CN110373891A - Load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene and preparation method thereof - Google Patents
Load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene and preparation method thereof Download PDFInfo
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- CN110373891A CN110373891A CN201910640160.5A CN201910640160A CN110373891A CN 110373891 A CN110373891 A CN 110373891A CN 201910640160 A CN201910640160 A CN 201910640160A CN 110373891 A CN110373891 A CN 110373891A
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- Prior art keywords
- titanium dioxide
- redox graphene
- visible light
- bismuth tungstate
- tungstate
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000004744 fabric Substances 0.000 title claims abstract description 64
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 47
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims description 20
- 229920000742 Cotton Polymers 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 6
- -1 modified bismuth tungstate Chemical class 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000013019 agitation Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 12
- 150000001621 bismuth Chemical class 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 8
- 229960004756 ethanol Drugs 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- KKMOSYLWYLMHAL-UHFFFAOYSA-N 2-bromo-6-nitroaniline Chemical compound NC1=C(Br)C=CC=C1[N+]([O-])=O KKMOSYLWYLMHAL-UHFFFAOYSA-N 0.000 claims description 5
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- WPZFLQRLSGVIAA-UHFFFAOYSA-N sodium tungstate dihydrate Chemical compound O.O.[Na+].[Na+].[O-][W]([O-])(=O)=O WPZFLQRLSGVIAA-UHFFFAOYSA-N 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 230000001954 sterilising effect Effects 0.000 abstract description 13
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 13
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000007812 deficiency Effects 0.000 abstract description 2
- 241000588724 Escherichia coli Species 0.000 description 4
- 229960000583 acetic acid Drugs 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000012362 glacial acetic acid Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 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 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229940036359 bismuth oxide Drugs 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- 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
- B01J23/16—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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B01J35/39—
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/48—Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Abstract
The present invention is modified bismuth tungstate/titania powder by secondary hydrothermal synthesis, its photocatalysis performance is significantly improved using the superior physicochemical characteristic of redox graphene, it is carried on cotton fabric again, forms load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene.Present invention process is simple, it is without secondary pollution, gained load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene can be realized sterilized under visible light conditions, Continuous sterilization ability is strong, it can be used by simple clean cycle, sterilization effect remains at 93% or more, not only solves traditional photocatalytic powder material and is difficult to the deficiency recycled, and cotton fabric can adjust fabric shape according to the actual situation, practicability is high.
Description
Technical field
The invention belongs to visible light catalytic material preparation and environmental applications field, in particular to a kind of load bismuth tungstate/bis-
The preparation method of the visible light-responded composite antibacterial fabric of titanium oxide/redox graphene.
Background technique
Frequent with mankind's activity with the rapid development of industry, environmental pollution is got worse, to have to human health
The microbial reproduction and deviation creation of risk advantage, especially invasive organism, such as bacterium, virus, fungi and are posted
It is infested etc., if efficiently pathogenic microorganisms in water cannot be killed, it will cause significant damage to organism.
Currently, municipal sewage plant, China sterilization process is mainly chemical disinfection and ultraviolet disinfection, wherein with chlorination
For the traditional chemical disinfection technology of representative have been found that carcinogenic chloroform etc., teratogenesis, mutagenesis by-product can be generated, and it is ultraviolet
Although disinfection technology has spectrum sterilizing ability, without secondary pollution, its Continuous sterilization ability is weaker, and ultraviolet lamp sleeve need to be determined
Phase cleaning, operating cost are higher.It can be seen that research and development with high security, it is without secondary pollution, Continuous sterilization ability is strong the features such as
Antimicrobial technology have become the research hotspot of current field of water pollution control.
