CN102703925A - Production process of double-coating combined electrode - Google Patents
Production process of double-coating combined electrode Download PDFInfo
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- CN102703925A CN102703925A CN201210118140XA CN201210118140A CN102703925A CN 102703925 A CN102703925 A CN 102703925A CN 201210118140X A CN201210118140X A CN 201210118140XA CN 201210118140 A CN201210118140 A CN 201210118140A CN 102703925 A CN102703925 A CN 102703925A
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Abstract
The invention discloses a production process of a double-coating combined electrode. The production process of the double-coating combined electrode includes the steps of using a titanium plate as a substrate; preparing quality precious-metal organic solution, performing ultrasonic oscillation for dissolution, and allowing for standing; adding SnC12 into the precious-metal organic solution after standing to obtain mixed solution, and allowing for standing of the mixed solution for standby; evenly multi-coating the prepared mixed solution to one side of the substrate to form a chlorine-evolving electrode layer; heating the substrate with the coated electrode layer on one side, and holding temperature; and grinding the other side of the heated titanium substrate to remove an oxide layer, and preparing a hydrogen-evolving electrode layer on the other side of the substrate by electroplating process. By the electrolytic cell electrode produced by the production process, using effect of an original single-coating electrode is changed. The double-coating combined electrode is produced by processing two sides of an electrode substrate. Therefore, electric energy is economized, materials for electrolytic plates are also economized, and service life of a plate electrode can be prolonged.
Description
Technical field
The present invention relates to be used for the battery lead plate of electrolyzer, be specifically related to a kind of combined electrode preparation technology of coated on both sides.
Background technology
In the coated electrode preparation of prior art, generally adopt the surface of thermolysis or electric plating method counter electrode base material to process.In the preparation process, general only the employing with an a kind of technology surface or two surfaces to base material processed.This method had both been wasted base material, and in practical application, can increase the internal resistance of electrolyzer.In original design of electrolysis cells, multipole type electricity groove is that the electrode with two opposed polarities is welded on the electrolyzer both sides, and the acyclic type electrolyzer to be electrode with two identical polars be welded on the electrolyzer both sides.In actual production, there is following shortcoming in this circuit that constitutes through welding process: increased the electrolyzer internal resistance, wasted energy, in electrolytic process, solder joint may generate heat and influence work-ing life of electrode, also wastes electrode materials simultaneously.
Summary of the invention
The objective of the invention is to overcome the defective that exists in the prior art, provide a kind of simple in structure, the electrolyzer internal resistance is little in the use, long service life, and the combined electrode preparation technology of a kind of coated on both sides of saving material.
For realizing above-mentioned purpose, technical scheme of the present invention is the combined electrode preparation technology of a kind of coated on both sides of design, it is characterized in that said preparation technology comprises following process step:
S1: adopt purity greater than 99.0% metallic titanium plate as substrate, and clean through pre-treatment;
S2: configuration quality per-cent is 1～10% precious metal organic solution, adopts the ultra-sonic oscillation dissolving, leaves standstill;
S3: add SnCl in the precious metal organic solution after S2 step left standstill
2Form mixing solutions, SnCl
2In the mixing solutions mass percent is 0.5～2%, leaves standstill, for use;
S4: the mixed solutions for many times that will pass through S3 step configuration is coated in S1 is ready to substrate in the step one side equably and forms and have the electrode layer of analysing the chlorine performance;
S5: the substrate of single face coated electrode layer in S4 step is heated to 200～500 ℃, and soaking time is 2～3 hours;
S6: the another side of titanium-base after the heat treated in S5 step is removed zone of oxidation through polishing, utilize electroplating technology another side to be processed electrode layer then with liberation of hydrogen performance.
Wherein optimized technical scheme is, the precious metal organic solution of said S1 in the step is RuCl
3, RhCl
3, PdCl
3, OsCl
3, Lr Cl
3With Pt Cl
3In the organic liquor of any one or its any combination.
Optimized technical scheme also has, and said S1 is pre-treatment cleaning employing abrasive paper for metallograph sanding and polishing in the step, the acetone oil removing, and alkali lye adds heat soaking, and mixing acid cleans, and uses the deionized water ultrasonic cleaning; Wherein the dipping by lye temperature is 80～120 ℃, and the time is 5～10 minutes; The alkali lye composition is NaOH, NaHCO
3And Na
3PO
4Mixed aqueous solution, the mass percent concentration of three kinds of compositions in mixed aqueous solution is 2～10%; Mixing acid scavenging period 40～80 seconds, each composition volume ratio of mixing acid is: volume percent is 40% hydrofluoric acid aqueous solution: 1.40gcm
-3Nitric acid: 1.84gcm
-3Sulfuric acid=5～15: 2～10: 1～5.
