CN109967111A - Activate the preparation method and applications of the nitrogen sulphur codope graphene of persulfate - Google Patents
Activate the preparation method and applications of the nitrogen sulphur codope graphene of persulfate Download PDFInfo
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- CN109967111A CN109967111A CN201910064100.3A CN201910064100A CN109967111A CN 109967111 A CN109967111 A CN 109967111A CN 201910064100 A CN201910064100 A CN 201910064100A CN 109967111 A CN109967111 A CN 109967111A
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- Prior art keywords
- graphene
- nitrogen sulphur
- sulphur codope
- preparation
- persulfate
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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
-
- 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
-
- 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
-
- 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
Abstract
The present invention provides the preparation and its application of the nitrogen sulphur codope graphene of activation persulfate comprising following steps: S1, raw material choose commercial graphene, thiocarbamide, ultrapure water, ethyl alcohol；Commercial graphene is uniformly mixed by S2, mixing with thiocarbamide；S3, calcining, commercial graphene and thiocarbamide that S2 step is uniformly mixed are placed in tube furnace under nitrogen atmosphere, temperature control is calcined at 350-800 DEG C, and heating rate control is in 8-12 DEG C/min, constant temperature 40-80min, and it is cooled to room temperature S4, washing under nitrogen atmosphere, the resulting sample of S3 step is washed with ultrapure water, ethyl alcohol respectively；The resulting sample of S4 step is placed under vacuum environment dry 20-28h, obtains nitrogen sulphur codope graphene and the application of the nitrogen sulphur codope graphene being prepared in water process by S5, drying.
Description
Technical field
The present invention relates to field of graphene, and in particular to the preparation side of the nitrogen sulphur codope graphene of activation persulfate
Method and its application.
Background technique
Traditional water process skill is difficult to effectively remove emerging pollutant in water, and high-level oxidation technology is for these organic dirts
The removal of dye object has the characteristics that efficient, thorough and economical, is therefore widely used in water treatment field.In recent years, it was based on
The high-level oxidation technology of sulfate activation, is concerned because of its Strong oxdiative ability and degradation efficiency.Nano-sized carbon (such as carbon nanotube
(CNT), graphene oxide (GO)) substitution metal-based catalyst is already functioned as persulfate activation, and Heteroatom doping can
To further increase its catalytic activity.Oxidation process based on Heteroatom doping carbon material does not need energy supply, and can be with
Avoid the potential secondary pollution of metallic catalyst.Therefore, Heteroatom doping carbon material is promising material.The report of early period
Mostly based on graphene oxide, the grapheme material of Heteroatom doping is prepared.There has been no with graphene (reduction-oxidation graphite
Alkene) it is that the nitrogen sulphur codope graphene of raw material preparation activates the document and patent report of persulfate oxidation removal water pollutant
Road.
Summary of the invention
(1) technical problems to be solved
In view of the foregoing, it is an object to provide being used to prepare efficient for the novel pollution of activation persulfate degradation
The method of the nitrogen sulphur codope graphene of object, utilizes above-mentioned nitrogen sulphur codope graphene
Adjustment nitrogen sulphur codope graphene preparation process has it, and increases the graphene answering in terms of water process
With.
(2) technical solution
To solve the technical problem, a purpose of the invention is to provide the system of the nitrogen sulphur codope graphene of activation persulfate
Preparation Method comprising following steps:
S1, raw material choose commercial graphene, thiocarbamide, ultrapure water, ethyl alcohol；
Commercial graphene is uniformly mixed by S2, mixing with thiocarbamide；
Commercial graphene and thiocarbamide that S2 step is uniformly mixed are placed in tube furnace, temperature control by S3, calcining under nitrogen atmosphere
System is calcined at 350-800 DEG C, and heating rate is controlled in 8-12 DEG C/min, constant temperature 40-80min, and under nitrogen atmosphere
It is cooled to room temperature；
S4, washing wash the resulting sample of S3 step with ultrapure water, ethyl alcohol respectively；
The resulting sample of S4 step is placed under vacuum environment dry 20-28h, obtains nitrogen sulphur codope graphene by S5, drying.
The technical program preferably, commercial graphene: the mass ratio of thiocarbamide=(1:1).
Preferably, the commercialization graphene is reduction-oxidation method preparation method, SSA > 500m to the technical program2/g。
Preferably, temperature control is at 350 DEG C, 400 DEG C, 600 DEG C, 700 DEG C, 800 DEG C in S3 step for the technical program.
The technical program preferably, 10 DEG C/min of heating rate, constant temperature 60min in S3 step.