Photocatalysis is considered a kind of very with the sterilization technology of application potential, and the research and development of novel photocatalysis material are always
Since be environmental material field hot subject.Titanium dioxide is as conventional semiconductors catalysis material, under ultraviolet excitation
Bacterial micro-organism growth can be effectively suppressed, cell membrane or DNA molecular chain are destroyed, but itself band gap is wide, only in ultraviolet striation
Part has response, to limit its photocatalysis effect.It in recent years, is considered as a kind of energy by adulterating other semiconductor materials
Enough significantly improve the effective ways of its photocatalysis efficiency.Bismuth tungstate/titanium dioxide composite photocatalyst can be under excited by visible light
Effectively degradation environmental organic pollutant, although its visible absorption performance is good, the light induced electron and photohole that generate
Easily occur compound, causes its practical electronic efficiency lower.Redox graphene is a kind of derivative of graphene, has two dimension
Layer structure, large specific surface area, oxygen-containing functional group are abundant, mechanics calorifics electric property is superior, are a kind of ideal nano materials
Complex carrier.Nevertheless, existing in actual application easy since gained catalysis material form is powder or graininess
Reunite, be easy to run off, difficult the defects of recycling.
Summary of the invention
Technical problem solved by the invention is how to obtain simple process, without secondary pollution, has and continues to sterilize energy by force
The visible light-responded composite antibacterial fabric of power, to overcome existing photoresponse wave-length coverage narrow, photocatalytic powder material has been lost difficulty
The defect of recycling.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is to provide a kind of load bismuth tungstate/titanium dioxide/also
The preparation method of the former visible light-responded composite antibacterial fabric of graphene oxide, which comprises the following steps:
Step 1: sodium hydroxide and paregal O is soluble in water, mixed solution is formed, it is molten that cotton fabric is then placed in mixing
In liquid, ultrasonic treatment can must pre-process cotton fabric；
Step 2: Disodium tungstate (Na2WO4) dihydrate being dissolved in deionized water, ultrasonic disperse obtains sodium tungstate solution；Bismuth salt is dissolved in nothing
Water-ethanol, ultrasonic disperse obtain bismuth salt suspension；Then resulting sodium tungstate solution and bismuth salt suspension are mixed, is mixed
Close liquid；
Step 3: butyl titanate instillation step 2 being prepared in resulting mixed liquor, Weak monoacid reaction is then added, so
PH value is adjusted using lye afterwards, magnetic agitation is uniform, carries out hydro-thermal reaction, is filtered, washed, dries, calcines, grinds, can obtain tungsten
Sour bismuth/titania powder；
Step 4: step 3 is prepared into resulting bismuth tungstate/titania powder and redox graphene in dehydrated alcohol
Middle ultrasonic disperse, magnetic agitation is uniform, then carries out hydro-thermal reaction, is filtered, washed, dries, grinds, and can obtain reduction-oxidation graphite
Alkene loads bismuth tungstate/composite titania material；
Step 5: step 4 is prepared into resulting bismuth tungstate/titanium dioxide/redox graphene composite material and step 1
It prepares resulting pretreatment cotton fabric to immerse in deionized water, polyethylene glycol 2000 is added, magnetic agitation is uniform, can obtain after dry
Load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene.
Preferably, in the step 1, sodium hydroxide and paregal O mass ratio are 1:4, naoh concentration is 10~
20g/L。
Preferably, in the step 2, bismuth salt is one of bismuth citrate, five nitric hydrate bismuths or bismuth chloride.
Preferably, in the step 2, bismuth salt and sodium tungstate mass ratio (2.0~3.0): 1, dehydrated alcohol and deionized water
Volume ratio is (1.0~2.0): 1.
Preferably, in the step 2, concentration of sodium tungstate is 0.025~0.055g/mL, bismuth salt and dehydrated alcohol mass ratio
For (0.06~0.22): 1.
Preferably, in the step 3, the volume ratio of butyl titanate and the resulting mixed liquor of step 1 be (0.02~
0.08):1。
Preferably, in the step 3, Weak monoacid can be formic acid or acetic acid, and concentration is 0.1~0.5mol/L, and unitary is weak
Acid is 1:(8.0~40.0 with butyl titanate volume ratio).
Preferably, in the step 3, lye is sodium hydroxide or potassium hydroxide solution, and concentration is 1.0~2.0mol/L,
PH value is finally adjusted to 2.0~5.0.
Preferably, in the step 3, hydrothermal temperature is 160~180 DEG C, and the reaction time is 6~8h.
Preferably, in the step 3, calcining is carried out in the Muffle furnace for being connected with nitrogen, and temperature is 450~550 DEG C, instead
2~4h between seasonable.
