CN104005047A - Novel mixed metal oxide electrode for low-temperature sea water electrolysis antifouling - Google Patents
Novel mixed metal oxide electrode for low-temperature sea water electrolysis antifouling Download PDFInfo
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- CN104005047A CN104005047A CN201410257504.1A CN201410257504A CN104005047A CN 104005047 A CN104005047 A CN 104005047A CN 201410257504 A CN201410257504 A CN 201410257504A CN 104005047 A CN104005047 A CN 104005047A
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Abstract
The invention provides a novel mixed metal oxide electrode for low-temperature sea water electrolysis antifouling. The novel mixed metal oxide electrode comprises an electrode matrix and a multiple-mixed-precious-metal-oxide coating. Compared with the prior art, the novel mixed metal oxide electrode for low-temperature sea water electrolysis antifouling has high chlorine evolution current efficiency and low chlorine evolution potential, chlorine evolution and oxygen evolution reaction selectivity of the electrode is improved, the service life is obviously prolonged, comprehensive performance of the electrode is remarkably improved, and the electrode is applicable to sea water electrolysis antifouling, sodium hypochlorite electrolysis production, ship ballast water treatment and the like in the low-temperature sea water chlorine evolution environment.
Description
Technical field
The present invention relates to technical field of electrochemistry, relate in particular to the antifouling mixed metal oxide electrode of using of a kind of novel electrolysis low temperature seawater.
Background technology
Electrolyzing seawater antifouling technique is to utilize to analyse chlorine active anode electrolytic seawater generation available chlorine, and available chlorine can hit dizzy or kill spore and the larva of marine life and marine life, thereby reach, prevents marine life growth and breeding, the object of adhering to.That electrolyzing seawater antifouling technique has is safe and reliable, convenient management, good antifouling effect, environmentally safe, economic dispatch advantage comparatively, is widely used in the field such as seawaterline anti-fouling system, ship ballast water treatment system of Coastal Power Plant.In electrolytic seawater antifouling system, anode is core building block, and its use properties and life-span directly determine anti-fouling effect.Electrolysis antifouling should have high reaction preference with anode, high current efficiency, work that can be efficient, stable in higher current density and wide temperature range.Ti-support metal oxide anode is a kind of dimensional stabilizing type anode, by applying one deck precious metal oxide coating on titanium matrix, forms, and itself has good corrosion resistance, rate of consumption is low, electrochemical activity is high, the advantage such as cheap is widely used.The main RuO that adopts in the antifouling engineering of current electrolysis seawater
2-IrO
2-SnO
2, Ru O
2-Ti O
2-IrO
2on ruthenium series metal oxide anode.
In electrolytic seawater antifouling system, seawater temperature alters a great deal with the difference in season and marine site, and the low energy of Bohai Sea in Winter seawater temperature reaches 0 ℃, and the highest water temperature of South China Sea In Summer can reach more than 35 ℃.In Practical Project, find, when seawater temperature is during lower than 10 ℃, conventional ruthenium series metal oxide anodic current efficiency sharply declines at present, and electrolytic bath is pressed significantly and raise, and antianode causes expendable destruction simultaneously, and obviously shorten work-ing life.Document [Zhang Shengjian, seawater temperature is on the impact of metal oxide anode intensified electrolysis failure behaviour, Rare Metals Materials and engineering, 2013,42 (12): 2613-2617] has been analyzed RuO under cold condition
2-IrO
2-SnO
2intensified electrolysis failure behaviour and the mechanism of anode, electrolytic seawater process Anodic chlorine evolution potential raises, analyse chlorine oxygen evolution reaction elective reduction, easily analyse oxygen side reaction, destroyed the solid solution structure of oxide coating, thus anode to lose efficacy be mainly that selective dissolution and coating localized delamination due to Ru active component causes.In order to improve broad spectrum and the anti-fouling effect of electrolytic seawater antifouling system, require metal oxide anode under low temperature seawater condition, should there is good analysing chlorine current efficiency and longer work-ing life.
