CN106630631B - A kind of antiseptic sanitary glaze and preparation method - Google Patents
A kind of antiseptic sanitary glaze and preparation method Download PDFInfo
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- CN106630631B CN106630631B CN201611029670.1A CN201611029670A CN106630631B CN 106630631 B CN106630631 B CN 106630631B CN 201611029670 A CN201611029670 A CN 201611029670A CN 106630631 B CN106630631 B CN 106630631B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 50
- 230000002421 anti-septic effect Effects 0.000 title claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 103
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 55
- 150000001875 compounds Chemical class 0.000 claims abstract description 40
- 239000000919 ceramic Substances 0.000 claims abstract description 39
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 33
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 claims abstract description 29
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 17
- MHLYOTJKDAAHGI-UHFFFAOYSA-N silver molybdate Chemical compound [Ag+].[Ag+].[O-][Mo]([O-])(=O)=O MHLYOTJKDAAHGI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000019738 Limestone Nutrition 0.000 claims abstract description 11
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 11
- NDUKHFILUDZSHZ-UHFFFAOYSA-N [Fe].[Zr] Chemical compound [Fe].[Zr] NDUKHFILUDZSHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001913 cellulose Substances 0.000 claims abstract description 11
- 229920002678 cellulose Polymers 0.000 claims abstract description 11
- 239000006028 limestone Substances 0.000 claims abstract description 11
- 239000002689 soil Substances 0.000 claims abstract description 11
- 238000001228 spectrum Methods 0.000 claims abstract description 11
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 11
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010459 dolomite Substances 0.000 claims abstract description 10
- 229910000514 dolomite Inorganic materials 0.000 claims abstract description 10
- 239000011787 zinc oxide Substances 0.000 claims abstract description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 40
- 239000011609 ammonium molybdate Substances 0.000 claims description 35
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 35
- 229940010552 ammonium molybdate Drugs 0.000 claims description 35
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 28
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 26
- 239000004411 aluminium Substances 0.000 claims description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 21
- 229910052782 aluminium Inorganic materials 0.000 claims description 21
- 230000000845 anti-microbial effect Effects 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 14
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 14
- 238000010304 firing Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims 2
- 239000011701 zinc Substances 0.000 claims 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 239000002131 composite material Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 230000003115 biocidal effect Effects 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 3
- -1 frit Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 44
- 241000894006 Bacteria Species 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 238000010790 dilution Methods 0.000 description 9
- 239000012895 dilution Substances 0.000 description 9
- 230000001954 sterilising effect Effects 0.000 description 8
- 239000013068 control sample Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 230000001580 bacterial effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000036541 health Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000009630 liquid culture Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000006916 nutrient agar Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-OIOBTWANSA-N zinc-62 Chemical compound [62Zn] HCHKCACWOHOZIP-OIOBTWANSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2204/00—Glasses, glazes or enamels with special properties
- C03C2204/02—Antibacterial glass, glaze or enamel
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2205/00—Compositions applicable for the manufacture of vitreous enamels or glazes
- C03C2205/04—Compositions applicable for the manufacture of vitreous enamels or glazes for self-cleaning enamels or glazes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to ceramic technology field, it is related to a kind of antiseptic sanitary glaze and preparation method, the antiseptic sanitary glaze, including the following raw material: potassium feldspar, sandstone, dolomite, lime stone, zirconium English powder, frit, aluminium oxide, zinc oxide, Suzhou soil, zirconium iron pink, spectrum is yellow, cellulose, compound antibacterial powder；The compound antibacterial powder includes the raw material of following mass percentage: silver molybdate 15~20%, zinc molybdate 60~65%, titanium dioxide 20~25%；The preparation method of its antiseptic sanitary glaze, comprising the following steps: the preparation of A, compound antibacterial powder, the preparation of B, glaze slip, C, the preparation of antiseptic sanitary glaze, preparation method of the present invention is simple, easy to operate, antiseptic sanitary glaze high temperature resistant, non-discolouring, antibiotic property is excellent.
Description
Technical field
The invention belongs to ceramic technology field more particularly to a kind of antiseptic sanitary glaze and preparation methods.