Optimized technical scheme also has, and said S2 is configuration precious metal organic solution in the step, and the organic solvent of use is ethanol, propyl alcohol, butanols, formic acid or acetate.
Optimized technical scheme also has, and time of repose was 12～24 hours during said S3 went on foot.
Optimized technical scheme also has, and said S4 after each the coating, applies after 5～20 minutes with 30～50 ℃ of temperature dryings in drying baker in the step more next time, repeats repeatedly to apply, and the final thickness of the film of coating remains on 10～50 μ m.
Optimized technical scheme also has, and the substrate heat temperature raising speed to single face coated electrode layer during said S5 goes on foot is 3～8 ℃/second.
Optimized technical scheme also has, and the electroplating technology of said S6 in the step is the one side nickel plating at titanium-base, and its thickness of coating is 2～10 μ m.
Further optimized technical scheme also has, and the composition of the nickel-plating liquid that said nickel plating technology adopts is: the NiSO of 25～40g/L
47H
2O, the NaH of 10～25g/L
2PO
2H
2O, the NH of 40～60g/L
4Cl, the Na of 70～90g/L
3C
6H
5O
72H
2O; Its pH value is 8～9.5; Technological temperature is 75～90 ℃, and the process time is 8～20 minutes.
Advantage of the present invention and beneficial effect are: adopt the electrolyzer of this explained hereafter to use electrode, changed the result of use of original single face coated electrode, the two sides through the counter electrode base material processes, and prepares a kind of combined electrode of coated on both sides.In the preparation process; Different processes is adopted on two surfaces through the counter electrode base material; Produce a kind of two surfaces and have the electrode that difference is separated out performance at a substrate; Thereby in electrolytic process, two surfaces of electrode are carried out plaing a part in the electrolytic reaction process different in electrolyzer separately.Use electrolysis to be example with chlorine industry, first one side at the titanium base material is prepared into through the pyrolysated method has the electrode of analysing the chlorine performance, after another side is removed zone of oxidation through polishing, utilizes electroplating technology to prepare a kind of electrode with liberation of hydrogen performance then.In the combined electrolytic cell structure; The battery lead plate that only needs to be positioned at both sides is connected with the positive and negative electrode of power supply; And be positioned at the intermediary battery lead plate under the effect of inductive emf; Be sensed as in the one side of substrate and have the positive pole of analysing chlorine property, be sensed as negative pole, thereby avoided the internal resistance that contacts between electrode and pole with liberation of hydrogen property at the another side of substrate.So both save electric energy, also saved the material of electrolytic zinc-coated steel sheet, can also prolong the work-ing life of battery lead plate simultaneously.
Embodiment
Below in conjunction with accompanying drawing and embodiment, specific embodiments of the invention further describes.Following examples only are used for technical scheme of the present invention more clearly is described, and can not limit protection scope of the present invention with this.
Embodiment 1
The present invention is a kind of combined electrode preparation technology of coated on both sides, and this preparation technology comprises following process step:
S1: adopt purity greater than 99.0% metallic titanium plate as substrate, and clean through pre-treatment;
S2: configuration quality per-cent is 1% precious metal organic solution, adopts the ultra-sonic oscillation dissolving, leaves standstill;
S3: add SnCl in the precious metal organic solution after S2 step left standstill
2Form mixing solutions, SnCl
2In the mixing solutions mass percent is 0.5%, leaves standstill, for use;
S4: the mixed solutions for many times that will pass through S3 step configuration is coated in S1 is ready to substrate in the step one side equably and forms and have the electrode layer of analysing the chlorine performance;
S5: the substrate of single face coated electrode layer in S4 step is heated to 200 ℃, and soaking time is 2 hours;
S6: the another side of titanium-base after the heat treated in S5 step is removed zone of oxidation through polishing, utilize electroplating technology another side to be processed electrode layer then with liberation of hydrogen performance.
Wherein embodiment preferred is, the precious metal organic solution of said S1 in the step is RuCl
3With RhCl
3Blended machine solution.
