CN106145276B - A kind of preparation method of the oxide coating electrode for wastewater treatment - Google Patents
A kind of preparation method of the oxide coating electrode for wastewater treatment Download PDFInfo
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- CN106145276B CN106145276B CN201610612891.5A CN201610612891A CN106145276B CN 106145276 B CN106145276 B CN 106145276B CN 201610612891 A CN201610612891 A CN 201610612891A CN 106145276 B CN106145276 B CN 106145276B
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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
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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
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
Abstract
The invention discloses a kind of preparation methods of oxide coating electrode for wastewater treatment, and its step are as follows: step 1, substrate cleaning, step 2, filler configures, step 3, filling foaming body, step 4, metal oxide solution configures, step 5, electrode plate plated film, step 6, it densifies, obtains fine and close coated electrode.Present invention process is simple, strong operability, and raw material sources are extensive, low in cost.
Description
Technical field
The invention belongs to environmentally conscious materials technical fields, and in particular to a kind of oxide coating electrode for wastewater treatment
Preparation method.
Background technique
Currently, DSA electrode is mainly used in sulfuric acid, chlorine industry, function is analysis oxygen and analysis chlorine, and in wastewater treatment side
Face, the DSA electrode lasted a long time, as Ti RuO2、Ti\IrO2Electrode, overpotential for oxygen evolution is lower, to catalytic organism degradation energy
Power is poor, and the electrocatalysis of electrode can meet the actual needs of wastewater treatment；The good DSA electrode of electrocatalysis characteristic, as Ti
SnO2、Ti\PbO2Electrode is not able to satisfy actual needs equally, and electrode surface coating is not fine and close, easily de- since the service life is shorter
It falls.DSA electro catalytic electrode preparation method complex process, raw material mixing is uneven, influences end product quality；Electrode conductive performance
It reduces, degradation property reduces, while easily falling off.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of oxide coating electrode for wastewater treatment, the present invention is mentioned
The coated electrode electric conductivity of confession is good, and coating structure, defect is few, not easily to fall off.
A kind of preparation method of the oxide coating electrode for wastewater treatment, its step are as follows:
Step 1, substrate cleaning impregnates in water using plate-shape metal foaming body as substrate, is heated to slightly boiled boiling, from
Right cooled and filtered, is then immersed in ethanol solution, carries out low temperature concussion, takes out plate-shape metal foaming body after concussion
It reapposes to stir in water and impregnate, clean plate-shape metal foaming body is obtained after drying；
Step 2, filler configures: using graphene nano material as material, silicone resin is bonding agent, and alcoholic solution is solvent,
Stirring configuration graphene nano suspension；
Step 3, filling foaming body: plate-shape metal foaming body is placed in the mold for communicating size, graphite is then added dropwise
Then alkene nanometer suspension, swing die while dropwise addition are placed and are dried in baking oven, repeatedly 5-8 until full mold is added dropwise
It is secondary, until foaming body is filled up, high temperature sintering is carried out, forms film graphene metal foam；
Step 4, metal oxide solution: nano-metal-oxide is placed in ethanol water, is aided with dispersing agent, is changed
Property agent, adhesive, ultrasonic agitation, metal oxide solution can be obtained；The nano-metal-oxide uses nanometer titanium dioxide
Titanium or nano zine oxide；
Step 5, electrode plate plated film: metal oxide solution is covered to foaming body surface by the way of spraying, then
High temperature sintering is carried out, the good oxide coating electrode plate of caking property is obtained；
Step 6, it densifies: oxide coating electrode plate being subjected to high-temperature expansion, ethanol water is carried out in the mode in step 5
Solution spray is shone, and is quickly cooled down, and fine and close coated electrode is obtained.
