CN116262668A - Preparation process of antibacterial high-strength ceramic - Google Patents
Preparation process of antibacterial high-strength ceramic Download PDFInfo
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- CN116262668A CN116262668A CN202111527057.3A CN202111527057A CN116262668A CN 116262668 A CN116262668 A CN 116262668A CN 202111527057 A CN202111527057 A CN 202111527057A CN 116262668 A CN116262668 A CN 116262668A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 135
- 239000000919 ceramic Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 68
- 239000002994 raw material Substances 0.000 claims abstract description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002002 slurry Substances 0.000 claims abstract description 38
- 238000010304 firing Methods 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 23
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims abstract description 21
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 21
- 229920002748 Basalt fiber Polymers 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 17
- 239000008187 granular material Substances 0.000 claims abstract description 15
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000007605 air drying Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000005507 spraying Methods 0.000 claims abstract description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 32
- 239000011248 coating agent Substances 0.000 claims description 27
- 238000000576 coating method Methods 0.000 claims description 27
- 239000005995 Aluminium silicate Substances 0.000 claims description 25
- 235000012211 aluminium silicate Nutrition 0.000 claims description 25
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 25
- 239000011701 zinc Substances 0.000 claims description 17
- 229910052656 albite Inorganic materials 0.000 claims description 16
- 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 description 16
- 239000010459 dolomite Substances 0.000 claims description 16
- 229910000514 dolomite Inorganic materials 0.000 claims description 16
- 239000011787 zinc oxide Substances 0.000 claims description 16
- VSZSIEBALNXIFG-UHFFFAOYSA-N 2-hydroxyethyl 2,2-bis(sulfanyl)acetate Chemical compound OCCOC(=O)C(S)S VSZSIEBALNXIFG-UHFFFAOYSA-N 0.000 claims description 15
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 14
- 230000003373 anti-fouling effect Effects 0.000 claims description 14
- 229910052744 lithium Inorganic materials 0.000 claims description 14
- 229910052573 porcelain Inorganic materials 0.000 claims description 14
- 239000004575 stone Substances 0.000 claims description 14
- 150000008040 ionic compounds Chemical class 0.000 claims description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 11
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 11
- 239000005913 Maltodextrin Substances 0.000 claims description 9
- 229920002774 Maltodextrin Polymers 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 9
- 239000010433 feldspar Substances 0.000 claims description 9
- 229940035034 maltodextrin Drugs 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 229920000609 methyl cellulose Polymers 0.000 claims description 9
- 239000001923 methylcellulose Substances 0.000 claims description 9
- 229960002900 methylcellulose Drugs 0.000 claims description 9
- 235000010981 methylcellulose Nutrition 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 9
- 239000010453 quartz Substances 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 230000005484 gravity Effects 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 238000003801 milling Methods 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 230000035939 shock Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 125000003396 thiol group Chemical group [H]S* 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 102000035195 Peptidases Human genes 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- -1 Silver ions Chemical class 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
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 210000000805 cytoplasm Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
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Abstract
The invention discloses a preparation process of antibacterial high-strength ceramic, which comprises the following steps: s1, preparing a blank: s11, mixing the raw materials, performing wet ball milling to obtain a particle size of 100-200 meshes, and then continuously adding calcined strontium carbonate, a nano antibacterial composition and basalt fiber to obtain powder; ball milling the powder to 300-400 mesh granularity, and granulating; s12, pressing and forming the green body granules to obtain a coarse green body, and naturally air-drying to obtain a green body; s2, glazing: mixing glaze raw material (containing nano antibacterial composition) and wet-processingBall milling to 400-500 mesh granularity, sieving to eliminate iron, and adding water to obtain glaze slurry with solid content of 50-60%; spraying glaze slurry on the blank body, and then drying for standby; s3, firing: and firing the glazed green body at 900-1000 ℃ for 100-150 minutes. The ceramic product of the invention is added with nano antibacterial composition in the green body and the glaze layer, the nano antibacterial composition is nano diatomite loaded antibacterial agent, wherein the antibacterial agent comprises Zn 2+ 、Ag + The antibacterial effect is good and the antibacterial effect is durable.
Description
Technical Field
The invention belongs to the technical field of ceramic products, and particularly relates to a preparation process of antibacterial high-strength ceramic.
Background
With the continuous development of healthy life concepts, people have new requirements on the antibacterial performance of ceramic products, especially ceramic products in the field of home decoration, and as the service life of home decoration ceramics increases, as the ceramic surface has tiny pinholes which are invisible to naked eyes, the service time is long, bacteria are easy to accumulate and breed and even infect, the health is seriously affected, and especially, pollution and bacteria breeding can occur in dead angles which are not easy to clean, especially in places such as home kitchens, toilets and the like. Therefore, the antibacterial property of ceramic products is becoming an important index of ceramic properties.