Embodiment preferred also has, and said S1 is pre-treatment cleaning employing abrasive paper for metallograph sanding and polishing in the step, the acetone oil removing, and alkali lye adds heat soaking, and mixing acid cleans, and uses the deionized water ultrasonic cleaning; Wherein the dipping by lye temperature is 80 ℃, and the time is 5 minutes; The alkali lye composition is NaOH, NaHCO
3And Na
3PO
4Mixed aqueous solution, the mass percent concentration of three kinds of compositions in mixed aqueous solution is 2～10%; Mixing acid scavenging period 40 seconds, each composition volume ratio of mixing acid is: volume percent is 40% hydrofluoric acid aqueous solution: 1.40gcm
-3Nitric acid: 1.84gcm
-3Sulfuric acid=5: 2: 1.
Embodiment preferred also has, and said S2 is configuration precious metal organic solution in the step, and the organic solvent of use is ethanol, propyl alcohol, butanols, formic acid or acetate.
Embodiment preferred also has, and time of repose was 12 hours during said S3 went on foot.
Embodiment preferred also has, and said S4 after each the coating, applies after 5 minutes with 30 ℃ of temperature dryings in drying baker in the step more next time, repeats repeatedly to apply, and the final thickness of the film of coating remains on 10 μ m.
Embodiment preferred also has, and the substrate heat temperature raising speed to single face coated electrode layer during said S5 goes on foot is 3 ℃/second.
Embodiment preferred also has, and the electroplating technology of said S6 in the step is the one side nickel plating at titanium-base, and its thickness of coating is 2 μ m.
Further preferred embodiment also has, and the composition of the nickel-plating liquid that said nickel plating technology adopts is: the NiSO of 25g/L
47H
2O, the NaH of 10g/L
2PO
2H
2O, the NH of 40g/L
4Cl, the Na of 70g/L
3C
6H
5O
72H
2O; Its pH value is 8～9.5; Technological temperature is 75 ℃, and the process time is 8 minutes.
Embodiment 2
The present invention is a kind of combined electrode preparation technology of coated on both sides, and this preparation technology comprises following process step:
S1: adopt purity greater than 99.0% metallic titanium plate as substrate, and clean through pre-treatment;
S2: configuration quality per-cent is 10% precious metal organic solution, adopts the ultra-sonic oscillation dissolving, leaves standstill;
S3: add SnCl in the precious metal organic solution after S2 step left standstill
2Form mixing solutions, SnCl
2In the mixing solutions mass percent is 2%, leaves standstill, for use;
S4: the mixed solutions for many times that will pass through S3 step configuration is coated in S1 is ready to substrate in the step one side equably and forms and have the electrode layer of analysing the chlorine performance;
S5: the substrate of single face coated electrode layer in S4 step is heated to 500 ℃, and soaking time is 3 hours;
S6: the another side of titanium-base after the heat treated in S5 step is removed zone of oxidation through polishing, utilize electroplating technology another side to be processed electrode layer then with liberation of hydrogen performance.
Wherein embodiment preferred is, the precious metal organic solution of said S1 in the step is PdCl
3With OsCl
3Blended machine solution.
Embodiment preferred also has, and said S1 is pre-treatment cleaning employing abrasive paper for metallograph sanding and polishing in the step, the acetone oil removing, and alkali lye adds heat soaking, and mixing acid cleans, and uses the deionized water ultrasonic cleaning; Wherein the dipping by lye temperature is 120 ℃, and the time is 10 minutes; The alkali lye composition is NaOH, NaHCO
3And Na
3PO
4Mixed aqueous solution, the mass percent concentration of three kinds of compositions in mixed aqueous solution is 2～10%; Mixing acid scavenging period 80 seconds, each composition volume ratio of mixing acid is: volume percent is 40% hydrofluoric acid aqueous solution: 1.40gcm
-3Nitric acid: 1.84gcm
-3Sulfuric acid=15: 10: 5.
Embodiment preferred also has, and said S2 is configuration precious metal organic solution in the step, and the organic solvent of use is ethanol, propyl alcohol, butanols, formic acid or acetate.
Embodiment preferred also has, and time of repose was 24 hours during said S3 went on foot.
Optimized technical scheme also has, and said S4 after each the coating, applies after 20 minutes with 50 ℃ of temperature dryings in drying baker in the step more next time, repeats repeatedly to apply, and the final thickness of the film of coating remains on 50 μ m.
Embodiment preferred also has, and the substrate heat temperature raising speed to single face coated electrode layer during said S5 goes on foot is 8 ℃/second.
Embodiment preferred also has, and the electroplating technology of said S6 in the step is the one side nickel plating at titanium-base, and its thickness of coating is 10 μ m.