Background technique
With the improvement of people ' s living standards with the enhancing of environmental consciousness, people increasingly pay close attention to daily necessity pair at one's side
The influence of own health.And the sanitary ceramic product of family kitchen, toilet, especially hospital, public place easily breeds bacterium,
Influence people's health.Antiseptic sanitary is a kind of new function material for protecting environment, it is by antimicrobial technology and ceramic material
Material combines, and it is original using function, decorative effect and while physical and chemical performance not only to have maintained ceramic, but increase antibacterial,
Sterilization and self-cleaning function, can be widely used in the environment such as health, medical treatment, family room.
Early in late 1980s, the developed countries such as Japan, the U.S., European Union open in hospital, dining room, high-end residential etc.
Begin using the construction sanitary ceramic product with antibacterial functions, domestic average family also gradually begins to use anti-bacteria ceramic in recent years
Product.Simultaneously at present antiseptic sanitary there are high production cost, Durability of antimicrobial effect is poor, anti-microbial property is bad the problems such as.
Summary of the invention
Technical problem to be solved by the invention is to provide the antiseptic sanitary glaze of a kind of low cost, excellent antibacterial performance
And preparation method.
The technical scheme to solve the above technical problems is that
A kind of antiseptic sanitary glaze, including following raw material: 23~24 parts of potassium feldspar, 34~35 parts of sandstone, white
3~4 parts of marble, 11~12 parts of lime stone, 9~11 parts of zirconium English powder, 4~6 parts of frit, 2~3 parts of aluminium oxide, 2~3 parts of zinc oxide,
4~5 parts of Suzhou soil, 0.01~0.03 part of zirconium iron pink, spectrum is 0.06~0.08 part yellow, and 0.1~0.2 part of cellulose, compound antibacterial powder
2~3 parts of body；
The compound antibacterial powder includes the raw material of following mass percentage: silver molybdate 15~20%, and zinc molybdate 60~
65%, titanium dioxide 20~25%.
Further, a kind of antiseptic sanitary glaze, including following raw material: 23.5 parts of potassium feldspar, sandstone
34.5 parts, 3.5 parts of dolomite, 11.5 parts of lime stone, 10 parts of zirconium English powder, 5 parts of frit, 2.5 parts of aluminium oxide, 2.5 parts of zinc oxide, Soviet Union
4.5 parts of state soil, 0.02 part of zirconium iron pink, spectrum is 0.07 part, 0.15 part of cellulose, 2.5 parts of compound antibacterial powder yellow；
The compound antibacterial powder includes the raw material of following mass percentage: silver molybdate 18%, zinc molybdate 62%, dioxy
Change titanium 20%.
A kind of preparation method of antiseptic sanitary glaze, comprising the following steps:
A, the preparation of compound antibacterial powder
The preparation of molybdic acid aluminium powder: by silver nitrate, 2:1~1.2 are added separately in deionized water in molar ratio with ammonium molybdate
Silver nitrate solution and ammonium molybdate solution are prepared, both the above solution is placed in 10~15min of mixing in reactor, is then set
3~5min of heating reaction in the micro-wave oven that power is 800~1000W, gained light yellow precipitate is washed with distilled water, mistake
Filter, dry 10~12h under 60~70 DEG C of constant temperatures, obtains the molybdic acid aluminium powder that partial size is 2~4 μm；
The preparation of zinc molybdate powder: by zinc nitrate, 1:1.2 is added separately to match in deionized water in molar ratio with ammonium molybdate
Zinc nitrate solution, is then slowly dropped in ammonium molybdate solution by zinc nitrate solution and ammonium molybdate solution processed, and stirring 20~
30min, gained white depositions are washed with distilled water, filter, and dry 10~12h, obtains grain under 80~100 DEG C of constant temperatures
The zinc molybdate powder that diameter is 3~5 μm；
Titanium dioxide powder, molybdic acid aluminium powder, zinc molybdate powder that partial size is 2~3 μm are mixed according to the ratio, obtained compound
Antimicrobial powder；
B, the preparation of glaze slip
The raw material of compound antibacterial powder and other proportions in step A is added in ball mill, carries out wet ball grinding to glaze
It is 2~4% that slurry fineness, which is 325 mesh 10000-hole sieve screen over-sizes, obtains glaze slip；
C, the preparation of antiseptic sanitary glaze
Glaze slip in step B is imposed on sanitary ceramic body surface, using tunnel oven, is aoxidized at 1200~1250 DEG C
It is fired in atmosphere, heating rate is 2.5~3 DEG C/min, and firing period is 16~18h, keeps the temperature 2~3h, i.e., in sanitary ceramics
Antiseptic sanitary glaze is obtained in billet surface.
