CN109985656A - A kind of synthetic method and application of the carbon nitride catalyst rich in defect - Google Patents
A kind of synthetic method and application of the carbon nitride catalyst rich in defect Download PDFInfo
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- CN109985656A CN109985656A CN201910349264.0A CN201910349264A CN109985656A CN 109985656 A CN109985656 A CN 109985656A CN 201910349264 A CN201910349264 A CN 201910349264A CN 109985656 A CN109985656 A CN 109985656A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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Abstract
The invention discloses a kind of synthetic methods of carbon nitride catalyst rich in defect and its carbon nitride catalyst obtained rich in defect, and the application in Advanced Oxidation Process Treating Organic Wastewater is being activated by persulfate.The synthetic method are as follows: use g-C3N4For precursor, by g-C3N4It is mixed in proportion with magnesium powder, and after grinding uniformly, obtains g-C after calcining in argon atmosphere3NxActive material, to get the carbon nitride catalyst for being rich in defect after pickling, drying.The present invention uses the carbon nitride catalyst rich in defect prepared using urea as raw material, and catalytic degradation performance is better than most metallic catalysts, while having prevented the inevitable digestion of metallic ion of metallic catalyst, green non-pollution.
Description
Technical field
The present invention relates to the synthetic methods and application of a kind of carbon nitride catalyst rich in defect, and in particular to a kind of with useless
The synthetic method for abandoning the non-metal carbon catalyst that diaper is raw material belongs to non-metal carbon catalyst preparation and application technology neck
Domain.
Background technique
In recent years, the advanced oxidation technology based on potentiometric titrations is due in degrading pesticide, perfluorocarboxylic acid and medicine
Advantage outstanding, which is shown, on the emerging pollutant such as object and personal-care supplies (PPCP) has drawn grinding for more and more scientific research personnel
Study carefully interest.Potentiometric titrations have high oxidation-reduction potential (2.5-3.1V), and can be reacted with most of organic matters with
The speed of nearly diffusion speed control sends out oxidation reaction.Meanwhile persulfate is mostly solid-state, easily stored and transport, in the environment
It is relatively stable, it is water-soluble preferable, therefore in practical applications, there is apparent advantage relative to other oxidants.It is single
Persulfuric acid peroxydisulfate etc. is usually used in generating potentiometric titrations.Due to the remarkable advantage of persulfate, in underground water and soil
The in-situ chemical reparation of earth and removal hardly degraded organic substance using upper, the novel activated high-level oxidation technology of persulfate is by more
Multiple view has obtained extensive concern and application as a kind of efficient treatment process to this problem.
Currently, the catalyst that persulfate advanced oxidation technology uses is divided into two major classes: one kind is traditional metal
Oxide (Fe3O4、CuO、Co3O4、MnO2) catalyst, another kind of is with carbon nanotube, carbon fiber, fullerene, graphene oxide
For the new carbon of representative.Research shows that new carbon is controlled because of its unique structure and chemical characteristic in environmental contaminants
Reason field illustrates good performance.It is also more and more to the environmental applications research of graphene and class grapheme material in recent years,
Such as: have studied the effect of graphene oxide composite material photocatalytic degradation of organic matter；Use modified graphene oxide as suction
It attached dose, is also repeatedly reported for the removal of environmental contaminants and the enrichment analysis of contaminant trace species.Graphene oxide is excellent
The defect sturcture at electron transmission ability, functional group abundant and surface and edge makes it in photocatalysis, chemical catalytic oxidation
Have a extensive future.And doping and metal oxide by being chemically modified to it, such as nonmetalloid nitrogen phosphate and sulfur
Forming composite material is even more the application for having widened the material.After N doping graphene oxide, live to the adsorption capacity and its of BPA
The reaction rate constant for changing persulfate degradation BPA improves a lot compared with common graphene oxide, and degradation efficiency significantly mentions
It is high.But grapheme material brings the raising of production cost that solution is not yet received due to its cumbersome preparation process, it is difficult in environment
Aspect is administered to be widely applied.
Summary of the invention
The technical problems to be solved by the present invention are: being currently used for the preparation process of the grapheme material of processing organic wastewater
It is cumbersome, the technical issues of high production cost.
To solve the above-mentioned problems, the present invention provides a kind of synthetic method of carbon nitride catalyst rich in defect,
It is characterized in that, using g-C3N4For precursor, by g-C3N4It mixes with magnesium powder, and after grinding uniformly, is forged in argon atmosphere in proportion
G-C is obtained after burning3NxActive material, to get the carbon nitride catalyst for being rich in defect after pickling, drying.
Preferably, the g-C3N4It is made by Material synthesis of urea.
Preferably, the g-C3N4Mass ratio with magnesium powder is (1~5): 1.
