CN110171872A - A kind of palladium/polyaniline/tin indium oxide combination electrode and preparation method and application - Google Patents
A kind of palladium/polyaniline/tin indium oxide combination electrode and preparation method and application Download PDFInfo
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- CN110171872A CN110171872A CN201910493771.1A CN201910493771A CN110171872A CN 110171872 A CN110171872 A CN 110171872A CN 201910493771 A CN201910493771 A CN 201910493771A CN 110171872 A CN110171872 A CN 110171872A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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- 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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- 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
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Abstract
The present invention is a kind of palladium/polyaniline/tin indium oxide method for preparing composite electrode, its main feature is that, comprising: polyaniline/tin indium oxide combination electrode is prepared using anodizing and palladium/polyaniline/tin indium oxide combination electrode step preparation palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process；And palladium/polyaniline/tin indium oxide combination electrode electrochemical degradation antibiotic waste water application of preparation.This method has the advantages that scientific and reasonable, operation is simple, energy conservation and environmental protection, at low cost, strong applicability wait: palladium/polyaniline of preparation/tin indium oxide combination electrode property is stable, high-quality；Palladium/polyaniline of preparation/tin indium oxide combination electrode electrochemical degradation antibiotic waste water application effect is good.
Description
Technical field
The invention belongs to electrochemical material preparation technical fields, and in particular to compound to a kind of palladium/polyaniline/tin indium oxide
Electrode preparation method and its application.
Background technique
In electrode production process, electrode material plays critically important role.Indium tin oxide-coated glass is that one kind exists
On the basis of sodium calcium base or silicon boryl substrate glass, indium oxide layer tin film is plated using a variety of methods such as sputtering, evaporations and is processed
Manufactured conductive material.Glass material itself is nonconducting, but due to having plated indium oxide tin film, is just provided with good conductive
Property, compared with high transmittance, alkaline-resisting and easily by characteristic the advantages that acid etching.In addition, electrode surface is urged during electrochemical catalysis
Change layer and also acts as vital part.The Catalytic Layer that a kind of catalytic effect is good, performance is stable is selected, it can be significantly
Improve electrochemical treatments effect.Polyaniline is a kind of with special light, electrical property, and can have high electrical conductivity after overdoping
And the high-molecular compound of chemical property.In addition, polyaniline structure is unique, is evenly distributed, large specific surface area, prepared in electrode
In, it can be used as the catalysis material of electrode surface.In electrochemical field, polyaniline and tin indium oxide can be coupled together, system
A kind of standby novel combination electrode material, and the organic pollutant in the form of electro-catalysis in removal water body.Tin indium oxide conduction glass
Glass can be combined with other surface catalysts and prepare combination electrode for every field, and prospect is very wide, will be compound
One new breakthrough in electrode material direction.
Summary of the invention
It is an object of the present invention to provide it is a kind of it is scientific and reasonable, be conducive to that environmental protection, operation is simple, property is stable, preparation cost is low
Palladium/polyaniline/tin indium oxide combination electrode preparation method；And provide palladium/polyaniline/indium oxide that this method directly obtains
Tin combination electrode；The application degraded to tetracycline is also provided.
Realize one of the object of the invention the technical solution adopted is that, a kind of palladium/polyaniline/tin indium oxide combination electrode preparation
Method, which comprises the following steps:
1) polyaniline/tin indium oxide combination electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 5 ~ 15 min of ultrasonic oil removing, then with ultrapure water 5
~ 15 min remove impurity, are then dried, spare；Polyaniline is prepared using anodizing, 1 mL aniline is slowly dripped
Enter and 99 mL are housed, concentration is to carry out 30 min of ultrasonic disperse in 0.1 ~ 5 mol/L sulfuric acid solution；It will be gathered using bipolar electrode system
Aniline polymerization is connected to programmable on indium tin oxide-coated glass surface using the indium tin oxide-coated glass of drying as working electrode
DC power anode, uses platinized platinum to be connected to power cathode forming circuit as to electrode, carries out electrochemical polymerization using galvanostatic method,
It is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, guarantees two electricity
Interpolar is away from for 10 ~ 40 mm；Sedimentation time is 1 ~ 20 min in indium tin oxide surfaces homogeneous polymerization polyaniline, and polyaniline/oxygen is made
Change indium tin combination electrode；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum, which is used as, accesses positive pole to electrode, with 0.1 ~ 2 mol/L sodium chloride solution and 0.001 ~ 10.0 mmol/L palladium chloride
Mixed liquor is as electric depositing solution, in 1 ~ 10 mA electric current, 2 ~ 20 min of electro-deposition, to palladium uniform deposition to polyaniline/indium oxide
On tin combination electrode, palladium/polyaniline/tin indium oxide combination electrode is made.