Preferably, sample obtained in S4 step first uses milli-Q water at least three times to the technical program, then uses second
Alcohol washs at least three times.
Preferably, drying time is for 24 hours to the technical program in S5 step.
Another object of the present invention provides the application of the nitrogen sulphur codope graphene of above-mentioned activation persulfate and its answers
Use method.
Application of the nitrogen sulphur codope graphene of the activation persulfate of above-mentioned preparation in removal water pollutant.
The nitrogen sulphur codope graphene of the activation persulfate of above-mentioned preparation preservative methylparaben in going water removal
(MP), the application in sun-screening agent UVINUL MS 40 (BP-4) and phenol.
Application method of the nitrogen sulphur codope graphene of the activation persulfate of above-mentioned preparation in water process, including it is following
Step takes the nitrogen sulphur codope graphene of a certain amount of activation persulfate prepared to be added in sewage to be processed, is being added
A certain amount of potassium hydrogen persulfate, stirring/oscillation under room temperature.
(3) beneficial effect
In nitrogen sulphur codope graphene (IrGO-NS) preparation method of activation persulfate provided by the invention, using industrial stone
Black alkene is prepared for IrGO-NS material by subsequent heat treatment, and repeatedly wash using ultrapure water and ethyl alcohol and to remove impurity and residual
Slag is more suitable industrialization large-scale production relative to pervious experiment preparation method and passes through above-mentioned preparation method at the same time
It obtains IrGO-NS and has biggish specific surface area.
And the IrGO-NS that preparation method provided by the invention obtains also is applied in water process, can remove sewage
In pollutant, particularly with the emerging pollutants such as preservative methylparaben, sun-screening agent BP-4 and Conventional pollution phenol
Removal has efficient effect, and it is nano-carbon material environmental protection that this, which is prepared IrGO-NS, is made in removal process without metal leaching
At secondary pollution, IrGO-NS is used cooperatively as catalyst in water treatment procedure, with potassium hydrogen persulfate (PMS) as oxidant,
Dosage is relatively fewer, is effectively reduced the cost of removal water pollutant.
Detailed description of the invention
Fig. 1 is the XRD diffraction spectrogram of the nitrogen sulphur codope commercial graphites alkene of preparation method provided by the invention preparation；
Fig. 2 is the Raman spectrogram of prepared nitrogen sulphur codope commercial graphites alkene；
Fig. 3 is that the SEM and TEM of prepared nitrogen sulphur codope commercial graphites alkene scheme；
Fig. 4 is that the BET of prepared nitrogen sulphur codope commercial graphites alkene schemes；
Fig. 5 is that the XPS of prepared nitrogen sulphur codope commercial graphites alkene schemes；
Fig. 6 is prepared nitrogen sulphur codope commercial graphites alkene to preservative methylparaben (MP) removal effect figure；
Fig. 7 is TOC removal effect figure of the prepared nitrogen sulphur codope commercial graphites alkene to preservative methylparaben (MP)；
Fig. 8 is prepared nitrogen sulphur codope commercial graphites alkene to sun-screening agent BP-4 and phenol removal effect figure.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below
Example is not intended to limit the scope of the invention for illustrating the present invention.
It takes a certain amount of commercial graphene (IrGO) and thiocarbamide after mixing, is put into and has led to nitrogen (N2) 30min tube furnace
(350 DEG C, 400 DEG C, 600 DEG C, the 700 DEG C, 800 DEG C) calcinings at different temperatures of middle difference.Calcination time is under different time
(40min, 50min, 60min, 70min, 80min), heating rate are then selected as under 8,10,12 DEG C/min and carry out test of many times.
After being cooled to room temperature under nitrogen atmosphere, gained sample first with milli-Q water three times, then three times with ethanol washing.Vacuum drying
Temperature be 60 DEG C, drying time 12h, after obtain IrGO-NS.
Embodiment 1
It takes a certain amount of commercial graphene (IrGO) and thiocarbamide after mixing, is put into and has led to nitrogen (N2) 350 in 30min tube furnace
DEG C calcining.Calcination time 60min under different time, heating rate, which is then selected as under 10 DEG C/min, carries out test of many times.In nitrogen
After atmosphere is cooled to room temperature under enclosing, gained sample first with milli-Q water three times, then three times with ethanol washing.Vacuum drying temperature
Be 60 DEG C, drying time 12h, after obtain test specimen IrGO-NS.
