JPS6136593B2 - - Google Patents
Info
- Publication number
- JPS6136593B2 JPS6136593B2 JP57076953A JP7695382A JPS6136593B2 JP S6136593 B2 JPS6136593 B2 JP S6136593B2 JP 57076953 A JP57076953 A JP 57076953A JP 7695382 A JP7695382 A JP 7695382A JP S6136593 B2 JPS6136593 B2 JP S6136593B2
- Authority
- JP
- Japan
- Prior art keywords
- iridium
- ion exchange
- exchange membrane
- platinum
- plating
- 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
- 238000007747 plating Methods 0.000 claims description 45
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 42
- 239000003014 ion exchange membrane Substances 0.000 claims description 22
- 229910052697 platinum Inorganic materials 0.000 claims description 20
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 18
- 229910052741 iridium Inorganic materials 0.000 claims description 17
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 8
- 150000002504 iridium compounds Chemical class 0.000 claims description 7
- 230000001603 reducing effect Effects 0.000 claims description 4
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 claims description 4
- 238000005341 cation exchange Methods 0.000 claims description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 14
- 239000000243 solution Substances 0.000 description 11
- 239000012670 alkaline solution Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000000872 buffer Substances 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 150000003058 platinum compounds Chemical class 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910000575 Ir alloy Inorganic materials 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229940069078 citric acid / sodium citrate Drugs 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Chemically Coating (AREA)
Description
【発明の詳細な説明】
この発明は、イオン交換膜とりわけカチオン交
換膜に化学メツキにより電極特にアノードを形成
する方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for forming an electrode, particularly an anode, on an ion exchange membrane, particularly a cation exchange membrane, by chemical plating.
最近、フロロカーボンを基材とするカチオン交
換膜の研究のめざましい進歩にともなつて、この
膜に直接電極を形成して、電極反応を行なわせる
SPE電解や燃料電池の研究開発が著しい発展をと
げている。 Recently, with the remarkable progress in research on cation exchange membranes based on fluorocarbon, electrodes can be formed directly on this membrane and electrode reactions can be carried out.
Research and development of SPE electrolysis and fuel cells is making remarkable progress.
イオン交換膜に設けられる電極としては、酸素
過電圧の低いものが要望されている。 There is a demand for electrodes provided in ion exchange membranes that have a low oxygen overvoltage.
イリジウムは白金より低い酸素過電圧を有して
いる。したがつてイリジウムよりなる電極膜を形
成すれば、酸素過電圧の低い電極が得られること
になるが、イリジウムは白金に比べて高価である
上に、電極として必要な導電性を保持するには、
イリジウム量を極端に減らすことができない。そ
こでイリジウムと白金の合金よりなる化学メツキ
層を成することこにより、イリジウム量を減少さ
せることが考えられるが、この場合イリジウムと
白金の還元特性が異なるため、所望のメツキ層が
得られない。 Iridium has a lower oxygen overpotential than platinum. Therefore, if an electrode film made of iridium is formed, an electrode with low oxygen overvoltage can be obtained, but iridium is more expensive than platinum, and in order to maintain the conductivity necessary for an electrode,
It is not possible to drastically reduce the amount of iridium. Therefore, it is possible to reduce the amount of iridium by forming a chemical plating layer made of an alloy of iridium and platinum, but in this case, the desired plating layer cannot be obtained because the reduction properties of iridium and platinum are different.
イリジウムの還元特性について検討したとこ
ろ、塩化イリジウムはアルカリ性においてはヒド
ラジンによつて還元されないが、白金が存在する
と、これが触媒作用を果して、塩化イリジウムが
還元されることがわかつた。 When investigating the reducing properties of iridium, it was found that iridium chloride is not reduced by hydrazine in alkaline conditions, but in the presence of platinum, it acts as a catalyst and reduces iridium chloride.
この発明は上記の知見に基づいてなされたもの
であつて、低価格でかつ酸素過電圧の低い電極層
を形成することのできる方法を提供することを目
的とする。 The present invention has been made based on the above findings, and an object of the present invention is to provide a method that can form an electrode layer at low cost and with a low oxygen overvoltage.
この発明による電極の形成方法は、イオン交換
膜に白金メツキ層を形成せしめ、ついでイリジウ
ム化合物をヒドラジンで還元させて、白金メツキ
層を被覆するイリジウムメツキ層を形成せしめる
ことを特徴とするイオン交換膜における電極の形
成方法である。 The method for forming an electrode according to the present invention includes forming a platinum plating layer on an ion exchange membrane, and then reducing an iridium compound with hydrazine to form an iridium plating layer covering the platinum plating layer. This is a method for forming an electrode.
