CN106470550A - Antibacterial antiviral composition, anti-bacteria and anti-virus agent, photocatalyst and bacterial viruses ablation method - Google Patents
Antibacterial antiviral composition, anti-bacteria and anti-virus agent, photocatalyst and bacterial viruses ablation method Download PDFInfo
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- CN106470550A CN106470550A CN201580033682.9A CN201580033682A CN106470550A CN 106470550 A CN106470550 A CN 106470550A CN 201580033682 A CN201580033682 A CN 201580033682A CN 106470550 A CN106470550 A CN 106470550A
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- antiviral composition
- compound
- antibacterial
- cupric
- antibacterial antiviral
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- 230000000840 anti-viral effect Effects 0.000 title claims abstract description 94
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000001580 bacterial effect Effects 0.000 title claims abstract description 22
- 239000003443 antiviral agent Substances 0.000 title claims abstract description 21
- 238000002679 ablation Methods 0.000 title claims abstract description 12
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- HVAQEDZZHIPFOM-UHFFFAOYSA-N copper;nonanoic acid Chemical compound [Cu].CCCCCCCCC(O)=O HVAQEDZZHIPFOM-UHFFFAOYSA-N 0.000 description 1
- QNZRVYCYEMYQMD-UHFFFAOYSA-N copper;pentane-2,4-dione Chemical compound [Cu].CC(=O)CC(C)=O QNZRVYCYEMYQMD-UHFFFAOYSA-N 0.000 description 1
- LMCVMQNMDSVUFJ-UHFFFAOYSA-N copper;pentanedioic acid Chemical compound [Cu].OC(=O)CCCC(O)=O LMCVMQNMDSVUFJ-UHFFFAOYSA-N 0.000 description 1
- KIJUYIWZRZZLJC-UHFFFAOYSA-N copper;pentanoic acid Chemical compound [Cu].CCCCC(O)=O KIJUYIWZRZZLJC-UHFFFAOYSA-N 0.000 description 1
- GARLGTQMDTVDFQ-UHFFFAOYSA-N copper;phthalic acid Chemical compound [Cu].OC(=O)C1=CC=CC=C1C(O)=O GARLGTQMDTVDFQ-UHFFFAOYSA-N 0.000 description 1
- QVLQKWQNKGVECJ-UHFFFAOYSA-N copper;propanoic acid Chemical compound [Cu].CCC(O)=O QVLQKWQNKGVECJ-UHFFFAOYSA-N 0.000 description 1
- DDXCBBLSEWZIJW-UHFFFAOYSA-N copper;tetradecanoic acid Chemical compound [Cu].CCCCCCCCCCCCCC(O)=O DDXCBBLSEWZIJW-UHFFFAOYSA-N 0.000 description 1
- 239000012531 culture fluid Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
- FWBOFUGDKHMVPI-UHFFFAOYSA-K dicopper;2-oxidopropane-1,2,3-tricarboxylate Chemical compound [Cu+2].[Cu+2].[O-]C(=O)CC([O-])(C([O-])=O)CC([O-])=O FWBOFUGDKHMVPI-UHFFFAOYSA-K 0.000 description 1
- PEVJCYPAFCUXEZ-UHFFFAOYSA-J dicopper;phosphonato phosphate Chemical compound [Cu+2].[Cu+2].[O-]P([O-])(=O)OP([O-])([O-])=O PEVJCYPAFCUXEZ-UHFFFAOYSA-J 0.000 description 1
- 241001493065 dsRNA viruses Species 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- FYIBGDKNYYMMAG-UHFFFAOYSA-N ethane-1,2-diol;terephthalic acid Chemical compound OCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 FYIBGDKNYYMMAG-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000937 inactivator Effects 0.000 description 1
- 206010022000 influenza Diseases 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- YDSWCNNOKPMOTP-UHFFFAOYSA-N mellitic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(O)=O)=C(C(O)=O)C(C(O)=O)=C1C(O)=O YDSWCNNOKPMOTP-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 125000005474 octanoate group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 235000019319 peptone Nutrition 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920005596 polymer binder Polymers 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 229910000161 silver phosphate Inorganic materials 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 241001515965 unidentified phage Species 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
-
- 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
-
- 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
- A01N59/20—Copper
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/08—Radiation
- A61L2/088—Radiation using a photocatalyst or photosensitiser
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/122—Halides of copper
-
- 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—
Abstract
The excellent antibacterial antiviral composition of present invention offer antimicrobial antiviral activity under visible light illumination, anti-bacteria and anti-virus agent, photocatalyst and bacterial viruses ablation method.The antibacterial antiviral composition of the present invention comprises to be supported with the titanium dioxide of cupric compound and silver compound altogether.The photocatalyst of the anti-bacteria and anti-virus agent of the present invention and the present invention contains the antibacterial antiviral composition of the present invention.The bacterial viruses ablation method of the present invention uses the antibacterial antiviral composition of the present invention, the anti-bacteria and anti-virus agent of the present invention or the photocatalyst of the present invention by antibacterial and inactivation of virus.
Description
Technical field
The present invention relates to antibacterial antiviral composition, anti-bacteria and anti-virus agent, photocatalyst and bacterial viruses ablation method.
More specifically, the photoresponse activity for antibacterial and virus being related under the radiation of visible light that wavelength is more than 400nm high and
And have the antibacterial antiviral composition of deactivation for the antibacterial in dark and virus, anti-bacteria and anti-virus agent, photocatalysis concurrently
Agent and bacterial viruses ablation method.
Background technology
From the viewpoint of anti-bacteria and anti-virus, antibacterial metal, organic based compound, native compound and photocatalyst etc.
Research is actively carried out.Wherein, photocatalyst has antimicrobial antiviral activity for many antibacterials, virus, and photocatalyst can
To regard one of promising material as.
Patent documentation 1 describes CuO/TiO under ultraviolet light2Phage virus are gone out by (anatase titanium dioxide)
Live.Patent documentation 2 describes and supports the tungsten oxide particle of platinum and show antiviral activity under visible light illumination.But, these
The photocatalyst with antimicrobial antiviral activity exists just active only under ultraviolet light or is only used as dilute
There is the tungsten of metal problem just active etc under visible light illumination.