Preferably, the temperature of the calcining is 550 DEG C~900 DEG C, and calcination time is 1~5h.
Preferably, the pickling specifically: using mass concentration 10% spirit of vinegar pickling twice, precipitating is collected by centrifugation
Object, then twice with deionized water washing, sediment is collected by centrifugation.
Preferably, the drying condition are as follows: 60 DEG C of vacuum drying.
The present invention also provides the nitrogen that defect is rich in made from the synthetic method of the above-mentioned carbon nitride catalyst rich in defect
Change C catalyst and activates the application in Advanced Oxidation Process Treating Organic Wastewater by persulfate.
Preferably, when handling organic wastewater, the pH value for first adjusting organic wastewater is 7, then, sequentially adds described be rich in
The carbon nitride catalyst and persulfate of defect, concussion reaction realize the degradation treatment to organic wastewater.
Preferably, the target organic pollutant in the organic wastewater is for rhodamine B, carbamazepine and to o-phenyl phenol
At least one of.
It is highly preferred that the concentration of the target organic pollutant in the organic wastewater is 10-50mg/L, the nitrogen rich in defect
The additional amount for changing C catalyst is 0.1-0.5g/L organic wastewater, and the additional amount of persulfate is 0.5-2.0mmol/L organic waste
Water.
It is highly preferred that the persulfate is ammonium persulfate-sodium bisulfate.
It is highly preferred that the condition of the concussion reaction are as follows: 25 DEG C of temperature, reaction time 30min.
For the present invention using carbonitride as catalyst, persulfate is oxidant, and activation persulfate forms it into high activity
Oxygenated species reach purpose of purifying the water quality to further aoxidize the biodegradable organic pollutant of water body Poisoning disaster.
For the non-metal carbon catalyst that the present invention synthesizes when handling organic wastewater, utilization is non-free-radical oxidation principle,
Its main active substances singlet oxygen (1O2) more other radical type oxidation activity species (O2 -·、OH·、SO4 2-) compare
There is the longest time-to-live (10 in aqueous solution-6~10-3Second), overcome that free radical is easily quenched in practical water body lacks
Point, the interference that can effectively resist background organic matter and inorganic matter in water efficiently aoxidizes and mineralising organic pollutant.With classics
Free-radical oxidation system compare,1O2The oxidation system of mediation has prominent in the recovery technique of the practical water body object of organic pollution
Advantage out.
Compared with prior art, the invention has the following advantages:
(1) grapheme material preparation complexity had both been overcome by the high nitrogen defect carbon nitride material of the hot denitrogenation technology synthesis of magnesium
The high cost problem of bring, and the low problem of carbonitride poorly conductive catalytic efficiency is overcome, have in activation persulfate degradation
Excellent performance is shown in machine pollution objects system, and preparation process is simple and easy and green non-pollution；
(2) material is using cheap urea as raw material, and gained catalyst is non-metallic catalyst after the hot denitrification process of magnesium
Green non-pollution and, great practical value and economic benefit.
(3) what is used during organic matter degradation is the mechanism of non-free-radical oxidation, and degradation effect is not vulnerable to background
The interference of other anion in pollutant and water, compared with traditional free-radical oxidation system,1O2The oxidation system of mediation is having
The recovery technique of the practical water body object of machine object pollution has advantage outstanding；
(4) catalyst is applied to activate high-level oxidation technology based on persulfate, to rhodamine B, carbamazepine, adjacent benzene
Base phenol has good degradation effect, especially has good remineralization efficacy to o-phenyl phenol waste water, and effluent quality clarification is saturating
It is bright.
Detailed description of the invention
Fig. 1 is the scanning electron microscope image of carbon nitride catalyst made from embodiment 1；
Fig. 2 is the images of transmissive electron microscope of carbon nitride catalyst made from embodiment 1；
Fig. 3 is in embodiment 2-4 respectively to the rhodamine B (RhB) of 20ppm concentration, carbamazepine (CBZ), 2- phenyl benzene
The degradation curve figure of phenol (OPP)；
Fig. 4 is comparative example 1-2, in embodiment 5 respectively to the degradation curve figure of carbamazepine.
Specific embodiment
In order to make the present invention more obvious and understandable, hereby with preferred embodiment, and attached drawing is cooperated to be described in detail below.
Embodiment 1
After using urea as Material synthesis carbonitride, done in conjunction with the hot denitrogenation technology of magnesium to denitrogenation, pickling is carried out at 750 DEG C
It is dry, obtain active material g-C3Nx, as carbon nitride catalyst.
Fig. 1 and Fig. 2 respectively illustrates active material g-C made from embodiment 13NxScanning electron microscope image and projection Electronic Speculum
Image.As can be seen from the figure the g-C after magnesium thermit3NxIt remains by laminar nanometer flower structure, and more loose
It is porous.
