CN116554784A - Epoxy modified methylphenyl organic silicon aerogel heat insulation coating and preparation method thereof - Google Patents
Epoxy modified methylphenyl organic silicon aerogel heat insulation coating and preparation method thereof Download PDFInfo
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- CN116554784A CN116554784A CN202210978817.0A CN202210978817A CN116554784A CN 116554784 A CN116554784 A CN 116554784A CN 202210978817 A CN202210978817 A CN 202210978817A CN 116554784 A CN116554784 A CN 116554784A
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- aerogel
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- 239000004964 aerogel Substances 0.000 title claims abstract description 129
- 238000009413 insulation Methods 0.000 title claims abstract description 57
- 239000011248 coating agent Substances 0.000 title claims abstract description 44
- 238000000576 coating method Methods 0.000 title claims abstract description 44
- 239000004593 Epoxy Substances 0.000 title claims abstract description 39
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 37
- 239000010703 silicon Substances 0.000 title claims abstract description 37
- 125000003944 tolyl group Chemical group 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 68
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 39
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
- 229920005989 resin Polymers 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 18
- 239000004005 microsphere Substances 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 229920003180 amino resin Polymers 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 239000011324 bead Substances 0.000 claims abstract description 13
- 239000011521 glass Substances 0.000 claims abstract description 13
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 11
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 6
- 239000010445 mica Substances 0.000 claims abstract description 5
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 27
- 238000000227 grinding Methods 0.000 claims description 26
- 239000011259 mixed solution Substances 0.000 claims description 26
- 239000002904 solvent Substances 0.000 claims description 21
- 239000002002 slurry Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 13
- 230000002209 hydrophobic effect Effects 0.000 claims description 12
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000003607 modifier Substances 0.000 claims description 11
- 230000004048 modification Effects 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- 239000004965 Silica aerogel Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000000413 hydrolysate Substances 0.000 claims description 7
- 230000007062 hydrolysis Effects 0.000 claims description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000001694 spray drying Methods 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 230000003449 preventive effect Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 6
- 230000001070 adhesive effect Effects 0.000 abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000013530 defoamer Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000003973 paint Substances 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 230000002528 anti-freeze Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- -1 polysiloxanes Polymers 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000005051 trimethylchlorosilane Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- MHKBSCHWKVCLJL-WUKNDPDISA-N (e)-octadec-2-enamide Chemical compound CCCCCCCCCCCCCCC\C=C\C(N)=O MHKBSCHWKVCLJL-WUKNDPDISA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229920003274 CYMEL® 303 LF Polymers 0.000 description 1
- 229920003275 CYMEL® 325 Polymers 0.000 description 1
- 229920003270 Cymel® Polymers 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- SFEWMGIPBBLNJX-KTKRTIGZSA-N amino (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)ON SFEWMGIPBBLNJX-KTKRTIGZSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001649 bromium compounds Chemical class 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000011490 mineral wool Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
- Paints Or Removers (AREA)
Abstract
The invention provides an epoxy modified methylphenyl organic silicon aerogel heat-insulating coating and a preparation method thereof. The epoxy modified methylphenyl organic silicon aerogel heat insulation coating is mainly prepared from the following raw materials: 20-58 parts of epoxy modified methylphenyl organic silicon resin, 2-6 parts of amino resin, 5-20 parts of aerogel composite heat insulation powder, 2-10 parts of modified aerogel, 1-10 parts of hollow glass beads, 1-5 parts of mica powder, 10-20 parts of water, 0.1-2 parts of dispersing agent, 0.1-1 part of defoaming agent, 0.1-1 part of leveling agent, 1-3 parts of silane coupling agent, 0.1-2 parts of antifreezing agent, 0.1-0.5 part of water retention agent and 0.1-0.5 part of antibacterial agent, wherein the inner layer structure of the aerogel composite heat insulation powder is that pressure-resistant silica hollow nano microspheres are filled in aerogel holes. The prepared epoxy modified methylphenyl organic silicon aerogel heat-insulating coating fully exerts the heat-insulating property of the aerogel, so that the heat-insulating property, heat resistance and adhesive force of the aerogel are good.