The existing process for preparing the antibacterial ceramic is mostly obtained by directly adding an antibacterial agent into a surface glaze raw material and then firing, but the antibacterial agent is not uniformly dispersed in the glaze and is easy to agglomerate due to poor compatibility of the antibacterial agent and the surface glaze raw material, so that the antibacterial durability of a final ceramic product is affected, the expected antibacterial effect cannot be achieved, and some technicians can achieve the antibacterial effect by coating an antibacterial coating on the surface of the ceramic surface glaze, but the surface glaze is not wear-resistant, the binding force of the antibacterial coating and the surface glaze is not high, so that the antibacterial coating is worn away quickly, and the corresponding function is lost.
Therefore, the research on the antibacterial high-strength ceramic with good antibacterial effect and good antibacterial durability has important application value.
Disclosure of Invention
The invention aims to provide a preparation process of an antibacterial high-strength ceramic with good antibacterial effect and good antibacterial durability, which is characterized in that nano diatomite loaded antibacterial agent is added into a blank raw material and a glaze raw material, so that the antibacterial agent is uniformly dispersed in the ceramic, does not agglomerate and has good antibacterial durability; and the strength of the finally prepared ceramic is high and the service life is long through the selection of raw materials.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation process of antibacterial high-strength ceramic comprises a blank body and a glaze layerThe green body is prepared from the following raw materials in parts by weight: 45-60 parts of potassium feldspar, 20-30 parts of albite, 15-20 parts of dolomite, 15-20 parts of kaolin, 3-6 parts of calcined strontium carbonate, 3-6 parts of nano antibacterial composition and 0.5-1 part of basalt fiber; the glaze layer is prepared from the following raw materials in parts by weight: 20-30 parts of quartz, 15-20 parts of feldspar, 10-20 parts of talcum powder, 10-20 parts of frit, 10-15 parts of kaolin, 8-12 parts of zirconium silicate, 5-8 parts of lithium porcelain stone, 5-8 parts of zinc oxide and 3-5 parts of nano antibacterial composition; the nanometer antibacterial composition is a nanometer diatomite loaded antibacterial agent, and the antibacterial agent comprises Zn-containing components 2+ 、Ag + One or two of the following components;
the preparation of the antibacterial high-strength ceramic comprises the following steps:
s1, preparing a blank:
s11, mixing potassium feldspar, albite, dolomite and kaolin, performing wet ball milling to a granularity of 100-200 meshes, then continuously adding calcined strontium carbonate, nano antibacterial composition and basalt fiber, uniformly mixing to obtain powder, performing further ball milling to a granularity of 300-400 meshes, and granulating in a spray tower to obtain green body granules;
s12, pressing and forming the green body granules to obtain a coarse green body, and naturally air-drying to obtain a green body;
s2, glazing: mixing the glaze raw materials, performing wet ball milling to obtain a particle size of 400-500 meshes, sieving to remove iron, and adding water to obtain glaze slurry with a solid content of 50-60%; spraying glaze slurry on the blank body, and then drying for standby;
s3, firing: firing the glazed green body at 900-1000 ℃ for 100-150 minutes to obtain the antibacterial high-strength ceramic.
The nano antibacterial composition is added into the green body and the glaze layer, so that the antibacterial effect is good and the antibacterial effect is durable, the nano antibacterial composition is a nano diatomite loaded antibacterial agent, and the antibacterial agent comprises Zn 2+ 、Ag + The zinc ion can oxidize and decompose the activity of cell membrane or cell protoplasm active enzyme of bacteria under lower concentration, so as to achieve the antibacterial effect. Silver ions specifically bind thiol groups with negative charges in proteases and pierce cell walls and membranesSo as to denature protein, achieve sterilization effect, and simultaneously realize Zn 2+ 、Ag + Has high temperature resistance, is suitable for the ceramic firing process, has a porous structure of nano diatomite, has water absorption rate of 2-4 times of self volume, has large specific surface area of nano size, and the inventor discovers that the nano diatomite has a high specific surface area to Zn 2+ 、Ag + In addition, in the invention, calcined strontium carbonate is selected as a raw material of the green body, so that the strength of the green body can be enhanced, and the green body has good stability during firing; the basalt fiber can improve the cracking resistance of the blank, strengthen the strength and toughness of the blank, and further improve the bonding performance of the blank and the glaze layer; the addition of talcum powder in the glaze can improve the fineness of the glaze, is uniform and bright, and can also play a role in reducing the firing temperature; the lithium porcelain stone can be used as a fluxing agent, so that the blank glaze can be well combined during firing, and meanwhile, the lithium porcelain stone has an opacifying effect and improves whiteness; the addition of the frit can reduce the firing temperature and improve the firing stability, thereby improving the quality of the glaze.
