CN116606584B - Water-based heat insulation coating and preparation method thereof - Google Patents
Water-based heat insulation coating and preparation method thereof Download PDFInfo
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- CN116606584B CN116606584B CN202310595064.XA CN202310595064A CN116606584B CN 116606584 B CN116606584 B CN 116606584B CN 202310595064 A CN202310595064 A CN 202310595064A CN 116606584 B CN116606584 B CN 116606584B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000576 coating method Methods 0.000 title claims abstract description 37
- 239000011248 coating agent Substances 0.000 title claims abstract description 36
- 238000009413 insulation Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000004964 aerogel Substances 0.000 claims abstract description 25
- 239000004642 Polyimide Substances 0.000 claims abstract description 24
- 229920001721 polyimide Polymers 0.000 claims abstract description 24
- 239000000839 emulsion Substances 0.000 claims abstract description 21
- 239000000945 filler Substances 0.000 claims abstract description 14
- 239000003973 paint Substances 0.000 claims abstract description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 239000002562 thickening agent Substances 0.000 claims abstract description 10
- 239000000080 wetting agent Substances 0.000 claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 9
- 239000000049 pigment Substances 0.000 claims abstract description 9
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 41
- 238000003756 stirring Methods 0.000 claims description 31
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 12
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 9
- 239000007868 Raney catalyst Substances 0.000 claims description 7
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 7
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 7
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 6
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 claims description 6
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 6
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 6
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 5
- 238000000352 supercritical drying Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000005457 ice water Substances 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 4
- 231100000252 nontoxic Toxicity 0.000 abstract description 4
- 230000003000 nontoxic effect Effects 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract 1
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910018557 Si O Inorganic materials 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005303 weighing Methods 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
- C08G73/1028—Preparatory processes from tetracarboxylic acids or derivatives and diamines characterised by the process itself, e.g. steps, continuous
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1057—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain
- C08G73/106—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain containing silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
-
- 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
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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
-
- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a water-based heat-insulating coating and a preparation method thereof, belonging to the technical field of heat-insulating coatings, wherein the water-based heat-insulating coating comprises the following raw materials in parts by weight: 30-50 parts of aqueous epoxy resin emulsion, 10-20 parts of aqueous acrylic emulsion, 0.5-1 part of dispersing agent, 3-5 parts of pigment, 10-20 parts of filler, 0.1-0.3 part of wetting agent, 0.3-0.6 part of thickener and 20-40 parts of water, wherein the filler is polyimide aerogel, and the filler has the non-toxic characteristic, so that the paint is more environment-friendly and safer to use, the-Si-O-Si-, is introduced into a main chain, the weather resistance, the heat aging resistance and the ultraviolet aging resistance are improved, the durability of the paint is improved, the aerogel structure enables the paint to have extremely low heat conductivity, the heat insulation performance of the paint is greatly increased, the air in the aerogel is separated by the nano structure of the aerogel, and the conduction of sound waves is greatly blocked, so that the paint has the noise reduction and sound insulation effects.
Description
Technical Field
The invention belongs to the technical field of heat-insulating paint, and particularly relates to water-based heat-insulating paint and a preparation method thereof.
Background
The building outer wall is directly irradiated by sunlight throughout the year, a large amount of heat is accumulated on the surface, the heat is transferred into the room to cause higher indoor temperature, the heat-insulating paint can be used on the building outer wall to keep proper indoor temperature, the water-based heat-insulating paint has excellent durability, easy construction, cleanness and long-term excellent light and color retention performance, is suitable for various building outer walls, roofs and various building materials, not only can play a role in heat insulation, but also can prolong the service life of the building, and from the aspect of environmental protection, the water-based paint takes water as a dispersion medium, is easier to obtain compared with organic solvent water, saves a lot of resources to a great extent, is free of toxic substances, is healthier and safer when the water-based heat-insulating paint is used, but the water-based paint is worn and subjected to ultraviolet aging and thermal aging, and causes the reduction of heat insulation performance and attractiveness, so that the performance such as aging resistance, hardness, fullness and the like are improved has important practical significance on the premise of ensuring excellent heat insulation performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a water-based heat-insulating coating and a preparation method thereof.
