CN116179045B - Fiber-reinforced water-based insulating paint and preparation method thereof - Google Patents
Fiber-reinforced water-based insulating paint and preparation method thereof Download PDFInfo
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- CN116179045B CN116179045B CN202211453128.4A CN202211453128A CN116179045B CN 116179045 B CN116179045 B CN 116179045B CN 202211453128 A CN202211453128 A CN 202211453128A CN 116179045 B CN116179045 B CN 116179045B
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- 239000003973 paint Substances 0.000 title claims abstract description 34
- 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 9
- 239000000835 fiber Substances 0.000 claims abstract description 54
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003063 flame retardant Substances 0.000 claims abstract description 20
- 239000003822 epoxy resin Substances 0.000 claims abstract description 17
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 239000006184 cosolvent Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000000945 filler Substances 0.000 claims abstract description 12
- 150000001412 amines Chemical class 0.000 claims abstract description 9
- 239000011858 nanopowder Substances 0.000 claims abstract description 8
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 30
- 239000010445 mica Substances 0.000 claims description 22
- 229910052618 mica group Inorganic materials 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 18
- 239000000839 emulsion Substances 0.000 claims description 17
- 208000012886 Vertigo Diseases 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 16
- 238000009987 spinning Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 241000779819 Syncarpia glomulifera Species 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000001739 pinus spp. Substances 0.000 claims description 12
- 229940036248 turpentine Drugs 0.000 claims description 12
- 238000010041 electrostatic spinning Methods 0.000 claims description 10
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 8
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 239000003093 cationic surfactant Substances 0.000 claims description 4
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 3
- QXONIHMUSQFKJU-UHFFFAOYSA-N 2-(prop-1-enoxymethyl)oxirane Chemical group CC=COCC1CO1 QXONIHMUSQFKJU-UHFFFAOYSA-N 0.000 claims description 3
- UUODQIKUTGWMPT-UHFFFAOYSA-N 2-fluoro-5-(trifluoromethyl)pyridine Chemical compound FC1=CC=C(C(F)(F)F)C=N1 UUODQIKUTGWMPT-UHFFFAOYSA-N 0.000 claims description 3
- 241000790917 Dioxys <bee> Species 0.000 claims description 3
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000011550 stock solution Substances 0.000 claims description 3
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 229910021487 silica fume Inorganic materials 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 239000002131 composite material Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 description 21
- 239000011248 coating agent Substances 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 239000002121 nanofiber Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000013530 defoamer Substances 0.000 description 5
- 230000003137 locomotive effect Effects 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- CNPURSDMOWDNOQ-UHFFFAOYSA-N 4-methoxy-7h-pyrrolo[2,3-d]pyrimidin-2-amine Chemical compound COC1=NC(N)=NC2=C1C=CN2 CNPURSDMOWDNOQ-UHFFFAOYSA-N 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 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
- 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
- C09D7/20—Diluents or solvents
-
- 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
-
- 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
Landscapes
- 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)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention relates to a fiber reinforced water-based insulating paint and a preparation method thereof, belonging to the technical field of insulating paint. The composite material comprises a component A and a component B, wherein the component A comprises the following components in percentage by weight: aqueous epoxy resin: 45-55%, 20-30% of nano insulating fiber, 3-10% of filler, 6-10% of flame-retardant nano powder, 1-2% of flame-retardant liquid, 0.3-0.5% of aqueous dispersing agent and aqueous defoaming agent: 0.5-1%, reactive monomer: 3-5%, cosolvent: 2-5% of amine neutralizer: 0.3-0.8%; the component B is a waterborne epoxy resin curing agent; the weight ratio of the component A to the component B is 2-5:1. the withstand voltage can reach more than 50KV, the breakdown voltage can reach 8KV when the thickness is 0.1mm, and the electrical strength can reach more than 80 KV/mm.