In the present invention, preferably, the nano-antibacterial composition is prepared as follows: dispersing nano diatomite and a multi-mercapto compound in a solvent; then adding Zn 2+ 、Ag + The preparation method of the nano antibacterial composition is that the inventor creatively researches and obtains the nano antibacterial composition by reacting a multi-mercapto compound with diatomite surface groups and then utilizing mercapto and Zn by spray drying to obtain powder, calcining the powder at 800-1000 ℃ for 2-4 hours 2+ 、Ag + Combining, calcining at high temperature to make diatomite and Zn 2+ 、Ag + The combination is firm, the nano diatomite is loaded with high antibacterial agent, and the antibacterial effect is good.
In the invention, preferably, the multi-mercapto compound is ethylene glycol dimercaptoacetate, and the mass ratio of the nano diatomite, the ethylene glycol dimercaptoacetate and the ionic compound is 10:0.5-1:1-3. The mass ratio is reasonably set, most of ethylene glycol dimercaptoacetate can react with nano diatomite, the ionic compound basically reacts completely, and the raw material cost is saved.
In the invention, the green body is preferably prepared from the following raw materials in parts by weight: 50 parts of potassium feldspar, 25 parts of albite, 16 parts of dolomite, 17 parts of kaolin, 5 parts of calcined strontium carbonate, 5 parts of nano antibacterial composition and 0.5 part of basalt fiber; the glaze layer is prepared from the following raw materials in parts by weight: 25 parts of quartz, 15 parts of feldspar, 13 parts of talcum powder, 15 parts of frit, 14 parts of kaolin, 10 parts of zirconium silicate, 6 parts of lithium porcelain stone, 6 parts of zinc oxide and 4 parts of nano antibacterial composition. The raw material content of the green body and the glaze layer is obtained through a large number of experiments and theoretical knowledge adjustment analysis, and the dosage is a preferable scheme of the invention, so that the firing effect is good, and ceramic products with good antibacterial effect, good antibacterial durability and high strength can be obtained.
In the present invention, preferably, the chemical composition of the frit includes: siO (SiO) 2 45 to 53 percent of Al 2 O 3 25 to 30 percent of MgO, 6.0 to 8.0 percent of CaO, 3.0 to 5.0 percent of Na 2 O is 3.5-4.0%, K 2 4.0 to 5.0 percent of O, 0.3 to 0.5 percent of ZnO and TiO 2 0.05 to 0.2 percent of Fe 2 O 3 0.1 to 0.3 percent. The frit is used as one of the main raw materials of the glaze layer raw material, and mainly plays roles of reducing the melting temperature of the glaze and improving the gloss, uniformity and fineness of the glaze surface.
In the invention, preferably, the ceramic obtained after firing also comprises a glazed layer surface for polishing, and then an antibacterial and antifouling coating is coated, further preferably, the antibacterial and antifouling coating comprises nano silver, silica sol, sodium dodecyl sulfate, polyvinyl alcohol, methyl cellulose and maltodextrin, and the mass ratio of the nano silver to the silica sol to the sodium dodecyl sulfate to the polyvinyl alcohol to the methyl cellulose to the maltodextrin is 0.5-1:10:3-5:1-2:0.5-1:0.5-1; the invention can also coat an antibacterial and antifouling coating on the surface of the glaze layer, further optimally designs the raw material composition of the antibacterial and antifouling coating, takes silica sol as a main film forming substance, and takes methylcellulose and maltodextrin to play a role in suspending nano silver, so that the nano silver is uniformly dispersed by sodium dodecyl sulfate and polyvinyl alcohol, and the dosage ratio of each raw material is optimized by continuous experimental adjustment, so that the coating has good film forming effect and uniform nano silver dispersion.
Further preferably, the curing process of the antibacterial and antifouling coating comprises the steps of after the antibacterial and antifouling coating is coated, airing at room temperature, and then carrying out secondary calcination on the ceramic at 400-500 ℃ for 2-3 hours to achieve effective combination of the surface coating and the glaze layer.
In the present invention, it is preferable that the nano-antibacterial composition has a particle size of 50nm to 200nm.
In the present invention, preferably, in S2, the slip is subjected to a vacuum degree of 10 before the slip is applied -3 ~1×10 -2 Vacuum bubble removal under the conditions of 50-55 ℃ and the pressure of MPa; when the glaze slurry is sprayed, the specific gravity of the glaze is 1.7-1.8 g/m 3 The glazing quantity is 700-800 g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The vacuum removal of bubbles from the glaze slip is difficult to produce defects such as air holes and the like in the firing process; when the glaze slurry is sprayed, the concentration of the glaze slurry is too low, an excessively thin glaze layer is easily formed on a green body, so that the surface of the fired glaze layer is not smooth, but the concentration of the glaze slurry is too high, the fluidity is relatively weakened, the slurry is not easy to flow uniformly, the phenomena of stacking glaze and the like are easy to generate, cracks are easy to generate in the firing process, the glaze disclosed by the invention can be spread uniformly, the thickness is uniformly distributed on the green body, and the obtained glaze surface is flat and smooth.
