CN115584206A - Water-based inorganic nano ceramic flame-retardant coating and preparation method thereof - Google Patents
Water-based inorganic nano ceramic flame-retardant coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 60
- 239000011248 coating agent Substances 0.000 title claims abstract description 56
- 239000000919 ceramic Substances 0.000 title claims abstract description 54
- 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 title claims abstract description 51
- 239000003063 flame retardant Substances 0.000 title claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 127
- 239000000654 additive Substances 0.000 claims abstract description 61
- 230000000996 additive effect Effects 0.000 claims abstract description 61
- 238000002156 mixing Methods 0.000 claims abstract description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- -1 tripropylamine azidobenzene isothiocyanate siloxane Chemical class 0.000 claims abstract description 37
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 18
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 18
- BHXFKXOIODIUJO-UHFFFAOYSA-N benzene-1,4-dicarbonitrile Chemical compound N#CC1=CC=C(C#N)C=C1 BHXFKXOIODIUJO-UHFFFAOYSA-N 0.000 claims abstract description 12
- YCYFLSYXIDCLPT-UHFFFAOYSA-N hydroxy-dioxo-diphenyl-lambda7-iodane Chemical compound C1(=CC=CC=C1)I(=O)(=O)(C1=CC=CC=C1)O YCYFLSYXIDCLPT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 108
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 26
- 239000011259 mixed solution Substances 0.000 claims description 23
- BZFKSWOGZQMOMO-UHFFFAOYSA-N 3-chloropropan-1-amine Chemical compound NCCCCl BZFKSWOGZQMOMO-UHFFFAOYSA-N 0.000 claims description 20
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- VWYTZNPMXYCBPK-UHFFFAOYSA-N 3-bromobenzene-1,2-diamine Chemical compound NC1=CC=CC(Br)=C1N VWYTZNPMXYCBPK-UHFFFAOYSA-N 0.000 claims description 9
- 238000007664 blowing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- KAHOWFCMRDOJOA-UHFFFAOYSA-N 1,2-diethyl-3-iodobenzene Chemical compound C(C)C=1C(=C(C=CC1)I)CC KAHOWFCMRDOJOA-UHFFFAOYSA-N 0.000 claims description 5
- YHIWBVHIGCRVLE-UHFFFAOYSA-N 3-bromo-1h-indole Chemical compound C1=CC=C2C(Br)=CNC2=C1 YHIWBVHIGCRVLE-UHFFFAOYSA-N 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(II) acetate Substances [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 5
- 229940076286 cupric acetate Drugs 0.000 claims description 5
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910000104 sodium hydride Inorganic materials 0.000 claims description 5
- 239000012312 sodium hydride Substances 0.000 claims description 5
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 5
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 5
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 2
- 102000020897 Formins Human genes 0.000 claims 1
- 108091022623 Formins Proteins 0.000 claims 1
- FCEHBMOGCRZNNI-UHFFFAOYSA-N 1-benzothiophene Chemical compound C1=CC=C2SC=CC2=C1 FCEHBMOGCRZNNI-UHFFFAOYSA-N 0.000 abstract description 12
- 230000006750 UV protection Effects 0.000 abstract description 10
- 238000005336 cracking Methods 0.000 abstract description 7
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 abstract description 6
- 150000003242 quaternary ammonium salts Chemical class 0.000 abstract description 5
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 17
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910021595 Copper(I) iodide Inorganic materials 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 238000005524 ceramic coating Methods 0.000 description 2
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 1
- 125000000852 azido group Chemical group *N=[N+]=[N-] 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000001246 bromo group Chemical group Br* 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002540 isothiocyanates Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 125000002560 nitrile group Chemical group 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000006308 propyl amino group Chemical group 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
-
- 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
- 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
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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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/28—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen sulfur-containing groups
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a water-based inorganic nano ceramic flame-retardant coating and a preparation method thereof, and relates to the technical field of coatings. The invention firstly mixes terephthalonitrile and 3-bromine-1, 2-diaminobenzene to form imidazoline, and prepares the self-made antibacterial additive; then mixing the self-made antibacterial additive with tripropylamine azidobenzene isothiocyanate siloxane to form quaternary ammonium salt and benzothiophene to prepare antibacterial film-forming sol; then, the hydrated diphenyl iodic acid is used for modifying the carbon nano tube to prepare a modified carbon nano tube; and finally, mixing the antibacterial film-forming sol and the modified carbon nano tube to generate a 1, 4-bis (2-arylthio phenyl) -1, 3-diacetylene compound and 1,2, 4-triazole, and preparing the aqueous inorganic nano ceramic flame-retardant coating. The water-based inorganic nano ceramic flame-retardant coating prepared by the invention has good antibacterial property, ultraviolet resistance and cracking resistance.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a water-based inorganic nano ceramic flame-retardant coating and a preparation method thereof.
