CN115353792A - Antibacterial weather-resistant multifunctional integrated intumescent transparent fireproof coating and preparation method thereof - Google Patents
Antibacterial weather-resistant multifunctional integrated intumescent transparent fireproof coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 79
- 239000011248 coating agent Substances 0.000 title claims abstract description 75
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 97
- 239000010452 phosphate Substances 0.000 claims abstract description 97
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 86
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 30
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 30
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003063 flame retardant Substances 0.000 claims abstract description 26
- 239000011787 zinc oxide Substances 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 18
- 229920003180 amino resin Polymers 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims description 65
- 239000002202 Polyethylene glycol Substances 0.000 claims description 31
- 229920001223 polyethylene glycol Polymers 0.000 claims description 31
- 239000007864 aqueous solution Substances 0.000 claims description 24
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 22
- 229920000877 Melamine resin Polymers 0.000 claims description 21
- 239000004640 Melamine resin Substances 0.000 claims description 21
- 150000007974 melamines Chemical class 0.000 claims description 20
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- -1 phosphate ester Chemical class 0.000 claims description 6
- 239000003242 anti bacterial agent Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 230000003115 biocidal effect Effects 0.000 claims 4
- 238000000034 method Methods 0.000 claims 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 15
- 238000013329 compounding Methods 0.000 abstract description 2
- 239000003973 paint Substances 0.000 description 17
- 239000000779 smoke Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- 238000010998 test method Methods 0.000 description 9
- 239000004566 building material Substances 0.000 description 7
- 238000012512 characterization method Methods 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 7
- 230000001629 suppression Effects 0.000 description 7
- 238000007605 air drying Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000000691 measurement method Methods 0.000 description 5
- LLESCOKXOGPFTP-UHFFFAOYSA-N zinc oxygen(2-) phosphoric acid Chemical compound [O-2].[Zn+2].OP(O)(O)=O LLESCOKXOGPFTP-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000004887 air purification Methods 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical class [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 241000205585 Aquilegia canadensis Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 240000000691 Houttuynia cordata Species 0.000 description 1
- 235000013719 Houttuynia cordata Nutrition 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910007541 Zn O Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- ZADYMNAVLSWLEQ-UHFFFAOYSA-N magnesium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[Mg+2].[Si+4] ZADYMNAVLSWLEQ-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- RAOCWFJKLAHUBB-UHFFFAOYSA-N methoxymethane;1,3,5-triazine-2,4,6-triamine Chemical compound COC.NC1=NC(N)=NC(N)=N1 RAOCWFJKLAHUBB-UHFFFAOYSA-N 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- MFPVDOIQNSMNEW-UHFFFAOYSA-N silver oxygen(2-) titanium(4+) Chemical compound [O--].[O--].[Ti+4].[Ag+] MFPVDOIQNSMNEW-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002023 wood 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
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C09D161/32—Modified amine-aldehyde condensates
-
- 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
-
- 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
- C09D5/18—Fireproof paints including high temperature resistant paints
- C09D5/185—Intumescent paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Plant Pathology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses an antibacterial weather-resistant multifunctional integrated intumescent transparent fireproof coating and a preparation method thereof, wherein the coating comprises nano metal oxide composite phosphate and amino resin, and the preparation process of the nano metal oxide composite phosphate comprises the following steps: firstly preparing phosphate, and then chemically grafting one of nano titanium dioxide and nano zinc oxide on the phosphate. According to the intumescent transparent fireproof coating, phosphate is prepared firstly, then the nanometer metal oxide is chemically grafted on a phosphate molecular chain, so that a better grafting rate can be obtained, and the transparent fireproof coating prepared by compounding with the amino resin can better enhance the flame retardant, weather resistance and antibacterial properties of the transparent fireproof coating while the transparency of the coating is maintained.
Description
Technical Field
The invention relates to an antibacterial weather-resistant multifunctional integrated intumescent transparent fireproof coating and a preparation method thereof, belonging to the technical field of coatings.