The heating time of slightly boiled boiling in the step 1 is 20-30min, and the mixing speed that the stirring is impregnated is
300-1200r/min。
Low temperature concussion in the step 1 is used to be carried out in ice-water bath, and temperature must not be higher than 5 DEG C, oscillation frequency 10-
30MHz。
Filling agent prescription in the step 2 are as follows: 20-25 parts of graphene nano material, 10-12 parts of silicone resin, alcoholic solution
50-65 parts, the silicone resin is using one in modified organic silicone resin, epoxy modified silicone resin or epoxy silicone resin
Kind, the alcoholic solution is 100-500nm using one of C1-C4 alcohol, the partial size of the graphene nano material.
The rate of addition of graphene nano suspension in the step 3 is 2-5mL/min, and the high temperature sintering temperature is
280-350 DEG C, the drying temperature is 50-75 DEG C.
Material prescription in the step 4 are as follows: 12-15 parts of nano-metal-oxide, 45-67 parts of ethanol water, dispersing agent 4-8
Part, 1-3 parts of modifying agent, 11-13 parts of adhesive, the nano-metal-oxide use nano-titanium dioxide or nano zine oxide,
The ethanol content of the ethanol water is 40-70%, and the dispersing agent uses polyvinylpyrrolidone, and the modifying agent uses
Nanometer calcium carbonate.
The nano-titanium dioxide is anatase titanium dioxide.
The supersonic frequency of ultrasonic agitation in the step 4 is 5-9MHz.
Quantity for spray in the step 5 is 20-50mg/cm2, high temperature sintering temperature is 400-500 DEG C.
The temperature of the high-temperature expansion of the step 6 is 200-300 DEG C, spray rate 10-20mg/min.
Compared with prior art, the invention has the following advantages:
1, the method and process that the present invention uses is simple, strong operability, and raw material sources are extensive, low in cost.
2, realize that the wide spectrum to organic matter, non-selectivity aoxidize by generating hydroxyl radical free radical when electrolysis of the invention
Degradation；Nano-structured coating increases the specific surface area of electrode, realizes the efficient degradation to organic matter, same with non-nano structure
Class electrode compares, and handles equivalent organic matter, and performance is greatly improved；Due to the presence of graphene filled layer, make electrode
With preferable stability, conduction velocity is greatly increased, and resistive substantially reduces, and compared with homogeneous electrode, is had and is significantly mentioned
It is high；Coating surface is fine and close, not easily to fall off, and the service life is long, can meet the actual needs of wastewater treatment.
Specific embodiment
The present invention is described further below with reference to embodiment:
Embodiment 1
A kind of preparation method of the oxide coating electrode for wastewater treatment, its step are as follows:
Step 1, substrate cleaning impregnates in water using plate-shape metal foaming body as substrate, is heated to slightly boiled boiling, from
Right cooled and filtered, is then immersed in ethanol solution, carries out low temperature concussion, takes out plate-shape metal foaming body after concussion
It reapposes to stir in water and impregnate, clean plate-shape metal foaming body is obtained after drying；
Step 2, filler configures: using graphene nano material as material, silicone resin is bonding agent, and alcoholic solution is solvent,
Stirring configuration graphene nano suspension；
Step 3, filling foaming body: plate-shape metal foaming body is placed in the mold for communicating size, graphite is then added dropwise
Then alkene nanometer suspension, swing die while dropwise addition are placed and are dried in baking oven until full mold is added dropwise, and repeatedly 5
It is secondary, until foaming body is filled up, high temperature sintering is carried out, forms film graphene metal foam；
Step 4, metal oxide solution: nano-metal-oxide is placed in ethanol water, is aided with dispersing agent, is changed
Property agent, adhesive, ultrasonic agitation, metal oxide solution can be obtained；
Step 5, electrode plate plated film: metal oxide solution is covered to foaming body surface by the way of spraying, then
High temperature sintering is carried out, the good oxide coating electrode plate of caking property is obtained；
Step 6, it densifies: oxide coating electrode plate being subjected to high-temperature expansion, ethanol water is carried out in the mode in step 5
Solution spray is shone, and is quickly cooled down, and fine and close coated electrode is obtained.