The beneficial effects of the present invention are:
1) present invention synthesizes silver molybdate, zinc molybdate antimicrobial powder using chemical synthesis, and preparation method is simple to operation, former
Expect at low cost.
2) silver molybdate, zinc molybdate and titanium dioxide powder are formed into compound antibacterial powder in proportion, by it as additive
It is introduced into ceramic glaze, there is reliable antibiotic property, glaze is non-discolouring when high temperature.
Its Antibacterial Mechanism of antiseptic sanitary glaze of the present invention: first is that due to the presence of moisture, silver molybdate, the zinc molybdate of glaze
The silver-colored zinc ion being sustained out enters in bacterial body, destroys the respiratory system and electron-transport system of microbial cell, causes enzyme
Damage；Second is that silver ion and optically catalytic TiO 2 and be adsorbed in the water on its surface and oxygen formed highly active hydroxyl from
It by base and active oxygen, can be reacted with most organic matters (including the organic matter in bacterium), carbon dioxide and water be generated, thus short
Bacterium is killed in time, stench and greasy dirt is eliminated, to guarantee glaze antibiotic property.
Detailed description of the invention
Fig. 1 is non-antibacterial Ceramic glaze electromicroscopic photograph figure；
Fig. 2 is anti-bacteria ceramic glaze electromicroscopic photograph figure of the present invention；
Fig. 3 is non-antibacterial ceramic blank glaze faying face scanning electron microscope (SEM) photograph；
Fig. 4 is anti-bacteria ceramic glaze-body bonding Surface scan electron microscope of the present invention.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
Fig. 1 is non-antibacterial Ceramic glaze electromicroscopic photograph figure
Fig. 2 is anti-bacteria ceramic glaze electromicroscopic photograph figure of the present invention, it can be seen that there are cubic for antiseptic sanitary glaze
Crystal, due to be added compound antibacterial powder caused by, and glaze face color with for add compound antibacterial powder it is consistent.
Fig. 3 is non-antibacterial ceramic blank glaze faying face scanning electron microscope (SEM) photograph
Fig. 4 is anti-bacteria ceramic glaze-body bonding Surface scan electron microscope of the present invention, it can be seen that after compound antibacterial powder is added, base
Glaze junction quality has not significant impact.
Embodiment 1
A, the preparation of compound antibacterial powder
The preparation of molybdic acid aluminium powder: by silver nitrate, 2:1 is added separately to prepare in deionized water in molar ratio with ammonium molybdate
Both the above solution is placed in reactor and 10min is mixed by silver nitrate solution and ammonium molybdate solution, is subsequently placed in power and is
Heating reaction 3min in the micro-wave oven of 800W, gained light yellow precipitate is washed with distilled water, filters, under 60 DEG C of constant temperatures
Dry 10h obtains the molybdic acid aluminium powder that partial size is 2 μm；
The preparation of zinc molybdate powder: by zinc nitrate, 1:1.2 is added separately to match in deionized water in molar ratio with ammonium molybdate
Zinc nitrate solution, is then slowly dropped in ammonium molybdate solution by zinc nitrate solution and ammonium molybdate solution processed, stirs 20min, institute
It obtains white depositions to be washed with distilled water, filter, the dry 10h under 80 DEG C of constant temperatures obtains the molybdic acid zinc powder that partial size is 3 μm
Body；
Titanium dioxide powder, molybdic acid aluminium powder, zinc molybdate powder that partial size is 2 μm are mixed according to the ratio, obtained compound anti-
Bacterium powder.
