CN117181261A - Preparation method and application of ultrahigh-activity nonmetal-doped coupling defect carbon nitride nano piezoelectric catalytic material - Google Patents
Preparation method and application of ultrahigh-activity nonmetal-doped coupling defect carbon nitride nano piezoelectric catalytic material Download PDFInfo
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- CN117181261A CN117181261A CN202311088497.2A CN202311088497A CN117181261A CN 117181261 A CN117181261 A CN 117181261A CN 202311088497 A CN202311088497 A CN 202311088497A CN 117181261 A CN117181261 A CN 117181261A
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- 239000000463 material Substances 0.000 title claims abstract description 33
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 24
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- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims description 14
- 229910017464 nitrogen compound Inorganic materials 0.000 claims description 14
- 229910052755 nonmetal Inorganic materials 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000000593 degrading effect Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- -1 carbon nitride compound Chemical class 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 230000009194 climbing Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
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- 239000003242 anti bacterial agent Substances 0.000 description 15
- 229940088710 antibiotic agent Drugs 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000008239 natural water Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
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Abstract
The invention relates to a preparation method and application of an ultrahigh-activity nonmetal-doped coupling defect carbon nitride nano piezoelectric catalytic material, which has ultrahigh piezoelectric catalytic activity and belongs to the technical field of preparation and application of novel functional materials. According to the invention, the growth of the coupling defect carbon nitride nano material is regulated and controlled in situ by a nonmetallic material, the coupling defect carbon nitride material is prepared first, and the nonmetallic doping coupling carbon nitride nano piezoelectric catalytic material with special morphology is further obtained through nonmetallic doping, so that the coupling defect carbon nitride nano piezoelectric catalytic material is used for removing pollutants in water through piezoelectric catalytic degradation. The invention has the advantages that: (1) The synthesis process is simpler and the industrialized amplified production is easier; (2) The piezoelectric catalytic activity of the modified coupling carbon nitride piezoelectric catalytic material is higher, and pollutants can be degraded green and efficiently; (3) The operation is simple, the reaction condition is mild, and the requirements of practical engineering application can be met. (4) The preparation method has the advantages of easily available raw materials, simple process and convenient operation, can degrade organic pollutants in water under the action of ultrasound, and provides an energy-saving and efficient feasible strategy for water environment pollution.
Description
[ field of technology ]
The invention belongs to the technical field of sewage treatment, and relates to a preparation method of an ultra-high-activity nonmetal-doped coupling defect carbon nitride nano piezoelectric catalytic material and application of the material in piezoelectric catalytic degradation of antibiotics.
[ background Art ]
The antibiotics has wide application range and large dosage, and the probability of the antibiotics in natural water environment is high. Many domestic and foreign researches report that various antibiotics are detected in natural water environment, including natural water bodies such as ocean, river, lake, groundwater and the like; the antibiotic waste water has high chroma and contains various refractory and biotoxic substances, and is high-concentration organic waste water, so that a method for removing antibiotics in water before entering a purified water plant is urgently needed. At present, technologies such as membrane separation, adsorption, biodegradation, advanced oxidation and the like are explored and researched to remove antibiotics in the environment, as a photocatalyst capable of degrading the antibiotics is disclosed in patent 202010655115.X, a preparation method and application thereof are provided, and a sulfur-doped iron-based metal-organic framework material and a method for adsorbing the antibiotics in a water body are provided. But must be coordinated with visible light to function, which is difficult to perform in dark environments. The conventional water purification process in China is mostly carried out in a dark environment, the overall process flow is simpler, equipment is not easy to improve, and the enhancement of the degradation of antibiotics in water under the conditions of dark environment and no chemical addition is the leading direction of the current research. Piezoelectric catalysis is an emerging water purification method in recent years, and is favored by researchers because of the advantages of no chemical addition, darkroom operation, rapid reaction, and the like. As patent 202111055062.9 discloses a barium titanate nanomaterial for piezoelectrically degrading micro organic pollutants in water and a preparation method thereof, the barium titanate nanomaterial prepared by the invention can strengthen separation of electron and hole pairs by absorbing environmental energy, thereby playing a catalytic role in the degradation process of micro organic pollutants; at room temperature, the trace organic pollutants such as antibiotics and the like can be efficiently degraded; can be stably recycled, etc.