Description
Technical Field
The invention relates to a fiber reinforced water-based insulating paint and a preparation method thereof, belonging to the technical field of insulating paint.
Background
With the rapid development of economy, the national requirements on environmental protection are higher and higher. In terms of coatings, "oil to water" has been essentially achieved in C1-C3 corrosive environments, but no complete water-borne is achieved for C4-C5 corrosive environments. Meanwhile, some functional coatings such as high-temperature paint, insulating paint and conductive paint still do not realize water-based, so that a plurality of difficult problems are difficult to solve. Aiming at the water-based insulating paint applied to locomotives, motor cars and high-speed rail locomotives, the breakdown voltage is required to be more than or equal to 43KV (3 mm thick), the electrical strength is required to be more than or equal to 12KV/mm, and meanwhile, the performances of tracking index, 45-degree angle combustion, harmful substances, fire resistance and the like are required, but for the water-based paint, bubbles are easy to generate in film formation, and when the bubble abnormality phenomenon exists in the coating, the breakdown voltage of the coating can be seriously influenced. Meanwhile, when the thickness of a paint film reaches more than 3mm, the problems of poor adhesive force, poor freezing cycle resistance, poor high temperature resistance, poor impact resistance, difficult removal of bubbles and the like can occur, and the quality and heat resistance of the surface insulating paint can be very important for the service efficiency of equipment and the service life of the equipment. Currently, there are several types of insulating paints widely used, including polyimides, silicones, inorganic insulating paints, and the like. With the increasing importance of energy and environmental problems in modern society, the insulating paint is developing towards water-based, high-solid, solvent-free and inorganic properties which are more suitable for the environmental requirements. The high-temperature-resistant inorganic insulating paint is increasingly valued by people because of the advantages of environmental protection, low cost, low carbon, high temperature resistance and the like, and the water-based inorganic insulating paint [1-4] is a development trend in the future.
However, since a large amount of inorganic filler is required in the water-based insulating paint, the problems of low adhesion and poor cold and heat cycle resistance of the coating are easy to occur, and how to maintain the stability of the coating while ensuring the insulating property of the paint is a problem to be solved by the adhesion.
Reference is made to:
[1] han Xu, chen Min preparation of high temperature resistant insulating coatings by sol-gel method [ J ]. University of Dai-Tex university journal of Industrial, 2008,27 (2): 137-139
[2] Zhou Jihua the national paint industry "twelve five" development planning concept and advice [ J ]. Chinese paint, 2010,25 (5): 1-4
[3] Li Guidong development of waterborne coatings [ J ]. Scientific forum, 2010,13 (2): 268-270
[4] Tang Linsheng, zhang Mei, zhang Shufen, et al, water paint research Instructions [ J ]. Modern chemical industry, 2003,23 (6): 14-17
Disclosure of Invention
The purpose of the invention is that: solves the problem of poor coating adhesion and weather resistance of the existing water-based insulating paint. The hollow nanofiber which is compounded with the insulating filler is adopted in the patent, so that the uniformity of the coating is ensured on one hand, and on the other hand, the strength of the coating is ensured due to the fibrous structure of the nanofiber, meanwhile, based on the middle-sized property, the polymer resin in the coating can be combined with the fiber in a gap and solidified, and the weather resistance of the coating is improved as a whole.
The technical proposal is as follows:
the fiber reinforced water-based insulating paint comprises an A component and a B component, wherein the A component comprises the following components in percentage by weight: aqueous epoxy resin: 45-55%, 20-30% of nano insulating fiber, 3-10% of filler, 6-10% of flame-retardant nano powder, 1-2% of flame-retardant liquid, 0.3-0.5% of aqueous dispersing agent and aqueous defoaming agent: 0.5-1%, reactive monomer: 3-5%, cosolvent: 2-5% of amine neutralizer: 0.3-0.8%; the component B is a waterborne epoxy resin curing agent; the weight ratio of the component A to the component B is 2-5:1.
the filler is silica micropowder.
