CN105597754A - Preparation method of Ag-rGO-BiVO4 compound photocatalyst - Google Patents
Preparation method of Ag-rGO-BiVO4 compound photocatalyst Download PDFInfo
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- 229910002915 BiVO4 Inorganic materials 0.000 title claims abstract description 42
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 150000001875 compounds Chemical class 0.000 title abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 26
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract 3
- 239000000243 solution Substances 0.000 description 48
- 239000000523 sample Substances 0.000 description 20
- 229910002651 NO3 Inorganic materials 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 9
- 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 8
- 239000000126 substance Substances 0.000 description 8
- 229940043267 rhodamine b Drugs 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000005286 illumination Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 101710134784 Agnoprotein Proteins 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000009938 salting Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 229910016331 Bi—Ag Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- WDVGLADRSBQDDY-UHFFFAOYSA-N holmium(3+);trinitrate Chemical compound [Ho+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O WDVGLADRSBQDDY-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229940100890 silver compound Drugs 0.000 description 1
- 150000003379 silver compounds Chemical class 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/682—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium, tantalum or polonium
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention discloses a preparation method of an Ag-rGO-BiVO4 compound photocatalyst. Ag nanoparticles and reduced oxidized graphene are utilized to conduct visible light modification on a BiVO4 photocatalyst, and Ag-BiVO4 micron-grade spheres are synthesized by adopting a one-step hydrothermal method and are supported on the oxidized graphene. According to the preparation method, the reduced oxidized graphene and the Ag nanoparticles are utilized to conduct modification on BiVO4, electrons on the BiVO4 are transferred to the reduced oxidized graphene through the supported Ag nanoparticles to enable absorption edge of the BiVO4 to produce red shift, electron and hole separation is achieved under visible light irradiation, the quantum utilization efficiency is improved, and catalytic activity is strengthened. The average particle size of the synthesized Ag-BiVO4 micron-grade spheres is 5-8 microns, and the micro-spherical catalyst particles are more beneficial to the transfer of the electrons.
Description
Technical field
The invention belongs to field of functional materials, be specifically related to a kind of Ag-rGO-BiVO4The preparation of three's composite photo-catalystMethod.
Background technology
Conductor photocatalysis sewage purification technology be take full advantage of the special valence band structure of semi-conducting material and develop onePlant Novel sewage treatment technology. Between the conduction band of semi-conducting material and valence band, have a forbidden band, when the energy of illumination photons largeIn the time of the energy of energy gap, the Electron absorption photon in Semiconductor Powder valence band, transits to conduction band (e－), in valence bandLeave hole (h+), forming electron-hole pair, electronics has reproducibility, and hole has oxidisability. Oxidation on conduction band-reduction potential is more negative, and semi-conductive reducing power is stronger; Oxidation-reduction potential in valence band more just, semi-conductive oxygenChange ability is stronger. In common semiconductor, SnO2Oxidability the strongest, the reducing power of SiC is the strongest, TiO2The strongest with the redox integration capability of ZnO, but ZnO is unstable, and photochemical corrosion easily occurs, and TiO2Can only inhaleReceive ultraviolet light, this just makes ZnO, TiO2Application be restricted. The BiVO of monoclinic form is found in research recently4ToolHave the ability of visible light catalytic decomposition water and degradable organic pollutant, its band gap is about 2.4eV, works as BiVO4Photocatalysis grainAfter being subject to being greater than the photon illumination of 2.4eV energy, there is light-catalyzed reaction, O in son2 －Energy and the reaction of most organic matter, by itOxidation Decomposition becomes CO2And H2O, and the oxidability of OH is stronger, can be oxidized most organic pollutants, BiVO simultaneously4The highly active e of particle surface－There is very strong reducing power, can be by heavy metal ion, the organic dirt of some poisonous difficult degradationsDye thing reduction, thereby reduce its toxicity.
As the patent documentation that publication number is CN103464137B, a kind of multiform looks Ho/BiVO is disclosed4Composite photocatalystThe preparation method of agent, the method respectively by five water bismuth nitrates and ammonium metavanadate soluble in water bismuth salting liquid and vanadic salts solution,Be that 1:1 mixes vanadic salts solution with bismuth salting liquid by Bi with the mol ratio of V, regulate pH of mixed to 8, then add sixWater holmium nitrate, the mol ratio of Ho and Bi is (2.04～13.64): 100, use microwave-hydrothermal method to exist with the power of 300W180 DEG C of insulation 40min prepare Ho/BiVO4. The multiform looks Ho/BiVO that the method is synthetic4Composite photo-catalyst hasHigher photocatalytic activity, can be applied to degraded environmental contaminants.
