CN113788498B - Material with visible light catalytic air purification and antibacterial functions and preparation method thereof - Google Patents
Material with visible light catalytic air purification and antibacterial functions and preparation method thereof Download PDFInfo
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- CN113788498B CN113788498B CN202111064637.3A CN202111064637A CN113788498B CN 113788498 B CN113788498 B CN 113788498B CN 202111064637 A CN202111064637 A CN 202111064637A CN 113788498 B CN113788498 B CN 113788498B
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 31
- 238000004887 air purification Methods 0.000 title claims abstract description 28
- 230000006870 function Effects 0.000 title claims abstract description 28
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 61
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 61
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 15
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 46
- 230000000694 effects Effects 0.000 claims description 33
- 239000004094 surface-active agent Substances 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 23
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 18
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 229910052709 silver Inorganic materials 0.000 claims description 16
- 239000004332 silver Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 14
- 239000007795 chemical reaction product Substances 0.000 claims description 12
- 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 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 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 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 230000003115 biocidal effect Effects 0.000 claims description 4
- 150000001621 bismuth Chemical class 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 22
- 239000013078 crystal Substances 0.000 description 10
- 239000011941 photocatalyst Substances 0.000 description 10
- 238000004090 dissolution Methods 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 8
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 description 7
- -1 modified bismuth tungstate Chemical class 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- JVYLIMILBNDJRH-UHFFFAOYSA-L dichloronickel;tetrahydrate Chemical compound O.O.O.O.Cl[Ni]Cl JVYLIMILBNDJRH-UHFFFAOYSA-L 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/006—Compounds containing, besides tungsten, two or more other elements, with the exception of oxygen or hydrogen
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- 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
- B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
- B01J23/687—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with tungsten
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the technical field of photocatalytic antibacterial materials, and in particular relates to a material with visible light catalytic air purification and antibacterial functions and a preparation method thereof. The method can synthesize the silver-doped nano bismuth tungstate which has uniform particle size, visible light catalytic degradation and high-efficiency durable antibacterial performance in a short time, has a simple process, saves energy, reduces consumption and is easy to realize industrialization.
Description
Technical Field
The invention belongs to the technical field of photocatalytic antibacterial materials, and particularly relates to a material with visible light catalytic air purification and antibacterial functions and a preparation method thereof.
Background
The bismuth-based semiconductor material has a unique electronic structure, and the bismuth-based semiconductor material has a narrower band gap due to the improvement of valence band boundaries caused by the hybridization of the orbitals of Bi6s and O2p, so that the bismuth-based semiconductor material has excellent visible light absorption capacity, has good photocatalytic activity in a visible light region, and can effectively degrade organic pollutants in visible light. In addition, the bismuth semiconductor material has a steep energy band absorption edge in a visible light region, and the absorption of the bismuth semiconductor material to visible light is caused by self band transition instead of the effect of impurity energy level, so that the impurity is effectively prevented from forming a composite center to reduce the photocatalysis efficiency of the bismuth semiconductor material. Wherein bismuth tungstate (Bi 2 WO 6 ) Is an Aurivillius-type oxide having a perovskite-like structure, and is a typical n-type semiconductor. Bi (Bi) 2 WO 6 Is composed of (Bi) 2 O 2 ) 2+ Layer and WO 6 A layered structure comprising perovskite lamellae arranged alternately with each other. Bi (Bi) 2 WO 6 Due to its unique crystal structure, it has thermoelectric, ferroelectric, piezoelectric, oxygen ion conductor, luminescent, nonlinear dielectric induction, catalytic and other properties.