The invention also provides a ceramic product prepared by the preparation process of the antibacterial high-strength ceramic and application of the ceramic product.
Compared with the prior art, the invention has the beneficial effects that:
(1) The ceramic product of the invention is added with nano antibacterial composition in the green body and the glaze layer, the nano antibacterial composition is nano diatomite loaded antibacterial agent, wherein the antibacterial agent comprises Zn 2+ 、Ag + The antibacterial effect is good and the antibacterial effect is durable;
(2) According to the invention, the calcined strontium carbonate is selected from the raw materials of the green body, and the calcined strontium carbonate can enhance the strength of the green body, so that the green body has good stability during firing; the basalt fiber can improve the cracking resistance of the blank, strengthen the strength and toughness of the blank, and further improve the bonding performance of the blank and the glaze layer; the addition of talcum powder in the glaze can improve the fineness of the glaze, is uniform and bright, and can also play a role in reducing the firing temperature; the lithium porcelain stone can be used as a fluxing agent, so that the blank glaze can be well combined during firing, and meanwhile, the lithium porcelain stone has an opacifying effect and improves whiteness; the addition of the frit can reduce the firing temperature and improve the firing stability, thereby improving the quality of the glaze;
(3) The preparation of the nano antibacterial composition is creatively researched and obtained by the inventor, and the thiol and Zn are recycled through the reaction of the multi-thiol compound and the diatomite surface group 2+ 、Ag + Combining, calcining at high temperature to make diatomite and Zn 2+ 、Ag + The combination is firm, the nano diatomite is loaded with high antibacterial agent, and the antibacterial effect is good.
Detailed Description
The present invention will be further described in detail with reference to the following specific examples, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent, but the scope of the present invention is not limited to the examples.
The test methods or test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise specified, are obtained from conventional commercial sources or prepared in conventional manner.
Example 1:
the preparation of the antibacterial high-strength ceramic comprises the following steps:
s1, preparing a blank:
s11, mixing potassium feldspar, albite, dolomite and kaolin, performing wet ball milling to obtain 100 meshes of granularity, continuously adding calcined strontium carbonate, nano antibacterial composition and basalt fiber, uniformly mixing to obtain powder, performing further ball milling to obtain 300 meshes of granularity, and granulating in a spray tower to obtain green body granules;
s12, pressing and forming the green body granules to obtain a coarse green body, and naturally air-drying to obtain a green body;
s2, glazing: mixing the glaze raw materials, performing wet ball milling to obtain a particle size of 400 meshes, sieving to remove iron, and adding water to obtain glaze slurry, wherein the solid content of the glaze slurry is about 50%; spraying glaze slurry on the blank body, and then drying for standby; drenching glazeBefore the slurry, the vacuum degree of the glaze slurry is 10 -3 Vacuum bubble removal under the condition of 50 ℃ at the temperature of MPa; when the glaze slurry is sprayed, the specific gravity of the glaze is 1.7g/m 3 Glazing amount is 700g/m 2 ;
S3, firing: and firing the glazed green body at 900 ℃ for 150 minutes to obtain the antibacterial high-strength ceramic.
The raw materials of the green body are as follows: 45Kg of potassium feldspar, 20Kg of albite, 15Kg of dolomite, 15Kg of kaolin, 3Kg of calcined strontium carbonate, 3Kg of nano antibacterial composition and 0.5Kg of basalt fiber.
The glaze layer is prepared from the following raw materials: 20Kg of quartz, 15Kg of feldspar, 10Kg of talcum powder, 10Kg of frit, 10Kg of kaolin, 8Kg of zirconium silicate, 5Kg of lithium porcelain stone, 5Kg of zinc oxide and 3Kg of nano antibacterial composition.
The chemical composition of the frit comprises: siO (SiO) 2 50% of Al 2 O 3 28% MgO, 7.0% CaO, 4.5% CaO, na 2 O is 3.8%, K 2 4.6% O, 0.4% ZnO and TiO 2 0.10% of Fe 2 O 3 0.2% and the balance loss on ignition.
The preparation of the nano antibacterial composition is as follows: dispersing nano diatomite and ethylene glycol dimercaptoacetate in a solvent; then adding Zn 2+ 、Ag + The ionic compound of (2) is stirred and dispersed uniformly, then spray-dried to obtain powder, and the powder is calcined for 4 hours at 800 ℃ to obtain the nano antibacterial composition, wherein the particle size of the nano antibacterial composition is 100-200 nm. The mass ratio of the nano diatomite to the ethylene glycol dimercaptoacetate to the ionic compound is 10:0.5:1.
