CN108554433B - Preparation method of sulfur-doped boron nitride nanosheet - Google Patents
Preparation method of sulfur-doped boron nitride nanosheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 27
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 11
- 230000001699 photocatalysis Effects 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 230000033444 hydroxylation Effects 0.000 claims description 3
- 238000005805 hydroxylation reaction Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 16
- 238000001782 photodegradation Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 231100000956 nontoxicity Toxicity 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 description 7
- 229910052755 nonmetal Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 231100000252 nontoxic Toxicity 0.000 description 4
- 230000003000 nontoxic effect Effects 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001424 field-emission electron microscopy Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003040 nociceptive effect Effects 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
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention relates to the field of photocatalysis, and provides a preparation method of a sulfur-doped boron nitride nanosheet. The method is simple and effective, and the prepared photocatalyst has the advantages of outstanding effect, no toxicity to the environment, high adsorption quantity and good photodegradation effect.
Description
Technical Field
The invention relates to the field of nanosheet preparation, and in particular relates to a preparation method of sulfur-doped boron nitride nanosheets.
Background
With the rapid development of economy, the urbanization trend is continuously strengthened, more and more domestic garbage are flushed into the water environment, and the water source is seriously polluted. The search for a nontoxic, cheap and efficient photocatalyst for photocatalytic water purification is a research hotspot in the field of photocatalysis. Cadmium sulfide, bismuth oxide and transition metal oxides have been found to exhibit good photodegradation properties under visible light long ago. (see references a.ye, w.fan, q.zhang, w.deng, y.wang, cat.sci.technol.2012, 2,969.g.zhao, s.w.liu, q.f.lu and l.j.song, ind.eng.chem.res.2012,51,10307.) however, most photocatalysts contain heavy metalsAnd toxic elements, causing irreversible pollution to the water body. Subsequently, titanium dioxide (TiO)2) Has been discovered and studied as a non-toxic photocatalyst. Compared with noble metal catalysts (Pt, Au), the catalyst has lower price, but is not metal catalysts (g-C)3N4S) phase ratio, TiO2The price of (a) is relatively high. Furthermore, TiO2The photoresponse under visible light is small, for example, photocatalytic degradation of organic pollutants under visible light is inefficient. Also, for pure non-metallic catalysts (g-C)3N4S), the photo-oxidative corrosion effect affects the photostability of the catalyst under visible light. (see reference A.Vitetadini, A.Selloni, F.P.Rotzinger, M.
Phys.rev.lett.1998,81,2954.c.w.peng, t.y.ke, l.brohan, m.r.plouet, j.c.huang, e.puzenat, h.t.chu and c.y.lee, chem.mater.2008,20,2426.x.q.gong, a.selloni, m.batzll, u.diebold, nat.mater.2006,5,665.x.c.wang, k.maeda, a.thomas, k.takanabe, g.xin, j.m.carlsson, k.domen, and m.antonieti, Nature mater.2009,8,76.g.liu, p.niu, l.c.yin h.m.m.90j.am.m.9070, amalga, non-toxic catalysts, anti-oxidative metals, nociceptive catalysts, sorla, etc. catalysts are sought.
Two-dimensional nanomaterials, e.g. graphene, MoS2(molybdenum disulfide) nanosheets, h-BN (hexagonal boron nitride) nanosheets, WS2The (tungsten disulfide) nanosheets and the like have excellent physical and chemical properties and have wide application prospects in the aspects of energy storage, laser modulation, fluorescence, catalysis, machinery and the like, so the nanosheets and the like become research hotspots in the material field in recent years. Among these materials, two-dimensional non-metallic hexagonal boron nitride nanosheets (h-BNNS) are attracting attention for their excellent adsorption and oxidation resistance. From the results of the present study, H-BNNS has very good adsorption of contaminants. (see references W.Lei, D.Portehault, D.Liu, S.Qin, Y.Chen, nat. Commun.20134,1777.) then, we designed and prepared a novel two-dimensional non-metal photocatalyst, namely sulfur-doped boron nitride nanosheet (S-BNNS), which is non-toxic, high in adsorption capacity and high in photodegradation effect, and researches show thatThe invention has excellent application prospect of purifying water source by photodegradation pollutants, therefore, the invention has good practical value.
Disclosure of Invention
Aiming at the problems of the existing two-dimensional non-metal photocatalyst in preparation and catalysis, the invention provides a method for simply and directly preparing a photocatalyst, namely a sulfur-doped boron nitride nanosheet (S-BNNS), which has the advantages of high adsorption capacity, high photodegradation efficiency, no toxicity to the environment, ultra-stable catalytic performance and the like when being used as the photocatalyst.
A preparation method of sulfur-doped boron nitride nanosheets comprises the following steps:
(1) preparing an activated boron nitride nanosheet:
preparing hexagonal boron nitride nanosheets in batches by a rotary ultrasonic stripping preparation method, and obtaining active boron nitride nanosheets through hydroxylation;
(2) preparing sulfur-doped boron nitride nanosheets:
adopting a double-heat-source vacuum tube furnace, and under the protective atmosphere, mixing sulfur powder with the HO-BNNS obtained in the step (1) according to the mass ratio of 1: 1-100:1, respectively arranged in a front heating zone and a rear heating zone of the tubular furnace, wherein the temperature of the front heating zone is set to 200-.
The protective atmosphere is one of argon, nitrogen or ammonia.
