CN108178248A - The graphite electrode modified based on CuO-CoO-ZnO and pyridine - Google Patents
The graphite electrode modified based on CuO-CoO-ZnO and pyridine Download PDFInfo
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- CN108178248A CN108178248A CN201711461121.6A CN201711461121A CN108178248A CN 108178248 A CN108178248 A CN 108178248A CN 201711461121 A CN201711461121 A CN 201711461121A CN 108178248 A CN108178248 A CN 108178248A
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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
- C02F1/467—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
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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
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Abstract
The invention discloses a kind of graphite electrodes modified based on CuO CoO ZnO and pyridine.Graphite rod after cleaning is through Cu (NO3)2, obtain substance C after the mixed liquor processing for preparing of 2 chlorine, 5 iodine pyridine, n-butanol, isopropanol, methanol and 3 methyl, 4 nitropyridine.Substance C is through Co (NO3)2, obtain substance D after the mixed liquor processing for preparing of 2 chlorine, 3 nitropyridine, n-butanol, isopropanol, methanol and 4 aminopyridines.Substance D is through Zn (NO3)2, the substance that obtains after the mixed liquor processing for preparing of 2 ethylpyridines, n-butanol, isopropanol, methanol and 3 amino, 2 fluorine pyridine be the graphite electrode modified based on CuO CoO ZnO and pyridine.The invention has the advantages that the features such as graphite electrode obtained modified based on CuO CoO ZnO and pyridine active high, adaptable, long lifespan.
Description
Technical field
The invention belongs to the chemically modified electrode technical fields of electrochemical treatment of wastewater, more particularly to a kind of to be based on CuO-
CoO-ZnO and the graphite electrode of pyridine modification.
Background technology
Electro-catalytic oxidation technology is by generating the active group of the strong oxidizing properties such as hydroxyl radical free radical come having in degrading waste water
Machine pollutant has the characteristics that non-secondary pollution, at low cost, strong applicability, efficient, in processing high concentration, bio-refractory
There is application potential in terms of waste water.Electrochemical reaction is usually what is carried out near electrode surface, therefore electrode surface performance is such as
What is most important, selects suitable electrode material and it is modified, to improve the surface catalysis performance of electrode, become electrochemistry
The new issue of worker's research.How to improve the hydrogen reduction catalytic performance of electrode becomes the hot spot of research, there is many research collection
In in modified electrode material to improve its hydrogen reduction catalytic performance.The surface microstructure and state of electro catalytic electrode are to influence electricity
An important factor for catalytic performance, also lacks high, adaptable, long lifespan the electrode of activity at present.
Invention content
The object of the present invention is to provide a kind of graphite electrodes modified based on CuO-CoO-ZnO and pyridine.Prepare the graphite
Electrode method is as follows：
(1) it is to be put into the burning equipped with 250mL ethyl alcohol after 4cm graphite rods are polished by a diameter of 1cm, length with 1000 mesh sand paper
It is impregnated 30 minutes in cup, takes out and obtain substance A 1 after rinsing with ruinning water with 500mL；Substance A 1 is put into 250mL percents by volume
It is impregnated 30 minutes in a concentration of 50% sulfuric acid solution, takes out and obtain substance A 2 after rinsing with ruinning water with 500mL；Substance A 2 is put
Enter and impregnated 30 minutes in the NaOH solution that 250mL mass percent concentrations are 10%, take out and obtained after rinsing with ruinning water with 500mL
Substance A 3；Substance A is obtained after substance A 3 is dried；
(2) by 4.52 grams of Cu (NO3)2It is added in 1500mL deionized waters, is stirred 3 minutes under the conditions of 1000r/min,
Then 1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor
H4, mixed liquor H5；
(3) by the chloro- 5- iodine pyridines of 2.61 grams of 2-, 15mL n-butanols, 25mL isopropanols and 10mL methanol be added to 150mL without
In water-ethanol, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor J1, mixed liquor J2,
Mixed liquor J3, mixed liquor J4, mixed liquor J5；
(4) mixed liquor J1 and 0.8 gram of 3- methyl -4- nitropyridine are added in mixed liquor H1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K1；
(5) substance A is added in mixed liquor K1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Substance B 1 is obtained, substance B 1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 2；
(6) mixed liquor J2 and 0.7 gram of 3- methyl -4- nitropyridine are added in mixed liquor H2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K2；
(7) substance B 2 is added in mixed liquor K2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 3, and substance B 3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 4；