Realize the object of the invention two the technical solution adopted is that: a kind of palladium/polyaniline/oxygen according to claim 1
Change palladium/polyaniline/tin indium oxide combination electrode of indium tin method for preparing composite electrode preparation.
Realize the three of the object of the invention the technical solution adopted is that: a kind of palladium/polyaniline as described in claim 1 or 2/
Tin indium oxide method for preparing composite electrode, palladium/polyaniline/tin indium oxide combination electrode electrochemical degradation antibiotic waste water of preparation
Application.
A kind of palladium/polyaniline/tin indium oxide method for preparing composite electrode of the invention is poly- using anodizing preparation
On the basis of aniline/tin indium oxide support electrode, then use constant current electrodeposition process by palladium uniform deposition to polyaniline/indium oxide
On tin combination electrode, obtain palladium/polyaniline/tin indium oxide combination electrode, this method is scientific and reasonable, operation is simple, energy conservation and environmental protection,
At low cost, strong applicability: palladium/polyaniline of preparation/tin indium oxide combination electrode property is stable, high-quality；Palladium/polyphenyl of preparation
Amine/tin indium oxide combination electrode electrochemical degradation antibiotic waste water application effect is good.
Detailed description of the invention
Fig. 1 is a kind of palladium/polyaniline/tin indium oxide combination electrode scanning electron microscope (SEM) photograph of the invention；
Fig. 2 is a kind of palladium/polyaniline/tin indium oxide combination electrode of the invention, in electrochemical degradation tetracycline wastewater lab diagram.
Specific embodiment
In order to be more clear the purpose of the present invention, technical scheme and beneficial effects, come below with reference to embodiment further
Illustrate the present invention, the embodiments are used only to illustrate the invention for these, is not intended to limit the present invention.Tin indium oxide in following examples is conductive
Glass is purchased in south China Xiang Cheng Science and Technology Ltd..Indium tin oxide-coated glass resistance is≤6 Ω/cm2, having a size of 10 mm ×
The mm of 40 mm × 1.1, transmitance are >=84%, and indium oxide tin glass is stained with dirt in production or transportational process in order to prevent,
It is pre-processed using preceding with dehydrated alcohol and ultrapure water ultrasound.
A kind of embodiment 1: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
1) polyaniline/tin indium oxide support electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 5 min of ultrasonic oil removing, then with ultrapure water 5
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 0.1 mol/L sulfuric acid solution；Using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, the indium tin oxide-coated glass of drying is connected to as working electrode can
DC power anode is programmed, platinized platinum is used to be connected to power cathode forming circuit as to electrode, carries out electrochemistry using galvanostatic method
Polymerization, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, is arranged
Source current is 1 mA, and two electrode spacings of guarantee are 10 mm；Sedimentation time is 1 min poly- in indium tin oxide surfaces homogeneous polymerization
Polyaniline/tin indium oxide combination electrode is made in aniline；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum, which is used as, accesses positive pole to electrode, with the mixed liquor of 0.1 mol/L sodium chloride solution and 0.001 mmol/L palladium chloride
As electric depositing solution, in 1 mA electric current, 2 min of electro-deposition, to palladium uniform deposition to polyaniline/tin indium oxide combination electrode
On, palladium/polyaniline/tin indium oxide combination electrode is made.
A kind of embodiment 2: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
1) polyaniline/tin indium oxide support electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 6 min of ultrasonic oil removing, then with ultrapure water 6
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 0.5 mol/L sulfuric acid solution；Using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, the indium tin oxide-coated glass of drying is connected to as working electrode can
DC power anode is programmed, platinized platinum is used to be connected to power cathode forming circuit as to electrode, carries out electrochemistry using galvanostatic method
Polymerization, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, is arranged
Source current is 2 mA, and two electrode spacings of guarantee are 15 mm；Sedimentation time is 3 min poly- in indium tin oxide surfaces homogeneous polymerization
Polyaniline/tin indium oxide combination electrode is made in aniline；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum, which is used as, accesses positive pole to electrode, with the mixed liquor of 0.3 mol/L sodium chloride solution and 0.01 mmol/L palladium chloride work
For electric depositing solution, in 2 mA electric currents, 4 min of electro-deposition, on palladium uniform deposition to polyaniline/tin indium oxide combination electrode,
Palladium/polyaniline/tin indium oxide combination electrode is made.
