CN113877632B - Preparation method of 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nanoparticles - Google Patents
Preparation method of 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nanoparticles Download PDFInfo
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 54
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 239000011258 core-shell material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 19
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 16
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 29
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000007853 buffer solution Substances 0.000 claims abstract description 19
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000002135 nanosheet Substances 0.000 claims abstract description 13
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 3
- 239000002351 wastewater Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 78
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 239000008367 deionised water Substances 0.000 claims description 34
- 229910021641 deionized water Inorganic materials 0.000 claims description 34
- 239000007864 aqueous solution Substances 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- CWGFSQJQIHRAAE-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol tetrahydrochloride Chemical compound Cl.Cl.Cl.Cl.OCC(N)(CO)CO CWGFSQJQIHRAAE-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- -1 bismuth salt Chemical class 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 239000000872 buffer Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000002064 nanoplatelet Substances 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 230000010355 oscillation Effects 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- 229910052720 vanadium Inorganic materials 0.000 claims description 9
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 150000001621 bismuth Chemical class 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000005580 one pot reaction Methods 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 229920001690 polydopamine Polymers 0.000 description 67
- 239000012456 homogeneous solution Substances 0.000 description 6
- 239000010970 precious metal Substances 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 230000005426 magnetic field effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
-
- B01J35/39—
-
- B01J35/393—
-
- B01J35/396—
-
- B01J35/40—
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a preparation method of a 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nanoparticles, which comprises the following steps: the sodium dodecyl benzene sulfonate is used as a template, and a one-pot hydrothermal method is adopted to prepare the 2D BiVO 4 A nanosheet; will 2D BiVO 4 Adding the nano-sheets into dopamine hydrochloride Tris-HCl buffer solution, separating, washing and drying after reaction to obtain the PDA coated 2D BiVO 4 Composite material with @ PDA core-shell structure, and the BiVO is prepared by the following steps of 4 Adding the @ PDA nano-sheet composite material into a noble metal salt solution, and reducing to obtain the 2D BiVO loaded by noble metal nano-particles 4 Composite material with PDA core-shell structure. The surface of the composite material provided by the invention contains rich hydroxyl groups, and has a greater application potential in the fields of removal of organic pollutants in catalytic wastewater, reduction of heavy metal ions and the like.
Description
Technical Field
The invention belongs to the field of preparation of organic-inorganic nanocomposite materials, and relates to a noble metal nanoparticle-loaded 2D BiVO 4 A preparation method of a PDA core-shell structure composite material.
Background
It is well known that the composition of semiconductor and metal nanoparticles into heterogeneous nanostructures is a common means of improving the photocatalytic quantum efficiency. The unique Surface Plasmon Resonance (SPR) characteristic of metals can widen the absorption spectrum range of semiconductors, and the generated strong magnetic field effect can promote the separation of electron holes of nearby semiconductors. Polydopamine (PDA) is one of the synthesized eumelanin polymers, has global absorption in the ultraviolet-visible-near infrared light region, so that the Polydopamine (PDA) becomes a photo-thermal conversion material with the most potential, is rich in catechol (catechol), amine, imine and other functional groups, and has adhesiveness and reducibility. Riesz et al and other researchers [ j. Phys. Chem. B, 2006, 110, 13985] demonstrated that in the wavelength range of 325-800 nm, all light energy is absorbed by polydopamine in the instrumental range, and more than 99% of the absorbed photon energy is converted non-radiatively to heat within 50 ps. Patent CN106215719A discloses a preparation method of a hybrid membrane containing titanium dioxide/polydopamine functional particles, and the prepared hybrid membrane has good separation performance, self-cleaning performance and performance stability.
If the SPR effect and the photo-thermal conversion effect of the noble metal nano particles and the polydopamine are utilized cooperatively, the enhanced absorption rate and the optical quantum efficiency in the visible-near infrared region are expected to be obtained. At present, only a small amount of research reports are provided for constructing a composite material based on noble metal nano particles and polydopamine co-modification strategies at home and abroad. Therefore, the invention uses noble metal nano particles, two-dimensional bismuth vanadate nano sheets (2D BiVO 4 ) And polydopamine as a structural unit, and designing and assembling noble metal nanoparticle-loaded 2D BiVO 4 Composite material with @ PDA core-shell structure, which greatly improves BiVO 4 Is used in the application range of (a). The technology has the advantages of simple method, energy conservation, green pollution-free property and the like, and no report on the technology exists at present, so that a new road is explored for the development of new materials.