Background
The traditional coating generally uses a low-toxicity organic solvent as a dispersing agent, and a large amount of organic cleaning agent is consumed for cleaning a coating tool after the traditional coating is used, so that the traditional coating is not only harmful to the health of people, but also generates a plurality of substances harmful to the environment in the use process; the water-based paint takes water as a dispersing agent, is nontoxic, and can be directly cleaned by water, so that the water-based paint gradually receives attention from people nowadays when environmental protection and health are more and more important.
The aqueous inorganic nano ceramic coating is a large variety of aqueous coatings, generally takes polysiloxane as a film forming agent, has large shrinkage in the curing process and is easy to crack; and various harmful microorganisms are easy to grow and propagate on the surface of the polysiloxane material to cause surface pollution, and when the polysiloxane material is exposed to the sun, the coating is easy to age and fall off to influence the service life of the coating, so that the application range of the water-based inorganic nano ceramic coating is limited, and the water-based inorganic nano ceramic flame retardant coating with good antibacterial property, ultraviolet resistance and cracking resistance is designed and developed.
Disclosure of Invention
The invention aims to provide a water-based inorganic nano ceramic flame-retardant coating and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the water-based inorganic nano ceramic flame-retardant coating comprises an antibacterial film-forming sol and a modified carbon nano tube.
Furthermore, the antibacterial film-forming sol is prepared by mixing tripropylamine azidobenzene isothiocyanate siloxane and a self-made antibacterial additive.
Further, the homemade antibacterial additive is prepared by mixing terephthalonitrile and 3-bromine-1, 2-diaminobenzene.
Furthermore, the modified carbon nano tube is prepared from hydrated diphenyl iodic acid modified carbon nano tube.
Further, the use method of the inorganic nano ceramic flame-retardant coating comprises the following steps: spraying the water-based nano ceramic flame-retardant coating on a base material, controlling the spraying thickness to be 25-30 mu m, standing for 1-2 h, blowing hot air at 50-70 ℃ for curing for 5-6 min at 3-5 m/s, and then blowing hot air at 90-120 ℃ for curing for 18-22 min at 5-8 m/s.
Further, a preparation method of the water-based inorganic nano-ceramic flame-retardant coating, which mainly comprises the following preparation steps:
(1) The method comprises the following steps of (1) mixing a self-made antibacterial additive, tripropylamine azidobenzene isothiocyanate siloxane and xylene according to a mass ratio of 1:0.9: 6-1: 1.1:8, heating to 142-144 ℃, stirring for 8-10 h at 50-80 r/min, adding a mixture A with the mass of 0.1-0.2 time of that of the self-made antibacterial additive, wherein the mass ratio of sodium hydride to dimethyl sulfoxide in the mixture A is 1:2 to 1:3, continuously stirring for 25-37 min, heating to 80-100 ℃, adding a mixed solution A which is 3-5 times of the mass of the self-made antibacterial additive, continuously stirring for 5-7 min, adding iodoidene which is 0.1-0.3 times of the mass of the self-made antibacterial additive, continuously stirring for 4-6 h, adding ethanol which is 1.5-2 times of the mass of the self-made antibacterial additive and deionized water which is 4-6 times of the mass of the self-made antibacterial additive, stirring for 20-30 min at 3000-5000 r/min, standing for 1-2 h, adding sodium chloride which is 0.3-0.5 times of the mass of the self-made antibacterial additive, continuously stirring for 20-30 min, adding a hydrochloric acid solution to adjust the pH to be 6.9-7.1, continuously stirring for 2-3 h at 30-32 ℃, and then carrying out ultrasonic oscillation for 18-24 min at 45000-50000 Hz to prepare the antibacterial film-forming sol;
(2) Mixing carbon nano tubes and hydrated diphenyl iodic acid according to the mass ratio of 1:3 to 1:5, mixing, stirring for 4-6 min at the speed of 60-70 r/min, heating to 90-100 ℃, continuously stirring for 2-4 h, filtering, washing for 3-5 times with deionized water, filtering, drying for 4-6 h at the temperature of 59-61 ℃ and the vacuum degree of 0.01-0.02 MPa, adding diphenyl iodic acid hydrate with the mass of 1-1.5 times of that of the carbon nano tubes, continuously stirring for 20-30 min, adding anhydrous sodium sulfate with the mass of 0.1-0.3 time of the carbon nano tubes, heating to 120-125 ℃, and stirring for 2-5 h at the speed of 500-600 r/min to prepare the modified carbon nano tubes;
(3) At the temperature of 128-132 ℃, mixing the antibacterial film-forming sol, the modified carbon nano tube and trifluoromethanesulfonic acid in a mass ratio of 1:0.5:3 to 1:1:4, stirring for 3-5 min at 80-100 r/min, adding the iodoidene with the mass of 0.1-0.2 time of that of the antibacterial film forming sol, continuing to stir for 30-40 min, cooling to room temperature, adding the ethanol solution with the mass fraction of 80-90% and the mass of 7-8 times of that of the antibacterial film forming sol, continuing to stir for 7-9 min, then dripping the mixed solution B with the mass of 0.2-0.4 time of that of the antibacterial film forming sol at 15-20 ml/min, stirring for 2-3 h at 45-75 r/min, adding the triethylamine with the mass of 0.1-0.2 time of that of the antibacterial film forming sol and the diethyliodobenzene with the mass of 0.05-0.1 time of that of the antibacterial film forming sol, continuing to stir for 30-50 min, and obtaining the aqueous inorganic nano ceramic flame-retardant coating.
