CN110255697A - A kind of preparation of N doping carbon materials anode and its application in catalytic wet air oxidation - Google Patents
A kind of preparation of N doping carbon materials anode and its application in catalytic wet air oxidation Download PDFInfo
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- CN110255697A CN110255697A CN201910559273.2A CN201910559273A CN110255697A CN 110255697 A CN110255697 A CN 110255697A CN 201910559273 A CN201910559273 A CN 201910559273A CN 110255697 A CN110255697 A CN 110255697A
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/74—Treatment of water, waste water, or sewage by oxidation with air
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
It is using common three-dimensional carbon materials as substrate the invention discloses a kind of preparation of N doping carbon materials anode and its application in catalytic wet air oxidation, EDTA is nitrogen source, carries out the reaction of hydro-thermal N doping under certain temperature；Carbon materials are taken out after cooling and cleaned, dried and be placed in tube furnace, are heat-treated in nitrogen atmosphere, obtain N doping carbon materials material.Under normal temperature and pressure, in single chamber three-electrode system, using the N doping carbon materials material of preparation as the anode of battery, platinum filament is to electrode, and calomel electrode is reference electrode, under 1.0V voltage, 0.05molL‑1Na2SO4For electrolyte, under certain pH conditions, catalytic air oxidation waste water from dyestuff can be such that certain density a variety of dyestuffs completely remove in 2h.
Description
Technical field
The present invention relates to a kind of preparation and application of electric co-catalysis wet air oxidation catalyst, specifically a kind of nitrogen
The preparation and its application in catalytic wet air oxidation for adulterating carbon materials anode.
Background technique
Nitrogen-atoms is close with the radius of carbon atom, therefore the compatibility between carbon materials is good, is easy to adulterate the crystalline substance into carbon
In lattice, and stability with higher and durability.In addition, the N-C key generated can be such that the carbon atom for adjoining nitrogen-atoms has
More positive charges, the enhancing of electron adsorption, which will create more preferably condition, these characteristics for catalytic oxidation-reduction reaction, also to be made
It obtains N doping and is widely used in each catalytic field.Solvent heat or hydro-thermal method are due to mild condition, easy to operate and be suitable for
The advantages that large scale preparation is to carry out nitrogen-doped modified common method to carbon material at present, wherein reporting that more nitrogen source has
Ammonium hydroxide, urea, ammonium salt, hydrazine hydrate, melamine, triethanolamine etc..
Wet air oxidation is a kind of advanced oxidation technology that Organic Pollutants in Wastewater can be effectively treated.The technology is most
Early to be proposed in the 1950s by the F.J.Zimmermann in the U.S., it is in high temperature (125-320 DEG C) and high pressure (0.5-
Under the conditions of 20MPa), use air or oxygen that the organic pollutant in liquid phase is oxidized into carbon dioxide, water for oxidant
With the oxidation process (Kim&Ihm, J.Hazard.Mater.2011,186,16-34) of the simple small molecule such as organic acid.Wet type is empty
Gas oxidation technology is relatively stable for the treatment effeciency of organic pollutants all kinds of in water body, does not depend on additional chemical agent and environment
It is friendly.However, the depth degradation in order to realize organic pollutant within a short period of time, wet air oxidation reaction is needed in high temperature
It is carried out under condition of high voltage, this not only proposes harsh requirement to equipment material, but also energy consumption is also very high.Selection is suitably urged
Agent can reduce the temperature and pressure of wet air oxidation reaction to a certain extent.However, so far, there is still a need for 80
DEG C or more operation temperature and 0.5MPa or more operating pressure (Zhang et al., Sci.Rep.2014,4,6797).And it is right
For heterogeneous catalysis, reaction temperature is higher, inactivates caused by sintering or metal ion leaching as catalyst etc. tighter
Weight (Keav et al., Catal.Sci.Technol.2011,1,342-353).Exploitation oxidability is strong, stability is high, without gold
Belong to the normal temperature and pressure catalysis wet(air)oxidation system that ion leaches, for pushing wet air oxidation technology commercialization application tool
It is significant.
The application selects carbon materials cheap and easy to get as substrate, using simple hydro-thermal method combination heat treatment process, by nitrogen
It is doped to carbon materials surface, prepares N doping carbon materials electrode material, catalytic air is in room temperature under the driving of lower applied voltage
Organic dye waste water is aoxidized under normal pressure.