Summary of the invention
For existing and analyse the deficiency that chlorine current efficiency is low, work-ing life is shorter under above-mentioned existing metal oxide anode low temperature seawater condition, the invention provides a kind of high-performance electrolysis low temperature seawater antifouling with mixed metal oxide electrode, this electrode has the good chlorine current efficiency of analysing under low temperature seawater condition, the defect of avoiding traditional ruthenium series metal oxide anode active component selective dissolution to come off, significantly improve the stability of electrode, obviously extend work-ing life, is conducive to improve the electrolysis antifouling effect under cold condition.
For solving the problems of the technologies described above, the invention provides a kind of electrolysis low temperature seawater antifouling with mixed metal oxide electrode, it comprises electrode matrix and Diversity precious metal oxide coating.
Described electrode matrix adopts valve metal titanium material to make, and the quality percentage composition of valve metal titanium in electrode matrix is greater than 99%.
The shape of described conducting base can be netted, tabular, tubulose, the structural shape such as bar-shaped.
Described Diversity precious metal oxide coating is P
to
x-S
no
2coating.
Described P
to
x-S
no
2the constitutive molar ratio of composition is P
t: S
n(50～95): (5～50).
Further, described in this, Diversity precious metal oxide coating can also contain platinum element, and it is by P
to
x-S
no
2the C that adds mol ratio 5%～20% in composition
oreplace the wherein S of corresponding proportion
nobtain.
Further, described Diversity precious metal oxide coating is P
to
x-S
no
2-Co
3o
4coating.
Described mixed metal oxide electrode is applied to electrolytic seawater device for preventing fouling due to marine organism, apparatus for treating ship ballast water and clorox electrolysis production device.
The present invention also provides the preparation method of above-mentioned mixed metal oxide electrode, and what it adopted is the preparation of masking liquid presoma thermal decomposition method.
Described preparation method is specially the halogenide metal salt solution of platinum, tin and cobalt by together with the mixed in molar ratio of above-mentioned platinum, tin and cobalt, obtain masking liquid, this masking liquid is adopted the methods such as artificial brushing, dip-coating or spraying be coated on titanium matrix, in oxidizing atmosphere successively through dry at 100～150 ℃ and 450～550 ℃ at the thermal treatment process such as sintering form the titanium base mixed metal oxide electro-catalytic coating conducting electricity.
The present invention also provides the application of above-mentioned mixed metal oxide electrode in the antifouling process of electrolysis low temperature seawater.
Beneficial effect of the present invention:
Compared to the prior art, the electrolysis low temperature seawater that the present invention relates to is antifouling has the good chlorine current efficiency of analysing under low temperature seawater condition with mixed metal oxide electrode, lower chlorine evolution potential, what strengthened electrode analyses chlorine oxygen evolution reaction selectivity, obviously extend work-ing life, significantly improved the over-all properties of electrode, be applicable to low temperature seawater and analyse electrolysis antifouling under chlorine environment, electrolysis production clorox and ballast for cruising water treatment etc.
Embodiment
The invention provides a kind of electrolysis low temperature seawater antifouling with mixed metal oxide electrode, it comprises electrode matrix and Diversity precious metal oxide coating.
Further, described mixed metal oxide electrode only consists of electrode matrix and Diversity precious metal oxide coating.
Described electrode matrix adopts valve metal titanium material to make, and the quality percentage composition of valve metal titanium in electrode matrix is greater than 99%.
The shape of described conducting base can be netted, tabular, tubulose, the structural shape such as bar-shaped.
Described Diversity precious metal oxide coating is P
to
x-S
no
2coating.
Described P
to
x-S
no
2the constitutive molar ratio of composition is P
t: S
n(50～95): (5～50).
Further, described in this, Diversity precious metal oxide coating can also contain platinum element, and it is by P
to
x-S
no
2the C that adds mol ratio 5%～20% in composition
oreplace the wherein S of corresponding proportion
nobtain.