Description
Technical Field
The invention relates to the technical field of high-temperature resistance and heat insulation of energy chemical equipment, in particular to an epoxy modified methylphenyl modified organic silicon aerogel heat insulation coating and a preparation method thereof.
Background
The energy and chemical industry has important strategic significance for the country, and under the drive of 'double carbon', the reduction of carbon emission is urgent for the energy and chemical industry. The energy waste problem of high-temperature equipment and high-temperature pipelines in the energy chemical industry is serious, and the energy waste can be effectively reduced by adopting the heat insulation material, so that the purposes of energy conservation and carbon reduction are achieved. The heat preservation and insulation materials commonly used at present mainly comprise: glass wool, expanded perlite, aerogel blanket, micro-nano insulation board, rock wool and some organic foam boards. However, most of these materials are applied to regular parts of the equipment, and the special-shaped parts cannot be fully covered by the materials.
The paint has the characteristics of easy construction and capability of coating special-shaped pieces. At present, although the energy and chemical industry has related reports of heat insulation through a coating, the effect is not ideal, mainly because the properties of corrosion resistance, adhesive force, high temperature resistance, heat insulation and thermal shock resistance cannot be considered. The inorganic film forming material has good high temperature resistance, but has poor cold and hot shock resistance. The organic silicon resin in the organic film forming material has certain high temperature resistance, but has poor adhesive force, and the service life of the prepared coating can be influenced by the poor adhesive force. Aerogels are the best heat insulating filler. However, the aerogel has large specific surface area and unstable nano-pore structure, and in a coating system, the problems of uneven dispersion, easy cracking, collapse of a porous structure and the like are easily caused, so that the related reports of the coating capable of exerting the heat insulation performance of the aerogel are very few at present. Because of the abundant pore structure, the heat conductivity coefficient of the aerogel is as low as 0.01W/(m.K), but when the pore structure is damaged, the heat conductivity coefficient is far more than 0.07W/(m.K), and the heat insulation performance is greatly reduced.
The resin is often applied to preparing the paint, the resin with different groups has different properties, and the prepared paint has a large performance difference. CN 102559048A discloses a preparation method of epoxy modified organosilicon insulating heat-conducting high-temperature-resistant coating and a product, and the insulating property is better due to the introduction of epoxy resin. CN101935498A uses silicone resin, modified silicone resin, epoxy resin, phenolic resin, amino resin, etc. to prepare the silicone anticorrosive paint, which has better adhesive force and corrosion resistance. CN104371506a is prepared by mixing resin and silica aerogel, and has the advantages of cathode stripping resistance and good adhesive force. However, since the existing studies use only resins to prepare the coating materials or simply use a combination of resins carrying different groups to prepare the coating materials, this causes the following problems: the high temperature resistance of the coating prepared in the step (1) is not excellent enough; (2) The mixing of different resins can increase the coating function, but simultaneously, due to the introduction of a plurality of resins, the resins are difficult to mix or have longer mixing time, and the production period is prolonged; (3) Although substances with better high temperature resistance such as aerogel are introduced to prepare the coating, the aerogel is not pretreated, so that the aerogel is difficult to disperse, aerogel holes are easily damaged in some coating systems, and the heat insulation performance of the coating is difficult to be exerted to a great extent.
Disclosure of Invention
The first aspect of the invention provides an epoxy modified methylphenyl organic silicon aerogel heat-insulating coating, which is mainly prepared from the following raw materials: 20-58 parts of epoxy modified methylphenyl organic silicon resin, 2-6 parts of amino resin, 5-20 parts of aerogel composite heat insulation powder, 2-10 parts of modified aerogel, 1-10 parts of hollow glass beads, 1-5 parts of mica powder, 10-20 parts of water, 0.1-2 parts of dispersing agent, 0.1-1 part of defoaming agent, 0.1-1 part of leveling agent, 1-3 parts of silane coupling agent, 0.1-2 parts of antifreezing agent, 0.1-0.5 part of water retention agent and 0.1-0.5 part of antibacterial agent, wherein the inner layer structure of the aerogel composite heat insulation powder is that pressure-resistant silica hollow nano microspheres are filled in aerogel holes.