B, the preparation of glaze slip
By 23 parts of potassium feldspar, 34 parts of sandstone, 3 parts of dolomite, 11 parts of lime stone, 9 parts of zirconium English powder, 4 parts of frit, aluminium oxide 2
Part, 2 parts of zinc oxide, 4 parts of Suzhou soil, 0.01 part of zirconium iron pink, spectrum is 0.06 part, 0.1 part of cellulose, 2 parts of compound antibacterial powder yellow；Institute
State the raw material that compound antibacterial powder includes following mass percentage: silver molybdate 15%, zinc molybdate 60%, titanium dioxide 25%,
It is added in ball mill, it is 2% that progress wet ball grinding to glaze slip fineness, which is 325 mesh 10000-hole sieve screen over-sizes, obtains glaze slip；
C, the preparation of antiseptic sanitary glaze
Glaze slip in step B is imposed on sanitary ceramic body surface, using tunnel oven, at 1200 DEG C in oxidizing atmosphere
It fires, heating rate is 2.5 DEG C/min, firing period 16h, keeps the temperature 2h, i.e., is resisted on sanitary ceramic body surface
Bacterium sanitary ceramics glaze.
Embodiment 2
A, the preparation of compound antibacterial powder
The preparation of molybdic acid aluminium powder: by silver nitrate, 2:1.1 is added separately to match in deionized water in molar ratio with ammonium molybdate
Silver nitrate solution and ammonium molybdate solution processed, both the above solution are placed in reactor, 13min are mixed, be subsequently placed in power
For heating reaction 4min in the micro-wave oven of 900W, gained light yellow precipitate is washed with distilled water, filters, in 65 DEG C of constant temperatures
Lower dry 11h obtains the molybdic acid aluminium powder that partial size is 3 μm；
The preparation of zinc molybdate powder: by zinc nitrate, 1:1.2 is added separately to match in deionized water in molar ratio with ammonium molybdate
Zinc nitrate solution, is then slowly dropped in ammonium molybdate solution by zinc nitrate solution and ammonium molybdate solution processed, stirs 25min, institute
It obtains white depositions to be washed with distilled water, filter, the dry 11h under 90 DEG C of constant temperatures obtains the molybdic acid zinc powder that partial size is 4 μm
Body；
Titanium dioxide powder, molybdic acid aluminium powder, zinc molybdate powder that partial size is 2.5 μm are mixed according to the ratio, obtained compound
Antimicrobial powder.
B, the preparation of glaze slip
By 23.5 parts of potassium feldspar, 34.5 parts of sandstone, 3.5 parts of dolomite, 11.5 parts of lime stone, 10 parts of zirconium English powder, frit 5
Part, 2.5 parts of aluminium oxide, 2.5 parts of zinc oxide, 4.5 parts of Suzhou soil, 0.02 part of zirconium iron pink, spectrum is 0.07 part yellow, and 0.15 part of cellulose,
2.5 parts of compound antibacterial powder；The compound antibacterial powder includes the raw material of following mass percentage: silver molybdate 18%, molybdic acid
Zinc 62%, titanium dioxide 20% are added in ball mill, and carrying out wet ball grinding to glaze slip fineness is that 325 mesh 10000-hole sieve screen over-sizes are
3%, obtain glaze slip；
C, the preparation of antiseptic sanitary glaze
Glaze slip in step B is imposed on sanitary ceramic body surface, using tunnel oven, at 1230 DEG C in oxidizing atmosphere
It fires, heating rate is 2.8 DEG C/min, firing period 17h, keeps the temperature 2.5h, i.e., obtains on sanitary ceramic body surface
Antiseptic sanitary glaze.