The coupled carbon nitride material is a novel two-dimensional material and consists of carbon and nitrogen elements. It has a layered structure similar to graphene in which carbon and nitrogen atoms form a network structure in a pulsed or cross arrangement. Coupled carbon nitride materials have many excellent properties including high conductivity, excellent mechanical strength, excellent optical properties, and tunable bandgap properties. The characteristics lead the coupled carbon nitride material to have wide application prospect in the fields of energy storage, catalysts, sensors, electronic devices and the like. At the same time, it is also considered as an environmentally friendly and sustainable material candidate.
[ invention ]
[ problem to be solved ]
In order to solve the technical problem that an effective means for removing antibiotics in tap water is lacking in a purified water plant, the preparation method and the application of the ultra-high activity nonmetal doping coupling defect carbon nitride nano piezoelectric catalytic material are provided. The ultra-high activity nonmetal doping coupling defect carbon nitride nano piezoelectric catalytic material is simple to prepare, convenient to use, pollution-free to the environment, easy to recycle and good in stability.
Technical scheme
The application of the ultra-high activity non-metal doped coupling defect carbon nitride nano piezoelectric catalytic material in degrading organic pollutants comprises the following steps:
(1) Weighing and weighing1-10g of nitrogen carbide precursor is fully ground and then is introduced into a covered quartz crucible, and is calcined for 1-8h at 200-800 ℃ by a muffle furnace, wherein the climbing speed is 1-20 ℃/min -1 Obtaining a carbon nitrogen compound;
(2) Collecting a carbon nitrogen compound precursor, performing ultrasonic treatment for 10-200min, washing with ultrapure water and ethanol for several times, and drying at 10-150 ℃ for 1-20 hours to obtain a modified carbon nitrogen compound sample;
(3) Grinding and mixing 1-10g of modified carbon nitrogen compound sample and 1-10g of nonmetallic material, and calcining in a muffle furnace at 200-800 ℃ for 1-8h at a climbing speed of 1-20 ℃/min -1 Obtaining the nonmetallic doping coupling defect carbon nitride nanomaterial.
(4) Weighing 1-500mg of modified coupled carbon nitride compound sample powder, and adding the powder into a pollutant water sample with the volume of 1-500 ml;
(5) Exciting piezoelectric catalytic reaction for 0.01-5h by using ultrasonic with power of 20-1000Hz, and measuring the concentration of target pollutants after filtering;
2. the coupling carbon nitride is one or more than two of carbon fiber, carbon black, graphene, carbon nano tube, carbon quantum dot, graphite alkyne and carbon nitrogen compound.
3. The use according to claim 1, characterized in that the nonmetallic material in step 3 is one or a mixture of two or more of silicic acid, silicate, aluminate, boric acid, borate, phosphoric acid, phosphate.
The invention has the beneficial effects that: according to the invention, the piezoelectric coupling defect carbon nitride and the nonmetallic material are effectively compounded, so that simple harmonic vibration can be realized under the action of ultrasound, piezoelectric power is generated, generation of active free radicals is promoted, the energy utilization rate is high, and a remarkable piezoelectric effect is achieved; the ultra-high activity nonmetal doped coupling carbon nitride nano piezoelectric catalytic material prepared by the invention can be used for piezoelectrically catalyzing and degrading antibiotic pollutants in sewage at normal temperature, and has remarkable degradation effect on partial antibiotics.
[ description of the drawings ]
Fig. 1 is an SEM image of the inner surface of the ultra-high activity non-metal doped coupled carbon nitride nano-piezoelectric catalytic material prepared after the embodiment.
Fig. 2 is a TEM image of an ultra-high activity non-metal doped coupled carbon nitride nano-piezoelectric catalytic material prepared after an embodiment.
FIG. 3 is a graph showing the effect of the ultra-high activity non-metal doped coupled carbon nitride nano-piezoelectric catalytic material prepared after the implementation of the method for rapidly degrading antibiotics.
[ detailed description ] of the invention
In order to further describe the technical means and effects adopted by the present invention to achieve the preset purpose, the following detailed description is given with reference to the accompanying drawings and examples.
(1) Weighing 3g of carbon nitride precursor, fully grinding by using a mortar, then placing into a crucible, and placing into a box-type resistance furnace at a speed of 8 ℃/min -1 And (3) heating to 350 ℃, and preserving heat for 5 hours to obtain brown powder, namely the carbon-nitrogen compound.
(2) Taking a synthesized carbon-nitrogen compound matrix, carrying out ultrasonic treatment for 10min, washing with ultrapure water for 3 times, washing with absolute ethyl alcohol for 3 times, and drying for 3h at 40 ℃ in a drying oven to obtain brown powder, namely the modified carbon-nitrogen compound sample.
