CN116285622B - Preparation method of fiber toughening coating - Google Patents
Preparation method of fiber toughening coating Download PDFInfo
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- CN116285622B CN116285622B CN202310106044.1A CN202310106044A CN116285622B CN 116285622 B CN116285622 B CN 116285622B CN 202310106044 A CN202310106044 A CN 202310106044A CN 116285622 B CN116285622 B CN 116285622B
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- polyvinyl alcohol
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- 239000000835 fiber Substances 0.000 title claims abstract description 65
- 238000000576 coating method Methods 0.000 title claims abstract description 50
- 239000011248 coating agent Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 48
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 34
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 34
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 239000012948 isocyanate Substances 0.000 claims abstract description 21
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 21
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000839 emulsion Substances 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 19
- 239000011324 bead Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- 239000002562 thickening agent Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 239000000049 pigment Substances 0.000 claims abstract description 6
- 239000000080 wetting agent Substances 0.000 claims abstract description 5
- 239000000654 additive Substances 0.000 claims abstract description 3
- 230000000996 additive effect Effects 0.000 claims abstract description 3
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- -1 polysiloxane Polymers 0.000 claims description 14
- 229910021389 graphene Inorganic materials 0.000 claims description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 11
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 11
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 11
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 11
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 11
- 229920000858 Cyclodextrin Polymers 0.000 claims description 10
- 239000001116 FEMA 4028 Substances 0.000 claims description 10
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 10
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 10
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 10
- 229960004853 betadex Drugs 0.000 claims description 10
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 10
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 claims description 9
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 9
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical group CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 9
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 claims description 9
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 9
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 9
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 7
- 229920000570 polyether Polymers 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 3
- 229920000896 Ethulose Polymers 0.000 claims description 2
- 239000001859 Ethyl hydroxyethyl cellulose Substances 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims description 2
- 235000019326 ethyl hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 2
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002480 mineral oil Substances 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 150000003890 succinate salts Chemical group 0.000 claims 1
- 239000003973 paint Substances 0.000 abstract description 12
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 238000005336 cracking Methods 0.000 abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 16
- 238000012360 testing method Methods 0.000 description 13
- 239000004408 titanium dioxide Substances 0.000 description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 7
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000011527 polyurethane coating Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 229920002126 Acrylic acid copolymer Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000005028 tinplate 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- 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
-
- 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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a preparation method of a fiber toughening coating, which comprises the following steps: adding a dispersing agent, a wetting agent, a defoaming agent and a pH regulator into water for uniform dispersion, and adding pigment for continuous stirring to obtain a pre-dispersion liquid; preparing polyvinyl alcohol fiber grafted isocyanate; adding polyvinyl alcohol fiber grafted isocyanate, organosilicon modified aqueous acrylic emulsion, film forming additive and hollow glass bead into the pre-dispersion liquid, stirring, adding thickener to adjust the viscosity of the system to 85-95KU/30 ℃, and continuing stirring for 5-10min to obtain a prefabricated material; and uniformly mixing the prefabricated material and the curing agent to obtain the fiber toughening coating. The invention has the advantages of high hardness, high water resistance, good flexibility, high adhesive force, excellent cracking resistance, no cracking after the paint film is dried, simple preparation method and convenient large-scale popularization and application.
Description
Technical Field
The invention relates to the technical field of toughening coating, in particular to a preparation method of fiber toughening coating.
Background
The paint is a chemical product made of resin and oil, which contains pigment or does not contain pigment. The coating can be dried to form a film on the surface of an object, so that the surface of the object to be coated is isolated from an environmental medium, and the object to be coated is protected and decorated.
Polyurethane coatings are a common type of coating consisting essentially of a resin component, which is essentially a hydroxyl-containing resin, and a curing agent component, which is essentially an isocyanate prepolymer. The existing polyurethane coating has the characteristics of low film forming temperature, good wear resistance, high hardness, high corrosion resistance, good weather resistance and the like, and is widely used for coating road markings, but the existing polyurethane coating has poor toughness and is used for the road markings, and cracks and the like are easy to occur.