Further, described Diversity precious metal oxide coating is P
to
x-S
no
2-Co
3o
4coating.
The mixed metal oxide coating the present invention relates to is selected P
to
xas active ingredient, there is higher chlorine electro catalytic activity and the stability analysed, this component chemical state is stable, avoids occurring the problem of activated coating selective dissolution, can provide the stable chlorine active site of analysing to electrode; In addition, in mixed metal oxide coating, add inert component S
no
2, and active ingredient P
to
xmix the stability that improves electrode, form under cold condition and there is the metal oxide anode of well analysing chlorine current efficiency and stability.Work as P
tcontent is lower than 50%, S
ncontent is higher than 50% time, and solidity to corrosion and the catalytic activity of low-temperature electrolytic condition lower electrode are poor; And work as P
tcontent is higher than 95% time, and the performance of Mixed Metal Oxide Coated Titanium Anodes is almost equal to platinum electrode, exists platinum coating wear rate fast, expensive problem, and electrode chlorine evolution potential is higher, and current efficiency is too low.If necessary, can add the addition of C o
3o
4suppress SnO in electrode production process
2the volatilization of component, thereby the stability of raising electrode.When Co content is higher than 20% time, weather resistance that can remarkably influenced electrode.Therefore, when Mixed Metal Oxide Coated Titanium Anodes regulation composition content range time, can make electrode under low-temperature electrolytic condition, obtains optimization over-all properties.
The present invention also provides the preparation method of above-mentioned mixed metal oxide electrode, and what it adopted is the preparation of masking liquid presoma thermal decomposition method.
Described preparation method is specially the halogenide metal salt solution of platinum, tin and cobalt is mixed by certain mol proportion example, obtain masking liquid, this masking liquid is adopted the methods such as artificial brushing, dip-coating or spraying be coated on titanium matrix, in oxidizing atmosphere successively through dry at 100～150 ℃ and 450～550 ℃ at the thermal treatment process such as sintering form the titanium base mixed metal oxide electro-catalytic coating conducting electricity.
This mixed metal oxide electrode can be used for electrolytic seawater device for preventing fouling due to marine organism, apparatus for treating ship ballast water and clorox electrolysis production device etc.
Below adopt embodiment to describe embodiments of the present invention in detail, to the present invention, how utilisation technology means solve technical problem whereby, and the implementation procedure of reaching technique effect can fully understand and implement according to this.
Embodiment 1
(1) substrate pretreated: adopt the TA2 industrially pure titanium plate of tabular 140mm * 110mm * 3mm as electrode matrix, first adopt the silicon carbide of granularity 120 μ m to carry out sandblasting to titanium plate, remove residual sand grains and scrap metal with distilled water flushing; Then titanium plate is put into acetone and carry out oil removing, finally the titanium plate after oil removing is put into 10% (massfraction) oxalic acid solution, under boiling state, keep 2h, after taking-up, in deionized water, use ultrasonic cleaning 10min.The titanium plate of above-mentioned processing is dried up to put into dehydrated alcohol standby.
(2) preparation masking liquid: by Platinic chloride (H
2ptCl
6) and tin tetrachloride (SnCl
4) by certain Pt:Sn mol ratio (specifically in Table 1), join in propyl carbinol solvent, magnetic agitation 0.5h, the volumetric molar concentration that regulates solvent to make GOLD FROM PLATING SOLUTION belong to ion is 0.3mol/L, masking liquid volume is 10mL.
(3) electrode preparation: by masking liquid with hairbrush brushing on pretreated titanium plate, first 120 ℃ of dry 10min in baking oven, then in sintering oven, at 500 ℃, after sintering 10min, take out air cooling, repeatedly apply, oven dry, sintering and cooling step, until metal oxide carrying capacity reaches 6g/m
2, last brushing, dry after in the retort furnace of 500 ℃ sintering 1h, obtain Mixed Metal Oxide Coated Titanium Anodes.