A kind of embodiment 3: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
1) polyaniline/tin indium oxide support electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 7 min of ultrasonic oil removing, then with ultrapure water 7
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 1.0 mol/L sulfuric acid solutions；Using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, the indium tin oxide-coated glass of drying is connected to as working electrode can
DC power anode is programmed, platinized platinum is used to be connected to power cathode forming circuit as to electrode, carries out electrochemistry using galvanostatic method
Polymerization, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, is arranged
Source current is 3 mA, and two electrode spacings of guarantee are 20 mm；Sedimentation time is 5 min poly- in indium tin oxide surfaces homogeneous polymerization
Polyaniline/tin indium oxide combination electrode is made in aniline；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum, which is used as, accesses positive pole to electrode, with the mixed liquor of 0.5 mol/L sodium chloride solution and 0.05 mmol/L palladium chloride work
For electric depositing solution, in 3 mA electric currents, 6 min of electro-deposition, on palladium uniform deposition to polyaniline/tin indium oxide combination electrode,
Palladium/polyaniline/tin indium oxide combination electrode is made.
A kind of embodiment 4: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
1) polyaniline/tin indium oxide support electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 8 min of ultrasonic oil removing, then with ultrapure water 8
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 1.5 mol/L sulfuric acid solutions；Using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, the indium tin oxide-coated glass of drying is connected to as working electrode can
DC power anode is programmed, platinized platinum is used to be connected to power cathode forming circuit as to electrode, carries out electrochemistry using galvanostatic method
Polymerization, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, is arranged
Source current is 4 mA, and two electrode spacings of guarantee are 25 mm；Sedimentation time is 8 min poly- in indium tin oxide surfaces homogeneous polymerization
Polyaniline/tin indium oxide combination electrode is made in aniline；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum, which is used as, accesses positive pole to electrode, with the mixed liquor of 0.8 mol/L sodium chloride solution and 0.1 mmol/L palladium chloride work
For electric depositing solution, in 4 mA electric currents, 8 min of electro-deposition, on palladium uniform deposition to polyaniline/tin indium oxide combination electrode,
Palladium/polyaniline/tin indium oxide combination electrode is made.
A kind of embodiment 5: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
1) polyaniline/tin indium oxide combination electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 10 min of ultrasonic oil removing, then with ultrapure water 10
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 2.5 mol/L sulfuric acid solutions；Using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, the indium tin oxide-coated glass of drying is connected to as working electrode can
DC power anode is programmed, platinized platinum is used to be connected to power cathode forming circuit as to electrode, carries out electrochemistry using galvanostatic method
Polymerization, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, is arranged
Source current is 5 mA, and two electrode spacings of guarantee are 30 mm；Sedimentation time is 10 min poly- in indium tin oxide surfaces homogeneous polymerization
Polyaniline/tin indium oxide combination electrode is made in aniline；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum be used as to electrode access positive pole, using the mixed liquor of 1 mol/L sodium chloride solution and 0.5 mmol/L palladium chloride as
Electric depositing solution, in 5 mA electric currents, 10 min of electro-deposition, to make on palladium uniform deposition to polyaniline/tin indium oxide combination electrode
Obtain palladium/polyaniline/tin indium oxide combination electrode.
A kind of embodiment 6: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 11 min of ultrasonic oil removing, then with ultrapure water 11
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 3 mol/L sulfuric acid solutions；It will using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, is connected to and can compile using the indium tin oxide-coated glass of drying as working electrode
Journey DC power anode uses platinized platinum to be connected to power cathode forming circuit as to electrode, and it is poly- to carry out electrochemistry using galvanostatic method
It closes, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, setting electricity
Ource electric current is 6 mA, and two electrode spacings of guarantee are 35 mm；Sedimentation time is 12 min in indium tin oxide surfaces homogeneous polymerization polyphenyl
Polyaniline/tin indium oxide combination electrode is made in amine；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum, which is used as, accesses positive pole to electrode, with the mixed liquor of 1.2 mol/L sodium chloride solutions and 0.5 mmol/L palladium chloride work
For electric depositing solution, in 6 mA electric currents, 12 min of electro-deposition, on palladium uniform deposition to polyaniline/tin indium oxide combination electrode,
Palladium/polyaniline/tin indium oxide combination electrode is made.