Pure Bi 2 WO 6 The specific surface area is small, the carrier recombination rate is high, and the adsorption efficiency and the photocatalysis efficiency are limited. Therefore, bi was studied and prepared 2 WO 6 Is particularly important. At present, Bi 2 WO 6 The modification method mainly comprises anion doping, cation doping, co-doping, semiconductor compounding and the like, and aims at changing Bi 2 WO 6 The morphology structure and the adsorption performance and the photocatalysis performance of the material are optimized. At present, the morphology of the synthesized bismuth tungstate material mainly comprises flower shapes, sheet shapes, tire shapes and the like, and the particle size is large and the dispersibility is poor. Although the literature has reported the application of bismuth tungstate materials in many technical fields, the bismuth tungstate materials are rarely reported in the antibacterial field.
Patent CN 109894123a discloses a preparation method and application of supported bismuth tungstate photocatalyst, which adopts a two-step method to prepare composite photocatalyst, firstly, bismuth nitrate pentahydrate and sodium tungstate dihydrate are dissolved in water, and the prepared mixed solution is placed in a reaction kettle, and after heating reaction, the mixed solution is centrifuged, washed, dried and ground; fe (NO) is then added to the mill grind 3 ) 3 ·9H 2 O, stirring and reacting at a certain temperature, and then roasting to obtain Fe 2 O 3 /Bi 2 WO 6 A composite photocatalyst; the patent CN 104117355A discloses a nano-silver surface modified bismuth tungstate photocatalyst and a preparation method thereof, and the nano-silver surface modified bismuth tungstate photocatalyst is prepared by adopting a two-step method to prepare a composite photocatalyst, firstly synthesizing bismuth tungstate, then adding silver nitrate, and carrying out reduction deposition on silver ions on the surface of bismuth tungstate under the irradiation of a xenon lamp; CN 106622271A discloses a nickel-doped nano bismuth tungstate visible-light-driven photocatalyst, a preparation method and application thereof, and Ni-Bi is synthesized by a hydrothermal method of sodium tungstate, nickel chloride tetrahydrate and bismuth nitrate for 12-13h 2 WO 6 A photocatalyst; CN 103101977a discloses a bismuth tungstate nano-crystal grain and a preparation method thereof, after respectively dissolving a bismuth source and tungstate, dripping and stirring the bismuth source and the tungstate, then hermetically reacting for 4-72h at high temperature, and then washing and drying to obtain the bismuth tungstate nano-crystal grain. The first two patents adopt a two-step method to synthesize the composite photocatalyst, the process is more complex, the latter two patents have long reaction time and lower efficiency although the one-step method is used for synthesizing, and the two patents have outstanding photocatalytic performance and do not pay attention to the antibacterial performance of the material; the composite photocatalytic material can be applied to products such as antibacterial master batches, antibacterial emulsion paint, antibacterial ceramics and the likeHas high and durable photocatalytic degradation and antibacterial performance.
Disclosure of Invention
Aiming at the singleness of the performances of the photocatalyst synthesized at present and the complexity of the synthesis process, the invention provides the high-activity silver-doped nano bismuth tungstate with the functions of visible light catalytic air purification and antibiosis and the preparation method thereof, and the silver-doped nano bismuth tungstate with uniform particle size, visible light catalytic degradation and high-efficiency durable antibiosis performance can be synthesized in a short time by adding various surfactants into a reaction system, so that the process is simple, energy conservation and consumption reduction are realized, and industrialization is easy to realize. The surfactant can be quickly adsorbed on crystal faces with higher surface energy to prevent aggregation of particles, and reach an equilibrium state through the interaction among electrostatic action, steric hindrance and Van der Waals force to realize the stabilization of the surfactant, so that the growth of the particles can be inhibited to a certain extent, the increase of specific surface area is facilitated due to the reduction of particle aggregation, the active material is enabled to be in more contact with a reaction system, the reaction rate is accelerated, and meanwhile, the material has better antibacterial performance due to the incorporation of silver ions.
The material with the functions of visible light catalytic air purification and antibiosis is high-activity silver doped nano bismuth tungstate, and the high-activity silver doped nano bismuth tungstate is prepared from bismuth salt, silver nitrate and sodium tungstate.
