CN114751388A - Porous boron nitride and preparation method thereof, nano gold boron nitride composite photocatalyst and preparation method and application thereof - Google Patents
Porous boron nitride and preparation method thereof, nano gold boron nitride composite photocatalyst and preparation method and application thereof Download PDFInfo
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 116
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- OPEKUPPJGIMIDT-UHFFFAOYSA-N boron gold Chemical compound [B].[Au] OPEKUPPJGIMIDT-UHFFFAOYSA-N 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000001354 calcination Methods 0.000 claims abstract description 21
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 20
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 20
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004327 boric acid Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 14
- 239000010431 corundum Substances 0.000 claims abstract description 14
- 230000001699 photocatalysis Effects 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 61
- 239000010931 gold Substances 0.000 claims description 37
- 229910052737 gold Inorganic materials 0.000 claims description 37
- 239000001509 sodium citrate Substances 0.000 claims description 36
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 36
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 32
- 239000011734 sodium Substances 0.000 claims description 32
- 229910052708 sodium Inorganic materials 0.000 claims description 32
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims description 26
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 10
- 238000006722 reduction reaction Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052724 xenon Inorganic materials 0.000 claims description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 238000006479 redox reaction Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002135 nanosheet Substances 0.000 abstract description 22
- 239000011148 porous material Substances 0.000 abstract description 11
- 239000012299 nitrogen atmosphere Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000010531 catalytic reduction reaction Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 5
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000004847 absorption spectroscopy Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- -1 boron nitride modified carbon nitride Chemical class 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 229960000789 guanidine hydrochloride Drugs 0.000 description 1
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229960003903 oxygen Drugs 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 231100001239 persistent pollutant Toxicity 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000010936 titanium Substances 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
- 238000012546 transfer Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
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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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- B01J35/39—
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
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- A—HUMAN NECESSITIES
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- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
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- C02F2101/345—Phenols
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to the field of photocatalytic composite materials, and particularly relates to porous boron nitride and a preparation method thereof, a nano gold boron nitride composite photocatalyst and a preparation method and application thereof. Mixing melamine, boric acid and water, heating in a water bath to fully dissolve the melamine, preserving heat in a water bath at the temperature of 75-85 ℃ for 4-8 hours, naturally cooling the obtained solution to room temperature, standing overnight, performing suction filtration and drying to obtain a boron nitride precursor; and placing the boron nitride precursor in a corundum boat, then placing the corundum boat in a tubular furnace, and calcining at constant temperature in the nitrogen atmosphere to obtain the porous boron nitride. The invention provides a porous hexagonal boron nitride nanosheet with rich pore channels and large specific surface area, and the specific surface area of the porous hexagonal boron nitride nanosheet can reach 1000m2More than g and simple preparation method.
Description
The application is a divisional application of an invention patent with the application date of 2019, 06, 14 and the application number of CN201910513102.6, namely a preparation method of a visible light response composite photocatalyst of nano-gold loaded porous hexagonal boron nitride and application thereof.
Technical Field
The invention belongs to the field of photocatalytic composite materials, and particularly relates to a porous boron nitride nanosheet and a preparation method thereof, a nanogold/boron nitride composite photocatalyst and a preparation method and application thereof.
Background
In recent years, with the development of modernization, the progress of industry, agriculture and urbanization is accelerated, and the environmental pollution, especially the pollution to water resources, is increasingly serious. Most dyes, even at very low concentrations in water, pose serious hazards to humans and aquatic ecosystems. The p-nitrophenol (4-NP) has higher solubility and stability in water, can be accumulated in the deep layer of soil, has long retention time in the water and the soil, and is one of the most difficult to treat important pollutants. Compared with 4-NP, the p-aminophenol (4-AP) is easier to biodegrade in the environment and has small harm to the environment. In addition, the 4-NP is a fine chemical engineering and medicine intermediate with wider application. Therefore, the conversion of organic pollutant 4-NP into important organic intermediate 4-AP by using a new technology with low energy consumption has become a hot problem in the fields of environmental management and new material research and development.
The photocatalytic material can be used for catalytic reduction and degradation of organic pollutants by fully utilizing solar energy. The photocatalysis technology has the outstanding advantages of high efficiency, simple and convenient operation, mild reaction conditions, no secondary pollution and the like, and simultaneously solves two important problems of treating environmental pollution and relieving energy shortage. Therefore, the preparation of high-performance photocatalyst has great research significance.