Further, the preparation method of the self-made antibacterial additive in the step (1) comprises the following steps: terephthalonitrile, 3-bromo-1, 2-diaminobenzene and indole-3-cupric acetate are mixed according to a mass ratio of 1:0.7:0.1-1: 0.9:0.2, stirring at 150-200 r/min for 8-10 min at 10-20W/m 2 The microwave irradiation is carried out for 1 to 3 hours under the condition of (1) to prepare the self-made antibacterial additive.
Further, the preparation method of the tripropylamine azide isothiocyanate siloxane in the step (1) comprises the following steps: 3-chloropropylamine and 4-azidobenzene isothiocyanate are mixed according to a mass ratio of 1:0.9 to 1:1.1 mixing, stirring for 3-5 min at 20-25 r/min, adding anhydrous aluminum trichloride with the mass of 0.1-0.2 time of that of 3-chloropropylamine, heating to 80-90 ℃, continuing to stir for 10-15 min, adding 3-glycidoxypropyltrimethoxysilane with the mass of 1.2-1.4 times of that of 3-chloropropylamine, continuing to stir for 0.5-2 h, heating to 140-160 ℃, and stirring for 2-4 m 3 Introducing hydrogen with the mass 5-10 times of that of the 3-chloropropylamine into the reactor per minute, and continuously stirring the mixture for 34-38 hours to prepare the tripropylamine azide isothiocyanate siloxane.
Further, the mixed solution A in the step (1) is prepared by mixing a palladium chloride solution with the mass fraction of 8-12% and a tetrabutyl ammonium bromide solution with the mass fraction of 15-25% according to the mass ratio of 1:0.5 to 1:0.6 and mixing.
Further, the mixed solution B in the step (3) is prepared by mixing sodium ethoxide and 60-80% ethanol solution according to a mass ratio of 1:0.1 to 1:0.2 and mixing.
Compared with the prior art, the invention has the following beneficial effects:
a water-based inorganic nano ceramic flame-retardant coating comprises an antibacterial film-forming sol and a modified carbon nano tube; the antibacterial film-forming sol is prepared by mixing tripropylamine azidobenzene isothiocyanate siloxane and a self-made antibacterial additive; the self-made antibacterial additive is prepared by mixing terephthalonitrile and 3-bromine-1, 2-diaminobenzene; the modified carbon nano tube is prepared from a hydrated diphenyl iodic acid modified carbon nano tube.
Firstly, reacting a nitrile group on terephthalonitrile with an amino group on 3-bromo-1, 2-diaminobenzene to generate imidazoline, so that the self-made antibacterial additive has an antibacterial effect; bromine atoms on the self-made antibacterial additive react with propylamine groups on the tripropylamine azide isothiocyanate siloxane to generate quaternary ammonium salt, and the self-made antibacterial additive is stably grafted on the tripropylamine azide isothiocyanate siloxane, so that the antibacterial property of the antibacterial film-forming sol is enhanced; meanwhile, benzonitrile on the self-made antibacterial additive reacts with isothiocyanate on the tripropylamine azidobenzene isothiocyanate siloxane to generate benzothiophene, so that the antibacterial property of the antibacterial film-forming sol is enhanced.
Secondly, under the action of hydrated diphenyl iodic acid, carboxyl on the hydrated diphenyl iodic acid reacts with hydroxyl on the surface of the carbon nano tube for grafting while forming a large number of hydroxyl hydrophilic groups on the surface of the carbon nano tube, and the modified carbon nano tube is uniformly dispersed in the antibacterial film-forming sol through the reaction of diphenyl iodic acid and benzothiophene of the antibacterial film-forming sol to generate a 1, 4-bis (2-arylthio phenyl) -1, 3-diacetylene compound, wherein during illumination, the 1, 4-bis (2-arylthio phenyl) -1, 3-diacetylene compound quickly absorbs ultraviolet rays for electron transfer, so that energy is released, and the ultraviolet resistance of the water-based inorganic nano ceramic flame-retardant coating is enhanced; the silicon-oxygen bond in the inorganic nano ceramic emulsion is condensed and copolymerized, the azido group of the inorganic nano ceramic emulsion reacts with the 1, 4-bis (2-arylthio phenyl) -1, 3-diacetylene compound and is crosslinked to generate the 1,2, 4-triazole, the modified carbon nano tubes are stably dispersed in the inorganic nano ceramic emulsion, the crosslinking density of the water-based inorganic nano ceramic flame retardant coating is enhanced, and the cracking resistance of the water-based inorganic nano ceramic flame retardant coating is enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to illustrate the method of the present invention, and the method for testing each index of the aqueous inorganic nano-ceramic flame retardant coating prepared in the following examples is as follows:
and (3) spraying the water-based inorganic nano ceramic flame-retardant coating prepared in the same quality example and the comparative example on the surface of a base material with the same size and material quality, controlling the spraying thickness to be 27.5 mu m, standing for 1.5h, blowing hot air with the temperature of 60 ℃ at 4m/s for curing for 5.5min, and then blowing hot air with the temperature of 105 ℃ at 6.5m/s for continuously curing for 20min to prepare the water-based inorganic nano ceramic flame-retardant coating.