白金メツキ層の形成は、白金化合物を用いた化
学メツキによつてなされる。白金化合物の代表例
としては塩化白金酸が挙げられる。 The platinum plating layer is formed by chemical plating using a platinum compound. A typical example of the platinum compound is chloroplatinic acid.
イリジウムメツキ層の形成は、イリジウム化合
物とヒドラジンを含みかつPH５〜６に維持された
メツキ液をイオン交換膜の一方の面に保持し、ア
ルカリ溶液を同膜の他方の面から浸透させ、同膜
〓〓〓〓〓
の一方の面上で透過アルカリの存在下にヒドラジ
ンによる還元反応を行なわせる方法か、またはヒ
ドラジンをアルカリ溶液とともにイオン交換膜の
他方の面から浸透させて、やはり同膜の一方の面
上で還元反応を行なわせる方法でなされる。 The iridium plating layer is formed by holding a plating solution containing an iridium compound and hydrazine and maintained at pH 5 to 6 on one side of the ion exchange membrane, and infiltrating the alkaline solution from the other side of the membrane. 〓〓〓〓〓
Either the reduction reaction with hydrazine is carried out on one side of the ion exchange membrane in the presence of a permeated alkali, or the hydrazine is permeated with an alkaline solution from the other side of the ion exchange membrane, and the reduction reaction is carried out on one side of the same membrane. It is done by a method that causes a reaction to occur.
イリジウム化合物の代表例としては塩化イリジ
ウムが挙げられる。またアルカリ溶液としては水
酸化ナトリウム溶液がよく用いられが、もちろん
これに限定されない。メツキ液のPHは、アルカリ
水溶液によつて５〜６に調整され、クエン酸、ク
エン酸ナトリウム系などの緩衝液によりこの範囲
に維持される。メツキ液および／またはアルカリ
液は界面活性剤を含むこともある。界面活性剤の
代表例としては、陰イオン系のものたとえばアル
キルベンゼンスルホン酸ナトリウムが挙げられ
る。 A typical example of the iridium compound is iridium chloride. Further, as the alkaline solution, a sodium hydroxide solution is often used, but of course it is not limited to this. The pH of the plating solution is adjusted to 5 to 6 with an aqueous alkaline solution, and maintained within this range with a buffer such as citric acid or sodium citrate. The plating solution and/or the alkaline solution may also contain a surfactant. Typical examples of surfactants include anionic surfactants, such as sodium alkylbenzenesulfonate.
この発明による電極の形成方法によれば、イオ
ン交換膜に白金メツキ層を形成せしめ、ついでイ
リジウム化合物をヒドラジンで還元させて、白金
メツキ層を被覆するイリジウムメツキ層を形成せ
しめるので、酸素過電圧の低い電極を比較的低価
格で形成することができる。またアルカリがイオ
ン交換膜の他方の面から浸透するので、還元反応
は同膜の一方の面上で透過アルカリの存在下に生
起し、そのため高価な白金化合物およびイリジウ
ム化合物のロスが少なくなり、またイオン交換膜
への付着性のすぐれた電極が形成される。 According to the method for forming an electrode according to the present invention, a platinum plating layer is formed on the ion exchange membrane, and then an iridium compound is reduced with hydrazine to form an iridium plating layer covering the platinum plating layer, so that the oxygen overvoltage is low. Electrodes can be formed at relatively low cost. Also, since the alkali permeates from the other side of the ion exchange membrane, the reduction reaction takes place on one side of the membrane in the presence of the permeating alkali, thus reducing the loss of expensive platinum and iridium compounds, and An electrode with excellent adhesion to the ion exchange membrane is formed.
実施例 １
0.1Mクエン酸・クエン酸ナトリウム系緩衝液
（PH＝６）にH2PtCl6・6H2OとH2NNH2・2HClと
ドデシルベンゼンスルホン酸ナトリウムを、それ
ぞれ重量濃度で0.5％と2.0％と0.8％になるように
溶解し、さらに２％NaOH水溶液を添加してPHを
５〜６に調整し、メツキ液を調製した。Example 1 H 2 PtCl 6 6H 2 O, H 2 NNH 2 2HCl and sodium dodecylbenzenesulfonate were added to a 0.1M citric acid/sodium citrate buffer (PH = 6) at a weight concentration of 0.5%. A plating solution was prepared by dissolving the components at concentrations of 2.0% and 0.8%, and further adding a 2% NaOH aqueous solution to adjust the pH to 5 to 6.