Embodiment 2
It takes waste water standard solution of the configured 20mg/L of 10mL containing RhB in conical flask, 90mL buffer solution is added, adjust
PH=7 is saved, g-C obtained by embodiment 1 is sequentially added3Nx0.2g/L, Oxone 2mmol/L are placed in constant temperature water bath concussion case
Carry out 30min reaction, by 0,5,10,15,20,25, after the timing node sampling of 30min, sample uses high performance liquid chromatography immediately
Carry out concentration analysis.30min dyestuff is completely degraded solution clear, colorless.
Embodiment 3
It takes waste water standard solution of the configured 20mg/L of 10mL containing carbamazepine in conical flask, it is molten that 90mL buffering is added
Liquid adjusts pH=7, according to sequentially adding g-C obtained by embodiment 13Nx0.2g/L, Oxone 2mmol/L, are placed in constant temperature water bath
Shake and carry out 30min reaction in case, by 0,5,10,15,20,25, after the timing node sampling of 30min, sample is used efficiently immediately
Liquid chromatogram carries out concentration analysis.30min carbamazepine is degraded 90% or more.
Embodiment 4
It takes waste water standard solution of the configured 20mg/L of 10mL containing p-phenyl phenol in conical flask, 90mL buffering is added
Solution adjusts pH=7, sequentially adds g-C obtained by embodiment 13Nx0.2g/L, Oxone 2mmol/L, are placed in constant temperature water bath
Shake and carry out 30min reaction in case, by 0,5,10,15,20,25, after the timing node sampling of 30min, sample is used efficiently immediately
Liquid chromatogram carries out concentration analysis.P-phenyl phenol is completely degraded after 30min.
The data result of embodiment 2-4 is as shown in Figure 3.
Comparative example 1
It takes pharmaceutical waste water standard solution of the configured 20mg/L of 10mL containing carbamazepine in conical flask, 90mL is added
Buffer solution adjusts pH=7, g-C is only added3N4Be placed in constant temperature water bath concussion case and carry out 30min reaction, by 0,5,10,15,
20,25, after the timing node sampling of 30min, sample carries out concentration analysis with high performance liquid chromatography immediately.To phenyl after 30min
Phenol is not degraded substantially.
Comparative example 2
It takes pharmaceutical waste water standard solution of the configured 20mg/L of 10mL containing carbamazepine in conical flask, 90mL is added
Buffer solution, adjusts pH=7, an Oxone 2mmol/L is only added is placed in constant temperature water bath concussion case and carry out 30min reaction, by 0,
5,10,15,20,25, after the timing node sampling of 30min, sample carries out concentration analysis with high performance liquid chromatography immediately.30min
P-phenyl phenol is not degraded substantially afterwards.
Comparative example 5
It takes pharmaceutical waste water standard solution of the configured 20mg/L of 10mL containing carbamazepine in conical flask, 90mL is added
Buffer solution adjusts pH=7, successively plus obtained g-C3N40.2g/L, Oxone 2mmol/L are placed in constant temperature water bath concussion
30min reaction is carried out in case, by 0,5,10,15,20,25, after the timing node sampling of 30min, sample uses efficient liquid phase immediately
Chromatography carries out concentration analysis.P-phenyl phenol is not degraded substantially after 30min.
Comparative example 1-2, the data result of embodiment 5 are as shown in Figure 4.
Claims (10)
1. a kind of synthetic method of the carbon nitride catalyst rich in defect, which is characterized in that use g-C3N4For precursor, by g-C3N4
It is mixed in proportion with magnesium powder, and after grinding uniformly, obtains g-C after calcining in argon atmosphere3NxActive material, pickling, drying
Afterwards to get the carbon nitride catalyst for being rich in defect.
2. the synthetic method of the carbon nitride catalyst rich in defect as described in claim 1, which is characterized in that the g-C3N4
It is made by Material synthesis of urea.
3. the synthetic method of the carbon nitride catalyst rich in defect as described in claim 1, which is characterized in that the g-C3N4
Mass ratio with magnesium powder is (1~5): 1.
4. the synthetic method of the carbon nitride catalyst rich in defect as described in claim 1, which is characterized in that the calcining
Temperature is 550 DEG C~900 DEG C, and calcination time is 1~5h.
5. the synthetic method of the carbon nitride catalyst rich in defect as described in claim 1, which is characterized in that the pickling tool
Body are as follows: using mass concentration 10% spirit of vinegar pickling twice, be collected by centrifugation sediment, then twice with deionized water washing, from
The heart collects sediment.
6. the synthetic method of the carbon nitride catalyst rich in defect as described in claim 1, which is characterized in that the dried strip
Part are as follows: 60 DEG C of vacuum drying.
