CN116987427A - Water-based acrylic resin coating for building and preparation method thereof - Google Patents
Water-based acrylic resin coating for building and preparation method thereof Download PDFInfo
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- CN116987427A CN116987427A CN202311106753.6A CN202311106753A CN116987427A CN 116987427 A CN116987427 A CN 116987427A CN 202311106753 A CN202311106753 A CN 202311106753A CN 116987427 A CN116987427 A CN 116987427A
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- acrylic resin
- silicon dioxide
- water
- resin coating
- nano silicon
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- 238000000576 coating method Methods 0.000 title claims abstract description 50
- 239000011248 coating agent Substances 0.000 title claims abstract description 47
- 239000004925 Acrylic resin Substances 0.000 title claims abstract description 43
- 229920000178 Acrylic resin Polymers 0.000 title claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 84
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 39
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 38
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 8
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 30
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 17
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- 239000003973 paint Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002390 rotary evaporation Methods 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- 239000003480 eluent Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 6
- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 238000004440 column chromatography Methods 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- DEUJSGDXBNTQMY-UHFFFAOYSA-N 1,2,2-trifluoroethanol Chemical compound OC(F)C(F)F DEUJSGDXBNTQMY-UHFFFAOYSA-N 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims 6
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000007789 gas Substances 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 238000009210 therapy by ultrasound Methods 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 7
- 239000003513 alkali Substances 0.000 abstract description 7
- 239000003995 emulsifying agent Substances 0.000 abstract description 5
- 239000003999 initiator Substances 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 230000002045 lasting effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- 239000003063 flame retardant Substances 0.000 description 9
- 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 description 8
- 239000000126 substance Substances 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 244000137852 Petrea volubilis Species 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- -1 acrylic ester Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229920003180 amino resin Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Classifications
-
- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/10—Homopolymers or copolymers of methacrylic acid esters
- C09D133/12—Homopolymers or copolymers of methyl methacrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- 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
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a water-based acrylic resin coating for buildings and a preparation method thereof, belonging to the technical field of building coatings. The modified nano silicon dioxide is prepared from butyl acrylate, methyl methacrylate, an emulsifier, water, a water-soluble initiator and modified nano silicon dioxide in a mass ratio of 25:25:2:80:1:5-15. The prepared coating has low raw material cost, reduces environmental pollution and is acid and alkali resistant; in addition, the modified nano silicon dioxide prepared by grafting the nano silicon dioxide with the organic molecular chain can improve the compatibility of the nano silicon dioxide and the aqueous acrylic resin coating, and the nano silicon dioxide can effectively prevent migration and exudation of the organic molecules and ensure the durability of the performance; the obtained water-based acrylic resin coating for the building has lasting and remarkable waterproof property, flexibility and hardness, has certain flame retardance and acid and alkali resistance, and is an excellent environment-friendly coating for the building.
Description
Technical Field
The invention belongs to the technical field of building coatings, and particularly relates to an aqueous acrylic resin coating for a building and a preparation method thereof.
Background
The acrylic resin coating is a thermoplastic or thermosetting resin coating prepared from (methyl) acrylic ester and styrene serving as main bodies and acrylic resin obtained by copolymerization of the (methyl) acrylic ester and styrene and other acrylic esters. Compared with the traditional solvent-based paint, the water-based paint has the advantages of low price, safe use, resource and energy conservation, environmental pollution reduction, pollution and the like, and the varnish prepared from the water-soluble acrylic resin has the characteristics of no toxicity, no smell, acid and alkali resistance, high glossiness, good adhesive force, no fading, chemical resistance and the like, is a green environment-friendly product of a low-Volatility Organic Compound (VOC), and has wide application in the field of building paint. However, it has some drawbacks, such as poor alcohol resistance, heat resistance, abrasion resistance, and insufficient hardness of the one-component acrylic resin coating.
The common solutions are: nanomaterial modified aqueous acrylic resin, organic fluorine/silicon modified aqueous acrylic resin, polyurethane and epoxy modified aqueous acrylic resin. The Chinese patent application with the related art publication number of CN110819193A discloses a self-flame-retardant acrylic resin water-based anticorrosive paint, which has good fireproof flame-retardant effect but poor waterproof performance by introducing phosphorus element. The Chinese patent application with the related art publication number of CN108467648A discloses a coating prepared from acrylic resin and amino resin, which has the advantages of good stability and waterproof capability, but has poor wear resistance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a water-based acrylic resin coating for building and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
the preparation method of the water-based acrylic resin coating for the building comprises the following steps:
adding butyl acrylate, methyl methacrylate and sodium dodecyl sulfate (emulsifier) into water, emulsifying to obtain emulsion, adding azo-diisopropylimidazoline (water-soluble initiator) to initiate polymerization, adding modified nano silicon dioxide after the reaction is completed, stirring with strong force, and dispersing with ultrasonic for 30min to obtain the water-based acrylic resin coating for building.