On the other hand, the metal such as known Cu, Ag, Zn, metal ion or comprise their compound as anti-all the time
Bacterium materials serve acts on.Wherein, (for example patent is civilian by the antibacterial of Ag and various oxide-metal combinations to report some
Offer 3,4).But, there are following problems in these compounds：There is no the photocatalyst function of showing under visible light illumination,
Therefore cannot utilize indoors, the antibacterial that inactivates in the dark, remains of virus etc. residue in these compounds, thus cannot the phase
Treat to maintain anti-bacteria and anti-virus function for a long time.
Additionally, it has been found that making CuO and Ag2The titanium dioxide that both O coexist shows under dark and ultraviolet irradiate
Anti-microbial property (such as patent documentation 5).But, this photocatalyst system does not carry out activation under visible light illumination, therefore for
This photocatalyst system activation is made to need to send the light source of ultraviolet.Be known as one of Ag compound AgCl response from
Ultraviolet region, to the light of visible region, produces photoreaction (such as non-patent literature 1).But, AgCl particle does not show itself
Antiviral property, and AgCl particle easily becomes oversize grain, there is the not disposable such problem of AgCl particle (for example non-
Patent documentation 2).
Citation
Patent documentation 1：Japanese Unexamined Patent Publication 2006-232729 publication
Patent documentation 2：Japanese Unexamined Patent Publication 2011-136984 publication
Patent documentation 3：Japanese Unexamined Patent Publication 11-228320 publication
Patent documentation 4：Japanese Unexamined Patent Publication 9-278615 publication
Patent documentation 5：Japanese Patent Publication No. 4169163
Non-patent literature 1：J.Photochem.Photobio.A,95(1996)175-180
Non-patent literature 2：The development evaluation of anti-bacteria and anti-virus material and process technology technical information association
Content of the invention
In patent documentation 1, CuO/TiO2Sample under ultraviolet irradiation (embodiment 1～4, comparative example 3～4), visible
In (comparative example 2) and dark under light irradiation, (comparative example 1) does not show the inactivating efficacy of phage virus completely.However, it is near
The light of the White LED fluorescent lamp quickly popularized over year does not contain ultraviolet light.The inactivator of the phage virus that patent documentation 1 is recorded exists
Under dark neutralization radiation of visible light, there is no antiviral activity completely, therefore predict and do not have completely under White LED fluorescent lamp yet
There is antiviral activity.
Although anti-microbial property under ultraviolet light or in dark has been expressly recited in patent documentation 3～5, do not close
In the record of antiviral, due to not containing the material of responding to visible light, the photocatalyst that therefore prediction patent documentation 3～5 is recorded
Antimicrobial antiviral activity is hardly shown under White LED fluorescent lamp.
AgCl has been recorded in the oxygen reaction of formation being derived from the aqueous solution containing sacrifice agent, visible in non-patent literature 1
Activity is shown under light irradiation.But, water oxidative decomposition activity and antimicrobial antiviral activity excellent between do not exist
Dependency.The anti-bacteria and anti-virus spectrum having recorded insoluble Ag compound in non-patent literature 2 is narrow, does not have tunicary phagocytosis
The inactivation of precursor virus hardly occurs.Therefore, those skilled in the art fail to give attention to comprise to be supported with altogether at all silver compound and
The titanium dioxide, responding to visible light of copper compound simultaneously shows the photocatalyst of antimicrobial antiviral activity.
It is an object of the invention to provide a kind of in such a case it is seen that the antimicrobial antiviral activity under light irradiation is high
Antibacterial antiviral composition, anti-bacteria and anti-virus agent and bacterial viruses ablation method.
The present inventor is to reach above-mentioned purpose conscientiously to be studied, it is found that supporting silver by making TiO 2 particles
Both compound and copper compound, can have the anti-bacteria and anti-virus characteristic under radiation of visible light concurrently.
The present invention is completed based on this opinion.
Furthermore, photocatalyst is referred to have the property of quasiconductor, is generated hole and electricity by absorbing light in this manual
Son simultaneously participates in chemical reaction by them and shows the material of catalyst action.In addition, promoter is in this manual
Refer to play the material of following effects：Catch the hole being generated by photocatalyst and electronics, so that the adsorbance of response matrix is increased or drop
The activation energy of the low chemical reaction in photocatalyst surface generation.In addition, carrier refers to play following effects in this manual
Material：By control above-mentioned photocatalyst or above-mentioned promoter size, shape and show these materials function or
These materials are made to increase.The divalent component of copper compound has the function as promoter, and silver compound has urges as light
The function of agent, titanium dioxide has the function as carrier and/or photocatalyst.
In addition, virus means DNA viruses and RNA viruses, also include bacterial infection virus be bacteriophage (below
Sometimes it is also referred to as " phage ").
That is, the present invention is as described below.
[1] a kind of antibacterial antiviral composition, comprises to be supported with the titanium dioxide of cupric compound and silver compound altogether.
[2] antibacterial antiviral composition according to above-mentioned [1], silver compound is the halogenide of silver.
[3] antibacterial antiviral composition according to above-mentioned [2], the halogenide of silver is AgCl.
[4] antibacterial antiviral composition described in any one according to above-mentioned [1]～[3], with respect to the two of 100 mass parts
Titanium oxide, the loading of silver compound is 0.01～20 mass parts.
[5] antibacterial antiviral composition described in any one according to above-mentioned [1]～[4], by scanning electron microscope
The mean diameter of the silver compound observing is 1nm～1 μm.
[6] antibacterial antiviral composition described in any one according to above-mentioned [1]～[5], with respect to total 100 mass parts
Titanium dioxide and silver compound, the copper quality of cupric compound is 0.01～20 mass parts.
[7] antibacterial antiviral composition described in any one according to above-mentioned [1]～[6], the Ag atom in silver compound
Mol ratio with the Cu atom in cupric compound is 1:0.0045～1:451.
[8] antibacterial antiviral composition described in any one according to above-mentioned [1]～[7], cupric compound is to be selected from
One of following (a)～(h) or two or more,
The cupric compound of a hydroxyl that () is represented by following formulas (1),
Cu2(OH)3X (1)
(in formula, X represents anion)
(b) cupric halogenide,
(c) cupric inorganic acid salt,
(d) cupric acylate,
(e) copper oxide,
(f) copper sulfide,
(g) copper azide,
(h) cupric silicate.
[9] antibacterial antiviral composition according to above-mentioned [8], the X of formula (1) is the conjugation selected from halogen, carboxylic acid
One of alkali, the conjugate base of mineral acid and OH or two or more.
[10] antibacterial antiviral composition according to above-mentioned [8] or [9], X is selected from Cl, CH3COO、NO3With
(SO4)1/2One of or two or more.