A preparation method of a material with visible light catalytic air purification and antibacterial functions comprises the following steps:
adding bismuth nitrate pentahydrate and silver nitrate into nitric acid, dissolving and then mixing with sodium tungstate solution; sequentially adding a silane coupling agent and a surfactant, fully stirring, and adjusting the pH value of a reaction system to 0.5-2; and (3) carrying out heat preservation reaction for 1.5-2 hours at 180-210 ℃, cooling to room temperature, washing and drying a reaction product, grinding the reaction product into powder, and calcining at 450-520 ℃ to obtain the high-activity silver doped nano bismuth tungstate material.
Further, the usage amount of the silane coupling agent is 0.5-2% of the total mass of the mixed solution.
Further, the silane coupling agent is one or two of gamma-aminopropyl triethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane.
Further, the use amount of the surfactant is 0.5-1.5% of the total mass of the mixed solution.
Further, the surfactant is one or more of polyethylene glycol, cetyltrimethylammonium bromide and polyvinyl alcohol.
Further, HNO is adopted 3 Or NaOH adjusts the pH of the reaction system to 0.5-2.
Further, the reaction product was washed 3 times with absolute ethanol and distilled water by centrifugation, respectively; the collected product was dried at 70-80 ℃ for 12h and then ground into powder.
Further, the concentration of the sodium tungstate is 0.02-0.04 mol/L.
Further, silver nitrate: bismuth nitrate: the molar ratio of the sodium tungstate is (0.1-0.3): 10:5.
the invention provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, which comprises the following steps: adding 2mmol of bismuth nitrate pentahydrate and silver nitrate into 5-8mL of 20% nitric acid, and stirring for dissolution; adding 1mmol of sodium tungstate dihydrate into 30-40mL of distilled water, and stirring for dissolution; mixing the two solutions, and sequentially adding a silane coupling agent accounting for 0.5-2% of the total mass of the mixed solution and a surfactant accounting for 0.5-1.5%, wherein the silane coupling agent is one or a combination of two of gamma-aminopropyl triethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane; the surfactant is one or more of polyethylene glycol, cetyltrimethylammonium bromide and polyvinyl alcohol, and is added with HNO after stirring for 30min 3 Or NaOH adjusts the pH value of the reaction system to be 0.5-2; keeping the temperature at 180-210 ℃ for reaction for 1.5-2 hours, cooling to room temperature, and centrifugally washing the reaction product with absolute ethyl alcohol and distilled water for 3 times respectively; drying the collected product at 70-80 ℃ for 12 hours, grinding the product into powder, and calcining the powder at 450-520 ℃ for 1 hour to obtain the high-activity silver-doped nano bismuth tungstate material. The addition of the silane coupling agent and the surfactant increases the band gap width of the silver doped nano bismuth tungstate and widens the lightThe sensitive range is increased, thus improving the photocatalysis performance, and simultaneously, the silane coupling agent is subjected to self-polycondensation reaction, and the obtained product plays a role of a soft template and induces the regular directional growth of synthetic grains; on the other hand, the dispersing agent can form a film on the surface of the crystal grains to isolate the contact between nano particles, so that the agglomeration of the crystal grains is reduced, the synthesized crystal grains are regular, and the particle size is uniform. The high-activity silver-doped nano bismuth tungstate can be widely applied to the fields of emulsion paint, plastic master batches, electrostatic powder spraying, aldehyde removing agents and the like.
Advantageous effects
According to the invention, silver nitrate is directly added into a reaction system of sodium tungstate and bismuth nitrate, so that the system is fully reacted, silver ions are more easily doped into crystal lattices of bismuth tungstate, the preparation process is simple and easy to control, the reaction time is shorter, the efficiency is improved, the energy consumption is low, and the industrialization is convenient to realize; the prepared silver-doped nano bismuth tungstate material has excellent photocatalytic degradation performance, has higher use value in the field of antibacterial and environment-friendly, and has high-efficiency and lasting antibacterial performance due to the fact that silver element replaces part of bismuth element in bismuth tungstate.
