CN113398973A - Graphite phase carbon nitride nanosheet and preparation method and application thereof - Google Patents
Graphite phase carbon nitride nanosheet and preparation method and application thereof Download PDFInfo
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- CN113398973A CN113398973A CN202110688746.6A CN202110688746A CN113398973A CN 113398973 A CN113398973 A CN 113398973A CN 202110688746 A CN202110688746 A CN 202110688746A CN 113398973 A CN113398973 A CN 113398973A
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 45
- 239000010439 graphite Substances 0.000 title claims abstract description 45
- 239000002135 nanosheet Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000001782 photodegradation Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000002055 nanoplate Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 15
- 239000004408 titanium dioxide Substances 0.000 abstract description 5
- 239000010842 industrial wastewater Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000002064 nanoplatelet Substances 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012719 thermal polymerization Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- -1 5-nitro-1,2, 4-triazine-3-one Chemical compound 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000010840 domestic wastewater Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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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
-
- B01J35/39—
-
- B01J35/40—
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a graphite phase carbon nitride nanosheet and a preparation method and application thereof. The graphite phase carbon nitride nanosheet has good potential in treating NTO-containing industrial wastewater, nearly 96.0% of NTO is degraded after visible light irradiation for 100min, and the performance of the graphite phase carbon nitride nanosheet is superior to that of massive graphite phase carbon nitride and commercial P25 type titanium dioxide.
Description
Technical Field
The invention belongs to the field of photocatalytic degradation, and relates to a graphite-phase carbon nitride nanosheet and a preparation method and application thereof.
Background
NTO is called 3-nitro-1, 2, 4-triazole-5-ketone, and is an energetic material with wide application. A large amount of industrial wastewater containing the NTO is inevitably generated during the process of preparing the NTO. The direct discharge of such waste water causes serious environmental pollution. At present, domestic wastewater treatment stations mainly adopt a biological method, and the method can not effectively treat NTO-containing industrial wastewater. Therefore, how to treat the industrial wastewater becomes an urgent problem to be solved.
The photodegradation technology is a green and environment-friendly technology which takes a photocatalyst as a medium and utilizes solar energy to decompose organic pollutants. Laurence et al (Photocosmetic grading of 5-nitro-1,2, 4-triazine-3-one NTO in aqueous Suspension of TiO2.Comparison with Fenton oxidation[J]Chemosphere,1999, 38(7):1561-1570.) for the first time reported titanium dioxide (TiO)2) As a photocatalyst to photodegrade NTO-containing wastewater; the experimental results show that NTO can be decomposed or mineralized through photodegradation. However, TiO2Has a wide energy band (3.2 eV), so that the ultraviolet light can only absorb ultraviolet light, and the ultraviolet light only accounts for 4% of the energy of the sunlight, so that the utilization efficiency of the sunlight is low. In the solar spectrum, visible light accounts for about 43%. Therefore, the development of a narrow-band semiconductor material with visible light response is beneficial to improving the utilization rate of solar energy. Graphite phase carbon nitride is an organic polymer semiconductor material with visible light response. The graphite phase carbon nitride has the advantages of narrow energy band, good chemical stability, easy preparation and low cost, and is widely applied to the field of photodegradation organic pollution. However, the graphite-phase carbon nitride obtained directly from the thermal polymerization of the precursor has a low specific surface area, resulting in a decrease in its photocatalytic activity.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a graphite-phase carbon nitride nanosheet photocatalyst and application of the photocatalyst in photodegradation of NTO. According to the invention, the graphite-phase carbon nitride obtained by thermal polymerization of the carbon-nitrogen-containing precursor is stripped by nitric acid to prepare the nanosheet, so that the specific surface area of the graphite-phase carbon nitride is increased, and the activity of the graphite-phase carbon nitride in photodegradation of NTO under the condition of visible light is enhanced.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of graphite phase carbon nitride nanosheets comprises the following steps:
(1) placing a carbon-nitrogen-containing precursor in a crucible;
(2) placing the crucible in the step (1) in a muffle furnace, heating the muffle furnace to 550 ℃, and preserving heat for 3-5 hours;
(3) after the reaction is finished, naturally cooling to room temperature, and grinding the obtained light yellow solid into powder by using a mortar;
(4) adding the powder obtained in the step (3) into a nitric acid aqueous solution, heating to 60 ℃ while stirring, and keeping the temperature for 3-5 hours;
(5) after the reaction is finished, naturally cooling to room temperature, transferring the suspension to a centrifugal tube, centrifuging for 10-20 min under the condition of 10000RPM to obtain a precipitate, washing the precipitate to be neutral by using a sodium carbonate solution, then washing for three times by using water, and washing for one time by using ethanol;
(6) and (5) placing the precipitate in the step (5) into an oven, and drying at 60 ℃ for 12h to finally obtain the graphite-phase carbon nitride nanosheet.