The aerogel in the aerogel composite heat insulation powder is silica aerogel modified by a hydrophobic modifier containing methyl. Specifically, the methyl-containing hydrophobic modifier is one or a combination of more than two of Trimethylchlorosilane (TMCS), hexamethyldisilazane (HMDS) and Hexamethyldisiloxane (HMDSO).
The aerogel composite heat insulation powder comprises the following components in parts by weight: 60-80 parts of aerogel and 15-25 parts of pressure-resistant silica hollow nano-microspheres.
The addition amounts of the raw materials are respectively as follows: epoxy modified methyl phenyl organic silicon resin, amino resin, aerogel composite heat insulation powder, modified aerogel, hollow glass beads, mica powder, water, dispersing agent, defoaming agent, leveling agent, silane coupling agent, antifreezing agent, water-retaining agent and antibacterial agent.
In the invention, the epoxy modified methylphenyl organosilicon resin is SH-9607 of New four seas in Hubei province.
The amino resin is selected from but not limited to CYMEL 325, CYMEL 380, CYMEL 303LF;
the density of the hollow glass beads is in the range of but not limited to 0.15g/cm 3 ～0.6g/cm 3 ；
The particle size of the mica powder is but not limited to 500-5000 mesh;
the dispersant is selected from but not limited to sulfonate, octadecenamide acetate, polyethylene glycol type polyol, phosphate type high molecular polymer and oil amino oleate;
the defoamer is selected from, but not limited to, polysiloxanes, modified polysiloxanes, higher alcohols, polyether defoamers. The leveling agent is selected from, but not limited to, acrylic, silicone, fluorocarbon.
The silane coupling agent is selected from, but not limited to, 3-aminopropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, 3- (2, 3-glycidoxy) propyl trimethoxysilane, gamma- (methacryloyloxy) propyl trimethoxysilane.
The antifreeze is selected from, but not limited to, ethylene glycol, propylene glycol, urea, thiourea, and the like.
The water-retaining agent is selected from, but not limited to, starch, hydroxymethyl cellulose, polyvinyl alcohol, ethylene glycol, propylene glycol, and the like.
The antibacterial agent is selected from but not limited to organic bromides, organic amines, and guatriazines.
The second aspect of the invention provides a preparation method of an epoxy modified methylphenyl organic silicon aerogel heat-insulating coating, which comprises the following steps:
1) Weighing epoxy modified methylphenyl organic silicon resin, amino resin, dispersing agent and aerogel composite heat insulation powder, sequentially adding the epoxy modified methylphenyl organic silicon resin, the amino resin, the dispersing agent and the aerogel composite heat insulation powder into water, and grinding to obtain grinding slurry;
2) Sequentially adding glass beads, a defoaming agent, a leveling agent and a silane coupling agent into the grinding slurry obtained in the step 1), and uniformly stirring and mixing;
3) And (3) sequentially adding the modified aerogel, the antifreezing agent, the water-retaining agent and the mildew preventive into the uniformly mixed liquid in the step (2) and stirring to obtain the epoxy modified methylphenyl organic silicon aerogel heat-insulating coating.
The aerogel composite heat insulation powder in the step 1) is prepared by the following method:
(1) Adding tetraethyl orthosilicate, water, ethanol and hydrochloric acid for hydrolysis to obtain tetraethyl orthosilicate hydrolysate;
(2) Adding an alkali solution into the obtained mixed solution by rapid stirring to adjust the pH of the system, adding the pressure-resistant silica hollow nano-microspheres into the mixed solution, and curing to obtain composite gel;
(3) Crushing the solidified composite gel into small particles, and then placing the small particles in an ethanol solvent for solvent replacement;
(4) Then placing the composite gel subjected to solvent replacement in a hydrophobic modifier containing methyl for modification;
(5) Separating out the liquid, and drying the composite gel to obtain the aerogel composite heat insulation powder.