Background
The transparent fireproof coating has excellent decorative performance and fireproof and flame-retardant performance, so that the transparent fireproof coating is widely applied to the fields of historical relics, historical buildings, high-grade furniture and the like, and has a wide application prospect. However, the main functions of the existing fireproof coating are only limited to fire resistance, flame retardance and decorative beauty, and the performances in other aspects are ignored. With the continuous development of science and technology, the requirements of modern buildings, ancient buildings, engineering structural materials and the like on the performance of fireproof coatings are higher and higher, and besides the conventional fireproof and decoration aspects, the fireproof coatings also need to have certain comprehensive performance in other aspects, such as good aging resistance, antibacterial performance and the like.
At present, the research work for multifunctional transparent fireproof paint at home and abroad is gradually emphasized. For example, patent publication No. CN113308133A discloses an inorganic antibacterial purifying fireproof paint, nano silver particles and nano zinc powder are introduced into nano modified inorganic silicone resin as an environment-friendly antibacterial bactericide, and the prepared fireproof paint not only can purify formaldehyde, but also has high efficiency of weather resistance, fire resistance, salt resistance and alkali resistance. Patent publication No. CN108299919A discloses a flame-retardant antibacterial coating, which mainly comprises expanded perlite, a flame retardant, a surfactant, antibacterial particles and the like, wherein the antibacterial particles are selected from one or more of an anionic antibacterial agent, zinc oxide or copper oxide, and the prepared coating is excellent in antibacterial property, flame retardant property and mechanical property and long in service life. Patent publication No. CN108299919A discloses a preparation method of a flame-retardant antibacterial paint for wood equipment, wherein a mesoporous silica composite flame retardant and a titanium dioxide silver-loaded antibacterial agent are adopted, so that the flame-retardant effect is improved, and the titanium dioxide and silver and the mesoporous silica loaded flame retardant also generate a synergistic effect. Patent publication No. CN107936639A discloses an environment-friendly coating with heat insulation and antibacterial functions and a preparation method thereof, additives such as sepiolite, magnesium silicate, nano zinc oxide, honeysuckle powder and houttuynia cordata powder are mainly introduced into the coating, and the environment-friendly coating is obtained by physically blending the additives with acrylic resin, epoxy resin and hydroxyethyl cellulose. Patent document CN112063255A reports a high weather-resistant photocatalytic air purification exterior wall fireproof coating which is mainly prepared from water, emulsion, titanium dioxide, nano titanium dioxide, a dispersing agent, a defoaming agent, a film-forming auxiliary agent and the like, maintains excellent photocatalytic air purification function, and has good fireproof flame retardance and weather resistance.
In the existing reports, the application of the nano metal oxide in the fireproof coating is mainly concentrated in the field of non-transparent fireproof coatings, the function of the coating is simplified, and the research on the application of the nano metal oxide for synergistically enhancing the multifunctional integration of the transparent fireproof coating is less, so that the application requirement of the transparent fireproof coating cannot be met.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide an antibacterial weather-resistant multifunctional integrated intumescent transparent fireproof coating and a preparation method thereof.
The multifunctional integrated antibacterial weather-resistant intumescent transparent fireproof coating comprises nano metal oxide composite phosphate and amino resin, wherein the preparation process of the nano metal oxide composite phosphate comprises the following steps: firstly, phosphate is prepared, and then one of the nanometer titanium dioxide and the nanometer zinc oxide is chemically grafted on the phosphate.
Preferably, the mass ratio of the nano metal oxide composite phosphate to the amino resin is 1:1-2.
Preferably, the amino resin is methylated melamine resin or butylated melamine resin.
Preferably, in the nano metal oxide composite phosphate, the nano metal oxide accounts for 0.3-5wt%.
The invention also provides a preparation method of the intumescent transparent fire-retardant coating, which comprises the steps of respectively preparing the nano metal oxide composite phosphate and the amino resin into 50-80wt% aqueous solution, and then blending and stirring uniformly to obtain the intumescent transparent fire-retardant coating.