7. the synthetic method of the carbon nitride catalyst as claimed in any one of claims 1 to 6 rich in defect is obtained to be rich in defect
Carbon nitride catalyst passing through persulfate activate Advanced Oxidation Process Treating Organic Wastewater in application.
8. the use as claimed in claim 7, which is characterized in that when handling organic wastewater, first adjust the pH value of organic wastewater
It is 7, then, sequentially adds the carbon nitride catalyst and persulfate for being rich in defect, concussion reaction is realized to organic waste
The degradation treatment of water.
9. application as claimed in claim 7 or 8, which is characterized in that the target organic pollutant in the organic wastewater is sieve
Red bright B, carbamazepine and at least one of o-phenyl phenol；Persulfate is ammonium persulfate-sodium bisulfate.
10. application as claimed in claim 8, which is characterized in that the concentration of the target organic pollutant in the organic wastewater
For 10-50mg/L, the additional amount of the carbon nitride catalyst rich in defect is 0.1-0.5g/L organic wastewater, the addition of persulfate
Amount is 0.5-2.0mmol/L organic wastewater；The condition of concussion reaction are as follows: 25 DEG C of temperature, reaction time 30min.
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| CN110311119A (en) * | 2019-07-10 | 2019-10-08 | 陕西科技大学 | A kind of preparation method of lithium ion battery negative material SnS/ND-CN |
| CN111185220A (en) * | 2020-03-20 | 2020-05-22 | 中国科学院长春应用化学研究所 | Carbon nitride supported Pd-based catalyst, and preparation method and application thereof |
| CN113617375A (en) * | 2021-08-09 | 2021-11-09 | 东莞理工学院 | Graphite phase carbon nitride photocatalytic material and preparation method thereof |
| CN113617350A (en) * | 2021-08-11 | 2021-11-09 | 北京林业大学 | Defective carbon material and preparation method and application thereof |
| CN113929197A (en) * | 2021-09-23 | 2022-01-14 | 重庆大学 | Method for treating organic wastewater by activating peroxymonosulfate under assistance of visible light |
| CN113964325A (en) * | 2021-12-20 | 2022-01-21 | 北京航空航天大学 | Nitrogen-deficient g-C3N4Loaded with Mg3N2Application of composite material as negative electrode material and lithium-based battery |
| CN115337952A (en) * | 2022-09-16 | 2022-11-15 | 东莞理工学院 | Method for synthesizing ferro-manganese bimetallic oxide loaded nitrogen vacancy-containing carbon nitride in one step |
| CN115845902A (en) * | 2022-12-08 | 2023-03-28 | 上海交通大学深圳研究院 | Graphite phase carbon nitride photocatalytic material and preparation method thereof |
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Cited By (11)
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|---|---|---|---|---|
| CN110311119A (en) * | 2019-07-10 | 2019-10-08 | 陕西科技大学 | A kind of preparation method of lithium ion battery negative material SnS/ND-CN |
| CN111185220A (en) * | 2020-03-20 | 2020-05-22 | 中国科学院长春应用化学研究所 | Carbon nitride supported Pd-based catalyst, and preparation method and application thereof |
| CN113617375A (en) * | 2021-08-09 | 2021-11-09 | 东莞理工学院 | Graphite phase carbon nitride photocatalytic material and preparation method thereof |
| CN113617375B (en) * | 2021-08-09 | 2023-06-30 | 东莞理工学院 | Graphite-phase carbon nitride photocatalytic material and preparation method thereof |
| CN113617350A (en) * | 2021-08-11 | 2021-11-09 | 北京林业大学 | Defective carbon material and preparation method and application thereof |
| CN113929197A (en) * | 2021-09-23 | 2022-01-14 | 重庆大学 | Method for treating organic wastewater by activating peroxymonosulfate under assistance of visible light |
| CN113964325A (en) * | 2021-12-20 | 2022-01-21 | 北京航空航天大学 | Nitrogen-deficient g-C3N4Loaded with Mg3N2Application of composite material as negative electrode material and lithium-based battery |
| CN113964325B (en) * | 2021-12-20 | 2022-03-18 | 北京航空航天大学 | Nitrogen-deficient g-C3N4Loaded with Mg3N2Application of composite material as negative electrode material and lithium-based battery |
| CN115337952A (en) * | 2022-09-16 | 2022-11-15 | 东莞理工学院 | Method for synthesizing ferro-manganese bimetallic oxide loaded nitrogen vacancy-containing carbon nitride in one step |
| CN115845902A (en) * | 2022-12-08 | 2023-03-28 | 上海交通大学深圳研究院 | Graphite phase carbon nitride photocatalytic material and preparation method thereof |
| CN115845902B (en) * | 2022-12-08 | 2024-04-19 | 上海交通大学深圳研究院 | Graphite-phase carbon nitride photocatalytic material and preparation method thereof |
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