CN112300696B - Organic-inorganic hybrid ablation-resistant coating and preparation method thereof - Google Patents
Organic-inorganic hybrid ablation-resistant coating and preparation method thereof Download PDFInfo
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/38—Paints containing free metal not provided for above in groups C09D5/00 - C09D5/36
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- 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
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- 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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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
Abstract
The invention relates to an organic-inorganic hybrid ablation-resistant coating and a preparation method thereof. An organic-inorganic hybrid ablation-resistant coating is characterized by comprising the following components in parts by weight: 80-90 parts of titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder, 18-25 parts of bis-terminal aminosilane with molecular weight of about 1000-3000, 10-16 parts of POSS (polyhedral oligomeric silsesquioxane) graft modified epoxy resin and ZrO2/Y2O3/Nb2O55-9 parts of powder and 20-30 parts of endothermic filler. The coating is applied to the surface of a substrate to form a coating with the thickness of 0.2mm, and the coating is completely dried and then subjected to an ablation test through a plasma flame simulation working condition. The coating can maintain performance for 2 hours at 1000 ℃.
Description
Technical Field
The invention relates to an ablation-resistant coating and a method for preparing the ablation-resistant coating, in particular to an organic-inorganic hybrid ablation-resistant coating and a preparation method thereof.
Background
Organic ablative materials are a new class of materials that emerged at the end of the fifties of the twentieth century to accommodate and satisfy the development of the aerospace industry. The aerodynamic heat generated by the far-range ultrahigh-speed aircraft due to the severe friction with air is far beyond the tolerance of high-temperature alloy. For example, the Apollo spacecraft may have a surface temperature of 5000F (2800℃) when it returns to the atmosphere. When the medium-range missile flies at the altitude of 3450 m/s at 10000 feet (30480 m), the stagnation point temperature can reach 3380 ℃. An intercontinental missile flying at 6600 m/s at the altitude mentioned above, the stagnation temperature was 7110 ℃. Under such extreme conditions, the metal will melt and burn out quickly. The head of the first generation missile developed in 1955 in the united states, leishen, used 60 kg of copper-molybdenum-beryllium alloy as a heat storage (Heatsink) thermal protection. The alloy is heated to melt and become blunt, and the alloy is eliminated because of influence on flying. The occurrence of the organic ablation material satisfactorily solves the thermal protection problem under high-heat-flow pneumatic heating, and lays a foundation for the development of the aerospace industry. With the development of the aerospace industry and the emergence of anti-guided missiles, heat protection measures capable of keeping good aerodynamic shape during high-speed flight in dense atmospheric layers are being developed, namely sweating cooling (also called active cooling, and for ablation, passive cooling).
The organic ablation material is a material which utilizes the complex processes of physical (melting, evaporation, sublimation, reflection, radiation, conduction and the like) and chemical (decomposition, depolymerization, ionization … …) and the like of the material under the action of high temperature, and the material itself ablates (like meteorite enters the atmosphere again) to carry away heat to protect the normal flight of an aircraft, and can be divided into four types, namely glass fiber reinforced plastic, honeycomb sandwich structure, soft sheet and coating according to different using modes.
Chinese patent application 201310209072.2 discloses a high-temperature resistant anticorrosive paint containing polyaryl organic silicon resin, which comprises the following components in parts by weight: 40-50 parts of polyaryl organic silicon resin, 20-30 parts of glycidyl p-hydroxybenzoate, 5-10 parts of acrylic resin, 10-15 parts of mica powder, 10-15 parts of graphene, 5-10 parts of ethyl acetate and 10-20 parts of diluent. The diluent is butanol or xylene. The prepared high-temperature-resistant anticorrosive paint can resist the temperature of 400-500 ℃, and has a good anticorrosive effect.