The porous hexagonal boron nitride has unique physical and chemical properties, including high specific surface area, many structural defects, low density, high thermal conductivity, good chemical stability and oxidation resistance and the like, so that the porous hexagonal boron nitride has a wide application field, and has a wide application prospect in the aspects of solving energy problems, environmental pollution and the like.
And mixing the hexagonal boron nitride with the graphite-phase carbon nitride precursor, and calcining the mixture precursor to obtain the hexagonal boron nitride modified graphite-phase carbon nitride composite photocatalyst. The composite photocatalyst is used for degrading dye wastewater [ CN 106732727A ].
The preparation method comprises the steps of preparing boron nitride by taking urea and boric acid as raw materials in the voyage of river-sea university and the like, converting blocky carbon nitride into layered carbon nitride, doping the boron nitride into the carbon nitride through ultrasonic assistance, and finally calcining to obtain the boron nitride modified carbon nitride photocatalyst. The photocatalyst can be used for degrading persistent pollutants in water and organic matters such as dyes [ CN 106140242A ].
Ying Chen et al of the university of deacon uses boron trioxide and guanidine hydrochloride as raw materials to prepare porous boron nitride by a dynamic template method, and further prepares porous boron nitride/titanium dioxide (BN/TiO) with novel active bonding matter B-O-Ti by a solvothermal synthesis method2) And (3) compounding nano sheets. The porous BN/TiO2High optical activity of hybrid nanosheet for catalytic degradation of harmful dye (rhodamine B) under visible light99% [ Dan Liu, Mingwen Zhang, Wanjie Xie, Lu Sun, Ying Chen, Weiwei Lei. Port BN/TiO2hybrid nanosheets as highly efficientvisible-light-driven photocatalysts.Applied Catalysis B:Environmental,2017,207.]。
The ultrafine porous g-C is prepared by template-free surface prepolymerization etching method in Yannan university, such as Yanghui3N4(UPCN) and a simple hydrothermal method to prepare Boron Nitride Quantum Dots (BNQDs), and then ultrasonically mixing the two in an ethanol solution to prepare a metal-free BNQD/UPCN9(BU) photocatalyst, which has excellent photocatalytic activity for OTC-HCl degradation [ YangYang, Chen Zhuang, Danlian Huang, Guangming Zeng, Jinhui Huang, Cui Lai, Chengyun Zhou, Wenjun Wang, Hai Guo, Wenjing Xue, Rui Deng, Min Cheng, Weiping Xiong3N4:Intensified excitondissociation and charge transfer for promoting visible-light-driven molecularoxygen activation.Applied Catalysis B:Environmental,2019,245.]。
Hexagon of Beijing Industrial university etc. takes magnesium oxide doped hexagonal boron nitride (MgO-h-BN) nano material as a carrier of palladium, adopts a deposition reduction method to prepare Pd/MgO-h-BN composite material, and the composite photocatalyst has better catalytic activity to CO oxidation reaction [ Lingcong Li, Xiaojun Liu, Hong He, Ningqiiang Zhang, Ziwen Liu, Guizhen Zhang. A novel twoo-dimensional MgO-h-BN nano material supported catalyst for CO oxidation reaction. catalysis Today,2019,332 ].
The technical problems of the above research are as follows: (1) the preparation method is complex; (2) the prepared boron nitride has smaller specific surface area.
Disclosure of Invention
The invention aims to solve the technical problem of providing porous boron nitride and a preparation method thereof, and a nanogold porous boron nitride composite photocatalyst and a preparation method and application thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the invention provides a preparation method of porous boron nitride, which comprises the following steps:
mixing melamine, boric acid and water, heating in a water bath to fully dissolve the melamine, preserving heat in a water bath at the temperature of 75-85 ℃ for 4-8 h, naturally cooling the obtained solution to room temperature, standing overnight, performing suction filtration and drying to obtain a boron nitride precursor;
placing the boron nitride precursor in a corundum boat, then placing the corundum boat in a tubular furnace, and calcining at constant temperature in the atmosphere of nitrogen to obtain the porous boron nitride;
the constant-temperature calcination process comprises the following steps: heating to 300 ℃ by a program of 2 ℃/min, and carrying out first constant-temperature calcination treatment for 1 h; heating to 1100 ℃ by a program of 2 ℃/min, and carrying out second constant-temperature calcination treatment for 2 h; then the temperature is raised to 1460 ℃ by the program of 5 ℃/min, and the third constant temperature calcination treatment is carried out for 4 h.