The self-made polyimide aerogel is used as the filler of the water-based heat-insulating coating, polyimide has the characteristics of higher mechanical property, high/low temperature resistance, corrosion resistance, irradiation resistance, low thermal expansion coefficient and the like, the durability of the water-based heat-insulating coating is improved, polyimide is nontoxic, the coating is environment-friendly and safe, and the introduced-Si-O-Si-improves the insulation, heat aging resistance and ultraviolet aging resistance of the coating, and the durability of the coating is improved.
Polyimide aerogel has extremely low coefficient of heat conductivity, makes the thermal-insulated performance greatly increased of coating, and aerogel is divided its inside air with nano-structured solid, has also greatly obstructed the conduction of sound wave, makes the coating have the effect of making an uproar falls and giving sound insulation.
The aim of the invention can be achieved by the following technical scheme:
a water-based heat insulation coating is prepared from the following raw materials in parts by weight: 30-50 parts of aqueous epoxy resin emulsion, 10-20 parts of aqueous acrylic emulsion, 0.5-1 part of dispersing agent, 3-5 parts of pigment, 10-20 parts of filler, 0.1-0.3 part of wetting agent, 0.3-0.6 part of thickener and 20-40 parts of water.
Further, the dispersant is a sodium polyphosphate dispersant.
Further, the wetting agent isWE3225。
Further, the thickener is Solthixa100.
Further, the filler is polyimide aerogel, and the polyimide aerogel is prepared through the following steps:
S1、N 2 under protection, 1, 3-tetramethyl-1, 3-disiloxane diol and K 2 CO 3 Adding the mixture into a three-neck flask, adding DMF as a solvent, stirring for 30min, slowly dropwise adding p-chloronitrobenzene, heating to 100 ℃ after the dropwise adding is completed, reacting for 10h, adding the reaction solution into ice water after the reaction is completed, precipitating solid, filtering, washing with water, and then drying in vacuum to obtain an intermediate 1;1, 3-tetramethyl-1, 3-disiloxane diol,K 2 CO 3 The ratio of DMF to p-chloronitrobenzene was 10g:16.6g:100mL:19g.
Nucleophilic substitution reaction is carried out on-OH on 1, 3-tetramethyl-1, 3-disiloxane diol molecules and-Cl on p-chloronitrobenzene molecules, and the molar ratio of the two is controlled to be close to 1:2, thus obtaining an intermediate 1, wherein the specific reaction process is as follows:
s2, adding the intermediate 1 and Raney nickel into a reaction kettle, adding 1, 4-dioxane as a solvent, and sequentially introducing N 2 、H 2 Performing replacement, and introducing H 2 The pressure is 3.6MPa, the reaction is carried out for 8 hours at 80 ℃, after the reaction is finished, the catalyst is filtered out while the reaction is hot, the filtrate is added into cold water, solid is separated out and filtered, the solid is washed by water, and then the intermediate 2 is obtained by vacuum drying; the dosage ratio of the intermediate 1, the Raney nickel and the 1, 4-dioxane is 10g to 1.44g to 100mL.
The nitro group on the intermediate 1 molecule is changed into amino group through Raney nickel catalytic hydrogenation, and an intermediate 2 is obtained, and the specific reaction process is as follows:
s3, at N 2 Under the protection, adding the intermediate 2 and dimethylacetamide into a flask, stirring for 20min, adding PMDA (pyromellitic dianhydride) in batches, controlling the temperature to be 0 ℃ for reaction for 2h, then reacting for 8h at room temperature, and distilling the reaction solution under reduced pressure after the reaction is completed to obtain an intermediate 3; the dosage ratio of the intermediate 2, the dimethylacetamide and the PMDA is 10g to 100mL to 6.3g.