The polyvinyl alcohol fiber has high strength and high elastic modulus, and is acid-base and sun-proof, easy to be adhered to cement pavement and relatively low in cost, so that the polyvinyl alcohol fiber becomes an ideal toughening material for reinforcing polyurethane paint. The nano graphene oxide flake is a product of graphite powder subjected to chemical oxidation and stripping, graphene oxide is a single atomic layer, can be expanded to tens of micrometers in transverse dimension at any time, has amphipathy, and shows hydrophilic to hydrophobic property distribution from the edge to the center of the graphene flake, and the nano graphene oxide flake and polyvinyl alcohol fiber are compounded to enable the coating to have excellent mechanical properties, but the nano graphene oxide flake is extremely easy to agglomerate and poor in intersolubility with the polyvinyl alcohol fiber, so that the coating has poor adhesive force, and meanwhile, the coating toughening effect cannot achieve an ideal effect, so that the problem needs to be solved.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a preparation method of a fiber toughening coating.
A preparation method of a fiber toughening coating comprises the following steps:
s1, adding 1-2 parts of dispersing agent, 1-2 parts of wetting agent, 1-2 parts of defoamer and 1-2 parts of pH regulator into 10-20 parts of water according to parts by weight, dispersing at a speed of 500-600r/min, adding 1-3 parts of pigment, and continuously stirring to obtain a pre-dispersion liquid;
s2, adding 1-3 parts of beta-cyclodextrin into 10-30 parts of DMF, stirring at the temperature of 80-90 ℃ under the protection of argon, adding 5-10 parts of isophorone diisocyanate, 1-3 parts of polytetrahydrofuran glycol with the molecular weight of 1000, 0.01-0.1 part of dibutyltin dilaurate, continuously stirring, adding 5-10 parts of polyvinyl alcohol fiber, 0.1-0.5 part of graphene oxide and 1-4 parts of sodium carboxymethyl cellulose, regulating the pH of a system to 5-6 by adopting hydrochloric acid, performing ultrasonic dispersion for 1-2 hours, wherein the ultrasonic frequency is 10-20kHz, and the ultrasonic power is 300-500W, so as to obtain polyvinyl alcohol fiber grafted isocyanate;
s3, adding polyvinyl alcohol fiber grafted isocyanate, 5-12 parts of organosilicon modified aqueous acrylic emulsion, 1-5 parts of film forming additive and 1-2 parts of hollow glass microsphere into the pre-dispersion liquid, stirring at the speed of 500-1500r/min, adding 1-5 parts of thickener to adjust the viscosity of the system, and continuing stirring for 5-10min to obtain a pre-material;
s4, uniformly mixing the prefabricated material with 1-2 parts of curing agent to obtain the fiber toughening coating.
Preferably, in S1, the viscosity of the organosilicon modified aqueous acrylic emulsion is 200-2500 mPa.s, the solid content is 36-48wt% and the pH is 7-9.
Preferably, in S1, the pH adjuster is 2-amino-2-methyl-1-propanol.
Preferably, in S1, the dispersant is one of an organic sulfosuccinate, a polymeric dispersant polymethacrylic acid or an acrylic acid copolymer dispersion resin, preferably a sulfosuccinate.
Preferably, in S1, the wetting agent is at least one of propylene glycol, glycerin, polyether modified polysiloxane.
Preferably, in S1, the antifoaming agent is a mineral oil or a silicone.
Preferably, in S1, the pigment is titanium dioxide.
Preferably, in S3, the hollow glass microspheres have a particle size of 1 to 100 μm and a density of 0.1 to 0.5g/cc.
Preferably, in S3, the thickener is a cellulose thickener, preferably at least one of hydroxyethyl cellulose, hydroxypropyl methylcellulose, carboxymethyl cellulose, and ethyl hydroxyethyl cellulose.
Preferably, in S3, the coalescent is an alcohol ester-12.
Preferably, in S4, the curing agent is HDI biuret.