Embodiment 3
A, the preparation of compound antibacterial powder
The preparation of molybdic acid aluminium powder: by silver nitrate, 2:1.2 is added separately to match in deionized water in molar ratio with ammonium molybdate
Silver nitrate solution and ammonium molybdate solution processed, both the above solution are placed in reactor, 15min are mixed, be subsequently placed in power
For heating reaction 5min in the micro-wave oven of 1000W, gained light yellow precipitate is washed with distilled water, filters, in 70 DEG C of constant temperature items
Dry 12h under part, obtains the molybdic acid aluminium powder that partial size is 4 μm；
The preparation of zinc molybdate powder: by zinc nitrate, 1:1.2 is added separately to match in deionized water in molar ratio with ammonium molybdate
Zinc nitrate solution, is then slowly dropped in ammonium molybdate solution by zinc nitrate solution and ammonium molybdate solution processed, stirs 30min, institute
It obtains white depositions to be washed with distilled water, filter, the dry 12h under 100 DEG C of constant temperatures obtains the zinc molybdate that partial size is 5 μm
Powder；
Titanium dioxide powder, molybdic acid aluminium powder, zinc molybdate powder that partial size is 3 μm are mixed according to the ratio, obtained compound anti-
Bacterium powder.
B, the preparation of glaze slip
By 24 parts of potassium feldspar, 35 parts of sandstone, 4 parts of dolomite, 12 parts of lime stone, 11 parts of zirconium English powder, 6 parts of frit, aluminium oxide 3
Part, 3 parts of zinc oxide, 5 parts of Suzhou soil, 0.03 part of zirconium iron pink, spectrum is 0.08 part, 0.2 part of cellulose, 3 parts of compound antibacterial powder yellow；Institute
State the raw material that compound antibacterial powder includes following mass percentage: silver molybdate 15%, zinc molybdate 65%, titanium dioxide 20%,
It is added in ball mill, it is 4% that progress wet ball grinding to glaze slip fineness, which is 325 mesh 10000-hole sieve screen over-sizes, obtains glaze slip；
C, the preparation of antiseptic sanitary glaze
Glaze slip in step B is imposed on sanitary ceramic body surface, using tunnel oven, at 1250 DEG C in oxidizing atmosphere
It fires, heating rate is 3 DEG C/min, firing period 18h, keeps the temperature 3h, i.e., obtains antibacterial on sanitary ceramic body surface
Sanitary ceramics glaze.
Comparative example 1
A, the preparation of compound antibacterial powder
The preparation of molybdic acid aluminium powder: by silver nitrate, 2:1.1 is added separately to match in deionized water in molar ratio with ammonium molybdate
Silver nitrate solution and ammonium molybdate solution processed, both the above solution are placed in reactor, 13min are mixed, be subsequently placed in power
For heating reaction 4min in the micro-wave oven of 900W, gained light yellow precipitate is washed with distilled water, filters, in 65 DEG C of constant temperatures
Lower dry 11h obtains the molybdic acid aluminium powder that partial size is 3 μm；
The preparation of zinc molybdate powder: by zinc nitrate, 1:1.2 is added separately to match in deionized water in molar ratio with ammonium molybdate
Zinc nitrate solution, is then slowly dropped in ammonium molybdate solution by zinc nitrate solution and ammonium molybdate solution processed, stirs 25min, institute
It obtains white depositions to be washed with distilled water, filter, the dry 11h under 90 DEG C of constant temperatures obtains the molybdic acid zinc powder that partial size is 4 μm
Body；
Titanium dioxide powder, molybdic acid aluminium powder, zinc molybdate powder that partial size is 2.5 μm are mixed according to the ratio, obtained compound
Antimicrobial powder.
B, the preparation of glaze slip
By 23.5 parts of potassium feldspar, 34.5 parts of sandstone, 3.5 parts of dolomite, 11.5 parts of lime stone, 10 parts of zirconium English powder, frit 5
Part, 2.5 parts of aluminium oxide, 2.5 parts of zinc oxide, 4.5 parts of Suzhou soil, 0.02 part of zirconium iron pink, spectrum is 0.07 part yellow, and 0.15 part of cellulose,
8 parts of compound antibacterial powder；The compound antibacterial powder includes the raw material of following mass percentage: silver molybdate 18%, zinc molybdate
62%, titanium dioxide 20% is added in ball mill, and carrying out wet ball grinding to glaze slip fineness is that 325 mesh 10000-hole sieve screen over-sizes are
3%, obtain glaze slip；
C, the preparation of antiseptic sanitary glaze
Glaze slip in step B is imposed on sanitary ceramic body surface, using tunnel oven, at 1230 DEG C in oxidizing atmosphere
It fires, heating rate is 2.8 DEG C/min, firing period 17h, keeps the temperature 2.5h, i.e., obtains on sanitary ceramic body surface
Antiseptic sanitary glaze.