Disclosure of Invention
The invention aims to provide a simple, energy-saving, green and pollution-free method for preparing a 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nanoparticles.
The invention aims at realizing the following steps: a preparation method of a 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nanoparticles is characterized by comprising the following steps of 4 Adding a @ PDA sample into a reaction container, adding deionized water, adjusting the pH of the solution after ultrasonic treatment, and then adding noble metal nano particles according to the following stepsBiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Adding noble metal nano particles=100:0.5-10 into a reaction container, stirring at a constant temperature of 35 ℃, heating to 95 ℃, and adding 4-8 ml 300mM reducing agent sodium borohydride (NaBH) 4 ) Stirring and mixing uniformly at constant temperature to obtain the target product of the BiVO loaded by the noble metal nano particles 4 Composite material with PDA core-shell structure.
More specifically, the specific steps are as follows:
step 1: weigh a certain amount of BiVO 4 Sample @ PDA, dissolved in 250mL deionized water, sonicated, then slowly add the appropriate amount of Na 2 CO 3 The pH value of the aqueous solution is regulated, then the aqueous solution is heated to 35 ℃ by an oil bath, and the aqueous solution is prepared according to BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Noble metal nanoparticle=100:1-10 noble metal salt is added, stirred, heated to 95 ℃, and 4-8 ml of 300mM NaBH is added 4 The solution is reacted for 0.5h with heat preservation;
step 2: cooling the solution obtained in the step 1 to room temperature, separating, washing and drying the obtained product to obtain the target product, namely the BiVO loaded by the noble metal nano particles 4 Composite material with PDA core-shell structure.
More specifically, the noble metal salt in the step 1 is silver nitrate, chloropalladate, chloroauric acid and potassium chloroplatinate.
More specifically, the pH value in the step 1 is 9-10.
More specifically, in the step 1, the ultrasonic time is 1-3 hours.
More specifically, the stirring time in step 1 is 3 hours.
More specifically, after the solid substances are separated in the step 2, deionized water and absolute ethyl alcohol are used for alternately washing, and the target product is obtained after drying.
More specifically, biVO 4 The preparation procedure for @ PDA was as follows:
step A: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and formulated as 10mM Tris-HCl buffer pH=8.5;
and (B) step (B): weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step C: weighing 0.1-0.6 g BiVO 4 B, dissolving the sample in the buffer solution obtained in the step B, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step D: cooling the solution obtained in the step C to room temperature, separating, washing and drying the obtained product to obtain the target product BiVO 4 Composite material with PDA core-shell structure.
More specifically, two-dimensional BiVO 4 The preparation steps of the nano-sheet are as follows:
step a: the molar ratio of bismuth salt to Sodium Dodecyl Benzene Sulfonate (SDBS) is as follows: bismuth salt Sodium Dodecyl Benzene Sulfonate (SDBS) =1:0.72 is dissolved in nitric acid solution to obtain solution A, and the solution A is stirred for 2 hours;
step b: the molar ratio of the vanadium-containing compound to the bismuth salt is as follows: vanadium-containing compounds: bismuth salt=1:1, adding a vanadium-containing compound to an aqueous NaOH solution to obtain solution B;
step c: b, adding the solution B obtained in the step B into the solution A obtained in the step a, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring for 2 hours to obtain a uniform suspension;
step d: adding the solution obtained in the step c into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, maintaining at 160 ℃ for 3 hours, separating, washing and drying the obtained product to obtain the two-dimensional BiVO 4 A nanoplatelet sample.
The invention has the beneficial effects that:
1. the invention realizes 2D BiVO based on noble metal nano particle and polydopamine common modification 4 The surface of the composite material contains rich hydroxyl groups, and has greater application potential in the fields of removal of organic pollutants in catalytic wastewater, reduction of heavy metal ions and the like.
2. The synthesis method provided by the invention is simple to operate, and the material has the advantages of environmental friendliness, degradation of harmful pollutants and the like.