Example 2:
the preparation of the antibacterial high-strength ceramic comprises the following steps:
s1, preparing a blank:
s11, mixing potassium feldspar, albite, dolomite and kaolin, performing wet ball milling to obtain a particle size of 200 meshes, continuously adding calcined strontium carbonate, a nano antibacterial composition and basalt fibers, uniformly mixing to obtain powder, performing further ball milling to obtain a particle size of 400 meshes, and granulating in a spray tower to obtain green body granules;
s12, pressing and forming the green body granules to obtain a coarse green body, and naturally air-drying to obtain a green body;
s2, glazing: mixing the glaze raw materials, performing wet ball milling to obtain a particle size of 500 meshes, sieving to remove iron, and adding water to obtain glaze slurry, wherein the solid content of the glaze slurry is about 60%; spraying glaze slurry on the blank body, and then drying for standby; before the coating, the vacuum degree of the glaze slurry is 1 multiplied by 10 -2 Vacuum bubble removal under the condition of the temperature of 55 ℃ under the pressure of MPa; when the glaze slurry is sprayed, the specific gravity of the glaze is 1.8g/m 3 The glazing amount is 800g/m 2 ;
S3, firing: and firing the glazed green body at 1000 ℃ for 100 minutes to obtain the antibacterial high-strength ceramic.
The raw materials of the green body are as follows: 60Kg of potassium feldspar, 30Kg of albite, 20Kg of dolomite, 20Kg of kaolin, 6Kg of calcined strontium carbonate, 6Kg of nano antibacterial composition and 1Kg of basalt fiber.
The glaze layer is prepared from the following raw materials: 30Kg of quartz, 20Kg of feldspar, 20Kg of talcum powder, 20Kg of frit, 15Kg of kaolin, 12Kg of zirconium silicate, 8Kg of lithium porcelain stone, 8Kg of zinc oxide and 5Kg of nano antibacterial composition.
The chemical composition of the frit comprises: siO (SiO) 2 48% of Al 2 O 3 27% MgO, 7.5% CaO, 4.0% CaO, na 2 O is 3.7%, K 2 4.4% O, 0.35% ZnO and TiO 2 0.15% of Fe 2 O 3 0.15% and the balance loss on ignition.
The preparation of the nano antibacterial composition is as follows: dispersing nano diatomite and ethylene glycol dimercaptoacetate in a solvent; then adding Zn 2+ 、Ag + The ionic compound of (2) is stirred and dispersed uniformly, then spray-dried to obtain powder, and the powder is calcined for 2 hours at the temperature of 1000 ℃ to obtain the nano antibacterial composition, wherein the particle size of the nano antibacterial composition is 50-100 nm. The mass ratio of the nano diatomite to the ethylene glycol dimercaptoacetate to the ionic compound is 10:1:3.
Example 3:
the preparation of the antibacterial high-strength ceramic comprises the following steps:
s1, preparing a blank:
s11, mixing potassium feldspar, albite, dolomite and kaolin, performing wet ball milling to a granularity of 150 meshes, then continuously adding calcined strontium carbonate, nano antibacterial composition and basalt fiber, uniformly mixing to obtain powder, performing further ball milling to a granularity of 350 meshes, and granulating in a spray tower to obtain green body granules;
s12, pressing and forming the green body granules to obtain a coarse green body, and naturally air-drying to obtain a green body;
s2, glazing: mixing the glaze raw materials, performing wet ball milling to obtain a particle size of 500 meshes, sieving to remove iron, and adding water to obtain glaze slurry, wherein the solid content of the glaze slurry is about 55%; spraying glaze slurry on the blank body, and then drying for standby; before the coating, the vacuum degree of the glaze slurry is 5 multiplied by 10 -3 Vacuum bubble removal under the condition of the temperature of 52 ℃ under the pressure of MPa; when the glaze slurry is sprayed, the specific gravity of the glaze is 1.76g/m 3 Glazing amount is 750g/m 2 ;
S3, firing: and firing the glazed green body at 950 ℃ for 120 minutes to obtain the antibacterial high-strength ceramic.
The raw materials of the green body are as follows: 50Kg of potassium feldspar, 25Kg of albite, 16Kg of dolomite, 17Kg of kaolin, 5Kg of calcined strontium carbonate, 5Kg of nano antibacterial composition and 0.5Kg of basalt fiber.
The glaze layer is prepared from the following raw materials: 25Kg of quartz, 15Kg of feldspar, 13Kg of talcum powder, 15Kg of frit, 14Kg of kaolin, 10Kg of zirconium silicate, 6Kg of lithium porcelain stone, 6Kg of zinc oxide and 4Kg of nano antibacterial composition.
The chemical composition of the frit comprises: siO (SiO) 2 48% of Al 2 O 3 28% MgO, 7.5% CaO, 4.5% CaO, na 2 O is 3.8%, K 2 4.6% O, 0.46% ZnO and TiO 2 0.09% of Fe 2 O 3 0.14% and the balance loss on ignition.
