CN110064429A - Preparation method of sulfur doping azotized carbon nano piece and products thereof and application - Google Patents
Preparation method of sulfur doping azotized carbon nano piece and products thereof and application Download PDFInfo
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- CN110064429A CN110064429A CN201910471511.4A CN201910471511A CN110064429A CN 110064429 A CN110064429 A CN 110064429A CN 201910471511 A CN201910471511 A CN 201910471511A CN 110064429 A CN110064429 A CN 110064429A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 44
- 239000011593 sulfur Substances 0.000 title claims abstract description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 41
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 39
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 39
- WZRRRFSJFQTGGB-UHFFFAOYSA-N 1,3,5-triazinane-2,4,6-trithione Chemical compound S=C1NC(=S)NC(=S)N1 WZRRRFSJFQTGGB-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 8
- 229910052573 porcelain Inorganic materials 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000002135 nanosheet Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 241000446313 Lamella Species 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229920001021 polysulfide Polymers 0.000 claims description 5
- 239000005077 polysulfide Substances 0.000 claims description 5
- 150000008117 polysulfides Polymers 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- XLJMAIOERFSOGZ-UHFFFAOYSA-N cyanic acid Chemical compound OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000011229 interlayer Substances 0.000 claims description 4
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N thiocyanic acid Chemical compound SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004098 Tetracycline Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229960002180 tetracycline Drugs 0.000 claims description 3
- 229930101283 tetracycline Natural products 0.000 claims description 3
- 235000019364 tetracycline Nutrition 0.000 claims description 3
- 150000003522 tetracyclines Chemical class 0.000 claims description 3
- 238000005829 trimerization reaction Methods 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229910052571 earthenware Inorganic materials 0.000 claims description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims 2
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims 1
- 229940113088 dimethylacetamide Drugs 0.000 claims 1
- 239000003242 anti bacterial agent Substances 0.000 abstract description 3
- 229940088710 antibiotic agent Drugs 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241000700605 Viruses Species 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- MEFUMNTZTUDUBG-UHFFFAOYSA-N oxalonitrile 1,3,5-triazine-2,4,6-triamine Chemical compound N#CC#N.N1=C(N)N=C(N)N=C1N MEFUMNTZTUDUBG-UHFFFAOYSA-N 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 241000712461 unidentified influenza virus Species 0.000 description 1
Classifications
-
- 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
-
- B01J35/39—
-
- B01J35/61—
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The present invention is a kind of preparation method of sulfur doping azotized carbon nano piece, this method is specific steps are as follows: precise melamine, trithiocyanuric acid and solvent, melamine and trithiocyanuric acid are added in solvent, stir evenly and are put into hydrothermal reaction kettle progress solvent thermal reaction after dissolving.It is put into crucible with cover and roasts after above-mentioned reaction product is dry, grinding, finally obtained solid is sulfur doping azotized carbon nano piece.The sulfur doping azotized carbon nano piece prepared using the method for the invention, large specific surface area, photo-generated carrier separative efficiency is high, and photocatalytic degradation effects of antibiotics is good, and preparation flow is simple, and yield is high, at low cost, is suitble to large-scale promotion.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of preparation method of sulfur doping azotized carbon nano piece and
Its product and application.
Background technique
Photocatalysis technology is that the sun that can use developed rapidly in recent years can be carried out the depollution of environment and energy conversion
New technology.On the one hand, we can convert highdensity chemical energy for the solar energy of low-density by photocatalysis technology, separately
On the one hand, we can decompose various pollutants by photocatalysis technology and kill bacterium and virus.Compared to other technologies,
Photocatalysis technology, which has the advantage that, can directly utilize sunlight environment purification；Thorough degradation of contaminant at room temperature, especially has
Malicious persistent organic pollutants；Effectively kill bacterium, virus, including typical pathogenic bacteria, SARS, influenza virus；Safely, without secondary
Pollution, pollutant are decomposed into CO by exhaustive oxidation2、H2The harmless products such as O；Wide spectrum, long-acting, hundreds of pollutant nearly all can quilt
Degradation.But existing catalysis material remains that conversion quantum efficiency is low, the low defect of solar energy utilization ratio.
Carbonitride is a kind of yellow graphite-structure substance, and carbonitride is free of metal, cheap and easy to get without toxicity, and it is former
Material rich reserves in the earth, are readily synthesized, and have good chemistry and thermal stability.Therefore, in photocatalysis field
Cause extensive concern.