The intermediate 2 and PMDA are condensed to obtain an intermediate 3, and the specific reaction process is as follows:
s4, at N 2 Under protection, adding the intermediate 3 and dimethylacetamide into a flask, stirring for 20min, adding acetic anhydride and pyridine, reacting at room temperature for 30min, removing bubbles by ultrasonic, stirring the solution for 10min, transferring into a mould, standing for 2h, soaking in a mixed solvent (volume ratio of 1:1) of N-methylpyrrolidone and acetone, replacing the solvent for 12h, soaking in an acetone solution for 24h, replacing the solvent for 12h, soaking in a supercritical drying kettle, and placing CO in the drying kettle 2 Adjusting to a supercritical state, drying for 3 days at 60 ℃ and 10MPa, decompressing, taking out the solid, and grinding to obtain polyimide aerogel filler; the dosage ratio of the intermediate 3, the dimethylacetamide, the acetic anhydride and the pyridine is 10g to 100mL to 3.6g to 3.1g.
The intermediate 3 is dehydrated and cyclized under the catalysis of a dehydrating agent acetic anhydride and pyridine to obtain polyimide, and then the polyimide aerogel is prepared by a supercritical drying method, wherein the specific reaction process is as follows:
the polyimide has the unique molecular chain structure, so that the molecular chain has high rigidity, high mechanical property, high/low temperature resistance, corrosion resistance, irradiation resistance, low thermal expansion coefficient and the like, is nontoxic, environment-friendly and safe when in use, and has unique weather resistance, heat aging resistance and ultraviolet aging resistance due to the fact that the Si-O bond has high bond energy and ionization tendency when being introduced into the main chain, and the durability of the coating is improved.
Polyimide aerogel has extremely low volume density and the crooked route of nano-grid structure has prevented gaseous state and solid-state heat conduction, and a large amount of wall of space have blockked the thermal radiation, and coefficient of heat conductivity is extremely low, has good heat insulating properties, and aerogel divides its inside air with nano-structured solid, has also greatly blockked the conduction of sound wave, has the effect of making an uproar falls the sound insulation.
The invention also aims to provide a water-based heat-insulating coating and a preparation method thereof, wherein the water-based heat-insulating coating comprises the following steps of;
first oneProportionally weighing aqueous epoxy resin emulsion, aqueous acrylic emulsion, sodium polyphosphate dispersing agent,Placing WE3225 wetting agent, solthixa100 thickener and pigment into a container, and dispersing for 15-20 minutes at a stirring rate of 1200-1500r/min to obtain a premix;
and secondly, adding polyimide aerogel into the premix obtained in the first step under the stirring state, stirring and dispersing for 20-30 minutes at the speed of 1200-1500r/min, and moving to a grinder for grinding for 2 hours to obtain the water-based heat-insulating coating.
The invention has the beneficial effects that:
the self-made polyimide aerogel is used as the filler of the water-based heat-insulating coating, the unique molecular chain structure of the polyimide ensures that the molecular chain has high rigidity, has the characteristics of higher mechanical property, high/low temperature resistance, corrosion resistance, irradiation resistance, low thermal expansion coefficient and the like, improves the durability of the water-based heat-insulating coating, and the polyimide is nontoxic, and the water-based heat-insulating coating takes water as a dispersion medium, so that the coating is more environment-friendly and safer to use, and has unique weather resistance, heat aging resistance and ultraviolet aging resistance due to the fact that the Si-O bond has high bond energy and ionization tendency, and the durability of the coating is improved.