The flame-retardant nano powder is one or two components of antimony trioxide or aluminum hydroxide.
The active monomer is propenyl glycidyl ether, phenyl glycidyl ether, dioxy ethylene glycol diglycidyl ether, resorcinol diglycidyl ether and the like.
The material of the nano insulating fiber is selected from one or a mixture of a plurality of mica powder, magnesium oxide, aluminum oxide and barium titanate.
The preparation method of the nano insulating fiber comprises the following steps:
step 1, grinding the mica powder, and mixing the mica powder with polyvinylpyrrolidone, a cationic surfactant, a pH regulator and a solvent according to the weight ratio of 1:1.5-3:0.05-0.1:0.2-0.4:5-10, adding an oil phase solution, wherein the weight of the oil phase solution is 1/4-1/3 of that of the solvent, and stirring at a high speed to obtain emulsion;
and 2, carrying out spinning treatment on the obtained emulsion through an electrostatic spinning method, calcining the obtained fiber, and carrying out grinding treatment to obtain the nano insulating fiber.
The cationic surfactant is one or a mixture of more of dodecyl dimethyl benzyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride.
The solvent is a mixture of ethanol and water, and the oil phase solution is one or a mixture of turpentine and naphtha.
The high-speed stirring is carried out at 500-1000rpm for 3-6h.
In the process of the electrostatic spinning method, the voltage is 10-30kV, the flow rate of the spinning solution is 0.5-1.5mL/h, and the distance between the needle tip and the receiving plate is 10-20cm.
The calcination process is carried out at 350-550 ℃ for 2-5h.
The preparation method of the fiber reinforced water-based insulating paint comprises the following steps:
s1, adding aqueous epoxy resin, aqueous dispersing agent, aqueous defoaming agent, active monomer and cosolvent into a production cylinder, and stirring for 5 minutes at 300-400 rpm;
s2, slowly adding an amine neutralizer while stirring, adjusting the pH value to 8.5-9.5, and stirring for 5-10 minutes at 300-400 rpm;
s3, slowly adding the nano insulating fiber, the filler and the flame-retardant nano powder while stirring, and stirring for 30-40 minutes at 800-1000 rpm;
s4, slowly adding the flame retardant liquid while stirring, and stirring for 10-15 minutes at 400-600 rpm;
s5, directly adopting the curing agent to supply the stock solution for packaging.
Advantageous effects
The insulating material can be applied to the 5-kilovolt high-voltage resistant technology and is prepared from a water-based epoxy resin system, a nanofiber insulating filler, a water-based functional material, a water-based additive and the like. The water-soluble insulating paint adopted in the invention is reinforced by adopting the nanofiber, and the nanofiber is prepared by insulating filler, has a hollow structure, so that on one hand, the strength of a coating can be improved, and on the other hand, the porous fiber can contain a resin polymer, after a cured coating is formed, good bonding property can be maintained under high-low temperature circulation, and peeling and foaming are not easy to occur.
The withstand voltage can reach more than 50KV, the breakdown voltage can reach 8KV when the thickness is 0.1mm, and the electrical strength can reach more than 80 KV/mm. The insulating material is widely applied to locomotive, motor train and high-speed rail train heads, and achieves the insulating effect.
Drawings
FIG. 1 is an SEM photograph of the prepared nanofibers;
fig. 2 is an enlarged cross-sectional view of the nanofiber.
Detailed Description
The main raw materials used in the following examples include:
water-based epoxy resin (6075 tin-free Hong Hui)
Water dispersant (4599S Elfukona)
Water-based antifoaming agent (900 Di Gao)
Nanometer insulating fiber (self-made)
Silica fume (1500 mesh Lianyuangang Ruiyuan)
Antimony trioxide (Chengdu Xin Zhi)
Aluminum hydroxide (Chengdu Xin industry)
Flame retardant liquid (S-13-A Shandong fire-fighting with rain)
Reactive monomers (propenyl glycidyl ether, phenyl glycidyl ether, dioxy ethylene glycol diglycidyl ether, resorcinol diglycidyl ether, etc.)
