CN112812669A - Method for preparing flower-like silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint - Google Patents
Method for preparing flower-like silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint Download PDFInfo
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- CN112812669A CN112812669A CN202011623911.1A CN202011623911A CN112812669A CN 112812669 A CN112812669 A CN 112812669A CN 202011623911 A CN202011623911 A CN 202011623911A CN 112812669 A CN112812669 A CN 112812669A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 95
- 239000002131 composite material Substances 0.000 title claims abstract description 68
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 67
- 239000003973 paint Substances 0.000 title claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 40
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 49
- 239000002243 precursor Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- FANANXQSVYPRCQ-UHFFFAOYSA-N azane;silicon Chemical compound N.[Si] FANANXQSVYPRCQ-UHFFFAOYSA-N 0.000 claims description 15
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 15
- 239000012498 ultrapure water Substances 0.000 claims description 15
- 239000000049 pigment Substances 0.000 claims description 13
- 239000000945 filler Substances 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- FRIKWZARTBPWBN-UHFFFAOYSA-N [Si].O=[Si]=O Chemical compound [Si].O=[Si]=O FRIKWZARTBPWBN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000002562 thickening agent Substances 0.000 claims description 7
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- 239000002518 antifoaming agent Substances 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 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 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 5
- 229920005749 polyurethane resin Polymers 0.000 claims description 5
- 239000005049 silicon tetrachloride Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002042 Silver nanowire Substances 0.000 claims description 2
- 229920000180 alkyd Polymers 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005052 trichlorosilane Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 34
- 241000588724 Escherichia coli Species 0.000 description 4
- 241000191967 Staphylococcus aureus Species 0.000 description 4
- 230000002159 abnormal effect Effects 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- 230000007774 longterm Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention discloses a method for preparing flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint, which comprises the steps of preparing a precursor solution of silicon dioxide-based composite photocatalytic particles; sequentially and mechanically stirring the precursor solution and the components of the water-based interior wall paint to obtain a mixed coating; the invention disperses the silicon dioxide-based composite photocatalytic nano particles in the aqueous interior wall paint in the form of precursor mixed liquid, so that the stability of the photocatalytic particles is better, the dispersibility is better, the attached photocatalytic nano particles are uniformly dispersed and coated on the flower-shaped silicon dioxide photocatalytic particles, the specific surface area is larger, more active site quantity is provided, the antibacterial and bactericidal effect of the prepared composite aqueous interior wall paint is effectively improved, the adsorption effect of silicon dioxide has important influence on the photocatalytic activity, the growth of the composite photocatalytic particles can be effectively controlled, the smaller particle size and the high specific surface area are obtained, and the photocatalytic and antibacterial effect is further improved.
Description
Technical Field
The invention belongs to the technical field of photocatalytic environment-friendly coatings, and particularly relates to a method for preparing a flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint.
Background
As interior wall decoration materials widely used in aqueous interior wall paints are in contact with human bodies for a long time in living and working, the contents of VOC, APEO and PFOS harmful substances and the contents of free formaldehyde, lead, chromium and other heavy metal ions in the aqueous interior wall paints have attracted much attention to the safety of long-term use thereof. Meanwhile, as the requirement of people on the indoor air quality is higher and higher, especially the continuous influence of air-borne diseases of various closed spaces, the people are forced to put forward higher requirements on the indoor antibacterial decorative material. The existing photocatalytic interior wall paint is basically prepared by simply mechanically stirring ready-made photocatalytic particles, resin emulsion and other additives, and the uniform dispersibility and agglomeration of the photocatalytic particles cannot be guaranteed. In addition, the addition of the single structure or single kind of photocatalytic particles can also cause the poor photocatalytic antibacterial effect of the water-based interior wall paint.
Disclosure of Invention
In summary, the present invention aims to provide a method for preparing a flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint, so as to solve the problem in the prior art that the antibacterial effect of the prepared photocatalytic aqueous interior wall paint is poor due to the fact that the added photocatalytic particles with a single structure or a single kind are easy to agglomerate and have non-uniform dispersibility in the aqueous interior wall paint.