Preferably, the molar ratio of melamine, boric acid and water is 1:2: 3.
Preferably, the water bath heating temperature is 90-100 ℃; and standing overnight for 12-24 hours.
Preferably, the flow rate of the nitrogen is 50-200 Sccm.
The invention also provides the porous boron nitride prepared by the preparation method in the technical scheme; the specific surface area of the porous boron nitride is 1028.9m2/g。
The invention also provides a preparation method of the nano-gold/porous boron nitride composite photocatalyst, which comprises the following steps:
preparing equal volumes of 0.25mM sodium chloroaurate solution and 0.75mM sodium citrate solution; the mass ratio of the sodium chloroaurate in the sodium chloroaurate solution to the sodium citrate in the sodium citrate solution is 1: 3;
uniformly mixing porous boron nitride and the sodium citrate solution, and stirring in a water bath kettle at 60 ℃ to obtain a mixed solution;
dropping the sodium chloroaurate solution into the mixed solution at a constant speed, stirring at a constant temperature for 2-4 h, filtering, and drying to obtain the nanogold/porous boron nitride composite photocatalyst;
the porous boron nitride is the porous boron nitride in the technical scheme.
Preferably, the constant speed is 3-10 s/drop.
The invention also provides the nanogold/porous boron nitride composite photocatalyst prepared by the preparation method in the technical scheme, and the nanogold/porous boron nitride composite photocatalyst comprises nanogold and porous boron nitride; the mass ratio of the nano gold to the porous boron nitride is 1/1000-1/50.
The invention also provides application of the nanogold/porous boron nitride composite photocatalyst in the technical scheme in photocatalytic reduction of p-nitrophenol.
Preferably, the photocatalytic reduction of p-nitrophenol comprises the following steps: mixing p-nitrophenol and NaBH4Placing deionized water in a container, adding the nano-gold/porous boron nitride composite photocatalyst under the condition of continuous stirring, and irradiating by using a 300W xenon lamp with a 400nm optical filter as a visible light source to perform oxidation-reduction reaction;
the p-nitrophenol and NaBH4The mass ratio of the nano-gold/porous boron nitride composite photocatalyst to the deionized water is 0.125:0.472:0.01: 100.
The invention has the advantages that:
the invention provides porous boron nitride with rich and ordered pore passages and large specific surface area, and the specific surface area can reach 1000m2More than g and simple preparation method.
The invention also provides a nano-gold porous boron nitride composite photocatalyst, nano-gold particles with narrow particle size distribution are uniformly dispersed on the surface and in the pore channels of porous boron nitride, the prepared composite photocatalyst has the capability of efficiently reducing nitro pollutants under the response of visible light, and the reaction rate is up to 1.02min-1And has good application prospect.
Drawings
FIG. 1 is a UV-VIS absorption spectrum of a photocatalytic reduction 4-NP solution of example 1 of the present invention;
FIG. 2 is an SEM photograph of the composite photocatalyst of example 1 of the present invention;
FIG. 3 is a TEM image of the composite photocatalyst of example 1 of the present invention.
Detailed Description
The following describes the present invention in detail.
Example 1
Mixing melamine, boric acid and water in a molar ratio of 1:2:3, weighing 18.92g of melamine and 18.55g of boric acid, sequentially adding into 800mL of distilled water, heating in a water bath to 98 ℃, stirring at a constant temperature until the melamine and the boric acid are completely dissolved, keeping the temperature at 80 ℃ for 6h, naturally cooling to room temperature, standing overnight for 12h, performing suction filtration, and fully drying at 60 ℃ to obtain a white fibrous porous boron nitride precursor; weighing 4g of prepared boron nitride precursor, placing the precursor in a corundum boat, placing the corundum boat in a tube furnace, and reacting in a reaction environment with nitrogen2And (3) heating to 1050 ℃ at a programmed temperature of 5 ℃/min under the atmosphere of 50Sccm flow, and calcining at constant temperature for 4h to obtain the porous hexagonal boron nitride nanosheet.
