JPS6340875B2 - - Google Patents
Info
- Publication number
- JPS6340875B2 JPS6340875B2 JP9755384A JP9755384A JPS6340875B2 JP S6340875 B2 JPS6340875 B2 JP S6340875B2 JP 9755384 A JP9755384 A JP 9755384A JP 9755384 A JP9755384 A JP 9755384A JP S6340875 B2 JPS6340875 B2 JP S6340875B2
- Authority
- JP
- Japan
- Prior art keywords
- coating
- metal
- electrode
- substrate
- aqueous solution
- 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.)
- Expired
Links
- 238000000576 coating method Methods 0.000 claims description 26
- 239000011248 coating agent Substances 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 11
- 229910000510 noble metal Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- -1 alkaline earth metal salt Chemical class 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 229910017053 inorganic salt Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000011282 treatment Methods 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 3
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 150000002730 mercury Chemical class 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- C23F—NON-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
- C23F1/00—Etching metallic material by chemical means
- C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
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)
- ing And Chemical Polishing (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、金属電極より被覆を除去する方法に
関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for removing coatings from metal electrodes.
近年、チタン等の金属基体上に、貴金属又は貴
金属酸化物を含む被覆を設けた不溶性金属電極
が、種々の電気化学分野、特に食塩電解工業にお
ける不溶性電極として大量に使用されている。こ
のような金属電極は、一般に、かなりの長寿命を
有するものであるが、使用中に電極被覆が徐々に
消耗、或いは低活性化し、一定の性能を維持でき
なくなつた際には、新しい電極に取り替えるか、
電極被覆を再被覆する必要がある。 In recent years, insoluble metal electrodes in which a metal substrate such as titanium is coated with a noble metal or a noble metal oxide have been used in large quantities as insoluble electrodes in various electrochemical fields, particularly in the salt electrolysis industry. Such metal electrodes generally have a fairly long lifespan, but when the electrode coating gradually wears out or becomes less active during use, and it is no longer possible to maintain a certain level of performance, a new electrode may be required. or replace it with
Electrode coating needs to be recoated.
こうした使用済の金属電極には、尚、相当量の
高価なルテニウム等の貴金属成分が被覆中に残存
し、これを除去して回収し、有効利用することは
工業上重要である。また、金属基体を再利用する
ために残存被覆を除去する必要がある。 A considerable amount of precious metal components such as expensive ruthenium still remains in the coating of these used metal electrodes, and it is industrially important to remove and recover this and make effective use of it. Also, in order to reuse the metal substrate, it is necessary to remove the remaining coating.
［従来技術］
この種の技術に関連するものとして、金属電極
被覆を溶融塩を用いて除去する方法（例えば特公
昭46−26978号、特公昭48−15144号）、ルテニウ
ム酸化物を含む被覆を陽極処理して基体から剥離
する方法（例えば特開昭51−68493号、特開昭51
−68499号）、ルテニウム酸化物を還元処理し、ル
テン酸アルカリとして基体から溶離する方法（特
開昭58−194745号）等が知られている。これら従
来の方法は、かなりの危険を伴う複雑固難な操作
を要するか、長時間の処理を要する等の問題があ
つた。[Prior art] Techniques related to this type of technology include methods for removing metal electrode coatings using molten salt (for example, Japanese Patent Publications No. 46-26978 and Japanese Patent Publication No. 15144-1982), and methods for removing coatings containing ruthenium oxide. A method of anodizing and peeling from the substrate (for example, JP-A-51-68493, JP-A-51
68499), and a method in which ruthenium oxide is reduced and eluted from the substrate as an alkali ruthenate (Japanese Patent Application Laid-open No. 194745/1982). These conventional methods have problems such as requiring complicated and difficult operations involving considerable risks, or requiring long processing times.
また、電極基体と被覆との間に、基体金属化合
物の非結合性中間層を、加熱又は酸化処理により
形成して被覆を除去する方法が知られている（特
開昭57−54289号）。しかし、この方法では、特に
被覆が消耗して薄い場合に、除去効果が不十分で
ある。 Furthermore, a method is known in which a non-bonding intermediate layer of a base metal compound is formed between the electrode base and the coating by heating or oxidation treatment, and then the coating is removed (Japanese Patent Laid-Open No. 57-54289). However, this method has insufficient removal effectiveness, especially when the coating is worn and thin.