In order to achieve the purpose, the invention provides the following technical scheme:
the method for preparing the flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint comprises the following steps:
step 1, preparing a precursor solution of the silicon dioxide-based composite photocatalytic particles; the method comprises the following specific steps:
step 1.1, weighing a silicon dioxide silicon source, dissolving the silicon dioxide silicon source in ultrapure water, adding an ammonia water solution to control a silicon-ammonia complex to separate out a precipitate, then performing suction filtration to separate the precipitate, fully cleaning the precipitate by using the ultrapure water and absolute ethyl alcohol, and drying in a constant-temperature drying oven to obtain the silicon-ammonia complex precipitate;
step 1.2, adding 6mg/mL of solution attached with photocatalytic nanoparticles into the silicon-ammonia complex precipitate prepared in the step 1.1, configuring the solution into 0.5-1.5mol/L precursor solution through ammonia water and ultrapure water, and carrying out ultrasonic oscillation for 30min to fully disperse the precursor solution so as to obtain a precursor solution of the silicon dioxide-based composite photocatalytic particles;
and 3, carrying out microwave reaction synthesis on the mixed coating to obtain the flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint.
Further, the silica-based composite photocatalytic particles include silica photocatalytic particles and attached photocatalytic nanoparticles.
Further, the silicon source of silicon dioxide in step 1.2 is one or more of trichlorosilane, silicon tetrachloride, dichlorosilane and silane.
Further, the attached photocatalytic nanoparticles in step 1.2 are one or more of silver nanowires, graphene oxide, reduced graphene oxide, or graphene quantum dots.
Further, in the step 2, the silica-based composite photocatalytic particle and the water-based interior wall paint comprise, by mass, 13-15 wt% of the silica-based composite photocatalytic particle, 47-65 wt% of single-component water-based resin, 14-20 wt% of pigment and filler, 2-3 wt% of a dispersant, 2-3 wt% of a defoaming agent, 1-2 wt% of a thickener and 17-20 wt% of water.
Further, the method for mixing the composite precursor solution and the components of the water-based interior wall paint in the step 2 is that the single-component water-based resin is added into the composite precursor solution and fully stirred for 30min at the stirring speed of 850r/min, and then the mixture of the pigment, the dispersant, the defoamer and the thickener is added and fully stirred for 1h at the stirring speed of 1600 + 1900 r/min.
Further, in the step 3, the heating temperature of the microwave reaction is 95-115 ℃, and the reaction time is 3-5.5 min.
Further, the single-component water-based resin is one or more of water-based alkyd resin, water-based acrylic resin and water-based polyurethane resin.
Furthermore, the pigment and filler is one or more of calcium carbonate, calcined kaolin and silicon dioxide.
The flower-shaped silicon dioxide based composite photocatalytic antibacterial water-based interior wall paint synthesized by microwave is observed under a scanning electron microscope, and the diameter of the obtained flower-shaped silicon dioxide based composite photocatalytic particles is concentrated between 2 and 2.5 mu m.
