CN116875185A - Double-silicon-system heat-resistant paint and preparation method thereof - Google Patents
Double-silicon-system heat-resistant paint and preparation method thereof Download PDFInfo
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- CN116875185A CN116875185A CN202310859052.3A CN202310859052A CN116875185A CN 116875185 A CN116875185 A CN 116875185A CN 202310859052 A CN202310859052 A CN 202310859052A CN 116875185 A CN116875185 A CN 116875185A
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- 239000003973 paint Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 61
- 239000011248 coating agent Substances 0.000 claims abstract description 59
- 239000010703 silicon Substances 0.000 claims abstract description 43
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 43
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- 230000001070 adhesive effect Effects 0.000 claims abstract description 20
- 239000000853 adhesive Substances 0.000 claims abstract description 18
- 239000004945 silicone rubber Substances 0.000 claims description 23
- 239000000945 filler Substances 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 20
- 239000012752 auxiliary agent Substances 0.000 claims description 12
- 239000003822 epoxy resin Substances 0.000 claims description 11
- 229920000647 polyepoxide Polymers 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000004593 Epoxy Substances 0.000 claims description 7
- 239000003085 diluting agent Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000011324 bead Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920002050 silicone resin Polymers 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 230000009977 dual effect Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 2
- 230000003449 preventive effect Effects 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims 2
- 239000012757 flame retardant agent Substances 0.000 claims 1
- 238000007689 inspection Methods 0.000 claims 1
- 238000005070 sampling Methods 0.000 claims 1
- 238000002679 ablation Methods 0.000 abstract description 27
- 238000005516 engineering process Methods 0.000 abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 11
- 229910002027 silica gel Inorganic materials 0.000 abstract description 7
- 239000000741 silica gel Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000014759 maintenance of location Effects 0.000 abstract description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 30
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 description 18
- 239000000463 material Substances 0.000 description 11
- 239000011253 protective coating Substances 0.000 description 10
- 238000009413 insulation Methods 0.000 description 8
- 238000005507 spraying Methods 0.000 description 7
- 238000011161 development Methods 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000004840 adhesive resin Substances 0.000 description 2
- 229920006223 adhesive resin Polymers 0.000 description 2
- 150000001412 amines Chemical group 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
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- 238000009472 formulation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
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- 238000011160 research Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 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 description 1
- 229920002943 EPDM rubber Polymers 0.000 description 1
- 235000015842 Hesperis Nutrition 0.000 description 1
- 235000012633 Iberis amara Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
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- 238000010835 comparative analysis Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 229910052902 vermiculite Inorganic materials 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
-
- 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
- C09D7/70—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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The application belongs to the technical field of special functional coatings, and particularly relates to a double-silicon-system heat-resistant coating and a preparation method thereof; under the condition of the existing resin-based heat-resistant paint forming technology, the core technology of the application is that the organic silicon resin is introduced to have high temperature resistance and environmental adaptability, the silicon rubber adhesive is introduced and the technology of high toughness and high temperature ablation dimension of the silica gel is applied, and the comprehensive performance of the application is far superior to that of the heat-resistant paint of a single organic silicon resin modified system, the heat-resistant paint modified by a single silicon rubber adhesive and the heat-resistant paint of a silicate system. The heat-resistant coating has low density, low heat conductivity coefficient, high quality retention rate and good mechanical property, optimizes the core technology of high-temperature ablation dimension, and effectively solves the technical problem of heat protection of the aircraft matrix.
Description
Technical Field
The application belongs to the technical field of special functional coatings, and particularly relates to a double-silicon-system heat-resistant coating and a preparation method thereof.
Background
Silicon heat-resistant coating materials are novel heat-resistant materials which are raised along with the development of the aerospace industry, and play a role in the development of the aerospace industry, which cannot be underestimated. With the development of weapon system rockets and missile technologies, the internal and external heat insulation protection requirements of various aircraft engine combustion chamber shells and projectile bodies are higher and higher, and the requirements on how to protect the heat insulation and heat protection of the internal and external base materials of the engine shells and the projectile bodies are higher, and the double-silicon heat protection coating material has specific technical advantages, mainly shows excellent mechanical properties and light low-conductivity ablation dimensional properties, so that the development of the forming technology of the double-silicon heat protection coating is significant.