And (3) antibacterial property: and testing the antibacterial rate of the treated water-based inorganic nano ceramic flame-retardant coating according to the standard GB/T21866.
Ultraviolet resistance: and (3) placing the water-based inorganic nano ceramic flame-retardant coating under the conditions of 135 ℃ and 270W ultraviolet irradiation for an artificial accelerated aging experiment, and testing the aging time.
Cracking resistance: the initial drying crack resistance of the aqueous inorganic nano ceramic flame-retardant coating is tested according to the standard JG/T298.
Example 1
(1) Terephthalonitrile, 3-bromo-1, 2-diaminobenzene and indole-3-cupric acetate are mixed according to a mass ratio of 1:0.7:0.1 mixing, stirring at 150r/min for 8min, at 10W/m 2 The self-made antibacterial additive is prepared after microwave irradiation for 1 hour; 3-chloropropylamine and 4-azidobenzene isothiocyanate are mixed according to a mass ratio of 1:0.9, stirring at 20r/min for 3min, adding anhydrous aluminum trichloride accounting for 0.1 time of the mass of 3-chloropropylamine, heating to 80 ℃, continuing to stir for 10min, adding 3-glycidoxypropyltrimethoxysilane accounting for 1.2 times of the mass of 3-chloropropylamine, continuing to stir for 0.5h, heating to 140 ℃, and stirring at 2m 3 Introducing hydrogen with the mass 5 times that of 3-chloropropylamine into the reactor per minute, and continuously stirring the mixture for 34 hours to prepare tripropylamine azide isothiocyanate siloxane; the method comprises the following steps of (1) mixing a self-made antibacterial additive, tripropylamine azidobenzene isothiocyanate siloxane and xylene according to a mass ratio of 1:0.9:6, mixing, heating to 142 ℃, stirring for 8h at 50r/min, adding a mixture A with the mass of 0.1 time of that of the self-made antibacterial additive, wherein the mass ratio of sodium hydride to dimethyl sulfoxide in the mixture A is 1:2, continuously stirring for 25min, heating to 80 ℃, adding a mixed solution A which is 3 times of the mass of the self-made antibacterial additive, wherein the mixed solution A is prepared by mixing a palladium chloride solution with the mass fraction of 8% and a tetrabutyl ammonium bromide solution with the mass fraction of 15% according to the mass ratio of 1:0.5 mixing to obtain; stirring for 5min, adding iodized acetone 0.1 times the weight of the antibacterial additive, stirring for 4 hr, adding ethanol 1.5 times the weight of the antibacterial additive, and stirringStirring deionized water 4 times the mass of the self-made antibacterial additive for 20min at 3000r/min, standing for 1h, adding sodium chloride 0.3 times the mass of the self-made antibacterial additive, continuously stirring for 20min, adding a hydrochloric acid solution to adjust the pH to 6.9, continuously stirring for 2h at 30 ℃, and ultrasonically shaking for 18min at 45000Hz to prepare antibacterial film-forming sol;
(2) Mixing carbon nano tubes and hydrated diphenyl iodic acid according to the mass ratio of 1:3, mixing, stirring for 4min at the speed of 60r/min, heating to 90 ℃, continuing to stir for 2h, filtering, washing for 3 times by using deionized water, filtering, drying for 4h at the temperature of 59 ℃ and the vacuum degree of 0.01MPa, adding diphenyl iodic acid hydrate, the mass of which is 1 time that of the carbon nano tube, continuing to stir for 20min, adding anhydrous sodium sulfate, the mass of which is 0.1 time that of the carbon nano tube, heating to 120 ℃, and stirring for 2h at the speed of 500r/min to prepare the modified carbon nano tube;
(3) At the temperature of 128 ℃, mixing the antibacterial film-forming sol, the modified carbon nano tube and trifluoromethanesulfonic acid in a mass ratio of 1:0.5:3, stirring for 3min at the speed of 80r/min, adding the iodoidene which is 0.1 time of the mass of the antibacterial film forming sol, continuing to stir for 30min, cooling to room temperature, adding an ethanol solution which is 80 percent of the mass of the antibacterial film forming sol and is 7 times of the mass of the antibacterial film forming sol, continuing to stir for 7min, and dropping a mixed solution B which is 0.2 time of the mass of the antibacterial film forming sol at the speed of 15ml/min, wherein the mixed solution B is prepared by mixing sodium ethoxide and a 60 percent ethanol solution according to the mass ratio of 1:0.1, stirring for 2 hours at a speed of 45r/min, adding triethylamine with the mass being 0.1 time of that of the antibacterial film-forming sol and diethyliodobenzene with the mass being 0.05 time of that of the antibacterial film-forming sol, and continuously stirring for 30 minutes to obtain the aqueous inorganic nano ceramic flame-retardant coating.