Detailed Description
Example 1
The embodiment provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, which comprises the following steps: 2mmol of bismuth nitrate pentahydrate and silver nitrate are added to 6mL of 20% nitric acid, and stirred for dissolution; adding 1mmol of sodium tungstate dihydrate into 35mL of distilled water, and stirring for dissolution; silver nitrate: bismuth nitrate: the molar ratio of sodium tungstate is 0.2:10:5. mixing the two solutions, and sequentially adding a silane coupling agent and a surfactant, wherein the silane coupling agent is one or a combination of two of gamma-aminopropyl triethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane, and the surfactant accounts for 1% of the total mass of the mixed solution; the surfactant is one or more of polyethylene glycol, cetyltrimethylammonium bromide and polyvinyl alcohol, and is added with HNO after stirring for 30min 3 Or NaOH adjusts the pH value of the reaction system to be 1; the reaction is carried out at 200 ℃ for 1.5h and then cooled toCentrifugally washing the reaction product with absolute ethyl alcohol and distilled water for 3 times at room temperature; and drying the collected product at 80 ℃ for 12 hours, grinding the product into powder, and calcining the powder at 480 ℃ for 1 hour to obtain the high-activity silver-doped nano bismuth tungstate material.
Example 2
The embodiment provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, which comprises the following steps: 2mmol of bismuth nitrate pentahydrate and silver nitrate are added into 5mL of 20% nitric acid, and stirred and dissolved; adding 1mmol of sodium tungstate dihydrate into 38mL of distilled water, and stirring for dissolution; silver nitrate: bismuth nitrate: the molar ratio of sodium tungstate is 0.3:10:5. mixing the two solutions, and sequentially adding a silane coupling agent with the total mass of 0.5 percent and a surfactant with the mass of 1.5 percent into the mixed solution, wherein the silane coupling agent is one or the combination of two of gamma-aminopropyl triethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane; the surfactant is one or more of polyethylene glycol, cetyltrimethylammonium bromide and polyvinyl alcohol, and is added with HNO after stirring for 30min 3 Or NaOH adjusts the pH value of the reaction system to 2; keeping the temperature at 180 ℃ for 2 hours, cooling to room temperature, and centrifugally washing the reaction product with absolute ethyl alcohol and distilled water for 3 times; and drying the collected product at 70 ℃ for 12 hours, grinding the product into powder, and calcining the powder at 520 ℃ for 1 hour to obtain the high-activity silver-doped nano bismuth tungstate material.
Example 3
The embodiment provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, which comprises the following steps: 2mmol of bismuth nitrate pentahydrate and silver nitrate are added into 8mL of 20% nitric acid, and stirred and dissolved; adding 1mmol of sodium tungstate dihydrate into 30mL of distilled water, and stirring for dissolution; silver nitrate: bismuth nitrate: the molar ratio of sodium tungstate is 0.1:10:5. mixing the two solutions, and sequentially adding a silane coupling agent and a surfactant, wherein the silane coupling agent is gamma-aminopropyl triethoxysilane and gamma- (methacryloyloxy) propyl trimethyl, and the surfactant accounts for 2% of the total mass of the mixed solutionOne or a combination of two of the oxysilanes; the surfactant is one or more of polyethylene glycol, cetyltrimethylammonium bromide and polyvinyl alcohol, and is added with HNO after stirring for 30min 3 Or NaOH adjusts the pH of the reaction system to 0.5; keeping the temperature at 210 ℃ for 1.5 hours, cooling to room temperature, and centrifugally washing the reaction product with absolute ethyl alcohol and distilled water for 3 times respectively; and drying the collected product at 75 ℃ for 12 hours, grinding the product into powder, and calcining the powder at 450 ℃ for 1 hour to obtain the high-activity silver-doped nano bismuth tungstate material.