Drawings
FIG. 1 shows the X-ray powder diffraction pattern (XRD) of the product obtained in example 2 of the present invention.
FIG. 2 shows a transmission electron micrograph and a high resolution transmission electron micrograph (TEM and HRTEM) of the product obtained in example 2 of the present invention.
Detailed Description
The invention is illustrated in further detail below in connection with examples.
A preparation method of a 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nano particles,
two-dimensional BiVO 4 The preparation steps of the nano-sheet are as follows:
step a: the molar ratio of bismuth salt to Sodium Dodecyl Benzene Sulfonate (SDBS) is as follows: bismuth salt Sodium Dodecyl Benzene Sulfonate (SDBS) =1:0.72 is dissolved in nitric acid solution to obtain solution A, and the solution A is stirred for 2 hours;
step b: the molar ratio of the vanadium-containing compound to the bismuth salt is as follows: vanadium-containing compounds: bismuth salt=1:1, adding a vanadium-containing compound to an aqueous NaOH solution to obtain solution B;
step c: b, adding the solution B obtained in the step B into the solution A obtained in the step a, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring for 2 hours to obtain a uniform suspension;
step d: adding the solution obtained in the step c into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, maintaining at 160 ℃ for 3 hours, separating, washing and drying the obtained product to obtain the two-dimensional BiVO 4 A nanoplatelet sample.
BiVO 4 The preparation procedure for @ PDA was as follows:
step A: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and formulated as 10mM Tris-HCl buffer pH=8.5;
and (B) step (B): weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step C: weighing 0.1-0.6 g BiVO 4 B, dissolving the sample in the buffer solution obtained in the step B, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step D: cooling the solution obtained in the step C toAfter room temperature, separating, washing and drying the obtained product to obtain the target product BiVO 4 Composite material with PDA core-shell structure.
Weigh a certain amount of BiVO 4 Dissolving a @ PDA sample in 250mL of deionized water, performing ultrasonic treatment for 1-3 hours, and then slowly adding a proper amount of Na 2 CO 3 The pH value of the aqueous solution is regulated to 9-10, then the aqueous solution is heated to 35 ℃ by an oil bath, and the aqueous solution is prepared according to BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Precious metal nanoparticle=100:1-10, adding precious metal salt, wherein the precious metal salt is silver nitrate, chloropalladic acid, chloroauric acid, potassium chloroplatinate, stirring for 3h, heating to 95 ℃, and adding 4-8 ml of 300mM NaBH 4 The solution is reacted for 0.5h with heat preservation; cooling the solution obtained in the step 1 to room temperature, separating the obtained product, alternately washing with deionized water and absolute ethyl alcohol, and drying to obtain the target product, namely the BiVO loaded with the noble metal nano particles 4 Composite material with PDA core-shell structure.
Example 1
Two-dimensional BiVO 4 The preparation steps of the nano-sheet are as follows:
step A: 1mmol of Bi (NO) 3 ) 3 •5H 2 O (0.485, g) and 0.72mmol SDBS (0.250, g) were dissolved in 10mL of 4M nitric acid to give a homogeneous solution;
and (B) step (B): 1mmol of NH 4 VO 3 (0.117, g) in 10mL of 2M aqueous NaOH;
step C: adding the solution obtained in the step B into the solution obtained in the step A, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring to obtain uniform suspension;
step D: adding the solution obtained in the step C into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, keeping at 160 ℃ for 3 hours, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for multiple times, and then drying at 100 ℃ for 8 hours to obtain the two-dimensional BiVO 4 A nanoplatelet sample.
BiVO 4 The preparation method of the composite material with the @ PDA core-shell structure comprises the following steps:
step a: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and prepared as 10mM, pH=8.5 Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) buffer;
step b: weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step c: weigh 0.1 g BiVO 4 C, dissolving the sample in the buffer solution obtained in the step b, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step d: cooling the solution obtained in the step c to room temperature, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for many times, and drying at 60 ℃ for 12 hours to obtain BiVO 4 Composite material with PDA core-shell structure.
