JPH05302183A - Treating method for preventing discoloration of copper and copper alloy - Google Patents
Treating method for preventing discoloration of copper and copper alloyInfo
- Publication number
- JPH05302183A JPH05302183A JP10988392A JP10988392A JPH05302183A JP H05302183 A JPH05302183 A JP H05302183A JP 10988392 A JP10988392 A JP 10988392A JP 10988392 A JP10988392 A JP 10988392A JP H05302183 A JPH05302183 A JP H05302183A
- Authority
- JP
- Japan
- Prior art keywords
- discoloration
- preventing
- copper
- washing
- treatment
- 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.)
- Granted
Links
Landscapes
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】銅および銅合金条のインヒビター
水溶液を用いた変色防止処理方法において、インヒビタ
ーによる変色防止処理効果を損なうことなく、かつ液切
り不良による変色が発生しにくい変色防止処理方法に関
する。TECHNICAL FIELD The present invention relates to a discoloration preventing treatment method using an aqueous solution of an inhibitor for copper and copper alloy strips, which does not impair the discoloration preventing treatment effect by the inhibitor and is less likely to cause discoloration due to poor drainage. ..
【0002】[0002]
【従来の技術】銅、黄銅、りん青銅等の銅合金は、比較
的耐食性の高い金属材料であるが、その表面を大気中に
さらすと酸化膜が成長して変色に至り、商品価値が低下
することがある。この変色を防ぐために、通常インヒビ
ターとしてベンゾトリアゾール系の化合物を含む水溶液
に浸漬して変色防止処理を施す。2. Description of the Related Art Copper alloys such as copper, brass and phosphor bronze are metallic materials having relatively high corrosion resistance, but when their surface is exposed to the atmosphere, an oxide film grows and discolors, which reduces the commercial value. I have something to do. In order to prevent this discoloration, it is usually immersed in an aqueous solution containing a benzotriazole-based compound as an inhibitor to perform discoloration prevention treatment.
【0003】条製品の製造工程では各種の熱処理と圧延
加工が行われるが、加工途中でも適宜一時防錆として変
色防止処理が行われる。例えば大気焼鈍ラインで最終の
湯洗槽にベンゾトリアゾール等のインヒビターを適宜添
加することにより、変色防止処理したり、圧延後、圧延
油を脱脂する工程で変色防止処理することもある。Although various heat treatments and rolling processes are carried out in the manufacturing process of strip products, discoloration preventing processes are appropriately performed as temporary rust prevention during the process. For example, discoloration prevention treatment may be performed by appropriately adding an inhibitor such as benzotriazole to the final hot water washing tank in an air annealing line, or discoloration prevention treatment may be performed in a step of degreasing rolling oil after rolling.
【0004】ところがインヒビター水溶液により変色防
止処理する場合、処理液から条を引き上げた後、ロール
やエアーナイフ等により、できる限り条表面の液膜を切
った後乾燥するのが通例である。ところがこの液切りお
よび乾燥が不均一であると、これによる変色が外観の斑
として認められることがある。この変色は処理直後には
目視で認められなくても、数日経過すると明確になり不
良品になることがある。However, when discoloration prevention treatment is carried out with an aqueous solution of an inhibitor, it is customary to pull up the strip from the treatment liquid, cut the liquid film on the strip surface as much as possible with a roll or an air knife, and then dry. However, if the drainage and the drying are not uniform, discoloration due to the unevenness may be recognized as a patch of appearance. Even if this discoloration is not visually observed immediately after the treatment, it may become clear after a few days and become a defective product.
【0005】[0005]
【発明が解決しようとする課題】本発明は銅および銅合
金条の変色防止処理工程における処理の不均一に起因す
る変色を抑制する方法を提供しようとするものである。DISCLOSURE OF THE INVENTION The present invention is intended to provide a method for suppressing discoloration due to nonuniform treatment in the discoloration preventing treatment step of copper and copper alloy strips.