[11] antibacterial antiviral composition described in any one according to above-mentioned [1]～[10], has and by illumination is
The radiation of visible light of 1000 luxs 1 hour and by more than 99% bacterial viruses inactivation ability.
[12] a kind of anti-bacteria and anti-virus agent, the antibacterial antiviral composition described in any one containing above-mentioned [1]～[11].
[13] a kind of photocatalyst, the antibacterial antiviral composition described in any one containing above-mentioned [1]～[11].
[14] a kind of bacterial viruses ablation method, using the anti-bacteria and anti-virus group described in any one of above-mentioned [1]～[11]
Anti-bacteria and anti-virus agent described in compound, above-mentioned [12] or the photocatalyst described in above-mentioned [13] are by antibacterial and inactivation of virus.
The excellent antibacterial antiviral composition of antimicrobial antiviral activity under radiation of visible light can be provided according to the present invention, resist
Bacterium antiviral agent, photocatalyst and bacterial viruses ablation method.
Brief description
Fig. 1 is the X-ray diffraction pattern of the titanium dioxide being supported with copper compound and silver compound altogether representing embodiment 1
Figure.
Fig. 2 is being shown by scanning electron of the titanium dioxide being supported with copper compound and silver compound altogether of embodiment 1
The reflected electron image photo that micro mirror obtains.
Fig. 3 is the secondary electron image photo being obtained by scanning electron microscope of the silver compound of comparative example 1.
Specific embodiment
Hereinafter, to the antibacterial antiviral composition of the present invention, the anti-bacteria and anti-virus agent of the present invention, the present invention photocatalyst
And bacterial viruses ablation method illustrates.
The antibacterial antiviral composition of the present invention is the titanium dioxide comprising to be supported with altogether copper compound and silver compound
Compositionss.By combining silver compound, copper compound and titanium dioxide, antibacterial antiviral composition shows at bright place and dark place
Go out excellent anti-bacteria and anti-virus.
Even if individually using silver compound, copper compound and titanium dioxide, each material is right under visible light illumination
Do not show activity in antibacterial and virus yet.Even and if, not supporting in the state of titanium dioxide using cupric compound
With the mixture of silver compound, activity is not shown yet for antibacterial and virus.But surprisingly carried on a shoulder pole by making titanium dioxide
Carry cupric compound and silver compound, show the antimicrobial antiviral activity under radiation of visible light.
＜ silver compound ＞
The silver compound being used for the antibacterial antiviral composition of the present invention is not particularly limited, as preferred patina
Compound for example can enumerate silver-colored oxide, the nitride of silver, the sulfide of silver, the phosphoric acid compound of silver, the halogenide of silver, silver-colored carbon
Compound and silver alloy etc., as preferred silver compound can enumerate silver oxide, silver sulfide, silver phosphoric acid compound and
The halogenide of silver.Oxide as preferred silver for example can enumerate AgNbO3、Ag0.5Pr0.5TiO3、AgLi1/3Ti2/3O2With
AgGaO2Deng.Sulfide as preferred silver for example can enumerate AgGaS2And AgInS2- ZnS solid solution etc..As preferred silver
Phosphoric acid compound for example can enumerate Ag3PO4Deng.Halogenide as preferred silver for example can enumerate such as AgCl, AgBr and AgI
Deng.These can be used alone one kind or mix two or more uses.Among them, most preferred silver compound is the halogenation of silver
Thing, this is because the color of its own is white.From the high universalizable of preparation method simplicity, chemicals, the halogenation of above-mentioned silver
Among thing, most preferred silver compound is AgCl.
Loading for silver compound is not particularly limited, with respect to 100 mass parts titanium dioxide be preferably 0.01～
20 mass parts, more preferably 0.05～10 mass parts, more preferably 1～7 mass parts.By the loading of silver compound it is
More than 0.01 mass parts, photocatalyst composition increases, the increasing number in the electronics of generation and hole, energy therefore in visible absorption
Enough raising anti-bacteria and anti-virus performances further.On the other hand, if the loading of silver compound is below 20 mass parts, can
The suppression precipitation in the place in addition on titanium dioxide for the silver compound, the particle diameter of silver compound will not become big, reduce by
The color change that the photobehavior of silver compound itself leads to.
Mean diameter for silver compound is not particularly limited, by scanning electron microscope (SEM) observe average
Particle diameter is preferably less than 1 μm, more preferably below 500nm, more preferably below 300nm.Average by silver compound
Particle diameter is less than 1 μm, and silver compound is increased with the contact probability of antibacterial and virus, shows high anti-bacteria and anti-virus performance.Separately
Outward, more than 1nm is preferably by the mean diameter that scanning electron microscope (SEM) is observed.With regard to micro- by scanning electron
The details of the mean diameter that mirror (SEM) is observed, can illustrate in embodiment described later.
＜ cupric compound ＞
Copper quality in the cupric compound that the antibacterial antiviral composition of the present invention is used (is scaled Cu's
Quality), with respect to silver compound and the titanium dioxide of total 100 mass parts, preferably 0.01～20 mass parts, more preferably
0.1～20 mass parts, more preferably 0.1～10 mass parts, particularly preferably 0.3～5 mass parts.If with respect to total
The silver compound of 100 mass parts and titanium dioxide, the copper quality in cupric compound is more than 0.01 mass parts, then may be used
See that the ntiviral characteristic under light irradiation can become good.In addition, if with respect to the silver chloride adding up to 100 mass parts and titanium dioxide
Titanium, the copper quality in copper compound is below 20 mass parts, then be prevented from the surface quilt of silver compound and titanium dioxide
Cupric compound is coated to, and improves the photocatalyst activity of antiviral composition.
Here, with respect to the copper in total silver compound of 100 mass parts and the cupric compound of titanium dioxide
Quality, can be calculated by the respective input amount of the raw material of copper compound, silver compound and titanium dioxide.
As long as the copper compound that the valence mumber that cupric compound is copper is 2 is just not particularly limited.Such as cupric compound
It is selected from one of following (a)～(h) or two or more,
The cupric compound of a hydroxyl that () is represented by following formulas (1),
Cu2(OH)3X (1)
(in formula, X represents anion)
(b) cupric halogenide,
(c) cupric inorganic acid salt,
(d) cupric acylate,
(e) copper oxide,
(f) copper sulfide,
(g) copper azide (II),
(h) cupric silicate.
