CN116751494A - Graphene anti-freezing coating with superhydrophobic performance and preparation method thereof - Google Patents
Graphene anti-freezing coating with superhydrophobic performance and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 91
- 238000007710 freezing Methods 0.000 title claims abstract description 76
- 238000000576 coating method Methods 0.000 title claims abstract description 74
- 239000011248 coating agent Substances 0.000 title claims abstract description 73
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 37
- 239000000839 emulsion Substances 0.000 claims abstract description 36
- 239000000945 filler Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007798 antifreeze agent Substances 0.000 claims abstract description 24
- 239000003085 diluting agent Substances 0.000 claims abstract description 24
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 24
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 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 abstract description 21
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 21
- 239000003822 epoxy resin Substances 0.000 claims abstract description 21
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 21
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 21
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 21
- 239000013530 defoamer Substances 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 75
- 239000006185 dispersion Substances 0.000 claims description 32
- 239000007864 aqueous solution Substances 0.000 claims description 24
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 24
- 230000002209 hydrophobic effect Effects 0.000 claims description 21
- 238000009210 therapy by ultrasound Methods 0.000 claims description 19
- VBGGLSWSRVDWHB-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(trifluoromethoxy)silane Chemical compound FC(F)(F)O[Si](OC(F)(F)F)(OC(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F VBGGLSWSRVDWHB-UHFFFAOYSA-N 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 18
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 17
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 12
- CWZPGMMKDANPKU-UHFFFAOYSA-L butyl-di(dodecanoyloxy)tin Chemical compound CCCC[Sn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O CWZPGMMKDANPKU-UHFFFAOYSA-L 0.000 claims description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000010907 mechanical stirring Methods 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical group CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000004952 Polyamide Substances 0.000 claims description 3
- QQWAKSKPSOFJFF-UHFFFAOYSA-N oxiran-2-ylmethyl 2,2-dimethyloctanoate Chemical compound CCCCCCC(C)(C)C(=O)OCC1CO1 QQWAKSKPSOFJFF-UHFFFAOYSA-N 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- -1 polysiloxane Polymers 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 229960004063 propylene glycol Drugs 0.000 claims description 3
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 abstract description 17
- 239000004890 Hydrophobing Agent Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 239000002105 nanoparticle Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000002528 anti-freeze Effects 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- 108010053481 Antifreeze Proteins Proteins 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000002519 antifouling agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000006115 industrial coating Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007921 spray Substances 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D7/65—Additives macromolecular
-
- 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
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention provides a graphene anti-freezing coating with super-hydrophobic performance and a preparation method thereof, wherein the coating comprises the following raw materials in parts by weight: 40-50 parts of active epoxy resin, 5-10 parts of graphene, 4-8 parts of active diluent, 5-10 parts of antifreeze agent, 1-5 parts of hydrophobing agent, 1-5 parts of thixotropic agent, 2-5 parts of emulsion defoamer, 5-10 parts of filler, 2-4 parts of sodium carboxymethylcellulose and 30-40 parts of deionized water. The invention uses fluorosilane to prepare nano TiO 2 And polyurethane resin, and then modifying nano TiO with fluorine-silicon 2 Mixing with fluorosilicone modified polyurethane resin to form super-hydrophobic composite emulsion, and adding graphene, anti-freezing agent and other assistants to further raise the paintHydrophobic properties and anti-freezing properties of (a).
Description
Technical Field
The invention relates to the technical field of industrial coatings, in particular to a graphene anti-freezing coating with superhydrophobic performance and a preparation method thereof.
Background
Most wind power plants in China are distributed in northern and northwest regions, and wind turbine generators in the regions are affected by severe weather such as sand, ice and snow during operation. The blade is used as a key component of the wind turbine generator, and various environmental tests are also encountered in actual operation, especially the icing problem of the surface of the blade, so that the problem to be solved is a urgent need. After the blade is frozen, the aerodynamic shape of the blade can be changed, the power generation of the wind turbine generator can be reduced, and when the blade is frozen seriously, the wind turbine generator must be stopped, so that the power generation can be influenced, the quality of the blade is unbalanced due to the ice, and the fatigue damage of the wind turbine generator component is increased; in addition, the ice cubes thrown out with the rotation of the blades may cause injury to people, animals, plants, buildings, etc. near the wind farm. Therefore, wind power blades are usually coated with protective paint, and obviously, the severe environment has higher performance requirements for wind power blade paint.