Amine neutralizer (AMP 95 Guangzhou Hengyu chemical industry)
Cosolvent (alcohol, ether solvent)
Water-based epoxy hardener (7013 tin-free Hong Hui)
Example 1
The following weight proportions are adopted:
| example 1 | |
| Water-based epoxy resin | 45.7 |
| Nano insulating fiber | 30 |
| Silica micropowder | 3 |
| Antimony trioxide | 3 |
| Aluminum hydroxide | 5 |
| Flame-retardant liquid | 2 |
| Aqueous dispersant | 0.5 |
| Aqueous defoamer | 0.5 |
| Reactive monomers | 5 |
| Cosolvent | 5 |
| Amine neutralizer | 0.3 |
| Totalizing | 100 |
The nano insulating fiber is prepared by the following steps:
step 1, grinding mica powder, and mixing the mica powder with polyvinylpyrrolidone, dodecyl dimethyl benzyl ammonium chloride, a pH regulator and a solvent (75% ethanol) according to a weight ratio of 1:1.5:0.1:0.2:10, adding turpentine, stirring for 3-6h at 1000rpm to obtain emulsion, wherein the weight of turpentine is 1/4 of that of the solvent;
and 2, carrying out spinning treatment on the obtained emulsion by an electrostatic spinning method, wherein the voltage is 30kV, the flow rate of a spinning solution is 1.5mL/h, the distance between a needle point and a receiving plate is 10cm, and carrying out grinding treatment after calcining the obtained fiber for 2 hours at 550 ℃ to obtain the nano insulating fiber.
Example 2
The following weight proportions are adopted:
the nano insulating fiber is prepared by the following steps:
step 1, grinding mica powder, and mixing the mica powder with polyvinylpyrrolidone, dodecyl dimethyl benzyl ammonium chloride, a pH regulator and a solvent (75% ethanol) according to a weight ratio of 1:3:0.05:0.4:5, mixing, adding turpentine, stirring for 3 hours at a rotating speed of 500rpm, wherein the weight of turpentine is 1/3 of that of the solvent, and obtaining emulsion;
and 2, carrying out spinning treatment on the obtained emulsion by an electrostatic spinning method, wherein the voltage is 30kV, the flow rate of a spinning solution is 1.5mL/h, the distance between a needle point and a receiving plate is 20cm, and carrying out grinding treatment after calcining the obtained fiber for 4 hours at 350 ℃ to obtain the nano insulating fiber.
Example 3
The following weight proportions are adopted:
| example 1 | |
| Water-based epoxy resin | 55.9 |
| Nano insulating fiber | 20 |
| Silica micropowder | 10 |
| Antimony trioxide | 3 |
| Aluminum hydroxide | 3 |
| Flame-retardant liquid | 1 |
| Aqueous dispersant | 0.3 |
| Aqueous defoamer | 1 |
| Reactive monomers | 3 |
| Cosolvent | 2 |
| Amine neutralizer | 0.8 |
| Totalizing | 100 |
The nano insulating fiber is prepared by the following steps:
step 1, grinding mica powder, and mixing the mica powder with polyvinylpyrrolidone, dodecyl dimethyl benzyl ammonium chloride, a pH regulator and a solvent according to the weight ratio of 1:2:0.06:0.3:60, adding turpentine, stirring for 4 hours at a speed of 700rpm, wherein the weight of turpentine is 1/4 of that of the solvent, and obtaining emulsion;
and 2, carrying out spinning treatment on the obtained emulsion by an electrostatic spinning method, wherein the voltage is 20kV, the flow rate of a spinning solution is 1mL/h, the distance between a needle point and a receiving plate is 15cm, and carrying out grinding treatment after calcining the obtained fiber for 4 hours at 450 ℃ to obtain the nano insulating fiber.