A kind of embodiment 7: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 12 min of ultrasonic oil removing, then with ultrapure water 12
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 3.5 mol/L sulfuric acid solutions；Using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, the indium tin oxide-coated glass of drying is connected to as working electrode can
DC power anode is programmed, platinized platinum is used to be connected to power cathode forming circuit as to electrode, carries out electrochemistry using galvanostatic method
Polymerization, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, is arranged
Source current is 7.5 mA, and two electrode spacings of guarantee are 40 mm；Sedimentation time is 15 min in indium tin oxide surfaces homogeneous polymerization
Polyaniline/tin indium oxide combination electrode is made in polyaniline；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum be used as to electrode access positive pole, using the mixed liquor of 1.5 mol/L sodium chloride solutions and 5 mmol/L palladium chlorides as
Electric depositing solution, in 7.5 mA electric currents, 15 min of electro-deposition, on palladium uniform deposition to polyaniline/tin indium oxide combination electrode,
Palladium/polyaniline/tin indium oxide combination electrode is made.
A kind of embodiment 8: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
Using indium tin oxide-coated glass as matrix, 13.5 min of ultrasonic oil removing is put into dehydrated alcohol, then use ultrapure water
13.5 min remove impurity, are then placed in 60 DEG C of baking oven and are dried for standby；Polyaniline is prepared using anodizing, by 1
ML aniline is slowly dropped into equipped with 99 mL, and concentration is to carry out 30 min of ultrasonic disperse in 4.5 mol/L sulfuric acid solutions；Using double electricity
Polyaniline is aggregated in indium tin oxide-coated glass surface by polar body system, using the indium tin oxide-coated glass of drying as working electrode
It is connected to programmable DC positive pole, uses platinized platinum to be connected to power cathode forming circuit as to electrode, is carried out using galvanostatic method
Electrochemical polymerization, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, makes cathode is parallel with anode to put
It sets, setting source current is 9 mA, and two electrode spacings of guarantee are 30 mm；Sedimentation time is that 18 min are equal in indium tin oxide surfaces
Polyaniline/tin indium oxide combination electrode is made in even polymerization polyaniline；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum be used as to electrode access positive pole, using the mixed liquor of 1.8 mol/L sodium chloride solutions and 8 mmol/L palladium chlorides as
Electric depositing solution, in 9 mA electric currents, 18 min of electro-deposition, to make on palladium uniform deposition to polyaniline/tin indium oxide combination electrode
Obtain palladium/polyaniline/tin indium oxide combination electrode.
A kind of embodiment 9: palladium/polyaniline/tin indium oxide method for preparing composite electrode, comprising the following steps:
1) polyaniline/tin indium oxide support electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 15 min of ultrasonic oil removing, then with ultrapure water 15
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 5 mol/L sulfuric acid solutions；It will using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, is connected to and can compile using the indium tin oxide-coated glass of drying as working electrode
Journey DC power anode uses platinized platinum to be connected to power cathode forming circuit as to electrode, and it is poly- to carry out electrochemistry using galvanostatic method
It closes, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode, setting electricity
Ource electric current is 10 mA, and two electrode spacings of guarantee are 40 mm；Sedimentation time is 20 min poly- in indium tin oxide surfaces homogeneous polymerization
Polyaniline/tin indium oxide combination electrode is made in aniline；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum, which is used as, accesses positive pole to electrode, using the mixed liquor of 2 mol/L sodium chloride solutions and 10 mmol/L palladium chlorides as electricity
Deposition solution, in 10 mA electric currents, 20 min of electro-deposition, to make on palladium uniform deposition to polyaniline/tin indium oxide combination electrode
Obtain palladium/polyaniline/tin indium oxide combination electrode.