［発明が解決しようとする問題点］
本発明は、貴金属又はその酸化物を含む被覆を
有する金属電極より、被覆を簡便な操作で十分に
除去する方法を提供することを主たる目的とす
る。特に、使用済の薄くなつた被覆を有する金属
電極において、従来の方法では簡単な方法で被覆
の除去が困難であつたが、本発明は、この場合を
も容易に解決し得るものである。[Problems to be Solved by the Invention] The main object of the present invention is to provide a method for sufficiently removing a coating containing a noble metal or its oxide from a metal electrode with a simple operation. In particular, in the case of used metal electrodes having thinned coatings, it has been difficult to remove the coating using a simple method using conventional methods, but the present invention can easily solve this problem as well.
［問題を解決するための手段］
本発明は、基体上に貴金属又は貴金属酸化物を
含む被覆を有する金属電極を、アルカリ金属又は
アルカリ土類金属の塩の水溶液に浸漬した後、
600℃以上に加熱し、水中にて急冷することを特
徴とする。[Means for Solving the Problems] The present invention provides the following methods: After immersing a metal electrode having a coating containing a noble metal or a noble metal oxide on a substrate in an aqueous solution of an alkali metal or alkaline earth metal salt,
It is characterized by being heated to over 600℃ and then rapidly cooled in water.
食塩電解工業等に用いられている金属電極は、
通常、チタン等の金属基体上に、ルテニウム、ロ
ジウム、パラジウム、イリジウム、白金等の白金
族金属又はその酸化物を含み、適宜、非貴金属の
酸化物等を組成させた被覆を設けたものである。
このような電極は、例えば特公昭48−3954号、特
公昭46−21884号に詳細に記載されている。 Metal electrodes used in the salt electrolysis industry, etc.
Usually, a metal substrate such as titanium is coated with a platinum group metal such as ruthenium, rhodium, palladium, iridium, platinum, or its oxide, and optionally an oxide of a non-noble metal. .
Such electrodes are described in detail in, for example, Japanese Patent Publications No. 48-3954 and Japanese Patent Publication No. 46-21884.
本発明において、使用済等の上記のような電極
を先ず、アルカリ金属又はアルカリ土類金属等の
無機塩を含む水溶液に浸漬する。該無機塩として
は、Na、Ｋ、Mg、Ca、Baの塩化物、硫酸塩、
硝酸塩が好適である。 In the present invention, a used electrode as described above is first immersed in an aqueous solution containing an inorganic salt such as an alkali metal or an alkaline earth metal. Examples of the inorganic salts include chlorides and sulfates of Na, K, Mg, Ca, and Ba.
Nitrates are preferred.
このような無機塩水溶液の濃度は、適宜選定可
能であり、通常約0.1M以上であればよい。また、
必要に応じて界面活性剤等の添加物を加えること
もできる。 The concentration of such an aqueous inorganic salt solution can be selected as appropriate, and generally should be about 0.1M or more. Also,
Additives such as surfactants can also be added as necessary.
次いで、無機塩水溶液に十分な時間浸漬した電
極を600℃以上に加熱処理する。該温度以下では
効果が不十分であり、600℃以上、好ましくは約
750℃〜880℃の温度で空気中等の気相中で加熱す
ることが好適であり、簡便である。加熱時間は、
通常電極が上記の温度に達してから１分以上、約
２〜10分程度とすることが好ましい。 Next, the electrode that has been immersed in the inorganic salt aqueous solution for a sufficient period of time is heated to 600° C. or higher. The effect is insufficient below this temperature, and above 600℃, preferably about
Heating in a gas phase such as air at a temperature of 750°C to 880°C is preferred and convenient. The heating time is
Normally, it is preferably 1 minute or more, and preferably about 2 to 10 minutes, after the electrode reaches the above temperature.
次に加熱処理した電極を直ちに、十分な量の室
温程度以下の水中に浸漬して急冷する。 Next, the heat-treated electrode is immediately immersed in a sufficient amount of water at room temperature or below to be rapidly cooled.
