CN106396028A - Preparation method of titanium-based metal oxide anode for seawater - Google Patents
Preparation method of titanium-based metal oxide anode for seawater Download PDFInfo
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- CN106396028A CN106396028A CN201611120716.0A CN201611120716A CN106396028A CN 106396028 A CN106396028 A CN 106396028A CN 201611120716 A CN201611120716 A CN 201611120716A CN 106396028 A CN106396028 A CN 106396028A
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- metal oxide
- titanium plate
- oxide anode
- roasting
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
- C02F1/4674—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation with halogen or compound of halogens, e.g. chlorine, bromine
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a titanium-based metal oxide anode for seawater. The preparation method comprises the following steps: (1) adopting a titanium plate as an electrode substrate, etching in an oxalic acid solution after washing, and then putting in distilled water for standby use; (2) taking a tantalum pentachloride n-butyl alcohol saturated solution, adding iN nano-powder, carrying out ultrasonic treatment to obtain a mixture, then applying the mixture onto the titanium plate in the step (1), drying, roasting, then repeating the process of coating, drying and roasting one time, thereby obtaining a titanium plate coated with an interlayer sample; and (3) uniformly mixing chloroiridic acid, n-butyl alcohol and hydrochloric acid, then applying the mixed liquor onto the titanium plate obtained in the step (2), drying, roasting, repeating the process of coating, drying and roasting three times all together, thereby obtaining the titanium-based metal oxide anode for seawater. The titanium-based metal oxide anode prepared and obtained with the method can be used in low temperature seawater (0 to 15 DEG C), and has relatively high electrocatalytic activity.
Description
Technical field
The invention belongs to the preparation field of electrode material is and in particular to a kind of system of sea water Ti-support metal oxide anode
Preparation Method.
Background technology
When installing ballast water additional, some biologies in sea water are also added in ballast tank foreign-going ship therewith, until boat
Journey terminates just to be discharged into purpose marine site, and this easily causes the pernicious propagation of unwanted aquatic organism and pathogen.The discharge of ballast water
Control is improper may to cause serious harm to marine ecosystems and public health.According to《Management of Ships ' Ballast Water and deposition
Thing controls and management contract》Regulation, all ships all must finally require ballast water is processed according to D-2.Ballast water
Processing method includes Filtration, cyclonic separation method, ultraviolet radioactive method, ultrasonic method, Ozone and electrolysis etc., wherein at electrolysis
Reason ballast water forms NaClO, Cl by electrolytic seawater2To kill the aquatile in ballast water with oxidizing species such as HClO
With pathogen etc., it is that there is one of main method of development prospect.Electrolytic seawater has electro catalytic activity using to analysis chlorine reaction
Electrode, mainly Ti-support metal oxide anode, are also dimensional stability anode (DSA), it is generally with RuO2And IrO2As master
Want active substance, the former catalysis activity is high, the latter then has higher durability it is also possible to by preparing metal composite oxide
Method, such as Ti/ RuO2-IrO2-Sb2O5-SnO2, to obtain the DSA having catalysis activity and durability concurrently, to open in this regard
Exhibition numerous studies work and practical application.
But, the ballast water treatment of foreign-going ship is often carried out under low temperature (0-15 DEG C).Traditional electrode material, such as Ti/
RuO2-IrO2-Sb2O5-SnO2Active extreme difference in low temperature use environment (5 and 10 DEG C), and using initial activity coating
Come off.Therefore, exploitation be applied to ballast for cruising water electrolysis process the low temperature resistant DSA of special type be one very urgent and meaningful
Work.
Content of the invention
The present invention provides a kind of preparation method of sea water Ti-support metal oxide anode, the titanium-based metal oxide obtaining
Anode, can use in low temperature seawater.