The preparation of the nano antibacterial composition is as follows: dispersing nano diatomite and ethylene glycol dimercaptoacetate in a solvent; then adding Zn 2+ 、Ag + The ionic compound of (2) is stirred and dispersed uniformly, then spray-dried to obtain powder, and the powder is calcined for 3 hours at 900 ℃ to obtain the nano antibacterial composition, wherein the particle size of the nano antibacterial composition is 50-200 nm. The nano diatomite, ethylene glycol dimercaptoacetate and ionic compoundThe mass ratio is 10:1:2.
Example 4:
the preparation of the antibacterial high-strength ceramic comprises the following steps:
s1, preparing a blank:
s11, mixing potassium feldspar, albite, dolomite and kaolin, performing wet ball milling to obtain a particle size of 200 meshes, continuously adding calcined strontium carbonate, a nano antibacterial composition and basalt fibers, uniformly mixing to obtain powder, performing further ball milling to obtain a particle size of 350 meshes, and granulating in a spray tower to obtain green body granules;
s12, pressing and forming the green body granules to obtain a coarse green body, and naturally air-drying to obtain a green body;
s2, glazing: mixing the glaze raw materials, performing wet ball milling to obtain a particle size of 450 meshes, sieving to remove iron, and adding water to obtain glaze slurry, wherein the solid content of the glaze slurry is about 60%; spraying glaze slurry on the blank body, and then drying for standby; before the coating, the vacuum degree of the glaze slurry is 10 -3 Vacuum bubble removal under the condition of the temperature of 55 ℃ under the pressure of MPa; when the glaze slurry is sprayed, the specific gravity of the glaze is 1.78g/m 3 The glazing amount is 760g/m 2 ;
S3, firing: firing the glazed green body at 1000 ℃ for 130 minutes to obtain the antibacterial high-strength ceramic;
s4, polishing the surface of the glaze layer, and then coating an antibacterial antifouling coating; the antibacterial and antifouling coating comprises nano silver, silica sol, sodium dodecyl sulfate, polyvinyl alcohol, methyl cellulose and maltodextrin, wherein the mass ratio of the nano silver to the silica sol to the sodium dodecyl sulfate to the polyvinyl alcohol to the methyl cellulose to the maltodextrin is 0.5:10:3:1:0.5:0.5;
s5, after the antibacterial antifouling coating is coated, the ceramic is firstly dried at room temperature and then subjected to secondary calcination, wherein the calcination temperature is 450 ℃ and the time is 3 hours.
The raw materials of the green body are as follows: 52Kg of potassium feldspar, 26Kg of albite, 16Kg of dolomite, 17Kg of kaolin, 4Kg of calcined strontium carbonate, 4Kg of nano antibacterial composition and 0.6Kg of basalt fiber.
The glaze layer is prepared from the following raw materials: 24Kg of quartz, 16Kg of feldspar, 13Kg of talcum powder, 12Kg of frit, 11Kg of kaolin, 9Kg of zirconium silicate, 6Kg of lithium porcelain stone, 6Kg of zinc oxide and 3Kg of nano antibacterial composition.
The chemical composition of the frit comprises: siO (SiO) 2 52% of Al 2 O 3 26% MgO, 8% CaO, 4.7% CaO, na 2 O is 3.8%, K 2 4.7% O, 0.4% ZnO and TiO 2 0.12% of Fe 2 O 3 0.21% and the balance loss on ignition.
The preparation of the nano antibacterial composition is as follows: dispersing nano diatomite and ethylene glycol dimercaptoacetate in a solvent; then adding Zn 2+ 、Ag + The ionic compound of (2) is stirred and dispersed uniformly, then spray-dried to obtain powder, and the powder is calcined for 3.5 hours at 950 ℃ to obtain the nano antibacterial composition, wherein the particle size of the nano antibacterial composition is 50-100 nm. The mass ratio of the nano diatomite to the ethylene glycol dimercaptoacetate to the ionic compound is 10:0.5:3.