Example 2
(1) Terephthalonitrile, 3-bromo-1, 2-diaminobenzene and indole-3-cupric acetate are mixed according to a mass ratio of 1:0.8:0.15 mixing, stirring at 175r/min for 9min at 15W/m 2 Performing microwave irradiation for 2 hours under the condition of (1) to prepare a self-made antibacterial additive; 3-chloropropylamine and 4-azidobenzene isothiocyanate are mixed according to a mass ratio of 1:1, stirring for 4min at 22.5/min, adding anhydrous aluminum trichloride accounting for 0.15 time of the mass of 3-chloropropylamine, heating to 85 ℃, continuing to stir for 12.5min, adding 3-glycidoxypropyltrimethoxysilane accounting for 1.3 times of the mass of 3-chloropropylamine, continuing to stir for 1.25h, heating to 150 ℃, and stirring for 3m 3 Permin the mass of the 3-chloropropylamine is 7.5 times that of the 3-chloropropylamineContinuously stirring for 36 hours to obtain tripropylamine azide isothiocyanate siloxane; the method comprises the following steps of (1) mixing a self-made antibacterial additive, tripropylamine azidobenzene isothiocyanate siloxane and xylene according to a mass ratio of 1:1:7, heating to 143 ℃, stirring for 9 hours at a speed of 65r/min, adding a mixture A with the mass 0.15 time that of the self-made antibacterial additive, wherein the mass ratio of sodium hydride to dimethyl sulfoxide in the mixture A is 1:2.5, continuously stirring for 31min, heating to 90 ℃, adding a mixed solution A which is 4 times of the mass of the self-made antibacterial additive, wherein the mixed solution A is prepared by mixing a palladium chloride solution with the mass fraction of 10% and a tetrabutyl ammonium bromide solution with the mass fraction of 20% according to the mass ratio of 1:0.55, continuously stirring for 6min, adding cuprous iodide with the mass 0.2 time of that of the self-made antibacterial additive, continuously stirring for 5h, adding ethanol with the mass 1.75 time of that of the self-made antibacterial additive and deionized water with the mass 5 time of that of the self-made antibacterial additive, stirring for 25min at 4000r/min, standing for 1.5h, adding sodium chloride with the mass 0.4 time of that of the self-made antibacterial additive, continuously stirring for 25min, adding a hydrochloric acid solution to adjust the pH to 7, continuously stirring for 2.5h at 31 ℃, and ultrasonically shaking for 21min at 47500Hz to prepare the antibacterial film-forming sol;
(2) Mixing carbon nano tubes and hydrated diphenyl iodic acid according to the mass ratio of 1:4, mixing, stirring for 5min at a speed of 65r/min, heating to 95 ℃, continuing to stir for 3h, filtering, washing for 4 times by using deionized water, filtering, drying for 5h at a temperature of 60 ℃ and a vacuum degree of 0.015MPa, adding diphenyl iodic acid hydrate, the mass of which is 1.25 times that of the carbon nano tube, continuing to stir for 25min, adding anhydrous sodium sulfate, the mass of which is 0.2 times that of the carbon nano tube, heating to 122.5 ℃, and stirring for 3.5h at a speed of 550r/min to obtain a modified carbon nano tube;
(3) At 130 ℃, mixing the antibacterial film-forming sol, the modified carbon nano tube and trifluoromethanesulfonic acid in a mass ratio of 1:0.75:3.5, stirring for 4min at 90r/min, adding the iodoidene which is 0.15 time of the mass of the antibacterial film forming sol, continuing to stir for 35min, cooling to room temperature, adding an ethanol solution which is 7.5 times of the mass of the antibacterial film forming sol and has a mass fraction of 85%, continuing to stir for 8min, and then dripping a mixed solution B which is 0.3 time of the mass of the antibacterial film forming sol into the mixed solution B at a rate of 17.5ml/min, wherein the mixed solution B is prepared by mixing sodium ethoxide and a 70% ethanol solution according to a mass ratio of 1:0.15, stirring for 2.5h at 60r/min, adding triethylamine of 0.15 time of the mass of the antibacterial film-forming sol and diethyliodobenzene of 0.075 time of the mass of the antibacterial film-forming sol, and continuously stirring for 40min to obtain the aqueous inorganic nano ceramic flame-retardant coating.