Polyimide aerogel has extremely low volume density and the curved path of nano grid structure prevents gaseous and solid heat conduction, a large amount of void walls block heat radiation, the heat conductivity is extremely low, the heat insulation performance of the coating is greatly improved, the aerogel divides the air in the aerogel by the nano-structured solid, and the conduction of sound waves is also greatly blocked, so that the coating has the effects of noise reduction and sound insulation.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparation of the filler
S1、N 2 10g of 1, 3-tetramethyl-1, 3-disiloxane diol and 16.6g of K are taken up in the protection 2 CO 3 Adding into a three-neck flask, adding 100mL of DMF as a solvent, stirring for 30min, slowly dropwise adding 19g of p-chloronitrobenzene, heating to 100 ℃ after the dropwise adding is completed, reacting for 10h, adding the reaction solution into ice water after the reaction is completed, precipitating a solid, filtering, washing with water, and then drying in vacuum to obtain an intermediate 1;
s2, adding 10g of the intermediate 1 and 1.44g of Raney nickel into a reaction kettle, adding 100mL of 1, 4-dioxane as a solvent, and sequentially introducing N 2 、H 2 Performing replacement, and introducing H 2 The pressure is 3.6MPa, the reaction is carried out for 8 hours at 80 ℃, after the reaction is finished, the catalyst is filtered out while the reaction is hot, the filtrate is added into cold water, solid is separated out and filtered, the solid is washed by water, and then the intermediate 2 is obtained by vacuum drying;
s3, at N 2 Under the protection, adding 10g of intermediate 2 and 100mL of dimethylacetamide into a flask, stirring for 20min, adding 6.26g of PMDA (pyromellitic dianhydride) in batches, controlling the temperature to be 0 ℃ for reaction for 2h, then reacting at room temperature for 8h, and distilling the reaction solution under reduced pressure after the reaction is completed to obtain an intermediate 3;
s4, at N 2 Under protection, adding 10g of intermediate 3 and 100mL of dimethylacetamide into a flask, stirring for 20min, adding 3.6g of acetic anhydride and 3.3g of pyridine, reacting at room temperature for 30min, removing bubbles by ultrasonic wave, stirring the solution for 10min, transferring into a mold, standing for 2h, soaking in a mixed solvent (volume ratio of 1:1) of N-methylpyrrolidone and acetone, replacing the solvent for 12h, soaking in an acetone solution for 24h, replacing the solvent for 12h, soaking in a supercritical drying kettle for 24h, and placing CO in the drying kettle 2 And (3) regulating to a supercritical state, drying for 3 days at 60 ℃ and 10MPa, decompressing, taking out the solid, and grinding to obtain the polyimide aerogel.
Example 2
Preparation of the filler
S1、N 2 20g of 1, 3-tetramethyl-1, 3-disiloxane diol and 33.2g of K are taken up in the protection 2 CO 3 Adding 200mL of DMF as a solvent into a three-necked flask, stirring for 30min, slowly dropwise adding 38g of p-chloronitrobenzene, heating to 100 ℃ for reaction for 10h after the dropwise adding is completed, adding the reaction solution into ice water after the reaction is completed, precipitating a solid, filtering, washing with water, and then drying in vacuum to obtain an intermediate 1;
s2, adding 20g of intermediate 2 and 2.88g of Raney nickel into a reaction kettle, adding 200mL of 1, 4-dioxane as a solvent, and sequentially introducing N 2 、H 2 Performing replacement, and introducing H 2 The pressure is 3.6MPa, the reaction is carried out for 8 hours at 80 ℃, after the reaction is finished, the catalyst is filtered out while the reaction is hot, the filtrate is added into cold water, solid is separated out and filtered, the solid is washed by water, and then the intermediate 3 is obtained by vacuum drying;
s3, at N 2 Under the protection, adding 20g of intermediate 3 and 200mL of dimethylacetamide into a flask, stirring for 20min, adding 12.52g of PMDA (pyromellitic dianhydride) in batches, controlling the temperature to be 0 ℃ for reaction for 2h, then reacting at room temperature for 8h, and distilling the reaction solution under reduced pressure after the reaction is completed to obtain an intermediate 4;
s4, at N 2 Under protection, adding 20g of intermediate 4 and 200mL of dimethylacetamide into a flask, stirring for 20min, adding 7.2g of acetic anhydride and 6.6g of pyridine, reacting at room temperature for 30min, removing bubbles by ultrasonic wave, stirring the solution for 10min, transferring into a mold, standing for 2h, soaking in a mixed solvent (volume ratio of 1:1) of N-methylpyrrolidone and acetone, replacing the solvent for 12h, soaking in an acetone solution for 24h, replacing the solvent for 12h, soaking in a supercritical drying kettle for 24h, and placing CO in the drying kettle 2 And (3) regulating to a supercritical state, drying for 3 days at 60 ℃ and 10MPa, decompressing, taking out the solid, and grinding to obtain the polyimide aerogel.