Further, the mass ratio of the butyl acrylate to the methyl methacrylate to the sodium dodecyl sulfate to the water to the azodiisopropylimidazoline to the modified nano silicon dioxide is 25:25:2:80:1:5-15.
Further, the modified nano-silica is prepared by the steps of:
s1, adding phosphorus oxychloride and 2, 2-trifluoroethanol into a three-neck flask provided with a stirring reflux device, mixing, adding aluminum trichloride (catalyst), stirring uniformly, slowly heating to 80 ℃, carrying out reflux reaction for 4 hours until no obvious HCl escapes, stopping the reaction, filtering to remove the aluminum trichloride, and then carrying out reduced pressure distillation to remove unreacted phosphorus oxychloride to obtain an intermediate 1; the dosage ratio of phosphorus oxychloride, 2-trifluoroethanol and aluminum trichloride is 17.2g:10.1g:0.3g;
under the catalysis of aluminum trichloride, phosphorus oxychloride and 2, 2-trifluoroethanol are subjected to esterification reaction, and only one-Cl on the phosphorus oxychloride participates in the reaction by controlling the molar ratio of the phosphorus oxychloride to the 2, 2-trifluoroethanol to be close to 1:1 and slightly excessive, so that an intermediate 1 is obtained; the specific reaction process is as follows:
s2, adding the intermediate 1 into a three-neck flask provided with a stirring reflux device, mixing hydroxyethyl acrylate with chloroform, adding aluminum trichloride (catalyst), stirring uniformly, slowly heating to 65 ℃, carrying out reflux reaction for 2 hours until no obvious HCl escapes, stopping the reaction, removing part of solvent by rotary evaporation, purifying by column chromatography (eluent adopts a mixed solvent of diethyl ether and ethyl acetate, the volume ratio of the diethyl ether to the ethyl acetate is 1:1), and removing eluent by rotary evaporation to obtain an intermediate 2; the dosage ratio of the intermediate 1 to the hydroxyethyl acrylate to the chloroform to the aluminum trichloride is 23.6g to 11.6g to 100mL to 0.4g;
under the catalysis of aluminum trichloride, the intermediate 1 and hydroxyethyl acrylate are subjected to esterification reaction, and only one-Cl on the intermediate 1 participates in the reaction by controlling the molar ratio of the intermediate 1 to the hydroxyethyl acrylate to be close to 1:1 and slightly excessive intermediate 1, so that an intermediate 2 is obtained; the specific reaction process is as follows:
s3, mixing the nano silicon dioxide with toluene, adding the mixture into a magnetic stirring device, adding magnetite, starting stirring, dispersing for 30min to uniformly disperse the silicon dioxide in toluene solution, vacuumizing the device, and introducing N 2 Adding gamma-aminopropyl triethoxysilane (silane coupling agent KH-550), heating in oil bath, setting 50deg.C, opening condensed water, setting 80deg.C, heating to moderate reaction, reacting at 80deg.C for 4 hr, filtering, washing with toluene, and drying in vacuum drying oven for 2 hr to obtain intermediate 3; the dosage ratio of the nano silicon dioxide, toluene and gamma-aminopropyl triethoxysilane is 10.0g to 100mL to 6.50g;
the nano silicon dioxide has a plurality of-OH on the surface, and can be introduced into-NH by reacting with KH-550 2 Reactive groups to give intermediate 3; the specific reaction process is as follows:
s4, under the protection of room temperature and nitrogen, the intermediate 3 is ultrasonically treated in ethyl acetate for 30min, uniformly dispersed, the intermediate 2 is added, uniformly stirred, slowly heated to 80 ℃, magnetically stirred (the rotating speed is 1000 r/min), stirred for 6h, then stopped heating, filtered after the temperature in a reaction bottle is reduced to 30 ℃, washed for 3-4 times by absolute ethyl alcohol, dried and ground, and modified nano silicon dioxide is obtained; the dosage ratio of the intermediate 3 to the ethyl acetate to the intermediate 2 is 10g to 100mL to 29.5g;
the intermediate 3 and the intermediate 2 undergo an acylation reaction to obtain modified nano silicon dioxide; the specific reaction process is as follows:
the obtained modified nano silicon dioxide is grafted with an organic molecular chain through chemical bonding, namely, an organic layer is formed on the surface of the modified nano silicon dioxide, so that the interface compatibility of the modified nano silicon dioxide and the acrylic resin coating can be greatly improved, the modified nano silicon dioxide is promoted to be uniformly dispersed in the acrylic resin coating, the modified nano silicon dioxide has good wear resistance and hardness, the wear resistance can be better exerted by being uniformly dispersed in the acrylic resin coating, and the hardness is improved; in addition, nano silicon dioxide belongs to inorganic filler, and organic molecular chains are dispersed in the coating through grafting on the surface of the nano silicon dioxide, so that exudation and migration are difficult, and the durability of various performances is ensured; from the structure of the organic molecular chain, the flame-retardant acrylic resin coating contains a plurality of C-F bonds, P-N flame-retardant components and unsaturated carbon-carbon double bonds, wherein the polarity of the C-F bonds is small, meanwhile, the C-F bonds have strong bond energy, the higher the chemical bond energy is, the better the stability is, and the acrylic resin coating can be endowed with remarkable waterproof property and flexibility; furthermore, the C-F bonds gradually migrate to the surface layer of the coating, so that the coating has very low surface energy; in addition, the C-F bond can well coat the C-C main chain, shield the C-C main chain and play a role in protection, so that the stability of the acrylic resin coating is improved; the P-N flame retardant component has the synergistic flame retardant effect of the phosphorus flame retardant and the nitrogen flame retardant, so that the paint can be endowed with safe and efficient flame retardant performance; and finally, the unsaturated carbon-carbon double bond can generate a chemical bonding effect with the acrylic resin matrix, so that the interaction force of the modified nano silicon dioxide and the coating is further improved, and various performances are further improved.
The invention has the beneficial effects that:
the aqueous acrylic resin coating for the building, which is obtained by blending the modified nano silicon dioxide and the acrylic resin, has low raw material cost, simple operation, environmental pollution reduction and acid and alkali resistance; in addition, the modified nano silicon dioxide prepared by grafting the nano silicon dioxide with the organic molecular chain can improve the compatibility of the nano silicon dioxide and the aqueous acrylic resin coating, and the nano silicon dioxide can effectively prevent migration and exudation of the organic molecules and ensure the durability of the performance; in addition, the introduced functional groups impart significant water repellency, flexibility, and a degree of flame retardancy to the aqueous acrylic resin coating. Therefore, the water-based acrylic resin coating for the building has lasting and remarkable waterproof property, flexibility and hardness, has certain flame retardance and acid and alkali resistance, and is an excellent environment-friendly coating for the building.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparation of modified nanosilicon dioxide
S1, adding 17.2g of phosphorus oxychloride and 10.1g of 2, 2-trifluoroethanol into a three-neck flask with a stirring reflux device, mixing, adding 0.3g of aluminum trichloride, stirring, slowly heating to 80 ℃, carrying out reflux reaction for 4 hours until no obvious HCl escapes, stopping the reaction, filtering, and carrying out reduced pressure distillation to remove unreacted phosphorus oxychloride to obtain an intermediate 1;
s2, adding 23.6g of intermediate 1, 11.6g of hydroxyethyl acrylate and 100mL of chloroform into a three-neck flask with a stirring reflux device, mixing, adding 0.4g of aluminum trichloride, stirring, slowly heating to 65 ℃, carrying out reflux reaction for 2 hours until no obvious HCl escapes, stopping the reaction, removing part of solvent by rotary evaporation, purifying by column chromatography (eluent adopts a mixed solvent of diethyl ether and ethyl acetate with the volume ratio of 1:1), and removing eluent by rotary evaporation to obtain intermediate 2;
s3, mixing 10.0g of nano silicon dioxide with 100mL of toluene, adding into a magnetic stirring device, adding a magnet, starting stirring, dispersing for 30min to uniformly disperse the silicon dioxide in the toluene solution, vacuumizing the device, and introducing N 2 Adding 6.50g of gamma-aminopropyl triethoxysilane, heating in oil bath, setting 50deg.C, opening condensate water, and setting 8Heating to 0 ℃ to make the reaction mild, enabling the temperature to reach 80 ℃, reacting for 4 hours, filtering, washing with toluene, and drying in a vacuum drying oven for 2 hours to obtain an intermediate 3;
s4, under the protection of room temperature and nitrogen, 10g of intermediate 3 is ultrasonically treated in 100mL of ethyl acetate for 30min, uniformly dispersed, 29.5g of intermediate 2 is added, uniformly stirred, slowly heated to 80 ℃, magnetically stirred (with the rotating speed of 1000 r/min), stirred for 6h, then stopped heating, after the temperature in a reaction bottle is reduced to 30 ℃, suction-filtered, washed for 3-4 times by absolute ethyl alcohol, dried and ground, and the modified nano silicon dioxide is obtained.