The technical effects of the invention are as follows:
meanwhile, compared with HDI and MDI with symmetrical structures, the structure symmetry of isophorone diisocyanate is poor, the distance between adjacent molecular chains is far, and hydrogen bonds are not easy to form, so that under the action of a catalyst DBTL, secondary alcohol of beta-cyclodextrin and-NCO react preferentially to form a crosslinked structure, meanwhile, the asymmetric structure of isophorone diisocyanate increases the distance between molecular chains, so that hydrogen bonds are not easy to form, in an acidic environment, the sodium carboxymethylcellulose long-chain structure contains a large number of carboxyl groups, the surface of polyvinyl alcohol fiber contains a large number of active hydroxyl groups, the edge of a nano graphene oxide lamellar structure contains a large number of hydroxyl groups and carboxyl groups, and therefore sodium carboxymethylcellulose of the long-chain structure is firmly combined with isophorone diisocyanate in a chemical bond mode, and is uniformly embedded into a polymer network structure, so that the polyvinyl alcohol fiber is chemically combined in a system, the flexibility and the shock resistance of the paint are improved, the migration is not easy to occur in the use process, the paint has better dispersibility, the good dispersion with the nano graphene oxide lamellar structure edge contains a large number of hydroxyl groups, the problem of the film forming capability is easy to overcome in the film forming process, and the film forming and the problem is easy to occur.
The invention satisfies the requirements that the surface drying time is within 20-40min, the real drying time is within 12-16h, and the paint film has higher hardness, water resistance and salt fog resistance, good flexibility, high adhesive force and excellent cracking resistance, and does not crack after the paint film is real dried; the polyurethane paint disclosed by the invention has low VOC emission, belongs to an environment-friendly paint, has low energy consumption, and promotes the environmental protection and sanitation of the paint.
Drawings
FIG. 1 is a graph comparing stress strain curves of the cured films of the coatings of example 5 and comparative examples 1-2.
Detailed Description
The invention is further illustrated below in connection with specific embodiments.
Example 1
A preparation method of a fiber toughening coating comprises the following steps:
s1, adding 1kg of succinate sulfonate, 1kg of propylene glycol, 1kg of polydimethylsiloxane and 1kg of 2-amino-2-methyl-1-propanol into 10kg of water, dispersing for 5min at a speed of 500r/min, adding 1kg of titanium dioxide, and continuously stirring for 5min at a speed of 1000r/min to obtain a pre-dispersion;
s2, adding 1kg of beta-cyclodextrin into 10kg of DMF, stirring for 10min at 80 ℃ under the protection of argon, adding 5kg of isophorone diisocyanate, 1kg of polytetrahydrofuran glycol with molecular weight of 1000 and 0.01kg of dibutyl tin dilaurate, continuously stirring for 1h, adding 5kg of polyvinyl alcohol fiber, 0.1kg of graphene oxide and 1kg of sodium carboxymethyl cellulose, regulating pH of a system to 5 by adopting hydrochloric acid, performing ultrasonic dispersion for 1h, wherein ultrasonic frequency is 10kHz, and ultrasonic power is 300W, so as to obtain polyvinyl alcohol fiber grafted isocyanate;
s3, adding polyvinyl alcohol fiber grafted isocyanate, 5kg of organosilicon modified aqueous acrylic emulsion, 1kg of alcohol ester-12 and 1kg of hollow glass beads into the pre-dispersion liquid, stirring at the speed of 500r/min for 5min, adding 1kg of carboxymethyl cellulose to adjust the viscosity of the system to 85KU/30 ℃, and continuing stirring for 5min to obtain a pre-material;
the viscosity of the organosilicon modified aqueous acrylic emulsion is 200 mPa.s, the solid content is 36wt% and the pH is 7;
the particle size of the hollow glass beads is 1-100 mu m, and the density is 0.1g/cc;
s4, uniformly mixing the prefabricated material with 1kg of HDI biuret to obtain the fiber toughening coating.
