CN113198453A - Lamellar Bi2O2SiO3-Si2Bi24O40Heterogeneous composite photocatalyst and preparation method thereof - Google Patents
Lamellar Bi2O2SiO3-Si2Bi24O40Heterogeneous composite photocatalyst and preparation method thereof Download PDFInfo
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- CN113198453A CN113198453A CN202110552269.0A CN202110552269A CN113198453A CN 113198453 A CN113198453 A CN 113198453A CN 202110552269 A CN202110552269 A CN 202110552269A CN 113198453 A CN113198453 A CN 113198453A
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- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 8
- 239000010935 stainless steel Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims abstract description 5
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- -1 silicon ions Chemical class 0.000 claims description 8
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910001451 bismuth ion Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 18
- 239000004793 Polystyrene Substances 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 229920002223 polystyrene Polymers 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract description 6
- 239000003607 modifier Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 abstract description 2
- 239000004005 microsphere Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- PHIQPXBZDGYJOG-UHFFFAOYSA-N sodium silicate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-][Si]([O-])=O PHIQPXBZDGYJOG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 229910052797 bismuth Inorganic materials 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910020489 SiO3 Inorganic materials 0.000 description 3
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229960004106 citric acid Drugs 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 208000012868 Overgrowth Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a lamellar Bi2O2SiO3‑Si2Bi24O40A heterogeneous composite photocatalyst and a preparation method thereof. Bismuth nitrate pentahydrate and sodium metasilicate nonahydrate are used as raw materials, absolute ethyl alcohol and deionized water are used as solvents, citric acid, Ethylene Glycol (EG), polyethylene glycol 400, polyethylene glycol 6000 and the like are used as dispersing agents, polystyrene microspheres (PS) are used as modifiers, and the mixture is reacted in a stainless steel closed high-pressure kettle for 8 to 15 hours, so that the lamellar Bi with more active sites is prepared2O2SiO3‑Si2Bi24O40A heterogeneous composite photocatalyst. The method is simple to operate, the prepared powder has uniform particle size distribution and good dispersibility, the obtained composite material not only has the function of a new heterostructure, but also has a smaller and thinner lamellar structure, provides more active sites and shows higher photocatalytic performance.
Description
Technical Field
The invention belongs to the technical field of photocatalysts, and particularly relates to lamellar Bi2O2SiO3-Si2Bi24O40A heterogeneous composite photocatalyst and a preparation method thereof.
Background
The bismuth-based semiconductor generally has good photocatalytic performance, has wide visible light response range and good physical and chemical stability due to the appropriate forbidden band width and the special layered structure, and is a great research hotspot in the field of photocatalysis. However, the problems of easy electron-hole recombination and narrow response wavelength range still exist, and further improvement and solution are needed.
The narrow forbidden band width can improve the utilization rate of sunlight, and the wide forbidden band width can inhibit the recombination of photon-generated carriers. Therefore, it is difficult for a single semiconductor photocatalytic material to simultaneously have excellent light absorption capability and higher photogenerated carrier separation and transfer efficiency.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a sheet-shaped heterogeneous composite photocatalyst and a preparation method thereof, the contradiction is solved by constructing a heterojunction, the obtained composite photocatalyst has uniform particle size distribution, a smaller and thinner sheet-shaped structure and more active sites, the structure can effectively improve the utilization rate of light and the photocatalytic activity, and the preparation process is simple.
In order to achieve the purpose, the invention adopts the technical scheme that:
a lamellar heterogeneous composite photocatalyst with Bi as expression2O2SiO3-Si2Bi24O40The structure is a three-dimensional cross-type lamellar structure consisting of sheets with the thickness of about 15-25 nm and the side length of not more than 1.5 mu m. Compared with the thick plate before modification, the modified plate has a smaller and thinner microstructure; the three-dimensional crossed lamellar structure provides more active sites and improves the photocatalytic activity of the photocatalyst.
The preparation method of the lamellar heterogeneous composite photocatalyst comprises the following steps:
step 1, adding a dispersing agent into a bismuth nitrate solution to obtain a solution A, and taking a sodium metasilicate solution as a solution B, wherein the molar ratio of silicon ions to bismuth ions is 1: 1-1.5: 1;
step 2, slowly dripping the solution B into the solution A, continuously stirring, uniformly mixing, and then adding the PS suspension to obtain a precursor solution;
step 3, keeping the precursor solution in a stainless steel closed high-pressure kettle with a polytetrafluoroethylene lining at the temperature of 150-250 ℃ for 8-15 hours, and naturally cooling to room temperature;
step 4, collecting and centrifuging the obtained product, washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, then drying the product at the temperature of between 60 and 80 ℃, and grinding the product to obtain the lamellar Bi2O2SiO3-Si2Bi24O40A heterogeneous composite photocatalyst.