(3) Taking 3g of synthesized modified carbon nitrogen compound sample and nonmetal material, fully grinding, then placing into a crucible, and placing into a box-type resistance furnace at a speed of 8 ℃/min -1 The temperature is raised to 350 ℃ and kept for 5 hours to obtain brown powder which is marked as nonmetal doped coupled carbon nitride nano material, and the scanning electron microscope and transmission electron microscope results are shown in figure 1.
(4) The scanning electron microscope image of the attached figure 1 can prove that the ultra-high activity non-metal doped coupling defect carbon nitride nano piezoelectric catalytic material which is a lamellar aggregate is successfully prepared. The transmission electron microscope image of fig. 2 shows that the prepared ultra-high activity non-metal doped coupling defect carbon nitride nano piezoelectric catalytic material has a lamellar porous structure.
(5) 100mg of the modified coupled carbon nitride sample powder was weighed and added to a contaminant water sample having a volume of 50 ml.
(6) The piezoelectric catalytic reaction is excited for 1h by using the ultrasonic with the power of 50Hz, and the concentration of the target pollutant is measured after filtration.
(7) As can be seen from the figure 3, the prepared ultra-high activity nonmetal doping coupling defect carbon nitride nano piezoelectric catalytic material can effectively remove antibiotics in water under the action of ultrasound, and the removal rate of the antibiotics is close to 92% when the reaction time is 80 min.
Claims (3)
1. The application of the ultra-high activity nonmetal doped coupling defect carbon nitride nano piezoelectric catalytic material in degrading organic pollutants in water is characterized in that the preparation of the nonmetal doped coupling defect carbon nitride material and the piezoelectric catalytic degradation of the organic pollutants in water comprise the following steps:
(1) Weighing 1-10g of carbon nitride precursor, fully grinding, introducing into a covered quartz crucible, calcining at 200-800 ℃ for 1-8h by using a muffle furnace, wherein the climbing rate is 1-20 ℃/min -1 Obtaining a carbon nitrogen compound;
(2) Collecting a carbon nitrogen compound precursor, performing ultrasonic treatment for 10-200min, washing with ultrapure water and ethanol for several times, and drying at 10-150 ℃ for 1-20 hours to obtain a modified carbon nitrogen compound sample;
(3) Grinding and mixing 1-10g of modified carbon nitrogen compound sample and 1-10g of nonmetallic material, and calcining in a muffle furnace at 200-800 ℃ for 1-8h at a climbing speed of 1-20 ℃/min -1 Obtaining the nonmetallic doping coupling defect carbon nitride nanomaterial.
(4) Weighing 1-500mg of modified coupled carbon nitride compound sample powder, and adding the powder into a pollutant water sample with the volume of 1-500 ml;
(5) The piezoelectric catalytic reaction is excited by ultrasonic with the power of 20-1000Hz for 0.01-5h, and the concentration of the target pollutant is measured after filtration.
2. The carbon nitride is one or more than two of carbon fiber, carbon black, graphene, carbon nano tube, carbon quantum dot, graphite alkyne and carbon nitrogen compound.
3. The use according to claim 1, characterized in that the nonmetallic material in step 3 is one or a mixture of two or more of silicic acid, silicate, aluminate, boric acid, borate, phosphoric acid, phosphate.
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| CN202311088497.2A CN117181261A (en) | 2023-08-28 | 2023-08-28 | Preparation method and application of ultrahigh-activity nonmetal-doped coupling defect carbon nitride nano piezoelectric catalytic material |
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| CN202311088497.2A CN117181261A (en) | 2023-08-28 | 2023-08-28 | Preparation method and application of ultrahigh-activity nonmetal-doped coupling defect carbon nitride nano piezoelectric catalytic material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117756069A (en) * | 2024-02-22 | 2024-03-26 | 中山大学 | nonmetal doping C for efficiently producing hydrogen peroxide3N5-xPiezoelectric material, preparation method thereof and application thereof in sewage treatment |
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2023
- 2023-08-28 CN CN202311088497.2A patent/CN117181261A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117756069A (en) * | 2024-02-22 | 2024-03-26 | 中山大学 | nonmetal doping C for efficiently producing hydrogen peroxide3N5-xPiezoelectric material, preparation method thereof and application thereof in sewage treatment |
| CN117756069B (en) * | 2024-02-22 | 2024-05-03 | 中山大学 | Nonmetal doping C for efficiently producing hydrogen peroxide3N5-xPiezoelectric material, preparation method thereof and application thereof in sewage treatment |
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