Example 2
A preparation method of a fiber toughening coating comprises the following steps:
s1, adding 2kg of succinate sulfonate, 2kg of propylene glycol, 2kg of polydimethylsiloxane and 2kg of 2-amino-2-methyl-1-propanol into 20kg of water, dispersing for 15min at a speed of 600r/min, adding 3kg of titanium dioxide, and continuously stirring for 15min at a speed of 2000r/min to obtain a pre-dispersion;
s2, adding 3kg of beta-cyclodextrin into 30kg of DMF, stirring for 30min at 90 ℃ under the protection of argon, adding 10kg of isophorone diisocyanate, 3kg of polytetrahydrofuran glycol with molecular weight of 1000 and 0.1kg of dibutyl tin dilaurate, continuously stirring for 2h, adding 10kg of polyvinyl alcohol fiber, 0.5kg of graphene oxide and 4kg of sodium carboxymethyl cellulose, regulating pH of a system to 6 by adopting hydrochloric acid, and performing ultrasonic dispersion for 2h at ultrasonic frequency of 20kHz and ultrasonic power of 500W to obtain polyvinyl alcohol fiber grafted isocyanate;
s3, adding polyvinyl alcohol fiber grafted isocyanate, 12kg of organosilicon modified aqueous acrylic emulsion, 5kg of alcohol ester-12 and 2kg of hollow glass beads into the pre-dispersion liquid, stirring at a speed of 1500r/min for 10min, adding 5kg of carboxymethyl cellulose to adjust the viscosity of the system to 95KU/30 ℃, and continuing stirring for 10min to obtain a pre-material;
the viscosity of the organosilicon modified aqueous acrylic emulsion is 2500 mPa.s, the solid content is 48wt% and the pH is 9;
the particle size of the hollow glass beads is 1-100 mu m, and the density is 0.5g/cc;
s4, uniformly mixing the prefabricated material with 2kg of HDI biuret to obtain the fiber toughening coating.
Example 3
A preparation method of a fiber toughening coating comprises the following steps:
s1, adding 1.2kg of succinate sulfonate, 1.2kg of polyether modified polysiloxane, 1.2kg of polydimethylsiloxane and 1.2kg of 2-amino-2-methyl-1-propanol into 12kg of water, dispersing for 6min at the speed of 520r/min, adding 1.2kg of titanium dioxide, and continuously stirring for 7min at the speed of 1200r/min to obtain a pre-dispersion;
s2, adding 1.5kg of beta-cyclodextrin into 15kg of DMF, stirring for 15min at 82 ℃ under the protection of argon, adding 6kg of isophorone diisocyanate, 1.2kg of polytetrahydrofuran glycol with molecular weight of 1000 and 0.04kg of dibutyl tin dilaurate, continuously stirring for 1.2h, adding 6kg of polyvinyl alcohol fiber, 0.2kg of graphene oxide and 2kg of sodium carboxymethyl cellulose, regulating the pH of a system to 5.2 by adopting hydrochloric acid, and performing ultrasonic dispersion for 1.5h, wherein the ultrasonic frequency is 12kHz, and the ultrasonic power is 350W to obtain polyvinyl alcohol fiber grafted isocyanate;
s3, adding polyvinyl alcohol fiber grafted isocyanate, 8kg of organosilicon modified aqueous acrylic emulsion, 2kg of alcohol ester-12 and 1.2kg of hollow glass beads into the pre-dispersion liquid, stirring at the speed of 700r/min for 6min, adding 2kg of carboxymethyl cellulose to adjust the viscosity of the system to 8KU/30 ℃, and continuing stirring for 6min to obtain a prefabricated material;
the viscosity of the organosilicon modified aqueous acrylic emulsion is 460 mPa.s, the solid content is 38wt% and the pH is 7.2;
the particle size of the hollow glass beads is 1-100 mu m, and the density is 0.4g/cc;
s4, uniformly mixing the prefabricated material with 1.2kg of HDI biuret to obtain the fiber toughening coating.