Example 3
(1) Terephthalonitrile, 3-bromo-1, 2-diaminobenzene and indole-3-cupric acetate are mixed according to a mass ratio of 1:0.9:0.2 mixing, stirring at 200r/min for 10min, at 20W/m 2 Performing microwave irradiation for 3 hours under the condition of (1) to prepare a self-made antibacterial additive; 3-chloropropylamine and 4-azidobenzene isothiocyanate are mixed according to a mass ratio of 1:1.1 mixing, stirring for 5min at 25r/min, adding anhydrous aluminum trichloride of which the mass is 0.2 time that of 3-chloropropylamine, heating to 90 ℃, continuing to stir for 15min, adding 3-glycidoxypropyltrimethoxysilane of which the mass is 1.4 times that of 3-chloropropylamine, continuing to stir for 2h, heating to 160 ℃, and stirring for 4m 3 Introducing hydrogen with the mass being 10 times that of 3-chloropropylamine into the reactor per minute, and continuously stirring for 38 hours to prepare tripropylamine azidobenzene isothiocyanate siloxane; the method comprises the following steps of (1) mixing a self-made antibacterial additive, tripropylamine azide isothiocyanate siloxane and xylene according to a mass ratio of 1:1.1:8, mixing, heating to 144 ℃, stirring for 10h at 80r/min, adding a mixture A with the mass 0.2 time that of the self-made antibacterial additive, wherein the mass ratio of sodium hydride to dimethyl sulfoxide in the mixture A is 1: and 3, continuously stirring for 37min, heating to 100 ℃, and adding a mixed solution A which is 5 times of the mass of the self-made antibacterial additive, wherein the mixed solution A is prepared by mixing a palladium chloride solution with the mass fraction of 12% and a tetrabutyl ammonium bromide solution with the mass fraction of 25% according to the mass ratio of 1:0.6, continuously stirring for 7min, adding cuprous iodide with the mass 0.3 time of that of the self-made antibacterial additive, continuously stirring for 6h, adding ethanol with the mass 2 times of that of the self-made antibacterial additive and deionized water with the mass 6 times of that of the self-made antibacterial additive, stirring for 30min at 5000r/min, standing for 2h, adding sodium chloride with the mass 0.5 time of that of the self-made antibacterial additive, continuously stirring for 30min, adding a hydrochloric acid solution to adjust the pH to 7.1, continuously stirring for 3h at 32 ℃, and then ultrasonically shaking for 24min at 50000Hz to prepare the antibacterial film-forming sol;
(2) Mixing carbon nano tubes and hydrated diphenyl iodic acid according to the mass ratio of 1:5, mixing, stirring for 6min at a speed of 70r/min, heating to 100 ℃, continuing stirring for 4h, filtering, washing with deionized water for 5 times, filtering, drying for 6h at 61 ℃ and a vacuum degree of 0.02MPa, adding diphenyl iodic acid hydrate with a mass of 1.5 times that of the carbon nano tube, continuing stirring for 30min, adding anhydrous sodium sulfate with a mass of 0.3 time that of the carbon nano tube, heating to 125 ℃, and stirring for 5h at a speed of 600r/min to obtain a modified carbon nano tube;
(3) At the temperature of 132 ℃, mixing the antibacterial film-forming sol, the modified carbon nano tube and trifluoromethanesulfonic acid in a mass ratio of 1:1:4, mixing, stirring for 5min at the speed of 100r/min, adding the iodoidene which is 0.2 time of the mass of the antibacterial film forming sol, stirring for 40min at the speed of 100r/min, cooling to room temperature, adding an ethanol solution which is 8 times of the mass of the antibacterial film forming sol and has the mass fraction of 90%, continuing stirring for 9min, and then dropping a mixed solution B which is 0.4 time of the mass of the antibacterial film forming sol at the speed of 20ml/min, wherein the mixed solution B is prepared by mixing sodium ethoxide and an 80% ethanol solution according to the mass ratio of 1:0.2, stirring for 3 hours at 75r/min, adding triethylamine with the mass being 0.2 time of that of the antibacterial film forming sol and diethyliodobenzene with the mass being 0.1 time of that of the antibacterial film forming sol, and continuously stirring for 50 minutes to prepare the aqueous inorganic nano ceramic flame retardant coating.
Comparative example 1
Comparative example 1 is different from example 2 in the step (1) of preparing a home-made antibiotic additive using only 3-bromo-1, 2-diaminobenzene, and the remaining preparation steps are the same as example 2.
Comparative example 2
Comparative example 2 is different from example 2 in the step (1) of preparing a homemade antibiotic additive using terephthalonitrile only, and the remaining preparation steps are the same as example 2.
Comparative example 3
Comparative example 3 is different from example 2 in the step (1), the home-made antibacterial additive is not prepared, the antibacterial film-forming sol is prepared only by using trispropylamino azidobenzene isothiocyanate siloxane, and the rest of the preparation steps are the same as example 2.
Comparative example 4
Comparative example 4 is different from example 2 in the step (1) of preparing an antibacterial film-forming sol using trimethoxysilane and a home-made antibacterial additive, and the rest of the preparation steps are the same as example 2.
Comparative example 5
Comparative example 5 is different from example 2 in the step (3), and the aqueous inorganic nano ceramic flame retardant coating is prepared using only the antibacterial film forming sol, and the rest of the procedure is the same as example 2.