The grinding rotating speed in the step 1) is 3000r/min, and the fineness of the ground slurry is below 80 mu m.
The stirring speeds in the step 2) and the step 3) are 300r/min, and the stirring time is 1h and 20min respectively.
The modified aerogel in the step 3) is prepared by the following method:
step 1, adding 0.1-1 part of surfactant into 70-90 parts of water, and stirring to obtain a mixed solution;
step 2, adding 10-30 parts of hydrophobic modifier containing methyl into the mixed solution while stirring to modify the silica aerogel, and stirring at a high speed to obtain aerogel dispersion liquid;
and step 3, spray drying the aerogel dispersion liquid to obtain the modified aerogel.
Compared with the prior art, the invention introduces a resin with multiple groups and composite functions, and then prepares the coating by matching with some light heat insulation fillers and adding the treated aerogel, and has the beneficial effects that:
(1) The resin containing multiple groups such as epoxy groups and phenyl groups is used, so that the problem that the high temperature resistance and other performances of the coating are not excellent enough is solved, and the prepared coating has better high temperature resistance, adhesion and heat insulation performance;
(2) The resin is used, so that the problem that the paint is difficult to disperse in use due to uneven mixing of multiple resins is solved, the production period is shortened, the preparation efficiency is improved, the prepared paint has uniform performance, and the service life of the paint is prolonged;
(3) The aerogel is pretreated, methyl hydrophobic modification is carried out, the compatibility of the aerogel and a coating system is improved, the pressure-resistant hollow nano-microspheres are filled in the aerogel holes, the weight of the aerogel is increased, the aerogel can be easily dispersed in the system, the dispersing time is shortened, and the prepared coating has uniform performance and shorter period;
(4) The pressure-resistant silica hollow nano-spheres with relatively smaller heat conductivity are used for filling the aerogel holes, so that the aerogel holes can be supported, the problem of collapse of the aerogel holes is solved while the mechanical strength of the aerogel is improved, the problem that the heat insulation performance of the aerogel is difficult to exert due to larger structural damage of the aerogel is solved, and the prepared coating still has a heat insulation effect at a high temperature of 450 ℃.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
It should be noted that, without conflict, the embodiments of the present invention and features in the embodiments may be combined with each other, where the parts by mass of all components are not specifically described.
The invention will be further illustrated, but is not limited, by the following examples.
Example 1
(1) Preparing aerogel composite heat insulation powder:
1) The molar ratio is 1:4:14:10 -4 Adding tetraethyl orthosilicate, water, ethanol and hydrochloric acid for hydrolysis to obtain tetraethyl orthosilicate hydrolysate;
2) Adding an alkali solution into the obtained mixed solution by rapid stirring to adjust the pH of the system to 5, adding the pressure-resistant silica hollow nano-microspheres into the mixed solution, and curing to obtain composite gel;
3) Crushing the solidified composite gel into small particles, then placing the small particles in an ethanol solvent for solvent replacement, and repeating for 4 times;
4) Then placing the composite gel subjected to solvent replacement into an epoxy silane coupling agent with the mass 4 times of that of the composite gel for modification for 48 hours;
5) Separating out liquid, and then grading and drying the composite gel under nitrogen hot air to obtain aerogel composite heat insulation powder (80 parts of aerogel and 25 parts of pressure-resistant silica hollow nano microspheres).
(2) Preparation of modified aerogel:
step 1, adding 0.5 part of surfactant into 70 parts of water, and stirring to obtain a mixed solution A1;
step 2, adding 20 parts of hydrophobic modifier containing methyl into the mixed solution A1 while stirring to modify the silica aerogel, and stirring at a high speed to obtain aerogel dispersion liquid;
and step 3, spray drying the aerogel dispersion liquid to obtain the modified aerogel.