Example 4
A preparation method of a fiber toughening coating comprises the following steps:
s1, adding 1.6kg of succinate sulfonate, 1.5kg of polyether modified polysiloxane, 1.5kg of polydimethylsiloxane and 1.6kg of 2-amino-2-methyl-1-propanol into 18kg of water, dispersing for 12min at a speed of 580r/min, adding 2.5kg of titanium dioxide, and continuously stirring for 12min at a speed of 1800r/min to obtain a pre-dispersion;
s2, adding 2.5kg of beta-cyclodextrin into 24kg of DMF, stirring at 88 ℃ for 25min under the protection of argon, adding 8kg of isophorone diisocyanate, 2.6kg of polytetrahydrofuran glycol with molecular weight of 1000 and 0.08kg of dibutyl tin dilaurate, continuously stirring for 1.8h, adding 8kg of polyvinyl alcohol fiber, 0.4kg of graphene oxide and 3kg of sodium carboxymethyl cellulose, regulating the pH of a system to 5.5 by adopting hydrochloric acid, and performing ultrasonic dispersion for 1.5h, wherein the ultrasonic frequency is 16kHz, and the ultrasonic power is 460W to obtain polyvinyl alcohol fiber grafted isocyanate;
s3, adding polyvinyl alcohol fiber grafted isocyanate, 10kg of organosilicon modified aqueous acrylic emulsion, 4kg of alcohol ester-12 and 1.9kg of hollow glass beads into the pre-dispersion liquid, stirring at the speed of 1200r/min for 8min, adding 4kg of carboxymethyl cellulose to adjust the viscosity of the system to 92KU/30 ℃, and continuing stirring for 8min to obtain a prefabricated material;
the viscosity of the organosilicon modified aqueous acrylic emulsion is 2200 mPa.s, the solid content is 46wt% and the pH is 8.4;
the particle size of the hollow glass beads is 1-100 mu m, and the density is 0.2g/cc;
s4, uniformly mixing the prefabricated material with 1.8kg of HDI biuret to obtain the fiber toughening coating.
Example 5
A preparation method of a fiber toughening coating comprises the following steps:
s1, adding 1.8kg of succinate sulfonate, 1.5kg of polyether modified polysiloxane, 1.3kg of polydimethylsiloxane and 1.2kg of 2-amino-2-methyl-1-propanol into 14kg of water, dispersing for 10min at a speed of 500r/min, adding 2kg of titanium dioxide, and continuously stirring for 10min at a speed of 1500r/min to obtain a pre-dispersion;
s2, adding 2kg of beta-cyclodextrin into 20kg of DMF, stirring for 20min at 85 ℃ under the protection of argon, adding 8kg of isophorone diisocyanate, 2kg of polytetrahydrofuran glycol with molecular weight of 1000 and 0.05kg of dibutyltin dilaurate, continuously stirring for 1.5h, adding 8kg of polyvinyl alcohol fiber, 0.3kg of graphene oxide and 2kg of sodium carboxymethyl cellulose, regulating pH of a system to 5.5 by adopting hydrochloric acid, performing ultrasonic dispersion for 1.5h, wherein ultrasonic frequency is 15kHz, and ultrasonic power is 420W, so as to obtain polyvinyl alcohol fiber grafted isocyanate;
s3, adding polyvinyl alcohol fiber grafted isocyanate, 10kg of organosilicon modified aqueous acrylic emulsion, 2kg of alcohol ester-12 and 1.5kg of hollow glass beads into the pre-dispersion liquid, stirring at the speed of 1000r/min for 8min, adding 3.6kg of carboxymethyl cellulose to adjust the viscosity of the system to 91KU/30 ℃, and continuing stirring for 7min to obtain a prefabricated material;
the viscosity of the organosilicon modified aqueous acrylic emulsion is 1541 mPas, the solid content is 40.6wt% and the pH is 8.3;
the particle size of the hollow glass beads is 1-100 mu m, and the density is 0.3g/cc;
s4, uniformly mixing the prefabricated material with 1kg of HDI biuret to obtain the fiber toughening coating.