The X of formula (1) is preferably selected from the halogens such as Cl, Br and I, CH3The conjugate base of the carboxylic acids such as COO, NO3(SO4)1/2Deng
Any one in the conjugate base of mineral acid and OH.The X of formula (1) is more preferably selected from Cl, CH3COO、NO3、(SO4)1/2And OH
In any one.In addition, from other viewpoints, the X of formula (1) is more preferably halogen.Preferred in these formulas (1)
Among X, X is more preferably Cl.
B () cupric halogenide is more preferably selected from one of copper chloride, copper fluoride and copper bromide or two or more.
B () cupric halogenide is more preferably copper chloride.
(c) cupric inorganic acid salt be preferably selected from copper sulfate, copper nitrate, Copper diiodate(Cu(IO3)2), cupric perchlorate, cupric oxalate, four
One of copper borate, Tetraamminecopper Sulfate, amido sulfuric acid copper, ammonium chloride copper, Copper pyrophosphate. and curpic carbonate or two or more.(c) two
The inorganic acid salt of valency copper is more preferably copper sulfate.
D () cupric acylate is more preferably cupric carboxylate.As preferably cupric carboxylate, can
Enumerate selected from Tubercuprose., copper acetate, propanoic acid copper, copper butyrate, valeric acid copper, caproic acid copper, enanthic acid copper, cupric octoate, n-nonanoic acid copper, capric acid
Copper, tetradecanoic acid copper, hexadecanoic acid copper, heptadecanoic acid copper, copper stearate, copper oleate, Cupric Lactate., malic acid copper, copper citrate,
Copper benzoate, phthalic acid copper, M-phthalic acid copper, p-phthalic acid copper, copper salicylate, mellic acid. copper, cupric oxalate, third
Diacid copper, succinic acid copper, 1,3-propanedicarboxylic acid copper, adipic acid copper, fumaric acid copper, glycolic copper, glyceric acid copper, copper gluconate, tartaric acid
Copper, acetylacetone copper, ethyl acetoacetate copper, isovaleric acid copper, beta-dihydroxy copper, diacetone copper acetate, formyl succinic acid copper, water
One of poplar acid amide copper, double (2 ethyl hexanoic acid) copper, decanedioic acid copper, copper naphthenate or two or more.Cupric carboxylate
More preferably copper acetate.
The cupric compound of preferably above-mentioned (a) hydroxyl being represented by formula (1) of the cupric compound of the present invention,
(b) cupric halogenide, (c) cupric inorganic acid salt and (d) cupric acylate.Further, since impurity few with
And low cost, the cupric compound of the present invention is more preferably the cupric chemical combination of the hydroxyl that above-mentioned formula (1) represents
Thing.Furthermore, the cupric compound of the hydroxyl that above-mentioned (a) is represented by formula (1) both can be anhydride can also be hydration
Thing.
The mol ratio of the Ag atom in silver compound and the Cu atom in cupric compound is preferably 1:0.0045～1:
451, more preferably 1:0.045～1:451, more preferably 1:0.045～1:338, particularly preferably 1:013～1:226.
If the mol ratio of the Ag atom in silver compound and the Cu atom in cupric compound is 1:0.0045～1:451, then make
The synergy that both silver compound and cupric compound support altogether in titanium dioxide is realized increases.
＜ titanium dioxide ＞
The titanium dioxide that the antibacterial antiviral composition of the present invention is used can be Detitanium-ore-type, rutile-type and plate titanium
Any one crystal habit of ore deposit type, is not particularly limited, it is possible to use any one is it is also possible to be mixed with arbitrary proportion.
Mean diameter for titanium dioxide is not particularly limited, the average grain obtained by BET specific surface area by following formula (2)
Footpath is preferably less than 1 μm, more preferably below 500nm, more preferably below 300nm.It is 1 by the mean diameter of titanium dioxide
Below μm, silver compound and/or cupric compound high dispersive can be supported in titanium dioxide, with antibacterial, viral connecing
Tactile probability improves, and can expect high anti-bacteria and anti-virus performance.
D (mean diameter)=6000/S (BET specific surface area) × ρ (density) (2)
The crystal habit of titanium dioxide and mean diameter can be adjusted, titanium dioxide by its manufacture method, initiation material
Titanium can be manufactured using any one method.But, titanium dioxide is preferably by TiCl4Liquid-phase hydrolysis or gaseous oxidation decompose
And the fine particulate titanium dioxide manufacturing.By by TiCl4As initiation material, a small amount of Cl ion remains in surface, therefore dioxy
Change the evolution reaction of silver compound on titanium surface, be particularly susceptible to the evolution reaction of AgCl from Ag ion, fine silver
Compound easily supports in titanium dioxide.
＜ is supported with the titanium dioxide ＞ of cupric compound and silver compound altogether
In the antibacterial antiviral composition of the present invention, as long as titanium dioxide is supported with cupric compound altogether and patina is closed
Thing, supports shape for it and stepped construction is not specially limited.That is, for make cupric compound and silver compound load
The order being loaded in titanium dioxide is not particularly limited.For example, it is possible to make silver compound support after titanium dioxide, then make to support
The titania supported cupric compound of silver compound.Alternatively, it is also possible to make cupric compound support in titanium dioxide it
Afterwards, then make to have supported the titania supported silver compound of cupric compound.And, cupric compound can also be made simultaneously
Support in titanium dioxide with silver compound.
Method as supporting silver compound in titanium dioxide and/or the titanium dioxide having supported cupric compound,
For example in the case that silver compound is for AgCl, can adopt AgCl powder and titanium dioxide and/or support cupric
Compound titania powder mixing mixing method, so that AgCl colloid is adsorbed in titanium dioxide and/or support copper compound
The colloid adsorption method of titania powder, make Ag ion (AgNO in the liquid phase3、Ag2SO4Deng) and chloride ion (NaCl, ZnCl2、
CuCl2Deng) reaction thus in titanium dioxide and/or supported copper compound titanium dioxide on separate out AgCl liquid phase deposition method
Any one method, but preferably easy liquid phase deposition method in manufacture method.
As making cupric compound support method in titanium dioxide and/or the titanium dioxide having supported silver compound,
Following methods for example can be adopted：By titanium dioxide and/or supported the titania powder of silver compound and the divalent salts of copper
(copper chloride, copper acetate, copper sulfate, copper nitrate etc.), it is preferably mixing in copper chloride (II) addition polar solvent, and then add alkali
Property material (sodium hydrate aqueous solution, potassium hydroxide aqueous solution, calcium hydroxide aqueous solution, lime water, aqueous sodium carbonate, ammonia
Solution, triethylamine aqueous solution, pyridine solution ethylenediamine solution, sodium bicarbonate aqueous solution etc.), make cupric compound two
On titanium oxide and/or supported and separate out on the titanium dioxide of cupric compound.