【0006】[0006]
【課題を解決するための手段】上記課題を解決するため
の本発明の方法は銅および銅合金の変色防止処理におい
て、変色防止処理液を出た金属を水洗液のシャワーによ
り水洗する際に、前記水洗液を予め60〜80℃に保持
した変色防止処理液に通して40℃以上に予熱し、変色
防止処理液を出た金属をこの40℃以上に予熱された水
洗液により水洗する銅および銅合金の変色防止処理方法
である。Means for Solving the Problems The method of the present invention for solving the above-mentioned problems, in the discoloration preventing treatment of copper and copper alloy, when the metal discharged from the discoloration preventing treatment liquid is washed with a shower of a washing liquid, Copper which is preheated to 40 ° C. or higher by passing the washing solution through a discoloration-preventing treatment solution which is previously held at 60 to 80 ° C., and the metal discharged from the discoloration-preventing treatment solution is washed with the washing solution preheated to 40 ° C. or higher; This is a method for preventing discoloration of a copper alloy.
【0007】銅および銅合金の連続的な変色防止処理は
脱脂処理、酸洗等の後水洗されてから、即ち金属の表面
はできるだけ清浄な状態にされた後、変色防止処理液に
浸漬処理されるのが通例である。ところが水洗液中には
前工程からの持ち込まれた各種不純物が存在し、変色防
止処理液に持ち込まれる。また、金属表面は完全に活性
化することが困難であり、表面酸化物や微量の有機物に
より被覆されている。これらの金属の表面皮膜は変色防
止処理を汚染することになる。こうした変色防止処理液
の汚染物は変色防止処理後液切りが不均一であると、表
面に不均一に残留し変色の原因となる。液切りロールの
場合、金属によりロール表面の損耗が不均一で、甚だし
い場合は傷がつくことがある。液切りロール表面の凹凸
は液切り不良の原因となるが、これを完全に管理するこ
とは困難である。またエアーナイフを用いた場合も金属
材料(条)の全幅にわたり常時均一に液を切ることは困
難である。そのため公知のいかなる液切り方法を用いて
も、長時間操業を続けると液切りの均一性は低下する。
そこで変色防止処理後純水で再度、条表面を洗浄する
と、液切り不良に起因する変色はほとんどなくすことが
できる。The continuous discoloration preventing treatment for copper and copper alloys is performed by degreasing, pickling, etc., followed by washing with water, that is, after the metal surface is made as clean as possible, it is immersed in a discoloration preventing treatment solution. It is customary to However, various impurities brought in from the previous step are present in the washing liquid and are brought into the discoloration preventing treatment liquid. Further, it is difficult to completely activate the metal surface, and the metal surface is covered with a surface oxide or a trace amount of organic matter. Surface coatings of these metals will contaminate the tarnish preventative treatment. If such a contaminant of the discoloration preventing treatment liquid is unevenly drained after the discoloration preventing treatment, it remains unevenly on the surface and causes discoloration. In the case of a liquid-draining roll, the wear of the roll surface is uneven due to the metal, and in extreme cases, it may be damaged. The unevenness on the surface of the liquid draining roll causes liquid draining failure, but it is difficult to completely manage this. Even when an air knife is used, it is difficult to always cut the liquid uniformly over the entire width of the metal material (strip). Therefore, even if any known draining method is used, if the operation is continued for a long time, the uniformity of draining will be deteriorated.
Therefore, if the strip surface is washed again with pure water after the discoloration prevention treatment, the discoloration due to the drainage failure can be almost eliminated.