Example 4
The embodiment provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, which comprises the following steps: 2mmol of bismuth nitrate pentahydrate and silver nitrate are added into 7mL of 20% nitric acid, and stirred and dissolved; adding 1mmol of sodium tungstate dihydrate into 40mL of distilled water, and stirring for dissolution; silver nitrate: bismuth nitrate: the molar ratio of sodium tungstate is 0.15:10:5. mixing the two solutions, and sequentially adding a silane coupling agent with the total mass of 1.5% and a surfactant with the mass of 0.8% into the mixed solution, wherein the silane coupling agent is one or a combination of two of gamma-aminopropyl triethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane; the surfactant is one or more of polyethylene glycol, cetyltrimethylammonium bromide and polyvinyl alcohol, and is added with HNO after stirring for 30min 3 Or NaOH adjusts the pH of the reaction system to be 1.5; keeping the temperature at 190 ℃ for 2 hours, cooling to room temperature, and centrifugally washing the reaction product with absolute ethyl alcohol and distilled water for 3 times; and drying the collected product at 75 ℃ for 12 hours, grinding the product into powder, and calcining the powder at 500 ℃ for 1 hour to obtain the high-activity silver-doped nano bismuth tungstate material.
Example 5
The embodiment provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, which comprises the following steps: 2mmol of bismuth nitrate pentahydrate and silver nitrate are added to 6mL of 20% nitric acid, and stirred for dissolution; adding 1mmol of sodium tungstate dihydrate into 32mL of distilled water, and stirring for dissolution;silver nitrate: bismuth nitrate: the molar ratio of sodium tungstate is 0.25:10:5. mixing the two solutions, and sequentially adding a silane coupling agent accounting for 2% of the total mass of the mixed solution and a surfactant accounting for 1.2%, wherein the silane coupling agent is one or a combination of two of gamma-aminopropyl triethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane; the surfactant is one or more of polyethylene glycol, cetyltrimethylammonium bromide and polyvinyl alcohol, and is added with HNO after stirring for 30min 3 Or NaOH adjusts the pH value of the reaction system to 2; keeping the temperature at 185 ℃ for 1.5 hours, cooling to room temperature, and centrifugally washing the reaction product with absolute ethyl alcohol and distilled water for 3 times respectively; and drying the collected product at 80 ℃ for 12 hours, grinding the product into powder, and calcining the powder at 460 ℃ for 1 hour to obtain the high-activity silver-doped nano bismuth tungstate material.
Comparative example 1
The comparative example provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, and other conditions are exactly the same as those of example 1 except that silver nitrate is not adopted in the preparation method.
Comparative example 2
The comparative example provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, except silver nitrate: bismuth nitrate: the molar ratio of sodium tungstate is 0.2:20:5, the other conditions were exactly the same as in example 1.
Comparative example 3
The comparative example provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, except silver nitrate: bismuth nitrate: the molar ratio of sodium tungstate is 0.2:10: except for 2, the other conditions were exactly the same as in example 1.
Comparative example 4
The comparative example provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, and other conditions are exactly the same as those of example 1 except that a silane coupling agent is not adopted in the preparation method.
Comparative example 5
The comparative example provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, and other conditions are identical to those of example 1 except that a surfactant is not adopted in the preparation method.
Comparative example 6
The comparative example provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, and other conditions are exactly the same as those of example 1 except that a calcining step is not adopted in the preparation method.
Comparative example 7
The comparative example provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, and other conditions are identical to those of example 1 except that the calcining temperature in the preparation method is 650 ℃.
Comparative example 8
The comparative example provides a preparation method of high-activity silver-doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, and other conditions are exactly the same as those of example 1 except that the preparation method adjusts the pH to 2 and then carries out heat preservation reaction for 1.5-2h at 60 ℃.