Disclosure of Invention
Based on the actual needs, the graphene anti-freezing coating with the superhydrophobic performance and the preparation method thereof are provided, and the aim is to reduce the high adhesive force between ice and the surface of a blade, so that the adhesive strength between ice water and a material is reduced, and the anti-freezing effect is achieved.
The technical scheme of the invention is realized as follows: the graphene anti-freezing coating with the superhydrophobic performance comprises the following raw materials in parts by weight: 40-50 parts of active epoxy resin, 5-10 parts of graphene, 4-8 parts of active diluent, 5-10 parts of antifreeze agent, 1-5 parts of hydrophobe, 1-5 parts of thixotropic agent, 5-10 parts of dispersing agent, 2-10 parts of emulsion defoamer, 5-10 parts of filler and 2-4 parts of sodium carboxymethyl cellulose.
Further described, the graphene anti-freezing coating with the superhydrophobic performance comprises the following raw materials in parts by weight: 45 parts of active epoxy resin, 8 parts of graphene, 6 parts of active diluent, 8 parts of antifreeze agent, 3 parts of hydrophobic agent, 3 parts of thixotropic agent, 4 parts of emulsion defoamer, 7 parts of filler, 3 parts of sodium carboxymethyl cellulose and 35 parts of water.
Further illustratively, the reactive diluent is one or more of glycidyl neodecanoate, beta-hydroxyethyl methacrylate, or 1, 6-hexanediol diacrylate.
Further, the antifreeze agent is 1, 2-propylene glycol aqueous solution or ethylene glycol aqueous solution.
Further illustratively, the hydrophobic agent is a polysiloxane.
Further illustratively, the thixotropic agent is a polyamide wax.
Further described, the filler is fluorosilicone modified nano TiO 2 Particles and fluorosilicone modified polyurethane resin.
Further described, the fluorosilane-modified nano TiO 2 The particles are as follows: in TiO 2 Adding 20-30wt% of perfluorodecyl trimethoxy silane aqueous solution into the particles, and then carrying out ultrasonic treatment for 10-20 min to obtain nano TiO 2 The modified solution is subjected to solid-liquid separation and drying treatment to obtain fluorosilane modified nano TiO 2 And (3) particles.
Further described, the fluorosilicone modified polyurethane resin is: firstly dehydrating polyethylene glycol at 120-200 ℃, then adding toluene diisocyanate and butyltin dilaurate, stirring to obtain isocyanate-terminated polyurethane prepolymer, then adding 20-30wt% of perfluorodecyl trimethoxysilane aqueous solution, trimethylolpropane and 1, 4-butanediol, and continuously stirring to obtain fluorosilicone modified polyurethane resin, wherein the stirring temperature is 70-80 ℃; wherein the mass ratio of polyethylene glycol, toluene diisocyanate, butyltin dilaurate, perfluorodecyl trimethoxy silane aqueous solution, trimethylolpropane and 1, 4-butanediol is 4-8:2.5-4.5:0.5-3:4-6:1-3:1.5-4.5.
Further described, the preparation method of the graphene anti-freezing coating with the superhydrophobic performance comprises the following steps:
(1) Grinding graphene, filler and sodium carboxymethyl cellulose. Adding deionized water and active epoxy resin to stir at a high speed, wherein the stirring speed is 800-1000 rpm, and the stirring temperature is 80-100 ℃ to obtain a mixed solution A;
(2) Modifying TiO with fluorine-silicon 2 Adding the nano particles into an ethanol aqueous solution, stirring and dispersing, then carrying out ultrasonic treatment for 30 min-1 h, and then adding the fluorosilicone modified polyurethane resin into the dispersion liquid for ultrasonic treatment for 20-30 min to obtain fluorosilicone modified polyurethane resin and nano titanium dioxide composite emulsion;
(3) Mixing the mixed solution A with the composite emulsion, then adding an antifreeze agent, an active diluent, a hydrophobic agent, a thixotropic agent and an emulsion defoamer at the same time for mechanical stirring, and then carrying out high-speed dispersion treatment, wherein the stirring speed is 270-350 rpm, and the stirring time is 30 min-1 h;
(4) And (3) after the step (1) to the step (3) are completed, taking out the graphene anti-freezing coating and placing the graphene anti-freezing coating in a cool and airtight space for cooling treatment, and after the temperature is reduced to 20-30 ℃, performing high-speed dispersion treatment to obtain the graphene anti-freezing coating with super-hydrophobic property.