Comparative example 2
A, the preparation of compound antibacterial powder
The preparation of molybdic acid aluminium powder: by silver nitrate, 2:1.1 is added separately to match in deionized water in molar ratio with ammonium molybdate
Silver nitrate solution and ammonium molybdate solution processed, both the above solution are placed in reactor, 13min are mixed, be subsequently placed in power
For heating reaction 4min in the micro-wave oven of 900W, gained light yellow precipitate is washed with distilled water, filters, in 65 DEG C of constant temperatures
Lower dry 11h obtains the molybdic acid aluminium powder that partial size is 3 μm；
The preparation of zinc molybdate powder: by zinc nitrate, 1:1.2 is added separately to match in deionized water in molar ratio with ammonium molybdate
Zinc nitrate solution, is then slowly dropped in ammonium molybdate solution by zinc nitrate solution and ammonium molybdate solution processed, stirs 25min, institute
It obtains white depositions to be washed with distilled water, filter, the dry 11h under 90 DEG C of constant temperatures obtains the molybdic acid zinc powder that partial size is 4 μm
Body；
Titanium dioxide powder, molybdic acid aluminium powder, zinc molybdate powder that partial size is 2.5 μm are mixed according to the ratio, obtained compound
Antimicrobial powder.
B, the preparation of glaze slip
By 23.5 parts of potassium feldspar, 34.5 parts of sandstone, 3.5 parts of dolomite, 11.5 parts of lime stone, 10 parts of zirconium English powder, frit 5
Part, 2.5 parts of aluminium oxide, 2.5 parts of zinc oxide, 4.5 parts of Suzhou soil, 0.02 part of zirconium iron pink, spectrum is 0.07 part yellow, and 0.15 part of cellulose,
1 part of compound antibacterial powder；The compound antibacterial powder includes the raw material of following mass percentage: silver molybdate 18%, zinc molybdate
62%, titanium dioxide 20% is added in ball mill, and carrying out wet ball grinding to glaze slip fineness is that 325 mesh 10000-hole sieve screen over-sizes are
3%, obtain glaze slip；
C, the preparation of antiseptic sanitary glaze
Glaze slip in step B is imposed on sanitary ceramic body surface, using tunnel oven, at 1230 DEG C in oxidizing atmosphere
It fires, heating rate is 2.8 DEG C/min, firing period 17h, keeps the temperature 2.5h, i.e., obtains on sanitary ceramic body surface
Antiseptic sanitary glaze.
Non- antiseptic sanitary glaze control sample example
A, the preparation of glaze slip
By 23.5 parts of potassium feldspar, 34.5 parts of sandstone, 3.5 parts of dolomite, 11.5 parts of lime stone, 10 parts of zirconium English powder, frit 5
Part, 2.5 parts of aluminium oxide, 2.5 parts of zinc oxide, 4.5 parts of Suzhou soil, 0.02 part of zirconium iron pink, spectrum is 0.07 part yellow, and 0.15 part of cellulose,
It 0 part of compound antibacterial powder, being added in ball mill, it is 3% that progress wet ball grinding to glaze slip fineness, which is 325 mesh 10000-hole sieve screen over-sizes,
Obtain glaze slip；
B, the preparation of sanitary ceramics glaze
Glaze slip in step A is imposed on sanitary ceramic body surface, using tunnel oven, at 1230 DEG C in oxidizing atmosphere
It fires, heating rate is 2.8 DEG C/min, firing period 17h, keeps the temperature 2.5h, i.e., obtains on sanitary ceramic body surface
Antiseptic sanitary glaze.
1, antiseptic sanitary glaze anti-microbial property test
Using colony counting method, increased and decreased by bacterial number in measurement comparative example and embodiment antimicrobial sample and control sample
Method evaluate the anti-anti-microbial property of material.