Method as supporting silver compound and copper compound in titanium dioxide simultaneously, for example, can adopt following sides
Method：Titania powder is made to be scattered in the solution containing Ag ion and Cu ion, simultaneously/or add chloride ion and alkalescence successively
Material, makes silver compound and copper compound separate out simultaneously.
＜ anti-bacteria and anti-virus agent and photocatalyst ＞
The anti-bacteria and anti-virus agent of the present invention and photocatalyst contain the antibacterial antiviral composition of the present invention.Thus, this
Bright anti-bacteria and anti-virus agent and photocatalyst have excellent anti-bacteria and anti-virus characteristic at bright place or dark place.
Occupation mode ＞ of ＜ antibacterial antiviral composition, anti-bacteria and anti-virus agent and photocatalyst
For the antibacterial antiviral composition of the present invention, anti-bacteria and anti-virus agent and photocatalyst (hereinafter sometimes referred to " this
Bright antibacterial antiviral composition etc. ") occupation mode be not particularly limited.For example, it is possible to the anti-bacteria and anti-virus group by the present invention
Compound etc. is used with the form of the solid, shaped such as micropowder and granule.In the case of being somebody's turn to do, such as by the antibacterial antiviral composition of the present invention
Use etc. being filled in predetermined container.Or it is it is also possible to pre- by making antibacterial antiviral composition of the present invention etc. be contained in
The occupation mode of the surface of fixed base material and/or inside carrys out antibacterial antiviral composition using the present invention etc..After generally preferably
The occupation mode of person.Furthermore, as above-mentioned base material, for example, can enumerate fiber, metal, pottery and glass etc. by general part
The single base material constituting and the composite base material being made up of the two or more part among above-mentioned part.But, base material is simultaneously
It is not limited to this.
Antibacterial containing the present invention can resist in the smearss such as the floor polishing wax that can be peeled off by suitable means
Virus composition etc..Alternatively, it is also possible to antibacterial antiviral composition of the present invention etc. is immobilized in predetermined film, make the present invention
Antibacterial antiviral composition etc. expose on the surface of continuous film.Alternatively, it is also possible to the antibacterial by using being dispersed with the present invention
The mode of the coating that the solvent of antiviral composition etc. makes carrys out antibacterial antiviral composition using the present invention etc..
As the material that antibacterial antiviral composition of the present invention etc. is immobilized in substrate surface, for example, can enumerate bonding
Antibacterial antiviral composition of the present invention etc. is immobilized in material of substrate surface etc. using common immobilization means by agent etc..
Organic system binding agent and inorganic system binding agent can be used as immobilized for antibacterial antiviral composition of the present invention etc. bonding
Agent, but the decomposition of the binding agent in order to avoid being led to by photocatalyst material, preferably use inorganic system binding agent.For binding agent
Species be not particularly limited.As inorganic system binding agent for example can enumerate in order to by substance fixed for photocatalyst in substrate surface
And the inorganic system binding agent of the silica-based grade being usually used.As organic system binding agent, for example can enumerate by polymerization and
Solvent volatilization can form polymer binder of thin film etc..
As the material being included in antibacterial antiviral composition of the present invention etc. within base material, for example, can enumerate by making
Antibacterial antiviral composition of the present invention etc. is scattered in resin and makes dispersion and make material obtained from the solidification of this dispersion
Material.As the scattered resin such as antibacterial antiviral composition making the present invention, it is possible to use the appointing of natural resin and synthetic resin
A kind of.As synthetic resin, for example, can enumerate acrylic resin, phenolic resin, polyurethane resin, acrylonitrile/styrene copolymerized
Resin, acrylonitrile/butadiene/styrene copolymer (ABS) resin, polyester resin and epoxy resin etc., but it is not limited to this
A little resins.
Place for the antibacterial antiviral composition using the present invention etc. is not particularly limited.For example except in any light
In the presence of outside, even if antibacterial antiviral composition etc. of the present invention can also be used in the dark.In addition, the antibacterial of the present invention
Even if (medium with sea water in such as water), the drying regime (low humidity in such as winter etc. in presence of water such as antiviral composition
State etc. of degree), under the coexisting of the state of high humility or Organic substance, all there is excellent inactivation of virus characteristic, can be constantly
By inactivation of virus.Antibacterial antiviral composition of the present invention etc. for example can be configured in wall, ground and ceiling etc..In addition,
The building such as hospital and factory, lathe, measure device class, the inside of electric equipment products and part (such as refrigerator, washing machine and wash the dishes
Filter of the inside of machine etc. and air purifier etc.) etc. arbitrary object can be suitable for the anti-bacteria and anti-virus group of the present invention
Compound etc..Machine internal, the storeroom of refrigerator for example can be enumerated as dark place and become dark place at night or when not using
Hospital facility (waiting room, operating room etc.) etc., but it is not limited to this.
All the time, as one of influenza countermeasure, propose to filter titanium dioxide-coated in ceramic filter or non-woven fabrics
Device, and it is assembled with the air purifier for the light source to this filter exposure ultraviolet.But, the antibacterial of the present invention is resisted
Virus composition etc. is used in the case of the filter of air purifier it is not necessary to ultraviolet light source, thus, it is possible to reduce air
The cost of depurator, improves the safety of air purifier.
＜ bacterial viruses ablation method ＞
The bacterial viruses ablation method of the present invention, the antibacterial using the antibacterial antiviral composition of the present invention, the present invention resists
The photocatalyst of viral agent or the present invention is by antibacterial and inactivation of virus.As described above, the antibacterial antiviral composition body of the present invention
Reveal anti-bacteria and anti-virus, therefore, it is possible to the antibacterial antiviral composition using the present invention by antibacterial and inactivation of virus.In addition, by
Contain the antibacterial antiviral composition of the present invention in the anti-bacteria and anti-virus agent of the present invention and photocatalyst, therefore, it is possible to using this
Bright anti-bacteria and anti-virus agent or photocatalyst are by antibacterial and inactivation of virus.
Embodiment
Hereinafter, by embodiment, the present invention is specifically described, but the present invention is not limited to these embodiments.