The conventional synthesis process of carbonitride is that carbonitride is prepared in the carbon containing nitrogen of high-temperature roasting raw material abundant at present, this
Although carbonitride is graphite-structure, do not peel away between lamella, which results in its specific surface area is not big enough, reaction is connect
Contacting surface product is too low, limits the raising of photocatalysis performance.In order to prepare sheet carbonitride, the stripping means generallyd use at present
Have: the mode of ultrasound after the removing of liquid phase ultrasound, the removing of solid phase pyroreaction and concentrated acid protonation.These method charge stripping efficiencies
Not high, cumbersome and yield is very low, is not suitable for amplification metaplasia and produces.On the other hand, carbonitride forbidden bandwidth is 2.7eV, forbidden band
Width is excessive, it is seen that light area absorptance is not high, and solar energy utilization ratio is not high.
The present invention uses melamine and trithiocyanuric acid for raw material, is prepared by hydro-thermal or solvent thermal reaction
Supermolecule presoma, the presoma are graphite-like structure, then make every a piece of supermolecule be condensed into sulphur by high-temperature roasting and mix
Miscellaneous carbonitride can strut lamella at a distance from piece interlayer, finally obtain flake simultaneously because pyroprocess has gas generation
Sulfur doping carbonitride.The sulfur doping azotized carbon nano piece obtained using preparation method proposed by the present invention, large specific surface area, forbidden band
Width is moderate, and photocatalytic degradation effects of antibiotics is good, and easy to operate, and step is few, and raw material is easy to get, at low cost, is suitble to amplificationization
Production.
Summary of the invention
Prepare that carbonitride specific surface area is not high, and forbidden bandwidth is larger for existing, it is seen that the not high disadvantage of light absorption, this hair
A kind of bright preparation method for being designed to provide sulfur doping azotized carbon nano piece.
Another object of the present invention is: providing a kind of sulfur doping azotized carbon nano flake products of above method preparation.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention is realized by following proposal: a kind of preparation method of sulfur doping azotized carbon nano piece, feature exist
In using melamine and trithiocyanuric acid as raw material, supermolecule forerunner is prepared by hydro-thermal or solvent thermal reaction
Body, the presoma are graphite-like structure, then make to be condensed into sulfur doping carbonitride per a piece of supermolecule by high-temperature roasting, together
When have gas generation due to pyroprocess, lamella can be strutted at a distance from piece interlayer, finally obtain laminar sulfur doping nitridation
Carbon includes the following steps:
1) melamine, trithiocyanuric acid and solvent accurately are weighed according to formula, first by melamine and three polysulfide cyanogen
Acid is added in solvent, and hydrothermal reaction kettle is added into after stirring evenly, and controls 100~200 DEG C of reaction temperature, reacts 1~72h
Cooled to room temperature later；
2) solid that above-mentioned reaction obtains cleaned, ground after drying, be then placed in porcelain boat ceramic earthenware with cover
Heating (heating rate is 1~20 DEG C/min) is to 400~650 DEG C in crucible, heat preservation 0.1~15h of roasting, consolidating after natural cooling
Body is sulfur doping azotized carbon nano piece.
Wherein solvent is deionized water, ethyl alcohol, isopropanol, ethylene glycol, N,N-dimethylformamide, second cyanogen, dimethyl Asia
The mass ratio of one or mixing in sulfone, n,N-dimethylacetamide, melamine and trithiocyanuric acid is 1:0.1~10, trimerization
The mass ratio of cyanamide and solvent is 1:5~200.
The present invention provides a kind of sulfur doping azotized carbon nano piece, is prepared according to described any the method.
The present invention provides a kind of application of sulfur doping azotized carbon nano piece in tetracycline of degrading under visible light.
Sulfur doping azotized carbon nano piece provided by the invention the preparation method comprises the following steps: precise melamine, three polysulfide cyanogen
Melamine and trithiocyanuric acid are added in solvent for acid and solvent, stir evenly and are put into hydro-thermal reaction after dissolving
Kettle carries out solvent thermal reaction.It is put into crucible with cover and roasts after above-mentioned reaction product is dry, grinding, it is finally obtained
Solid is sulfur doping azotized carbon nano piece.
The invention using trithiocyanuric acid as sulphur source, on the one hand provide doping carbonitride in element sulphur source,
Another aspect trithiocyanuric acid and melamine can form the oversubscription of graphite-like structure in the reactive mode of hydro-thermal solvent heat
Minor structure, and generate gas during heating roasting and strut the layer of class graphite with layer, a final step forms sulfur doping
Azotized carbon nano piece.Compared to current other azotized carbon nano piece preparation methods, preparation flow is simple, and step is few, and yield is high,
Low energy consumption, and preparation difficulty is small, is suitble to large-scale production.In addition to this, the present invention passes through the introducing of doped chemical sulphur, reduces taboo
Bandwidth, improves efficiency of light absorption, and large specific surface area, hole and is electrically separated high-efficient, and catalytic performance is also more preferable.