The method is used for the boron nitride ceramic artware, so that the boron nitride ceramic artware has a photocatalysis function.
The invention has the following beneficial effects:
(1) the invention discloses a method for preparing a two-dimensional non-metal photocatalyst S-BNNS by using a chemical vapor deposition method, which realizes the adjustment of the band gap of an h-BNNS nanosheet through the doping of sulfur atoms, so that the h-BNNS with originally non-photocatalytic performance is changed into the S-BNNS photocatalyst with visible light degradation performance.
(2) The method is simple and effective, and the prepared photocatalyst has the advantages of outstanding effect, no toxicity to the environment, high adsorption quantity and good photodegradation effect.
(3) The method can be used for boron nitride ceramic artware to enable the boron nitride ceramic artware to have a photocatalytic function.
Drawings
FIG. 1 field emission and transmission electron microscopy scans of HO-BNNS obtained in example 1, step (1).
FIG. 2 is a schematic flow diagram of the present invention.
FIG. 3 is a field emission electron microscope scan and an EDX scan of the two-dimensional non-metallic photocatalyst S-BNNS obtained in example 1 (panel b corresponds to sulfur element; panel c corresponds to boron element; panel d corresponds to nitrogen element).
FIG. 4 shows the photodegradability of the two-dimensional non-metal photocatalyst S-BNNS obtained in example 1 to rhodamine B.
FIG. 5 is a comparison of the photo-degradation performance of the two-dimensional non-metal photocatalyst S-BNNS obtained in example 1 and rhodamine B by using several commonly used photocatalysts.
Detailed Description
Example 1
In this example, a two-dimensional nonmetal sulfur-doped hexagonal boron nitride nanosheet (S-BNNS) photocatalyst is prepared as follows:
(1) preparing H-BNNS nanosheets by batch stripping with a rotary ultrasonic stripping method, and obtaining H0-BNNS through hydroxylation.
(2) 0.1 g of HO-BNNS is placed in a post-heating zone of a CVD tube furnace, and 1g of sulfur powder is used as a sulfur source and is placed in a pre-heating zone.
(3) Heating to 300 ℃ in a preposed heating zone to obtain sublimed sulfur.
(4) In the post-reaction zone, the sulfur rising and HO-BNNS react at the high temperature of 600 ℃ in the protective atmosphere of argon for 0.5 h.
(5) And finally, characterizing the product by means of a scanning electron microscope, a Fourier transform infrared spectrum and the like.
Example 2
The present group of examples includes 9 embodiments, and differs from example 1 in that the dosage of HO-BNNS in step (2) is changed to 0.2g, 0.3g, 0.4g, 0.5g, 0.6g, 0.7g, 0.8g, 0.9g, 1g, respectively, and the dosage ratio of HO-BNNS to S is ensured to be 1: 10.
Example 3
This example is different from example 1 in that the temperature of the preheating zone in step (3) was changed from 300 ℃ to 200 ℃.
Example 4
This example is different from example 1 in that the temperature of the preheating zone in step (3) was changed from 300 ℃ to 400 ℃.
Example 5
This example is different from example 1 in that in step (4), the post-reaction temperature was changed to 700 ℃.
Example 6
This example is different from example 1 in that in step (4), the post-reaction temperature was changed to 800 ℃.
Example 7
The difference between this example and example 1 is that in step (4), the protective atmosphere was changed from argon to nitrogen or ammonia.
Example 8
This example differs from example 1 in that the reaction time of the sulfur uptake and HO-BNNS in step (4) is 1 h.
Example 9
This example differs from example 1 in that the reaction time of the sulphur hydride with HO-BNNS in step (4) is 1.5 h.
Claims (3)
1. A preparation method of sulfur-doped boron nitride nanosheets comprises the following steps:
(1) preparing an activated boron nitride nanosheet:
preparing hexagonal boron nitride nanosheets in batches by a rotary ultrasonic stripping preparation method, and obtaining active boron nitride nanosheets through hydroxylation;
(2) preparing sulfur-doped boron nitride nanosheets:
adopting a double-heat-source vacuum tube furnace, and under the protective atmosphere, mixing sulfur powder with the HO-BNNS obtained in the step (1) according to the mass ratio of 1: 1-100:1, respectively arranged in a front heating zone and a rear heating zone of the tubular furnace, wherein the temperature of the front heating zone is set to 200-.
2. The method of producing sulfur-doped boron nitride nanosheets of claim 1, wherein the protective atmosphere is one of argon, nitrogen or ammonia.
3. The method for preparing sulfur-doped boron nitride nanosheets of claim 1, wherein the method is used in boron nitride ceramic artwork, such that it has a photocatalytic function.
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| CN103910345A (en) * | 2014-03-24 | 2014-07-09 | 中国科学院深圳先进技术研究院 | Preparation method of boron nitride composite material |
| CN104591181A (en) * | 2015-02-13 | 2015-05-06 | 山东大学 | Method for preparing two-dimensional composite material by utilizing nanosheet layer peeling |
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| CN103910345A (en) * | 2014-03-24 | 2014-07-09 | 中国科学院深圳先进技术研究院 | Preparation method of boron nitride composite material |
| CN104591181A (en) * | 2015-02-13 | 2015-05-06 | 山东大学 | Method for preparing two-dimensional composite material by utilizing nanosheet layer peeling |
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