The heating time of slightly boiled boiling in the step 1 is 20min, and the mixing speed that the stirring is impregnated is 300r/
min。
Low temperature concussion in the step 1 is used to be carried out in ice-water bath, and temperature is 5 DEG C, oscillation frequency 10MHz.
Filling agent prescription in the step 2 are as follows: 20 parts of graphene nano material, 10 parts of silicone resin, 50 parts of alcoholic solution, institute
Silicone resin is stated using modified organic silicone resin, the alcoholic solution uses methanol, and the partial size of the graphene nano material is
100nm。
The rate of addition of graphene nano suspension in the step 3 is 2mL/min, and the high temperature sintering temperature is
280 DEG C, the drying temperature is 50 DEG C.
Material prescription in the step 4 are as follows: 12 parts of nano-metal-oxide, 4 parts of dispersing agent, is modified 45 parts of ethanol water
1 part of agent, 11 parts of adhesive, the nano-metal-oxide use nano-titanium dioxide, the ethanol content of the ethanol water
It is 40%, the dispersing agent uses polyvinylpyrrolidone, and the modifying agent uses nanometer calcium carbonate.
The nano-titanium dioxide is anatase titanium dioxide.
Supersonic frequency in the step 4 is 5MHz.
Quantity for spray in the step 5 is 20mg/cm2, high temperature sintering temperature is 400 DEG C.
The temperature of the high-temperature expansion of the step 6 is 200 DEG C, spray rate 10mg/min.
Embodiment 2
A kind of preparation method of the oxide coating electrode for wastewater treatment, its step are as follows:
Step 1, substrate cleaning impregnates in water using plate-shape metal foaming body as substrate, is heated to slightly boiled boiling, from
Right cooled and filtered, is then immersed in ethanol solution, carries out low temperature concussion, takes out plate-shape metal foaming body after concussion
It reapposes to stir in water and impregnate, clean plate-shape metal foaming body is obtained after drying；
Step 2, filler configures: using graphene nano material as material, silicone resin is bonding agent, and alcoholic solution is solvent,
Stirring configuration graphene nano suspension；
Step 3, filling foaming body: plate-shape metal foaming body is placed in the mold for communicating size, graphite is then added dropwise
Then alkene nanometer suspension, swing die while dropwise addition are placed and are dried in baking oven until full mold is added dropwise, and repeatedly 8
It is secondary, until foaming body is filled up, high temperature sintering is carried out, forms film graphene metal foam；
Step 4, metal oxide solution: nano-metal-oxide is placed in ethanol water, is aided with dispersing agent, is changed
Property agent, adhesive, ultrasonic agitation, metal oxide solution can be obtained；
Step 5, electrode plate plated film: metal oxide solution is covered to foaming body surface by the way of spraying, then
High temperature sintering is carried out, the good oxide coating electrode plate of caking property is obtained；
Step 6, it densifies: oxide coating electrode plate being subjected to high-temperature expansion, ethanol water is carried out in the mode in step 5
Solution spray is shone, and is quickly cooled down, and fine and close coated electrode is obtained.
The heating time of slightly boiled boiling in the step 1 is 30min, and the mixing speed that the stirring is impregnated is 1200r/
min。
Low temperature concussion in the step 1 is used to be carried out in ice-water bath, and temperature is 0 DEG C, oscillation frequency 30MHz.
Filling agent prescription in the step 2 are as follows: 25 parts of graphene nano material, 12 parts of silicone resin, 65 parts of alcoholic solution, institute
Silicone resin is stated using epoxy modified silicone resin, the alcoholic solution uses ethyl alcohol, and the partial size of the graphene nano material is
500nm。
The rate of addition of graphene nano suspension in the step 3 is 5mL/min, and the high temperature sintering temperature is
350 DEG C, the drying temperature is 75 DEG C.
Material prescription in the step 4 are as follows: 15 parts of nano-metal-oxide, 8 parts of dispersing agent, is modified 67 parts of ethanol water
3 parts of agent, 13 parts of adhesive, the nano-metal-oxide use nano zine oxide, and the ethanol content of the ethanol water is
70%, the dispersing agent uses polyvinylpyrrolidone, and the modifying agent uses nanometer calcium carbonate.