【0008】しかし、インヒビターによる保護皮膜は、
特に変色防止処理直後に水洗を過度に行なうと、保護性
が低下する。特に、水洗温度が高いと、インヒビター皮
膜の保護性が低下するため、水洗液の温度管理を適正値
に厳重に管理することが重要となる。銅および銅合金の
変色防止処理はインヒビターの錯化合物生成反応である
ため、水溶液の温度は高い方が効率よく、操業性も勘案
して60〜80℃で行われるのが通例である。この場
合、水洗温度としても、インヒビター水溶液と同程度の
温度が適している。水洗液の温度は変色防止処理液の温
度より低く、しかも変色防止処理液の温度より40℃以
上が適している。これより高いと、保護皮膜の保護性が
低下し、これより低いと洗浄効果が低下し、しかも、連
続的な乾燥に支障をきたすことになる。条は変色防止処
理槽で60〜80℃に予熱されているため、変色防止処
理後の水洗の温度が多少低くても、水洗時間が短時間で
あるため乾燥を行い易いが、それでも40℃以下になる
と乾燥むらによる変色が発生し易くなる。However, the protective film formed by the inhibitor is
In particular, if water is excessively washed immediately after the discoloration preventing treatment, the protective property is lowered. In particular, if the washing temperature is high, the protective property of the inhibitor film is lowered, so it is important to strictly control the temperature of the washing solution to an appropriate value. The discoloration-preventing treatment of copper and copper alloys is a reaction to form a complex compound of an inhibitor. Therefore, the higher the temperature of the aqueous solution is, the more efficient it is, and it is usually performed at 60 to 80 ° C in consideration of operability. In this case, the washing temperature is preferably the same as that of the inhibitor aqueous solution. The temperature of the washing liquid is lower than the temperature of the discoloration-preventing treatment liquid, and 40 ° C. or higher is more suitable than the temperature of the discoloration-preventing treatment liquid. If it is higher than this, the protective property of the protective film is lowered, and if it is lower than this, the cleaning effect is lowered and, further, it impedes continuous drying. Since the strips are preheated to 60 to 80 ° C in the discoloration prevention treatment tank, even if the temperature of washing with water after the discoloration prevention treatment is somewhat low, it is easy to dry because the washing time is short, but still 40 ° C or less. In this case, discoloration due to uneven drying is likely to occur.
【0009】そこで、水洗液は、変色防止処理液中に配
管を通入し熱交換させることにより、変色防止処理液と
同程度の温度にした後、変色防止後の洗浄に供すると非
常に効率的である。変色防止処理効果を安定させ、かつ
液切り不良による変色を起こさないために本発明の、液
温制御方法は極めて有効である。さらに、水洗水専用の
温度制御装置を設ける場合と比べて、操業管理面でも容
易に、かつ安定操業が可能である。Therefore, the washing liquid is very efficient when it is subjected to cleaning after the discoloration prevention treatment after the pipes are passed through the discoloration prevention treatment liquid to exchange heat with the same temperature as the discoloration prevention treatment liquid. Target. The liquid temperature control method of the present invention is extremely effective for stabilizing the discoloration preventing treatment effect and preventing discoloration due to defective drainage. Further, as compared with the case where a temperature control device dedicated to washing water is provided, the operation management can be performed easily and stably.
【0010】水洗方法としては、条材を変色防止処理液
から引き上げた後、液切りまでの間にスプレー方式等と
するか、1秒程度の短時間浸漬処理とするなどの方法が
考えられるが、特に制約はない。As a method of washing with water, a method such as a spraying method after pulling up the strip from the discoloration-preventing treatment liquid until the drainage, or a short-time immersion treatment of about 1 second can be considered. , There are no particular restrictions.
【0011】また、同洗浄液中にインヒビターを添加す
ると変色防止皮膜の保護性を低下する事なく、条表面を
洗浄化することができる。洗浄液の不純物もなく、しか
も少量の洗浄液で液切り不良による変色問題を効果的に
解決できる。When an inhibitor is added to the cleaning solution, the surface of the strip can be cleaned without lowering the protective property of the discoloration preventing film. There are no impurities in the cleaning liquid, and a small amount of cleaning liquid can effectively solve the discoloration problem due to poor drainage.
【0012】図面を参照して、本発明を具体的に説明す
ると、図1は本発明を実施する場合のラインプロセスの
概念図である。The present invention will be described in detail with reference to the drawings. FIG. 1 is a conceptual diagram of a line process for carrying out the present invention.