The sulfur doping azotized carbon nano piece prepared using the method for the invention, large specific surface area, photo-generated carrier separation
High-efficient, photocatalytic degradation effects of antibiotics is good, and preparation flow is simple, and yield is high, at low cost, is suitble to large-scale promotion.
Detailed description of the invention
The SEM photograph of Fig. 1 sulfur doping azotized carbon nano piece.
Specific embodiment
The present invention is further illustrated below by embodiment, is not intended to limit the scope of the invention.
Embodiment 1
A kind of sulfur doping azotized carbon nano piece, uses melamine and trithiocyanuric acid for raw material, passes through hydro-thermal or solvent
Supermolecule presoma is prepared in thermal response, which is graphite-like structure, is then made by high-temperature roasting per a piece of super
Molecule is condensed into sulfur doping carbonitride, simultaneously because pyroprocess has gas generation, to strut lamella at a distance from piece interlayer, most
Laminar sulfur doping carbonitride is obtained eventually, is prepared as follows:
1) precise melamine, trithiocyanuric acid and solvent, wherein solvent is deionized water, melamine and three polysulfides
The mass ratio of cyanic acid is 1:2, and the mass ratio of melamine and solvent is 1:50, melamine and trithiocyanuric acid is added molten
In agent, it is added into hydrothermal reaction kettle after stirring evenly, when controlling 150 DEG C of reaction temperature, reacts 12h, later natural cooling
To room temperature, obtained solid reactant；
2) it will be ground after the cleaning of above-mentioned reaction product, drying, and be then placed in porcelain boat ceramic crucible with cover and add
Heat, heating rate are 10 DEG C/min, roast 3 h to 500 DEG C of heat preservations, the solid obtained after natural cooling is sulfur doping nitridation
Carbon nanosheet.SEM photograph is as shown in Figure 1.
Embodiment 2
A kind of sulfur doping azotized carbon nano piece, prepares as follows:
1) precise melamine, trithiocyanuric acid and solvent, wherein solvent is ethyl alcohol, melamine and trithiocyanuric acid
Mass ratio be 1:1, the mass ratio of melamine and solvent is 1:20, and solvent is added in melamine and trithiocyanuric acid
In, it is added into hydrothermal reaction kettle after stirring evenly, reacts 5h when controlling 180 DEG C of reaction temperature, naturally cools to room later
Temperature obtains solid reaction product；
2) it will be ground after the cleaning of above-mentioned solid reaction product, drying, be then placed in porcelain boat ceramic crucible with cover
Middle heating, heating rate are 2 DEG C/min, roast 5h to 550 DEG C of heat preservations, the solid obtained after natural cooling is sulfur doping nitrogen
Change carbon nanosheet.
Embodiment 3
A kind of sulfur doping azotized carbon nano piece, prepares as follows:
1) precise melamine, trithiocyanuric acid and solvent, wherein solvent is n,N-Dimethylformamide, melamine
It is 1:0.1 with the mass ratio of trithiocyanuric acid, the mass ratio of melamine and solvent is 1:100, by melamine and trimerization
Thiocyanic acid is added in solvent, hydrothermal reaction kettle is added into after stirring evenly, control is reacted for 24 hours at 130 DEG C, naturally cold later
But to room temperature, solid reaction product is obtained；
2) it will be ground after the cleaning of above-mentioned solid reaction product, drying, be then placed in porcelain boat ceramic crucible with cover
Middle heating, heating rate are 5 DEG C/min, roast 4h to 600 DEG C of heat preservations, the solid obtained after natural cooling is sulfur doping nitrogen
Change carbon nanosheet.
Subordinate list 1 prepares sulfur doping azotized carbon nano piece using the method for the present invention and degrades under visible light the performance of tetracycline
The sulfur doping azotized carbon nano piece that the method for the present invention obtains is than pure carbonitride superior performance.
Claims (7)
1. a kind of preparation method of sulfur doping azotized carbon nano piece, it is characterised in that use melamine and trithiocyanuric acid for
Supermolecule presoma is prepared by hydro-thermal or solvent thermal reaction in raw material, which is graphite-like structure, then passes through
High-temperature roasting to be condensed into sulfur doping carbonitride per a piece of supermolecule, simultaneously because pyroprocess has gas generation, to strut
Lamella finally obtains laminar sulfur doping carbonitride, includes the following steps: at a distance from piece interlayer
1) melamine, trithiocyanuric acid and solvent accurately are weighed according to formula, first by melamine and three polysulfide cyanogen
Acid is added in solvent, and hydrothermal reaction kettle is added into after stirring evenly, and controls 100~200 DEG C of reaction temperature, reacts 1~72h
Cooled to room temperature later；
2) solid that above-mentioned reaction obtains cleaned, ground after drying, be then placed in porcelain boat ceramic earthenware with cover
Heating (heating rate is 1~20 DEG C/min) is to 400~650 DEG C in crucible, heat preservation 0.1~15h of roasting, consolidating after natural cooling
Body is sulfur doping azotized carbon nano piece.