Preferably, the preparation process of the nano metal oxide composite phosphate comprises the following steps:
(1) Mixing and reacting polyethylene glycol and boric acid at 110-150 ℃ for 2-5h according to a molar ratio of 1-2.5; (ii) a Mixing and reacting the prepared polyethylene glycol borate with acid phosphate at the mass ratio of 10-20 to 90-80 at 30-70 ℃ for 0.5-2 h, and mixing and reacting at 120-150 ℃ for 2-6 h to obtain phosphate;
(2) Drying the nano metal oxide at 50-60 ℃ for 3-5h, then blending and stirring the nano metal oxide and the phosphate uniformly, performing ultrasonic dispersion at 40-60 ℃ for 0.5-1h, and mixing and reacting at 120-140 ℃ for 4-6h to obtain the nano metal oxide composite phosphate.
According to the invention, the nano metal oxide filler with the refractive index similar to that of the amino resin is selected, so that the light scattering phenomenon is reduced, the light transmittance of the fireproof coating can reach more than 80%, and the application requirements of the transparent fireproof coating are met while the flame retardant, weather resistant and antibacterial properties are provided. Compared with in-situ grafting, namely adding the nano metal oxide for grafting in the preparation process of the phosphate, the inventor surprisingly finds that the phosphate is prepared firstly, then the nano metal oxide is chemically grafted on a phosphate molecular chain to obtain better grafting rate, and the transparent fireproof coating prepared by mixing the phosphate with the amino resin can better enhance the flame retardant property, the weather resistance and the antibacterial property of the transparent fireproof coating while keeping the transparency of the coating.
The invention has the advantages that:
(1) The refractive index of the metal oxide filler selected in the invention is similar to that of the amino resin, so that the light scattering phenomenon is reduced, the light transmittance of the fireproof coating reaches more than 80%, and the application requirements of the transparent fireproof coating are met while the flame retardant, weather-resistant and antibacterial properties are provided.
(2) According to the intumescent transparent fireproof coating, phosphate is prepared firstly, then the nanometer metal oxide is chemically grafted on a phosphate molecular chain, so that a better grafting rate can be obtained, and the transparent fireproof coating prepared by compounding with the amino resin can better enhance the flame retardant, weather resistance and antibacterial properties of the transparent fireproof coating while the transparency of the coating is maintained.
(3) The intumescent transparent fireproof coating can form a compact intumescent carbon layer structure, has a good fireproof protection effect on a base material, wherein the nano metal oxide and the intumescent flame retardant have a synergistic effect, and can remarkably improve the flame retardant, weather resistance and antibacterial effects of the transparent fireproof coating.
Drawings
FIG. 1 is an infrared spectrum of a nano titanium dioxide chemically grafted phosphate and an ungrafted phosphate;
as shown in figure 1, the nanometer titanium dioxide graft phosphate ester is 800-1400cm -1 Significant broadening and enhancement of absorption peaks between, 650cm -1 Ti-O bonds appear nearby, which shows that the nano titanium dioxide is successfully grafted to the molecular chain of the phosphate ester.
FIG. 2 is an infrared spectrum of a chemical grafted phosphate and an ungrafted phosphate of nano zinc oxide;
as shown in figure 2, the nano zinc oxide grafted phosphate is 800-1400cm -1 The absorption peak between them is obviously widened and enhanced, 419cm -1 Zn-O bonds appear nearby, which shows that the nano zinc oxide is successfully grafted to the molecular chain of the phosphate ester.
