CN109607696A - A kind of natural magnetite/carbon black/graphite felt composite cathode preparation method applied to electric Fenton-like system - Google Patents
A kind of natural magnetite/carbon black/graphite felt composite cathode preparation method applied to electric Fenton-like system Download PDFInfo
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- CN109607696A CN109607696A CN201811626109.0A CN201811626109A CN109607696A CN 109607696 A CN109607696 A CN 109607696A CN 201811626109 A CN201811626109 A CN 201811626109A CN 109607696 A CN109607696 A CN 109607696A
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- Prior art keywords
- graphite felt
- carbon black
- natural magnetite
- composite cathode
- electric fenton
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
A kind of natural magnetite/carbon black/graphite felt composite cathode preparation method applied to electric Fenton-like system, belongs to technical field of electrochemical water treatment.Natural magnetite is added in carbon black and polytetrafluoroethylene (PTFE) mixed solution in the present invention, is supported on graphite felt surface by concussion method, prepares natural magnetite/carbon black/graphite felt composite cathode by calcining.Heterogeneous electric Fenton-like system is formed in the electrolytic cell containing electrolyte solution with inert anode, handles classes of herbicides organic pollutant difficult to degrade.Magnetic iron ore used in the present invention is natural minerals, cheap, from a wealth of sources, and using the cathode composite that it is prepared, process is simple, and electro catalytic activity with higher.
Description
Technical field
The invention belongs to technical field of electrochemical water treatment, and in particular to a kind of natural magnetite/carbon black/graphite felt is compound
The preparation method of cathode.
Background technique
Electro-fenton process is to generate strong oxidizing property by the hydrogen peroxide of transition-metal catalyst catalytic cathode original position electro synthesis
Substance (OH) carrys out a kind of electrochemical water treatment technology of the organic matter in degrading waste water.With other high-level oxidation technology phases
Than, electro-fenton process because have the characteristics that reaction speed it is faster, it is easily operated be considered as a kind of excellent high-level oxidation technology.But
This method needs to adjust wastewater pH to acidity and there are secondary pollution problems caused by since metallic catalyst is added.Therefore many
More researchers avoid iron ion in electric Fenton-like system under high ph conditions by the way that iron oxide is supported on cathode material surface
Precipitating occurs and complex reaction generates iron cement.
In these iron oxide, magnetic iron ore is considered as a kind of effective heterogeneous catalysis.Natural magnetite is a kind of
Cheap mineral mining by-product, widely distributed, main component Fe3O4.Due to the octahedral position of natural magnetite crystal structure
Set that there are Fe2+And Fe3+Ion, itself can catalyzing and decomposing H2O2, hydroxyl radical free radical is generated, so that having during electro-Fenton reaction
There is higher catalytic activity.On the other hand, the intrinsic magnetism of natural magnetite make at the end of electric Fenton technology catalyst with
The separation of reaction solution becomes easy.
The present invention modifies graphite felt cathode using natural magnetite and carbon black, avoids wastewater pH adjusting and metal
Catalyst adds and the secondary pollution problem that generates.
Summary of the invention
It is an object of the invention to solve the problems of the prior art, provide a kind of low in cost, production method is simple, tool
There is natural magnetite/carbon black of more active site and good hydrogen reduction electrocatalysis characteristic/graphite felt composite cathode preparation
Method.
The preparation method of above-mentioned natural magnetite/carbon black/graphite felt composite cathode, comprising the following steps:
(1) graphite felt ultrasonic cleaning removal impurity in acetone soln is placed in then for several times with ultrapure water to remove residual
Acetone is stayed, is dried in drying box, pretreated graphite felt is obtained；
(2) hydrocarbon black powder and polytetrafluoroethylsolution solution are added sequentially in the mixed solution of isopropanol and ultrapure water, are surpassed
Sound dispersion, obtains finely dispersed dispersion solution；The volume ratio of ultrapure water and isopropanol is (0.5-2) in mixed solution: 1；
(3) the natural magnetite powder of different quality is added in step (2) mixed solution, is shaken in constant temperature oscillator
It swings uniformly mixed；
(4) graphite felt for cleaning step (1), is impregnated in the mixed solution that step (3) obtains, in constant temperature oscillator
Concussion is 10~120min, and revolving speed is 120~200r/min；
(5) composite graphite felt obtained step (4) takes out, and dries in drying box, be subsequently placed in 250 in Muffle furnace~
400 DEG C of 1~2h of calcining, can be obtained natural magnetite/carbon black/graphite felt composite cathode.
Further preferred hydrocarbon black powder: polytetrafluoroethylsolution solution: the dosage relation of natural magnetite powder is every 0.8g charcoal
Black powder corresponding 0.8~5.6g (preferably 4g) polytetrafluoroethylsolution solution, 0.1~1.0g (preferably 0.7g) natural magnetite powder.
Compared with prior art, the present invention has following excellent effect:
1, the present invention increases the electro-chemical activity of electrode, improves cathode peroxidating in graphite felt area load carbon black
Hydrogen yield provides a large amount of attachment sites for magnetic iron ore.