Effects of the invention
Table 1 below shows the results of performance analysis of antibacterial property, ultraviolet resistance and crack resistance of the aqueous inorganic nano ceramic flame retardant coating prepared by using examples 1 to 3 of the present invention and comparative examples 1 to 5.
TABLE 1
From table 1, it can be found that the antibacterial property, the ultraviolet resistance and the cracking resistance of the aqueous inorganic nano ceramic flame retardant coatings prepared in the embodiments 1,2 and 3 are strong; from the comparison of experimental data of examples 1,2 and 3 and comparative example 1, it can be found that imidazoline can be formed by using terephthalonitrile to prepare a self-made antibacterial additive, benzothiophene can be formed by subsequently preparing an antibacterial film-forming sol, 1, 4-bis (2-arylthiophenyl) -1, 3-diacetylene compound and 1,2, 4-triazole can be formed when preparing the aqueous inorganic nano ceramic flame-retardant coating, and the prepared aqueous inorganic nano ceramic flame-retardant coating has strong antibacterial property, ultraviolet resistance and crack resistance; the experimental data comparison of the examples 1,2 and 3 and the comparative example 2 shows that imidazoline can be formed by using 3-bromo-1, 2-diaminobenzene to prepare the self-made antibacterial additive, quaternary ammonium salt can be formed by subsequently preparing the antibacterial film-forming sol, and the prepared water-based inorganic nano ceramic flame-retardant coating has stronger antibacterial property; the comparison of experimental data of examples 1,2 and 3 and comparative example 3 shows that quaternary ammonium salt and benzothiophene can be formed by using the self-made antibacterial additive to prepare the antibacterial film-forming sol, 1, 4-bis (2-arylthiophenyl) -1, 3-diacetylene compound and 1,2, 4-triazole can be formed by subsequently preparing the aqueous inorganic nano ceramic flame-retardant coating, and the prepared aqueous inorganic nano ceramic flame-retardant coating has stronger antibacterial property, ultraviolet resistance and cracking resistance; from the comparison of experimental data of examples 1,2 and 3 and comparative example 4, it can be found that quaternary ammonium salt and benzothiophene can be formed by using trispropylamino azidobenzene isothiocyanate siloxane to prepare an antibacterial film-forming sol, and 1, 4-bis (2-arylthiophenyl) -1, 3-diacetylene compound and 1,2, 4-triazole can be formed by subsequently preparing the aqueous inorganic nano ceramic flame-retardant coating, so that the prepared aqueous inorganic nano ceramic flame-retardant coating has stronger antibacterial property, ultraviolet resistance and cracking resistance; from the comparison of experimental data of examples 1,2 and 3 and comparative example 5, it can be found that 1, 4-bis (2-arylthiophenyl) -1, 3-diacetylene compound and 1,2, 4-triazole can be formed by using the modified carbon nanotubes to prepare the waterborne inorganic nano ceramic flame retardant coating, and the prepared waterborne inorganic nano ceramic flame retardant coating has stronger ultraviolet resistance and crack resistance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The water-based inorganic nano-ceramic flame-retardant coating is characterized by comprising an antibacterial film-forming sol and a modified carbon nano tube.
2. The aqueous inorganic nano-ceramic flame-retardant coating as claimed in claim 1, wherein the antibacterial film-forming sol is prepared by mixing tripropylamine azide isothiocyanate siloxane with a self-made antibacterial additive.
3. The aqueous inorganic nano-ceramic flame-retardant coating of claim 2, wherein the homemade antibacterial additive is prepared by mixing terephthalonitrile and 3-bromo-1, 2-diaminobenzene.
4. The water-based inorganic nano-ceramic flame-retardant coating of claim 1, wherein the modified carbon nanotubes are prepared from hydrated diphenyl iodic acid modified carbon nanotubes.
5. The water-based inorganic nano-ceramic flame-retardant coating as claimed in claim 1, wherein the inorganic nano-ceramic flame-retardant coating is prepared by the following steps: spraying the water-based nano ceramic flame-retardant coating on a base material, controlling the spraying thickness to be 25-30 mu m, standing for 1-2 h, blowing hot air at 50-70 ℃ for curing for 5-6 min at 3-5 m/s, and then blowing hot air at 90-120 ℃ for curing for 18-22 min at 5-8 m/s.