(3) An epoxy modified methylphenyl organic silicon aerogel heat insulation coating is coated on a 15cm x 7cm x 0.5cm steel plate substrate, and the preparation method comprises the following steps:
1) Sequentially adding 36 parts of epoxy modified methylphenyl organic silicon resin, 6 parts of amino resin, 2 parts of dispersing agent and 20 parts of aerogel composite heat insulation powder into 10 parts of water, and carrying out high-speed grinding for 3 hours at a speed of 3000r/min, wherein the fineness of grinding slurry is controlled below 80 mu m;
2) 10 parts of glass beads, 1 part of defoamer, 1 part of flatting agent and 2 parts of silane coupling agent are sequentially added into the grinding slurry obtained in the step 1), and the mixture is stirred for 1h at 300r/min and uniformly mixed.
3) 10 parts of modified aerogel, 1 part of antifreezing agent, 0.5 part of water-retaining agent and 0.5 part of antibacterial agent are sequentially added into the liquid uniformly mixed in the step 2), and the mixture is stirred for 20 minutes at 300r/min to prepare a sample plate.
Example 2
(1) Preparing aerogel composite heat insulation powder:
1) The molar ratio is 1:4:14:10 -4 Adding tetraethyl orthosilicate, water, ethanol and hydrochloric acid for hydrolysis to obtain tetraethyl orthosilicate hydrolysate;
2) Adding an alkali solution into the obtained mixed solution by rapid stirring to adjust the pH of the system to 5, adding 20 parts of pressure-resistant silica hollow nano-microspheres into the mixed solution, and curing to obtain composite gel;
3) Crushing the solidified composite gel into small particles, then placing the small particles in an ethanol solvent for solvent replacement, and repeating for 4 times;
4) Then placing the composite gel subjected to solvent replacement into an epoxy silane coupling agent with the mass 4 times of that of the composite gel for modification for 48 hours;
5) Separating out liquid, and then grading and drying the composite gel under nitrogen hot air to obtain aerogel composite heat insulation powder (80 parts of aerogel and 25 parts of pressure-resistant silica hollow nano microspheres).
(2) Preparation of modified aerogel:
step 1, adding 0.5 part of surfactant into 70 parts of water, and stirring to obtain a mixed solution A1;
step 2, adding 20 parts of hydrophobic modifier containing methyl into the mixed solution A1 while stirring to modify the silica aerogel, and stirring at a high speed to obtain aerogel dispersion liquid;
and step 3, spray drying the aerogel dispersion liquid to obtain the modified aerogel.
(3) An epoxy modified methylphenyl organic silicon aerogel heat insulation coating is coated on a 15cm x 7cm x 0.5cm steel plate substrate, and the preparation method comprises the following steps:
1) Sequentially adding 58 parts of epoxy modified methylphenyl organic silicon resin, 2 parts of amino resin, 1 part of dispersing agent and 5 parts of aerogel composite heat insulation powder into 10 parts of water, and carrying out high-speed grinding for 3 hours at a speed of 3000r/min, wherein the fineness of grinding slurry is controlled below 80 mu m;
2) Sequentially adding 10 parts of glass beads, 1 part of defoamer, 1 part of flatting agent and 3 parts of silane coupling agent into the grinding slurry obtained in the step 1), stirring for 1h at 300r/min, and uniformly mixing;
3) 7 parts of modified aerogel, 1 part of antifreezing agent, 0.5 part of water-retaining agent and 0.5 part of antibacterial agent are sequentially added into the liquid uniformly mixed in the step 2), and the mixture is stirred for 20 minutes at 300r/min to prepare a sample plate.