Summary of the invention
The present invention is intended to provide a kind of preparation of N doping carbon materials anode and its application in catalytic wet air oxidation,
N doping is obtained to carbon materials surface, then by suitably heat treatment by N doping carbon materials using hydro-thermal method first.It is mixed again with the nitrogen
Miscellaneous carbon materials are the certain density organic dye waste water of anode-catalyzed air oxidation, and degradation rate reaches 100% in 2h.
The preparation method of N doping carbon materials anode of the present invention, comprising the following steps:
Using common three-dimensional carbon materials as substrate, disodium EDTA is nitrogen source, carries out hydro-thermal nitrogen in certain temperature and mixes
Miscellaneous reaction；Carbon materials are taken out after cooling and cleaned, dried and be placed in tube furnace, are heat-treated in nitrogen atmosphere, obtain nitrogen and mix
Miscellaneous carbon materials material.
The three-dimensional carbon materials are selected from carbon fiber, carbon felt, foamy carbon or carbon cloth.It is first cleaned with acetone using preceding, then passes through 1%
H2O2Aqueous solution is in 120 DEG C of hydro-thermal process 12h.
The nitrogen source is disodium EDTA, and dosage is 2.5-12.5 times of carbon materials quality.
The reaction temperature of hydro-thermal N doping reaction is 120~200 DEG C, the reaction time is 8~for 24 hours.
The heat treatment temperature is 300~900 DEG C, and heat treatment time is 1~5h.
The application of N doping carbon materials anode prepared by the present invention is under applied voltage driving, with the N doping carbon materials
It is reacted as catalyst wet air oxidation, realizes the degradation of organic dyestuff at normal temperatures and pressures.Specifically in single chamber three
In electrode system, under normal temperature and pressure, using N doping carbon materials prepared by the present invention as the anode of battery, platinum filament be to electrode, it is sweet
Mercury electrode is reference electrode, under 1.0V voltage, 0.05molL-1Na2SO4For electrolyte, under certain pH conditions, catalytic air oxygen
Change waste water from dyestuff, certain density a variety of dyestuffs can be made to completely remove in 2h.
The organic dyestuff be one of neutral fuchsin, methylene blue, crystal violet, rhodamine B, concentration be 0~
50mg·L-1。
The pH value is 3-9, preferably 3-7.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
1, the present invention uses disodium EDTA for nitrogen source, passes through simple hydro-thermal reaction combination heat treatment process
The nitrogen-doped carbon material of available high nitrogen-containing.
2, the N doping carbon materials that the present invention obtains, the oxidation under normal temperature and pressure and the driving of lower external voltage, to oxygen
With high catalytic activity, organic pollutant can be made to obtain fast degradation.
3, the present invention is applied to the degradation of organic dye waste water using nonmetallic modifying carbon materials as anode material, due to
The leaching phenomenon of non-metallic ion, avoids the possibility that secondary pollution is caused to environment.
Detailed description of the invention
Fig. 1 is the XPS score (a) and N1s high-resolution XPS spectrum figure (b) of N doping carbon materials prepared by embodiment 1, can be with
Find out 700 DEG C heat treatment after nitrogen doping be 5.73%, wherein the ratio of pyrroles's nitrogen and pyridine nitrogen be 85:15；
Fig. 2 is the XPS score (a) and N1s high-resolution XPS spectrum figure (b) of N doping carbon materials prepared by embodiment 2, can be with
Find out 300 DEG C heat treatment after nitrogen doping be 10.1%, wherein the ratio of pyrroles's nitrogen and pyridine nitrogen be 68:32；
Fig. 3 is the XPS score (a) and N1s high-resolution XPS spectrum figure (b) of N doping carbon materials prepared by embodiment 3, can be with
Find out 900 DEG C heat treatment after nitrogen doping be 3.36%, wherein the ratio of pyrroles's nitrogen and pyridine nitrogen be 87:13；
Fig. 4 be embodiment 1 prepare N doping carbon materials anode during catalytic air oxidation rhodamine B degradation solution
UV-visible spectrum, it can be seen that the characteristic absorption peak of rhodamine B completely disappears in 2h；
Fig. 5 is that the N doping carbon materials anode of embodiment 1-4 preparation drops during catalytic air oxidation degrades organic contamination
The graph of relation of solution rate and time, it can be seen that removal rate of several dyestuffs in 2h has reached 100%.