The preparation method of sea water Ti-support metal oxide anode, comprises the steps of:
(1)Using titanium plate as electrode matrix, cleaned with the NaOH solution of pH=8-9 3 times, then distilled water cleaning 5 times, in matter
Amount fraction etches 3h in the oxalic acid solution for 8-12% at 95 DEG C, is then placed within standby in distilled water;
(2)Take 2 mL tantalic chloride n-butyl alcohol saturated solutions, add the TiN nano-powder of 16 mg, supersound process, then will
This solution is coated on step(1)Titanium plate on, dry 10 min at 121 DEG C, then in 350 DEG C of air gas in Muffle furnace
Roasting 15min under atmosphere, repeats this coating-drying-roasting process 1 time, that is, obtains being coated with the titanium plate of intermediate layer sample;
(3)Chloro-iridic acid, n-butyl alcohol and hydrochloric acid are pressed 1:10:1 volume ratio mix homogeneously, obtains chloro-iridic acid-n-butyl alcohol-hydrochloric acid and mixes
Close liquid, then this mixed liquor is coated on step(2)In the titanium plate being coated with intermediate layer sample obtaining, dry at 121 DEG C
10 min, then in Muffle furnace under 400-500 DEG C of air atmosphere roasting 15min, repeat this coating-drying-roasting process
Totally 3 times, that is, obtain sea water Ti-support metal oxide anode.
Preferably, step(1)The size of middle titanium plate is 25 mm × 25 mm × 2 mm.
Preferably, step(1)The mass fraction of medium-height grass acid solution is 10%.
Preferably, step(2)In, the condition of supersound process is process 1h under the ultrasonic power of 200W.
Advantages of the present invention:
The Ti-support metal oxide anode that the present invention prepares, can be in low temperature seawater(0-15℃)Middle use, has relatively
High electro catalytic activity.
Specific embodiment
Embodiment 1
The preparation method of sea water Ti-support metal oxide anode, comprises the steps of:
(1)Using titanium plate as electrode matrix, cleaned with the NaOH solution of pH=8-9 3 times, then distilled water cleaning 5 times, in matter
Measure in the oxalic acid solution that fraction is 8% and etch 3h at 95 DEG C, be then placed within standby in distilled water;
(2)Take 2 mL tantalic chloride n-butyl alcohol saturated solutions, add the TiN nano-powder of 16 mg, supersound process, then will
This solution is coated on step(1)Titanium plate on, dry 10 min at 121 DEG C, then in 350 DEG C of air gas in Muffle furnace
Roasting 15min under atmosphere, repeats this coating-drying-roasting process 1 time, that is, obtains being coated with the titanium plate of intermediate layer sample;
(3)Chloro-iridic acid, n-butyl alcohol and hydrochloric acid are pressed 1:10:1 volume ratio mix homogeneously, obtains chloro-iridic acid-n-butyl alcohol-hydrochloric acid and mixes
Close liquid, then this mixed liquor is coated on step(2)In the titanium plate being coated with intermediate layer sample obtaining, dry at 121 DEG C
10 min, then in Muffle furnace under 400-500 DEG C of air atmosphere roasting 15min, repeat this coating-drying-roasting process
Totally 3 times, that is, obtain sea water Ti-support metal oxide anode.
Embodiment 2
The preparation method of sea water Ti-support metal oxide anode, comprises the steps of:
(1)Using titanium plate as electrode matrix, cleaned with the NaOH solution of pH=8-9 3 times, then distilled water cleaning 5 times, in matter
Measure in the oxalic acid solution that fraction is 12% and etch 3h at 95 DEG C, be then placed within standby in distilled water;
(2)Take 2 mL tantalic chloride n-butyl alcohol saturated solutions, add the TiN nano-powder of 16 mg, supersound process, then will
This solution is coated on step(1)Titanium plate on, dry 10 min at 121 DEG C, then in 350 DEG C of air gas in Muffle furnace
Roasting 15min under atmosphere, repeats this coating-drying-roasting process 1 time, that is, obtains being coated with the titanium plate of intermediate layer sample;
(3)Chloro-iridic acid, n-butyl alcohol and hydrochloric acid are pressed 1:10:1 volume ratio mix homogeneously, obtains chloro-iridic acid-n-butyl alcohol-hydrochloric acid and mixes
Close liquid, then this mixed liquor is coated on step(2)In the titanium plate being coated with intermediate layer sample obtaining, dry at 121 DEG C
10 min, then in Muffle furnace under 400-500 DEG C of air atmosphere roasting 15min, repeat this coating-drying-roasting process
Totally 3 times, that is, obtain sea water Ti-support metal oxide anode.