The Chinese patent application 201310269529.9 provides a novel high-temperature-resistant insulating coating which comprises the following components in percentage by mass: 30-40 parts of polyalkylaryl organic silicon resin, 40-60 parts of filler, 1-28 parts of curing agent, 0.01-0.1 part of anti-settling agent, 0.01-0.7 part of defoaming agent and 0.01-0.3 part of flatting agent; the polyalkylaryl organic silicon resin is polymethylphenyl organic silicon resin or polyethylphenyl organic silicon resin; the filler is one or more of silicon oxide, zinc oxide, aluminum oxide and mica; the curing agent is a polyamide epoxy curing agent. The high-temperature-resistant insulating paint has the advantages of strong heat resistance, good insulating property, good mechanical property and stability, long service life, simple preparation method and accordance with the requirement of saving cost, and can be used at high temperature of 600 ℃.
The Chinese patent application 201310270511.0 provides a high-temperature-resistant insulating paint which comprises the following components in percentage by mass: 30-40 parts of organic silicon resin, 40-60 parts of filler, 10-45 parts of curing agent, 0-0.1 part of anti-settling agent, 0-0.5 part of defoaming agent and 0-0.3 part of flatting agent; the organic silicon resin is polymethyl silicon resin, polyethyl silicon resin or polyaryl organic silicon resin, and the ratio of the number of ethyl groups to the number of silicon atoms in the polyethyl silicon resin polymer is 0.5-1.5; the filler is one or more of silicon oxide, zinc oxide, aluminum oxide and mica; the curing agent is a polyamide epoxy curing agent. The high-temperature-resistant insulating coating has strong heat resistance, can be used at a high temperature of more than 600 ℃, has good insulating property and stable chemical property, and the preparation method of the coating is simple.
Disclosure of Invention
The technical scheme of the invention is as follows: an organic-inorganic hybrid ablation-resistant coating is characterized by comprising the following components: titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder, bis-terminal aminosilane with molecular weight of about 1000-3000, POSS graft modified epoxy resin and ZrO2/Y2O3/Nb2O5A powder and a heat absorbing filler; the weight parts of the components are as follows:
80-90 parts of titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder
Molecular weight of about 1000-3000 double-terminal aminosilane 18-25
POSS graft modified epoxy resin 10-16
ZrO2/Y2O3/Nb2O5Powder 5-9
Dimethylformamide 18-28
20-30 parts of heat absorbing filler;
the preparation method of the titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder comprises the following steps: uniformly spraying a silane coupling agent solution on the titanium dioxide hollow microspheres, standing for 10-20 minutes, then mixing the titanium dioxide hollow microspheres with an organic silicon resin monomer for reaction to obtain polyaryl organic silicon resin, and crushing the polyaryl organic silicon resin to obtain powder with the average particle size of about 1.6 microns; the heat absorption filler is a mixture of glass powder and aluminum powder, and the mass ratio of the glass powder to the aluminum powder is as follows: the aluminum powder is about 1-3:2-7, and the average particle size is about 2 microns.
Preferably, the weight parts of each component are as follows:
titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder 80
Two-terminal aminosilane 18 having molecular weight of about 1000-3000
POSS graft modified epoxy resin 10
ZrO2/Y2O3/Nb2O5Powder 5
Dimethylformamide 18
A heat absorbing filler 20.
Preferably, the weight parts of each component are as follows:
titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder 85
Two-terminal aminosilane 21 having molecular weight of about 1000-3000
POSS graft modified epoxy resin 13
ZrO2/Y2O3/Nb2O5Powder 7
Dimethylformamide 23
And a heat absorbing filler 25.
Preferably, the weight parts of each component are as follows:
titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder 90
Bis-terminal aminosilane 25 having a molecular weight of about 1000-3000
POSS graft modified epoxy resin 16
ZrO2/Y2O3/Nb2O5Powder 9
Dimethylformamide 28
A heat absorbing filler 30.
Further preferably, the mass ratio of the titanium dioxide hollow microspheres to the polyaryl organic silicon resin is 1-2: 7.
Further preferably, the mass ratio of POSS to epoxy resin in the POSS graft modified epoxy resin is 1-1.2: 20. A preparation method of an organic-inorganic hybrid ablation-resistant coating is characterized by comprising the following preparation steps:
uniformly mixing titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder with 1000-3000 aminosilane and part of dimethylformamide to obtain material A, and mixing POSS modified epoxy resin with ZrO2/Y2O3/Nb2O5And uniformly mixing the powder and the residual dimethylformamide to obtain a material B, and uniformly mixing the material A, the material B and the heat-absorbing filler to obtain the organic-inorganic hybrid ablation-resistant coating.