Example 2
Preparation of modified nanosilicon dioxide
S1, adding 34.4g of phosphorus oxychloride and 20.2g of 2, 2-trifluoroethanol into a three-neck flask with a stirring reflux device, mixing, adding 0.6g of aluminum trichloride, stirring, slowly heating to 80 ℃, carrying out reflux reaction for 4 hours until no obvious HCl escapes, stopping the reaction, filtering, and carrying out reduced pressure distillation to remove unreacted phosphorus oxychloride to obtain an intermediate 1;
s2, adding 47.2g of intermediate 1, 23.2g of hydroxyethyl acrylate and 200mL of chloroform into a three-neck flask with a stirring reflux device, mixing, adding 0.8g of aluminum trichloride, stirring, slowly heating to 65 ℃, carrying out reflux reaction for 2 hours until no obvious HCl escapes, stopping the reaction, removing part of solvent by rotary evaporation, purifying by column chromatography (eluent adopts a mixed solvent of diethyl ether and ethyl acetate with the volume ratio of 1:1), and removing eluent by rotary evaporation to obtain intermediate 2;
s3, mixing 20.0g of nano silicon dioxide with 200mL of toluene, adding into a magnetic stirring device, adding a magnet, starting stirring, dispersing for 30min to uniformly disperse the silicon dioxide in the toluene solution, vacuumizing the device, and introducing N 2 Adding 13.0g of gamma-aminopropyl triethoxysilane, heating in an oil bath, setting 50 ℃, opening condensate water, setting 80 ℃, heating to moderate reaction, reacting for 4 hours at 80 ℃, filtering, washing with toluene, and drying in a vacuum drying oven for 2 hours to obtain an intermediate 3;
s4, under the protection of room temperature and nitrogen, 20g of intermediate 3 is ultrasonically treated in 200mL of ethyl acetate for 30min, uniformly dispersed, 59.0g of intermediate 2 is added, uniformly stirred, slowly heated to 80 ℃, magnetically stirred (with the rotating speed of 1000 r/min), stirred for 6h, then stopped heating, after the temperature in a reaction bottle is reduced to 30 ℃, suction-filtered, washed for 3-4 times by absolute ethyl alcohol, dried and ground, and the modified nano silicon dioxide is obtained.
Example 3
Adding 25g of butyl acrylate, 25g of methyl methacrylate and 2g of sodium dodecyl sulfate (emulsifier) into 80g of water, emulsifying to prepare emulsion, then adding 1g of azobisisopropylimidazoline (water-soluble initiator) to initiate polymerization reaction, adding 5g of modified nano silicon dioxide prepared in example 1 after the reaction is completed, stirring strongly, and dispersing ultrasonically for 30min to obtain the water-based acrylic resin coating for building.
Example 4
Adding 25g of butyl acrylate, 25g of methyl methacrylate and 2g of sodium dodecyl sulfate (emulsifier) into 80g of water, emulsifying to prepare emulsion, then adding 1g of azobisisopropylimidazoline (water-soluble initiator) to initiate polymerization reaction, adding 10g of modified nano silicon dioxide prepared in example 1 after the reaction is completed, stirring strongly, and dispersing ultrasonically for 30min to obtain the water-based acrylic resin coating for building.
Example 5
Adding 25g of butyl acrylate, 25g of methyl methacrylate and 2g of sodium dodecyl sulfate (emulsifier) into 80g of water, emulsifying to prepare emulsion, then adding 1g of azobisisopropylimidazoline (water-soluble initiator) to initiate polymerization reaction, adding 15g of modified nano silicon dioxide prepared in example 2 after the reaction is completed, stirring strongly, and dispersing ultrasonically for 30min to obtain the water-based acrylic resin coating for building.
Comparative example
The same mass of unmodified ordinary nanosilica was used, the remainder of the procedure being as in example 5.