Supersonic frequency in the step 4 is 9MHz.
Quantity for spray in the step 5 is 50mg/cm2, high temperature sintering temperature is 500 DEG C.
The temperature of the high-temperature expansion of the step 6 is 300 DEG C, spray rate 20mg/min.
Embodiment 3
A kind of preparation method of the oxide coating electrode for wastewater treatment, its step are as follows:
Step 1, substrate cleaning impregnates in water using plate-shape metal foaming body as substrate, is heated to slightly boiled boiling, from
Right cooled and filtered, is then immersed in ethanol solution, carries out low temperature concussion, takes out plate-shape metal foaming body after concussion
It reapposes to stir in water and impregnate, clean plate-shape metal foaming body is obtained after drying；
Step 2, filler configures: using graphene nano material as material, silicone resin is bonding agent, and alcoholic solution is solvent,
Stirring configuration graphene nano suspension；
Step 3, filling foaming body: plate-shape metal foaming body is placed in the mold for communicating size, graphite is then added dropwise
Then alkene nanometer suspension, swing die while dropwise addition are placed and are dried in baking oven until full mold is added dropwise, and repeatedly 7
It is secondary, until foaming body is filled up, high temperature sintering is carried out, forms film graphene metal foam；
Step 4, metal oxide solution: nano-metal-oxide is placed in ethanol water, is aided with dispersing agent, is changed
Property agent, adhesive, ultrasonic agitation, metal oxide solution can be obtained；
Step 5, electrode plate plated film: metal oxide solution is covered to foaming body surface by the way of spraying, then
High temperature sintering is carried out, the good oxide coating electrode plate of caking property is obtained；
Step 6, it densifies: oxide coating electrode plate being subjected to high-temperature expansion, ethanol water is carried out in the mode in step 5
Solution spray is shone, and is quickly cooled down, and fine and close coated electrode is obtained.
The heating time of slightly boiled boiling in the step 1 is 25min, and the mixing speed that the stirring is impregnated is 900r/
min。
Low temperature concussion in the step 1 is used to be carried out in ice-water bath, and temperature is 3 DEG C, oscillation frequency 20MHz.
Filling agent prescription in the step 2 are as follows: 23 parts of graphene nano material, 11 parts of silicone resin, 57 parts of alcoholic solution, institute
Silicone resin is stated using epoxy silicone resin, the alcoholic solution uses butanol, and the partial size of the graphene nano material is
300nm。
The rate of addition of graphene nano suspension in the step 3 is 3mL/min, and the high temperature sintering temperature is
330 DEG C, the drying temperature is 65 DEG C.
Material prescription in the step 4 are as follows: 14 parts of nano-metal-oxide, 6 parts of dispersing agent, is modified 55 parts of ethanol water
2 parts of agent, 12 parts of adhesive, the nano-metal-oxide use nano-titanium dioxide, the ethanol content of the ethanol water
It is 60%, the dispersing agent uses polyvinylpyrrolidone, and the modifying agent uses nanometer calcium carbonate.
The nano-titanium dioxide is anatase titanium dioxide.
Supersonic frequency in the step 4 is 7MHz.
Quantity for spray in the step 5 is 40mg/cm2, high temperature sintering temperature is 450 DEG C.
The temperature of the high-temperature expansion of the step 6 is 250 DEG C, spray rate 15mg/min.
The foregoing is merely one embodiment of the invention, are not intended to limit the present invention, all to use equivalent substitution or equivalent transformation
Mode technical solution obtained, fall within the scope of protection of the present invention.