A coating is characterized by being obtained by applying the organic-inorganic hybrid ablation-resistant coating.
The invention has the beneficial effects that: the coating is applied to the surface of a substrate to form a coating with the thickness of 0.2mm, and the coating is completely dried and then subjected to an ablation test through a plasma flame simulation working condition. The coating can maintain performance for 2 hours at 1000 ℃.
Detailed Description
Example 1
Uniformly mixing 800g of titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder with the particle size of 1.6 microns (the mass ratio of the titanium dioxide hollow microspheres to the polyaryl organic silicon resin is 1:7), 180g of aminosilane (the number average molecular weight is 1000) and 100g of dimethylformamide to obtain a material A; 100g of POSS graft modified epoxy resin (the mass ratio of POSS to epoxy resin is 1:20) and 50g of ZrO2/Y2O3/Nb2O5Uniformly mixing powder (the particle size is 1.4 microns) and 80g of dimethylformamide to obtain a material B; and uniformly mixing the material A, the material B and 200g of heat-absorbing filler (a mixture of glass powder and aluminum powder, the mass ratio of the glass powder to the aluminum powder is 1:2, and the average particle size is 2 microns) to obtain the organic-inorganic hybrid ablation-resistant coating.
Example 2
Uniformly mixing 850g of titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder with the particle size of 1.6 microns (the mass ratio of the titanium dioxide hollow microspheres to the polyaryl organic silicon resin is 1:7), 210g of aminosilane (the number average molecular weight is 2000) and 130g of dimethylformamide to obtain a material A; 130g of POSS graft modified epoxy resin (the mass ratio of POSS to epoxy resin is 1.2:20) and 70g of ZrO2/Y2O3/Nb2O5Uniformly mixing powder (the particle size is 1.4 microns) and 100g of dimethylformamide to obtain a material B; uniformly mixing the material A, the material B and 250g of heat absorption filler (a mixture of glass powder and aluminum powder, the mass ratio of the glass powder to the aluminum powder is 1:7, and the average particle size is 2 microns) to obtain the organic-inorganic hybrid ablation-resistant coating.
Example 3
Taking 900g of titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder with the particle size of 1.6 microns (the mass ratio of the titanium dioxide hollow microspheres to the polyaryl organic silicon resin is 2:7) and250g of aminosilane (with the number average molecular weight of 3000) and 180g of dimethylformamide are uniformly mixed to obtain a material A; 160g of POSS graft modified epoxy resin (the mass ratio of POSS to epoxy resin is 1.2:20) and 90g of ZrO2/Y2O3/Nb2O5Uniformly mixing powder (the particle size is 1.4 microns) and 100g of dimethylformamide to obtain a material B; and uniformly mixing the material A, the material B and 300g of heat absorption filler (a mixture of glass powder and aluminum powder, the mass ratio of the glass powder to the aluminum powder is 3:2, and the average particle size is 2 microns) to obtain the organic-inorganic hybrid ablation-resistant coating.
The coatings of examples 1 to 3 were applied to the surface of stainless steel to form a 0.2mm thick coating, thoroughly dried and then tested for ablation by plasma flame simulation.
Comparative example 1, the coating of chinese patent application 201310209072.2 was applied to a stainless steel body using the application method of the present invention to form a 0.2mm thick coating, which was thoroughly dried and then subjected to an ablation test using plasma flame simulation.
Comparative example 2 the coating of chinese patent application 201310269529.9 was applied to a stainless steel body using the application method of the present invention to form a 0.2mm thick coating which was thoroughly dried and then tested for ablation by plasma flame simulation.
Data of performance test of examples and comparative examples
TABLE 1 test data for ablation resistance of coatings
The upper and lower limit values and interval values of the use amount of each raw material and the upper and lower limit values and interval values of the component parameters can realize the invention, and the embodiment is not listed in detail here.
The scope of the present invention is not limited thereto, and any changes or substitutions that can be easily made by those skilled in the art within the technical scope of the present invention will be covered by the scope of the present invention.