Weighing 0.0249g of sodium chloroaurate, dissolving, placing into a 25mL brown volumetric flask, and performing constant volume to obtain a sodium chloroaurate solution with the concentration of 2.5 mM; 0.0551g of sodium citrate is weighed and placed in a 25mL volumetric flask, and the volume is fixed to obtain a sodium citrate solution with the concentration of 7.5mM, so that the mass ratio of the sodium chloroaurate to the sodium citrate is 1: 3. Respectively transferring 4mL of solution from the prepared sodium chloroaurate and sodium citrate solution into a 25mL volumetric flask to obtain 0.4mM sodium chloroaurate solution and 1.2mM sodium citrate solution at constant volume, weighing 0.2g of porous hexagonal boron nitride nanosheet and 25mL of sodium citrate solution, ultrasonically dispersing for 20min to uniformly mix the porous hexagonal boron nitride nanosheet and the 25mL of sodium citrate solution, placing the mixed solution into a water bath at 60 ℃, dropwise adding the sodium chloroaurate solution into the mixed solution at a dropping speed of 5 s/drop, continuing keeping the temperature for 2h after the dropwise adding is finished, filtering and washing the obtained solution, and drying at 60 ℃ to obtain the nano-gold/porous boron nitride composite nano-photocatalyst with the mass concentration of 1 wt.% of nano-gold.
The prepared 1 wt.% nano-gold/porous boron nitride composite nano-photocatalyst is used for carrying out a photocatalytic reduction experiment, and 1.25mM 4-NP and 0.125M NaBH are added4In a beaker, 100mg/L of prepared 1 wt.% nano-gold/porous boron nitride was added thereto under continuous stirringA composite nano photocatalyst. A300W xenon lamp with a 400nm filter is used as a visible light source. During the irradiation, 1mL of the reaction solution was taken out of the beaker every 1min, diluted 25-fold, and the change in the absorption peak of 4-NP in the catalytic reduction reaction was characterized by ultraviolet-visible absorption spectroscopy (UV-vis).
The boron nitride prepared by the condition has rich pore channel structure, and the specific surface area of the boron nitride can reach 941.9m2And/g, the nanogold is uniformly dispersed on the surface and in the pore channel of the porous hexagonal boron nitride nanosheet in a spherical shape, and the average particle size of the nanogold is about 20 nm. The prepared nano gold/porous boron nitride composite nano photocatalyst is used for reducing p-nitrophenol, and the reaction rate is up to 0.260min after the nano gold/porous boron nitride composite nano photocatalyst is obtained through testing-1。
Example 2
Mixing melamine, boric acid and water in a molar ratio of 1:2:3, weighing 18.92g of melamine and 18.55g of boric acid, sequentially adding into 800mL of distilled water, heating in a water bath to 98 ℃, stirring at a constant temperature until the melamine and the boric acid are completely dissolved, keeping the temperature at 80 ℃ for 6h, naturally cooling to room temperature, standing overnight for 24h, performing suction filtration, and fully drying at 70 ℃ to obtain a white fibrous porous boron nitride precursor; weighing 4g of prepared boron nitride precursor, placing the precursor in a corundum boat, placing the corundum boat in a tube furnace, and reacting in a reaction environment with nitrogen2And (3) heating to 1050 ℃ at a programmed temperature of 5 ℃/min under the atmosphere of 100Sccm flow, and calcining at constant temperature for 4h to obtain the porous hexagonal boron nitride nanosheet.