The invention has the beneficial effects that:
1. according to the invention, the silica-based composite photocatalytic nanoparticles are dispersed in the water-based interior wall paint in the form of precursor mixed liquid, so that the stability of the photocatalytic particles is better, the dispersibility of the silica-based composite photocatalytic particles in the water-based interior wall paint is better, the particles are not easy to agglomerate, and the prepared water-based interior wall paint has more excellent photocatalytic antibacterial performance;
2. the flower-shaped silicon-based composite photocatalytic particles are synthesized in the water-based interior wall paint through a microwave rapid reaction, compared with the traditional photocatalytic particles, the attached photocatalytic nanoparticles are uniformly dispersed and coated on the flower-shaped silicon dioxide photocatalytic particles, the specific surface area of the synthesized flower-shaped silicon dioxide-based composite photocatalytic particles is larger, more active site numbers are provided, the antibacterial and bactericidal effects of the prepared composite water-based interior wall paint can be effectively improved, and finally, the photocatalytic antibacterial inactivation of escherichia coli and staphylococcus aureus in the composite water-based interior wall paint under the condition of visible light can be realized in a short time;
3. according to the invention, by adopting different adding sequences and adding processes of the precursor mixed solution of the silica-based composite photocatalytic particles and various water-based interior wall paint raw materials, on one hand, the resin in the water-based interior wall paint has the advantages of good mechanical property, good machining property, good film forming property, strong adhesive force, high drying speed and the like, and the defects of insufficient mechanical property of direct mixing of the photocatalytic particles and various water-based interior wall paint raw materials are solved. On the other hand, the flower-shaped silicon dioxide-based composite photocatalytic particles are more tightly combined with the water-based interior wall paint, the photocatalytic particles are not easy to fall off and agglomerate in the construction and long-term use processes, and the problems that the photocatalytic particles with single structures or single components are not tightly combined with the water-based interior wall paint, and the photocatalytic particles are easy to fall off or agglomerate are solved;
4. the adsorption effect of the silicon dioxide has an important influence on the photocatalytic activity, the silicon dioxide can increase the strong adsorption effect of the acid sites on the surface of the composite photocatalytic particles on organic matters, and stronger groups are formed on the surface and are used as the capture sites of holes to prevent the recombination of electron-hole pairs, so that the silicon dioxide has a better photocatalytic effect. Meanwhile, the silicon dioxide can effectively control the growth of the composite photocatalytic particles, so that smaller particle size and high specific surface area are obtained, and the photocatalytic antibacterial effect is further improved.
5. Compared with other shapes of the silicon dioxide composite photocatalytic particles, such as particles, rods and the like, the flower-shaped silicon dioxide composite photocatalytic particles have larger specific surface area, more photocatalytic nanoparticles can be supported and attached on the surface, and the supported space direction and active sites are more abundant, so that the degradability and the bactericidal property of the flower-shaped silicon dioxide composite photocatalytic particle antibacterial water-based interior wall paint under visible light are higher under the same photocatalytic particle loading.
Drawings
FIG. 1 is a 5000-fold enlarged microscopic structure diagram of the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint prepared in example 3 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will become apparent to those skilled in the art after reading the present application and which fall within the limits of the appended claims.
Example 1
The method for preparing the flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint comprises the following steps:
step 1, preparing a precursor solution of the silica-based composite photocatalytic particle: weighing silicon dioxide silicon source silicon tetrachloride and dissolving in ultrapure water, adding an ammonia water solution to control the silicon-ammonia complex to separate out precipitate, then performing suction filtration to separate the precipitate, fully cleaning the precipitate by using ultrapure water and absolute ethyl alcohol, and drying in a constant-temperature drying oven to obtain the silicon-ammonia complex precipitate. And then adding a solution of 6mg/mL attached photocatalytic nanoparticle graphene and reduced graphene oxide into the prepared silicon-ammonia complex precipitate, configuring the solution into a precursor solution of 0.5mol/L by ammonia water and ultrapure water, and performing ultrasonic oscillation for 30min to obtain the uniformly dispersed silicon dioxide-based composite photocatalytic particle precursor solution. And 2, selecting 30 wt% of the composite precursor solution prepared in the step 1 and 51 wt% of waterborne polyurethane resin, fully stirring for 30min in a reaction kettle at a stirring speed of 750r/min, then adding a mixture of 14 wt% of pigment and filler, 2 wt% of dispersing agent, 2 wt% of defoaming agent and 1 wt% of thickening agent, and fully stirring for 1h in the reaction kettle at a stirring speed of 1700r/min, wherein the pigment and filler comprises 33 wt% of calcium carbonate, 11 wt% of calcined kaolin and 56 wt% of silicon dioxide. And 3, putting the mixed coating prepared in the step 2 into a microwave rapid reaction synthesizer to react for 3min at 95 ℃. The photocatalytic degradation performance of the finally prepared flower-shaped silica-based composite photocatalytic antibacterial water-based interior wall paint reaches that 95% of 10mg/L rhodamine B solution is degraded within 40min under the condition of visible light, 100% of escherichia coli and staphylococcus aureus are killed within 50min under the condition of visible light, the VOC content is 0, the alkali resistance is not abnormal (24h), and the drying time is 30min (surface drying).