Further preferred embodiment also has, and the composition of the nickel-plating liquid that said nickel plating technology adopts is: the NiSO of 40g/L
47H
2O, the NaH of 25g/L
2PO
2H
2O, the NH of 60g/L
4Cl, the Na of 90g/L
3C
6H
5O
72H
2O; Its pH value is 8～9.5; Technological temperature is 90 ℃, and the process time is 20 minutes.
Embodiment 3
The combined electrode preparation technology of a kind of coated on both sides of the present invention, this preparation technology comprises following process step:
S1: adopt purity greater than 99.0% metallic titanium plate as substrate, and clean through pre-treatment;
S2: configuration quality per-cent is 5% precious metal organic solution, adopts the ultra-sonic oscillation dissolving, leaves standstill;
S3: add SnCl in the precious metal organic solution after S2 step left standstill
2Form mixing solutions, SnCl
2In the mixing solutions mass percent is 1.25%, leaves standstill, for use;
S4: the mixed solutions for many times that will pass through S3 step configuration is coated in S1 is ready to substrate in the step one side equably and forms and have the electrode layer of analysing the chlorine performance;
S5: the substrate of single face coated electrode layer in S4 step is heated to 350 ℃, and soaking time is 2～3 hours;
S6: the another side of titanium-base after the heat treated in S5 step is removed zone of oxidation through polishing, utilize electroplating technology another side to be processed electrode layer then with liberation of hydrogen performance.
Wherein embodiment preferred is that the precious metal organic solution of said S1 in the step is LrCl
3With PtCl
3Blended machine solution.
Embodiment preferred also has, and said S1 is pre-treatment cleaning employing abrasive paper for metallograph sanding and polishing in the step, the acetone oil removing, and alkali lye adds heat soaking, and mixing acid cleans, and uses the deionized water ultrasonic cleaning; Wherein the dipping by lye temperature is 100 ℃, and the time is 7.5 minutes; The alkali lye composition is NaOH, NaHCO
3And Na
3PO
4Mixed aqueous solution, the mass percent concentration of three kinds of compositions in mixed aqueous solution is 6%; Mixing acid scavenging period 60 seconds, each composition volume ratio of mixing acid is: volume percent is 40% hydrofluoric acid aqueous solution: 1.40gcm
-3Nitric acid: 1.84gcm
-3Sulfuric acid=10: 6: 2.5.
Embodiment preferred also has, and said S2 is configuration precious metal organic solution in the step, and the organic solvent of use is ethanol, propyl alcohol, butanols, formic acid or acetate.
Embodiment preferred also has, and time of repose was 18 hours during said S3 went on foot.
Optimized technical scheme also has, and said S4 after each the coating, applies after 17.5 minutes with 40 ℃ of temperature dryings in drying baker in the step more next time, repeats repeatedly to apply, and the final thickness of the film of coating remains on 12.5 μ m.
Embodiment preferred also has, and the substrate heat temperature raising speed to single face coated electrode layer during said S5 goes on foot is 5.5 ℃/second.
Embodiment preferred also has, and the electroplating technology of said S6 in the step is the one side nickel plating at titanium-base, and its thickness of coating is 6 μ m.
Further preferred embodiment also has, and the composition of the nickel-plating liquid that said nickel plating technology adopts is: the NiSO of 32.5g/L
47H
2O, the NaH of 12.5g/L
2PO
2H
2O, the NH of 50g/L
4Cl, the Na of 80g/L
3C
6H
5O
72H
2O; Its pH value is 8～9.5; Technological temperature is 82.5 ℃, and the process time is 13.5 minutes.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from know-why of the present invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (9)
1. the combined electrode preparation technology of a coated on both sides is characterized in that, said preparation technology comprises following process step:
S1: adopt purity greater than 99.0% metallic titanium plate as substrate, and clean through pre-treatment;
S2: configuration quality per-cent is 1～10% precious metal organic solution, adopts the ultra-sonic oscillation dissolving, leaves standstill;
S3: add SnCl in the precious metal organic solution after S2 step left standstill
2Form mixing solutions, SnCl
2In the mixing solutions mass percent is 0.5～2%, leaves standstill, for use;
S4: the mixed solutions for many times that will pass through S3 step configuration is coated in S1 is ready to substrate in the step one side equably and forms and have the electrode layer of analysing the chlorine performance;
S5: the substrate of single face coated electrode layer in S4 step is heated to 200～500 ℃, and soaking time is 2～3 hours;
S6: the another side of titanium-base after the heat treated in S5 step is removed zone of oxidation through polishing, utilize electroplating technology another side to be processed electrode layer then with liberation of hydrogen performance.