Comparative example 9
The comparative example provides a preparation method of high-activity silver doped nano bismuth tungstate with visible light catalytic air purification and antibacterial functions, and other conditions are exactly the same as those of example 1 except that anhydrous alcohol and distilled water are not adopted for centrifugal washing of reaction products.
The high-activity silver doped nano bismuth tungstate of the above examples and comparative examples was added to latex paint for performance testing, and the results were as follows:
from the data, the silver-doped nano bismuth tungstate material prepared by the method has excellent photocatalytic degradation performance and has higher use value in the field of antibacterial and environmental protection.
As can be seen from the comparison of examples 1-5 and comparative examples 1-3, the silver nitrate is directly added into the reaction system of sodium tungstate and bismuth nitrate, so that the system is fully reacted, silver ions are more easily doped into crystal lattices of bismuth tungstate, the preparation process is simple and easy to control, and the silver element replaces part of bismuth element in bismuth tungstate to endow the bismuth tungstate material with high-efficiency and durable antibacterial performance, and the proportion adopted by the invention can obtain the optimal technical effect.
As can be seen from the comparison of examples 1-5 and comparative examples 4-5, the addition of the silane coupling agent and the surfactant increases the band gap width of the silver doped nano bismuth tungstate, thereby improving the photocatalytic performance, and meanwhile, the silane coupling agent undergoes self-polycondensation reaction, and the obtained product plays a role of a soft template and induces the regular directional growth of synthetic grains; on the other hand, the dispersing agent can form a film on the surface of the crystal grains to isolate the contact between nano particles, so that the agglomeration of the crystal grains is reduced, the synthesized crystal grains are regular, and the particle size is uniform.
As can be seen from the comparison of examples 1 to 5 and comparative examples 6 to 9, the preparation process of the invention can ensure that the product has excellent photocatalytic degradation performance and high-efficiency and durable antibacterial performance.
Claims (6)
1. The preparation method of the material with the functions of visible light catalytic air purification and antibiosis is characterized in that the material is high-activity silver doped nano bismuth tungstate, and the high-activity silver doped nano bismuth tungstate is prepared from bismuth salt, silver nitrate and sodium tungstate;
the preparation method comprises the following steps:
adding bismuth nitrate pentahydrate and silver nitrate into nitric acid, dissolving and then mixing with sodium tungstate solution; sequentially adding a silane coupling agent and a surfactant, fully stirring, and adjusting the pH value of a reaction system to 0.5-2; reacting at 180-210 ℃ for 1.5-2h, cooling to room temperature, washing and drying the reaction product, grinding into powder, and calcining at 450-520 ℃ to obtain the high-activity silver doped nano bismuth tungstate material; the silane coupling agent is one or two of gamma-aminopropyl triethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane; the surfactant is one or more of polyethylene glycol, cetyltrimethylammonium bromide and polyvinyl alcohol; silver nitrate: bismuth nitrate: the molar ratio of the sodium tungstate is (0.1-0.3): 10:5.
2. the method for preparing a material with both visible light catalytic air purification and antibacterial functions according to claim 1, wherein the usage amount of the silane coupling agent is 0.5-2% of the total mass of the mixed solution.
3. The method for preparing a material with both visible light catalytic air purification and antibacterial functions according to claim 1, wherein the usage amount of the surfactant is 0.5-1.5% of the total mass of the mixed solution.
4. The method for preparing a material with both visible light catalytic air purification and antibacterial functions according to claim 1, wherein HNO is adopted 3 Or NaOH adjusts the pH of the reaction system to 0.5-2.
5. The method for preparing a material with both visible light catalytic air purification and antibacterial functions according to claim 1, wherein the reaction product is centrifugally washed 3 times with absolute ethanol and distilled water respectively; the collected product was dried at 70-80 ℃ for 12h and then ground into powder.
6. The method for preparing a material with both visible light catalytic air purification and antibacterial functions according to claim 1, wherein the concentration of sodium tungstate is 0.02-0.04 mol/L.
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