Example 2
The method for preparing the flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint comprises the following steps:
step 1, preparing a precursor solution of the silica-based composite photocatalytic particle: weighing silicon dioxide silicon source silicon tetrachloride and dissolving in ultrapure water, adding an ammonia water solution to control the silicon-ammonia complex to separate out precipitate, then performing suction filtration to separate the precipitate, fully cleaning the precipitate by using ultrapure water and absolute ethyl alcohol, and drying in a constant-temperature drying oven to obtain the silicon-ammonia complex precipitate. And then adding a solution of 6mg/mL attached photocatalytic nanoparticle graphene and reduced graphene oxide into the prepared silicon-ammonia complex precipitate, configuring the solution into a precursor solution of 1.0mol/L by ammonia water and ultrapure water, and performing ultrasonic oscillation for 30min to obtain the uniformly dispersed silicon dioxide-based composite photocatalytic particle precursor solution. And 2, selecting 31 wt% of the composite precursor solution prepared in the step 1 and 50 wt% of waterborne polyurethane resin, fully stirring for 30min at a stirring speed of 800r/min in a reaction kettle, then adding a mixture of 14 wt% of pigment and filler, 2 wt% of dispersing agent, 2 wt% of defoaming agent and 1 wt% of thickening agent, and fully stirring for 1h at a stirring speed of 1800r/min in the reaction kettle, wherein the pigment and filler comprises 33 wt% of calcium carbonate, 11 wt% of calcined kaolin and 56 wt% of silicon dioxide. And 3, putting the mixed coating prepared in the step 2 into a microwave rapid reaction synthesizer to react for 4.5min at 105 ℃. The photocatalytic degradation performance of the finally prepared flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint reaches that a 10mg/L rhodamine B solution which degrades 96% in 30min under the visible light condition kills 100% of escherichia coli and staphylococcus aureus in 30 hours under the visible light condition, the VOC content is 0, the alkali resistance is not abnormal (24h), and the drying time is 30min (surface drying).
Example 3
The method for preparing the flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint comprises the following steps:
step 1, preparing a precursor solution of the silica-based composite photocatalytic particle: weighing silicon dioxide silicon source silicon tetrachloride and dissolving in ultrapure water, adding an ammonia water solution to control the silicon-ammonia complex to separate out precipitate, then performing suction filtration to separate the precipitate, fully cleaning the precipitate by using ultrapure water and absolute ethyl alcohol, and drying in a constant-temperature drying oven to obtain the silicon-ammonia complex precipitate. And then adding a solution of 6mg/mL attached photocatalytic nanoparticle graphene and reduced graphene oxide into the prepared silicon-ammonia complex precipitate, configuring the solution into a precursor solution of 1.5mol/L by ammonia water and ultrapure water, and performing ultrasonic oscillation for 30min to obtain the uniformly dispersed silicon dioxide-based composite photocatalytic particle precursor solution. And 2, selecting 34 wt% of the composite precursor solution prepared in the step 1 and 47 wt% of waterborne polyurethane resin, fully stirring for 30min in a reaction kettle at a stirring speed of 850r/min, then adding a mixture of 14 wt% of pigment and filler, 2 wt% of dispersing agent, 2 wt% of defoaming agent and 1 wt% of thickening agent, and fully stirring for 1h in the reaction kettle at a stirring speed of 1900r/min, wherein the pigment and filler comprises 33 wt% of calcium carbonate, 11 wt% of calcined kaolin and 56 wt% of silicon pigment. And 3, putting the mixed coating prepared in the step 2 into a microwave rapid reaction synthesizer to react for 5.5min at the temperature of 115 ℃. The photocatalytic degradation performance of the finally prepared flower-shaped silica-based composite photocatalytic antibacterial water-based interior wall paint reaches 98% of 10mg/L rhodamine B solution degraded within 20min under the visible light condition, 100% of escherichia coli and staphylococcus aureus are killed within 25min under the visible light condition, the VOC content is 0, the alkali resistance is not abnormal (24h), and the drying time is 30min (surface drying).