Weigh 2g BiVO 4 Sample @ PDA, dissolved in 250mL deionized water, sonicated for 1h, then slowly add the appropriate amount of Na 2 CO 3 The pH value of the aqueous solution is regulated to 9-10, then the aqueous solution is heated to 35 ℃ by an oil bath, and the aqueous solution is prepared according to BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 @ PDA: noble metal nanoparticle = 100:1 0.0315g AgNO was added 3 Stirring for 3h, then heating to 95℃and adding 4ml of 300mM NaBH 4 The solution was reacted for 0.5h with heat preservation. Cooling the obtained solution to room temperature, separating, washing and drying the obtained product to obtain the target product of the BiVO loaded by the noble metal nano particles Ag 4 Composite material with @ PDA core-shell structure (marked as 1% Ag/BiVO) 4 @PDA）。
Example 2
Two-dimensional BiVO 4 The preparation steps of the nano-sheet are as follows:
step A: 1mmol of Bi (NO) 3 ) 3 •5H 2 O (0.485, g) and 0.72mmol SDBS (0.250, g) were dissolved in 10mL of 4M nitric acid to give a homogeneous solution;
and (B) step (B): 1mmol of NH 4 VO 3 (0.117, g) in 10mL of 2M aqueous NaOH;
step C: adding the solution obtained in the step B into the solution obtained in the step A, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring to obtain uniform suspension;
step D: adding the solution obtained in the step C into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, keeping at 160 ℃ for 3 hours, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for multiple times, and then drying at 100 ℃ for 8 hours to obtain the two-dimensional BiVO 4 A nanoplatelet sample.
BiVO 4 The preparation method of the composite material with the @ PDA core-shell structure comprises the following steps:
step a: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and prepared as 10mM, pH=8.5 Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) buffer;
step b: weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step c: weigh 0.1 g BiVO 4 C, dissolving the sample in the buffer solution obtained in the step b, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step d: cooling the solution obtained in the step c to room temperature, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for many times, and drying at 60 ℃ for 12 hours to obtain BiVO 4 Composite material with PDA core-shell structure.
Weigh 2g BiVO 4 Sample @ PDA, dissolved in 250mL deionized water, sonicated for 1h, then slowly add the appropriate amount of Na 2 CO 3 The pH value of the aqueous solution is regulated to 9-10, and then the aqueous solution is heated to 35 ℃ by an oil bath to obtain BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Precious metal nanoparticle=100:1 0.04g chloroauric acid was added and stirred for 3h, then warmed to 95 ℃, 4ml 300mm NaBH was added 4 The solution was reacted for 0.5h with heat preservation. Cooling the obtained solution to room temperature, separating, washing and drying the obtained product to obtain the target product of the BiVO loaded by the noble metal nano particles Au 4 Composite material of @ PDA core-shell structure (marked as 1% Au/BiVO) 4 @ PDA). FIG. 1 is a 1% Au/BiVO synthesized 4 XRD spectrum of @ PDA sample, corresponding to monoclinic scheelite phase BiVO 4 (JCPDS No. 14-0688). FIGS. 2a and 2b are respectively 1% Au/BiVO synthesized in the present example 4 Transmission electron microscope image and height of @ PDA sampleResolving transmission electron microscope images, it can be seen that 2D BiVO 4 The amorphous PDA shell layer is wrapped around, the thickness of the shell layer is 8-16 nm, the average particle diameter of the Au nano-particles is about 42nm, and the interval between crystal faces is 0.26nm in figure 2b corresponds to BiVO 4 The (200) crystal plane of (2) and the (111) crystal plane of Au with the interplanar distance of 0.23 nm.
Example 3
Two-dimensional BiVO 4 The preparation steps of the nano-sheet are as follows:
step A: 1mmol of Bi (NO) 3 ) 3 •5H 2 O (0.485, g) and 0.72mmol SDBS (0.250, g) were dissolved in 10mL of 4M nitric acid to give a homogeneous solution;
and (B) step (B): 1mmol of NH 4 VO 3 (0.117, g) in 10mL of 2M aqueous NaOH;
step C: adding the solution obtained in the step B into the solution obtained in the step A, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring to obtain uniform suspension;
step D: adding the solution obtained in the step C into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, keeping at 160 ℃ for 3 hours, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for multiple times, and then drying at 100 ℃ for 8 hours to obtain the two-dimensional BiVO 4 A nanoplatelet sample.