Use Quanta400FEG scanning electron microscope (SEM) (FEI, USA) and JEM- respectively for test specimen
The morphological analysis of 2100F high resolution transmission electron microscope (HRTEM) (Japanese JEOL) progress sample.It uses
ESCALAB250XIX X-ray photoelectron spectroscopy X (XPS) system (ThermoFisherScientific, USA) analyzes surface-element
Composition.Use TriStarII3020 surface area and Porosimetry (Micromeritics, USA) measurement N2 adsorption-desorption etc.
Warm line, specific surface area (BET) and pore-size distribution.It is observed on LabRAMHREvolution spectrometer (HORIBAJY, France)
Raman spectrum.X-ray diffraction (XRD) spectrum is recorded with D8-X x ray diffractometer x (Bruker, Germany).
Wherein Fig. 1 is the XRD diffraction spectrogram of the nitrogen sulphur codope commercial graphites alkene of preparation method provided by the invention preparation,
Graphene IrGO can be compared by Fig. 1, N doping commercial graphites alkene IrGO-N, nitrogen sulphur codope commercial graphites alkene IrGO-NS, returned
Nitrogen sulphur codope commercial graphites alkene IrGO-NS-recycled comparative situation is received, it can be seen that 26 ° of spy in all samples
Peak is levied, and does not find the obvious offset of these diffraction maximums, it means that doping process is without obviously destroying graphite crystal knot
Structure.
Fig. 2 can be seen that IrGO-NS has relatively low intensity ratio (ID/IG), quality with higher.
Fig. 3 can be seen that in SEM electron microscope the folding it can be observed that two graphene samples (A IrGO, B IrGO-NS)
Wrinkle and stack layer form.The sheet form of wrinkle is further disclosed by TEM.
BET figure shown in Fig. 4 is it is found that the V-type thermoisopleth of two kinds of grapheme materials shows that there are mesoporous.IrGO and IrGO-
The specific surface area of NS distinguishes 647 and 576 m2g-1, this shows that IrGO-NS has biggish specific surface area.
XPS analysis shown in fig. 5 is the results show that the nitrogen content of codope sample (IrGO-NS) is 3.31 at.%, mainly
N containing pyridine, pyrroles N and graphite N；S group in IrGO-NS becomes 1.10 at.%, predominantly thiophenic sulfur.
Embodiment 2
The test specimen being prepared in Example 1 carries out degradation preservative methylparaben (MP) experiment.In 15 mg/L
In MP solution, 20 mg/L IrGO-NS and 307 mg/L PMS are added, at regular intervals, sampling is filtered to remove IrGO-NS,
Methanol is added and terminates reaction, using HPLC analysis reaction solution MP concentration variation.
As a comparison, being separately added into conventional GO and its N doped samples or classical metallic catalyst (nano Co3O4And Fe3O4)
As catalyst, other conditions are same as above.
It is individually added into IrGO-NS, PMS is not added, other conditions are same as above.
It is individually added into PMS, IrGO-NS is not added, other conditions are same as above.
As shown in fig. 6, in the case where catalyst amount and less oxidizer, conventional GO and its N doped samples or
Classical metallic catalyst (nano Co3O4And Fe3O4) it cannot effectively activate PMS removal MP.As can be seen from Figure 6B, IrGO
Simple thermal treatment does not enhance its activity, but heteroatomic doping can accomplish this point.In addition, ought be only by oxidant PMS sheet
When body or individual activator IrGO-NS are added in system, the removal rate of MP is only 5% when 30 min, this shows that PMS's is straight
Connecing the adsorption approach of oxidation and IrGO-NS on MP can ignore.But when adding IrGO-NS and PMS simultaneously, 30 min
It can complete 100% MP removal.
Embodiment 3
The test specimen being prepared in Example 1 carries out the remineralization efficacy experiment of preservative methylparaben (MP).15
In mg/L MP solution, the PMS of the IrGO-NS and 307 mg/L of 20 mg/L is added, at regular intervals, sampling is filtered to remove
IrGO-NS, analysis reaction solution TOC variation.As shown in fig. 7, can remove 70% TOC after 30 min, it is seen that under experiment condition,
IrGO-NS and PMS has good remineralization efficacy to MP.
Embodiment 4
The test specimen being prepared in Example 1 is removed sun-screening agent BP-4 experiment.In 10 mg/L BP-4 solution,
The PMS of the IrGO-NS and 307 mg/L of 20 mg/L is added, at regular intervals, sampling is filtered to remove IrGO-NS, using liquid
Phase chromatography analyzes BP-4 concentration variation in reaction solution.As shown in figure 8, can remove 100% BP-4 after 30 min.