Detailed Description
The following examples are further illustrative of the present invention and are specifically detailed below:
nano titanium dioxide, shanghai Yingyun New Material Co., ltd., CAS No.13463-67-7
Nano zinc oxide, shanghai Yingyun New Material Co., ltd., CAS No.1314-13-2
Methylated melamine resin, shanghai Xinhua resin plant, model number 5386-60
Butylated melamine resin, shanghai Xinhua resin plant, type 582-2
Escherichia coli, peking biological Collection, model ATCC 25922
Example 1
(1) Preparation of nano titanium dioxide grafted phosphate
Mixing polyethylene glycol and boric acid according to a molar ratio of 2.5:1, mixing and reacting for 3 hours at 130 ℃ to obtain polyethylene glycol borate; mixing phosphoric acid, pentaerythritol and n-butanol according to a molar ratio of 3.85; mixing the prepared polyethylene glycol borate and acid phosphate according to the mass ratio of 15;
and (2) placing the nano titanium dioxide in a 50 ℃ forced air drying oven for drying for 5h, cooling the prepared phosphate to room temperature, uniformly stirring and mixing the phosphate with the nano titanium dioxide accounting for 0.3 percent of the mass of the phosphate, ultrasonically dispersing the phosphate in an ultrasonic disperser at 50 ℃ for 30min, and placing the phosphate in a three-neck flask for mixing and reacting at 120 ℃ for 4h to obtain the nano titanium dioxide composite phosphate.
(2) Preparation of nano expansion type transparent fire-proof paint
In the embodiment, the modified nano-titanium dioxide grafted phosphate is prepared by blending a component A of nano-titanium dioxide grafted phosphate and a component B of methylated melamine resin according to a mass ratio of 1:2, wherein the component A is prepared into a nano-titanium dioxide grafted phosphate aqueous solution with a mass percentage of 60%, the component B is prepared into an aqueous solution of methylated melamine resin with a mass percentage of 60%, and the two aqueous solutions are mixed according to a ratio of 1:2 blending and stirring evenly.
(3) Characterization of fire-retardant coating Properties
The flame retardance, smoke suppression performance, antibacterial performance and weather resistance of the multifunctional integrated transparent fireproof coating prepared in the embodiment are measured by GB 12441-2018 ' finishing type fireproof coating ', GB/T8626-2007 ' smoke density test method for combustion or decomposition of building materials ' and GB/T21866-2008 ' antibacterial property test method and antibacterial effect of antibacterial coating (paint film), and the results are shown in the following table.
TABLE 1
Example 2
(1) Preparation of nano zinc oxide grafted phosphate
Mixing polyethylene glycol and boric acid according to a molar ratio of 2.5:1, mixing and reacting for 3 hours at 130 ℃ to obtain polyethylene glycol borate; mixing phosphoric acid, pentaerythritol and n-butanol according to a molar ratio of 3.85; mixing and reacting the prepared polyethylene glycol borate with acid phosphate at 50 ℃ for 1h, and mixing and reacting at 115 ℃ for 4h according to the mass ratio of 15;
and (2) placing the nano zinc oxide in a 50 ℃ forced air drying oven for drying for 5h, cooling the prepared phosphate to room temperature, uniformly stirring and mixing the phosphate with the nano zinc oxide accounting for 5% of the mass percent of the phosphate, ultrasonically dispersing the phosphate in an ultrasonic disperser at 50 ℃ for 30min, and placing the phosphate in a three-neck flask for mixing and reacting at 120 ℃ for 4h to obtain the nano zinc oxide composite phosphate.
(2) Preparation of nano expansion type transparent fire-proof paint
In the embodiment, the modified zinc phosphate is prepared by blending nanometer zinc oxide grafted phosphate of component A and methylated melamine resin of component B according to the mass ratio of 1:2, wherein the component A is prepared into a nanometer zinc oxide grafted phosphate aqueous solution with the mass percentage of 60%, the component B is prepared into an aqueous solution of methylated melamine resin with the mass percentage of 60%, and the two aqueous solutions are mixed according to the mass ratio of 1:2 blending and stirring evenly.