2. the combined electrode preparation technology of coated on both sides as claimed in claim 1 is characterized in that, the precious metal organic solution of said S1 in the step is RuCl
3, RhCl
3, PdCl
3, OsCl
3, LrCl
3And PtCl
3In the organic liquor of any one or its any combination.
3. the combined electrode preparation technology of coated on both sides as claimed in claim 1 is characterized in that, said S1 is pre-treatment cleaning employing abrasive paper for metallograph sanding and polishing in the step, the acetone oil removing, and alkali lye adds heat soaking, and mixing acid cleans, and uses the deionized water ultrasonic cleaning; Wherein the dipping by lye temperature is 80～120 ℃, and the time is 5～10 minutes; The alkali lye composition is NaOH, NaHCO
3And Na
3PO
4Mixed aqueous solution, the mass percent concentration of three kinds of compositions in mixed aqueous solution is 2～10%; Mixing acid scavenging period 40～80 seconds, each composition volume ratio of mixing acid is: volume percent is 40% hydrofluoric acid aqueous solution: 1.40gcm
-3Nitric acid: 1.84gcm
-3Sulfuric acid=5～15: 2～10: 1～5.
4. the combined electrode preparation technology of coated on both sides as claimed in claim 2 is characterized in that, said S2 is configuration precious metal organic solution in the step, and the organic solvent of use is ethanol, propyl alcohol, butanols, formic acid or acetate.
5. the combined electrode preparation technology of coated on both sides as claimed in claim 1 is characterized in that, time of repose was 12～24 hours during said S3 went on foot.
6. the combined electrode preparation technology of coated on both sides as claimed in claim 1; It is characterized in that; After said S4 applied in the step at every turn; In drying baker, apply after 5～20 minutes with 30～50 ℃ of temperature dryings next time again, repeat repeatedly to apply, the final thickness of the film of coating remains on 10～50 μ m.
7. the combined electrode preparation technology of coated on both sides as claimed in claim 1 is characterized in that, the substrate heat temperature raising speed to single face coated electrode layer during said S5 goes on foot is 3～8 ℃/second.
8. the combined electrode preparation technology of coated on both sides as claimed in claim 1 is characterized in that, the electroplating technology of said S6 in the step is the one side nickel plating at titanium-base, and its thickness of coating is 2～10 μ m.
9. the combined electrode preparation technology of coated on both sides as claimed in claim 8 is characterized in that, the composition of the nickel-plating liquid that said nickel plating technology adopts is: the NiSO of 25～40g/L
47H
2O, the NaH of 10～25g/L
2PO
2H
2O, the NH of 40～60g/L
4Cl, the Na of 70～90g/L
3C
6H
5O
72H
2O; Its pH value is 8～9.5; Technological temperature is 75～90 ℃, and the process time is 8～20 minutes.
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|---|---|---|---|
| CN201210118140.XA CN102703925B (en) | 2012-04-23 | 2012-04-23 | Production process of double-coating combined electrode |
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|---|---|---|---|
| CN201210118140.XA CN102703925B (en) | 2012-04-23 | 2012-04-23 | Production process of double-coating combined electrode |
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| CN102703925B CN102703925B (en) | 2014-12-17 |
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ID=46896966
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103103561A (en) * | 2012-12-13 | 2013-05-15 | 苏州新区化工节能设备厂 | Tubular titanium anode |
| CN104532291A (en) * | 2014-12-22 | 2015-04-22 | 江阴安凯特电化学设备有限公司 | Processing technique of tantalum protection layer electrode |
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| CN104532291A (en) * | 2014-12-22 | 2015-04-22 | 江阴安凯特电化学设备有限公司 | Processing technique of tantalum protection layer electrode |
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| Publication number | Publication date |
|---|---|
| CN102703925B (en) | 2014-12-17 |
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| C14 | Grant of patent or utility model | ||
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| C56 | Change in the name or address of the patentee | ||
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Address after: 214400, No. 221 East Road, Jiangyin Town Industrial Park, Jiangsu, China Patentee after: Jiangsu ankaite Polytron Technologies Inc Address before: 214400, No. 221 East Road, Jiangyin Town Industrial Park, Jiangsu, China Patentee before: Jiangyin Ancan Electrochemical Equipment Co., Ltd. |