Further, the high-speed dispersing and stirring speed in the step (4) is 2000-4000 rpm, and the dispersing time is 30 min-1 h.
Compared with the prior art, the invention has the technical effects that:
the graphene anti-freezing coating with the super-hydrophobic property has an excellent super-hydrophobic effect and an anti-freezing effect. The modified titanium dioxide nano material and polyurethane resin have the characteristics of super-hydrophobic surface, wear resistance and high flexibility, and the application performance of graphene and antifreeze is combined, so that the anti-freezing performance of the coating is further improved. The prepared coating has the comprehensive properties of difficult icing, low shearing force, wear-resistant surface and ageing-resistant surface when being applied to blades of wind turbines.
Detailed Description
In order to better understand the technical content of the present invention, the following provides specific examples to further illustrate the present invention.
The experimental methods used in the embodiment of the invention are conventional methods unless otherwise specified.
Materials, reagents, and the like used in the examples of the present invention are commercially available unless otherwise specified.
In the following examples and comparative examples, the reactive diluent, the anti-freeze agent, the hydrophobic agent, the thixotropic agent, and the emulsion type defoamer were selected from the group consisting of glycidyl neodecanoate, 15wt%1, 2-propanediol aqueous solution, polysiloxane, polyamide wax, and BYK-530, respectively.
Example 1
The graphene anti-freezing coating with the superhydrophobic performance comprises the following raw materials in parts by weight: 40 parts of active epoxy resin, 5 parts of graphene, 4 parts of active diluent, 5 parts of antifreeze agent, 1 part of hydrophobing agent, 5 parts of thixotropic agent, 2 parts of defoamer, 5 parts of filler, 2 parts of sodium carboxymethylcellulose and 30 parts of deionized water;
the filler is fluorosilicone modified nano TiO with the mass ratio of 1:1 2 Particles and fluorosilicone modified polyurethane resins.
The fluorine-silicon modified nano TiO 2 The method comprises the following steps: in TiO 2 Adding 20wt% of perfluorodecyl trimethoxy silane aqueous solution into the nano particles, and then carrying out ultrasonic treatment for 10-20 min to obtain nano TiO 2 The modified solution is subjected to solid-liquid separation and drying treatment, and the fluorine-silicon modified nano TiO is obtained 2 And (3) particles.
The fluorosilicone modified polyurethane resin is as follows: firstly dehydrating polyethylene glycol 2000 at 120 ℃, then adding toluene diisocyanate and butyltin dilaurate, stirring to obtain isocyanate-terminated polyurethane prepolymer, then adding 20wt% of perfluorodecyl trimethoxy silane aqueous solution, trimethylolpropane and 1, 4-butanediol, and continuously stirring to obtain fluorosilicone modified polyurethane resin, wherein the stirring temperature is 70 ℃; wherein the mass ratio of polyethylene glycol, toluene diisocyanate, butyltin dilaurate, perfluorodecyl trimethoxysilane aqueous solution, trimethylolpropane and 1, 4-butanediol is 4:2.5:0.5:4:1:1.5.
The preparation method of the graphene anti-freezing coating with the superhydrophobic performance comprises the following steps of:
(1) Grinding graphene, filler and sodium carboxymethyl cellulose, then adding deionized water and active epoxy resin, and stirring at a high speed of 900rpm and at a stirring temperature of 80 ℃ to obtain a mixed solution A;
(2) Modifying nano TiO with fluorine-silicon 2 Adding the particles into 45wt% ethanol water solution, stirring and dispersing, dispersing the dispersion, then performing ultrasonic treatment for 1h, and adding the fluorosilicone modified polyurethane resin into the dispersion for ultrasonic treatment for 30min to obtain fluorosilicone modified polyurethane resin and nano titanium dioxide composite emulsion;
(3) Mixing the mixed solution A with the composite emulsion, then simultaneously adding an antifreeze agent, an active diluent, a hydrophobic agent, a thixotropic agent and an emulsion type defoamer for mechanical stirring, and then carrying out high-speed dispersion treatment, wherein the stirring speed is 300rpm, and the stirring time is 1h;
(4) And (3) after the step (1) to the step (3) are completed, taking out the graphene anti-freezing coating, placing the graphene anti-freezing coating in a cool and airtight space, cooling the graphene anti-freezing coating, and performing high-speed dispersion treatment (the stirring speed is 2000rpm and the dispersion time is 20 min) after the temperature is reduced to 20 ℃ to obtain the graphene anti-freezing coating with super-hydrophobic property.