Embodiment 10: referring to Figures 1 and 2, a kind of palladium/polyaniline/tin indium oxide method for preparing composite electrode, including it is following
Step:
1) polyaniline/tin indium oxide support electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, it is put into dehydrated alcohol 15 min of ultrasonic oil removing, then with ultrapure water 15
Min removes impurity, is then placed in 60 DEG C of baking oven and is dried for standby；Polyaniline is prepared using anodizing, by 1 mL aniline
It is slowly dropped into equipped with 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 1 mol/L sulfuric acid solution；It will using bipolar electrode system
Polyaniline is aggregated in indium tin oxide-coated glass surface, and the indium tin oxide-coated glass of drying is connected to as working electrode 2 can
The anode for programming DC power supply 6, uses platinized platinum to be connected to power cathode forming circuit as to electrode 3, carries out electricity using galvanostatic method
Chemical polymerization, it is the mm of 20 mm × 10 that indium tin oxide-coated glass, which immerses solution effective area, is placed in parallel cathode and anode,
Setting source current is 2 mA, and two electrode spacings of guarantee are 20 mm；Sedimentation time is that 10 min uniformly gather in indium tin oxide surfaces
Polyaniline is closed, polyaniline/tin indium oxide combination electrode is made；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
The negative of programmable DC power supply 6 is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode 2
Pole, platinized platinum, which is used as, accesses positive pole to electrode 3, with the mixed liquor of 1 mol/L sodium chloride solution and 0.2 mmol/L palladium chloride
As electric depositing solution, in 3 mA electric currents, 10 min of electro-deposition, to palladium uniform deposition to polyaniline/tin indium oxide combination electrode
On, palladium/polyaniline/tin indium oxide combination electrode is made.Reactor 1 is reaction vessel, step 1) and 2) in make solution
Uniformly mixing heat-collecting magnetic stirring device 5 drives rotor 4 to be stirred material, and provides constant temperature for reaction, this is this field
Common sense.
Using tetracycline wastewater as degradation object, using the palladium/polyaniline/tin indium oxide combination electrode prepared as work
Make electrode 2 to be connected with the cathode of power supply, platinum electrode is connected as to electrode 3 with the anode of power supply.
2,4- tetracycline is carried out electrically-degradable:
Optimum experimental condition: 1mL aniline is mixed with 0.5 mol/L sulfuric acid of 99mL, and operating current is 2 mA when loading polyaniline,
Load time is 10 min, and when depositing Pd, NaCl concentration is 1 mol/L, PdCl2Concentration is 0.2 mmol/L, constant current 4
MA, sedimentation time are 30 min.In order to investigate palladium/polyaniline/tin indium oxide combination electrode degradation effect, electrode is carried out
The research of electrochemical degradation tetracycline, test result are as follows: in 3 mA of operating current, 30 min of reaction time, the palladium/polyaniline/
Tin indium oxide combination electrode makes tetracycline wastewater be down to 5.87 mg/L by 20 mg/L of initial concentration, and degradation rate is reachable
70.65%.60 min are reacted, degradation rate is up to 100%.Fig. 1 palladium/polyaniline/tin indium oxide combination electrode scanning electron microscope (SEM) photograph explanation
Palladium/polyaniline/tin indium oxide combination electrode degradation effect is good, stability is good.Result of study proves that the invention has very
Good practical potentiality and development prospect.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill of the art
For personnel, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications
It should be considered as protection scope of the present invention.
Claims (3)
1. a kind of palladium/polyaniline/tin indium oxide method for preparing composite electrode, which is characterized in that it the following steps are included:
1) polyaniline/tin indium oxide combination electrode is prepared using anodizing
Using indium tin oxide-coated glass as matrix, be put into dehydrated alcohol 5 ~ 15min of ultrasonic oil removing, then with ultrapure water 5 ~
15min removes impurity, is then dried, spare；Polyaniline is prepared using anodizing, 1mL aniline is slowly dropped into dress
There are 99 mL, concentration is to carry out 30 min of ultrasonic disperse in 0.1 ~ 5 mol/L sulfuric acid solution；Using bipolar electrode system by polyaniline
It is aggregated in indium tin oxide-coated glass surface, the indium tin oxide-coated glass of drying is connected to programmable DC as working electrode
Positive pole uses platinized platinum to be connected to power cathode forming circuit as to electrode, carries out electrochemical polymerization, oxidation using galvanostatic method
It is the mm of 20 mm × 10 that indium tin electro-conductive glass, which immerses solution effective area, is placed in parallel cathode and anode, between two electrodes of guarantee
Away from for 10 ~ 40 mm；Sedimentation time is 1 ~ 20 min in indium tin oxide surfaces homogeneous polymerization polyaniline, and polyaniline/indium oxide is made
Tin combination electrode；
2) palladium/polyaniline/tin indium oxide combination electrode is prepared using constant current electrodeposition process
Programmable DC power cathode is accessed using polyaniline made from step 1)/tin indium oxide combination electrode as working electrode,
Platinized platinum, which is used as, accesses positive pole to electrode, with 0.1 ~ 2 mol/L sodium chloride solution and 0.001 ~ 10.0 mmol/L palladium chloride
Mixed liquor is as electric depositing solution, in 1 ~ 10 mA electric current, 2 ~ 20 min of electro-deposition, to palladium uniform deposition to polyaniline/indium oxide
On tin combination electrode, palladium/polyaniline/tin indium oxide combination electrode is obtained.