(8) mixed liquor J3 and 0.6 gram of 3- methyl -4- nitropyridine are added in mixed liquor H3, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K3；
(9) substance B 4 is added in mixed liquor K3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 5, and substance B 5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 6；
(10) mixed liquor J4 and 0.5 gram of 3- methyl -4- nitropyridine are added in mixed liquor H4, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K4；
(11) substance B 6 is added in mixed liquor K4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 7, and substance B 7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 8；
(12) mixed liquor J5 and 0.4 gram of 3- methyl -4- nitropyridine are added in mixed liquor H5, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K6；
(13) substance B 8 is added in mixed liquor K5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 9, and substance B 9 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C；
(14) by 3.66 grams of Co (NO3)2It is added in 1500mL deionized waters, is stirred 3 minutes under the conditions of 1000r/min,
Then 1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor L1, mixed liquor L2, mixed liquor L3, mixed liquor
L4, mixed liquor L5；
(15) the chloro- 3- nitropyridines of 2.03 grams of 2-, 15mL n-butanols, 25mL isopropanols and 10mL methanol are added to
It in 150mL absolute ethyl alcohols, is stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor M1, mix
Close liquid M2, mixed liquor M3, mixed liquor M4, mixed liquor M5；
(16) mixed liquor M1 and 0.96 gram of 4-aminopyridine are added in mixed liquor L1, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N1；
(17) substance C is added in mixed liquor N1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 2；
(18) mixed liquor M2 and 0.91 gram of 4-aminopyridine are added in mixed liquor L2, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N2；
(19) substance C 2 is added in mixed liquor N2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 3, and substance C 3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 4；
(20) mixed liquor M3 and 0.86 gram of 4-aminopyridine are added in mixed liquor L3, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N3；
(21) substance C 4 is added in mixed liquor N3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 5, and substance C 5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 6；
(22) mixed liquor M4 and 0.81 gram of 4-aminopyridine are added in mixed liquor L4, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N4；
(23) substance C 6 is added in mixed liquor N4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 7, and substance C 7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 8；
(24) mixed liquor M5 and 0.76 gram of 4-aminopyridine are added in mixed liquor L5, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N5；
(25) substance C 8 is added in mixed liquor N5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 9, and substance C 9 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D；
(26) by 2.99 grams of Zn (NO3)2It is added in 1500mL deionized waters, is stirred 3 minutes under the conditions of 1000r/min,
Then 1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor O1, mixed liquor O2, mixed liquor O3, mixed liquor
O4, mixed liquor O5；
(27) that 1.04 grams of 2- ethylpyridines, 15mL n-butanols, 25mL isopropanols and 10mL methanol are added to 150mL is anhydrous
It in ethyl alcohol, is stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor P1, mixed liquor P2, mix
Close liquid P3, mixed liquor P4, mixed liquor P5；
(28) mixed liquor P1 and 0.77 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q1；
(29) substance D is added in mixed liquor Q1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D1, and substance D1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D2；
(30) mixed liquor P2 and 0.73 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q2；
(31) substance D2 is added in mixed liquor Q2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D3, and substance D3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D4；
(32) mixed liquor P3 and 0.69 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O3, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q3；
(33) substance D4 is added in mixed liquor Q3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D5, and substance D5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D6；
(34) mixed liquor P4 and 0.65 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O4, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q4；
(35) substance D6 is added in mixed liquor Q4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D7, and substance D7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D8；
(36) mixed liquor P5 and 0.61 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O5, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q5；
(37) substance D8 is added in mixed liquor Q5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D9, substance D9 is placed 180 minutes in drying box of the temperature for 95 DEG C, obtained substance is based on CuO-
CoO-ZnO and the graphite electrode of pyridine modification.
The invention has the advantages that the graphite electrode obtained modified based on CuO-CoO-ZnO and pyridine is active
The features such as high, adaptable, long lifespan.