Example 3
In the first step, 300g of aqueous epoxy resin emulsion, 100g of aqueous acrylic emulsion, 5g of sodium polyphosphate dispersing agent and 1g of aqueous acrylic acid emulsionPlacing WE3225 wetting agent, 3g of SolthixA100 thickening agent, 3g of pigment and 200g of water into a container, and dispersing for 15-20 minutes at a stirring rate of 1200-1500r/min to obtain a premix;
and secondly, adding 100g of the polyimide aerogel prepared in the example 1 into the premix obtained in the first step under the stirring state, stirring and dispersing for 20-30 minutes at the speed of 1200-1500r/min, and transferring to a grinder for grinding for 2 hours to obtain the water-based heat-insulating coating.
Example 4
In the first step, 400g of aqueous epoxy resin emulsion, 150g of aqueous acrylic emulsion, 7.5g of sodium polyphosphate dispersing agent and 2g of aqueous acrylic acid emulsionPlacing WE3225 wetting agent, 4.5g of SolthixA100 thickening agent, 4g of pigment and 300g of water into a container, and dispersing for 15-20 minutes at a stirring rate of 1200-1500r/min to obtain a premix;
and secondly, adding 150g of the polyimide aerogel prepared in the example 2 into the premix obtained in the first step under stirring, stirring and dispersing for 20-30 minutes at a speed of 1200-1500r/min, and transferring to a grinder for grinding for 2 hours to obtain the water-based heat-insulating coating.
Example 5
In the first step, 500g of aqueous epoxy resin emulsion, 200g of aqueous acrylic emulsion, 10g of sodium polyphosphate dispersing agent and 3g of aqueous acrylic acid emulsionPlacing WE3225 wetting agent, 6g of SolthixA100 thickening agent, 5g of pigment and 400g of water into a container, and dispersing for 15-20 minutes at a stirring rate of 1200-1500r/min to obtain a premix;
and secondly, adding 200g of the polyimide aerogel prepared in the example 1 into the premix obtained in the first step under the stirring state, stirring and dispersing for 20-30 minutes at the speed of 1200-1500r/min, and transferring to a grinder for grinding for 2 hours to obtain the water-based heat-insulating coating.
The aqueous heat-insulating coating obtained in examples 3 to 5 was prepared as a template according to the standard, and the dry film thickness was 250. Mu.m, and the following performance test was conducted;
from the data in the above table, the aqueous heat-insulating coating materials prepared in examples 3 to 5 have good adhesion, and are excellent in impact resistance, heat-insulating property, water resistance and acid-base resistance.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (6)
1. The water-based heat insulation coating is characterized by being prepared by mixing water-based epoxy resin emulsion, water-based acrylic emulsion, dispersing agent, pigment, filler, wetting agent, thickening agent and water;
wherein the filler is prepared by the following steps:
S1、N 2 under protection, 1, 3-tetramethyl-1, 3-disiloxane diol and K 2 CO 3 Adding into a three-neck flask, adding DMF as solvent, stirring for 30min, slowly dripping p-chloronitrobenzene, heating to 100deg.C for reaction for 10 hr, adding the reaction solution into ice water, precipitating solid, and filteringWashing with water, and then vacuum drying to obtain intermediate 1;
s2, adding the intermediate 1 and Raney nickel into a reaction kettle, adding 1, 4-dioxane as a solvent, and sequentially introducing N 2 、H 2 Performing replacement, and introducing H 2 The pressure is 3.6MPa, the reaction is carried out for 8 hours at 80 ℃, after the reaction is finished, the catalyst is filtered out while the reaction is hot, the filtrate is added into cold water, solid is separated out and filtered, the solid is washed by water, and then the intermediate 2 is obtained by vacuum drying; the dosage ratio of the intermediate 1, the Raney nickel and the 1, 4-dioxane is 10g to 1.44g to 100mL;
s3, at N 2 Under the protection, adding the intermediate 2 and dimethylacetamide into a flask, stirring for 20min, adding pyromellitic dianhydride in batches, controlling the temperature to be 0 ℃ for reaction for 2h, then reacting at room temperature for 8h, and distilling the reaction solution under reduced pressure after the reaction is finished to obtain an intermediate 3;
s4, at N 2 Under protection, adding the intermediate 3 and dimethylacetamide into a flask, stirring for 20min, adding acetic anhydride and pyridine, reacting for 30min at room temperature, removing bubbles by ultrasonic, stirring the solution for 10min, transferring into a mould, standing for 2h, soaking in a mixed solvent of N-methylpyrrolidone and acetone in a volume ratio of 1:1, replacing the solvent for 12h, immersing in an acetone solution after 24h, replacing the solvent for 12h, soaking in a supercritical drying kettle after 24h, and placing CO in the drying kettle 2 And (3) regulating to a supercritical state, drying for 3 days at 60 ℃ and 10MPa, decompressing, taking out the solid, and grinding to obtain the polyimide aerogel filler.