Example 4
The following weight proportions are adopted:
| example 1 | |
| Water-based epoxy resin | 45.7 |
| Nano insulating fiber | 30 |
| Silica micropowder | 3 |
| Antimony trioxide | 3 |
| Aluminum hydroxide | 5 |
| Flame-retardant liquid | 2 |
| Aqueous dispersant | 0.5 |
| Aqueous defoamer | 0.5 |
| Reactive monomers | 5 |
| Cosolvent | 5 |
| Amine neutralizer | 0.3 |
| Totalizing | 100 |
The nano insulating fiber is prepared by the following steps:
step 1, grinding mica powder, and mixing the mica powder with polyvinylpyrrolidone, dodecyl dimethyl benzyl ammonium chloride, a pH regulator and a solvent (75% ethanol) according to a weight ratio of 1:2.5:0.08:0.25:6, mixing, adding turpentine, stirring for 5 hours at 600rpm, wherein the weight of turpentine is 1/4 of that of the solvent, and obtaining emulsion;
and 2, carrying out spinning treatment on the obtained emulsion by an electrostatic spinning method, wherein the voltage is 25kV, the flow rate of a spinning solution is 1.2mL/h, the distance between a needle point and a receiving plate is 12cm, and carrying out grinding treatment after calcining the obtained fiber for 3 hours at 450 ℃ to obtain the nano insulating fiber.
Example 5
The following weight proportions are adopted:
the nano insulating fiber is prepared by the following steps:
step 1, grinding mica powder, and mixing the mica powder with polyvinylpyrrolidone, dodecyl dimethyl benzyl ammonium chloride, a pH regulator and a solvent (75% ethanol) according to a weight ratio of 1:3:0.1:0.4:5, mixing, adding turpentine, stirring for 3 hours at 1000rpm, wherein the weight of turpentine is 1/3 of that of the solvent, and obtaining emulsion;
and 2, carrying out spinning treatment on the obtained emulsion by an electrostatic spinning method, wherein the voltage is 10-30kV, the flow rate of a spinning solution is 1.5mL/h, the distance between a needle point and a receiving plate is 20cm, and carrying out grinding treatment after calcining the obtained fiber for 3 hours at 550 ℃ to obtain the nano insulating fiber.
Comparative example 1
The difference from example 5 is that: and (3) performing dispersion molding of emulsion particles without adding an oil phase solution to prepare the nanofiber with the solid structure.
The following weight proportions are adopted:
| example 1 | |
| Water-based epoxy resin | 55.9 |
| Nano insulating fiber | 20 |
| Silica micropowder | 10 |
| Antimony trioxide | 3 |
| Aluminum hydroxide | 3 |
| Flame-retardant liquid | 1 |
| Aqueous dispersant | 0.3 |
| Aqueous defoamer | 1 |
| Reactive monomers | 3 |
| Cosolvent | 2 |
| Amine neutralizer | 0.8 |
| Totalizing | 100 |
The nano insulating fiber is prepared by the following steps:
step 1, grinding mica powder, and mixing the mica powder with polyvinylpyrrolidone, dodecyl dimethyl benzyl ammonium chloride, a pH regulator and a solvent (75% ethanol) according to a weight ratio of 1:3:0.1:0.4:5, mixing, and stirring for 3 hours at a rotating speed of 1000rpm to obtain a dispersion liquid;
and 2, carrying out spinning treatment on the obtained dispersion liquid by an electrostatic spinning method, wherein the voltage is 10-30kV, the flow rate of the spinning liquid is 1.5mL/h, the distance between a needle point and a receiving plate is 20cm, and carrying out grinding treatment after calcining the obtained fiber for 3 hours at 550 ℃ to obtain the nano insulating fiber.
Comparative example 2
The difference from example 5 is that: the nano insulating fiber is replaced by mica powder with the same weight.