【0013】まず、巻き出しロール1から金属条2を巻
き出し、脱脂槽3へ送る。脱脂槽3の内部にはブラシロ
ール5とバックアップロール4とが対向しており、金属
条2はそれらの間を通過する間に例えばアルカリ洗浄液
で付着している油を除去される。First, the metal strip 2 is unwound from the unwinding roll 1 and sent to the degreasing tank 3. Inside the degreasing tank 3, a brush roll 5 and a backup roll 4 are opposed to each other, and the metal strip 2 removes the oil adhering thereto with, for example, an alkaline cleaning liquid while passing between them.
【0014】次に何組かの水洗スプレーを備えた水洗槽
に入り、洗浄液を洗い流した後、変色防止処理槽8に入
り、インヒビターを含有する変色防止液をスプレー12
から噴射される。インヒビターを含有する変色防止液
は、変色防止液循環管17によって、変色防止処理槽8
と循環槽9との間を循環される。循環槽9ではスチーム
等の熱源によって、変色防止液を所定の温度に維持して
いる。Next, after entering the washing tank equipped with several sets of washing sprays to wash away the washing solution, it enters the discoloration preventing treatment tank 8 and sprays 12 the discoloration preventing solution containing the inhibitor.
Is jetted from. The discoloration preventing solution containing the inhibitor is treated by the discoloration preventing solution circulating pipe 17 to prevent the discoloration preventing treatment tank 8
And the circulation tank 9 are circulated. In the circulation tank 9, the discoloration preventing liquid is maintained at a predetermined temperature by a heat source such as steam.
【0015】変色防止処理をされた金属条2は水洗スプ
レー13によって水洗される。この水洗液は、水洗液送
給管11から送られ、循環槽9に内蔵された熱交換器1
0によって予熱された後、水洗スプレー13から金属条
2に対して噴射される。The metal strip 2 which has been subjected to the discoloration prevention treatment is washed with a washing spray 13. The washing liquid is sent from the washing liquid supply pipe 11 and is installed in the circulation tank 9 in the heat exchanger 1.
After being preheated by 0, it is sprayed from the water spray 13 onto the metal strip 2.
【0016】水洗後、金属条2は液切りロール14によ
って液切りされた後、乾燥器15を通過した後巻き取り
ロール16に巻き取られる。After washing with water, the metal strip 2 is drained by the draining roll 14, passed through the dryer 15, and then wound up by the winding roll 16.
【0017】以下、実施例および比較例によって、本発
明を具体的に説明する。The present invention will be specifically described below with reference to examples and comparative examples.
【0018】[0018]
【実施例】板厚0.2mm、幅600mmのりん青銅条
(Cu−8%Sn−0.1%P)の圧延油の付着した圧
延材をアルカリ浸漬脱脂、水洗、変色防止処理、乾燥と
連続脱脂ラインにより、脱脂および変色防止処理を施し
た。各種条件で処理した後、耐変色性を試験した結果を
表1に示す。[Example] A rolled material of phosphor bronze strip (Cu-8% Sn-0.1% P) having a plate thickness of 0.2 mm and a width of 600 mm to which rolling oil is adhered is subjected to alkali immersion degreasing, water washing, discoloration prevention treatment, and drying. Degreasing and discoloration prevention treatment were performed by a continuous degreasing line. Table 1 shows the results of testing discoloration resistance after treating under various conditions.
【0019】通板試験条件は以下に示すものである。液
切り後は乾燥させてコイル状に巻き取った後、サンプリ
ングして硫化水素ガスによる変色防止効果、および液切
り不良による変色の発生の有無を評価した。The strip running test conditions are shown below. After the liquid was drained, it was dried and wound into a coil, and then sampled to evaluate the effect of preventing discoloration due to hydrogen sulfide gas, and the occurrence of discoloration due to poor liquid draining.