2. The water-based heat insulation coating as claimed in claim 1, wherein the water-based heat insulation coating is prepared from the following raw materials in parts by weight: 30-50 parts of aqueous epoxy resin emulsion, 10-20 parts of aqueous acrylic emulsion, 0.5-1 part of dispersing agent, 3-5 parts of pigment, 10-20 parts of filler, 0.1-0.3 part of wetting agent, 0.3-0.6 part of thickener and 20-40 parts of water.
3. The water-based heat-insulating paint according to claim 1, wherein in the step S1, 3-tetramethyl-1, 3-disiloxane diol and K 2 CO 3 DMF, p-chloronitrobenzeneThe dosage ratio of (2) is 10g:16.6g:100mL:19g.
4. The water-based heat insulation coating according to claim 1, wherein the dosage ratio of the intermediate 2, the dimethylacetamide and the pyromellitic dianhydride in the step S3 is 10g to 100mL to 6.26g.
5. The water-based heat insulation coating according to claim 1, wherein the dosage ratio of the intermediate 3, dimethylacetamide, acetic anhydride and pyridine in the step S4 is 10g to 100mL to 3.6g to 3.3g.
6. A method for preparing the aqueous heat insulating coating according to claim 1, comprising the steps of:
firstly, placing the water-based epoxy resin emulsion, the water-based acrylic emulsion, the sodium polyphosphate dispersing agent, the wetting agent, the thickening agent and the pigment which are weighed in proportion into a container, and dispersing for 15-20 minutes at the stirring rate of 1200-1500r/min to obtain a premix;
and secondly, adding polyimide aerogel into the premix obtained in the first step under the stirring state, stirring and dispersing for 20-30 minutes at the speed of 1200-1500r/min, and moving to a grinder for grinding for 2 hours to obtain the water-based heat-insulating coating.
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| CN110437470A (en) * | 2018-05-04 | 2019-11-12 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of polyimide aerogels and the preparation method and application thereof with lotus leaf effect |
| CN111286076A (en) * | 2020-02-12 | 2020-06-16 | 青岛科技大学 | aminopropyl-POSS modified polyimide aerogel, and preparation method and application thereof |
| CN113387977A (en) * | 2021-06-10 | 2021-09-14 | 中国科学院长春应用化学研究所 | Diamine and preparation method thereof, and polyimide and preparation method thereof |
| CN115010841A (en) * | 2022-07-20 | 2022-09-06 | 巩义市泛锐熠辉复合材料有限公司 | Modified aerogel, thermal insulation coating prepared from modified aerogel and preparation method of thermal insulation coating |
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| US9109088B2 (en) * | 2012-02-03 | 2015-08-18 | Ohio Aerospace Institute | Porous cross-linked polyimide networks |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110437470A (en) * | 2018-05-04 | 2019-11-12 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of polyimide aerogels and the preparation method and application thereof with lotus leaf effect |
| CN111286076A (en) * | 2020-02-12 | 2020-06-16 | 青岛科技大学 | aminopropyl-POSS modified polyimide aerogel, and preparation method and application thereof |
| CN113387977A (en) * | 2021-06-10 | 2021-09-14 | 中国科学院长春应用化学研究所 | Diamine and preparation method thereof, and polyimide and preparation method thereof |
| CN115010841A (en) * | 2022-07-20 | 2022-09-06 | 巩义市泛锐熠辉复合材料有限公司 | Modified aerogel, thermal insulation coating prepared from modified aerogel and preparation method of thermal insulation coating |
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