The coatings prepared in examples 3-5, comparative examples were uniformly applied to 10cm cement panels and left to dry for performance testing as follows:
the flexibility of the coating film is measured by adopting national standard GB/T1731-1993 'film flexibility measuring method';
the pencil hardness of the coating film is determined to be 6B-6H by the measurement of national standard GB/T6739-1996 pencil hardness determination method;
the acid resistance and the alkali resistance of the coating film are measured by adopting national standard GB/T1763-79 'determination of chemical resistance of a paint film';
the water resistance of the coating film is measured by a water immersion test method according to national standard GB/T1733-1993 paint film water resistance measurement method;
the fire-resistant time and the quality loss are measured by adopting national standard GB 12441-2005 'facing type fireproof paint';
the abrasion resistance of the abrasive paper is tested by adopting a sand paper linear abrasion method, a weight with the mass of 100g is added on 2000-mesh sand paper, so that the sand paper moves on a coating at a constant speed for 1cm for 1 time, and after 10 times, the water contact angle of the coating is tested;
the results of some tests are shown in table 1:
TABLE 1
The remaining test results are shown in table 2:
TABLE 2
As can be seen from Table 1 and Table 2, the aqueous acrylic resin coating for building has durable and remarkable water resistance, flexibility and hardness, has certain flame retardance and acid and alkali resistance, and is an excellent environment-friendly coating for building.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (8)
1. The preparation method of the water-based acrylic resin coating for the building is characterized by comprising the following steps of:
adding butyl acrylate, methyl methacrylate and sodium dodecyl sulfate into water, emulsifying, then adding azodiisopropylimidazoline to initiate polymerization, adding modified nano silicon dioxide, stirring strongly, and dispersing ultrasonically to obtain the water-based acrylic resin coating for building.
2. The preparation method of the aqueous acrylic resin coating for the building, according to claim 1, is characterized in that the mass ratio of butyl acrylate to methyl methacrylate to sodium dodecyl sulfate to water to azodiisopropylimidazoline to modified nano-silica is 25:25:2:80:1:5-15.
3. The method for preparing the aqueous acrylic resin coating for construction according to claim 1, wherein the modified nano silica is prepared by the steps of:
s1, mixing phosphorus oxychloride and 2, 2-trifluoroethanol, adding aluminum trichloride, stirring, heating to 80 ℃, carrying out reflux reaction for 4 hours, filtering, and carrying out reduced pressure distillation to obtain an intermediate 1;
s2, mixing the intermediate 1, hydroxyethyl acrylate and chloroform, adding aluminum trichloride, stirring, heating to 65 ℃, carrying out reflux reaction for 2 hours, carrying out rotary evaporation, purifying by column chromatography, and removing eluent by rotary evaporation to obtain an intermediate 2;
s3, mixing nano silicon dioxide with toluene, magnetically stirring, dispersing for 30min, vacuumizing the device, introducing N2 gas, adding gamma-aminopropyl triethoxysilane, starting oil bath heating, reacting for 4h at 80 ℃, carrying out suction filtration, washing with toluene, and drying for 2h to obtain an intermediate 3;
and S4, under the protection of room temperature and nitrogen, the intermediate 3 is subjected to ultrasonic treatment in ethyl acetate for 30min, dispersed uniformly, added with the intermediate 2, stirred uniformly, heated to 80 ℃, stirred by magnetic force for 6h, filtered by suction, washed by absolute ethyl alcohol, dried and ground to obtain the modified nano silicon dioxide.
4. The method for producing an aqueous acrylic resin paint for construction according to claim 3, wherein the ratio of phosphorus oxychloride, 2-trifluoroethanol and aluminum trichloride in the step S1 is 17.2g to 10.1g to 0.3g.
5. The method for producing an aqueous acrylic resin coating for construction according to claim 3, wherein the ratio of the amounts of intermediate 1, hydroxyethyl acrylate, chloroform, and aluminum trichloride in step S2 is 23.6 g/11.6 g/100 mL/0.4 g.
6. The method for producing an aqueous acrylic resin paint for construction according to claim 3, wherein the ratio of the amounts of nano silica, toluene and γ -aminopropyl triethoxysilane used in step S2 is 10.0g to 100mL to 6.50g.
7. The method for producing an aqueous acrylic resin paint for construction according to claim 3, wherein the ratio of the amounts of intermediate 3, ethyl acetate and intermediate 2 in step S2 is 10 g/100 mL/29.5 g.
8. An aqueous acrylic resin coating for construction, characterized by being prepared according to the method of any one of claims 1 to 7.
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| CN105111882A (en) * | 2014-06-15 | 2015-12-02 | 朱蕾 | Light-resistant antibacterial water-based acrylic resin coating used in building industry |
| CN113416459A (en) * | 2021-06-11 | 2021-09-21 | 安徽强邦新材料股份有限公司 | Printing plate protective coating and preparation method thereof |
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| CN113980533A (en) * | 2021-12-17 | 2022-01-28 | 鹤山市金润纳新型材料有限公司 | Water-based acrylic resin coating |
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