Comparative example 1
A preparation method of a fiber toughening coating comprises the following steps:
s1, adding 1.8kg of succinate sulfonate, 1.5kg of polyether modified polysiloxane, 1.3kg of polydimethylsiloxane and 1.2kg of 2-amino-2-methyl-1-propanol into 14kg of water, dispersing for 10min at a speed of 500r/min, adding 2kg of titanium dioxide, and continuously stirring for 10min at a speed of 1500r/min to obtain a pre-dispersion;
s2, adding 2kg of beta-cyclodextrin into 20kg of DMF, stirring for 20min at 85 ℃ under the protection of argon, adding 8kg of hexamethylene-1, 6-diisocyanate, 2kg of polytetrahydrofuran glycol with molecular weight of 1000 and 0.05kg of dibutyl tin dilaurate, continuously stirring for 1.5h, adding 8kg of polyvinyl alcohol fiber, 0.3kg of graphene oxide and 2kg of sodium carboxymethyl cellulose, regulating the pH of a system to 5.5 by adopting hydrochloric acid, performing ultrasonic dispersion for 1.5h, performing ultrasonic frequency to 15kHz, and performing ultrasonic power to 420W to obtain polyvinyl alcohol fiber grafted isocyanate;
s3, adding polyvinyl alcohol fiber grafted isocyanate, 10kg of organosilicon modified aqueous acrylic emulsion, 2kg of alcohol ester-12 and 1.5kg of hollow glass beads into the pre-dispersion liquid, stirring at the speed of 1000r/min for 8min, adding 3.6kg of carboxymethyl cellulose to adjust the viscosity of the system to 91KU/30 ℃, and continuing stirring for 7min to obtain a prefabricated material;
the viscosity of the organosilicon modified aqueous acrylic emulsion is 1541 mPas, the solid content is 40.6wt% and the pH is 8.3;
the particle size of the hollow glass beads is 1-100 mu m, and the density is 0.3g/cc;
s4, uniformly mixing the prefabricated material with 1kg of HDI biuret to obtain the fiber toughening coating.
Comparative example 2
A preparation method of a fiber toughening coating comprises the following steps:
s1, adding 1.8kg of succinate sulfonate, 1.5kg of polyether modified polysiloxane, 1.3kg of polydimethylsiloxane and 1.2kg of 2-amino-2-methyl-1-propanol into 14kg of water, dispersing for 10min at a speed of 500r/min, adding 2kg of titanium dioxide, and continuously stirring for 10min at a speed of 1500r/min to obtain a pre-dispersion;
s2, adding 2kg of beta-cyclodextrin into 20kg of DMF, stirring for 20min at 85 ℃ under the protection of argon, adding 8kg of isophorone diisocyanate, 2kg of polytetrahydrofuran glycol with molecular weight 1000 and 0.05kg of dibutyl tin dilaurate, and continuously stirring for 1.5h to obtain pretreated isocyanate;
s3, adding pretreated isocyanate, 8kg of polyvinyl alcohol fiber, 0.3kg of graphene oxide, 2kg of sodium carboxymethyl cellulose, 10kg of organosilicon modified aqueous acrylic emulsion, 2kg of alcohol ester-12 and 1.5kg of hollow glass beads into the pre-dispersion liquid, stirring at the speed of 1000r/min for 8min, adding 3.6kg of carboxymethyl cellulose to adjust the viscosity of the system to 91KU/30 ℃, and continuing stirring for 7min to obtain a pre-material;
the viscosity of the organosilicon modified aqueous acrylic emulsion is 1541 mPas, the solid content is 40.6wt% and the pH is 8.3;
the particle size of the hollow glass beads is 1-100 mu m, and the density is 0.3g/cc;
s4, uniformly mixing the prefabricated material with 1kg of HDI biuret to obtain the fiber toughening coating.
Performance testing
Mechanical property test
The coatings prepared in examples 1-5 and comparative examples 1-2 were coated with a reticle and each parameter of the reticle obtained by coating was examined, wherein:
flexibility: testing by using a GB/T1731-1993 testing method;
impact resistance: testing by using a GB/T1732-93 testing method;
adhesion force: testing by using a GB/T9286-1988 testing method;
the test results are shown in the following table:
as can be seen from the above table, the toughening coating prepared by the invention has better high toughness and impact resistance, and the coating film has better comprehensive performance, wherein the best example is the example 5.
Appearance and gloss testing
The coatings prepared in examples 1-5 and comparative examples 1-2 were coated with a marking and the appearance and gloss of the coated marking were examined, wherein:
paint film appearance: measured by the method of GB/T1729-1979.
Paint film thickness: measured by the method of GB/T1764-1979.