Example 3
(1) Preparing aerogel composite heat insulation powder:
1) The molar ratio is 1:4:14:10 -4 Adding tetraethyl orthosilicate, water, ethanol and hydrochloric acid for hydrolysis to obtain tetraethyl orthosilicate hydrolysate;
2) Adding an alkali solution into the obtained mixed solution by rapid stirring to adjust the pH of the system to 5, adding 20 parts of pressure-resistant silica hollow nano-microspheres into the mixed solution, and curing to obtain composite gel;
3) Crushing the solidified composite gel into small particles, then placing the small particles in an ethanol solvent for solvent replacement, and repeating for 4 times;
4) Then placing the composite gel subjected to solvent replacement into an epoxy silane coupling agent with the mass 4 times of that of the composite gel for modification for 48 hours;
5) Separating out liquid, and then grading and drying the composite gel under nitrogen hot air to obtain aerogel composite heat insulation powder (80 parts of aerogel and 25 parts of pressure-resistant silica hollow nano microspheres).
(2) Preparation of modified aerogel:
step 1, adding 0.5 part of surfactant into 90 parts of water, and stirring to obtain a mixed solution A1;
step 2, adding 20 parts of hydrophobic modifier containing methyl into the mixed solution A1 while stirring to modify the silica aerogel, and stirring at a high speed to obtain aerogel dispersion liquid;
and step 3, spray drying the aerogel dispersion liquid to obtain the modified aerogel.
(3) An epoxy modified methylphenyl organic silicon aerogel heat insulation coating is coated on a 15cm x 7cm x 0.5cm steel plate substrate, and the preparation method comprises the following steps:
1) Sequentially adding 58 parts of epoxy modified methylphenyl organic silicon resin, 2 parts of amino resin, 1 part of dispersing agent and 5 parts of aerogel composite heat insulation powder into 10 parts of water, and carrying out high-speed grinding for 3 hours at a speed of 3000r/min, wherein the fineness of grinding slurry is controlled below 80 mu m;
2) Sequentially adding 10 parts of glass beads, 1 part of defoamer, 1 part of flatting agent and 3 parts of silane coupling agent into the grinding slurry obtained in the step 1), stirring for 1h at 300r/min, and uniformly mixing;
3) 7 parts of modified aerogel, 1 part of antifreezing agent, 0.5 part of water-retaining agent and 0.5 part of antibacterial agent are sequentially added into the liquid uniformly mixed in the step 2), and the mixture is stirred for 20 minutes at 300r/min to prepare a sample plate.
Example 4
(1) Preparing aerogel composite heat insulation powder:
1) The molar ratio is 1:4:14:10 -4 Adding tetraethyl orthosilicate, water, ethanol and hydrochloric acid for hydrolysis to obtain tetraethyl orthosilicate hydrolysate;
2) Adding an alkali solution into the obtained mixed solution by rapid stirring to adjust the pH of the system to 5, adding 20 parts of pressure-resistant silica hollow nano-microspheres into the mixed solution, and curing to obtain composite gel;
3) Crushing the solidified composite gel into small particles, then placing the small particles in an ethanol solvent for solvent replacement, and repeating for 4 times;
4) Then placing the composite gel subjected to solvent replacement into an epoxy silane coupling agent with the mass 4 times of that of the composite gel for modification for 48 hours;
5) Separating out liquid, and then grading and drying the composite gel under nitrogen hot air to obtain aerogel composite heat insulation powder (60 parts of aerogel and 15 parts of pressure-resistant silica hollow nano microspheres).
(2) Preparation of modified aerogel:
step 1, adding 0.5 part of surfactant into 90 parts of water, and stirring to obtain a mixed solution A1;
step 2, adding 20 parts of hydrophobic modifier containing methyl into the mixed solution A1 while stirring to modify the silica aerogel, and stirring at a high speed to obtain aerogel dispersion liquid;
and step 3, spray drying the aerogel dispersion liquid to obtain the modified aerogel.