The following weight proportions are adopted:
| example 1 | |
| Water-based epoxy resin | 55.9 |
| Mica powder | 20 |
| Silica micropowder | 10 |
| Antimony trioxide | 3 |
| Aluminum hydroxide | 3 |
| Flame-retardant liquid | 1 |
| Aqueous dispersant | 0.3 |
| Aqueous defoamer | 1 |
| Reactive monomers | 3 |
| Cosolvent | 2 |
| Amine neutralizer | 0.8 |
| Totalizing | 100 |
The preparation method of the coating A component in the above examples and comparative examples is as follows:
s1, adding aqueous epoxy resin, aqueous dispersing agent, aqueous defoaming agent, active monomer and cosolvent into a production cylinder, and stirring for 5 minutes at 300-400 rpm;
s2, slowly adding an amine neutralizer while stirring, adjusting the pH value to 8.5-9.5, and stirring for 5-10 minutes at 300-400 rpm;
3. slowly adding the nano insulating fiber (mica powder in comparative example 2), the filler and the flame-retardant nano powder while stirring, and stirring for 30-40 minutes at 800-1000 rpm;
4. the flame retardant liquid is slowly added while stirring, and stirring is carried out for 10-15 minutes at 400-600 rpm.
5. The component B of the curing agent is directly packaged by adopting the curing agent to supply stock solution.
Dry plate implementation: because the area of the top surface of the locomotive, the motor car and the high-speed rail locomotive is 8.5-10 square meters, the construction technology is generally adopted for quick construction. Component A: b=4: 1, after being uniformly mixed, the casting construction can be carried out, when physical property detection is needed, 20% deionized water can be added for dilution, the mixture is sprayed on a tinplate or a sand-spraying plate, the thickness is controlled between 20 and 100 microns, the physical property is detected, a physical property dry plate is placed in a constant temperature oven at 25 ℃ for self-drying for 48 hours, the conventional performance is detected, and breakdown voltage, electric strength and chemical resistance are tested after curing for 7 d. The irrigation thickness is 1mm, 2mm and 3mm respectively.
Examples 1 to 5 dry plate Properties
Note 1: high and low temperature resistant cyclic alternating test conditions: 80+/-2 ℃, 95% RH for 4 hours, 80 ℃ to-40 ℃ for 2 hours (the temperature changing speed is 1 ℃/min), 40+/-2 ℃ for 4 hours, 40 ℃ to 80 ℃ and 95% RH for 2 hours (the temperature changing speed is 1 ℃/min), 12 hours are a period, and a sample plate is placed for more than 16 hours at room temperature after the 60-period test is completed and then is tested; x-cut tests were carried out at coating thicknesses > 300. Mu.m.
It can be seen from examples 1 to 5 that the addition amount of the electronic grade mica powder is in a direct proportion relation with the breakdown voltage of the coating, but the breakdown voltage of the sheet in example 5 is increased to 11KV from 0.1mm along with the non-absolute change of the ratio of the electronic grade mica powder to the resin, and the electrical strength reaches 140KG/mm. When the thickness reaches 2mm, the breakdown voltage reaches 47KV, and when the thickness reaches 3mm, the breakdown voltage reaches 58KV, so that the 43KV breakdown voltage requirement of the middle vehicle is completely met. As can be seen from the comparison between the example 5 and the comparative example 1, by using the oil phase emulsion in the process of preparing the nanofiber by the electrospinning method, dispersed emulsion particles can be formed in the fiber, porous morphology can be formed on the surface of the fiber after calcination, the porous morphology can allow the water-based resin to permeate, the binding force between the fiber and the polymer is improved, and the stability of the coating can be improved after the cold and hot circulation test is performed; meanwhile, as can be seen from comparison of the embodiment 5 and the comparative example 2, the nanofiber adopted in the patent is used as the conductive filler, the physical strength and the binding force of the coating can be improved through the fiber morphology, and the effect of the nanofiber applied to the coating is better than that of the nanofiber directly adopting the powdered insulating filler.