Specific embodiment
Embodiments of the present invention are described in detail below in conjunction with portion of techniques scheme:
Embodiment 1:
2.0g disodium EDTA is added in 30mL deionized water, dissolution is transferred to after forming clear solution
In 50mL hydrothermal reaction kettle, then by 0.4g through hydrogen peroxide treated carbon felt submergence in the solution, react at 160 DEG C
14h；Carbon felt is taken out after cooling, respectively with alternately washing three times of deionized water and dehydrated alcohol, the dry 12h in 80 DEG C of baking ovens；
The carbon felt after drying is put into tube furnace again, the lower 700 DEG C of heat treatment 1h of nitrogen protection obtains nitrogen-doped carbon felt material.
In single chamber three-electrode system, under normal temperature and pressure, using the nitrogen-doped carbon felt material of preparation as anode, platinum filament is pair
Electrode, calomel electrode is reference electrode, with 0.05molL-1Na2SO4For electrolyte, pH 7.0,30mLs-1Flow velocity from
Reactor bottom blasts air, and catalytic air oxidation 130mL concentration is 25mgL under 1.0V external voltage-1Rhodamine B, in 2h
The degradation rate of rhodamine B reaches 100%.
Embodiment 2:
5.0g disodium EDTA is added in 30mL deionized water, dissolution is transferred to after forming clear solution
In 50mL hydrothermal reaction kettle, then by 0.4g through hydrogen peroxide treated carbon felt submergence in the solution, react at 200 DEG C
8h；Carbon felt is taken out after cooling, respectively with alternately washing three times of deionized water and dehydrated alcohol, the dry 12h in 80 DEG C of baking ovens；Again
Carbon felt after drying is put into tube furnace, the lower 300 DEG C of heat treatment 5h of nitrogen protection obtains nitrogen-doped carbon felt material.
In single chamber three-electrode system, under normal temperature and pressure, using the nitrogen-doped carbon felt material of preparation as anode, platinum filament is pair
Electrode, calomel electrode is reference electrode, with 0.05molL-1Na2SO4For electrolyte, pH 3.0,30mLs-1Flow velocity from
Reactor bottom blasts air, and catalytic air oxidation 130mL concentration is 25mgL under 1.0V external voltage-1Rhodamine B, in 2h
The degradation rate of rhodamine B reaches 100%.
Embodiment 3:
1.0g disodium EDTA is added in 30mL deionized water, dissolution is transferred to after forming clear solution
In 50mL hydrothermal reaction kettle, then by 0.4g through hydrogen peroxide treated carbon fiber submergence in the solution, react at 120 DEG C
24h；Carbon fiber is taken out after cooling, it is dry in 80 DEG C of baking ovens respectively with alternately washing three times of deionized water and dehydrated alcohol
12h；The carbon felt after drying is put into tube furnace again, the lower 900 DEG C of heat treatment 1h of nitrogen protection obtains nitrogen-doped carbon undulation degree
Material.
In single chamber three-electrode system, under normal temperature and pressure, using the nitrogen-doped carbon fibrous material of preparation as anode, platinum filament is
To electrode, calomel electrode is reference electrode, with 0.05molL-1Na2SO4For electrolyte, pH 5.0,30mLs-1Flow velocity
Air is blasted from reactor bottom, catalytic air oxidation 130mL concentration is 25mgL under 1.0V external voltage-1Crystal violet, in 2h
The degradation rate of crystal violet reaches 100%.
Embodiment 4:
4.0g disodium EDTA is added in 30mL deionized water, dissolution is transferred to after forming clear solution
In 50mL hydrothermal reaction kettle, then by 0.4g through hydrogen peroxide treated carbon cloth submergence in the solution, react at 140 DEG C
16h；Carbon cloth is taken out after cooling, respectively with alternately washing three times of deionized water and dehydrated alcohol, the dry 12h in 80 DEG C of baking ovens；
The carbon cloth after drying is put into tube furnace again, the lower 700 DEG C of heat treatment 2h of nitrogen protection obtains nitrogen-doped carbon cloth material.