(3) An epoxy modified methylphenyl organic silicon aerogel heat insulation coating is coated on a 15cm x 7cm x 0.5cm steel plate substrate, and the preparation method comprises the following steps:
1) Sequentially adding 58 parts of epoxy modified methylphenyl organic silicon resin, 2 parts of amino resin, 1 part of dispersing agent and 5 parts of aerogel composite heat insulation powder into 10 parts of water, and carrying out high-speed grinding for 3 hours at a speed of 3000r/min, wherein the fineness of grinding slurry is controlled below 80 mu m;
2) Sequentially adding 10 parts of glass beads, 1 part of defoamer, 1 part of flatting agent and 3 parts of silane coupling agent into the grinding slurry obtained in the step 1), stirring for 1h at 300r/min, and uniformly mixing;
3) 7 parts of modified aerogel, 1 part of antifreezing agent, 0.5 part of water-retaining agent and 0.5 part of antibacterial agent are sequentially added into the liquid uniformly mixed in the step 2), and the mixture is stirred for 20 minutes at 300r/min to prepare a sample plate.
Comparative example 1
(1) Preparing aerogel composite heat insulation powder:
1) The molar ratio is 1:4:14:10 -4 Adding orthosilicic acidCarrying out hydrolysis on tetraethyl ester, water, ethanol and hydrochloric acid to obtain tetraethyl orthosilicate hydrolysate;
2) Adding an alkali solution into the obtained mixed solution by rapid stirring to adjust the pH of the system to 5, adding 20 parts of pressure-resistant silica hollow nano-microspheres into the mixed solution, and curing to obtain composite gel;
3) Crushing the solidified composite gel into small particles, then placing the small particles in an ethanol solvent for solvent replacement, and repeating for 4 times;
4) Then placing the composite gel subjected to solvent replacement into an epoxy silane coupling agent with the mass 4 times of that of the composite gel for modification for 48 hours;
5) Separating out liquid, and then grading and drying the composite gel under nitrogen hot air to obtain the aerogel composite heat insulation powder.
(2) The preparation method of the pure organosilicon aerogel heat insulation coating coated on a 15cm x 7cm x 0.5cm steel plate substrate comprises the following steps:
1) Sequentially adding 12 parts of pure organic silicon resin, 6 parts of amino resin, 12 parts of epoxy resin, 12 parts of phenyl-containing resin, 2 parts of dispersing agent and 20 parts of aerogel composite heat insulation powder into 10 parts of water, and carrying out high-speed grinding for 3 hours at 3000r/min (the resin is not uniformly mixed), wherein the fineness of the grinding slurry is controlled below 80 mu m;
2) Sequentially adding 10 parts of glass beads, 1 part of defoamer, 1 part of flatting agent and 2 parts of silane coupling agent into the grinding slurry obtained in the step 1), stirring for 1h at 300r/min, and uniformly mixing.
3) 10 parts of modified aerogel, 1 part of antifreezing agent, 0.5 part of water-retaining agent and 0.5 part of antibacterial agent are sequentially added into the liquid uniformly mixed in the step 2), and the mixture is stirred for 20 minutes at 300r/min to prepare a sample plate.
Comparative example 2
The preparation method of the mixed resin aerogel heat insulation coating coated on a 15cm x 7cm x 0.5cm steel plate substrate comprises the following steps:
1) Sequentially adding 58 parts of epoxy modified methylphenyl organic silicon resin, 2 parts of amino resin and 1 part of dispersing agent into 10 parts of water, and carrying out high-speed grinding for 3 hours at 3000r/min, wherein the fineness of the grinding slurry is controlled below 80 mu m;
2) Sequentially adding 10 parts of glass beads, 1 part of defoamer, 1 part of flatting agent and 3 parts of silane coupling agent into the grinding slurry obtained in the step 1), stirring for 1h at 300r/min, and uniformly mixing;
3) To the liquid uniformly mixed in 2), 12 parts of aerogel, 1 part of antifreeze, 0.5 part of water-retaining agent and 0.5 part of antibacterial agent are added in sequence, and the mixture is stirred for 20 minutes at 300r/min to prepare a sample plate.
The sample performance tests provided in the examples of the present invention and comparative examples 1-2 are shown in the following table:
as shown in the table above, the epoxy modified methylphenyl organic silicon aerogel heat-insulating coating provided by the invention has better high temperature resistance, adhesion, heat insulation and thermal shock resistance.