Embodiment 5
The test specimen being prepared in Example 1 is removed phenol experiment.In 20 mg/L phenol solutions, it is added 25
The PMS of the IrGO-NS and 307mg/L of mg/L, at regular intervals, sampling are filtered to remove IrGO-NS, using liquid chromatogram, divide
Analyse phenol concentration variation in reaction solution.As shown in figure 8, can remove 100% phenol after 30 min.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. activating the preparation method of the nitrogen sulphur codope graphene of persulfate, which comprises the following steps:
S1, raw material choose commercial graphene, thiocarbamide, ultrapure water, ethyl alcohol；
Commercial graphene is uniformly mixed by S2, mixing with thiocarbamide；
Commercial graphene and thiocarbamide that S2 step is uniformly mixed are placed in tube furnace, temperature control by S3, calcining under nitrogen atmosphere
System is calcined at 350-800 DEG C, and heating rate is controlled in 8-12 DEG C/min, constant temperature 40-80min, and under nitrogen atmosphere
It is cooled to room temperature；
S4, washing wash the resulting sample of S3 step with ultrapure water, ethyl alcohol respectively；
The resulting sample of S4 step is placed under vacuum environment dry 20-28h, obtains the nitrogen sulphur of activation persulfate by S5, drying
Codope graphene.
2. the preparation method of the nitrogen sulphur codope graphene of activation persulfate according to claim 1, which is characterized in that
Commercial graphene in S1 step: the mass ratio of thiocarbamide=(1:1).
3. the preparation method of the nitrogen sulphur codope graphene of activation persulfate according to claim 2, which is characterized in that
The commercialization graphene is reduction-oxidation method preparation method, SSA > 500m2/g。
4. the preparation method of the nitrogen sulphur codope graphene of activation persulfate according to claim 3, which is characterized in that
Temperature control is at 350 DEG C, 400 DEG C, 600 DEG C, 700 DEG C, 800 DEG C in S3 step.
5. the preparation method of the nitrogen sulphur codope graphene of activation persulfate according to claim 4, which is characterized in that
10 DEG C/min of heating rate in S3 step, constant temperature 60min.
6. the preparation method of the nitrogen sulphur codope graphene of activation persulfate according to claim 5, which is characterized in that
Sample obtained in S4 step first uses milli-Q water at least three times, then at least three times using ethanol washing.
7. the preparation method of the nitrogen sulphur codope graphene of activation persulfate according to claim 6, which is characterized in that
Drying time is for 24 hours in S5 step.
8. activating application of the nitrogen sulphur codope graphene of persulfate in removal water pollutant, which is characterized in that the nitrogen
Sulphur codope graphene is as according to claim 1 to the nitrogen sulphur codope graphene for activating persulfate described in 7 any one
Preparation method be prepared.
9. the nitrogen sulphur codope graphene of activation persulfate is preservative methylparaben (MP), sun-screening agent two in water removal
Benzophenone -4(BP-4) and phenol application, which is characterized in that the nitrogen sulphur codope graphene is by according to claim 1 to 7
The preparation method of the nitrogen sulphur codope graphene of activation persulfate described in meaning one is prepared.
10. activating application method of the nitrogen sulphur codope graphene of persulfate in removal water pollutant, which is characterized in that
Include the following steps, takes a certain amount of according to claim 1 to the nitrogen sulphur codope stone for activating persulfate described in 7 any one
The nitrogen sulphur codope graphene that the preparation method of black alkene is prepared is added in sewage to be processed as catalyst, is taken a certain amount of
Potassium hydrogen persulfate as oxidant be added treatment sewage in, stirring/oscillation under room temperature.
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| CN111804322A (en) * | 2020-03-05 | 2020-10-23 | 嘉兴学院 | Preparation method and application of persulfate-activated nitrogen-doped graphene loaded carbon nitride composite material |
| CN112246265A (en) * | 2020-09-04 | 2021-01-22 | 广东工业大学 | Active complex for degrading bisphenol A and application thereof |
| CN113171785A (en) * | 2021-04-26 | 2021-07-27 | 嘉兴学院 | Nitrogen-sulfur co-doped ordered mesoporous carbon material and preparation method and application thereof |
| CN113559912A (en) * | 2021-08-16 | 2021-10-29 | 哈尔滨工业大学（深圳） | Nitrogen-sulfur co-doped graphene supported cobalt catalyst, and preparation method and application thereof |
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| CN113559912A (en) * | 2021-08-16 | 2021-10-29 | 哈尔滨工业大学（深圳） | Nitrogen-sulfur co-doped graphene supported cobalt catalyst, and preparation method and application thereof |
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Application publication date: 20190705 |