Example 2
The graphene anti-freezing coating with the superhydrophobic performance comprises the following raw materials in parts by weight: 45 parts of active epoxy resin, 8 parts of graphene, 6 parts of active diluent, 8 parts of antifreeze agent, 3 parts of hydrophobic agent, 3 parts of thixotropic agent, 4 parts of emulsion defoamer, 7 parts of filler, 3 parts of sodium carboxymethyl cellulose and 35 parts of deionized water;
the filler is fluorosilicone modified nano TiO with the mass ratio of 1:1 2 Particles and fluorine modified polyurethane resin.
The fluorine-silicon modified nano TiO 2 The particles are in TiO 2 Adding 25wt% of perfluoro decyl trimethoxy silane aqueous solution into the nano particles, and then carrying out ultrasonic treatment for 10-20 min to obtain nano TiO 2 The modified solution is subjected to solid-liquid separation and drying treatment, and the fluorosilane modified nano TiO is obtained 2 And (3) particles.
The fluorosilicone modified polyurethane resin is as follows: firstly dehydrating polyethylene glycol 2000 at 170 ℃, then adding toluene diisocyanate and butyltin dilaurate, stirring to obtain isocyanate-terminated polyurethane prepolymer, then adding 25wt% of perfluorodecyl trimethoxy silane aqueous solution, trimethylolpropane and 1, 4-butanediol, and continuously stirring to obtain fluorosilicone modified polyurethane resin, wherein the stirring temperature is 75 ℃; wherein the mass ratio of polyethylene glycol, toluene diisocyanate, butyltin dilaurate, perfluorodecyl trimethoxysilane aqueous solution, trimethylolpropane and 1, 4-butanediol is 6:3:2:5:2:3. The preparation method of the graphene anti-freezing coating with the superhydrophobic performance comprises the following steps of:
(1) Grinding graphene, filler and sodium carboxymethyl cellulose, then adding deionized water and active epoxy resin, and stirring at a high speed of 800rpm and at a stirring temperature of 80 ℃ to obtain a mixed solution A;
(2) Modifying nano TiO with fluorine-silicon 2 Adding the particles into 45wt% ethanol water solution, stirring and dispersing, then carrying out ultrasonic treatment for 1h, and adding the fluorosilicone modified polyurethane resin into the dispersion liquid for ultrasonic treatment for 30min to obtain the fluorosilicone modified polyurethane resin and nano titanium dioxide composite emulsion.
(3) Mixing the mixed solution A with the composite emulsion, then simultaneously adding an antifreeze agent, an active diluent, a hydrophobic agent, a thixotropic agent and an emulsion type defoamer for mechanical stirring, and then carrying out high-speed dispersion treatment, wherein the stirring speed is 300rpm, and the stirring time is 1h;
(4) And (3) after the step (1) to the step (3) are completed, taking out the graphene anti-freezing coating, placing the graphene anti-freezing coating in a cool and airtight space, cooling the graphene anti-freezing coating, and performing high-speed dispersion treatment (the stirring speed is 3000rpm and the dispersion time is 40 min) after the temperature is reduced to 25 ℃, thus obtaining the graphene anti-freezing coating with super-hydrophobic property.
Example 3
The graphene anti-freezing coating with the superhydrophobic performance comprises the following raw materials in parts by weight: 50 parts of active epoxy resin, 10 parts of graphene, 8 parts of active diluent, 10 parts of antifreeze agent, 5 parts of hydrophobic agent, 5 parts of thixotropic agent, 5 parts of emulsion defoamer, 10 parts of filler, 4 parts of sodium carboxymethyl cellulose and 40 parts of deionized water;
the filler is fluorine modified TiO with the mass ratio of 2:1 2 Nano-and fluorine-modified polyurethane resins.