At present, most of internal heat insulation layers of engines adopt materials such as ethylene propylene diene monomer rubber, RTV silicone rubber and the like, the materials have low density and excellent high-temperature ablation performance, but the mechanical performance of the materials is poor, and according to the requirements of heat protection of a future elastomer structure and development of novel internal heat protection materials of the engines, the design, preparation and performance optimization research of a high-toughness high-quality retention double-silicon system heat protection coating are developed, key technologies such as an organosilicon and silica gel miscible modification technology and special heat insulation filler compounding are mainly broken through, the synergistic unification of good coating adhesion, light weight, ablation resistance and high toughness is realized, and the flexible ablation heat insulation coating with low density and low heat conductivity coefficient is developed, and meanwhile, the coating has excellent mechanical performance and high ablation dimensional performance so as to meet the requirements of heat insulation and heat protection inside and outside the novel aircraft engine shell and elastomer.
Disclosure of Invention
The application aims to solve the technical problem of insufficient heat protection in the high heat flow environment in the prior art, and provides a double-silicon-system heat-resistant coating and a preparation method thereof.
The method is realized by the following technical scheme:
1. the heat-proof coating with double silicon systems comprises, by weight, 20-30 parts of organic silicon resin, 10-18 parts of silicone rubber adhesive, 5-10 parts of epoxy resin, 15-30 parts of light low-conductivity nano filler, 4-12 parts of fiber reinforced heat-proof filler, 1-3 parts of auxiliary agent, 10-20 parts of special solvent for silicone resin, 4-12 parts of special solvent for silicone rubber adhesive and 3-7 parts of epoxy diluent, wherein the A component of the heat-proof coating is formed by the above components; the component B of the heat-resistant paint is curing agent with the mass percent of 3-6% of the component A, and the components are packaged; the component C of the heat-proof paint is a cross-linking agent with the mass percent of 1-3% of the component A, and the coating is packaged.
Further, the heat-proof coating is a component A of the heat-proof coating, which comprises 23-28 parts of organic silicon resin, 12-15 parts of silicone rubber adhesive, 7-9 parts of epoxy resin, 20-25 parts of low-density low-conductivity nano filler, 6-10 parts of fiber reinforced heat-insulating filler, 1-3 parts of auxiliary agent, 13-17 parts of silicone resin special solvent, 6-10 parts of silicone rubber special solvent and 4-6 parts of epoxy diluent; the component B of the heat-resistant paint is an amine curing agent with the mass percent of 3-6% of the component A, and the components are packaged; the component C of the heat-proof paint is a silicone rubber cross-linking agent with the mass percent of 1-3% of the component A, and the components are packaged.
Further, the optimal formula of the heat-resistant coating comprises 26 parts of organic silicon resin, 13 parts of silicone rubber adhesive, 8 parts of epoxy resin, 22 parts of light low-conductivity nano filler, 8 parts of fiber-reinforced heat-insulating filler, 1 part of auxiliary agent, 15 parts of special solvent for silicone resin, 8 parts of special solvent for silicone rubber and 5 parts of epoxy diluent, wherein the component A of the heat-resistant coating is formed by the above components; the component B of the heat-resistant paint is an amine curing agent with the mass percent of 3.5% of the component A, and the components are packaged; the component C of the heat-resistant paint is a silicone rubber cross-linking agent with the mass percent of 2% of the component A, and the components are packaged.
Further, the auxiliary agent is one or more of an anti-settling agent, a flame retardant and a mildew preventive.