In single chamber three-electrode system, under normal temperature and pressure, using the nitrogen-doped carbon cloth material of preparation as anode, platinum filament conduct
To electrode, calomel electrode is as reference electrode, with 0.05molL-1Na2SO4For electrolyte, 30mLs-1Flow velocity from reaction
Device bottom blasts air, and catalytic air oxidation 130mL concentration is 25mgL under 1.0V external voltage-1Neutral fuchsin, it is neutral in 2h
Pinkish red degradation rate reaches 100%.
Embodiment 5:
3.0g disodium EDTA is added in 30mL deionized water, dissolution is transferred to after forming clear solution
In 50mL hydrothermal reaction kettle, then by 0.4g through hydrogen peroxide treated foamy carbon submergence in the solution, react at 160 DEG C
12h；Foamy carbon is taken out after cooling, it is dry in 80 DEG C of baking ovens respectively with alternately washing three times of deionized water and dehydrated alcohol
12h；The foamy carbon after drying is put into tube furnace again, the lower 700 DEG C of heat treatment 1h of nitrogen protection obtains N doping foam carbon materials
Material.
In single chamber three-electrode system, under normal temperature and pressure, using the N doping foamed carbon material of preparation as anode, platinum filament is made
For to electrode, calomel electrode is as reference electrode, with 0.05molL-1Na2SO4For electrolyte, 30mLs-1Flow velocity from anti-
Device bottom is answered to blast air, catalytic air oxidation 130mL concentration is 50mgL under 1.0V external voltage-1Methylene blue, it is sub- in 2h
The degradation rate of methyl blue reaches 100%.
Claims (10)
1. a kind of preparation of N doping carbon materials anode, it is characterised in that:
Using common three-dimensional carbon materials as substrate, disodium EDTA is nitrogen source, carries out hydro-thermal N doping at a certain temperature
Reaction；Carbon materials are taken out after cooling and cleaned, dried and be placed in tube furnace, are heat-treated in nitrogen atmosphere, obtain N doping
Carbon materials material.
2. the preparation of N doping carbon materials anode according to claim 1, it is characterised in that:
The three-dimensional carbon materials are selected from carbon fiber, carbon felt, foamy carbon or carbon cloth；The three-dimensional carbon materials are using preceding first clear with acetone
It washes, then passes through 1%H2O2Aqueous solution is in 120 DEG C of hydro-thermal process 12h.
3. the preparation of N doping carbon materials anode according to claim 1, it is characterised in that:
The addition quality of the nitrogen source is 2.5-12.5 times of carbon materials quality.
4. the preparation of N doping carbon materials anode according to claim 1, it is characterised in that:
The reaction temperature of hydro-thermal N doping reaction is 120~200 DEG C, the reaction time is 8~for 24 hours.
5. the preparation of N doping carbon materials anode according to claim 1, it is characterised in that:
The heat treatment temperature is 300~900 DEG C, and heat treatment time is 1~5h.
6. the application for the N doping carbon materials anode that any preparation method is prepared in claim 1-5, it is characterised in that:
It is to be reacted using the N doping carbon materials as catalyst wet air oxidation, under applied voltage driving in room temperature
The degradation of organic dyestuff is realized under normal pressure.
7. application according to claim 6, it is characterised in that:
In single chamber three-electrode system, under normal temperature and pressure, using the N doping carbon materials of preparation as the anode of battery, platinum filament is to electricity
Pole, calomel electrode are reference electrode, under 1.0V voltage, 0.05molL-1 Na2SO4For electrolyte, under certain pH conditions, catalysis
Air oxidation waste water from dyestuff.
8. application according to claim 7, it is characterised in that:
The organic dyestuff is one of neutral fuchsin, methylene blue, crystal violet, rhodamine B, and concentration is 0~50mgL-1。
9. application according to claim 7, it is characterised in that:
The pH value is 3-9.
10. application according to claim 7, it is characterised in that:
The pH value is preferably 3-7.
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Cited By (3)
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| CN113322668A (en) * | 2021-04-21 | 2021-08-31 | 北京化工大学 | Preparation method and application of carbon nitride-loaded mesophase pitch-based carbon fiber |
| CN114392747A (en) * | 2022-01-20 | 2022-04-26 | 合肥工业大学 | Preparation method and application of nickel-doped sludge substrate block electrode anode |
| CN115467159A (en) * | 2022-09-06 | 2022-12-13 | 昆明云大新能源有限公司 | In-situ etching nitrogen-doped modified carbon cloth and preparation method and application thereof |
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Cited By (5)
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