The precursor containing carbon and nitrogen in the step (1) is urea.
The temperature rise rate in the step (2) is 2.3 ℃ min-1。
The powder in step (3) should be ground to no grainy feel.
The concentration of the aqueous nitric acid solution in the step (4) was 40.0 ω t%.
The concentration of the sodium carbonate solution in the step (5) is 1.0 omega t%.
The graphite phase carbon nitride nanosheet is prepared by the preparation method.
The application of the graphite-phase carbon nitride nanosheet obtained by the invention is application in photodegradation of NTO.
The invention has the beneficial effects that: the raw materials used in the invention have low price, the preparation process is simple, and the large-scale production is easy. The specific surface area of the prepared graphite phase carbon nitride nanosheet is remarkably improved compared with that of bulk graphite phase carbon nitride, and the activity of photodegradation NTO is higher than that of the bulk graphite phase carbon nitride and commercially available titanium dioxide.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
Fig. 1 is an XRD spectrum of graphite-phase carbon nitride nanosheets prepared in example 1 and bulk graphite-phase carbon nitride prepared in comparative example 1;
fig. 2 is an SEM image of graphite phase carbon nitride nanoplates prepared in example 1;
FIG. 3 is an SEM image of bulk graphite phase carbon nitride prepared in comparative example 1;
fig. 4 is a nitrogen adsorption-desorption curve for the graphite phase carbon nitride nanosheets prepared in example 1 and the bulk graphite phase carbon nitride prepared in comparative example 1;
fig. 5 is an ultraviolet diffuse reflection absorption spectrum of graphite phase carbon nitride nanoplatelets prepared in example 1 and bulk graphite phase carbon nitride prepared in comparative example 1;
FIG. 6 is a graph showing the concentration change of photo-degraded NTO of the samples of example 1, comparative example 1 and comparative example 2;
fig. 7 is a first order kinetic fit curve of photodegradation NTO of the samples of example 1, comparative example 1 and comparative example 2.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Example 1:
the preparation method of the graphite phase carbon nitride nanosheet comprises the following specific preparation steps:
(1) 50.0g of urea was placed in a crucible;
(2) placing the crucible in the step (1) in a muffle furnace, and enabling the muffle furnace to be at 2.3 ℃ per minute-1The temperature is raised to 550 ℃ at the temperature raising rate, and the temperature is kept for 4 hours;
(3) after the reaction is finished, naturally cooling to room temperature, and grinding the obtained light yellow solid into powder by using a mortar;
(4) adding 1.0g of the powder obtained in the step (3) into 50ml of nitric acid aqueous solution with the concentration of 40.0 omega t%, heating to 60 ℃ while stirring, and keeping the temperature for 4 hours;
(5) after the reaction is finished, naturally cooling to room temperature, transferring the suspension to a centrifugal tube, centrifuging for 15min under the condition of 10000RPM to obtain a precipitate, washing the precipitate to be neutral by using a sodium carbonate solution with the concentration of 1.0 omega t%, then washing for three times by using water, and washing for one time by using ethanol;
(6) and (5) placing the precipitate in the step (5) into an oven, and drying at 60 ℃ for 12h to finally obtain the graphite-phase carbon nitride nanosheet.