Preferably, in the step 4, bismuth tungstate/titania powder and redox graphene mass ratio be (100~
150): 1, the mass volume ratio of redox graphene and dehydrated alcohol is 0.25~0.5g/L.
Preferably, in the step 4, hydrothermal temperature is 180~200 DEG C, and the reaction time is 6~8h.
Preferably, in the step 3 and 4, washing includes deionized water and ethanol washing, and drying uses vacuum oven,
Time is 20~30h, and temperature is 45~65 DEG C.
Preferably, in the step 5, the polyethylene glycol 2000 and bismuth tungstate/titanium dioxide/redox graphene
Composite material mass ratio is 1:(100~200), bismuth tungstate/titanium dioxide/redox graphene composite material dosage is 10
~20g/L.
Preferably, dry to use vacuum oven in the step 5, the time is 24~36h, and temperature is 40~60 DEG C.
The present invention also provides load bismuth tungstate/titanium dioxide/redox graphene visible lights of above method preparation
Respond composite antibacterial fabric.
Compared with prior art, it Fa Ming not have the following beneficial effects:
(1) present invention is modified bismuth tungstate/titania powder by secondary hydrothermal synthesis, utilizes oxygen reduction fossil
The black superior physicochemical characteristic of alkene significantly improves its photocatalysis performance, then is carried on cotton fabric, and load bismuth tungstate/bis- are formed
The visible light-responded composite antibacterial fabric of titanium oxide/redox graphene, solves that photocatalytic powder material is easily rolled into a ball, difficult recycling follows
The defect that ring utilizes.
(2) present invention process is simple, without secondary pollution, and gained loads bismuth tungstate/titanium dioxide/redox graphene can
Light-exposed response composite antibacterial fabric can be realized sterilized under visible light conditions, and Continuous sterilization ability is strong, overcomes current light
The defect that catalytic antimicrobial technique only responds under ultraviolet light conditions.
(3) load of the invention bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene can
To be used by simple clean cycle, sterilization effect remains at 93% or more, not only solves traditional photocatalytic powder material
Material is difficult to the deficiency recycled, and cotton fabric can adjust fabric shape according to the actual situation, can practicability height.
Detailed description of the invention
Fig. 1 is visible light-responded composite antibacterial fabric material pictorial diagram；
Fig. 2 is visible light-responded composite antibacterial fabric micro-structure diagram；
Fig. 3 is visible light-responded composite antibacterial fabric preparation flow schematic diagram；
Fig. 4 is visible light-responded composite antibacterial fabric electron-microscope scanning figure；
Fig. 5 is the antibacterial experiment verification the verifying results figure in embodiment 1 under visible light conditions；
Fig. 6 is that the 1 visible light-responded composite antibacterial fabric of gained of embodiment repeats the antibacterial effect figure after washing.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Reagent used in the embodiment of the present invention is purchased from the limited public affairs of Chinese medicines group chemical reagent in addition to graphene oxide
Department, graphene oxide are purchased from Suzhou Si Bin nanosecond science and technology Co., Ltd.