6. A preparation method of a water-based inorganic nano ceramic flame-retardant coating is characterized by mainly comprising the following preparation steps:
(1) The method comprises the following steps of (1) mixing a self-made antibacterial additive, tripropylamine azidobenzene isothiocyanate siloxane and xylene according to a mass ratio of 1:0.9:6 to 1:1.1:8, heating to 142-144 ℃, stirring for 8-10 h at 50-80 r/min, adding a mixture A with the mass of 0.1-0.2 time of that of the self-made antibacterial additive, wherein the mass ratio of sodium hydride to dimethyl sulfoxide in the mixture A is 1:2 to 1:3, continuously stirring for 25-37 min, heating to 80-100 ℃, adding a mixed solution A which is 3-5 times of the mass of the self-made antibacterial additive, continuously stirring for 5-7 min, adding iodoidene which is 0.1-0.3 times of the mass of the self-made antibacterial additive, continuously stirring for 4-6 h, adding ethanol which is 1.5-2 times of the mass of the self-made antibacterial additive and deionized water which is 4-6 times of the mass of the self-made antibacterial additive, stirring for 20-30 min at 3000-5000 r/min, standing for 1-2 h, adding sodium chloride which is 0.3-0.5 times of the mass of the self-made antibacterial additive, continuously stirring for 20-30 min, adding a hydrochloric acid solution to adjust the pH to be 6.9-7.1, continuously stirring for 2-3 h at 30-32 ℃, and then carrying out ultrasonic oscillation for 18-24 min at 45000-50000 Hz to prepare the antibacterial film-forming sol;
(2) Mixing carbon nano tubes and hydrated diphenyl iodic acid according to the mass ratio of 1:3 to 1:5, mixing, stirring for 4-6 min at the speed of 60-70 r/min, heating to 90-100 ℃, continuously stirring for 2-4 h, filtering, washing for 3-5 times with deionized water, filtering, drying for 4-6 h at the temperature of 59-61 ℃ and the vacuum degree of 0.01-0.02 MPa, adding diphenyl iodic acid hydrate with the mass of 1-1.5 times of that of the carbon nano tubes, continuously stirring for 20-30 min, adding anhydrous sodium sulfate with the mass of 0.1-0.3 time of the carbon nano tubes, heating to 120-125 ℃, and stirring for 2-5 h at the speed of 500-600 r/min to prepare the modified carbon nano tubes;
(3) At the temperature of 128-132 ℃, mixing the antibacterial film-forming sol, the modified carbon nano tube and trifluoromethanesulfonic acid in a mass ratio of 1:0.5:3 to 1:1:4, stirring for 3-5 min at the speed of 80-100 r/min, adding the iodoidene of which the mass is 0.1-0.2 time of that of the antibacterial film forming sol, continuing to stir for 30-40 min, cooling to room temperature, adding the ethanol solution of which the mass fraction is 80-90% and the mass is 7-8 times of that of the antibacterial film forming sol, continuing to stir for 7-9 min, then dripping the mixed solution B of which the mass is 0.2-0.4 time of that of the antibacterial film forming sol into the mixed solution at the speed of 15-20 ml/min, stirring for 2-3 h at the speed of 45-75 r/min, adding the triethylamine of which the mass is 0.1-0.2 time of that of the antibacterial film forming sol and the diethyliodobenzene of which the mass is 0.05-0.1 time of that of the antibacterial film forming sol into the mixed solution B, continuing to stir for 30-50 min, and obtaining the aqueous inorganic nano ceramic flame retardant coating.
7. The preparation method of the water-based inorganic nano-ceramic flame-retardant coating according to claim 6, wherein the preparation method of the self-made antibacterial additive in the step (1) comprises the following steps: terephthalonitrile, 3-bromo-1, 2-diaminobenzene and indole-3-cupric acetate are mixed according to a mass ratio of 1:0.7:0.1 to 1:0.9:0.2, stirring at 150-200 r/min for 8-10 min at 10-20W/m 2 The microwave irradiation is carried out for 1 to 3 hours under the condition of (1) to prepare the self-made antibacterial additive.
8. The preparation method of the water-based inorganic nano-ceramic flame retardant coating according to claim 6, wherein the preparation method of the tripropylamine azide isothiocyanate siloxane in the step (1) comprises the following steps: 3-chloropropylamine and 4-azidobenzene isothiocyanate are mixed according to a mass ratio of 1:0.9 to 1:1.1, stirring for 3-5 min at 20-25 r/min, adding anhydrous aluminum trichloride accounting for 0.1-0.2 time of the mass of 3-chloropropylamine, heating to 80-90 ℃, continuing to stir for 10-15 min, adding 3-glycidoxypropyltrimethoxysilane accounting for 1.2-1.4 times of the mass of 3-chloropropylamine, continuing to stir for 0.5-2 h, heating to 140-160 ℃, and stirring for 2-4 m 3 Introducing hydrogen with the mass 5-10 times of that of 3-chloropropylamine for min, and thenStirring for 34-38 h to obtain the tripropylamine azidobenzene isothiocyanate siloxane.
9. The preparation method of the water-based inorganic nano-ceramic flame-retardant coating according to claim 6, wherein the mixed solution A in the step (1) is prepared by mixing a palladium chloride solution with a mass fraction of 8-12% and a tetrabutyl ammonium bromide solution with a mass fraction of 15-25% in a mass ratio of 1:0.5 to 1:0.6 and mixing.
10. The preparation method of the water-based inorganic nano-ceramic flame-retardant coating according to claim 6, wherein the mixed solution B obtained in the step (3) is prepared by mixing sodium ethoxide and 60-80% ethanol solution according to a mass ratio of 1:0.1 to 1:0.2 and mixing.
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