Summary of the invention
The object of this invention is to provide a kind of Ag-rGO-BiVO4The preparation method of three's composite photo-catalyst, the party's legal systemThe Ag-rGO-BiVO obtaining4Three's composite photo-catalyst is compared to existing BiVO4Photochemical catalyst, photocatalysis performance is better,And preparation technology is simple.
Concrete technical scheme of the present invention is: a kind of Ag-rGO-BiVO4The preparation method of three's composite photo-catalyst, bagDraw together following steps:
(1) by Bi (NO3)3·5H2O is dissolved in salpeter solution, stirs and obtains solution A; By NH4VO3Be dissolved inIn sodium hydroxide solution, stir and obtain solution B, described Bi (NO3)3·5H2O and NH4VO3Mol ratio be 1:1;
(2) graphene oxide is added water ultrasonic dispersion obtains solution C; By AgNO3Be dissolved in ethylene glycol and obtain solution D;
(3) solution A and solution B are mixed evenly, regulate after pH to 7.0, add solution C and solution D simultaneously,After mixing, mixed liquor is carried out ultrasonic;
(4) mixed liquor after ultrasonic is transferred to and in hydrothermal reaction kettle, carries out hydro-thermal reaction;
(5) reacted mixed liquor is cooled to room temperature, collects the precipitation generating, precipitation cleans, dry after and get final productAg-rGO-BiVO4Three's composite photo-catalyst.
The present invention utilizes Graphene and nanometer Ag load to BiVO4Carry out modification, BiVO4Electronics is above by loadNanometer Ag particle pass to graphene oxide, make the ABSORPTION EDGE red shift of BiVO4, make on the one hand the hole-electricity of materialSub-recombination rate reduces, thereby improves BiVO4Quantum efficiency; Can produce surface etc. adding of nanometer Ag on the other handIon resonance effect, thus make the catalyst obtaining absorb more visible ray. In the photochemical catalyst that the present invention makes, alsoIt is membranaceous that former graphene oxide is the thin transparent of dispersion, Ag-BiVO4The average grain diameter of microspheroidal, between 5～8 μ m, is receivedThe load capacity of rice Ag is 0.1～0.2g/gBiVO4, the load capacity of Graphene is 0.0005～0.00125g/gBiVO4。
As preferably, described step (1) salpeter solution concentration is 1～5mol/L, and concentration of sodium hydroxide solution is 1～5mol/L.
As preferably, the quality of described step (2) graphene oxide is Bi (NO3)3·5H20.5%～2% of O quality,Because graphene oxide is difficult to disperse, when use, after first adding appropriate water ultrasonic wave to disperse, then add reaction.
As preferably, described step (2) AgNO3Quality be Bi (NO3)3·5H213%～35% of O quality, AgNO3First dissolve with appropriate ethylene glycol before use.
As preferably, described step (4) hydrothermal reaction condition is 190～210 DEG C, and the reaction time is 16～20h.
The invention has the beneficial effects as follows: the present invention is at BiVO4Area load redox graphene and nanometer Ag, BiVO4Electronics above passes to redox graphene by the nanometer Ag particle of load, makes BiVO4ABSORPTION EDGE red shift,Realize electronics under radiation of visible light, hole separation, improve quantum utilization ratio, increase photocatalytic activity; Nanometer simultaneouslyAdding of Ag can produce surface plasma resonance effect, thereby makes the catalyst obtaining absorb more visible ray, entersOne step strengthens photocatalytic activity; The catalyst that the present invention makes is microspheroidal, is conducive to the transmission of electronics.
Brief description of the drawings
Fig. 1 is the XRD figure of the sample prepared of embodiment 1;
Fig. 2 is that sample prepared by embodiment 1 amplifies the SEM figure of 2000 times under 10 μ m;
Fig. 3 is that sample prepared by embodiment 1 amplifies the SEM figure of 40,000 times under 100nm;
Fig. 4 is the XPS figure of the sample prepared of embodiment 1;
Fig. 5 is the XPS figure of loaded Ag in the sample prepared of embodiment 1;
Fig. 6 is the sample prepared of embodiment 1 and embodiment 2 and the curve map of other photocatalyst for degrading rhodamine Bs.