(3) Characterization of fire-retardant coating Properties
The flame retardance, smoke suppression performance, antibacterial performance and weather resistance of the multifunctional integrated transparent fireproof coating prepared in the embodiment are measured by GB 12441-2018 'finishing type fireproof coating', GB/T8626-2007 'smoke density test method for combustion or decomposition of building materials' and GB/T21866-2008 'antibacterial property measurement method and antibacterial effect of antibacterial coating (paint film)', and the results are shown in the following table.
TABLE 2
Comparative example 1
In the embodiment, the modified phosphate is formed by blending phosphate in a component A and methylated melamine resin in a component B according to a mass ratio of 1:2, wherein the component A is a phosphate aqueous solution with a mass percentage of 60%, and the component B is an aqueous solution of methylated melamine resin with a mass percentage of 60%.
(1) Preparation of phosphoric esters
Mixing polyethylene glycol and boric acid according to a molar ratio of 2.5:1, mixing and reacting for 3 hours at 130 ℃ to obtain polyethylene glycol borate; mixing phosphoric acid, pentaerythritol and n-butanol according to a molar ratio of 3.85; mixing and reacting the prepared polyethylene glycol borate with acid phosphate at 50 ℃ for 1h, and mixing and reacting at 115 ℃ for 4h according to the mass ratio of 15. And then, dissolving phosphate into distilled water to prepare a phosphate aqueous solution with the mass percent of 60 percent, namely the component A.
(2) Preparation of expansion type transparent fire-retardant coating
Uniformly blending the component A and the component B according to the mass ratio of 1:2 to prepare the intumescent transparent fireproof coating, wherein the component B is 60 mass percent of aqueous solution of methyl ether melamine resin.
(3) Characterization of intumescent transparent fire-retardant coating
The flame retardance, smoke suppression performance, antibacterial performance and weather resistance of the transparent fireproof coating prepared in the comparative example are measured by GB 12441-2018 'finishing type fireproof coating', GB/T8626-2007 'smoke density test method for combustion or decomposition of building materials' and GB/T21866-2008 'antibacterial property measurement method and antibacterial effect of antibacterial coating (paint film)', and the results are shown in the following table.
TABLE 3
Comparative example 2
(1) Preparation of nano titanium dioxide phosphate
Mixing polyethylene glycol and boric acid according to a molar ratio of 2.5:1, mixing and reacting for 3 hours at 130 ℃ to obtain polyethylene glycol borate; mixing phosphoric acid, pentaerythritol and n-butanol according to a molar ratio of 3.85; mixing the prepared polyethylene glycol borate and acid phosphate according to the mass ratio of 15;
and (3) placing the nano titanium dioxide in a 50 ℃ forced air drying oven for drying for 5h, cooling the prepared phosphate to room temperature, and uniformly stirring and mixing the phosphate with the nano titanium dioxide accounting for 0.3 percent of the mass of the phosphate to obtain the nano titanium dioxide phosphate.
(2) Preparation of nano expansion type transparent fire-proof paint
In the embodiment, the nano titanium dioxide phosphate ester is prepared by blending a component A and a methylated melamine resin of a component B according to a mass ratio of 1:2, wherein the component A is prepared into a nano titanium dioxide phosphate ester aqueous solution with a mass percentage of 60%, the component B is prepared into an aqueous solution of methylated melamine resin with a mass percentage of 60%, and the two aqueous solutions are mixed according to a ratio of 1:2 blending and stirring evenly.
(3) Characterization of intumescent transparent fire-retardant coating
The flame retardance, smoke suppression performance, antibacterial performance and weather resistance of the transparent fireproof coating prepared in the comparative example are measured by GB 12441-2018 'finishing type fireproof coating', GB/T8626-2007 'smoke density test method for combustion or decomposition of building materials' and GB/T21866-2008 'antibacterial property measurement method and antibacterial effect of antibacterial coating (paint film)', and the results are shown in the following table.