The fluorine-silicon modified nano TiO 2 The particles are in TiO 2 Adding 30wt% of perfluoro decyl trimethoxy silane aqueous solution into the nano particles, and then carrying out ultrasonic treatment for 10-20 min to obtain nano TiO 2 The modified solution is subjected to solid-liquid separation and drying treatment, and the fluorine-silicon modified nano TiO is obtained 2 And (3) particles.
The fluorosilicone modified polyurethane resin is as follows: firstly dehydrating polyethylene glycol 2000 at 200 ℃, then adding toluene diisocyanate and butyltin dilaurate, stirring to obtain isocyanate-terminated polyurethane prepolymer, then adding 30wt% of perfluorodecyl trimethoxysilane aqueous solution, trimethylolpropane and 1, 4-butanediol, and continuously stirring to obtain fluorosilicone modified polyurethane resin, wherein the stirring temperature is 80 ℃; wherein the mass ratio of polyethylene glycol, toluene diisocyanate, butyltin dilaurate, perfluorodecyl trimethoxysilane aqueous solution, trimethylolpropane and 1, 4-butanediol is 8:4.5:3:6:3:4.5.
The preparation method of the graphene anti-freezing coating with the superhydrophobic performance comprises the following steps of:
(1) Grinding graphene, filler and sodium carboxymethyl cellulose, then adding deionized water and active epoxy resin, and stirring at a high speed of 1000rpm and a stirring temperature of 100 ℃ to obtain a mixed solution A;
(2) Modifying nano TiO with fluorine-silicon 2 Adding the particles into 45wt% ethanol water solution, stirring and dispersing, then carrying out ultrasonic treatment for 1h, and adding the fluorosilicone modified polyurethane resin into the dispersion liquid for ultrasonic treatment for 30min to obtain the fluorosilicone modified polyurethane resin and nano titanium dioxide composite emulsion.
(3) Mixing the mixed solution A with the composite emulsion, then simultaneously adding an antifreeze agent, an active diluent, a hydrophobic agent, a thixotropic agent and an emulsion type defoamer for mechanical stirring, and then carrying out high-speed dispersion treatment, wherein the stirring speed is 350rpm, and the stirring time is 1h;
(4) And (3) after the step (1) to the step (3) are completed, taking out the graphene anti-freezing coating, placing the graphene anti-freezing coating in a cool and airtight space, cooling the graphene anti-freezing coating, and performing high-speed dispersion treatment (the stirring speed is 4000rpm and the dispersion time is 1 h) after the temperature is reduced to 30 ℃ to obtain the graphene anti-freezing coating with super-hydrophobic property.
Comparative example 1
This comparative example differs from example 3 in that no nano-TiO is present in the filler 2 And modifying the polyurethane resin. The graphene anti-freezing coating with the super-hydrophobic performance comprises the following raw materials in parts by weight: 50 parts of active epoxy resin, 10 parts of graphene, 8 parts of active diluent, 10 parts of antifreeze agent, 5 parts of hydrophobic agent, 5 parts of thixotropic agent, 5 parts of emulsion defoamer, 10 parts of filler, 4 parts of sodium carboxymethyl cellulose and 40 parts of deionized water.
The preparation method of the graphene anti-freezing coating with the superhydrophobic performance comprises the following steps of:
(1) Grinding graphene, filler and sodium carboxymethyl cellulose, then adding deionized water and active epoxy resin, and stirring at a high speed of 1000rpm at a stirring temperature of 80-100 ℃ to obtain a mixed solution A;
(2) TiO is mixed with 2 Adding the nano particles into 45wt% ethanol water solution, stirring and dispersing, then carrying out ultrasonic treatment for 1h, and adding polyurethane resin into the dispersion liquid for ultrasonic treatment for 30min to obtain polyurethane resin and nano titanium dioxide composite emulsion;
(3) Mixing the mixed solution A with the composite emulsion, then simultaneously adding an antifreeze agent, an active diluent, a hydrophobic agent, a thixotropic agent and an emulsion type defoamer for mechanical stirring, and then carrying out high-speed dispersion treatment, wherein the stirring speed is 350rpm, and the stirring time is 1h;
(4) And (3) after the step (1) to the step (3) are completed, taking out the graphene anti-freezing coating, placing the graphene anti-freezing coating in a cool and airtight space, cooling the graphene anti-freezing coating, and performing high-speed dispersion treatment (the stirring speed is 4000rpm and the dispersion time is 1 h) after the temperature is reduced to 20-30 ℃ to obtain the graphene anti-freezing coating with super-hydrophobic property.