(4) contrast sample preparation: by chloro-iridic acid, ruthenium trichloride, tin tetrachloride by Ru: Ir: Sn mol ratio joins in propyl carbinol solvent at 20: 20: 60, coating liquid concentration is 0.3mol/L, according to above-mentioned preparation method, on pretreated titanium matrix, prepare oxide coating, guarantee that metal oxide carrying capacity reaches 6g/m
2, this electrode is as the contrast sample of anode material of the present invention.
Embodiment 2
(1) substrate pretreated: electrode matrix is selected netted titanium material, is of a size of 100mm * 100mm * 3mm, adopts and the same method of embodiment 1 is carried out sandblast, oil removing and oxalic acid etching processing successively, obtains pretreated titanium matrix standby.
(2) preparation masking liquid: by Platinic chloride (H
2ptCl
6), tin tetrachloride (SnCl
4) and cobalt chloride (CoCl
22H
2o) by certain Pt: Sn: Co mol ratio (specifically in Table 2) joins in propyl carbinol solvent, magnetic agitation 0.5h, the volumetric molar concentration that regulates solvent to make GOLD FROM PLATING SOLUTION belong to ion is 0.3mol/L, masking liquid volume is 10mL.
(3) electrode preparation: adopt and method that embodiment 1 is same to adopt the mode of manually brushing to be coated in titanium masking liquid online, dry successively, the operation steps such as sintering and air cooling, until metal oxide carrying capacity reaches 6g/m
2, obtain Mixed Metal Oxide Coated Titanium Anodes.
For Mixed Metal Oxide Coated Titanium Anodes material more of the present invention and traditional RuO
2-IrO
2-SnO
2the difference of anode, has carried out test relatively by contrast sample and embodiment 1 and 2 resulting electrode materialss.Tested the chlorine evolution potential (E of the metal oxide anode of preparation
cl2), current efficiency (η), groove presses (CV) intensified electrolysis life-span (ALT).
The saturated NaCl solution of anode chlorine evolution potential test selection is as test(ing) medium, and test temperature is 10 ℃, and reference electrode is saturated calomel electrode (sCE), and applying current density is 2000A/m
2.
Anodic current efficiency test, by measuring the oxide coating anode available chlorine content that electrolysis for some time produces in the seawater of certain volume, is then compared and obtains with theoretical chlorine yield (can be calculated by Faraday's law).Analytical procedure with reference to GB GB12176-90 effective chlorine density.Select natural sea-water as test(ing) medium, test temperature is 10 ℃, and reference electrode is saturated calomel electrode (SCE), applies current density and selects 0.5A/m
2, titrimetry current efficiency after electrolysis time 10min.
Intensified electrolysis life test is carried out in the natural sea-water of 10 ℃, and mixed metal oxide electrode is anode, and titanium plate is negative electrode, and interpole gap is 1cm, and the constant current density of electrolysis is 5000A/m
2, adopt the groove in digital versatile table record electrolytic process to press data, regulation groove presses electrolysis time while rising 5V left and right as the intensified electrolysis life-span.
Mixed Metal Oxide Coated Titanium Anodes the performance test results of the present invention is in Table 1 and table 2.With contrast sample (RuO
2-IrO
2-SnO
2anode) compare, Mixed Metal Oxide Coated Titanium Anodes of the present invention forms when the content range of regulation, all has excellent chemical property and stability under cold condition.In seawater, analyse chlorine current efficiency more than 85%, chlorine evolution potential is 1.11V, and under cold condition, the chlorine electro catalytic activity of analysing of anode obviously improves; In addition, only for 42h compares, the anode intensified electrolysis life-span of the present invention is longer, shows that the stability of anode under cold condition significantly improves with contrast sample reinforcing life.
The performance test results of table 1PtSn metal oxide anode
The performance test results of table 2PtSnCo metal oxide anode
All above-mentioned these intellecture properties of primary enforcement, do not set restriction this product innovation of other forms of enforcement and/or novel method.Those skilled in the art will utilize this important information, and foregoing is revised, to realize similar implementation status.But all modifications or transformation belong to the right of reservation based on product innovation of the present invention.