Weighing 0.0249g of sodium chloroaurate, dissolving and placing in a 25mL brown volumetric flask, and performing constant volume to obtain a sodium chloroaurate solution with the concentration of 2.5 mM; 0.0551g of sodium citrate is weighed and placed in a 25mL volumetric flask, and the volume is fixed to obtain a sodium citrate solution with the concentration of 7.5mM, so that the mass ratio of the sodium chloroaurate to the sodium citrate is 1: 3. And respectively transferring 4mL of solution from the prepared sodium chloroaurate solution and sodium citrate solution into a 25mL volumetric flask to obtain 0.4mM sodium chloroaurate solution and 1.2mM sodium citrate solution with constant volume, weighing 0.2g of porous hexagonal boron nitride nanosheet and 25mL of sodium citrate solution, ultrasonically dispersing for 20min to uniformly mix the porous hexagonal boron nitride nanosheet and the 25mL of sodium citrate solution, placing the mixed solution into a water bath at 60 ℃, dropwise adding the sodium chloroaurate solution into the mixed solution at a dropping speed of 5 s/drop, continuing to keep the temperature for 2h after the dropwise adding is finished, filtering and washing the obtained solution, and drying at 60 ℃ to obtain the nano-gold/porous boron nitride composite nano-photocatalyst with the mass concentration of 1 wt.% of nano-gold.
The prepared 1 wt.% nano-gold/porous boron nitride composite nano-photocatalyst is used for carrying out a photocatalytic reduction experiment, and 1.25mM 4-NP and 0.125M NaBH are added4In a beaker, 1 wt.% of the prepared nano-gold/porous boron nitride composite nano-photocatalyst was added thereto under continuous stirring. A300W xenon lamp with a 400nm filter is used as a visible light source. During the irradiation, 1mL of the reaction solution was removed from the beaker at 1min intervals, diluted 25-fold and characterized by ultraviolet-visible absorption spectroscopy (UV-vis) for the change in the absorption peak of 4-NP in the catalytic reduction reaction.
The boron nitride prepared by the condition has rich pore channel structure, and the specific surface area of the boron nitride can reach 812m2The nano gold is uniformly dispersed on the surface and in the pore channels of the porous hexagonal boron nitride nano sheet in a spherical shape, and the specific surface area of the nano gold can reach 536m2Per gram, its average particle size is about 20 nm. The prepared nano gold/porous boron nitride composite nano photocatalyst is used for reducing p-nitrophenol, and the reaction rate is up to 2.19min after the nano gold/porous boron nitride composite nano photocatalyst is tested-1。
Example 3
Mixing melamine, boric acid and water in a molar ratio of 1:2:3, weighing 18.92g of melamine and 18.55g of boric acid, sequentially adding into 800mL of distilled water, heating in a water bath to 98 ℃, stirring at a constant temperature until the melamine and the boric acid are completely dissolved, keeping the temperature at 80 ℃ for 6h, naturally cooling to room temperature, standing overnight for 18h, performing suction filtration, and fully drying at 60 ℃ to obtain a white fibrous porous boron nitride precursor; weighing 4g of prepared boron nitride precursor, placing the precursor in a corundum boat, placing the corundum boat in a tube furnace, and reacting in a reaction environment with nitrogen2And under the atmosphere of 50Sccm of flow, raising the temperature to 300 ℃ by a program of 2 ℃/min, carrying out constant-temperature calcination treatment for 1h, raising the temperature to 1100 ℃ by a program of 2 ℃/min, and carrying out constant-temperature calcination treatment for 2 h. And then raising the temperature to 1460 ℃ by a program of 5 ℃/min, and carrying out constant-temperature calcination treatment for 4h to obtain the porous hexagonal boron nitride nanosheet.
Weighing 0.0249g of sodium chloroaurate, dissolving and placing in a 25mL brown volumetric flask, and performing constant volume to obtain a sodium chloroaurate solution with the concentration of 2.5 mM; 0.0551g of sodium citrate is weighed and placed in a 25mL volumetric flask, and the volume is fixed to obtain a sodium citrate solution with the concentration of 7.5mM, so that the mass ratio of the sodium chloroaurate to the sodium citrate is 1: 3. Respectively transferring 0.8mL of solution from the prepared sodium chloroaurate and sodium citrate solution into a 25mL volumetric flask to perform constant volume to obtain 0.08mM sodium chloroaurate solution and 0.24mM sodium citrate solution, weighing 0.2g of porous hexagonal boron nitride nanosheet and 25mL of sodium citrate solution, performing ultrasonic dispersion for 20min to uniformly mix the porous hexagonal boron nitride nanosheet and the 25mL of sodium citrate solution, placing the mixed solution into a water bath at 60 ℃, dropwise adding the sodium chloroaurate solution into the mixed solution at a dropping speed of 5 s/drop, continuing to perform constant temperature for 2h after the dropwise addition is completed, filtering and washing the obtained solution, and drying at 60 ℃ to obtain the nano-gold/porous boron nitride composite nano photocatalyst with the nano-gold mass concentration of 0.2 wt.%.