TABLE 4
Comparative example 3
(1) Preparation of nano zinc oxide phosphate
Mixing polyethylene glycol and boric acid according to a molar ratio of 2.5:1, mixing and reacting for 3 hours at 130 ℃ to obtain polyethylene glycol borate; phosphoric acid, pentaerythritol and n-butanol are mixed and reacted for 4h at 105 ℃ and 2h at 120 ℃ according to the molar ratio of 3; mixing the prepared polyethylene glycol borate and acid phosphate according to the mass ratio of 15;
and (2) placing the nano zinc oxide in a 50 ℃ forced air drying oven for drying for 5h, cooling the prepared phosphate to room temperature, and uniformly stirring and mixing the phosphate with the nano zinc oxide accounting for 5% of the mass of the phosphate to obtain the nano zinc oxide phosphate.
(2) Preparation of nano expansion type transparent fire-proof paint
In the embodiment, the modified zinc phosphate is prepared by blending nanometer zinc oxide phosphate of component A and methylated melamine resin of component B according to the mass ratio of 1:2, wherein the component A is prepared into a nanometer zinc oxide phosphate aqueous solution with the mass percentage of 60%, the component B is prepared into an aqueous solution of methylated melamine resin with the mass percentage of 60%, and the two aqueous solutions are mixed according to the ratio of 1:2 blending and stirring uniformly.
(3) Characterization of intumescent transparent fire-retardant coating
The flame retardance, smoke suppression performance, antibacterial performance and weather resistance of the transparent fireproof coating prepared in the comparative example are measured by GB 12441-2018 ' finishing type fireproof coating ', GB/T8626-2007 ' smoke density test method for combustion or decomposition of building materials ' and GB/T21866-2008 ' antibacterial property test method and antibacterial effect of antibacterial coating (paint film), and the results are shown in the following table.
TABLE 5
Comparative example 4
(1) Preparation of nano titanium dioxide grafted phosphate
Mixing polyethylene glycol and boric acid according to a molar ratio of 2.5:1, mixing and reacting for 3 hours at 130 ℃ to obtain polyethylene glycol borate; mixing phosphoric acid, pentaerythritol and n-butanol according to a molar ratio of 3.85; the preparation method comprises the following steps of putting the nano titanium dioxide into a 50 ℃ forced air drying oven to be dried for 5 hours, cooling the prepared polyethylene glycol borate and the prepared acid phosphate to room temperature, mixing and reacting the polyethylene glycol borate, the prepared acid phosphate (the mass ratio of the polyethylene glycol borate to the prepared acid phosphate is 15) and the nano titanium dioxide accounting for 0.3 percent of the total mass of the polyethylene glycol borate and the prepared acid phosphate at 50 ℃ for 1 hour, and mixing and reacting at 115 ℃ for 4 hours to obtain the nano titanium dioxide phosphate.
(2) Preparation of nano expansion type transparent fire-proof paint
In the embodiment, the modified nano-titanium dioxide grafted phosphate is prepared by blending a component A of nano-titanium dioxide grafted phosphate and a component B of methylated melamine resin according to a mass ratio of 1:2, wherein the component A is prepared into a nano-titanium dioxide grafted phosphate aqueous solution with a mass percentage of 60%, the component B is prepared into an aqueous solution of methylated melamine resin with a mass percentage of 60%, and the two aqueous solutions are mixed according to a ratio of 1:2 blending and stirring uniformly.
(3) Characterization of fire-retardant coating Properties
The flame retardance, smoke suppression performance, antibacterial performance and weather resistance of the transparent fireproof coating prepared in the comparative example are measured by GB 12441-2018 'finishing type fireproof coating', GB/T8626-2007 'smoke density test method for combustion or decomposition of building materials' and GB/T21866-2008 'antibacterial property measurement method and antibacterial effect of antibacterial coating (paint film)', and the results are shown in the following table.