Detailed description of the invention
Below by specific embodiment, technical scheme of the present invention is described further.
If not raw material of the present invention and equipment refer in particular to, all can buy from market or this area is conventional, embodimentIn method, if no special instructions, be the conventional method of this area.
Embodiment 1
A kind of Ag-rGO-BiVO4The preparation method of three's composite photo-catalyst, comprises the following steps:
(1) by the Bi (NO of 10mmol3)3·5H2O (4.851g) is dissolved in the salpeter solution that 50mL concentration is 2mol/LIn, stir 30min and obtain solution A; By the NH of 10mmol4VO3(1.170g) being dissolved in 50mL concentration is 2mol/LSodium hydroxide solution in, stir 30min obtain solution B;
(2) taking quality is Bi (NO3)3·5H2The graphene oxide (48.51mg) of O quality 1%, adds 15mL water and entersThe ultrasonic dispersion 1h of row, obtains solution C; Taking quality is Bi (NO3)3·5H2The AgNO of O quality 13%3(0.63g)Be dissolved in 10mL ethylene glycol and obtain solution D;
(3) solution A and solution B are mixed evenly, with after buffer solution adjusting pH to 7.0, add solution C simultaneouslyAnd solution D, mixed liquor is carried out to ultrasonic 1h;
(4) mixed liquor after ultrasonic is transferred in hydrothermal reaction kettle, at 200 DEG C, reacts 18h;
(5) reacted mixed liquor is cooled to room temperature, collects the precipitation generating, precipitation is used respectively distilled water, ethanolWashing, obtains Ag-rGO-BiVO after freeze drying4Three's composite photo-catalyst.
The Ag-rGO-BiVO that the present embodiment makes4Three's composite photo-catalyst, the load capacity of nanometer Ag is0.1248g/gBiVO4, the load capacity of redox graphene is 0.001g/gBiVO4。
Embodiment 2
A kind of Ag-rGO-BiVO4The preparation method of three's composite photo-catalyst, comprises the following steps:
(1) by the Bi (NO of 10mmol3)3·5H2O (4.851g) is dissolved in the salpeter solution that 50mL concentration is 4mol/LIn, stir 30min and obtain solution A; By the NH of 10mmol4VO3(1.170g) being dissolved in 80mL concentration is 1mol/LSodium hydroxide solution in, stir 30min obtain solution B;
(2) taking quality is Bi (NO3)3·5H2The graphene oxide (24.255mg) of O quality 0.5%, adds 10mL waterCarry out ultrasonic dispersion 1h, obtain solution C; Taking quality is Bi (NO3)3·5H2The AgNO of O quality 20%3(0.97g)Be dissolved in 15mL ethylene glycol and obtain solution D;
(3) solution A and solution B are mixed evenly, with after buffer solution adjusting pH to 7.0, add solution C simultaneouslyAnd solution D, mixed liquor is carried out to ultrasonic 1h;
(4) mixed liquor after ultrasonic is transferred in hydrothermal reaction kettle, at 200 DEG C, reacts 18h;
(5) reacted mixed liquor is cooled to room temperature, collects the precipitation generating, precipitation is used respectively distilled water, ethanolWashing, obtains Ag-rGO-BiVO after freeze drying4Three's composite photo-catalyst.
The Ag-rGO-BiVO that the present embodiment makes4Three's composite photo-catalyst, the load capacity of nanometer Ag is0.192g/gBiVO4, the load capacity of redox graphene is 0.0075g/gBiVO4。
Embodiment 3
A kind of Ag-rGO-BiVO4The preparation method of three's composite photo-catalyst, comprises the following steps:
(1) by the Bi (NO of 10mmol3)3·5H2O (4.851g) is dissolved in the salpeter solution that 50mL concentration is 2mol/LIn, stir 30min and obtain solution A; By the NH of 10mmol4VO3(1.170g) being dissolved in 50mL concentration is 2mol/LSodium hydroxide solution in, stir 30min obtain solution B;
(2) taking quality is Bi (NO3)3·5H2The graphene oxide (60.638mg) of O quality 1.25%, adds 25mLWater carries out ultrasonic dispersion 1h, obtains solution C; Taking quality is Bi (NO3)3·5H2The AgNO of O quality 35%3(1.70g)Be dissolved in 30mL ethylene glycol and obtain solution D;
(3) solution A and solution B are mixed evenly, with after buffer solution adjusting pH to 7.0, add solution C simultaneouslyAnd solution D, mixed liquor is carried out to ultrasonic 1h;
(4) mixed liquor after ultrasonic is transferred in hydrothermal reaction kettle, at 200 DEG C, reacts 18h;
(5) reacted mixed liquor is cooled to room temperature, collects the precipitation generating, precipitation is used respectively distilled water, ethanolWashing, obtains Ag-rGO-BiVO after freeze drying4Three's composite photo-catalyst.