水中に浸漬する直前の電極の温度は600℃以上
であり、これを急冷することにより、基体上の電
極被覆は、完全に、容易に剥離し、除去すること
ができる。本発明の一連の処理により、基体から
被覆を容易に剥離除去できる優れた効果を達成す
る理由は明らかでないが、加熱急冷による熱衝撃
による効果が、予め行う無機塩水溶液浸漬処理に
より助長されるためと思われる。 The temperature of the electrode immediately before being immersed in water is 600° C. or higher, and by rapidly cooling it, the electrode coating on the substrate can be completely and easily peeled off and removed. The reason why the series of treatments of the present invention achieves the excellent effect of easily peeling and removing the coating from the substrate is not clear, but it is because the effect of thermal shock caused by heating and quenching is promoted by the inorganic salt aqueous solution immersion treatment performed in advance. I think that the.
実施例 １
工業的に水銀法食塩電解に陽極として使用した
金属電極の電極板（厚さ1.5mmのエキスパンドチ
タン網を基体としたもの）を30mm×30mm角に切断
し、供試した。Example 1 An electrode plate of a metal electrode (based on an expanded titanium mesh having a thickness of 1.5 mm) used industrially as an anode in mercury salt electrolysis was cut into a 30 mm x 30 mm square and used as a test sample.
該電極板には、片面（Ａ面）に約1μｍ、他面
（Ｂ面）に約3μｍの厚さのルテニウム酸化物と、
チタン酸化物を主成分とする被覆層が残存してい
た。 The electrode plate has ruthenium oxide with a thickness of about 1 μm on one side (side A) and about 3 μm on the other side (side B),
A coating layer mainly composed of titanium oxide remained.
次に該試料を(1)1M・NaCl水溶液に約１分間浸
漬した後、電気炉中で850℃に５分間保持し、直
ちに水中に投入した。その結果、被覆層はＡ面、
Ｂ面とも完全に剥離し、チタン基体の金属光沢が
目視された。更にＸ線マイクロアナライザーで、
被覆が十分除去されていることが確認された。 Next, the sample was immersed in (1) a 1M NaCl aqueous solution for about 1 minute, kept at 850°C for 5 minutes in an electric furnace, and immediately put into water. As a result, the coating layer is A side,
Both sides of B were completely peeled off, and the metallic luster of the titanium substrate was visually observed. Furthermore, with an X-ray microanalyzer,
It was confirmed that the coating had been sufficiently removed.
また、同じ試料を(2)0.1M NaCl水溶液及び(3)
5M NaCl水溶液に浸漬して同様の処理を行つた
結果、(2)の場合、Ｂ面は完全に剥離し、Ａ面は少
量残留物が見られたが、ブラシ掛けにより簡単に
除くことができた。(3)の場合、AB面をも完全に
剥離した。 In addition, the same sample was added to (2) 0.1M NaCl aqueous solution and (3)
As a result of immersion in a 5M NaCl aqueous solution and the same treatment, in case (2), the B side was completely peeled off, and a small amount of residue was observed on the A side, but it could be easily removed by brushing. Ta. In case (3), the AB surface was also completely peeled off.
尚、比較のため、同じ試料を無機塩水溶液に浸
漬処理せずに、850℃に５分間保持し、その後、
室温まで大気中で放冷した。その結果、AB両面
とも被覆が残留し、被覆層の薄いＡ面はブラシ掛
けを行つても被覆を除去することができなかつ
た。 For comparison, the same sample was held at 850°C for 5 minutes without immersion treatment in an inorganic salt aqueous solution, and then
It was allowed to cool to room temperature in the atmosphere. As a result, the coating remained on both sides of A and B, and the coating could not be removed from side A, where the coating layer was thin, even when brushing was performed.