TABLE 6
Comparative example 5
(1) Preparation of nano zinc oxide grafted phosphate
Mixing polyethylene glycol and boric acid according to a molar ratio of 2.5:1, mixing and reacting for 3 hours at 130 ℃ to obtain polyethylene glycol borate; mixing phosphoric acid, pentaerythritol and n-butanol according to a molar ratio of 3.85; the preparation method comprises the following steps of putting nano titanium dioxide in a 50 ℃ forced air drying oven to dry for 5 hours, cooling the prepared polyethylene glycol borate and acid phosphate to room temperature, mixing and reacting the polyethylene glycol borate, the acid phosphate (the mass ratio of the polyethylene glycol borate to the acid phosphate is 15) and nano zinc oxide accounting for 5% of the total mass of the polyethylene glycol borate and the acid phosphate at 50 ℃ for 1 hour, and mixing and reacting at 115 ℃ for 4 hours to obtain the nano zinc oxide phosphate.
(2) Preparation of nano expansion type transparent fire-proof paint
In the embodiment, the nano zinc oxide grafted phosphate ester of the component A and the methylated melamine resin of the component B are blended according to the mass ratio of 1:2, wherein the component A is prepared into a nano titanium dioxide grafted phosphate ester aqueous solution with the mass percentage of 60%, the component B is prepared into a methylated melamine resin aqueous solution with the mass percentage of 60%, and the two aqueous solutions are mixed according to the ratio of 1:2 blending and stirring uniformly.
(3) Characterization of fire-retardant coating Properties
The flame retardance, smoke suppression performance, antibacterial performance and weather resistance of the transparent fireproof coating prepared in the comparative example are measured by GB 12441-2018 'finishing type fireproof coating', GB/T8626-2007 'smoke density test method for combustion or decomposition of building materials' and GB/T21866-2008 'antibacterial property measurement method and antibacterial effect of antibacterial coating (paint film)', and the results are shown in the following table.
TABLE 7
Claims (6)
1. The utility model provides an antibiotic resistant weather multifunctional integral expansion type transparent fireproof coating, which is characterized in that: the preparation method comprises the following steps of preparing nano metal oxide composite phosphate and amino resin: firstly preparing phosphate, and then chemically grafting one of nano titanium dioxide and nano zinc oxide on the phosphate.
2. An expansion type transparent fireproof coating with integrated functions of antibiosis, weather resistance and the like is characterized in that: the mass ratio of the nano metal oxide composite phosphate to the amino resin is 1:1-2.
3. An expansion type transparent fireproof coating with integrated functions of antibiosis, weather resistance and the like is characterized in that: the amino resin is methylated melamine resin or butylated melamine resin.
4. The utility model provides an antibiotic resistant weather multifunctional integral expansion type transparent fireproof coating, which is characterized in that: in the nano metal oxide composite phosphate, the nano metal oxide accounts for 0.3-5wt%.
5. The preparation method of the antibacterial weather-resistant multifunctional integrated intumescent transparent fire-retardant coating as claimed in any one of claims 1 to 4, characterized in that: respectively preparing the nano metal oxide composite phosphate and the amino resin into 50-80wt% aqueous solution, and then blending and stirring uniformly to obtain the intumescent transparent fireproof coating.
6. The method of claim 5, wherein: the preparation process of the nano metal oxide composite phosphate ester comprises the following steps:
(1) Mixing polyethylene glycol and boric acid according to a molar ratio of 1-2.5; mixing phosphoric acid, pentaerythritol and n-butanol according to a molar ratio of 1-3; mixing and reacting the prepared polyethylene glycol borate with acid phosphate at the mass ratio of 10-20 to 90-80 at 30-70 ℃ for 0.5-2 h, and mixing and reacting at 120-150 ℃ for 2-6 h to obtain phosphate;
(2) Drying the nano metal oxide at 50-60 ℃ for 3-5h, then blending and stirring the nano metal oxide and the phosphate uniformly, performing ultrasonic dispersion at 40-60 ℃ for 0.5-1h, and mixing and reacting at 120-140 ℃ for 4-6h to obtain the nano metal oxide composite phosphate.
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Application publication date: 20221118 |