The above, be only preferred embodiment of the present invention, is not the present invention to be done to the restriction of other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (10)
1. electrolysis low temperature seawater is antifouling with a mixed metal oxide electrode, it is characterized in that: comprise electrode matrix and Diversity precious metal oxide coating.
2. mixed metal oxide electrode as claimed in claim 1, is characterized in that: described electrode matrix adopts valve metal titanium material to make.
3. mixed metal oxide electrode as claimed in claim 1 or 2, is characterized in that: the shape of described conducting base can be netted, tabular, tubulose, the structural shape such as bar-shaped.
4. the mixed metal oxide electrode as described in claims 1 to 3, is characterized in that: described Diversity precious metal oxide coating is P
to
x-S
no
2coating.
5. the mixed metal oxide electrode as described in claim 1 to 4, is characterized in that: described P
to
x-S
no
2the constitutive molar ratio of composition is P
t: S
n=(50～95): (5～50).
6. the mixed metal oxide electrode as described in claim 1 to 5, is characterized in that: described in this, Diversity precious metal oxide coating can also contain Co element.
7. the mixed metal oxide electrode as described in claim 1 to 6, is characterized in that: described Diversity precious metal oxide coating is P
to
x-S
no
2-Co
3o
4coating.
8. the mixed metal oxide electrode as described in claim 1 to 7, is characterized in that: described mixed metal oxide electrode is applied to electrolytic seawater device for preventing fouling due to marine organism, apparatus for treating ship ballast water and clorox electrolysis production device.
9. the preparation method of mixed metal oxide electrode described in claim 1 to 8, it is characterized in that: by the halogenide metal salt solution of platinum, tin and cobalt by together with the mixed in molar ratio of above-mentioned platinum, tin and cobalt, obtain masking liquid, this masking liquid is adopted the methods such as artificial brushing, dip-coating or spraying be coated on titanium matrix, in oxidizing atmosphere successively through dry at 100～150 ℃ and 450～550 ℃ at the thermal treatment process such as sintering form the titanium base mixed metal oxide electro-catalytic coating conducting electricity.
10. the application of mixed metal oxide electrode in the antifouling engineering of electrolysis low temperature seawater described in claim 1 to 9.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521404A (en) * | 2016-11-02 | 2017-03-22 | 苏州云瑞环境科技有限公司 | Process for manufacturing titanium anode by once oxidation |
| CN112763523A (en) * | 2020-12-30 | 2021-05-07 | 上海大学 | Three-dimensional etching characterization method for high-nickel maraging steel nonmetallic inclusions |
| CN113529132A (en) * | 2021-08-09 | 2021-10-22 | 中国科学院海洋研究所 | Cobalt-based catalyst electrode and preparation method thereof |
| CN114717590A (en) * | 2022-03-10 | 2022-07-08 | 中国科学院海洋研究所 | Preparation method of cobalt-based chlorine evolution catalyst electrode |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521404A (en) * | 2016-11-02 | 2017-03-22 | 苏州云瑞环境科技有限公司 | Process for manufacturing titanium anode by once oxidation |
| CN112763523A (en) * | 2020-12-30 | 2021-05-07 | 上海大学 | Three-dimensional etching characterization method for high-nickel maraging steel nonmetallic inclusions |
| CN113529132A (en) * | 2021-08-09 | 2021-10-22 | 中国科学院海洋研究所 | Cobalt-based catalyst electrode and preparation method thereof |
| CN114717590A (en) * | 2022-03-10 | 2022-07-08 | 中国科学院海洋研究所 | Preparation method of cobalt-based chlorine evolution catalyst electrode |
| CN114717590B (en) * | 2022-03-10 | 2023-08-08 | 中国科学院海洋研究所 | Preparation method of cobalt-based chlorine evolution catalyst electrode |
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