BiVO 4 The preparation method of the composite material with the @ PDA core-shell structure comprises the following steps:
step a: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and prepared as 10mM, pH=8.5 Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) buffer;
step b: weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step c: weigh 0.1 g BiVO 4 C, dissolving the sample in the buffer solution obtained in the step b, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step d: cooling the solution obtained in the step c to room temperature, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for multiple times, and drying at 60 DEG C12h to obtain BiVO 4 Composite material with PDA core-shell structure.
Weigh 2g BiVO 4 Sample @ PDA, dissolved in 250mL deionized water, sonicated for 1h, then slowly add the appropriate amount of Na 2 CO 3 The pH value of the aqueous solution is regulated to 9-10, and then the aqueous solution is heated to 35 ℃ by an oil bath to obtain BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Precious metal nanoparticle = 100:3 0.12g chloroauric acid was added and stirred for 3h, then warmed to 95 ℃, 4ml 300mm NaBH was added 4 The solution was reacted for 0.5h with heat preservation. Cooling the obtained solution to room temperature, separating, washing and drying the obtained product to obtain the target product of the BiVO loaded by the noble metal nano particles Au 4 Composite material of @ PDA core-shell structure (marked as 3% Au/BiVO) 4 @PDA）。
Example 4
Two-dimensional BiVO 4 The preparation steps of the nano-sheet are as follows:
step A: 1mmol of Bi (NO) 3 ) 3 •5H 2 O (0.485, g) and 0.72mmol SDBS (0.250, g) were dissolved in 10mL of 4M nitric acid to give a homogeneous solution;
and (B) step (B): 1mmol of NH 4 VO 3 (0.117, g) in 10mL of 2M aqueous NaOH;
step C: adding the solution obtained in the step B into the solution obtained in the step A, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring to obtain uniform suspension;
step D: adding the solution obtained in the step C into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, keeping at 160 ℃ for 3 hours, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for multiple times, and then drying at 100 ℃ for 8 hours to obtain the two-dimensional BiVO 4 A nanoplatelet sample.
BiVO 4 The preparation method of the composite material with the @ PDA core-shell structure comprises the following steps:
step a: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and prepared as 10mM, pH=8.5 Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) buffer;
step b: weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step c: weigh 0.1 g BiVO 4 C, dissolving the sample in the buffer solution obtained in the step b, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step d: cooling the solution obtained in the step c to room temperature, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for many times, and drying at 60 ℃ for 12 hours to obtain BiVO 4 Composite material with PDA core-shell structure.
Weigh 2g BiVO 4 Sample @ PDA, dissolved in 250mL deionized water, sonicated for 1h, then slowly add the appropriate amount of Na 2 CO 3 The pH value of the aqueous solution is regulated to 9-10, and then the aqueous solution is heated to 35 ℃ by an oil bath to obtain BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Precious metal nanoparticle = 100:5 0.2g chloroauric acid was added and stirred for 3h, then warmed to 95 ℃, 4ml 300mm NaBH was added 4 The solution was reacted for 0.5h with heat preservation. Cooling the obtained solution to room temperature, separating, washing and drying the obtained product to obtain the target product of the BiVO loaded by the noble metal nano particles Au 4 Composite material of @ PDA core-shell structure (marked as 5% Au/BiVO) 4 @PDA）。
Example 5
Two-dimensional BiVO 4 The preparation steps of the nano-sheet are as follows:
step A: 1mmol of Bi (NO) 3 ) 3 •5H 2 O (0.485, g) and 0.72mmol SDBS (0.250, g) were dissolved in 10mL of 4M nitric acid to give a homogeneous solution;
and (B) step (B): 1mmol of NH 4 VO 3 (0.117, g) in 10mL of 2M aqueous NaOH;
step C: adding the solution obtained in the step B into the solution obtained in the step A, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring to obtain uniform suspension;
step D: adding the solution obtained in the step C into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, maintaining at 160 ℃ for 3h, and using deionized water and anhydrous water to obtain the productEthanol is alternately washed and centrifuged for multiple times, and then dried for 8 hours at 100 ℃ to obtain the two-dimensional BiVO 4 A nanoplatelet sample.