Embodiment 1
As shown in figures 1-4, it is visible to present embodiments provide a kind of load bismuth tungstate/titanium dioxide/redox graphene
The preparation method of photoresponse composite antibacterial fabric, the specific steps are as follows:
Step 1: 0.5g sodium hydroxide and 0.7g paregal O being dissolved in 100mL water, mixed solution is formed, by 0.8g cotton
Fabric (5cm × 5cm) is placed in mixed solution, ultrasound 20min under the conditions of 70 DEG C, is removed fabric surface greasy dirt, can be obtained and locate in advance
Manage cotton fabric；
Step 2: 0.825g Disodium tungstate (Na2WO4) dihydrate being added in 30mL deionized water, ultrasonic 30min, it is transparent to form sodium tungstate
Solution；Five nitric hydrate bismuth of 2.4254g is added in 30mL dehydrated alcohol, ultrasonic 30min, forms bismuth nitrate suspension；By tungsten
Sour sodium clear solution and bismuth nitrate suspension are sufficiently mixed 30min, and revolving speed 500r/min obtains mixed liquor；
Step 3: 4mL butyl titanate being added dropwise in the mixed liquor that step 2 obtains, 0.2mL concentration, which is then added, is
The glacial acetic acid of 0.05mol/L reacts 30min, adjusts pH value to 2, magnetic agitation 60min using 1mol/L sodium hydroxide solution,
Hydro-thermal reaction 6h under the conditions of 180 DEG C, vacuum filter are successively used deionized water and ethanol washing, are placed in 60 DEG C of vacuum ovens
It is dry to be ground to using agate mortar powdered for 24 hours, it is placed in 450 DEG C of Muffle furnaces and calcines 2h, bismuth tungstate/titanium dioxide can be obtained
Powder；
Step 4: by the above-mentioned bismuth tungstate/titania powder of 2.0g and 0.015g redox graphene in the anhydrous second of 50mL
In alcohol, ultrasonic 30min, magnetic agitation 60min, revolving speed 500r/min, hydro-thermal reaction 6h, vacuum filter successively uses deionized water
And ethanol washing, being placed in drying in 60 DEG C of vacuum ovens for 24 hours, it is compound can to obtain bismuth tungstate/titanium dioxide/redox graphene
Material；
Step 5: by the above-mentioned bismuth tungstate/titanium dioxide/redox graphene composite material of 2.0g and pretreatment cotton fabric
It immerses in 100mL deionized water, 0.02g polyethylene glycol 2000, magnetic agitation 30min under the conditions of 85 DEG C, vacuum drying is added
Bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene can must be loaded after for 24 hours.
Embodiment 2
As shown in figures 1-4, it is visible to present embodiments provide a kind of load bismuth tungstate/titanium dioxide/redox graphene
The preparation method of photoresponse composite antibacterial fabric, the specific steps are as follows:
Step 1: 0.5g sodium hydroxide and 0.7g paregal O being dissolved in 100mL water, mixed solution is formed, by 1.0g cotton
Fabric (6cm × 6cm) is placed in mixed solution, ultrasound 20min under the conditions of 70 DEG C, is removed fabric surface greasy dirt, can be obtained and locate in advance
Manage cotton fabric；
Step 2: 1.24g Disodium tungstate (Na2WO4) dihydrate being added in 25mL deionized water, ultrasonic 30min, it is transparent to form sodium tungstate
Solution；2.98g bismuth citrate is added in 40mL dehydrated alcohol, ultrasonic 30min, forms bismuth citrate suspension；By sodium tungstate
Clear solution and bismuth citrate suspension are sufficiently mixed 60min, and revolving speed 100r/min obtains mixed liquor；
Step 3: 2mL butyl titanate being added dropwise in the mixed liquor that step 2 obtains, 0.25mL concentration, which is then added, is
The glacial acetic acid of 0.25mol/L reacts 30min, adjusts pH value to 3, magnetic agitation 60min using 2mol/L sodium hydroxide solution,
Hydro-thermal reaction 8h under the conditions of 160 DEG C, vacuum filter are successively used deionized water and ethanol washing, are placed in 65 DEG C of vacuum ovens
Dry 20h, is ground to powdered using agate mortar, is placed in 550 DEG C of Muffle furnaces and is calcined 4h, can obtain bismuth tungstate/titanium dioxide
Powder；
Step 4: by the above-mentioned bismuth tungstate/titania powder of 1.5g and 0.01g redox graphene in the anhydrous second of 60mL
In alcohol, ultrasonic 60min, magnetic agitation 60min, revolving speed 500r/min, hydro-thermal reaction 8h, vacuum filter successively uses deionized water
And ethanol washing, it is placed in 65 DEG C of vacuum ovens dry 20h, it is compound that bismuth tungstate/titanium dioxide/redox graphene can be obtained
Material；
Step 5: by the above-mentioned bismuth tungstate/titanium dioxide/redox graphene composite material of 3.0g and pretreatment cotton fabric
It immerses in 150mL deionized water, 0.03g polyethylene glycol 2000, magnetic agitation 30min under the conditions of 80 DEG C, vacuum drying is added
Bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene can must be loaded after 30h.