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (9)
1. The method for preparing the flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint is characterized by comprising the following steps of:
step 1, preparing a precursor solution of the silicon dioxide-based composite photocatalytic particles; the method comprises the following specific steps:
step 1.1, weighing a silicon dioxide silicon source, dissolving the silicon dioxide silicon source in ultrapure water, adding an ammonia water solution to control a silicon-ammonia complex to separate out a precipitate, then performing suction filtration to separate the precipitate, fully cleaning the precipitate by using the ultrapure water and absolute ethyl alcohol, and drying in a constant-temperature drying oven to obtain the silicon-ammonia complex precipitate;
step 1.2, adding 6mg/mL of solution attached with photocatalytic nanoparticles into the silicon-ammonia complex precipitate prepared in the step 1.1, configuring the solution into 0.5-1.5mol/L precursor solution through ammonia water and ultrapure water, and carrying out ultrasonic oscillation for 30min to fully disperse the precursor solution so as to obtain a precursor solution of the silicon dioxide-based composite photocatalytic particles;
step 2, sequentially mechanically stirring and uniformly mixing the composite precursor solution obtained in the step 1 and the components of the water-based interior wall paint in a reaction kettle to obtain a mixed coating;
and 3, carrying out microwave reaction synthesis on the mixed coating to obtain the flower-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint.
2. The method for preparing the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint according to claim 1, wherein the silica-based composite photocatalytic particles comprise silica photocatalytic particles and attached photocatalytic nanoparticles.
3. The method for preparing the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint according to claim 1, wherein the silica silicon source in step 1.2 is one or more of trichlorosilane, silicon tetrachloride, dichlorosilane and silane.
4. The method for preparing the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint according to claim 2, wherein the attached photocatalytic nanoparticles in the step 1.2 are one or more of silver nanowires, graphene oxide, reduced graphene oxide or graphene quantum dots.
5. The method for preparing the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint as claimed in claim 1, wherein the silica-based composite photocatalytic particle and the aqueous interior wall paint in step 2 comprise, by mass, 13-15% of the silica-based composite photocatalytic particle, 47-65% of the one-component aqueous resin, 14-20% of the pigment and filler, 2-3% of the dispersant, 2-3% of the defoaming agent, 1-2% of the thickener and 17-20% of water.
6. The method for preparing the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint as claimed in claim 1, wherein the step 2 of mixing the composite precursor solution and the aqueous interior wall paint comprises the steps of adding single-component aqueous resin into the composite precursor solution, fully stirring for 30min at the stirring speed of 550-850r/min, then adding a mixture of pigment, filler, dispersant, defoamer and thickener, and fully stirring for 1h at the stirring speed of 1600-1900 r/min.
7. The method for preparing the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint as claimed in claim 1, wherein the microwave reaction heating temperature in step 3 is 95-115 ℃ and the reaction time is 3-5.5 min.
8. The method for preparing the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint according to claim 5, wherein the single-component aqueous resin is one or more of an aqueous alkyd resin, an aqueous acrylic resin and an aqueous polyurethane resin.
9. The method for preparing the flower-like silica-based composite photocatalytic antibacterial aqueous interior wall paint as claimed in claim 5, wherein the pigment and filler is one or more of calcium carbonate, calcined kaolin and silicon dioxide.
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