2. The preparation method of the double-silicon-system heat-resistant paint comprises the following steps: the preparation method comprises the steps of taking organic silicon resin, adding a special solvent for organic silicon, taking a silicon rubber adhesive, adding a special solvent for silicon rubber, taking epoxy resin, adding an epoxy diluent, fully dissolving, mixing three film forming systems, dispersing for more than 30min at the rotating speed of 500-800 r/min, adding a light low-conductivity nano filler, a fiber reinforced heat insulation filler, an auxiliary agent and a mixed solvent, dispersing for 60-90 min at the high speed at the rotating speed of 1000-1200 r/min, and standing for 60min. And (3) sanding the dispersed heat-proof paint for 3 cycles, filtering the paint with a sieve with the size not smaller than 100 meshes, adding a solvent after filtering to adjust the viscosity, controlling the viscosity of the heat-proof paint after sanding to be 20-40 s (room temperature, coating-4), and obtaining the component A of the double-silicon heat-proof paint with the fineness not larger than 45 mu m.
Further, the silicone resin, silicone rubber adhesive, light low-conductivity nano filler, fiber-reinforced heat insulating filler, auxiliary agent and solvent may be conventionally selected according to common general knowledge in the art, for example: the silicone rubber adhesive is one or two of silicone rubber with hydroxyl-containing end groups, methyl diphenyl room temperature vulcanized silicone rubber and single-component room temperature vulcanized silicone rubber.
Further, the low-density nano filler is one or more of vermiculite powder, superfine cork powder, expanded perlite and fumed silica.
Further, the high-temperature-resistant heat insulation filler is one or more of glass beads, phenolic hollow microspheres, fibrous asbestos, sepiolite and antimony trioxide. The solvent is a mixture of esters, alcohols, benzene, ketones, ethers and the like.
In summary, the beneficial effects of the application are as follows: the core technology of the double-silicon system heat-resistant paint provided by the application is that organic silicon resin is introduced to have high temperature resistance and environmental adaptability, silicone rubber adhesive is introduced to apply the high-toughness and high-temperature ablation maintenance technology of silica gel, and the comprehensive performance of the double-silicon system heat-resistant paint is far superior to that of a heat-resistant paint of a single organic silicon resin modified system, a heat-resistant paint of a single silicone rubber adhesive modified and a silicate system heat-resistant paint under the condition of the existing resin-based heat-resistant paint forming technology. The heat-proof coating has low density, low heat conductivity coefficient, high quality retention rate and good mechanical property, optimizes the core technology of high-temperature ablation dimension, effectively solves the technical problem of heat protection of an aircraft matrix, has been manufactured and verified on a certain product part, has completed mechanical property, thermal property and environmental test verification and examination, and has the performance index meeting the requirements of engineering application of a certain part.
The existing organic silicon resin and silicone rubber adhesive mixed modified heat-resistant paint has the main film-forming substance of a double mixed modified system of adding silica gel and epoxy resin into the organic silicon resin, but the paint processed by pure silica gel has poor comprehensive performance (poor adhesive force) and poor heat-resistant temperature ablation performance. The inventor of the application adopts a great deal of experimental research and screening, selects and uses double modification technology of organic silicon and silica gel adhesive and epoxy resin for treatment, screens out the preferable proportion of organic silicon resin, silicone rubber adhesive, epoxy resin, filler and auxiliary agent through experiments, effectively improves the technological property of the organic silicon resin, and the modified coating system can realize normal-temperature curing, adopts anti-ablation, low-density and low-heat-conduction composite filler, realizes a mixed modification technology of the organic silicon resin and the silica gel, and completes the preparation of the heat-resistant coating material.
Drawings
Fig. 1 is a front view of the ignition screw cap after surface cleaning.
Fig. 2 is a photograph of the back of the ignition screw cap after surface cleaning.
FIG. 3 is a sample of a dual silicon thermal protection coating made on the surface of the ignition screw cap.
FIG. 4 is a photograph of a sample of a thermal protective coating being ablated for 6 seconds under oxyacetylene.
Fig. 5 is a front photograph of a sample without a thermal protective coating ablated for 6s under oxyacetylene.
FIG. 6 is a photograph of the reverse side of a sample without a thermal protective coating ablated for 6s under oxyacetylene.