【0020】脱脂及び変色防止処理 1)脱脂液 組成 炭酸ナトリウム 20g/L りん酸第三ナトリウム 35g/L トリポリリン酸ナトリウム 5g/L メタケイ酸ナトリウム 30g/L 界面活性剤 10g/L 温度 50℃ 時間 10秒 2)水洗 スプレー水洗 時間 3秒 3)変色防止処理 組成 ベンゾトリアゾール 100ppm 温度 70℃ 時間 3秒 4)洗浄 図1に示すように、変色防止処理槽8から引き出された
後、リンガーロール(液切りロール)14によって液切
りが行なわれる以前に水洗スプレー13を設け、純水を
かけた。 Degreasing and discoloration prevention treatment 1) Degreasing liquid composition Sodium carbonate 20 g / L Tertiary sodium phosphate 35 g / L Sodium tripolyphosphate 5 g / L Sodium metasilicate 30 g / L Surfactant 10 g / L Temperature 50 ° C. Time 10 seconds 2) Washing with water Spray washing time 3 seconds 3) Discoloration prevention treatment Composition benzotriazole 100 ppm Temperature 70 ° C time 3 seconds 4) Cleaning As shown in Fig. 1, after being pulled out from the discoloration prevention treatment tank 8, a ringer roll (drainage roll) ) 14, a washing spray 13 was provided before the liquid was drained, and pure water was sprinkled on it.
【0021】洗浄時間すなわち、スプレーをかけてから
液切りロール14で液を切られるまでの時間は1秒と一
定にした。The washing time, that is, the time from spraying to draining the liquid by the draining roll 14 was kept constant at 1 second.
【0022】スプレーによる液供給量は材料の600m
m幅に対し6L/minの流量で一定とした。洗浄液の
温度は70℃とした。Liquid supply amount by spray is 600 m of material
The flow rate was 6 L / min with respect to the m width. The temperature of the cleaning liquid was 70 ° C.
【0023】5)洗浄液の温度管理 洗浄用の純水は、変色防止処理液の循環槽内に配置した
熱交換器を通して加温した。また、変色防止処理への水
洗温度の影響を見る目的で、一部の条件では熱交換器を
通した洗浄用純水を更に加熱した。5) Temperature Control of Cleaning Solution Pure water for cleaning was heated through a heat exchanger arranged in a circulation tank for the discoloration preventing treatment solution. Further, in order to see the effect of the washing temperature on the discoloration prevention treatment, under some conditions, the pure water for washing passed through the heat exchanger was further heated.
【0024】6)液切り ネオプレン性の200mmφのゴムロールで条の両面か
ら、抑えて、液切りを行った。液切り不良の影響を見る
目的でゴムロール表面には、深さ0.5mm、長さ20
0mmの傷のあるものを用いた。6) Draining Draining was performed by using a neoprene rubber roll having a diameter of 200 mmφ from both sides of the strip. For the purpose of seeing the effect of poor drainage, the rubber roll surface has a depth of 0.5 mm and a length of 20 mm.
A scratch with 0 mm was used.
【0025】耐変色性評価方法 りん青銅条を短冊状試験片に切り出し、3ppmH
2S,40℃、50%RHの硫化水素雰囲気に20分間
暴露し、試験片の硫化変色の程度を目視により評価し
た。Discoloration resistance evaluation method A phosphor bronze strip was cut into a strip-shaped test piece and 3 ppmH
The test piece was exposed to a hydrogen sulfide atmosphere of 2 S, 40 ° C. and 50% RH for 20 minutes, and the degree of sulfurization discoloration of the test piece was visually evaluated.
【0026】液切り不良による変色の発生の評価 各通板条件毎にりん青銅条を通板幅(600mm)で1
mの長さ切り出し、1週間室内暴露して、液切り不良に
起因する変色の発生の有無を目視観察した。 Evaluation of occurrence of discoloration due to poor drainage 1 for each strip width (600 mm) of phosphor bronze strip for each strip condition
The sample was cut out to a length of m and exposed to a room for 1 week, and the presence or absence of discoloration due to poor drainage was visually observed.