The graphite phase carbon nitride nanosheet is used for photodegradation NTO, and the method comprises the following specific steps:
adding 50.0mg of graphite-phase carbon nitride nanosheets into 50.0ml of NTO aqueous solution with the concentration of 40 mg/L; stirring for 30min in the dark to reach physical adsorption equilibrium, and placing in a 300W xenon lamp (lambda)>400nm, and optical power density of about 1000mW/cm2) Carrying out reaction under irradiation; the concentration change of NTO was monitored by sampling 3ml every 20min and measuring the absorbance of the solution at 325nm with a UV spectrophotometer.
Comparative example 1:
the preparation method of the blocky graphite-phase carbon nitride comprises the following specific steps:
(1) 50.0g of urea was placed in a crucible;
(2) placing the crucible in the step (1) in a muffle furnace, and enabling the muffle furnace to be at 2.3 ℃ per minute-1The temperature is raised to 550 ℃ at the temperature raising rate, and the temperature is kept for 4 hours;
(3) and after the reaction is finished, naturally cooling to room temperature, and grinding the obtained light yellow solid into powder by using a mortar, wherein the obtained powder is the blocky graphite phase carbon nitride.
The NTO is photodegraded, and the specific steps are as follows:
adding 50.0mg of blocky graphite-phase carbon nitride into 50.0ml of NTO aqueous solution with the concentration of 40 mg/L; stirring for 30min in the dark to reach physical adsorption equilibrium, and placing in a 300W xenon lamp (lambda)>400nm, and optical power density of about 1000mW/cm2) Carrying out reaction under irradiation; sampling 3ml every 20min, measuring the solution at 325nm with UV spectrophotometerAbsorbance, and thus, the concentration change of NTO was monitored.
Comparative example 2:
the titanium dioxide used was commercial type P25.
The NTO is photodegraded, and the specific steps are as follows:
adding 50.0mg of titanium dioxide into 50.0ml of NTO aqueous solution with the concentration of 40 mg/L; stirring for 30min in the dark to reach physical adsorption equilibrium, and placing in a 300W xenon lamp (lambda)>400nm, and optical power density of about 1000mW/cm2) Carrying out reaction under irradiation; the concentration change of NTO was monitored by sampling 3ml every 20min and measuring the absorbance of the solution at 325nm with a UV spectrophotometer.
As shown in fig. 1, bulk graphite phase carbon nitride has two distinct characteristic reflections at 13.1 ° and 27.5 ° 2 θ, which are assigned to the (100) and (002) crystal planes of graphite phase carbon nitride, respectively; wherein the (100) crystal face corresponds to the tris-s-triazine repeating unit in the graphite-phase carbon nitride plane, and the (002) crystal face corresponds to the layered structure of graphite-phase carbon nitride. The reflection corresponding to the (002) crystal plane of the graphite-phase carbon nitride nanosheets was shifted to 27.8 ° compared to that of the bulk graphite-phase carbon nitride. This indicates that the interlaminar spacing of the graphite phase carbon nitride nanoplatelets is reduced, which may facilitate the transfer of electrons between the layers, thereby improving the photocatalytic performance of the graphite phase carbon nitride.
As shown in fig. 2, the graphite phase carbon nitride nanosheets are in a typical lamellar structure; the flake stacking topography of the graphite phase carbon nitride nanoplatelets is reduced, and instead is a more fractured surface topography, as compared to the bulk graphite phase carbon nitride as shown in fig. 3.
As shown in FIG. 4, from the nitrogen adsorption-desorption curves of the graphite phase carbon nitride nanosheets and the bulk graphite phase carbon nitride, specific surface areas of the graphite phase carbon nitride nanosheets and the bulk graphite phase carbon nitride of 71.4 m and 9.2m, respectively, can be obtained2·g-1。
As shown in FIG. 5, the absorption edge of bulk graphite phase carbon nitride is at 460 nm; in contrast, the absorption edge of graphite phase carbon nitride nanoplatelets is blue-shifted to about 420 nm. This is a result of the quantum effect of the nanomaterial.