BiVO 4 The preparation method of the composite material with the @ PDA core-shell structure comprises the following steps:
step a: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and prepared as 10mM, pH=8.5 Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) buffer;
step b: weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step c: weigh 0.1 g BiVO 4 C, dissolving the sample in the buffer solution obtained in the step b, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step d: cooling the solution obtained in the step c to room temperature, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for many times, and drying at 60 ℃ for 12 hours to obtain BiVO 4 Composite material with PDA core-shell structure.
Weigh 0.43 g BiVO 4 Sample @ PDA, dissolved in 250mL deionized water, sonicated for 1h, then slowly add the appropriate amount of Na 2 CO 3 The pH value of the aqueous solution is regulated to 9-10, then the aqueous solution is heated to 35 ℃ by an oil bath, and the aqueous solution is prepared according to BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Noble metal nanoparticle=100:1 10ml of 10mM chloropalladate are added and stirred for 3h, then warmed to 95℃and 4ml of 300mM NaBH are added 4 The solution was reacted for 0.5h with heat preservation. Cooling the obtained solution to room temperature, separating, washing and drying the obtained product to obtain the target product of the noble metal nano particle Pd-loaded BiVO 4 Composite material with @ PDA core-shell structure (marked as 1% Pd/BiVO) 4 @PDA）。
Example 6
Two-dimensional BiVO 4 The preparation steps of the nano-sheet are as follows:
step A: 1mmol of Bi (NO) 3 ) 3 •5H 2 O (0.485, g) and 0.72mmol SDBS (0.250, g) were dissolved in 10mL of 4M nitric acid to give a homogeneous solution;
and (B) step (B): 1mmol ofNH 4 VO 3 (0.117, g) in 10mL of 2M aqueous NaOH;
step C: adding the solution obtained in the step B into the solution obtained in the step A, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring to obtain uniform suspension;
step D: adding the solution obtained in the step C into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, keeping at 160 ℃ for 3 hours, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for multiple times, and then drying at 100 ℃ for 8 hours to obtain the two-dimensional BiVO 4 A nanoplatelet sample.
BiVO 4 The preparation method of the composite material with the @ PDA core-shell structure comprises the following steps:
step a: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and prepared as 10mM, pH=8.5 Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) buffer;
step b: weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step c: weigh 0.1 g BiVO 4 C, dissolving the sample in the buffer solution obtained in the step b, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step d: cooling the solution obtained in the step c to room temperature, alternately washing and centrifuging the obtained product with deionized water and absolute ethyl alcohol for many times, and drying at 60 ℃ for 12 hours to obtain BiVO 4 Composite material with PDA core-shell structure.
Weigh 2g BiVO 4 Sample @ PDA, dissolved in 250mL deionized water, sonicated for 1h, then slowly add the appropriate amount of Na 2 CO 3 The pH value of the aqueous solution is regulated to 9-10, then the aqueous solution is heated to 35 ℃ by an oil bath, and the aqueous solution is prepared according to BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Noble metal nanoparticle=100:1 0.05g potassium chloroplatinate was added and stirred for 3h, then warmed to 95℃and 4ml 300mM NaBH were added 4 The solution was reacted for 0.5h with heat preservation. Cooling the obtained solution to room temperature, separating, washing and drying the obtained product to obtain the target product of the BiVO loaded by the noble metal nano particles Pt 4 Composite material with @ PDA core-shell structure (marked as 1% Pt/BiVO) 4 @PDA）。
Although embodiments of the present invention have been described herein, it will be appreciated by those of ordinary skill in the art that changes can be made to the embodiments herein without departing from the spirit of the invention. The above-described embodiments are exemplary only, and should not be taken as limiting the scope of the claims herein.
