / l Sodium phosphate 6 g / l (Na 4 P 2 O 7 , Na 5 P 3 O 10 , Na 6 P 4 O) 13 ) Sodium carbonate 7g / l Mill rotation speed 30rpm Polishing time 4 hours

【0012】湿式バレル研磨終了後の電解鉄片を良く水
洗し、亜硝酸ナトリウム0.9g/l、リン酸ナトリウ
ム1.05g/lおよびイソプロピルアルコール0.9
g/lを含む80℃に加熱した水溶液中に浸漬した。1
0分後浸漬した後取り出して完全に乾燥させた。このよ
うな防錆処理した電解鉄片を密封した缶中に保存し、3
ヶ月経過後に検査したところ、錆の発生は全く認められ
なかった。
After the completion of the wet barrel polishing, the electrolytic iron pieces were thoroughly washed with water, sodium nitrite 0.9 g / l, sodium phosphate 1.05 g / l and isopropyl alcohol 0.9.
It was immersed in an aqueous solution containing g / l and heated to 80 ° C. 1
After soaking for 0 minute, it was taken out and completely dried. Store the rustproof electrolytic iron piece in a sealed can and
Upon inspection after a lapse of months, no rust was found.

【0013】比較のため、上記実施例に用いたものと同
一ロットの電解鉄を、電解析出後充分水洗して乾燥する
以外は何らの処理も施さずに缶中に密封して保存した。
1週間経過後検査したところ、約5%のものに錆の発生
が認められた。また、3ヶ月経過後には90%以上のも
のに錆の発生が認められた。
For comparison, electrolytic iron of the same lot as that used in the above example was stored in a can sealed without any treatment, except that it was sufficiently washed with water after electrolytic deposition and dried.
After one week, the inspection revealed that rust was found in about 5%. After 3 months, 90% or more of the rusts were found to be rusted.

【0014】[0014]

【発明の効果】本発明によれば簡便な方法で錆の発生を
効果的に予防することができ、電子部品用原料として使
用した場合にも、電解鉄表面の防錆皮膜は何ら障害とな
らない。
According to the present invention, rust can be effectively prevented by a simple method, and even when used as a raw material for electronic parts, the rust preventive coating on the surface of electrolytic iron does not cause any trouble. ..

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 電解鉄小片を亜硝酸塩、リン酸塩および
炭酸塩を含む溶液と共に湿式バレル研磨し、次いで亜硝
酸塩とリン酸塩を含む防錆液中に浸漬した後、乾燥する
ことを特徴とする電解鉄の防錆方法。
1. An electrolytic iron piece is wet barrel polished with a solution containing nitrite, phosphate and carbonate, and then immersed in an anticorrosive solution containing nitrite and phosphate and then dried. How to prevent corrosion of electrolytic iron.
JP12639492A 1992-05-19 1992-05-19 Rust preventing method for electrolytic iron Pending JPH05320959A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP12639492A JPH05320959A (en) 1992-05-19 1992-05-19 Rust preventing method for electrolytic iron

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP12639492A JPH05320959A (en) 1992-05-19 1992-05-19 Rust preventing method for electrolytic iron

Publications (1)

Publication Number Publication Date
JPH05320959A true JPH05320959A (en) 1993-12-07

Family

ID=14934059

Family Applications (1)

Application Number Title Priority Date Filing Date
JP12639492A Pending JPH05320959A (en) 1992-05-19 1992-05-19 Rust preventing method for electrolytic iron

Country Status (1)

Country Link
JP (1) JPH05320959A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008197022A (en) * 2007-02-15 2008-08-28 Sumika Enviro-Science Co Ltd Simple concentration measuring composition and simple concentration measuring method for dilute fungicide solution

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008197022A (en) * 2007-02-15 2008-08-28 Sumika Enviro-Science Co Ltd Simple concentration measuring composition and simple concentration measuring method for dilute fungicide solution

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