As shown in fig. 6After 100min of illumination, bulk graphite phase carbon nitride, graphite phase carbon nitride nanosheets and TiO286.3%, 96.0% and 90.0% of NTO in the solution were removed, respectively. Further, as shown in fig. 7, bulk graphite phase carbon nitride, graphite phase carbon nitride nanosheets, and TiO2Respectively has an apparent kinetic constant k value of 0.0196min-1、0.0253min-1And 0.0238min-1。
Claims (8)
1. A preparation method of graphite phase carbon nitride nanosheets is characterized by comprising the following steps:
(1) placing a carbon-nitrogen-containing precursor in a crucible;
(2) placing the crucible in the step (1) in a muffle furnace, heating the muffle furnace to 550 ℃, and preserving heat for 3-5 hours;
(3) after the reaction is finished, naturally cooling to room temperature, and grinding the obtained light yellow solid into powder by using a mortar;
(4) adding the powder obtained in the step (3) into a nitric acid aqueous solution, heating to 60 ℃ while stirring, and keeping the temperature for 3-5 hours;
(5) after the reaction is finished, naturally cooling to room temperature, transferring the suspension to a centrifugal tube, centrifuging for 10-20 min under the condition of 10000RPM to obtain a precipitate, washing the precipitate to be neutral by using a sodium carbonate solution, then washing for three times by using water, and washing for one time by using ethanol;
(6) and (5) placing the precipitate in the step (5) into an oven, and drying at 60 ℃ for 12h to finally obtain the graphite-phase carbon nitride nanosheet.
2. A method for preparing graphite-phase carbon nitride nanosheets according to claim 1, wherein the carbon-nitrogen-containing precursor in step (1) is urea.
3. A method of making graphite phase carbon nitride nanoplates as in claim 1, wherein the rate of temperature rise in step (2) is 2.3 ° c.min-1。
4. A method of preparing graphite phase carbon nitride nanoplates as in claim 1, wherein the powder in step (3) should be ground to a graininess free.
5. A method of preparing graphite phase carbon nitride nanoplates as in claim 1, wherein the concentration of the aqueous nitric acid solution in step (4) is 40.0 ω t%.
6. A method of making graphite phase carbon nitride nanoplates as in claim 1, wherein the sodium carbonate solution concentration in step (5) is 1.0 wt%.
7. Graphite-phase carbon nitride nanosheets obtainable by the production method of any one of claims 1 to 6.
8. Use of graphite phase carbon nitride nanoplates in the preparation of a photodegradation NTO according to claim 7.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113880184A (en) * | 2021-10-12 | 2022-01-04 | 南京理工大学 | Method for recycling NTO in wastewater |
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| CN110560125A (en) * | 2019-09-06 | 2019-12-13 | 北京交通大学 | N-g-C3N4Preparation method and application of visible light catalytic material |
| CN112495420A (en) * | 2020-12-09 | 2021-03-16 | 北华大学 | Preparation method of nitrogen-rich graphite phase carbon nitride/silver metavanadate composite photocatalyst |
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- 2021-06-22 CN CN202110688746.6A patent/CN113398973A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2553137A1 (en) * | 1974-12-19 | 1976-07-01 | Basf Wyandotte Corp | TRIAZINE |
| CN106311348A (en) * | 2016-08-19 | 2017-01-11 | 浙江理工大学 | Composite photocatalyst, and preparation method and application thereof |
| CN110560125A (en) * | 2019-09-06 | 2019-12-13 | 北京交通大学 | N-g-C3N4Preparation method and application of visible light catalytic material |
| CN112495420A (en) * | 2020-12-09 | 2021-03-16 | 北华大学 | Preparation method of nitrogen-rich graphite phase carbon nitride/silver metavanadate composite photocatalyst |
Non-Patent Citations (1)
| Title |
|---|
| YING-SHA LIU 等: "Improved fluorescence test of chromium (VI) in aqueous solution with g-C3N4 nanosheet and mechanisms", 《MATERIALS RESEARCH BULLETIN》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113880184A (en) * | 2021-10-12 | 2022-01-04 | 南京理工大学 | Method for recycling NTO in wastewater |
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