Claims (6)
1. An organic-inorganic hybrid ablation-resistant coating is characterized by comprising the following components: titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder, double-ended aminosilane with molecular weight of 1000-3000, POSS (polyhedral oligomeric silsesquioxane) graft modified epoxy resin and ZrO2/Y2O3/Nb2O5A powder and a heat absorbing filler; the weight parts of the components are as follows:
the preparation method of the titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder comprises the following steps: uniformly spraying a silane coupling agent solution on the titanium dioxide hollow microspheres, standing for 10-20 minutes, then mixing the titanium dioxide hollow microspheres with an organic silicon resin monomer for reaction to obtain polyaryl organic silicon resin, and crushing the polyaryl organic silicon resin to obtain powder with the average particle size of 1.6 microns;
the heat absorption filler is a mixture of glass powder and aluminum powder, and the mass ratio of the glass powder to the aluminum powder is as follows: the aluminum powder is 1-3:2-7, and the average particle size is 2 microns;
the mass ratio of the titanium dioxide hollow microspheres to the polyaryl organic silicon resin in the titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder is 1-2: 7;
the mass ratio of POSS to epoxy resin in the POSS graft modified epoxy resin is 1-1.2: 20.
2. The organic-inorganic hybrid ablation-resistant coating as claimed in claim 1, wherein the organic-inorganic hybrid ablation-resistant coating comprises the following components in parts by weight:
3. the organic-inorganic hybrid ablation-resistant coating as claimed in claim 1, wherein the organic-inorganic hybrid ablation-resistant coating comprises the following components in parts by weight:
4. the organic-inorganic hybrid ablation-resistant coating as claimed in claim 1, wherein the organic-inorganic hybrid ablation-resistant coating comprises the following components in parts by weight:
5. the preparation method of the organic-inorganic hybrid ablation-resistant coating as claimed in claim 1, which is characterized by comprising the following steps:
uniformly mixing titanium dioxide hollow microsphere modified polyaryl organic silicon resin powder, aminosilane with molecular weight of 1000-3000 and part of dimethylformamide to obtain material A, and mixing POSS modified epoxy resin and ZrO2/Y2O3/Nb2O5And uniformly mixing the powder and the residual dimethylformamide to obtain a material B, and uniformly mixing the material A, the material B and the heat-absorbing filler to obtain the organic-inorganic hybrid ablation-resistant coating.
6. A coating layer characterized by being applied from the organic-inorganic hybrid ablation-resistant coating material of any one of claims 1 to 4.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106995641A (en) * | 2017-04-25 | 2017-08-01 | 晶锋集团股份有限公司 | Epoxy resin-matrix heat conductive insulating coating that a kind of epoxy radicals polyhedral silsesquioxane is modified and preparation method thereof |
| CN108947591A (en) * | 2018-08-24 | 2018-12-07 | 中国航空制造技术研究院 | A kind of high temperature insulating protective coating structure and preparation method thereof |
| CN111019424A (en) * | 2019-12-04 | 2020-04-17 | 北京科技大学 | Vacuum ceramic microbead heat-insulating anticorrosive paint for steel structure equipment and preparation method thereof |
| CN111171721A (en) * | 2020-01-22 | 2020-05-19 | 西安近代化学研究所 | Ceramizable ablation-resistant coating and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106995641A (en) * | 2017-04-25 | 2017-08-01 | 晶锋集团股份有限公司 | Epoxy resin-matrix heat conductive insulating coating that a kind of epoxy radicals polyhedral silsesquioxane is modified and preparation method thereof |
| CN108947591A (en) * | 2018-08-24 | 2018-12-07 | 中国航空制造技术研究院 | A kind of high temperature insulating protective coating structure and preparation method thereof |
| CN111019424A (en) * | 2019-12-04 | 2020-04-17 | 北京科技大学 | Vacuum ceramic microbead heat-insulating anticorrosive paint for steel structure equipment and preparation method thereof |
| CN111171721A (en) * | 2020-01-22 | 2020-05-19 | 西安近代化学研究所 | Ceramizable ablation-resistant coating and preparation method thereof |
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