イオン交換膜として米国デユポン社製のイオン
交換膜（商品名：ナフイオン125）を用意し、添
付図面に示すメツキ槽１において上側のメツキ液
ホルダ２と下側のアルカリ液ホルダ３の間にイオ
ン交換膜４を挟持した。そして先に調製したメツ
キ液５をメツキ液ホルダ２にイオン交換膜１cm2当
り0.5ml入れて保持した。またNaOHとドデシル
ベンゼンスルホン酸ナトリウムをそれぞれ0.02重
量％と0.3重量％含むアルカリ水溶液６をマイク
ロポンプで入口７からイオン交換膜１cm2当り２
ml／分の流量で３時間アルカリ液ホルダ３に流入
して、同ホルダ３を満たし、出力８から排出し
た。こうしてイオン交換膜４の一方の面に白金メ
ツキ層を形成した。 An ion exchange membrane (product name: Nafion 125) manufactured by DuPont in the United States was prepared as an ion exchange membrane, and ion exchange was carried out between the upper plating liquid holder 2 and the lower alkaline liquid holder 3 in the plating tank 1 shown in the attached drawing. Membrane 4 was sandwiched. Then, 0.5 ml of the plating solution 5 prepared earlier was put into the plating solution holder 2 per 1 cm 2 of the ion exchange membrane and held. In addition, an alkaline aqueous solution 6 containing 0.02% by weight and 0.3% by weight of NaOH and sodium dodecylbenzenesulfonate, respectively, was added to the inlet 7 using a micropump at a rate of 2 per 1 cm 2 of the ion exchange membrane.
The alkaline solution flowed into the lye holder 3 for 3 hours at a flow rate of ml/min, filling the holder 3 and discharging through the output 8. In this way, a platinum plating layer was formed on one side of the ion exchange membrane 4.
つぎに、H2PtCl6・6H2Oの代わりにIrCl4を0.2
％含むメツキ液を用いる点を除いて上記と同一条
件で、上記化学メツキ操作を再度実施し、白金メ
ツキ層の上にイリジウムメツキ層を形成した。こ
うしてイオン交換膜４の一方の面に白金層とこれ
を被覆するイリジウム層よりなるメツキ層９を形
成した。 Next, add 0.2 IrCl 4 instead of H 2 PtCl 6 6H 2 O.
The above chemical plating operation was carried out again under the same conditions as above except that a plating solution containing % of the plating solution was used to form an iridium plating layer on the platinum plating layer. In this way, a plating layer 9 consisting of a platinum layer and an iridium layer covering the platinum layer was formed on one surface of the ion exchange membrane 4.
上記メツキ層を有するイオン交換膜をヒドラジ
ンのアルカリ水溶液に浸漬したところ、気泡が発
生した。イリジウムはアルカリ性でヒドラジンを
分解する性質を有するので、上記気泡の発生によ
り白金とともにイリジウムがメツキされたことが
証明された。 When the ion exchange membrane having the plating layer was immersed in an alkaline aqueous solution of hydrazine, bubbles were generated. Since iridium is alkaline and has the property of decomposing hydrazine, the generation of the bubbles proved that iridium was plated together with platinum.
つぎに、イオン交換膜４をメツキ槽１から外し
て、これを上下逆にして再びメツキ液ホルダ２と
アルカリ液ホルダ３の間に挟持した。そして、
H2PtCl6・6H2Oを含む上記メツキ液を用いて上記
と同一条件で、上記化学メツキ操作をもう一度実
施した。こうしてイオン交換膜の他方の面に白金
のメツキ層を形成した。 Next, the ion exchange membrane 4 was removed from the plating tank 1, turned upside down, and again sandwiched between the plating liquid holder 2 and the alkaline liquid holder 3. and,
The above chemical plating operation was performed once again using the above plating solution containing H 2 PtCl 6 .6H 2 O under the same conditions as above. In this way, a platinum plating layer was formed on the other side of the ion exchange membrane.