Comparative example 2
The difference between the comparative example and the example 2 is that no filler is added in the raw materials of the graphene anti-freezing coating with super-hydrophobic property, specifically a graphene anti-freezing coating with super-hydrophobic property, which comprises the following raw materials in parts by weight: 45 parts of active epoxy resin, 8 parts of graphene, 6 parts of active diluent, 3 parts of hydrophobic agent, 3 parts of thixotropic agent, 4 parts of emulsion defoamer, 3 parts of sodium carboxymethyl cellulose and 35 parts of deionized water;
the preparation method of the graphene anti-freezing coating with the superhydrophobic performance comprises the following steps of:
(1) Grinding graphene and sodium carboxymethyl cellulose, then adding deionized water and active epoxy resin, and stirring at a high speed, wherein the stirring speed is 800rpm, and the stirring temperature is 80 ℃ to obtain a mixed solution A;
(3) Adding an antifreeze agent, an active diluent, a hydrophobic agent, a thixotropic agent and an emulsion defoaming agent into the mixed solution A, mechanically stirring, and then performing high-speed dispersion treatment, wherein the stirring speed is 300rpm, and the stirring time is 1h;
(4) And (3) after the step (1) to the step (3) are completed, taking out the graphene anti-freezing coating, placing the graphene anti-freezing coating in a cool and airtight space, cooling the graphene anti-freezing coating, and performing high-speed dispersion treatment (the stirring speed is 3000rpm and the dispersion time is 40 min) after the temperature is reduced to 20-30 ℃.
Comparative example 3
The comparative example is different from example 2 in that only fluorosilicone modified nano TiO is added 2 The particles act as a filler. The graphene anti-freezing coating with the super-hydrophobic property comprises the following raw materials in parts by weight: 45 parts of active epoxy resin, 8 parts of graphene, 6 parts of active diluent, 8 parts of antifreeze agent, 3 parts of hydrophobic agent, 3 parts of thixotropic agent, 4 parts of emulsion defoamer, 7 parts of filler, 3 parts of sodium carboxymethyl cellulose and 35 parts of deionized water;
the filler is fluorine-silicon modified nano TiO 2 And (3) particles.
The fluorine-silicon modified nano TiO 2 The particles are in TiO 2 Adding 25wt% of perfluoro decyl trimethoxy silane aqueous solution into the nano particles, and then carrying out ultrasonic treatment for 10-20 min to obtain nano TiO 2 The modified solution is subjected to solid-liquid separation and drying treatment, and the fluorosilane modified nano TiO is obtained 2 And (3) particles.
The preparation method of the graphene anti-freezing coating with the superhydrophobic performance comprises the following steps of:
(1) Grinding graphene, filler and sodium carboxymethyl cellulose, then adding deionized water and active epoxy resin, and stirring at a high speed of 800rpm and at a stirring temperature of 80 ℃ to obtain a mixed solution A;
(2) Modifying nano TiO with fluorine-silicon 2 The particles are added into 45wt% ethanol water solution for stirring and dispersing, and then ultrasonic treatment is carried out for 1h, thus obtaining the nano titanium dioxide composite emulsion.
(3) Mixing the mixed solution A with the composite emulsion, then simultaneously adding an antifreeze agent, an active diluent, a hydrophobic agent, a thixotropic agent and an emulsion type defoamer for mechanical stirring, and then carrying out high-speed dispersion treatment, wherein the stirring speed is 300rpm, and the stirring time is 1h;
(4) And (3) after the step (1) to the step (3) are completed, taking out the graphene anti-freezing coating, placing the graphene anti-freezing coating in a cool and airtight space, cooling the graphene anti-freezing coating, and performing high-speed dispersion treatment (the stirring speed is 3000rpm and the dispersion time is 40 min) after the temperature is reduced to 25 ℃, thus obtaining the graphene anti-freezing coating with super-hydrophobic property.
Comparative example 4
This comparative example differs from example 2 in that only a fluorosilicone-modified polyurethane resin was added as a filler.