The Ag-rGO-BiVO that the present embodiment makes4Three's composite photo-catalyst, the load capacity of nanometer Ag is0.3359g/gBiVO4, the load capacity of redox graphene is 0.00187g/gBiVO4。
Fig. 1 is the XRD collection of illustrative plates of the sample that makes of embodiment 1, and as we know from the figure, BiVO4 has complete monoclinic form.BiVO4Mainly containing three kinds of crystal phase structures, is respectively cubic zircon, monocline scheelite and cubic scheelite-type structure, Qi ZhongdanThe tiltedly BiVO of scheelite-type structure4There is good visible light catalytic performance, therefore, after modification, keep monoclinic phase structureFor BiVO4The raising of photocatalysis performance is extremely important. As seen from Figure 1 at 28.60 °, 30.50 °, 35.2 °, 39.7 °And near 53.1 °, there is obvious diffraction maximum, with BiVO4Standard card (JCPDS14-0688) consistent, explanationThe prepared photochemical catalyst sample of this method is monocline scheelite-type structure, and adding of rGO do not cause BiVO4Crystalline phaseTransformation, and after rGO load, the diffraction maximum of sample is sharpened, degree of crystallinity improves. At 38.1 °, 44.3 ° and 64.51 °There is obvious diffraction maximum in position, consistent with the simple substance silver (JCPDS.65-2871) of face-centered cubic crystal face, and we are describedThe standby sample of legal system success load simple substance Ag, simple substance Ag crystal formation can promote BiVO4Leading away of upper electronics, therebyImprove BiVO4The separative efficiency of electron-hole.
Fig. 2 and Fig. 3 are respectively sample prepared by embodiment 1 and under 10 μ m, amplify the SEM figure of 2000 times and transfer at 100nmThe SEM figure of large 40,000 times can see microspheric Ag-BiVO in sample from Fig. 2 and Fig. 34The nano junction of structure, silverStructure and transparent graphene oxide thin layer. BiVO4, simple substance silver compound with redox graphene after, simple substance silver and BiVO4Formation is of a size of the microballoon of 5～8 μ m, and loads on redox graphene lamella, and the thin layer of graphene oxide is conducive toThe transmission of photogenerated charge, and improve the separative efficiency of carrier. In addition can also see that a small amount of nano-Ag particles is (straightFootpath is in 40 nanometer left and right) load on redox graphene, nano-Ag particles can produce surface plasma resonance effect,Be conducive to catalyst and absorb more visible ray.
Fig. 4 is the XPS collection of illustrative plates of the sample prepared of embodiment 1, and Fig. 5 is the XPS of Ag in the sample prepared of embodiment 1Collection of illustrative plates, from Fig. 4 and Fig. 5, Ag-rGO-BiVO prepared by this method4In three's composite photo-catalyst, loadAg is the simple substance silver of zeroth order, because the simple substance silver of zeroth order can promote BiVO4Leading away of upper electronics, thus BiVO improved4The separative efficiency of electron-hole.
Fig. 6 is the curve map of the photocatalyst for degrading rhodamine B of the sample prepared of the present invention and control sample thereof. In figureBi uses pure BiVO4Carry out photocatalytic degradation, Bi-Ag is for using BiVO4The compound photocatalytic degradation that carries out of-Ag,Bi-rGO is for using BiVO4The compound photocatalytic degradation that carries out of-rGo, AgBG-0.5 is the sample that uses embodiment 1 to prepareCarry out photocatalytic degradation, AgBG-1 is that the sample that uses embodiment 2 to prepare carries out photocatalytic degradation; C0For rhodamine B(dark reaction 30 minutes is that the absorption in order to reach between catalyst and organic matter is put down to the concentration of solution dark reaction after 30 minutesWeighing apparatus), CtFor rhodamine B solution concentration after illumination t hour.