実施例 ２
実施例１におけるNaCl水溶液を種々の無機塩
水溶液に代えて実施例１と同様に電極被覆の除去
を行つた。無機塩の濃度はいずれも1Mとした。
その結果、KCl、MgCl2、CaCl2、BaCl2を使用
した場合、いずれも良好な剥離効果が得られた。
また、Na2SO4、K2SO4、MgSO4、NaNO3、
KNO3、Mg（NO3）2を使用した場合、上記の塩化
物を使用した場合より、やや効果が劣るが十分使
用できることがわかつた。Example 2 The electrode coating was removed in the same manner as in Example 1 except that the NaCl aqueous solution in Example 1 was replaced with various inorganic salt aqueous solutions. The concentration of inorganic salt was 1M in all cases.
As a result, when KCl, MgCl 2 , CaCl 2 , and BaCl 2 were used, good peeling effects were obtained in all cases.
Also, Na 2 SO 4 , K 2 SO 4 , MgSO 4 , NaNO 3 ,
It was found that when KNO 3 and Mg(NO 3 ) 2 were used, the effect was slightly lower than when the above-mentioned chloride was used, but it could be used satisfactorily.
実施例 ３
実施例１と同様に、但し、急冷直前の電極の加
熱温度を(1)800℃、(2)600℃、(3)500℃、(4)300℃に
それぞれ変えて、電極被覆の除去処理を行つた。Example 3 The electrode was coated in the same manner as in Example 1, except that the heating temperature of the electrode immediately before quenching was changed to (1) 800°C, (2) 600°C, (3) 500°C, and (4) 300°C. The removal process was carried out.
その結果、(1)、(2)の場合は、AB面とも完全に
剥離していることが確認された。(3)の場合、Ｂ面
は剥離したがＡ面に被覆が尚残留していた。また
(4)の場合は、AB両面に残留していた。 As a result, it was confirmed that in cases (1) and (2), both sides of AB were completely peeled off. In case (3), side B was peeled off, but the coating still remained on side A. Also
In case (4), it remained on both sides of AB.
［発明の効果］
本発明の方法により、使用済等の金属電極から
被覆を、長時間を要せず簡単な処理で容易に除去
できる。また、被覆を十分に除去された基体は容
易に再使用でき、除去された被覆は、夾雑物が少
ないので、白金族金属等の有価成分を回収するプ
ロセスがより容易となる。[Effects of the Invention] According to the method of the present invention, the coating can be easily removed from a used metal electrode by a simple process without requiring a long time. Furthermore, the substrate from which the coating has been sufficiently removed can be easily reused, and the removed coating has less contaminants, making the process of recovering valuable components such as platinum group metals easier.
Claims (1)
を有する金属電極を、アルカリ金属又はアルカリ
土類金属の塩を含む水溶液に浸漬した後、600℃
以上に加熱し、水中にて急冷することを特徴とす
る金属電極より被覆を除去する方法。1. A metal electrode having a coating containing a noble metal or a noble metal oxide on a substrate is immersed in an aqueous solution containing an alkali metal or alkaline earth metal salt, and then heated at 600°C.
A method for removing a coating from a metal electrode, which is characterized by heating the electrode to a temperature above and rapidly cooling it in water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9755384A JPS60243285A (en) | 1984-05-17 | 1984-05-17 | Method for removing cover from metallic electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9755384A JPS60243285A (en) | 1984-05-17 | 1984-05-17 | Method for removing cover from metallic electrode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60243285A JPS60243285A (en) | 1985-12-03 |
| JPS6340875B2 true JPS6340875B2 (en) | 1988-08-12 |
Family
ID=14195429
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9755384A Granted JPS60243285A (en) | 1984-05-17 | 1984-05-17 | Method for removing cover from metallic electrode |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60243285A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0561867U (en) * | 1992-01-30 | 1993-08-13 | 太陽誘電株式会社 | Optical disk storage case |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5115936B2 (en) * | 2009-07-14 | 2013-01-09 | 有限会社シーエス技術研究所 | Method for collecting insoluble metal electrode |
| CN105344694B (en) * | 2015-09-29 | 2017-12-29 | 北京工业大学 | One kind removes carbide surface Al2O3With the method for TiCN composite coatings |
-
1984
- 1984-05-17 JP JP9755384A patent/JPS60243285A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0561867U (en) * | 1992-01-30 | 1993-08-13 | 太陽誘電株式会社 | Optical disk storage case |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60243285A (en) | 1985-12-03 |
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