The graphene anti-freezing coating with the superhydrophobic performance comprises the following raw materials in parts by weight: 45 parts of active epoxy resin, 8 parts of graphene, 6 parts of active diluent, 8 parts of antifreeze agent, 3 parts of hydrophobic agent, 3 parts of thixotropic agent, 4 parts of emulsion defoamer, 7 parts of filler, 3 parts of sodium carboxymethyl cellulose and 35 parts of deionized water;
the filler is fluorine modified polyurethane resin.
The fluorosilicone modified polyurethane resin is as follows: firstly dehydrating polyethylene glycol 2000 at 170 ℃, then adding toluene diisocyanate and butyltin dilaurate, stirring to obtain isocyanate-terminated polyurethane prepolymer, then adding 25wt% of perfluorodecyl trimethoxy silane aqueous solution, trimethylolpropane and 1, 4-butanediol, and continuously stirring to obtain fluorosilicone modified polyurethane resin, wherein the stirring temperature is 75 ℃; wherein the mass ratio of polyethylene glycol, toluene diisocyanate, butyltin dilaurate, perfluorodecyl trimethoxysilane aqueous solution, trimethylolpropane and 1, 4-butanediol is 6:3:2:5:2:3.
The preparation method of the graphene anti-freezing coating with the superhydrophobic performance comprises the following steps of:
(1) Grinding graphene, filler and sodium carboxymethyl cellulose, then adding deionized water and active epoxy resin, and stirring at a high speed of 800rpm and at a stirring temperature of 80 ℃ to obtain a mixed solution A;
(2) Mixing and stirring the mixed solution A and the fluorosilicone modified polyurethane resin, then simultaneously adding an antifreeze agent, a reactive diluent, a hydrophobic agent, a thixotropic agent and an emulsion type defoaming agent for mechanical stirring, and then carrying out high-speed dispersion treatment, wherein the stirring speed is 300rpm, and the stirring time is 20min;
(3) And (3) after the step (1) to the step (2) are completed, taking out the graphene anti-freezing coating, placing the graphene anti-freezing coating in a cool and airtight space, cooling the graphene anti-freezing coating, and performing high-speed dispersion treatment (the stirring speed is 3000rpm and the dispersion time is 40 min) after the temperature is reduced to 25 ℃, thus obtaining the graphene anti-freezing coating with super-hydrophobic property.
Performance testing
The super-hydrophobic graphene anti-freezing coatings prepared in examples 1 to 3 and comparative examples 1 to 4 were subjected to hardness test (see GB/T6739-2006), paint film adhesion test (see GB/T5210-2006) and anti-freezing test.
Medium resistance test: salt spray resistance is measured according to GB 1763-1979 (1989) with reference to GB/T1771-2007 for acid resistance and alkali resistance.
Anti-freezing performance test: the coated samples were prepared with reference to GB-T1727-1992, then placed at-10deg.C for an anti-freeze test, each 15 days for a period, and the appearance (color change, chalking, cracking) of the coated samples was tested for 60 days.
Using an shanghai clostridian SL200B contact angle meter, 2 μl of clean deionized water was measured for contact angle on the example and comparative coating surfaces;
the test results were as follows:
experimental results show that the graphene anti-freezing coating with the superhydrophobic performance has good dielectric resistance and high adhesive force. As can be seen from comparison of example 3 with comparative examples 1 and 2, the modification of the nano titanium dioxide and polyurethane resin increases the adhesion of the coating, enhances the acid, alkali and salt resistance, and remarkably improves the contact angle.
According to the invention, the materials are selected to be scientifically proportioned, the filler with super-hydrophobic property and the antifreeze agent are prepared, and the unique functions of the graphene are combined, so that the coating of the coating achieves the effects of hydrophobicity, no ice hanging, freezing resistance and wear resistance. The product has long adaptation period and excellent construction performance, meets the anti-icing technical requirement of the wind turbine blades, provides technical support for the freezing climate test in the development process of wind power plants in the middle and south of China, and has very important practical significance.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. The graphene anti-freezing coating with the superhydrophobic performance is characterized in that: the material comprises the following raw materials in parts by weight: 40-50 parts of active epoxy resin, 5-10 parts of graphene, 4-8 parts of active diluent, 5-10 parts of antifreeze agent, 1-5 parts of hydrophobic agent, 1-5 parts of thixotropic agent, 2-5 parts of emulsion defoamer, 5-10 parts of filler, 2-4 parts of sodium carboxymethylcellulose and 30-40 parts of water.