FIG. 7 is a photograph of a sample of a thermal protective coating being ablated for 12 seconds under oxyacetylene.
FIG. 8 is a photograph of a sample of a thermal protective coating being ablated for 24 seconds under oxyacetylene.
FIG. 9 is a photograph of the back of a sample without a thermal protective coating ablated for 24 seconds under oxyacetylene.
Fig. 10 is a front photograph of a sample without a thermal protective coating ablated for 24s under oxyacetylene.
FIG. 11 is a photograph of a sample without a thermal protective coating, cooled by ablation for 24 seconds with oxyacetylene.
FIG. 12 is a photograph of the reverse side of a sample without a thermal protective coating ablated for 24 seconds under oxyacetylene.
Detailed Description
The following detailed description of the application is provided in further detail, but the application is not limited to these embodiments, any modifications or substitutions in the basic spirit of the present examples, which still fall within the scope of the application as claimed.
Example 1
1. The heat-resistant paint formulation is shown in table 1:
table 1 Heat protective coating formulation of double silicon systems
2. The preparation method comprises the following steps:
(1) Weighing: firstly, weighing high-temperature organic silicon resin, silicone rubber adhesive and epoxy resin, adding a mixed solvent, dispersing for more than 10min at the rotating speed of 900r/min, and then adding filler and auxiliary agent and mixing for more than 20 min.
(2) Dispersing: the premixed coating is dispersed for 55min at the rotating speed of 700r/min and then dispersed for 70min at the high speed at the rotating speed of 1000r/min (the material temperature during dispersion is not more than 35 ℃), so that the uniform premixing of the coating system is ensured.
(3) Grinding: the grinding medium (glass beads or zirconia beads with phi 1.5-phi 3) is filled in the horizontal sand mill, cooling water is connected, three circulation sand grinding is carried out after the temperature and the pressure are set, and the material temperature during sand grinding is not more than 35 ℃.
(4) And (3) filtering: the sanded paint is filtered by a copper wire mesh which is not smaller than 100 meshes, and the copper wire mesh must be kept clean and intact.
(5) Mixing paint: adding solvent to prepare uniformly, controlling the viscosity of the prepared paint to be 25-45 s, and barreling and carrying out quality consistency test, wherein the fineness is not more than 45 mu m.
1. Thermal protection coating performance test
And (3) spraying a test piece: mainly comprises pretreatment of test pieces, preparation of paint, spraying and curing.
(a) Pretreatment of a test piece: the test pieces (aluminum test piece anodized, magnesium test piece oxidized) were washed with gasoline or acetone.
(b) And (3) preparing a coating: 1000g of the component A of the heat-resistant paint is weighed, then the component B, the component C and the component D are weighed and mixed uniformly, and the viscosity easy to spray is adjusted by adding the solvent.
(c) Spraying: and a small spray gun is selected for spraying, the air pressure is controlled to be about 0.3MPa, the distance between the spray gun and the spray gun is about 20 cm-30 cm, and the thickness of a single-layer wet film is 30 mu m-50 mu m. The thickness of the conventional performance and heat-resistant performance coating is controlled to be 30-50 mu m, the thickness of the heat-insulating performance coating is controlled to be 0.8-1.0 mm, and the thickness of the thermal performance test coating is controlled to be 2-3 mm (after processing according to standard size).
(d) Curing: the test piece is cured and naturally dried for 96 hours or the test piece is placed at room temperature for 3 hours and then is baked for 24 hours in an oven at the temperature of 35-45 ℃.
(e) Test piece test: the test pieces were subjected to performance test according to the relevant standards, and the test indexes are shown in Table 2.
TABLE 2 Dual silicon System thermal protection coating Performance requirement and test results
2. Verification of thermal protection coating ablation
Flame jet ablation of oxyacetylene is adopted, and the flame temperature is changed by adjusting the content of oxygen and acetylene, so that the temperature reaches an expected value. The jet pressure of the flame is changed by adjusting the input size of the air flow, so that the flame forms a required high-temperature high-speed flow field at the outlet of the jet pipe, and an ablation test is carried out on the surface of the test piece.