The mass concentration of the bismuth nitrate solution is 60-80%, and the concentration of the dispersing agent in the solution A is controlled to be 0.3-1.2 mol/L.
The dispersing agent is one or more of citric acid, EG, polyethylene glycol 400 and polyethylene glycol 6000, and when the dispersing agent is multiple, the proportion is random.
The mass concentration of the sodium metasilicate solution is 20-50%.
The addition amount of the PS suspension is 20-80% of the total volume of the solution B and the solution A, and the PS suspension serves as a modifier.
The filling ratio of the precursor solution in a stainless steel closed high-pressure kettle is 46-70%.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with other types of heterojunction, the bismuth-based/bismuth-based semiconductor heterojunction can solve the problem of difficult carrier transmission caused by lattice distortion of a heterojunction interface, and the heterojunction formed between two bismuth-based semiconductors can share [ Bi2O2]2+Unit of layered structure, which favors charges in [ Bi ]2O2]2+The transmission in the layer is transferred, so that the photocatalytic performance of the bismuth semiconductor is improved.
2. Effectively utilize Bi2O2SiO3With Si2Bi24O40Similar structure and matching energy bands, passing throughPolymerization reaction, homogeneous reaction, hydrothermal reaction, etc. to form new Bi2O2SiO3-Si2Bi24O40A heterojunction.
3. The utilization rate of sunlight is improved while the recombination rate of photo-generated electrons and holes is reduced.
4. The PS suspension is added to generate steric hindrance effect in a hydrothermal environment, so that overgrowth of crystal grains is effectively controlled, an original thick plate is changed into a smaller and thinner lamellar shape, more active sites are exposed, and the photocatalytic performance of the composite material is further improved.
5. Under the action of visible light, Bi2O2SiO3Electron generated in the electron donor will transit to Si2Bi24O40On the conduction band of (2), reacts with surface oxygen to generate superoxide radical (. O)2-) At the same time, Si2Bi24O40Upper hole (h)+) Will migrate to Bi2O2SiO3The superoxide radical and the cavity in the system are main catalytic degradation active groups of the system, namely, the generated superoxide radical reacts with the cavity and pollutants to complete degradation reaction.
6. The preparation process is simple, the prepared powder has uniform particle size distribution and lighter agglomeration, and the photocatalytic activity is enhanced by the synergistic effect of the heterojunction interface and the layered structure.
Drawings
FIG. 1 is an XRD pattern of the powder prepared by the present invention.
FIG. 2 is an SEM image of the powder prepared by the present invention.
FIG. 3 is a graph showing the pollutant degradation performance of the powder prepared by the present invention.
Detailed Description
The method uses bismuth nitrate pentahydrate and sodium metasilicate nonahydrate as raw materials, absolute ethyl alcohol and deionized water as solvents, citric acid, Ethylene Glycol (EG), polyethylene glycol 400, polyethylene glycol 6000 and the like as dispersing agents, polystyrene microspheres (PS) as modifiers, the raw materials and the deionized water are mixed and then react in a stainless steel closed high-pressure kettle for 8 to 15 hours, and the mixture is subjected to reactionSo as to prepare lamellar Bi with more active sites2O2SiO3-Si2Bi24O40A heterogeneous composite photocatalyst. The method is simple to operate, the prepared powder has good dispersibility, the obtained composite material not only has the function of a new heterostructure, but also has a smaller and thinner lamellar structure, provides more active sites and shows higher photocatalytic performance.