2. the preparation method of sulfur doping azotized carbon nano piece according to claim 1, which is characterized in that wherein solvent be go from
Sub- water, ethyl alcohol, isopropanol, ethylene glycol, N,N-dimethylformamide, second cyanogen, dimethyl sulfoxide, its in DMAC N,N' dimethyl acetamide
One or mixing, the mass ratio of melamine and trithiocyanuric acid is 1:0.1~10, and the mass ratio of melamine and solvent is 1:5
~200.
3. the preparation method of sulfur doping azotized carbon nano piece according to claim 1 or claim 2, which is characterized in that as follows
Preparation:
1) precise melamine, trithiocyanuric acid and solvent, wherein solvent is deionized water, melamine and three polysulfides
The mass ratio of cyanic acid is 1:2, and the mass ratio of melamine and solvent is 1:50, melamine and trithiocyanuric acid is added molten
In agent, it is added into hydrothermal reaction kettle after stirring evenly, when controlling 150 DEG C of reaction temperature, reacts 12h, later natural cooling
To room temperature, obtained solid reactant；
2) it will be ground after the cleaning of above-mentioned reaction product, drying, and be then placed in porcelain boat ceramic crucible with cover and add
Heat, heating rate are 10 DEG C/min, roast 3 h to 500 DEG C of heat preservations, the solid obtained after natural cooling is sulfur doping nitridation
Carbon nanosheet.
4. the preparation method of sulfur doping azotized carbon nano piece according to claim 1 or claim 2, which is characterized in that as follows
Preparation:
1) precise melamine, trithiocyanuric acid and solvent, wherein solvent is ethyl alcohol, melamine and trithiocyanuric acid
Mass ratio be 1:1, the mass ratio of melamine and solvent is 1:20, and solvent is added in melamine and trithiocyanuric acid
In, it is added into hydrothermal reaction kettle after stirring evenly, reacts 5h when controlling 180 DEG C of reaction temperature, naturally cools to room later
Temperature obtains solid reaction product；
2) it will be ground after the cleaning of above-mentioned solid reaction product, drying, be then placed in porcelain boat ceramic crucible with cover
Middle heating, heating rate are 2 DEG C/min, roast 5h to 550 DEG C of heat preservations, the solid obtained after natural cooling is sulfur doping nitrogen
Change carbon nanosheet.
5. the preparation method of sulfur doping azotized carbon nano piece according to claim 1 or claim 2, which is characterized in that as follows
Preparation:
1) precise melamine, trithiocyanuric acid and solvent, wherein solvent is n,N-Dimethylformamide, melamine
It is 1:0.1 with the mass ratio of trithiocyanuric acid, the mass ratio of melamine and solvent is 1:100, by melamine and trimerization
Thiocyanic acid is added in solvent, hydrothermal reaction kettle is added into after stirring evenly, control is reacted for 24 hours at 130 DEG C, naturally cold later
But to room temperature, solid reaction product is obtained；
2) it will be ground after the cleaning of above-mentioned solid reaction product, drying, be then placed in porcelain boat ceramic crucible with cover
Middle heating, heating rate are 5 DEG C/min, roast 4h to 600 DEG C of heat preservations, the solid obtained after natural cooling is sulfur doping nitrogen
Change carbon nanosheet.
6. a kind of sulfur doping azotized carbon nano piece, it is characterised in that be prepared into according to claim 1 to any one of 5 the methods
It arrives.
A kind of application 7. sulfur doping azotized carbon nano piece according to claim 6 is degraded under visible light in tetracycline.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110560129A (en) * | 2019-09-10 | 2019-12-13 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of modified carbon nitride for improving tetracycline degradation efficiency, and product and application thereof |
| CN110639588A (en) * | 2019-09-30 | 2020-01-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of iodine and sulfur co-doped carbon nitride |
| CN111129510A (en) * | 2019-12-16 | 2020-05-08 | 江苏大学 | Preparation method and application of carbon material modified graphite phase carbon nitride nanosheet loaded platinum nano electro-catalyst |
| CN111203262A (en) * | 2020-03-05 | 2020-05-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for rapidly preparing carbon nitride nanosheet loaded nano-copper, product and application thereof |
| CN111330616A (en) * | 2020-03-05 | 2020-06-26 | 江苏海洋大学 | Preparation of graphite-like phase carbon nitride |
| CN111547688A (en) * | 2020-05-21 | 2020-08-18 | 福州大学 | Fluorescence-controllable carbon nitride, preparation method thereof and application thereof in LED |
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