Hardness: measured by the method of GB/T1730-1993.
Water resistance: measured by the method of GB/T1733-1993.
Storage period: centrifugation was carried out at 3000r/min for 30min without sedimentation.
The test results are shown in the following table:
stress strain testing
The toughening coatings prepared in example 5 and comparative examples 1-2 were respectively applied to the surface of the pretreated steel structure or tinplate, the thickness of the coating is 1.+ -. 0.2cm, and the test results are shown in FIG. 1.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (12)
1. The preparation method of the fiber toughening coating is characterized by comprising the following steps:
s1, adding 1-2 parts of dispersing agent, 1-2 parts of wetting agent, 1-2 parts of defoamer and 1-2 parts of pH regulator into 10-20 parts of water according to parts by weight, dispersing at a speed of 500-600r/min, adding 1-3 parts of pigment, and continuously stirring to obtain a pre-dispersion liquid;
s2, adding 1-3 parts of beta-cyclodextrin into 10-30 parts of DMF, stirring at the temperature of 80-90 ℃ under the protection of argon, adding 5-10 parts of isophorone diisocyanate, 1-3 parts of polytetrahydrofuran glycol with the molecular weight of 1000, 0.01-0.1 part of dibutyltin dilaurate, continuously stirring, adding 5-10 parts of polyvinyl alcohol fiber, 0.1-0.5 part of graphene oxide and 1-4 parts of sodium carboxymethyl cellulose, regulating the pH of a system to 5-6 by adopting hydrochloric acid, performing ultrasonic dispersion for 1-2 hours, wherein the ultrasonic frequency is 10-20kHz, and the ultrasonic power is 300-500W, so as to obtain polyvinyl alcohol fiber grafted isocyanate;
the strength of the polyvinyl alcohol fiber is 106-115cN/dtex;
s3, adding polyvinyl alcohol fiber grafted isocyanate, 5-12 parts of organosilicon modified aqueous acrylic emulsion, 1-5 parts of film forming additive and 1-2 parts of hollow glass microsphere into the pre-dispersion liquid, stirring at the speed of 500-1500r/min, adding 1-5 parts of thickener to adjust the viscosity of the system, and continuing stirring for 5-10min to obtain a pre-material;
s4, uniformly mixing the prefabricated material with 1-2 parts of curing agent to obtain the fiber toughening coating.
2. The method of preparing a fiber toughening coating according to claim 1, wherein in S3, the viscosity of the organosilicon modified aqueous acrylic emulsion is 200-2500 mPa-S, the solid content is 36-48wt%, and the pH is 7-9.
3. The method of producing a fiber toughening coating according to claim 1, wherein in S1, the pH adjuster is 2-amino-2-methyl-1-propanol.
4. The method for producing a fiber-reinforced coating according to claim 1, wherein in S1, the dispersant is an organic-based sulfosuccinate or a polymeric dispersant, polymethacrylic acid.
5. The method of producing a fiber toughening coating according to claim 4, wherein in S1, the dispersant is succinate sulfonate.
6. The method for preparing a fiber toughening coating according to claim 1, wherein in S1, the wetting agent is at least one of propylene glycol, glycerin, polyether modified polysiloxane.
7. The method of producing a fiber-reinforced coating according to claim 1, wherein in S1, the defoaming agent is mineral oils or silicones.
8. The method of producing a fiber-reinforced coating according to claim 1, wherein in S3, the hollow glass beads have a particle diameter of 1 to 100 μm and a density of 0.1 to 0.5g/cc.
9. The method of producing a fiber-reinforced coating according to claim 1, wherein in S3, the thickener is a cellulose thickener.
10. The method of producing a fiber toughening coating according to claim 9, wherein in S3, the thickener is at least one of hydroxyethyl cellulose, hydroxypropyl methylcellulose, carboxymethyl cellulose, and ethyl hydroxyethyl cellulose.
11. The method of preparing a fiber toughening coating according to claim 1, wherein in S3, the film forming aid is an alcohol ester-12.
12. The method of preparing a fiber toughening coating according to claim 1, wherein in S4, the curing agent is HDI biuret.
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