Embodiment 3
As shown in figures 1-4, it is visible to present embodiments provide a kind of load bismuth tungstate/titanium dioxide/redox graphene
The preparation method of photoresponse composite antibacterial fabric, the specific steps are as follows:
Step 1: 0.5g sodium hydroxide and 0.7g paregal O being dissolved in 100mL water, mixed solution is formed, by 1.0g cotton
Fabric (6cm × 6cm) is placed in mixed solution, ultrasound 20min under the conditions of 70 DEG C, is removed fabric surface greasy dirt, can be obtained and locate in advance
Manage cotton fabric；
Step 2: 1.65g Disodium tungstate (Na2WO4) dihydrate being added in 40mL deionized water, ultrasonic 30min, it is transparent to form sodium tungstate
Solution；3.16g bismuth chloride is added in 40mL dehydrated alcohol, ultrasonic 30min, forms bismuth chloride suspension；Sodium tungstate is transparent
Solution and bismuth chloride suspension are sufficiently mixed 30min, and revolving speed 300r/min obtains mixed liquor；
Step 3: 6mL butyl titanate being added dropwise in the mixed liquor that step 2 obtains, 0.60mL concentration, which is then added, is
The glacial acetic acid of 0.125mol/L reacts 30min, uses 1.5mol/L sodium hydroxide solution adjusting pH value to 3, magnetic agitation
60min, hydro-thermal reaction 8h under the conditions of 180 DEG C, vacuum filter successively use deionized water and ethanol washing, are placed in 55 DEG C of vacuum
It is dry in drying box to be ground to using agate mortar powdered for 24 hours, be placed in 500 DEG C of Muffle furnaces and calcine 3h, can obtain bismuth tungstate/
Titania powder；
Step 4: by the above-mentioned bismuth tungstate/titania powder of 1.0g and 0.01g redox graphene in the anhydrous second of 40mL
In alcohol, ultrasonic 60min, magnetic agitation 30min, revolving speed 300r/min, hydro-thermal reaction 6h, vacuum filter successively uses deionized water
And ethanol washing, being placed in drying in 65 DEG C of vacuum ovens for 24 hours, it is compound can to obtain bismuth tungstate/titanium dioxide/redox graphene
Material；
Step 5: by the above-mentioned bismuth tungstate/titanium dioxide/redox graphene composite material of 2.0g and pretreatment cotton fabric
It immerses in 150mL deionized water, 0.02g polyethylene glycol 2000, magnetic agitation 30min under the conditions of 80 DEG C, vacuum drying is added
Bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene can must be loaded after 36h.
It can using load bismuth tungstate/titanium dioxide/redox graphene obtained in spread plate testing example 1
Light-exposed response composite antibacterial fabric is under visible light conditions to the bactericidal effect of Escherichia coli.First by resulting load wolframic acid
The visible light-responded composite antibacterial fabric of bismuth/titanium dioxide/redox graphene is added in Escherichia coli solution, in visible striation
60min is reacted under part, samples and is coated with every the set time, be put into incubator and cultivated at 37 DEG C for 24 hours, then observe its clump count
Amount calculates Escherichia coli sterilizing rate, the results are shown in Table 1.
The visible light-responded composite antibacterial fabric of table 1 irradiates the antibacterial effect after 60min under visible light conditions
As shown in table 1, the present invention loads bismuth tungstate/visible light-responded composite antibacterial of titanium dioxide/redox graphene
Fabric can be used by simple clean cycle, and sterilization effect remains at 93% or more.
As shown in figure 4, bismuth tungstate/titanium dioxide/redox graphene uniform load prepared by the present invention is in fabric table
Face.As shown in Fig. 5~6, it is visible that the embodiment of the present invention 1 prepares resulting load bismuth tungstate/titanium dioxide/redox graphene
Photoresponse composite antibacterial fabric is good to Escherichia coli bactericidal effect, and stability is high, and rate is fast, and sterilizing rate maintains in 60min
96.5% or more (Fig. 5), and by clean cycle using after 10 times, sterilizing rate can still maintain 93% or more (Fig. 6).