Example 5:
the preparation of the antibacterial high-strength ceramic comprises the following steps:
s1, preparing a blank:
s11, mixing potassium feldspar, albite, dolomite and kaolin, performing wet ball milling to a granularity of 150 meshes, then continuously adding calcined strontium carbonate, nano antibacterial composition and basalt fiber, uniformly mixing to obtain powder, performing further ball milling to a granularity of 350 meshes, and granulating in a spray tower to obtain green body granules;
s12, pressing and forming the green body granules to obtain a coarse green body, and naturally air-drying to obtain a green body;
s2, glazing: mixing the glaze raw materials, performing wet ball milling to obtain a particle size of 500 meshes, sieving to remove iron, and adding water to obtain glaze slurry, wherein the solid content of the glaze slurry is about 57%; spraying glaze slurry on the blank body, and then drying for standby; before the coating, the vacuum degree of the glaze slurry is 4.0X10 -3 Vacuum bubble removal under the condition of the temperature of 52 ℃ under the pressure of MPa; when the glaze slurry is sprayed, the specific gravity of the glaze is 1.79g/m 3 The glazing amount is 780g/m 2 ;
S3, firing: firing the glazed green body at 1000 ℃ for 120 minutes to obtain the antibacterial high-strength ceramic;
s4, polishing the surface of the glaze layer, and then coating an antibacterial antifouling coating; the antibacterial and antifouling coating comprises nano silver, silica sol, sodium dodecyl sulfate, polyvinyl alcohol, methyl cellulose and maltodextrin, wherein the mass ratio of the nano silver to the silica sol to the sodium dodecyl sulfate to the polyvinyl alcohol to the methyl cellulose to the maltodextrin is 1:10:3:2:1:1;
s5, after the antibacterial antifouling coating is coated, the ceramic is firstly dried at room temperature and then is subjected to secondary calcination, wherein the calcination temperature is 500 ℃ and the time is 2.5 hours.
The raw materials of the green body are as follows: 48Kg of potassium feldspar, 26Kg of albite, 17Kg of dolomite, 18Kg of kaolin, 4.2Kg of calcined strontium carbonate, 4.3Kg of nano antibacterial composition and 0.6Kg of basalt fiber.
The glaze layer is prepared from the following raw materials: 26Kg of quartz, 17Kg of feldspar, 16Kg of talcum powder, 17Kg of frit, 13Kg of kaolin, 9Kg of zirconium silicate, 7Kg of lithium porcelain stone, 6Kg of zinc oxide and 3.5Kg of nano antibacterial composition.
The chemical composition of the frit comprises: siO (SiO) 2 50% of Al 2 O 3 28% MgO, 7.5% CaO, 4.3% CaO, na 2 O is 3.8%, K 2 4.8% O, 0.42% ZnO and TiO 2 0.16% of Fe 2 O 3 0.13% and the balance loss on ignition.
The preparation of the nano antibacterial composition is as follows: dispersing nano diatomite and ethylene glycol dimercaptoacetate in a solvent; then adding Zn 2+ 、Ag + The ionic compound of (2) is stirred and dispersed uniformly, then spray-dried to obtain powder, and the powder is calcined for 4 hours at 900 ℃ to obtain the nano antibacterial composition, wherein the particle size of the nano antibacterial composition is 100-200 nm. The mass ratio of the nano diatomite to the ethylene glycol dimercaptoacetate to the ionic compound is 10:1:1.
Comparative examples 1 to 4 comparative example 1 did not contain the nano-antimicrobial composition, only the same and equivalent amount of antimicrobial agent as in example 3 was added, the other operations were the same as in example 3, comparative example 2 did not contain lithium porcelain stone, the other operations were the same as in example 3, comparative example 3 did not contain frit, the other materials having a chemical composition similar to that of frit were added, the other operations were the same as in example 3, comparative example 4 did not contain calcined strontium carbonate, and the other operations were the same as in example 3.
Performance testing
The antibacterial high-strength ceramic products finally prepared in examples 1 to 5 and comparative examples 1 to 4 were tested for abrasion resistance, thermal shock resistance and antibacterial properties, and the test results are shown in table 1.
The test method is as follows:
abrasion resistance test: the abrasion resistance of the ceramic was tested according to GB/T3810.7-2016 method part 7 of the ceramic tile test method, which comprises measuring the abrasion resistance of the glazed tile surface.
Thermal shock resistance test: according to the method for measuring the thermal shock resistance of the GB/T3298-2008 daily ceramic ware, the thermal shock resistance of the ceramic is tested.
Antibacterial property detection: the antibacterial property of the ceramic product against Escherichia coli was examined according to JC/T897-2002. The antibacterial persistence test was tested according to the JC/T897-2014 standard.
As can be seen from Table 1, the ceramic product prepared by the preparation process of the antibacterial high-strength ceramic has excellent wear resistance, thermal shock resistance and antibacterial performance, and has a large market prospect.
Variations and modifications of the above-described embodiments may occur to those skilled in the art in light of the foregoing disclosure and are, therefore, not to be limited to the specific embodiments disclosed and described, but rather, are intended to fall within the scope of the appended claims, and in addition, although specific terms are used herein, these terms are for convenience and are not intended to be limiting.