The prepared nano gold/porous boron nitride composite nano photocatalyst of 0.2 wt.% is used for carrying out a photocatalytic reduction experiment, and 1.25mM of 4-NP and 0.125M of NaBH are added4In a beaker, 100mg/L of the prepared 1 wt.% nano-gold/porous boron nitride composite nano-photocatalyst was added thereto under continuous stirring. A300W xenon lamp with a 400nm filter is used as a visible light source. During the irradiation, 1mL of the reaction solution was taken out of the beaker every 1min, diluted 25-fold, and the change in the absorption peak of 4-NP in the catalytic reduction reaction was characterized by ultraviolet-visible absorption spectroscopy (UV-vis).
The boron nitride prepared by the condition has rich pore channel structure, and the specific surface area of the boron nitride can reach 1028.9m2The nano gold is uniformly dispersed on the surface and in the pore channels of the porous hexagonal boron nitride nano sheet in a spherical shape, and the specific surface area of the nano gold can reach 568m2(iv)/g, having an average particle diameter of about 20 nm. The prepared nano gold/porous boron nitride composite nano photocatalyst is used for reducing p-nitrophenol, and the reaction rate is up to 0.45min after the nano gold/porous boron nitride composite nano photocatalyst is tested-1。
Example 4
Mixing melamine, boric acid and water in a molar ratio of 1:2:3, weighing 18.92g of melamine and 18.55g of boric acid, sequentially adding into 800mL of distilled water, heating in a water bath to 98 ℃, stirring at constant temperature until the melamine and the boric acid are completely dissolvedPreserving heat at 80 ℃ for 6h, naturally cooling to room temperature, keeping the temperature overnight for 15h, performing suction filtration, and fully drying at 60 ℃ to obtain a white fibrous porous boron nitride precursor; weighing 4g of prepared boron nitride precursor, placing the precursor in a corundum boat, placing the corundum boat in a tube furnace, and reacting in a reaction environment with nitrogen2And under the atmosphere of 50Sccm of flow, raising the temperature to 300 ℃ by a program of 2 ℃/min, carrying out constant-temperature calcination treatment for 1h, raising the temperature to 1100 ℃ by a program of 2 ℃/min, and carrying out constant-temperature calcination treatment for 2 h. And then, raising the temperature to 1460 ℃ by a program of 5 ℃/min, and carrying out constant-temperature calcination treatment for 4 hours to obtain the porous hexagonal boron nitride nanosheet.
Weighing 0.0249g of sodium chloroaurate, dissolving and placing in a 25mL brown volumetric flask, and performing constant volume to obtain a sodium chloroaurate solution with the concentration of 2.5 mM; 0.0551g of sodium citrate is weighed and placed in a 25mL volumetric flask, and the volume is fixed to obtain a sodium citrate solution with the concentration of 7.5mM, so that the mass ratio of the sodium chloroaurate to the sodium citrate is 1: 3. Respectively transferring 4mL of solution from the prepared sodium chloroaurate and sodium citrate solution into a 25mL volumetric flask to obtain 0.4mM sodium chloroaurate solution and 1.2mM sodium citrate solution at constant volume, weighing 0.2g of porous hexagonal boron nitride nanosheet and 25mL of sodium citrate solution, ultrasonically dispersing for 20min to uniformly mix the porous hexagonal boron nitride nanosheet and the 25mL of sodium citrate solution, placing the mixed solution into a water bath at 60 ℃, dropwise adding the sodium chloroaurate solution into the mixed solution at a dropping speed of 5 s/drop, continuing keeping the temperature for 2h after the dropwise adding is finished, filtering and washing the obtained solution, and drying at 60 ℃ to obtain the nano-gold/porous boron nitride composite nano-photocatalyst with the mass concentration of 1.0 wt.% of nano-gold.