2, the present invention is directly carried on electrode using natural magnetite as catalyst, increases reactivity site, is shortened
Reaction time is conducive to the catalytic activity for enhancing electrode, improves electro-fenton process and handles organic wastewater efficiency.
3, the present invention is modified natural magnetite in electrode surface using concussion method, easy to operate, is subsequent native magnet
The preparation of mine/carbon black/graphite felt composite cathode provides basis.
4, natural magnetite/carbon black prepared by the present invention/graphite felt composite cathode electrode, catalytic activity with higher.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of pretreating graphite felt.
Fig. 2 is carbon black/graphite felt cathode scanning electron microscopic picture.
Fig. 3 is natural magnetite/carbon black/graphite felt composite cathode scanning electron microscopic picture.
Fig. 4 is compound for natural magnetite/carbon black/graphite felt composite cathode of embodiment, carbon black/graphite felt of comparative example 1
The effect picture of cathode and the graphite felt cathode of comparative example 2 degradation Atrazine.
Specific embodiment
Following example and comparative example will the present invention is further illustrated in conjunction with attached drawing, but the present invention is not limited to
Lower embodiment.
Embodiment:
(1) graphite felt (4cm × 5cm) is placed in ultrasonic cleaning removal impurity in acetone soln, then uses ultrapure water
For several times, residual acetone is removed, dries, is obtained by pretreated graphite felt in drying box；
(2) hydrocarbon black powder (0.8g) and 60% polytetrafluoroethylsolution solution of mass percentage (4g) are added sequentially to 40mL
In the mixed solution of isopropanol and ultrapure water, ultrasonic disperse obtains finely dispersed mixed solution；
(3) 0.7g natural magnetite powder is added in step (2) mixed solution, dispersion is shaken in constant temperature oscillator
Uniformly；
(4) graphite felt for cleaning step (1), is impregnated in the mixed solution that step (3) obtains, in constant temperature oscillator
30min is shaken with the revolving speed of 180r/min；
(5) composite graphite felt for obtaining step (4) takes out, and dries in drying box, is subsequently placed in Muffle furnace 360 DEG C
1h is calcined, natural magnetite/carbon black/graphite felt composite cathode can be obtained.
(6) for the natural magnetite/carbon black/graphite felt combination electrode obtained using step (5) as cathode, Pt piece is anode, drop
Solve the Atrazine waste water that 250mL concentration is 10mg/L.0.05mol/L anhydrous sodium sulfate is as electrolyte, kinetic current
100mA, reaction solution pH are 6.8.
Comparative example 1:
Step (1) step (2) preparation process same embodiment step (1) step (2)
(3) graphite felt for cleaning step (1), is impregnated in the mixed solution that step (2) obtains, in constant temperature oscillator
Shake 20min；
(4) composite graphite felt for obtaining step (3) takes out, and dries in drying box, is subsequently placed in Muffle furnace 360 DEG C
1h is calcined to get carbon black/graphite felt composite cathode of preparation is arrived.
(5) carbon black obtained using step (4)/graphite felt combination electrode is cathode, remaining experiment same embodiment of reaction condition
Step (6).
Comparative example 2:
(1) graphite felt (4cm × 5cm) is placed in ultrasonic cleaning removal impurity in acetone soln, then uses ultrapure water
For several times, residual acetone is removed, dries, is obtained by pretreated graphite felt in drying box；
(2) using the graphite felt after cleaning as cathode, remaining experiment same embodiment step of reaction condition (6).
From fig. 4, it can be seen that Atrazine, (Atrazine initial concentration is embodiment compared with comparative example 1 and comparative example 2
10mg/L) treatment effect is more preferable, and anodizing efficiency is higher.
Claims (6)
1. a kind of natural magnetite/carbon black/graphite felt composite cathode preparation method applied to electric Fenton-like system, feature exist
In, comprising the following steps:
(1) graphite felt is placed in ultrasonic cleaning removal impurity in acetone soln, then for several times with ultrapure water, removal residual third
Ketone is dried in drying box, obtains pretreated graphite felt；
(2) hydrocarbon black powder and polytetrafluoroethylsolution solution are added sequentially in the mixed solution of isopropanol and ultrapure water, ultrasound point
It dissipates, obtains finely dispersed dispersion solution；The volume ratio of ultrapure water and isopropanol is (0.5-2) in mixed solution: 1；
(3) the natural magnetite powder of different quality is added in step (2) mixed solution, is shaken in constant temperature oscillator mixed
It closes uniform；
(4) graphite felt for cleaning step (1), is impregnated in the mixed solution that step (3) obtains, shakes in constant temperature oscillator
10~120min；The revolving speed of constant temperature oscillator is 120~200r/min；
(5) composite graphite felt for obtaining step (4) takes out, and dries, is subsequently placed in 250~400 in Muffle furnace in drying box
DEG C calcining 1~2h, natural magnetite/carbon black/graphite felt composite cathode can be obtained.