Furthermore, each spy of the antibacterial antiviral composition of embodiment and comparative example is obtained according to method described below
Property.
(1) X-ray diffraction pattern measures
Investigate the X-ray diffraction pattern of the antibacterial antiviral composition of embodiment and comparative example, investigate antibacterial disease-resistant
The state of the Ag in malicious compositionss.X-ray diffraction pattern measures and uses copper target, using Cu-K α 1 line, tube voltage be 45kV,
Tube current is 40mA, measurement range is 2 θ=20～80deg, sampling width is 0.0167deg, scanning speed is 1.1deg/min
Under conditions of carry out.
Measure the X ' perPRO that used device is Panalytical company system.
(2) mean diameter of the silver compound observed by scanning electron microscope
Using scanning electron microscope ((strain) Hitachi Ha イ テ Network ノ ロ ジ ズ system, model：S-5500) measure
The mean diameter of the silver compound in the antibacterial antiviral composition of embodiment and comparative example.Determine patina as follows
The mean diameter of compound.
Survey the diameter (AgCl) of 100 particles emitting white light in backscattered electron image, counted average as flat
All particle diameters.In addition, so-called particle diameter, in particle for referring to diameter in the case of spherical, in the case that particle is for beyond spherical it is
Refer to centroidal the longest while with the shortest while being added divided by 2.
(3) backscattered electron image being obtained by scanning electron microscope and the observation of secondary electron image
Using scanning electron microscope ((strain) Hitachi Ha イ テ Network ノ ロ ジ ズ system, model：S-5500) observe
Backscattered electron image in the antibacterial antiviral composition of embodiment and comparative example and secondary electron image.In anti-bacteria and anti-virus group
In the backscattered electron image and secondary electron image of compound, cupric compound in antibacterial antiviral composition, silver compound and
The profile of titanium dioxide is different.Therefore, by observing backscattered electron image and secondary electron image in antibacterial antiviral composition,
Cupric compound can be investigated and silver compound supports the state in titanium dioxide.
(4) antiviral property (inactivation of phage)
《The evaluation of inactivation of virus performance：LOG(N/N0) mensure》
With regard to inactivation of virus performance, confirmed by using the model test of phage and using following methods.In addition, surveying
Method of determining is carried out on the basis of JIS R 1756.
The solution coating being dispersed with powder test portion in ethanol on glass plate (50mm × 50mm × 1mm), in room temperature
Under diel is dried, made the coating weight of per unit area and 1.0g/m be calculated as with powder conversion2Anti-bacteria and anti-virus evaluation use
Test portion.
Apply filter paper in deep type disk, add a small amount of sterilized water.The evaluation test portion of above-mentioned record is placed on filter paper
On.Phage-infect titre to the use 1/500NB modulation of the 100 μ L that drip thereon is about 6.7 × 106～2.6 ×
107Q phagus beta (NBRC20012) suspension of pfu/mL, in order that test portion surface is contacted with phage and covers PET and (gather
Ethylene glycol terephthalate) thin film made.Cover this deep type disk with glass plate, as mensure assembly.Prepare multiple same
The mensure assembly of sample.
In addition, as light source on 15W white fluorescent lamp (パ Na ソ ニ ッ Network (strain) makes, whole white fluorescent lamp, FL15N)
It is mounted with that ultraviolet cutoff light filter (day east Resin Industry (strain) makes, N-113) uses.(make for 1000 luxs in illumination
Use illumination meter：(strain) ト プ U Application IM-5 measure) position stand multiple mensure assemblies.Start to little through 1 from light irradiation
When after carried out the phage concentration mensuration of test portion on glass plate.In addition, measure when room illumination be 200 luxs with
Under.
Carry out the mensure of phagocytosis bulk concentration using following methods.The test portion on glass plate is made to infiltrate the phage of 9.9mL
Recovered liquid (SCDLP culture medium), using vibration machine vibration 10 minutes.By this normal saline containing peptone for phage recovered liquid
Suitably dilute.To being mixed with 5.0 × 10 separately cultivating8～2.0 × 109Escherichia coli (NBRC106373) culture fluid of individual/mL
In the liquid of the LB soft agar medium adding calcium, after the liquid of dilution is mixed before adding 1mL, this liquid is applied and spreads
In the LB soft agar medium adding calcium, after 37 DEG C of cultures 15 hours, determine the speckle quantity of phage by visual observation.Logical
Cross obtained plaque quantity to be multiplied by the dilution ratio of phage recovered liquid and obtain phagocytosis bulk concentration N.
By initial phagocytosis bulk concentration N0Obtain phage relative concentration (LOG with the phagocytosis bulk concentration N after the scheduled time
(N/N0)).Furthermore, LOG (N/N0) value less (negative value is bigger), the ntiviral characteristic of test portion is more excellent.
(the evaluation of the ntiviral characteristic of dark place：LOG(N/N0) mensure)
Mensure assembly is placed in dark place, not from light source irradiation light, carried out in addition with above-mentioned (bright place disease-resistant
The evaluation of malicious characteristic：LOG(N/N0) mensure) same mensure.Furthermore, LOG (N/N0) value less (negative value is bigger), test portion
Ntiviral characteristic more excellent.
(5) anti-microbial property (escherichia coli, the inactivation of staphylococcus aureuses)
《The evaluation of bacteria inactivation performance：LOG(N/N0) mensure》
With regard to bacteria inactivation performance, by using the model test of escherichia coli or staphylococcus aureuses and adopt with
Lower method confirms.In addition, this method is carried out on the basis of JIS R 1752.
Apply filter paper in deep type disk, add a small amount of sterilized water.The evaluation test portion of above-mentioned record is placed on filter paper
On.Escherichia coli (NBRC3972) or staphylococcus aureuses to the use 1/500NB modulation of the 100 μ L that drip thereon
(NBRC12732) bacterial population is about 6.7 × 105～2.6 × 106The antibacterial liquid of individual/mL, in order that test portion surface and antibacterial connect
Touch and cover the thin film that PET (polyethylene terephthalate) makes.Cover this deep type disk with glass plate, as mensure group
Part.Multiple same mensure assemblies are prepared.
In addition, as light source on 15W white fluorescent lamp (パ Na ソ ニ ッ Network (strain) makes, whole white fluorescent lamp, FL15N)
It is mounted with that ultraviolet cutoff light filter (day east Resin Industry (strain) makes, N-113) uses.(make for 1000 luxs in illumination
Use illumination meter：(strain) ト プ U Application IM-5 measure) position stand multiple mensure assemblies.Start to little through 1 from light irradiation
When after carried out the phage concentration mensuration of test portion on glass plate.In addition, measure when room illumination be 200 luxs with
Under.