The embodiments of the present invention will be described in detail below with reference to the drawings and examples. The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
Example 1
(1) Mixing styrene, alpha-methacrylic acid and deionized water, taking potassium persulfate as an initiator, stirring at a constant temperature of 60-80 ℃, and carrying out polymerization reaction for 6-10 hours. Centrifuging and washing after the reaction is finished, and finally dissolving in absolute ethyl alcohol to obtain a Polystyrene (PS) suspension;
(2) preparing a bismuth nitrate solution with the mass percentage of 60-80%, adding a certain amount of dispersant in the stirring process, and stirring until the dispersant is dissolved to obtain a solution A;
(3) slowly dripping 20-50% of sodium metasilicate solution (the molar ratio of silicon ions to bismuth ions is 1: 1-1: 1.5) in percentage by mass into the solution A, and continuously stirring. After mixing evenly, adding 12mL of PS suspension to obtain a precursor solution;
(4) keeping the precursor solution in a stainless steel closed high-pressure kettle with a polytetrafluoroethylene lining at the temperature of 150-250 ℃ for 8-15 hours, and naturally cooling to room temperature;
(5) and collecting and centrifuging the obtained product, washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, drying the product at the temperature of between 60 and 80 ℃, and grinding the product to obtain the lamellar heterogeneous composite photocatalyst.
Example 2
(1) Mixing styrene, alpha-methacrylic acid and deionized water, taking potassium persulfate as an initiator, stirring at a constant temperature of 60-80 ℃, and carrying out polymerization reaction for 6-10 hours. Centrifuging and washing after the reaction is finished, and finally dissolving in absolute ethyl alcohol to obtain a Polystyrene (PS) suspension;
(2) preparing a bismuth nitrate solution with the mass percentage of 60-80%, adding a certain amount of dispersing agents (including citric acid, EG, polyethylene glycol 400, polyethylene glycol 6000 and the like, controlling the concentration of each dispersing agent to be 0.3-1.2 mol/L) in the stirring process, and stirring until the dispersing agents are dissolved to obtain a solution A;
(3) slowly dripping 20-50% of sodium metasilicate solution (the molar ratio of silicon ions to bismuth ions is 1: 1-1: 1.5) in percentage by mass into the solution A, and continuously stirring. After uniform mixing, adding 16mL of PS suspension to obtain a precursor solution;
(4) keeping the precursor solution in a stainless steel closed high-pressure kettle with a polytetrafluoroethylene lining at the temperature of 150-250 ℃ for 8-15 hours, and naturally cooling to room temperature;
(5) collecting and centrifuging the obtained product, washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, drying the product at the temperature of between 60 and 80 ℃, and grinding the product to obtain the lamellar Bi2O2SiO3-Si2Bi24O40A heterogeneous composite photocatalyst.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, substitutions, combinations, simplifications, etc. made based on the principle or spirit of the present invention should be considered as equivalent replacements within the protection scope of the present invention.
Claims (7)
1. Lamellar Bi2O2SiO3-Si2Bi24O40A heterogeneous composite photocatalyst and a preparation method thereof, wherein the expression is Bi2O2SiO3-Si2Bi24O40The structure is a three-dimensional cross-type lamellar structure consisting of sheets with the thickness of about 15-25 nm and the side length of not more than 1.5 mu m.
2. The lamellar Bi of claim 12O2SiO3-Si2Bi24O40Preparation of heterogeneous composite photocatalystThe method is characterized by comprising the following steps:
step 1, adding a dispersing agent into a bismuth nitrate solution to obtain a solution A, and taking a sodium metasilicate solution as a solution B, wherein the molar ratio of silicon ions to bismuth ions is 1: 1-1.5: 1;
step 2, slowly dripping the solution B into the solution A, continuously stirring, uniformly mixing, and then adding the PS suspension to obtain a precursor solution;
step 3, keeping the precursor solution in a stainless steel closed high-pressure kettle with a polytetrafluoroethylene lining at the temperature of 150-250 ℃ for 8-15 hours, and naturally cooling to room temperature;
step 4, collecting and centrifuging the obtained product, washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, then drying the product at the temperature of between 60 and 80 ℃, and grinding the product to obtain the lamellar Bi2O2SiO3-Si2Bi24O40A heterogeneous composite photocatalyst.
3. The preparation method according to claim 2, wherein the mass concentration of the bismuth nitrate solution is 60 to 80%, and the concentration of the dispersant in the solution A is controlled to be 0.3 to 1.2 mol/L.
4. The preparation method according to claim 2 or 3, wherein the dispersant is one or more of citric acid, EG, polyethylene glycol 400 and polyethylene glycol 6000, and when the dispersant is more than one, the proportion is arbitrary.
5. The preparation method according to claim 2, wherein the mass percent of the sodium metasilicate solution is 20-50%.
6. The method according to claim 2, wherein the PS suspension is added in an amount of 20 to 80% of the total volume of the solutions B and A.
7. The preparation method according to claim 2, wherein the filling ratio of the precursor solution in the stainless steel closed autoclave is 46-70%.
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