The prepared 1.0 wt.% nano-gold/porous boron nitride composite nano-photocatalyst is used for carrying out a photocatalytic reduction experiment, and 1.25mM 4-NP and 0.125M NaBH are added4In a beaker, 100mg/L of the prepared 1 wt.% nanogold/boron nitride composite photocatalyst was added thereto under continuous stirring. A300W xenon lamp with a 400nm filter is used as a visible light source. During the irradiation, 1mL of the reaction solution was taken out of the beaker every 1min, diluted 25-fold, and the change in the absorption peak of 4-NP in the catalytic reduction reaction was characterized by ultraviolet-visible absorption spectroscopy (UV-vis).
The boron nitride prepared by the condition has rich pore channel structure, and the specific surface area of the boron nitride can reach 1028.9m2The nano gold is uniformly dispersed on the surface and in pore channels of the porous hexagonal boron nitride nanosheet in a spherical shape, and the specific surface area of the nano gold can reach 696m2(iv)/g, having an average particle diameter of about 20 nm. The prepared nano gold/porous boron nitride composite nano photocatalyst is used for reducing p-nitrophenol, and the reaction rate is up to 1.02min after the nano gold/porous boron nitride composite nano photocatalyst is tested-1。
Although the above embodiments have been described in detail, they are only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (10)
1. A preparation method of porous boron nitride is characterized by comprising the following steps:
mixing melamine, boric acid and water, heating in a water bath to fully dissolve the melamine, preserving heat in a water bath at 75-85 ℃ for 4-8 h, naturally cooling the obtained solution to room temperature, standing overnight, performing suction filtration and drying to obtain a porous boron nitride precursor;
placing the porous boron nitride precursor in a corundum boat, then placing the corundum boat in a tubular furnace, and calcining at constant temperature in the atmosphere of nitrogen to obtain the porous boron nitride;
the constant-temperature calcination process comprises the following steps: heating to 300 ℃ by a program of 2 ℃/min, and carrying out first constant-temperature calcination treatment for 1 h; heating to 1100 ℃ by a program of 2 ℃/min, and carrying out second constant-temperature calcination treatment for 2 h; then the temperature is raised to 1460 ℃ by the program of 5 ℃/min, and the third constant temperature calcination treatment is carried out for 4 h.
2. The process according to claim 1, characterized in that the molar ratio of melamine, boric acid and water is 1:2: 3.
3. The preparation method of claim 1, wherein the temperature of the water bath heating is 90-100 ℃; and standing overnight for 12-24 hours.
4. The method according to claim 1, wherein the flow rate of the nitrogen gas is 50 to 200 Sccm.
5. Porous boron nitride produced by the production method according to any one of claims 1 to 4; the specific surface area of the porous boron nitride is 1028.9m2/g。
6. A preparation method of a nano gold boron nitride composite photocatalyst is characterized by comprising the following steps:
preparing equal volumes of 0.25mM sodium chloroaurate solution and 0.75mM sodium citrate solution; the mass ratio of the sodium chloroaurate in the sodium chloroaurate solution to the sodium citrate in the sodium citrate solution is 1: 3;
uniformly mixing porous boron nitride and the sodium citrate solution, and stirring in a 60 ℃ water bath to obtain a mixed solution;
dropping the sodium chloroaurate solution into the mixed solution at a constant speed, stirring at a constant temperature for 2-4 h, filtering, and drying to obtain the nano gold boron nitride composite photocatalyst;
the porous boron nitride of claim 5.
7. The method of claim 6, wherein the constant speed is 3 to 10 s/drop.
8. The nanogold boron nitride composite photocatalyst prepared by the preparation method of claim 6 or 7, which is characterized by comprising nanogold and porous boron nitride; the mass ratio of the nano gold to the porous boron nitride is 1/1000-1/50.
9. The application of the nanogold boron nitride composite photocatalyst disclosed by claim 8 in photocatalytic reduction of p-nitrophenol.
10. Use according to claim 9, wherein the photocatalytic reduction of p-nitrophenol comprisesThe method comprises the following steps: mixing p-nitrophenol and NaBH4Placing deionized water in a container, adding the nano gold boron nitride composite photocatalyst under the condition of continuous stirring, and irradiating by using a 300W xenon lamp with a 400nm optical filter as a visible light source to perform oxidation-reduction reaction;
the p-nitrophenol and NaBH4The mass ratio of the nano gold boron nitride composite photocatalyst to the deionized water is 0.125:0.472:0.01: 100.
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