2. a kind of natural magnetite/carbon black/graphite felt composite cathode applied to electric Fenton-like system described in accordance with the claim 1
Preparation method, which is characterized in that hydrocarbon black powder: polytetrafluoroethylsolution solution: the dosage relation of natural magnetite powder is every
0.8g hydrocarbon black powder corresponds to 0.8~5.6g (preferably 4g) polytetrafluoroethylsolution solution, 0.1~1.0g (preferably 0.7g) natural magnetite
Powder.
3. a kind of natural magnetite/carbon black/graphite felt composite cathode applied to electric Fenton-like system described in accordance with the claim 1
Preparation method, which is characterized in that in step (4) the concussion time of constant temperature oscillator be 10~80min (preferably 30min), turn
Speed is 120~200r/min (preferably 180r/min).
4. natural magnetite/carbon black/graphite felt the composite cathode being prepared according to the described in any item methods of claim 1-3
Material.
5. natural magnetite/carbon black/graphite felt the composite cathode being prepared according to the described in any item methods of claim 1-3
The application of material, the electric Fenton oxidation processing as cathode, for classes of herbicides pollutant in water.
6. according to the application of claim 5, which is characterized in that carry out electric Fenton oxidation processing in neutral conditions.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112076759A (en) * | 2020-09-08 | 2020-12-15 | 湖南农业大学 | Graphite felt cathode, preparation method and application thereof |
| CN112456634A (en) * | 2020-10-15 | 2021-03-09 | 南京工业大学 | Water body purification system device with photo/bioelectrochemical integrated module and application thereof |
| CN113526646A (en) * | 2021-08-20 | 2021-10-22 | 中南大学 | electro-Fenton system for in-situ production of hydrogen peroxide by cathode/anode and application of electro-Fenton system in strengthening degradation of organic pollutants |
| CN114368807A (en) * | 2022-01-14 | 2022-04-19 | 中国科学技术大学 | Preparation method and application of chitosan-coated electro-Fenton cathode |
| CN114538569A (en) * | 2022-02-25 | 2022-05-27 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell0/FeOxGranular electro-Fenton cathode and preparation and application thereof |
| CN114620814A (en) * | 2022-03-31 | 2022-06-14 | 中国科学院南京土壤研究所 | Difunctional composite biomass carbon-based material and application thereof, difunctional composite carbon-based electrode and preparation method thereof |
| CN114804302A (en) * | 2022-04-19 | 2022-07-29 | 南京工业大学 | Iron-carbon-nitrogen-based catalyst/carbon black composite cathode and preparation and application thereof |
| CN115072839A (en) * | 2022-03-14 | 2022-09-20 | 南京理工大学 | Iron-containing composite magnetic material and preparation method and catalytic application thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112076759B (en) * | 2020-09-08 | 2023-07-25 | 湖南农业大学 | Graphite felt cathode, preparation method and application thereof |
| CN112076759A (en) * | 2020-09-08 | 2020-12-15 | 湖南农业大学 | Graphite felt cathode, preparation method and application thereof |
| CN112456634B (en) * | 2020-10-15 | 2022-12-27 | 南京工业大学 | Water body purification system device with photo/bioelectrochemical integrated module and application thereof |
| CN112456634A (en) * | 2020-10-15 | 2021-03-09 | 南京工业大学 | Water body purification system device with photo/bioelectrochemical integrated module and application thereof |
| CN113526646B (en) * | 2021-08-20 | 2022-04-05 | 中南大学 | electro-Fenton system for in-situ production of hydrogen peroxide by cathode/anode and application of electro-Fenton system in strengthening degradation of organic pollutants |
| CN113526646A (en) * | 2021-08-20 | 2021-10-22 | 中南大学 | electro-Fenton system for in-situ production of hydrogen peroxide by cathode/anode and application of electro-Fenton system in strengthening degradation of organic pollutants |
| CN114368807A (en) * | 2022-01-14 | 2022-04-19 | 中国科学技术大学 | Preparation method and application of chitosan-coated electro-Fenton cathode |
| CN114368807B (en) * | 2022-01-14 | 2023-03-10 | 中国科学技术大学 | Preparation method and application of chitosan-coated electro-Fenton cathode |
| CN114538569A (en) * | 2022-02-25 | 2022-05-27 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell0/FeOxGranular electro-Fenton cathode and preparation and application thereof |
| CN114538569B (en) * | 2022-02-25 | 2023-03-10 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell 0 /FeO X Granular electro-Fenton cathode and preparation and application thereof |
| CN115072839A (en) * | 2022-03-14 | 2022-09-20 | 南京理工大学 | Iron-containing composite magnetic material and preparation method and catalytic application thereof |
| CN115072839B (en) * | 2022-03-14 | 2023-08-08 | 南京理工大学 | Iron-containing composite magnetic material, preparation method and catalytic application thereof |
| CN114620814A (en) * | 2022-03-31 | 2022-06-14 | 中国科学院南京土壤研究所 | Difunctional composite biomass carbon-based material and application thereof, difunctional composite carbon-based electrode and preparation method thereof |
| CN114804302A (en) * | 2022-04-19 | 2022-07-29 | 南京工业大学 | Iron-carbon-nitrogen-based catalyst/carbon black composite cathode and preparation and application thereof |
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