Carry out the mensure of bacterial concentration using following methods.The antibacterial that the test portion on glass plate infiltrates 9.9mL is made to reclaim
Liquid (SCDLP culture medium), using vibration machine vibration 10 minutes.This antibacterial recovered liquid normal saline is suitably diluted.1mL is dilute
Put into culture dish after the liquid released and agar culture medium mixing, after 37 DEG C of cultures 15 hours, determine bacterial population by visual observation.
The dilution ratio of recovered liquid is multiplied by by obtained bacterial population and obtains bacterial concentration N.
By initial bacterial concentration N0Obtain antibacterial relative concentration (LOG (N/N with the bacterial concentration N after the scheduled time0)).
Furthermore, LOG (N/N0) value less (negative value is bigger), the antibacterial characteristics of test portion are more excellent.
(the evaluation of the antibacterial characteristics of dark place：LOG(N/N0) mensure)
Mensure assembly is placed in dark place, not from light source irradiation light, has carried out in addition and the above-mentioned (antibacterial at bright place
The evaluation of characteristic：LOG(N/N0) mensure) same mensure.Furthermore, LOG (N/N0) value less (negative value is bigger), test portion
Antibacterial characteristics are more excellent.
Embodiment 1：
The anatase titanium dioxide (Showa electrotechnical ceramics (strain) system) making 5g in 200mL distilled water suspends and makes outstanding
Supernatant liquid, and prepared the AgNO being dissolved with 0.296g of each 50mL respectively3The solution in (Northeast chemistry (strain) system) and being dissolved with
The solution of the NaCl (Northeast chemistry (strain) system) of 0.204g, by AgNO3Solution and NaCl solution put in suspension successively.So
Afterwards, it is stirred at room temperature 10 minutes.Obtained suspension is filtered, is dried, resulting in the Detitanium-ore-type supporting AgCl
Titania powder (with respect to the AgCl of titania supported 5 mass parts of 100 mass parts).
The AgCl/ titania powder making 3g in 200mL distilled water suspends and makes suspension, adds to this suspension
The CuCl of 0.04g (0.5 mass parts being calculated as with copper with respect to the AgCl/ rutile titania powder of 100 mass parts)2·
2H2O (Northeast chemistry (strain) system), stirs 10 minutes.Add sodium hydroxide (Northeast chemistry (strain) system) aqueous solution of 1mol/L with
Make the pH value of suspension become 10, carry out stirring in 30 minutes and be obtained by mixing serosity.This serosity is filtered, cleans institute with pure water
The powder body obtaining, in 80 DEG C of dryings, is pulverized with blender, has made the test portion of embodiment 1.Furthermore, CuCl2·2H2O is hydrolyzed into
For Cu2(OH)3Cl.
PH meter employs (strain) hole field and makes made D-51.
Embodiment 2：
In addition to making AgCl loading be 1 mass parts with respect to 100 mass parts titanium dioxide, using same with embodiment 1
The method of sample has made the test portion of embodiment 2.
Embodiment 3：
In addition to making AgCl loading be 0.1 mass parts with respect to 100 mass parts titanium dioxide, adopt and embodiment 1
Same method has made the test portion of embodiment 3.
Embodiment 4：
In addition to anatase titanium dioxide is changed into rutile titanium dioxide (Showa electrotechnical ceramics (strain) system), adopt
Make the test portion of embodiment 4 of method similarly to Example 1.
Embodiment 5：
In addition to anatase titanium dioxide is changed into brookite type titanium dioxide (Showa electrotechnical ceramics (strain) system), adopt
Make the test portion of embodiment 5 of method similarly to Example 1.
Comparative example 1：
To by the AgNO of 5.920g3(Northeast chemistry (strain) system) is dissolved in the solution of 300mL distilled water, puts into 50mL molten
Solution has the solution of the NaCl (Northeast chemistry (strain) system) of 4.080g.Then, it is stirred at room temperature 10 minutes.By obtained suspension
Filter, be dried, resulting in the test portion (AgCl powder) of comparative example 1.
Comparative example 2：
So that the AgCl powder of comparative example 1 is suspended in 100mL distilled water and make suspension, add to this suspension
The CuCl of 0.04g (0.5 mass parts being calculated as with copper with respect to the AgCl powder of 100 mass parts)2·2H2O (Northeast chemistry (strain)
System), stir 10 minutes.Sodium hydroxide (Northeast chemistry (strain) system) aqueous solution adding 1mol/L is so that the pH value of suspension is changed into
10, carry out stirring in 30 minutes and be mixed to get serosity.This serosity is filtered, the powder body obtained by being cleaned with pure water, dry at 80 DEG C
Dry, pulverized with blender, made the test portion (Cu compound/AgCl powder) of comparative example 2.Furthermore, CuCl2·2H2O is hydrolyzed into
For Cu2(OH)3Cl.
Comparative example 3：
By silver compound is only supported by the Detitanium-ore-type being used in embodiment 1 using method similarly to Example 1
Titanium dioxide, has obtained the test portion (AgCl/TiO of comparative example 32Powder).
Comparative example 4：
The anatase titanium dioxide powder that embodiment 1 is used is made to suspend in 100mL distilled water and make suspension,
Add the CuCl of 0.04g (0.5 mass parts being calculated as with copper with respect to the titania powder of 100 mass parts) to this suspension2·
2H2O (Northeast chemistry (strain) system), stirs 10 minutes.Add sodium hydroxide (Northeast chemistry (strain) system) aqueous solution of 1mol/L with
Make the pH value of suspension be changed into 10, carry out stirring in 30 minutes and be mixed to get serosity.This serosity is filtered, cleans gained with pure water
The powder body arriving, in 80 DEG C of dryings, is pulverized with blender, has made the test portion (Cu compound/titania powder) of comparative example 3.
Furthermore, CuCl2·2H2O hydrolysis becomes Cu2(OH)3Cl.
Comparative example 5：
Former state employs the anatase titanium dioxide that embodiment 1 is used.
＜ result ＞
(X-ray diffraction pattern mensure)
The compound comprising Ag present in the test portion of embodiment 1～5 and comparative example 1～5 is all confirmed as chlorination
The AgCl of sodium form structure.As one, the X-ray diffraction pattern of the test portion of embodiment 1 is shown in Fig. 1.