Specific experiment step:
A. will by coupons l.0cm × 3.0cm and control print (with by coupons homogeneous material, same size, but be free of
Anti-biotic material, and sterilized processing) it is 3 each, it is divided into 3 groups and is placed in the PBS solution of sterilizing.Tested bacterial liquid culture is added
Dilution, sufficiently oscillation, which is placed in 36 DEG C of insulating boxs, cultivates 6h.
B. the bacterium solution 0.5ml after taking culture with pipette is instilled along tube wall containing (attention in 4.5ml sterilizing PBS buffer solution
Pipette tip not touch in-line dilution liquid), oscillation test tube is uniformly mixed, and is made the dilution of 1:10.
C. it separately takes 1ml sterilizing pipette to make 10 times of incremental thin liquids by aforesaid operations sequence, is so often incremented by dilution once,
Use 1 1ml sterilizing pipette instead.
D. cooling in the culture dish of the nutrient agar injection sterilizing of proper temperature is spare.
E. 3 acceptable diluent degree are selected, respectively while making 10 times and being incremented by dilution, i.e. the liquid relief to draw the dilution
Pipe moves 0.1ml in culture dish, and is coated with uniform.Each dilution makees two culture dishes.
F. culture dish is put into 36 DEG C of constant incubator, culture 18~take out counting afterwards for 24 hours.
G. method for counting colonies.Plate of the clump count between 30~300 is chosen as total plate count and measures standard.One
Dilution uses two plates, should use two plate averages, when wherein plate has the growth of larger sheet bacterium colony, does not then adopt
With, and using the plate that no sheet bacterium colony is grown as the clump count of the dilution, if sheet falls the half less than plate, and remaining
Bacterium colony distribution is again very uniform in half, multiplies 2 after can calculating half of plate to represent full ware clump count.
H. calculate in bacteriostasis rate (part)=(A-B)/A × 100 formula: A represents non-anti-bacteria ceramic control sample and averagely recycles bacterium
Number；B represents test specimen (comparative example and embodiment) average bacterial count recovered.
Antiseptic sanitary glaze (comparative example and embodiment) and non-anti-bacteria ceramic control sample are put by the above process
It is diluted in the buffer solution of certain density Escherichia coli, impregnates the antibiotic rate for testing them afterwards for 24 hours.As a result such as table 1.
The anti-microbial property of 1 antibacterial ceramic glaze of table
| Embodiment | Clump count before sterilizing | Clump count after sterilization | Antibiotic rate (%) |
| Embodiment 1 | 2650 | 133 | 95.0 |
| Embodiment 2 | 2650 | 90 | 96.6 |
| Embodiment 3 | 2650 | 95 | 96.4 |
| Comparative example 1 | 2650 | 81 | 96.9 |
| Comparative example 2 | 2650 | 1315 | 50.4 |
| Control sample example | 2650 | 2650 | 0 |
It can be seen from Table 1 that antiseptic sanitary glaze of the present invention, antibiotic rate is up to 95~96%.When antimicrobial powder exists
When the solubility of glaze reaches saturation, increase its content, the ion that glaze superficial dissolution goes out will not change, and such as comparative example 1, resist
Bacterium powder content has increased to 8 parts, and compared in embodiment 2 2.5 parts of antimicrobial powder content, the other preparation conditions of the two are all the same,
But antibacterial effect essentially unchangedization.
2, antiseptic sanitary physicochemical property is tested
Comparative example and embodiment antimicrobial sample and non-anti-bacteria ceramic control sample are done into physical and chemical quality according to GB6952-2015
Testing result such as table 2.It can be seen from the test results that anti-bacteria ceramic no matter appearance detection or physical and chemical performance detect, meet
Standard.