2. a kind of palladium/polyaniline/tin indium oxide method for preparing composite electrode according to claim 1, characterized in that preparation
Palladium/polyaniline/tin indium oxide combination electrode.
3. a kind of palladium/polyaniline/tin indium oxide method for preparing composite electrode according to claim 1 or 2, characterized in that
The application of palladium/polyaniline of preparation/tin indium oxide combination electrode electrochemical degradation antibiotic waste water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111606353A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO target grinding waste liquid |
| CN113231059A (en) * | 2021-04-09 | 2021-08-10 | 厦门大学 | Composite catalyst for electron beam sewage treatment and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003092100A1 (en) * | 2001-08-24 | 2003-11-06 | The Government Of The United States Of America As Represented By The Secretary Of The Navy | Bio-based microbattery and methods for fabrication of same |
| US20060152147A1 (en) * | 2005-01-07 | 2006-07-13 | Lee Tae-Woo | Electroluminescent device and method for preparing the same |
| CN101412855A (en) * | 2008-12-04 | 2009-04-22 | 中国科学院长春应用化学研究所 | Bipyridine ruthenium dye containing S, Se or Te as donating electron group and use thereof in dye sensitization solar cell |
| CN103107212A (en) * | 2013-02-01 | 2013-05-15 | 中国科学院上海微系统与信息技术研究所 | Heterojunction solar battery with electroplate electrodes and preparation method |
| CN104610543A (en) * | 2013-11-04 | 2015-05-13 | 新昌县冠阳技术开发有限公司 | Conductive polymeric material |
-
2019
- 2019-06-07 CN CN201910493771.1A patent/CN110171872A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003092100A1 (en) * | 2001-08-24 | 2003-11-06 | The Government Of The United States Of America As Represented By The Secretary Of The Navy | Bio-based microbattery and methods for fabrication of same |
| US20060152147A1 (en) * | 2005-01-07 | 2006-07-13 | Lee Tae-Woo | Electroluminescent device and method for preparing the same |
| CN101412855A (en) * | 2008-12-04 | 2009-04-22 | 中国科学院长春应用化学研究所 | Bipyridine ruthenium dye containing S, Se or Te as donating electron group and use thereof in dye sensitization solar cell |
| CN103107212A (en) * | 2013-02-01 | 2013-05-15 | 中国科学院上海微系统与信息技术研究所 | Heterojunction solar battery with electroplate electrodes and preparation method |
| CN104610543A (en) * | 2013-11-04 | 2015-05-13 | 新昌县冠阳技术开发有限公司 | Conductive polymeric material |
Non-Patent Citations (2)
| Title |
|---|
| A. NIRMALA GRACE ETC.: ""Pt,Pt-Pd and Pt-Pd/Ru nanoparticles entrapped polyaniline electrodes-A potent electrocatalyst towards the oxidation of glycerol"", 《ELECTROCHEMISTRY COMMUNICATIONS》 * |
| 张健: "钯修饰电极的制备及电催化降解氯代有机物的研究", 《中国博士学位论文全文数据库 (工程科技Ⅰ辑)》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111606353A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO target grinding waste liquid |
| CN111606353B (en) * | 2020-06-03 | 2022-04-26 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO target grinding waste liquid |
| CN113231059A (en) * | 2021-04-09 | 2021-08-10 | 厦门大学 | Composite catalyst for electron beam sewage treatment and preparation method and application thereof |
| CN113231059B (en) * | 2021-04-09 | 2022-08-05 | 厦门大学 | Composite catalyst for electron beam sewage treatment and preparation method and application thereof |
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