1. The main test process comprises the following steps:
according to the test requirement, firstly carrying out surface treatment on a sample before the test, and then manufacturing a heat-resistant coating of a double-silicon system, wherein the specific steps are as follows:
a) Pretreatment: before spraying, surface treatment is carried out, and a sample is soaked by No. 200 gasoline to remove oil stains on the surface.
b) Spraying: the coating is prepared on the sample by adopting a spraying method, and can be coated for multiple times, wherein the interval is 5-10 min each time, and the thickness of the coating is controlled between (0.15-0.3) mm.
c) Curing: the test piece is naturally dried for 96 hours or the test piece is firstly placed for 3 hours at room temperature and then is baked for 24 hours in an oven at the temperature of 35-45 ℃.
Ablation of test piece: and (3) horizontally placing the sample on a steel plate, adjusting the gas combination and the gas flow density, and performing oxyacetylene flame ablation test on the sample. The combustion time is 6s, 12s and 24s respectively, and the flame temperature is more than 2000 ℃.
2. Analysis of test data
The test performed oxyacetylene ablation assessment for 5 groups of samples. And (3) photographing and analyzing the appearance of the samples before and after the test, wherein the photographs are shown in figures 1-12. Wherein, fig. 1, fig. 2 are the front and back of the ignition screw cap after surface cleaning, fig. 3 is a sample of the double silicon heat-proof coating made on the surface of the ignition screw cap, fig. 4 is a sample for making the heat-proof coating which is ablated for 6s under oxyacetylene, fig. 5 and fig. 6 are the front and back pictures of the sample without the heat-proof coating which is ablated for 6s under oxyacetylene. Fig. 7 is a photograph of a sample for producing a heat-resistant coating layer ablated under oxyacetylene for 12s, fig. 8 is a photograph of a sample for producing a heat-resistant coating layer ablated under oxyacetylene for 24s, fig. 9 is a photograph of a back side of a sample for producing no heat-resistant coating layer ablated under oxyacetylene for 24s, and fig. 10-12 are photographs of a front side, a cooling side and a back side of a sample for producing no heat-resistant coating layer ablated under oxyacetylene for 24 s.
Comparing fig. 3 and fig. 4, it can be seen that after 6s of high temperature ablation, the coating on the sample surface has no foaming, falling off and cracking, and the carbonization degree of the coating is not obvious, which indicates that the heat-resistant coating has good temperature resistance and dimensional effect at the temperature and the ablation time. As can be seen by comparing fig. 3, fig. 4, fig. 5 and fig. 6, when the surface of the sample is not coated with the heat-proof coating, the sample is reddened after being ablated for 6 seconds at high temperature, and the electroplated coating on the surface of the sample is fallen after cooling.
As can be seen from fig. 7 and 8, as the ablation time is prolonged, the coating on the surface of the sample starts to be carbonized uniformly, the color of the coating gradually changes into gray black, but the coating still has no foaming, falling off and cracking, which indicates that the heat-resistant coating has better high temperature resistance and dimensional effect at the temperature and the ablation time. Comparing fig. 8 and 9 with fig. 10-12 without the heat-proof coating, it can be seen that the sample without the heat-proof coating turns red after 24s of high-temperature ablation, spots and pits appear on the outer surface after cooling, and the surface of the sample is seriously damaged by the high-temperature ablation. Comparing fig. 2, 9 and 12, the surface of the sample in fig. 9 is almost undamaged, and the back of the sample in fig. 12 is obviously deformed by melting, which indicates that the existence of the heat-proof coating obviously reduces the temperature of the back of the sample, plays a certain role in protecting the sample, has better heat-insulating and heat-proof effects, and the comparison result is shown in table 3.
TABLE 3 comparative analysis of the ablative status of ignition screw caps
3. Test results
According to the above test analysis, the following test results were obtained:
1) The double-silicon heat-resistant coating material has the advantages of uniform carbonization of the coating under high-temperature ablation, no bubbling and crack falling phenomena, good high-temperature resistance and heat resistance and good ablation shape maintenance effect.