2 antiseptic sanitary glaze physical and chemical quality testing result of table
| Embodiment | Color difference | Water absorption rate (%) | Crack resistance | Open defect | Antibiotic rate (%) |
| Embodiment 1 | It is unobvious | 0.3 | Flawless | Nothing | 95.0 |
| Embodiment 2 | It is unobvious | 0.3 | Flawless | Nothing | 96.6 |
| Embodiment 3 | It is unobvious | 0.2 | Flawless | Nothing | 96.4 |
| Comparative example 1 | It is more apparent | 0.7 | Flawless | Low in glossiness | 96.9 |
| Comparative example 2 | It is unobvious | 0.8 | Flawless | Nothing | 50.4 |
| Control sample example | It is unobvious | 0.3 | Flawless | Nothing | 0 |
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of antiseptic sanitary glaze, which is characterized in that including following raw material: 23~24 parts of potassium feldspar, sandstone 34
~35 parts, 3~4 parts of dolomite, 11~12 parts of lime stone, 9~11 parts of zirconium English powder, 4~6 parts of frit, 2~3 parts of aluminium oxide, oxidation
2~3 parts of zinc, 4~5 parts of Suzhou soil, 0.01~0.03 part of zirconium iron pink, spectrum is 0.06~0.08 part yellow, 0.1~0.2 part of cellulose, multiple
Close 2~3 parts of antimicrobial powder；
The compound antibacterial powder includes the raw material of following mass percentage: silver molybdate 15~20%, zinc molybdate 60~65%,
Titanium dioxide 20~25%.
2. a kind of antiseptic sanitary glaze according to claim 1, which is characterized in that including following raw material: potassium is long
23.5 parts of stone, 34.5 parts of sandstone, 3.5 parts of dolomite, 11.5 parts of lime stone, 10 parts of zirconium English powder, 5 parts of frit, 2.5 parts of aluminium oxide,
2.5 parts of zinc oxide, 4.5 parts of Suzhou soil, 0.02 part of zirconium iron pink, spectrum is 0.07 part yellow, and 0.15 part of cellulose, compound antibacterial powder 2.5
Part；
The compound antibacterial powder includes the raw material of following mass percentage: silver molybdate 18%, zinc molybdate 62%, titanium dioxide
20%.
3. a kind of a kind of preparation method of antiseptic sanitary glaze as claimed in claim 1 or 2, which is characterized in that including following
Step:
A, the preparation of compound antibacterial powder
The preparation of molybdic acid aluminium powder: by silver nitrate, 2:1~1.2 are added separately to prepare in deionized water in molar ratio with ammonium molybdate
Both the above solution is placed in 10~15min of mixing in reactor, is subsequently placed in function by silver nitrate solution and ammonium molybdate solution
Rate is that 3~5min of heating reaction, gained light yellow precipitate are washed with distilled water, filter in the micro-wave oven of 800~1000W,
Dry 10~12h under 60~70 DEG C of constant temperatures, obtains the molybdic acid aluminium powder that partial size is 2~4 μm；
The preparation of zinc molybdate powder: by zinc nitrate, 1:1.2 is added separately to prepare nitre in deionized water in molar ratio with ammonium molybdate
Zinc nitrate solution, is then slowly dropped in ammonium molybdate solution by sour zinc solution and ammonium molybdate solution, stirs 20~30min, institute
It obtains white depositions to be washed with distilled water, filter, dry 10~12h under 80~100 DEG C of constant temperatures, obtaining partial size is 3~5
μm zinc molybdate powder；
Titanium dioxide powder, molybdic acid aluminium powder, zinc molybdate powder that partial size is 2~3 μm are mixed according to the ratio, obtain composite antibacterial
Powder；
B, the preparation of glaze slip
The raw material of compound antibacterial powder and other proportions in step A is added in ball mill, it is thin to glaze slip to carry out wet ball grinding
Degree is that 325 mesh 10000-hole sieve screen over-sizes are 2~4%, obtains glaze slip；
C, the preparation of antiseptic sanitary glaze
Glaze slip in step B is imposed on sanitary ceramic body surface, using tunnel oven, the oxidizing atmosphere at 1200~1250 DEG C
Middle firing, heating rate are 2.5~3 DEG C/min, and firing period is 16~18h, keep the temperature 2~3h, i.e., in sanitary ceramic body
Antiseptic sanitary glaze is obtained on surface.
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