Claims (10)
1. The preparation process of the antibacterial high-strength ceramic is characterized in that the antibacterial high-strength ceramic comprises a blank body and a glaze layer, and the blank body is prepared from the following raw materials in parts by weight: 45-60 parts of potassium feldspar, 20-30 parts of albite, 15-20 parts of dolomite, 15-20 parts of kaolin, 3-6 parts of calcined strontium carbonate, 3-6 parts of nano antibacterial composition and 0.5-1 part of basalt fiber; the glaze layer is prepared from the following raw materials in parts by weight: 20-30 parts of quartz, 15-20 parts of feldspar, 10-20 parts of talcum powder, 10-20 parts of frit, 10-15 parts of kaolin, 8-12 parts of zirconium silicate, 5-8 parts of lithium porcelain stone, 5-8 parts of zinc oxide and 3-5 parts of nano antibacterial composition; the nanometer antibacterial composition is a nanometer diatomite loaded antibacterial agent, and the antibacterial agent comprises Zn-containing components 2+ 、Ag + One or two of the following components;
the preparation of the antibacterial high-strength ceramic comprises the following steps:
s1, preparing a blank:
s11, mixing potassium feldspar, albite, dolomite and kaolin, performing wet ball milling until the granularity is 100-200 meshes, then continuously adding calcined strontium carbonate, nano antibacterial composition and basalt fiber, and uniformly mixing to obtain powder; ball milling the powder until the granularity is 300-400 meshes, and granulating in a spray tower to obtain green body granules;
s12, pressing and forming the green body granules to obtain a coarse green body, and naturally air-drying to obtain a green body;
s2, glazing: mixing the glaze raw materials, performing wet ball milling to obtain a particle size of 400-500 meshes, sieving to remove iron, and adding water to obtain glaze slurry with a solid content of 50-60%; spraying glaze slurry on the blank body, and then drying for standby;
s3, firing: firing the glazed green body at 900-1000 ℃ for 100-150 minutes to obtain the antibacterial high-strength ceramic.
2. The process for preparing the antibacterial high-strength ceramic according to claim 1, wherein the preparation of the nano antibacterial composition is as follows: dispersing nano diatomite and a multi-mercapto compound in a solvent; then adding Zn 2+ 、Ag + One or two of the ionic compounds are stirred and dispersed uniformly, then spray-dried to obtain powder, and the powder is calcined for 2 to 4 hours at the temperature of 800 to 1000 ℃ to obtain the nano antibacterial composition.
3. The preparation process of the antibacterial high-strength ceramic according to claim 1, wherein the multi-mercapto compound is ethylene glycol dimercaptoacetate, and the mass ratio of the nano diatomite to the ethylene glycol dimercaptoacetate to the ionic compound is 10:0.5-1:1-3.
4. The preparation process of the antibacterial high-strength ceramic according to claim 1, wherein the green body is prepared from the following raw materials in parts by weight: 50 parts of potassium feldspar, 25 parts of albite, 16 parts of dolomite, 17 parts of kaolin, 5 parts of calcined strontium carbonate, 5 parts of nano antibacterial composition and 0.5 part of basalt fiber; the glaze layer is prepared from the following raw materials in parts by weight: 25 parts of quartz, 15 parts of feldspar, 13 parts of talcum powder, 15 parts of frit, 14 parts of kaolin, 10 parts of zirconium silicate, 6 parts of lithium porcelain stone, 6 parts of zinc oxide and 4 parts of nano antibacterial composition.
5. The process for preparing an antibacterial high-strength ceramic according to claim 1, wherein the chemical composition of the frit comprises: siO (SiO) 2 45 to 53 percent of Al 2 O 3 25 to 30 percent of MgO, 6.0 to 8.0 percent of CaO, 3.0 to 5.0 percent of Na 2 O is 3.5-4.0%, K 2 4.0 to 5.0 percent of O, 0.3 to 0.5 percent of ZnO and TiO 2 0.05 to 0.2 percent of Fe 2 O 3 0.1 to 0.3 percent.
6. The process for preparing an antibacterial high-strength ceramic according to claim 1, wherein the ceramic obtained after firing further comprises polishing the surface of the glaze layer, and then coating an antibacterial antifouling coating.
7. The preparation process of the antibacterial high-strength ceramic according to claim 6, wherein the antibacterial antifouling coating comprises nano silver, silica sol, sodium dodecyl sulfate, polyvinyl alcohol, methyl cellulose and maltodextrin, and the mass ratio of the nano silver to the silica sol to the sodium dodecyl sulfate to the polyvinyl alcohol to the methyl cellulose to the maltodextrin is 0.5-1:10:3-5:1-2:0.5-1:0.5-1.
8. The method for preparing antibacterial high-strength ceramic according to claim 1, wherein the particle size of the nano antibacterial composition is 50 nm-200 nm.
9. The method for preparing antibacterial high-strength ceramic according to claim 1, wherein in S2, before the slip is sprayed, the slip is subjected to vacuum degree of 10 -3 ~1×10 -2 Vacuum bubble removal under the conditions of 50-55 ℃ and the pressure of MPa; when the glaze slurry is sprayed, the specific gravity of the glaze is 1.7-1.8 g/m 3 The glazing quantity is 700-800 g/m 2 。
10. The ceramic product prepared by the preparation process of the antibacterial high-strength ceramic according to any one of claims 1 to 9.
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