2. The graphene anti-freezing coating with superhydrophobic performance as claimed in claim 1, wherein: the material comprises the following raw materials in parts by weight: 45 parts of active epoxy resin, 8 parts of graphene, 6 parts of active diluent, 8 parts of antifreeze agent, 3 parts of hydrophobic agent, 3 parts of thixotropic agent, 4 parts of emulsion defoamer, 7 parts of filler, 3 parts of sodium carboxymethyl cellulose and 35 parts of water.
3. The graphene anti-freezing coating with superhydrophobic performance as claimed in claim 1, wherein: the reactive diluent is one or more of glycidyl neodecanoate, beta-hydroxyethyl methacrylate or 1, 6-hexanediol diacrylate.
4. The graphene anti-freezing coating with superhydrophobic performance as claimed in claim 1, wherein: the antifreeze agent is 1, 2-propylene glycol aqueous solution or ethylene glycol aqueous solution; the hydrophobic agent is polysiloxane.
5. The graphene anti-freezing coating with superhydrophobic performance as claimed in claim 1, wherein: the thixotropic agent is polyamide wax.
6. The graphene anti-freezing coating with superhydrophobic performance as claimed in claim 1, wherein: the filler is fluorine-silicon modified nano TiO 2 Particles and fluorosilicone modified polyurethane resins.
7. The graphene anti-freezing coating with superhydrophobic performance as claimed in claim 1, wherein: the fluorine-silicon modified nano TiO 2 The particles are as follows: in TiO 2 Adding 20-30wt% of perfluorodecyl trimethoxy silane aqueous solution into the particles, and then carrying out ultrasonic treatment for 10-20 min to obtain nano TiO 2 The modified solution is subjected to solid-liquid separation and drying treatment, and the fluorine-silicon modified nano TiO is obtained 2 And (3) particles.
8. The graphene anti-freezing coating with super-hydrophobic performance as claimed in claim 7, wherein: the fluorosilicone modified polyurethane resin is as follows: firstly dehydrating polyethylene glycol at 120-200 ℃, then adding toluene diisocyanate and butyltin dilaurate, stirring to obtain isocyanate-terminated polyurethane prepolymer, then adding 20-30wt% of perfluorodecyl trimethoxysilane aqueous solution, trimethylolpropane and 1, 4-butanediol, and continuously stirring to obtain fluorosilicone modified polyurethane resin, wherein the stirring temperature is 70-80 ℃; wherein the mass ratio of polyethylene glycol, toluene diisocyanate, butyltin dilaurate, perfluorodecyl trimethoxy silane aqueous solution, trimethylolpropane and 1, 4-butanediol is 4-8:2.5-4.5:0.5-3:4-6:1-3:1.5-4.5.
9. The method for preparing the graphene anti-freezing coating with superhydrophobic performance according to any one of claims 1-8, which is characterized by comprising the following steps: the method comprises the following steps:
(1) Grinding graphene, filler and sodium carboxymethyl cellulose, then adding water and active epoxy resin, stirring at a high speed, wherein the stirring speed is 800-1000 rpm, and the stirring temperature is 80-100 ℃ to obtain a mixed solution A;
(2) Modifying nano TiO with fluorine-silicon 2 Adding the particles into ethanol water solution, stirring and dispersing, then carrying out ultrasonic treatment for 30-1 h, and then adding the fluorosilicone modified polyurethane resin into the dispersion liquid for ultrasonic treatment for 20-30 min to obtain the fluorosilicone modified polyurethane resin and nano titanium dioxide composite emulsion.
(3) Mixing the mixed solution A with the composite emulsion, then adding an antifreeze agent, an active diluent, a hydrophobic agent, a thixotropic agent and an emulsion defoamer at the same time for mechanical stirring, and then carrying out high-speed dispersion treatment, wherein the stirring speed is 270-350 rpm, and the stirring time is 30-60 min;
(4) And (3) cooling after the step (1) to the step (3), and performing high-speed dispersion treatment after the temperature is reduced to 20-30 ℃ to obtain the super-hydrophobic graphene anti-freezing coating.
10. The method for preparing the graphene anti-freezing coating with super-hydrophobic performance as claimed in claim 9, which is characterized by comprising the following steps: the high-speed dispersing and stirring speed of the step (4) is 2000-4000 rpm, and the dispersing time is 20-60 min.
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