こうして製作したSPEを用いて、イリジウムを
含むメツキ層をアノードとし、白金メツキ層をカ
ソードとし、白金メツキしたチタン製エキスパン
ドメタルを電極コレクタとしたSPE電解槽で、水
の電解を行なつた。この場合の電流−電圧曲線を
第２図に示す。また白金のみをメツキしてなるア
ノードを用いた場合の同曲線も、同図に示した。
これらの曲線の比較から明らかなように、この実
施例で形成したアノードを備えたSPEを用いれ
ば、高い電流密度でも低い電圧で電解を行なうこ
とができる。 Using the SPE fabricated in this way, water was electrolyzed in an SPE electrolytic cell with a plating layer containing iridium as an anode, a platinum plating layer as a cathode, and a platinum-plated expanded titanium metal as an electrode collector. The current-voltage curve in this case is shown in FIG. The same curve is also shown in the same figure when an anode plated only with platinum is used.
As is clear from the comparison of these curves, by using the SPE with the anode formed in this example, electrolysis can be performed at a low voltage even at a high current density.
実施例 ２
イリジウムメツキ層の形成工程において、
H2NNH2・2HClがメツキ液に含まれないで、アル
カリ水溶液に0.5％含まれ、同水溶液のPHが１％
NaOHで12に調整されており、同水溶液をボルダ
３に５時間流す点を除いて、実施例１と同一条件
で、メツキ操作を繰返し、得られたSPEを用いて
実施例１と同一条件で水の電解を行なつた。その
結果温度95℃、電流密度１A/cm2の電解条件で、
〓〓〓〓〓
電解槽電圧は1.69Vであり、実施例１の場合とほ
ぼ等しい（第２図）。Example 2 In the process of forming an iridium plating layer,
H 2 NNH 2・2HCl is not included in the plating solution, but is included in the alkaline aqueous solution at 0.5%, and the pH of the aqueous solution is 1%.
12 with NaOH, and the plating operation was repeated under the same conditions as in Example 1, except that the same aqueous solution was passed through Boulder 3 for 5 hours. Using the obtained SPE, the plating operation was performed under the same conditions as in Example 1. Performed water electrolysis. As a result, under the electrolytic conditions of a temperature of 95℃ and a current density of 1A/ cm2 ,
〓〓〓〓〓
The electrolytic cell voltage was 1.69V, which was almost the same as in Example 1 (FIG. 2).
第１図は、この発明の実施例で用いたメツキ槽
を示す垂直断面図、第２図は電流密度と槽電圧の
関係を示すグラフである。
２……メツキ液ホルダ、３……アルカリ液ホル
ダ、４……イオン交換膜、９……メツキ層。
〓〓〓〓〓
FIG. 1 is a vertical sectional view showing a plating tank used in an example of the present invention, and FIG. 2 is a graph showing the relationship between current density and tank voltage. 2... Plating liquid holder, 3... Alkaline liquid holder, 4... Ion exchange membrane, 9... Plating layer. 〓〓〓〓〓
Claims (1)
ついでイリジウム化合物をヒドラジンで還元させ
て、白金メツキ層を被覆するイリジウムメツキ層
を形成せしめることを特徴とするイオン交換膜に
おける電極の形成方法。 ２ イリジウム化合物が塩化イリジウムである特
許請求の範囲第１項記載の方法。 ３ イオン交換膜がカチオン交換膜である特許請
求の範囲第１または２項記載の方法。[Claims] 1. Forming a platinum plating layer on an ion exchange membrane,
1. A method for forming an electrode in an ion exchange membrane, comprising: then reducing an iridium compound with hydrazine to form an iridium plating layer covering the platinum plating layer. 2. The method according to claim 1, wherein the iridium compound is iridium chloride. 3. The method according to claim 1 or 2, wherein the ion exchange membrane is a cation exchange membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57076953A JPS58193380A (en) | 1982-05-07 | 1982-05-07 | Formation of electrode in ion-exchange membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57076953A JPS58193380A (en) | 1982-05-07 | 1982-05-07 | Formation of electrode in ion-exchange membrane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58193380A JPS58193380A (en) | 1983-11-11 |
| JPS6136593B2 true JPS6136593B2 (en) | 1986-08-19 |
Family
ID=13620137
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57076953A Granted JPS58193380A (en) | 1982-05-07 | 1982-05-07 | Formation of electrode in ion-exchange membrane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58193380A (en) |
-
1982
- 1982-05-07 JP JP57076953A patent/JPS58193380A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58193380A (en) | 1983-11-11 |
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