【0027】[0027]
【表1】 [Table 1]
【0028】[0028]
【発明の効果】以上説明したように本発明によれば、銅
および銅合金条の変色防止処理工程において、インヒビ
ターによる変色防止処理効果を低下させることなく、液
切り不良による変色の発生を防止することができる。As described above, according to the present invention, in the discoloration preventing treatment step of copper and copper alloy strips, discoloration due to drainage failure is prevented without lowering the discoloration preventing treatment effect by the inhibitor. be able to.
【図1】本発明の一具体例の説明図である。FIG. 1 is an explanatory diagram of a specific example of the present invention.
1 巻き出しロール 2 条 3 脱脂槽 4 バックアップロール 5 ブラシロール 6 水洗槽 7 水洗スプレー 8 変色防止処理槽 9 循環槽 10 熱交換器 11 水洗液送給管 12 スプレー 13 水洗スプレー 14 液切りロール 15 乾燥器 16 巻き取りロール 17 変色防止液循環管 1 Unwinding roll 2 Article 3 Degreasing tank 4 Backup roll 5 Brush roll 6 Washing tank 7 Washing spray 8 Discoloration prevention treatment tank 9 Circulation tank 10 Heat exchanger 11 Washing liquid supply pipe 12 Spray 13 Washing spray 14 Draining roll 15 Drying Container 16 Winding roll 17 Discoloration prevention liquid circulation pipe
Claims (1)
いて、変色防止処理液を出た金属条材を水洗液のシャワ
ーにより水洗する際に、前記水洗液を予め60〜80℃
に保持した変色防止処理液に通して40℃以上に予熱
し、変色防止処理液を出た金属条材をこの40℃以上に
予熱された水洗液により水洗することを特徴とする銅お
よび銅合金の変色防止処理方法。1. In the discoloration-preventing treatment of copper and copper alloy strips, when the metal strip having discharged the discoloration-preventing treatment solution is washed with a shower of a washing solution, the washing solution is preheated to 60 to 80 ° C.
Characterized in that it is preheated to 40 ° C. or higher by passing it through the discoloration prevention treatment liquid held in the above step, and the metal strip discharged from the discoloration prevention treatment liquid is washed with this washing water preheated to 40 ° C. or higher. Discoloration prevention treatment method.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP10988392A JP2796214B2 (en) | 1992-04-28 | 1992-04-28 | Discoloration prevention treatment method for copper and copper alloy |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP10988392A JP2796214B2 (en) | 1992-04-28 | 1992-04-28 | Discoloration prevention treatment method for copper and copper alloy |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH05302183A true JPH05302183A (en) | 1993-11-16 |
JP2796214B2 JP2796214B2 (en) | 1998-09-10 |
Family
ID=14521583
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP10988392A Expired - Lifetime JP2796214B2 (en) | 1992-04-28 | 1992-04-28 | Discoloration prevention treatment method for copper and copper alloy |
Country Status (1)
Country | Link |
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JP (1) | JP2796214B2 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2014156361A1 (en) * | 2013-03-28 | 2014-10-02 | 古河電気工業株式会社 | Surface-treated copper foil |
WO2014156362A1 (en) * | 2013-03-28 | 2014-10-02 | 古河電気工業株式会社 | Surface-treated copper foil |
-
1992
- 1992-04-28 JP JP10988392A patent/JP2796214B2/en not_active Expired - Lifetime
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2014156361A1 (en) * | 2013-03-28 | 2014-10-02 | 古河電気工業株式会社 | Surface-treated copper foil |
WO2014156362A1 (en) * | 2013-03-28 | 2014-10-02 | 古河電気工業株式会社 | Surface-treated copper foil |
JPWO2014156362A1 (en) * | 2013-03-28 | 2017-02-16 | 古河電気工業株式会社 | Surface treatment electrolytic copper foil |
JPWO2014156361A1 (en) * | 2013-03-28 | 2017-02-16 | 古河電気工業株式会社 | Surface treatment electrolytic copper foil |
Also Published As
Publication number | Publication date |
---|---|
JP2796214B2 (en) | 1998-09-10 |
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