Specific embodiment
The present invention provides the graphite electrode modified based on CuO-CoO-ZnO and pyridine, illustrates below by an example
Its implementation process.
Embodiment 1.
(1) it is to be put into the burning equipped with 250mL ethyl alcohol after 4cm graphite rods are polished by a diameter of 1cm, length with 1000 mesh sand paper
It is impregnated 30 minutes in cup, takes out and obtain substance A 1 after rinsing with ruinning water with 500mL；Substance A 1 is put into 250mL percents by volume
It is impregnated 30 minutes in a concentration of 50% sulfuric acid solution, takes out and obtain substance A 2 after rinsing with ruinning water with 500mL；Substance A 2 is put
Enter and impregnated 30 minutes in the NaOH solution that 250mL mass percent concentrations are 10%, take out and obtained after rinsing with ruinning water with 500mL
Substance A 3；Substance A is obtained after substance A 3 is dried；
(2) by 4.52 grams of Cu (NO3)2It is added in 1500mL deionized waters, is stirred 3 minutes under the conditions of 1000r/min,
Then 1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor
H4, mixed liquor H5；
(3) by the chloro- 5- iodine pyridines of 2.61 grams of 2-, 15mL n-butanols, 25mL isopropanols and 10mL methanol be added to 150mL without
In water-ethanol, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor J1, mixed liquor J2,
Mixed liquor J3, mixed liquor J4, mixed liquor J5；
(4) mixed liquor J1 and 0.8 gram of 3- methyl -4- nitropyridine are added in mixed liquor H1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K1；
(5) substance A is added in mixed liquor K1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Substance B 1 is obtained, substance B 1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 2；
(6) mixed liquor J2 and 0.7 gram of 3- methyl -4- nitropyridine are added in mixed liquor H2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K2；
(7) substance B 2 is added in mixed liquor K2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 3, and substance B 3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 4；
(8) mixed liquor J3 and 0.6 gram of 3- methyl -4- nitropyridine are added in mixed liquor H3, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K3；
(9) substance B 4 is added in mixed liquor K3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 5, and substance B 5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 6；
(10) mixed liquor J4 and 0.5 gram of 3- methyl -4- nitropyridine are added in mixed liquor H4, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K4；
(11) substance B 6 is added in mixed liquor K4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 7, and substance B 7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 8；
(12) mixed liquor J5 and 0.4 gram of 3- methyl -4- nitropyridine are added in mixed liquor H5, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K6；
(13) substance B 8 is added in mixed liquor K5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 9, and substance B 9 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C；
(14) by 3.66 grams of Co (NO3)2It is added in 1500mL deionized waters, is stirred 3 minutes under the conditions of 1000r/min,
Then 1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor L1, mixed liquor L2, mixed liquor L3, mixed liquor
L4, mixed liquor L5；
(15) the chloro- 3- nitropyridines of 2.03 grams of 2-, 15mL n-butanols, 25mL isopropanols and 10mL methanol are added to
It in 150mL absolute ethyl alcohols, is stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor M1, mix
Close liquid M2, mixed liquor M3, mixed liquor M4, mixed liquor M5；
(16) mixed liquor M1 and 0.96 gram of 4-aminopyridine are added in mixed liquor L1, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N1；
(17) substance C is added in mixed liquor N1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 2；
(18) mixed liquor M2 and 0.91 gram of 4-aminopyridine are added in mixed liquor L2, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N2；
(19) substance C 2 is added in mixed liquor N2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 3, and substance C 3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 4；
(20) mixed liquor M3 and 0.86 gram of 4-aminopyridine are added in mixed liquor L3, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N3；
(21) substance C 4 is added in mixed liquor N3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 5, and substance C 5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 6；
(22) mixed liquor M4 and 0.81 gram of 4-aminopyridine are added in mixed liquor L4, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N4；
(23) substance C 6 is added in mixed liquor N4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 7, and substance C 7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 8；
(24) mixed liquor M5 and 0.76 gram of 4-aminopyridine are added in mixed liquor L5, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N5；
(25) substance C 8 is added in mixed liquor N5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 9, and substance C 9 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D；
(26) by 2.99 grams of Zn (NO3)2It is added in 1500mL deionized waters, is stirred 3 minutes under the conditions of 1000r/min,