Embodiment 3
The preparation method of sea water Ti-support metal oxide anode, comprises the steps of:
(1)Using titanium plate as electrode matrix, wherein, the size of titanium plate is 25 mm × 25 mm × 2 mm, with pH=8-9's
NaOH solution clean 3 times, then distilled water clean 5 times, mass fraction be 10% oxalic acid solution at 95 DEG C etch 3h,
It is then placed within standby in distilled water;
(2)Take 2 mL tantalic chloride n-butyl alcohol saturated solutions, add the TiN nano-powder of 16 mg, in the ultrasonic power of 200W
Then this solution be coated on step by lower process 1h(1)Titanium plate on, dry 10 min at 121 DEG C, then in Muffle furnace
In under 350 DEG C of air atmospheres roasting 15min, repeat this coating-drying-roasting process 1 time, that is, obtain being coated with intermediate layer
The titanium plate of sample;
(3)Chloro-iridic acid, n-butyl alcohol and hydrochloric acid are pressed 1:10:1 volume ratio mix homogeneously, obtains chloro-iridic acid-n-butyl alcohol-hydrochloric acid and mixes
Close liquid, then this mixed liquor is coated on step(2)In the titanium plate being coated with intermediate layer sample obtaining, dry at 121 DEG C
10 min, then in Muffle furnace under 400-500 DEG C of air atmosphere roasting 15min, repeat this coating-drying-roasting process
Totally 3 times, that is, obtain sea water Ti-support metal oxide anode.
Claims (4)
1. sea water Ti-support metal oxide anode preparation method it is characterised in that:Comprise the steps of:
(1)Using titanium plate as electrode matrix, cleaned with the NaOH solution of pH=8-9 3 times, then distilled water cleaning 5 times, in matter
Amount fraction etches 3h in the oxalic acid solution for 8-12% at 95 DEG C, is then placed within standby in distilled water;
(2)Take 2 mL tantalic chloride n-butyl alcohol saturated solutions, add the TiN nano-powder of 16 mg, supersound process, then will
This solution is coated on step(1)Titanium plate on, dry 10 min at 121 DEG C, then in 350 DEG C of air gas in Muffle furnace
Roasting 15min under atmosphere, repeats this coating-drying-roasting process 1 time, that is, obtains being coated with the titanium plate of intermediate layer sample;
(3)Chloro-iridic acid, n-butyl alcohol and hydrochloric acid are pressed 1:10:1 volume ratio mix homogeneously, obtains chloro-iridic acid-n-butyl alcohol-hydrochloric acid and mixes
Close liquid, then this mixed liquor is coated on step(2)In the titanium plate being coated with intermediate layer sample obtaining, dry at 121 DEG C
10 min, then in Muffle furnace under 400-500 DEG C of air atmosphere roasting 15min, repeat this coating-drying-roasting process
Totally 3 times, that is, obtain sea water Ti-support metal oxide anode.
2. sea water Ti-support metal oxide anode according to claim 1 preparation method it is characterised in that:Step
(1)The size of middle titanium plate is 25 mm × 25 mm × 2 mm.
3. sea water Ti-support metal oxide anode according to claim 1 preparation method it is characterised in that:Step
(1)The mass fraction of medium-height grass acid solution is 10%.
4. sea water Ti-support metal oxide anode according to claim 1 preparation method it is characterised in that:Step
(2)In, the condition of supersound process is process 1h under the ultrasonic power of 200W.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113716654A (en) * | 2021-09-01 | 2021-11-30 | 安徽康菲尔检测科技有限公司 | Preparation method of high-conductivity alloy catalytic electrode and prepared electrode |
CN114890508A (en) * | 2021-09-24 | 2022-08-12 | 中国船舶重工集团公司第七二五研究所 | Metal oxide nanowire array mesh electrode material and preparation method thereof |
-
2016
- 2016-12-08 CN CN201611120716.0A patent/CN106396028A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113716654A (en) * | 2021-09-01 | 2021-11-30 | 安徽康菲尔检测科技有限公司 | Preparation method of high-conductivity alloy catalytic electrode and prepared electrode |
CN113716654B (en) * | 2021-09-01 | 2023-12-26 | 安徽康菲尔检测科技有限公司 | Preparation method of high-conductivity alloy catalytic electrode and prepared electrode |
CN114890508A (en) * | 2021-09-24 | 2022-08-12 | 中国船舶重工集团公司第七二五研究所 | Metal oxide nanowire array mesh electrode material and preparation method thereof |
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