As can be seen from the figure: along with the increase of time, under visible ray shines, rhodamine B is rapid in the absorption of 552nmDecline, and do not add the rhodamine B solution of catalyst that light degradation does not almost occur. Therefore, only have when illumination andRhodamine B degradation effectively when catalyst exists simultaneously, the degradation and decolorization that rhodamine B solution has also been described be byUnder visible ray illumination, occur in sample that light-catalyzed reaction just produces. Prepared by embodiment 1 and embodiment 2BiVO4-rGO-Ag photocatalytic activity is all higher than pure BiVO4, BiVO4-Ag and BiVO4-rGO sample, this be byCan promote electronics transmission and effectively promote the separation of photo-generated carrier in rGO, simple substance Ag can produce plasma resonance effect,While also can promote electronics transmission and effectively promote the separation of photo-generated carrier, urge therefore can significantly improve the light of BiVO4Change active. Along with the increase of rGO content, the photocatalytic activity of compound does not strengthen, and this is because too much rGOThe complex centre that can form electronics and hole, can not effectively participate in light-catalyzed reaction light induced electron and hole, therefore mistakeThe rGO of high-load can make photocatalytic activity decline, and the strongest containing the sample activity of 0.5%GO. Through the degraded of 10h,The clearance of rhodamine B reaches 82%.
Claims (5)
1. an Ag-rGO-BiVO4The preparation method of three's composite photo-catalyst, is characterized in that, comprises the following steps:
(1) by Bi (NO3)3·5H2O is dissolved in salpeter solution, stirs and obtains solution A; By NH4VO3Be dissolved inIn sodium hydroxide solution, stir and obtain solution B, described Bi (NO3)3·5H2O and NH4VO3Mol ratio be1:1；
(2) graphene oxide is added water ultrasonic dispersion obtains solution C; By AgNO3Be dissolved in ethylene glycol and obtain solution D;
(3) solution A and solution B are mixed evenly, regulate after pH to 7.0, add solution C and solution D simultaneously,After mixing, then mixed liquor is carried out ultrasonic;
(4) mixed liquor after ultrasonic is transferred to and in hydrothermal reaction kettle, carries out hydro-thermal reaction;
(5) reacted mixed liquor is cooled to room temperature, collects the precipitation generating, precipitation cleans, dry after and get final productAg-rGO-BiVO4Three's composite photo-catalyst.
2. a kind of Ag-rGO-BiVO according to claim 14The preparation method of three's composite photo-catalyst, its spyLevy and be, described step (1) salpeter solution concentration is 1～5mol/L, and concentration of sodium hydroxide solution is 1～5mol/L.
3. a kind of Ag-rGO-BiVO according to claim 14The preparation method of three's composite photo-catalyst, its spyLevy and be, the quality of described step (2) graphene oxide is Bi (NO3)3·5H20.5%～2% of O quality.
4. a kind of Ag-rGO-BiVO according to claim 14The preparation method of three's composite photo-catalyst, its spyLevy and be, described step (2) AgNO3Quality be Bi (NO3)3·5H213%～35% of O quality.
5. a kind of Ag-rGO-BiVO according to claim 14The preparation method of three's composite photo-catalyst, its spyLevy and be, described step (4) hydrothermal reaction condition is 190～210 DEG C, and the reaction time is 16～20h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106006929A (en) * | 2016-06-17 | 2016-10-12 | 大连理工大学 | Method for all-weather sewage treatment through coupling of photoelectrocatalysis membrane and microbial fuel cell |
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| CN107497450A (en) * | 2017-09-25 | 2017-12-22 | 辽宁大学 | A kind of compound bismuth tantalate photochemical catalyst and its preparation method and application |
| CN113559841A (en) * | 2021-08-12 | 2021-10-29 | 台州学院 | Nano CuO/GO/BiVO4Heterogeneous heterojunction photocatalyst, preparation method and application thereof |
| CN113559841B (en) * | 2021-08-12 | 2023-10-31 | 台州学院 | Nano CuO/GO/BiVO 4 Multiphase heterojunction photocatalyst, preparation method and application thereof |
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