Then 1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor O1, mixed liquor O2, mixed liquor O3, mixed liquor
O4, mixed liquor O5；
(27) that 1.04 grams of 2- ethylpyridines, 15mL n-butanols, 25mL isopropanols and 10mL methanol are added to 150mL is anhydrous
It in ethyl alcohol, is stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor P1, mixed liquor P2, mix
Close liquid P3, mixed liquor P4, mixed liquor P5；
(28) mixed liquor P1 and 0.77 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q1；
(29) substance D is added in mixed liquor Q1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D1, and substance D1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D2；
(30) mixed liquor P2 and 0.73 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q2；
(31) substance D2 is added in mixed liquor Q2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D3, and substance D3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D4；
(32) mixed liquor P3 and 0.69 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O3, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q3；
(33) substance D4 is added in mixed liquor Q3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D5, and substance D5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D6；
(34) mixed liquor P4 and 0.65 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O4, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q4；
(35) substance D6 is added in mixed liquor Q4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D7, and substance D7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D8；
(36) mixed liquor P5 and 0.61 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O5, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor Q5；
(37) substance D8 is added in mixed liquor Q5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid
Body obtains substance D9, substance D9 is placed 180 minutes in drying box of the temperature for 95 DEG C, obtained substance is based on CuO-
CoO-ZnO and the graphite electrode of pyridine modification.
Here is to be seated in two with the method for the present invention graphite electrode obtained modified based on CuO-CoO-ZnO and pyridine
Degrading experiment has been carried out to pharmacy waste water in dimension electrode reactor, has been further illustrated the present invention.
Two-dimentional electricity will be seated in the graphite electrode modified made from the method for the present invention based on CuO-CoO-ZnO and pyridine
In the reactor of pole, Degrading experiment is carried out to pharmacy waste water, the results showed that the two-dimensional electrode reactor for being filled with the electrode can
COD in efficient process pharmacy waste water, when influent COD is 986mg/L, the COD in being discharged after processing is reduced to 64mg/L.
Claims (1)
1. a kind of graphite electrode modified based on CuO-CoO-ZnO and pyridine, which is characterized in that prepare the graphite electrode method
It is as follows：
(1) it is to be put into the beaker equipped with 250mL ethyl alcohol after 4cm graphite rods are polished by a diameter of 1cm, length with 1000 mesh sand paper
It impregnates 30 minutes, takes out and obtain substance A 1 after rinsing with ruinning water with 500mL；Substance A 1 is put into 250mL concentration of volume percent
To be impregnated 30 minutes in 50% sulfuric acid solution, take out and obtain substance A 2 after rinsing with ruinning water with 500mL；Substance A 2 is put into
250mL mass percent concentrations are to be impregnated 30 minutes in 10% NaOH solution, take out and obtain object after rinsing with ruinning water with 500mL
Matter A3；Substance A is obtained after substance A 3 is dried；
(2) by 4.52 grams of Cu (NO3)2It is added in 1500mL deionized waters, stirs 3 minutes under the conditions of 1000r/min, then
1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, mixed liquor H1 is obtained, mixed liquor H2, mixed liquor H3, mixed liquor H4, mixes
Close liquid H5；
(3) the chloro- 5- iodine pyridines of 2.61 grams of 2-, 15mL n-butanols, 25mL isopropanols and 10mL methanol are added to the anhydrous second of 150mL
It in alcohol, is stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor J1, mixed liquor J2, mixing
Liquid J3, mixed liquor J4, mixed liquor J5；
(4) mixed liquor J1 and 0.8 gram of 3- methyl -4- nitropyridine are added in mixed liquor H1, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor K1；
(5) substance A is added in mixed liquor K1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
Substance B 1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 2 by substance B 1；
(6) mixed liquor J2 and 0.7 gram of 3- methyl -4- nitropyridine are added in mixed liquor H2, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor K2；
(7) substance B 2 is added in mixed liquor K2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance B 3, substance B 3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 4；
(8) mixed liquor J3 and 0.6 gram of 3- methyl -4- nitropyridine are added in mixed liquor H3, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor K3；
(9) substance B 4 is added in mixed liquor K3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance B 5, substance B 5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 6；