Claims (8)
1. The epoxy modified methylphenyl organic silicon aerogel heat-insulating coating is characterized by being mainly prepared from the following raw materials: 20-58 parts of epoxy modified methylphenyl organic silicon resin, 2-6 parts of amino resin, 5-20 parts of aerogel composite heat insulation powder, 2-10 parts of modified aerogel, 1-10 parts of hollow glass beads, 1-5 parts of mica powder, 10-20 parts of water, 0.1-1 part of dispersing agent, 0.1-1 part of defoaming agent, 0.1-1 part of leveling agent, 1-3 parts of silane coupling agent, 0.1-2 parts of antifreezing agent, 0.1-0.5 part of water retention agent and 0.1-0.5 part of antibacterial agent; the inner layer structure of the aerogel composite heat insulation powder is that pressure-resistant silica hollow nano microspheres are filled in aerogel holes.
2. The epoxy modified methylphenyl organic silicon aerogel heat-insulating coating according to claim 1, wherein the aerogel in the aerogel composite heat-insulating powder is silica aerogel modified by a hydrophobic modifier containing methyl.
3. The epoxy modified methylphenyl organosilicon aerogel heat-insulating coating according to claim 1, wherein the aerogel composite heat-insulating powder comprises the following components in parts by mass: 60-80 parts of aerogel and 15-25 parts of pressure-resistant silica hollow nano-microspheres.
4. The preparation method of the epoxy modified methylphenyl organic silicon aerogel heat-insulating coating is characterized by comprising the following steps of:
1) Weighing epoxy modified methylphenyl organic silicon resin, amino resin, dispersing agent and aerogel composite heat insulation powder, sequentially adding the epoxy modified methylphenyl organic silicon resin, the amino resin, the dispersing agent and the aerogel composite heat insulation powder into water, and grinding to obtain grinding slurry;
2) Sequentially adding glass beads, a defoaming agent, a leveling agent and a silane coupling agent into the grinding slurry obtained in the step 1), and uniformly stirring and mixing;
3) And (3) sequentially adding the modified aerogel, the antifreezing agent, the water-retaining agent and the mildew preventive into the uniformly mixed liquid in the step (2) and stirring to obtain the epoxy modified methylphenyl organic silicon aerogel heat-insulating coating.
5. The method for preparing the organic silicon aerogel heat insulation coating according to claim 4, wherein the method for preparing the aerogel composite heat insulation powder in the step 1) comprises the following steps:
(1) Adding tetraethyl orthosilicate, water, ethanol and hydrochloric acid for hydrolysis to obtain tetraethyl orthosilicate hydrolysate;
(2) Adding an alkali solution into the obtained mixed solution by rapid stirring to adjust the pH of the system, adding the pressure-resistant silica hollow nano-microspheres into the mixed solution, and curing to obtain composite gel;
(3) Crushing the solidified composite gel into small particles, and then placing the small particles in an ethanol solvent for solvent replacement;
(4) Then placing the composite gel subjected to solvent replacement in a hydrophobic modifier containing methyl for modification;
(5) Separating out the liquid, and drying the composite gel to obtain the aerogel composite heat insulation powder.
6. The method for preparing an organic silicon aerogel heat-insulating coating according to claim 4, wherein the grinding speed in the step 1) is 3000r/min, and the fineness of the ground slurry is less than 80 μm.
7. The method for preparing the organic silicon aerogel heat insulation coating according to claim 4, wherein the stirring speed in the step 2) and the stirring speed in the step 3) are 300r/min, and the stirring time is 1h and 20min respectively.
8. The method for preparing the organic silicon aerogel heat insulation coating according to claim 4, wherein the method for preparing the modified aerogel in the step 3) comprises the following steps:
step 1, adding 0.1-1 part of surfactant into 70-90 parts of water, and stirring to obtain a mixed solution A1;
step 2, adding 10-30 parts of hydrophobic modifier modified silica aerogel containing methyl into the mixed solution A1 while stirring, and stirring at a high speed to obtain aerogel dispersion liquid;
and step 3, spray drying the aerogel dispersion liquid to obtain the modified aerogel.
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