Claims (10)
1. a kind of load bismuth tungstate/titanium dioxide/redox graphene visible light-responded composite antibacterial fabric preparation method,
Characterized by comprising the following steps:
Step 1: sodium hydroxide and paregal O is soluble in water, mixed solution is formed, cotton fabric is then placed in mixed solution
In, ultrasonic treatment can must pre-process cotton fabric；
Step 2: Disodium tungstate (Na2WO4) dihydrate being dissolved in deionized water, ultrasonic disperse obtains sodium tungstate solution；Bismuth salt is dissolved in anhydrous second
Alcohol, ultrasonic disperse obtain bismuth salt suspension；Then resulting sodium tungstate solution and bismuth salt suspension are mixed, obtains mixed liquor；
Step 3: butyl titanate instillation step 2 being prepared in resulting mixed liquor, Weak monoacid reaction is then added, then makes
With lye adjust pH value, magnetic agitation is uniform, carry out hydro-thermal reaction, be filtered, washed, dry, calcine, grind, can obtain bismuth tungstate/
Titania powder；
Step 4: it is super in dehydrated alcohol that step 3 being prepared into resulting bismuth tungstate/titania powder and redox graphene
Sound dispersion, magnetic agitation is uniform, then carries out hydro-thermal reaction, is filtered, washed, dries, grinds, and it is negative can to obtain redox graphene
Carry bismuth tungstate/composite titania material；
Step 5: step 4 being prepared into resulting bismuth tungstate/titanium dioxide/redox graphene composite material and is prepared by step 1
Resulting pretreatment cotton fabric immerses in deionized water, and polyethylene glycol 2000 is added, and magnetic agitation is uniform, can must load after dry
Bismuth tungstate/visible light-responded the composite antibacterial fabric of titanium dioxide/redox graphene.
2. load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene as described in claim 1
Preparation method, which is characterized in that in the step 1, sodium hydroxide and paregal O mass ratio are 1:4, and naoh concentration is
10~20g/L.
3. load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene as described in claim 1
Preparation method, which is characterized in that in the step 2, bismuth salt be bismuth citrate, five nitric hydrate bismuths or bismuth chloride in one
Kind；Bismuth salt and sodium tungstate mass ratio (2.0~3.0): 1, dehydrated alcohol and deionized water volume ratio are (1.0~2.0): 1.
4. load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene as described in claim 1
Preparation method, which is characterized in that in the step 3, in the step 3, Weak monoacid can be formic acid or acetic acid, and concentration is
0.1~0.5mol/L, Weak monoacid and butyl titanate volume ratio are 1:(8.0~40.0).
5. load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene as described in claim 1
Preparation method, which is characterized in that in the step 3, lye be sodium hydroxide or potassium hydroxide solution, concentration be 1.0~
2.0mol/L finally adjusts pH value to 2.0~5.0.
6. load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene as described in claim 1
Preparation method, which is characterized in that in the step 3, hydrothermal temperature be 160~180 DEG C, the reaction time be 6~8h；It forges
Burning is carried out in the Muffle furnace for being connected with nitrogen, and temperature is 450~550 DEG C, 2~4h of reaction time.
7. load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene as described in claim 1
Preparation method, which is characterized in that in the step 4, hydrothermal temperature be 180~200 DEG C, the reaction time be 6~8h.
8. load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene as described in claim 1
Preparation method, which is characterized in that in the step 3 and 4, washing includes deionized water and ethanol washing, dry to use vacuum
Drying box, time are 20~30h, and temperature is 45~65 DEG C；It is dry to use vacuum oven in the step 5, the time is 24~
36h, temperature are 40~60 DEG C.
9. load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene as described in claim 1
Preparation method, which is characterized in that in the step 5, the polyethylene glycol 2000 and bismuth tungstate/titanium dioxide/oxygen reduction
Graphite alkene composite material mass ratio is 1:(100~200), bismuth tungstate/titanium dioxide/redox graphene composite material is thrown
Dosage is 10~20g/L.
10. load bismuth tungstate/titanium dioxide/redox graphene of any one of claim 1~9 the method preparation is visible
Photoresponse composite antibacterial fabric.
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