(10) mixed liquor J4 and 0.5 gram of 3- methyl -4- nitropyridine are added in mixed liquor H4, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor K4；
(11) substance B 6 is added in mixed liquor K4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance B 7, substance B 7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance B 8；
(12) mixed liquor J5 and 0.4 gram of 3- methyl -4- nitropyridine are added in mixed liquor H5, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor K6；
(13) substance B 8 is added in mixed liquor K5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance B 9, substance B 9 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C；
(14) by 3.66 grams of Co (NO3)2It is added in 1500mL deionized waters, stirs 3 minutes under the conditions of 1000r/min, then
1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, mixed liquor L1 is obtained, mixed liquor L2, mixed liquor L3, mixed liquor L4, mixes
Close liquid L5；
(15) by the chloro- 3- nitropyridines of 2.03 grams of 2-, 15mL n-butanols, 25mL isopropanols and 10mL methanol be added to 150mL without
In water-ethanol, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor M1, mixed liquor M2,
Mixed liquor M3, mixed liquor M4, mixed liquor M5；
(16) mixed liquor M1 and 0.96 gram of 4-aminopyridine are added in mixed liquor L1,3 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor N1；
(17) substance C is added in mixed liquor N1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance C 1, substance C 1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 2；
(18) mixed liquor M2 and 0.91 gram of 4-aminopyridine are added in mixed liquor L2,3 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor N2；
(19) substance C 2 is added in mixed liquor N2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance C 3, substance C 3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 4；
(20) mixed liquor M3 and 0.86 gram of 4-aminopyridine are added in mixed liquor L3,3 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor N3；
(21) substance C 4 is added in mixed liquor N3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance C 5, substance C 5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 6；
(22) mixed liquor M4 and 0.81 gram of 4-aminopyridine are added in mixed liquor L4,3 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor N4；
(23) substance C 6 is added in mixed liquor N4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance C 7, substance C 7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance C 8；
(24) mixed liquor M5 and 0.76 gram of 4-aminopyridine are added in mixed liquor L5,3 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor N5；
(25) substance C 8 is added in mixed liquor N5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance C 9, substance C 9 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D；
(26) by 2.99 grams of Zn (NO3)2It is added in 1500mL deionized waters, stirs 3 minutes under the conditions of 1000r/min, then
1.5mL concentrated nitric acids are added in, 5 parts of equivalent is divided into after shaking up, mixed liquor O1 is obtained, mixed liquor O2, mixed liquor O3, mixed liquor O4, mixes
Close liquid O5；
(27) 1.04 grams of 2- ethylpyridines, 15mL n-butanols, 25mL isopropanols and 10mL methanol are added to 150mL absolute ethyl alcohols
In, it is stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor
P3, mixed liquor P4, mixed liquor P5；
(28) mixed liquor P1 and 0.77 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O1, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor Q1；
(29) substance D is added in mixed liquor Q1, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance D1, substance D1 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D2；
(30) mixed liquor P2 and 0.73 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O2, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor Q2；
(31) substance D2 is added in mixed liquor Q2, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance D3, substance D3 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D4；
(32) mixed liquor P3 and 0.69 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O3, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor Q3；
(33) substance D4 is added in mixed liquor Q3, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance D5, substance D5 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D6；
(34) mixed liquor P4 and 0.65 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O4, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor Q4；
(35) substance D6 is added in mixed liquor Q4, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance D7, substance D7 in drying box of the temperature for 95 DEG C is placed 180 minutes, obtains substance D8；
(36) mixed liquor P5 and 0.61 gram of 3- amino -2- fluorine pyridine are added in mixed liquor O5, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor Q5；
(37) substance D8 is added in mixed liquor Q5, is shaken 180 minutes in the shaking table for being 40 DEG C in temperature, be filtered to remove liquid and obtain
To substance D9, substance D9 is placed 180 minutes in drying box of the temperature for 95 DEG C, obtained substance is based on CuO-CoO-
ZnO and the graphite electrode of pyridine modification.
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