Claims (7)
1. The fiber reinforced water-based insulating paint comprises a component A and a component B, and is characterized in that the component A comprises the following components in percentage by weight: aqueous epoxy resin: 45-55%, 20-30% of nano insulating fiber, 3-10% of filler, 6-10% of flame-retardant nano powder, 1-2% of flame-retardant liquid, 0.3-0.5% of aqueous dispersing agent, 0.5-1% of aqueous defoaming agent, 3-5% of active monomer, 2-5% of cosolvent and 0.3-0.8% of amine neutralizer; the component B is a waterborne epoxy resin curing agent; the weight ratio of the component A to the component B is 2-5:1, a step of;
the preparation method of the nano insulating fiber comprises the following steps:
step 1, grinding the mica powder, and mixing the mica powder with polyvinylpyrrolidone, a cationic surfactant, a pH regulator and a solvent according to the weight ratio of 1:1.5-3:0.05-0.1:0.2-0.4:5-10, adding an oil phase solution, wherein the weight of the oil phase solution is 1/4-1/3 of the weight of a solvent, and stirring at a high speed to obtain emulsion, the solvent is a mixture of ethanol and water, and the oil phase solution is one or two of turpentine or naphtha;
and 2, carrying out spinning treatment on the obtained emulsion through an electrostatic spinning method, calcining the obtained fiber, and carrying out grinding treatment to obtain the nano insulating fiber.
2. The fiber reinforced aqueous insulating paint of claim 1, wherein the filler is silica fume.
3. The fiber reinforced aqueous insulating paint according to claim 1, wherein the flame retardant nano powder is one or both of antimony trioxide or aluminum hydroxide.
4. The fiber reinforced aqueous insulating paint according to claim 1, wherein the reactive monomer is propenyl glycidyl ether, phenyl glycidyl ether, dioxy ethylene glycol diglycidyl ether or resorcinol diglycidyl ether.
5. The fiber reinforced aqueous insulating paint according to claim 1, wherein the cationic surfactant is selected from one or more of dodecyl dimethyl benzyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride.
6. The fiber reinforced aqueous insulating paint according to claim 1, wherein the high-speed stirring is stirring at 500-1000rpm for 3-6 hours;
in the electrostatic spinning process, the voltage is 10-30kV, the flow rate of the spinning solution is 0.5-1.5mL/h, and the distance between the needle tip and the receiving plate is 10-20cm;
the calcination refers to calcination at 350-550 ℃ for 2-5h.
7. The method for preparing the fiber reinforced aqueous insulating paint as claimed in claim 1, comprising the steps of:
s1, adding aqueous epoxy resin, aqueous dispersing agent, aqueous defoaming agent, active monomer and cosolvent into a production cylinder, and stirring for 5 minutes at 300-400 rpm;
s2, slowly adding an amine neutralizer while stirring, adjusting the pH value to 8.5-9.5, and stirring for 5-10 minutes at 300-400 rpm;
s3, slowly adding the nano insulating fiber, the filler and the flame-retardant nano powder while stirring, and stirring for 30-40 minutes at 800-1000 rpm;
s4, slowly adding the flame retardant liquid while stirring, and stirring for 10-15 minutes at 400-600 rpm;
s5, directly adopting the aqueous epoxy resin curing agent to supply the stock solution for packaging.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112094561B (en) * | 2019-06-17 | 2022-01-04 | Ppg工业俄亥俄公司 | Insulating coating composition |
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| GB750137A (en) * | 1952-09-30 | 1956-06-13 | Pearl Varnish Company Ltd | Improvements in or relating to coating compositions |
| JP2006124633A (en) * | 2004-09-29 | 2006-05-18 | Toto Ltd | Dispersion and coating |
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