Claims (9)
1. The preparation method of the 2D bismuth vanadate@PDA core-shell structure composite material loaded by the noble metal nano particles is characterized by comprising the following specific preparation steps:
step 1: weigh a certain amount of BiVO 4 Sample @ PDA, dissolved in deionized water, sonicated, then slowly add the appropriate amount of Na 2 CO 3 The pH value of the aqueous solution is regulated, then the aqueous solution is heated to 35 ℃ by an oil bath, and the aqueous solution is prepared according to BiVO 4 The mass ratio of the @ PDA sample to the noble metal nano particles is as follows: biVO (BiVO) 4 Noble metal nanoparticle=100:1-10 noble metal salt is added, stirred, heated to 95 ℃, and 4-8 ml of 300mM NaBH is added 4 The solution is reacted for 0.5h with heat preservation;
step 2: cooling the solution obtained in the step 1 to room temperature, separating, washing and drying the obtained product to obtain the target product, namely the BiVO loaded by the noble metal nano particles 4 Composite material with PDA core-shell structure.
2. The method for preparing the 2D bismuth vanadate@PDA core-shell structure composite material loaded by the noble metal nanoparticles according to claim 1, wherein the noble metal salt in the step 1 is silver nitrate, chloropalladate, chloroauric acid or potassium chloroplatinate.
3. The method for preparing the 2D bismuth vanadate@PDA core-shell structure composite material loaded by the noble metal nanoparticles according to claim 1, wherein the pH value in the step 1 is 9-10.
4. The method for preparing the 2D bismuth vanadate@PDA core-shell structure composite material loaded by the noble metal nanoparticles according to claim 1, wherein the ultrasonic time in the step 1 is 1-3 h.
5. The method for preparing the 2D bismuth vanadate@PDA core-shell structure composite material loaded by the noble metal nanoparticles according to claim 1, wherein the stirring time in the step 1 is 3h.
6. The method for preparing the 2D bismuth vanadate@PDA core-shell structure composite material loaded by the noble metal nanoparticles according to claim 1, wherein deionized water and absolute ethyl alcohol are used for washing alternately in the step 2.
7. The method for preparing the 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nanoparticles as claimed in claim 1, wherein the method is characterized by BiVO 4 The preparation procedure for @ PDA was as follows:
step A: 30mg of Tris (hydroxymethyl) aminomethane hydrochloride (Tris-HCl) was dissolved in 20ml of deionized water and formulated as 10mM Tris-HCl buffer pH=8.5;
and (B) step (B): weighing 40mg of dopamine hydrochloride powder, adding the dopamine hydrochloride powder into the solution, and performing ultrasonic oscillation to form 2mg/ml of dopamine hydrochloride Tris-HCl buffer solution;
step C: weighing 0.1-0.6 g BiVO 4 B, dissolving the sample in the buffer solution obtained in the step B, placing the sample in an oil bath pot, and stirring at 60 ℃ for 24 hours;
step D: cooling the solution obtained in the step C to room temperature, separating, washing and drying the obtained product to obtain the target product BiVO 4 Composite material with PDA core-shell structure.
8. The method for preparing the 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nanoparticles as claimed in claim 1, wherein the method is characterized by BiVO 4 The preparation steps of the nano-sheet are as follows:
step a: the molar ratio of bismuth salt to Sodium Dodecyl Benzene Sulfonate (SDBS) is as follows: bismuth salt: sodium Dodecyl Benzene Sulfonate (SDBS) =1:0.72 was dissolved in nitric acid solution together to obtain solution a, and stirred for 2h;
step b: the molar ratio of the vanadium-containing compound to the bismuth salt is as follows: vanadium-containing compounds: bismuth salt=1:1, adding a vanadium-containing compound to an aqueous NaOH solution to obtain solution B;
step c: b, adding the solution B obtained in the step B into the solution A obtained in the step a, then slowly adding a proper amount of 2M NaOH aqueous solution, adjusting the pH value to 6.5, and stirring for 2 hours to obtain a uniform suspension;
step d: adding the solution obtained in the step c into a 50mL stainless steel reaction kettle with polytetrafluoroethylene lining, maintaining at 160 ℃ for 3 hours, separating, washing and drying the obtained product to obtain BiVO 4 A nanoplatelet sample.
9. The application of the noble metal nanoparticle-supported 2D bismuth vanadate@PDA core-shell structure composite material prepared by the method of any one of claims 1-8, which is characterized by being used for catalyzing the removal of organic pollutants and the reduction of heavy metal ions in wastewater.
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