Claims (10)
1. a kind of preparation method of the oxide coating electrode for wastewater treatment, which is characterized in that its step are as follows:
Step 1, substrate cleaning impregnates in water using plate-shape metal foaming body as substrate, is heated to slightly boiled boiling, naturally cold
But it filters, is then immersed in ethanol solution afterwards, carry out low temperature concussion, take out plate-shape metal foaming body again after concussion
It places to stir in water and impregnate, clean plate-shape metal foaming body is obtained after drying；
Step 2, filler configures: using graphene nano material as material, silicone resin is bonding agent, and alcoholic solution is solvent, stirring
Configure graphene nano suspension；
Step 3, filling foaming body: plate-shape metal foaming body is placed in the mold for communicating size, and graphene is then added dropwise and receives
Then rice suspension, swing die while dropwise addition are placed and are dried in baking oven until full mold is added dropwise, and 5-8 times repeatedly,
Until foaming body is filled up, high temperature sintering is carried out, forms film graphene metal foam；
Step 4, metal oxide solution: nano-metal-oxide is placed in ethanol water, is aided with dispersing agent, modification
Agent, adhesive, ultrasonic agitation, can be obtained metal oxide solution；The nano-metal-oxide uses nano-titanium dioxide
Or nano zine oxide；
Step 5, electrode plate plated film: metal oxide solution is covered to foaming body surface by the way of spraying, is then carried out
High temperature sintering obtains the good oxide coating electrode plate of caking property；
Step 6, it densifies: oxide coating electrode plate being subjected to high-temperature expansion, ethanol water is carried out in the mode in step 5
Spray is shone, and is quickly cooled down, and fine and close coated electrode is obtained.
2. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 1, feature
It is, the slightly boiled heating time in the step 1 is 20-30min, and the mixing speed being stirred is 300-1200r/
min。
3. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 1, feature
It is, the low temperature concussion in the step 1 is used to be carried out in ice-water bath, and temperature must not be higher than 5 DEG C, oscillation frequency 10-
30MHz。
4. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 1, feature
It is, the filling agent prescription in the step 2 are as follows: 20-25 parts of graphene nano material, 10-12 parts of silicone resin, alcoholic solution 50-
65 parts, the silicone resin uses one of modified organic silicone resin, epoxy modified silicone resin or epoxy silicone resin,
The alcoholic solution is 100-500nm using one of C1-C4 alcohol, the partial size of the graphene nano material.
5. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 1, feature
It is, the rate of addition of the graphene nano suspension in the step 3 is 2-5mL/min, and high temperature sintering temperature is 280-350
DEG C, the drying temperature is 50-75 DEG C.
6. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 1, feature
Be, the material prescription in the step 4 are as follows: 12-15 parts of nano-metal-oxide, 45-67 parts of ethanol water, 4-8 parts of dispersing agent,
1-3 parts of modifying agent, 11-13 parts of adhesive, the nano-metal-oxide uses nano-titanium dioxide or nano zine oxide, described
The ethanol content of ethanol water is 40-70%, and the dispersing agent uses polyvinylpyrrolidone, and the modifying agent uses nanometer
Calcium carbonate.
7. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 6, feature
It is, the nano-titanium dioxide is anatase titanium dioxide.
8. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 1, feature
It is, the supersonic frequency of the ultrasonic agitation in the step 4 is 5-9MHz.
9. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 1, feature
It is, the quantity for spray in the step 5 is 20-50mg/cm2, high temperature sintering temperature is 400-500 DEG C.
10. a kind of preparation method of oxide coating electrode for wastewater treatment according to claim 1, feature
It is, the temperature of the high-temperature expansion of the step 6 is 200-300 DEG C, spray rate 10-20mg/min.
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| KR100923304B1 (en) * | 2007-10-29 | 2009-10-23 | 삼성전자주식회사 | Graphene sheet and process for preparing the same |
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| CN1360356A (en) * | 2002-01-24 | 2002-07-24 | 南开大学 | Foam-metal current collector of secondary battery using zinc as negative electrode and its preparing process |
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