(backscattered electron image and secondary electron image are observed)
The photo of the backscattered electron image of embodiment 1 is shown in Fig. 2, the photo of the secondary electron image of comparative example 1 is shown in
Fig. 3.In FIG, especially bright particle in backscattered electron image can be determined that the place that the Ag as heavy element exists.By
These photos understand that the AgCl of about 50nm size in embodiment 1 is supported in titanium dioxide.On the other hand it is known that comparative example 1
AgCl become the oversize grain of hundreds of micron of size.From the comparison of embodiment 1 and comparative example 1, by supporting in dioxy
Change titanium, being sized to of AgCl becomes very little.
By the silver compound obtained from antibacterial antiviral composition with regard to above embodiment 1～5 and comparative example 1～5
Mean diameter and the data of antibacterial, antiviral property be shown in table 1.
Table 1 embodiment and the evaluation result of comparative example
Understand embodiment 1～5 test portion illumination be 1000 luxs radiation of visible light under, such short at 1 hour
Time has more than 99% Virus inactivation capacity.In the photocatalyst of comparative example 1～5, even if under the same conditions, also several
Do not show antiviral property.This be due to the structure of comparative example 1 lack silver compound, copper compound and titanium dioxide these three
Any one of composition.
Although the test portion of comparative example 1～3 shows activity to escherichia coli, staphylococcus aureuses, this is Ag chemical combination
The effect that thing brings, does not therefore have the function as photocatalyst it is impossible to expect that semipermanent uses.The examination of comparative example 4 and 5
Material does not comprise antibiotic property, the visible absorption source realized by Ag, does not therefore show activity for virus, both antibacterials.
From the contrast of embodiment 1～5 and comparative example 1～5, by by silver compound, copper compound, titanium dioxide this
Three combines, for antibacterial and both display inactivating efficacy of virus.
Claims (14)
1. a kind of antibacterial antiviral composition, comprises to be supported with the titanium dioxide of cupric compound and silver compound altogether.
2. antibacterial antiviral composition according to claim 1, described silver compound is the halogenide of silver.
3. antibacterial antiviral composition according to claim 2, the halogenide of described silver is AgCl.
4. the antibacterial antiviral composition according to any one of claims 1 to 3, with respect to described the two of 100 mass parts
Titanium oxide, the loading of described silver compound is 0.01～20 mass parts.
5. the antibacterial antiviral composition according to any one of Claims 1 to 4, is observed by scanning electron microscope
Described silver compound mean diameter be 1nm～1 μm.
6. the antibacterial antiviral composition according to any one of Claims 1 to 5, with respect to the institute of total 100 mass parts
State titanium dioxide and described silver compound, the copper quality of described cupric compound is 0.01～20 mass parts.
7. the antibacterial antiviral composition according to any one of claim 1～6, the Ag atom in described silver compound with
The mol ratio of the Cu atom in described cupric compound is 1:0.0045～1:451.
8. the antibacterial antiviral composition according to any one of claim 1～7, described cupric compound is to be selected from down
State one of (a)～(h) or two or more,
The cupric compound of a hydroxyl that () is represented by following formulas (1),
Cu2(OH)3X (1)
In formula, X represents anion,
(b) cupric halogenide,
(c) cupric inorganic acid salt,
(d) cupric acylate,
(e) copper oxide,
(f) copper sulfide,
(g) copper azide,
(h) cupric silicate.
9. antibacterial antiviral composition according to claim 8, the X of formula (1) be selected from halogen, the conjugate base of carboxylic acid,
One of the conjugate base of mineral acid and OH or two or more.
10. antibacterial antiviral composition according to claim 8 or claim 9, X is selected from Cl, CH3COO、NO3(SO4)1/2In
One or more.
11. antibacterial antiviral compositions according to any one of claim 1～10, having by illumination is 1000 Le gram
This radiation of visible light 1 hour and by more than 99% bacterial viruses inactivation ability.
A kind of 12. anti-bacteria and anti-virus agent, the antibacterial antiviral composition described in any one containing claim 1～11.
A kind of 13. photocatalysts, the antibacterial antiviral composition described in any one containing claim 1～11.
A kind of 14. bacterial viruses ablation methods, the antibacterial antiviral composition described in any one of usage right requirement 1～11,
Anti-bacteria and anti-virus agent described in claim 12 or the photocatalyst described in claim 13 are by antibacterial and inactivation of virus.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2014191353 | 2014-09-19 | ||
| JP2014-191353 | 2014-09-19 | ||
| PCT/JP2015/070726 WO2016042913A1 (en) | 2014-09-19 | 2015-07-21 | Antibacterial/antiviral composition, antibacterial/antiviral agent, photocatalyst, and bacteria/virus inactivation method |
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|---|---|
| CN106470550A true CN106470550A (en) | 2017-03-01 |
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| Country | Link |
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| JP (1) | JPWO2016042913A1 (en) |
| KR (1) | KR20170010408A (en) |
| CN (1) | CN106470550A (en) |
| TW (1) | TW201618672A (en) |
| WO (1) | WO2016042913A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107164995A (en) * | 2017-05-24 | 2017-09-15 | 常德金德镭射科技股份有限公司 | A kind of preparation method of antimildew and antibacterial coating paper |
| CN111296416A (en) * | 2018-12-12 | 2020-06-19 | 韩国绿水滴(株) | Antibacterial, antifungal and antiviral composition with enhanced deodorizing function and preparation method thereof |
| CN111661898A (en) * | 2020-07-09 | 2020-09-15 | 广西碧福环保工程有限公司 | Multi-ion strong oxidation catalytic sterilizer |
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| CN113226039A (en) * | 2018-12-06 | 2021-08-06 | 隆萨解决方案股份公司 | Copper chelate complexes for antifouling protection |
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| CN112080940B (en) * | 2020-08-21 | 2022-01-14 | 中国科学院金属研究所 | Fabric with lasting antibacterial and antiviral properties and preparation method thereof |
| CN114271292A (en) * | 2020-09-27 | 2022-04-05 | 苏州森锋医疗器械有限公司 | Disinfectant and preparation method thereof |
| CN114271292B (en) * | 2020-09-27 | 2023-09-01 | 苏州森锋医疗器械有限公司 | Disinfectant and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2016042913A1 (en) | 2017-04-27 |
| WO2016042913A1 (en) | 2016-03-24 |
| KR20170010408A (en) | 2017-01-31 |
| TW201618672A (en) | 2016-06-01 |
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