After the surface of the ignition screw cap is sprayed with the double-silicon heat-proof coating, the screw cap is well insulated and protected. The high-temperature ablation resistant and anti-scouring performance of the screw cap is improved, the service life of the screw cap is obviously improved, and the heat protection requirement of an engine ignition device of a certain model product in the flight process is met.
Claims (6)
1. The double-silicon system heat-resistant paint is characterized by comprising, by weight, 20-30 parts of organic silicon resin, 10-18 parts of silicone rubber adhesive, 5-10 parts of epoxy resin, 15-30 parts of light low-conductivity nano filler, 4-12 parts of fiber reinforced heat-insulating filler, 1-3 parts of auxiliary agent, 10-20 parts of special solvent for silicone resin, 4-12 parts of special solvent for silicone rubber adhesive and 3-7 parts of epoxy diluent, wherein the A component of the heat-resistant paint is formed by the components; the component B of the heat-resistant paint is curing agent with the mass percent of 3-6% of the component A, and the components are packaged; the component C of the heat-proof paint is a cross-linking agent with the mass percent of 1-3% of the component A, and the coating is packaged.
2. The dual-silicon system heat-resistant paint as claimed in claim 1, wherein the A component of the heat-resistant paint comprises 23-28 parts of organic silicon resin, 12-15 parts of silicon rubber adhesive, 7-9 parts of epoxy resin, 20-25 parts of low-density low-conductivity nano filler, 6-10 parts of fiber reinforced heat-insulating filler, 1-3 parts of auxiliary agent, 13-17 parts of special solvent for silicon resin, 6-10 parts of special solvent for silicon rubber and 4-6 parts of epoxy diluent; the component B of the heat-resistant paint is an amine curing agent with the mass percent of 3-6% of the component A, and the components are packaged; the component C of the heat-proof paint is a silicone rubber cross-linking agent with the mass percent of 1-3% of the component A, and the components are packaged.
3. The dual-silicon system heat-resistant paint as claimed in claim 1, wherein the component A of the heat-resistant paint comprises 26 parts of organic silicon resin, 13 parts of silicon rubber adhesive, 8 parts of epoxy resin, 22 parts of light low-conductivity nano filler, 8 parts of fiber reinforced heat-insulating filler, 1 part of auxiliary agent, 15 parts of silicon resin special solvent, 8 parts of silicon rubber special solvent and 5 parts of epoxy diluent; the component B of the heat-resistant paint is an amine curing agent with the mass percent of 3.5% of the component A, and the components are packaged; the component C of the heat-resistant paint is a silicone rubber cross-linking agent with the mass percent of 2% of the component A, and the components are packaged.
4. A method for preparing a dual-silicon heat-resistant coating as claimed in any one of claims 1 to 3, wherein the auxiliary agent is one or more of an anti-settling agent, a flame retardant agent and a mildew preventive.
5. A method for preparing a dual silicon system heat protection coating as defined in any one of claims 1-3, comprising the steps of:
the coating after standing is sanded by a sand mill, grinding media are filled before sanding, the filling media are uniformly distributed along the axial direction, the filling coefficient is controlled to be 70% -80%, cooling water is connected, the states of a temperature gauge and a pressure gauge are checked, the heat-proof coating is sanded for 3 cycles, the temperature of the coating in the sanding process is not higher than 35 ℃, stopping machine is allowed to naturally cool for more than 30min when the temperature is higher, proper solvent is added after sanding is finished, the viscosity is controlled to be within the range of 20-40 s, and the fineness is not more than 45 mu m; and filtering the mixture by a sieve with the size not smaller than 100 meshes, sampling and inspecting the filtered mixture, and obtaining the component A of the double-silicon heat-resistant coating after inspection.
6. The method for preparing a dual silicon system heat-resistant paint as claimed in claim 5, wherein the grinding medium is a zirconia bead or glass bead with a diameter of 1.5-3.
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