CN107760194A - A kind of anti-heat insulating coat of silicon rubber base and preparation method thereof - Google Patents
A kind of anti-heat insulating coat of silicon rubber base and preparation method thereof Download PDFInfo
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- CN107760194A CN107760194A CN201710944900.5A CN201710944900A CN107760194A CN 107760194 A CN107760194 A CN 107760194A CN 201710944900 A CN201710944900 A CN 201710944900A CN 107760194 A CN107760194 A CN 107760194A
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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
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/56—Three layers or more
- B05D7/58—No clear coat specified
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
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- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention provides a kind of anti-heat insulating coat of silicon rubber base and preparation method thereof, including heat insulating coat, radiation coating and ablative coating；The heat insulating coat is arranged on substrate surface, and the radiation coating is arranged between heat insulating coat and ablative coating；The heat insulating coat, radiation coating and ablative coating are silicon rubber base coating；The radiation coating carries out in-situ ceramic reaction by penetrating the heat of ablative coating；Polyparaphenylene Benzo-dioxazole fiber is distributed with the ablative coating.Made Preparation Method includes preparing ablative coating, radiation coating and heat insulating coat.Compared to prior art, the present invention has the advantages that：The mechanical property of ablative coating is improved using polyparaphenylene Benzo-dioxazole fiber, high radiation coating is prepared for by in-situ ceramicization reaction, successfully solve the drawbacks of silicon rubber base thermal protective coating mechanical property and relatively low anti-heat-proof quality, there is wide application prospect in thermal protection fields such as rocket delivery, missile armament body structure surfaces.
Description
Technical field
The present invention relates to field of material technology, in particular it relates to a kind of anti-heat insulating coat of silicon rubber base and preparation method thereof.
Background technology
For the boosting module afterbody of high thrust carrier rocket 3350 by more engine wake effects, hot-fluid is high in short-term on surface, needs
Thermal protection processing is carried out to boosting module aluminum alloy surface, to ensure its structural-load-carrying capacity.Coating is due to its convenient construction, matter
Amount uniformity is good and turns into a kind of effective thermal protection means.But the ablative-type protective coating thermal protective coating of single kind is due to added with a large amount of
Inorganic heat-resistant filler, poor mechanical property；Radiation coating density is big, complicated can not disposably make in extreme hot-fluid environment
Promote the use of on rocket surface；And insulating moulding coating is generally using polyurethane or epoxy resin as matrix, intolerant to ablation, therefore single work(
The thermal protective coating of energy can not meet high-heat environment condition to the growing active demand of efficient anti-thermal technology.
At present, in the prior art there is not yet having among ablative coating and heat insulating coat, reaction in-situ builds one layer
The report of the anti-heat insulating coat of silicon rubber base of radiation coating presoma.
The content of the invention
For the deficiency of simple function thermal protective coating in the prior art, it is an object of the invention to provide a kind of silicon rubber base to prevent
Heat insulating coat and preparation method thereof.The mechanical property of ablative coating is improved using polyparaphenylene Benzo-dioxazole fiber, is being burnt
One layer of radiation presoma coating of structure among erosion resisting coating and heat insulating coat, ceramic is carried out using the heat for penetrating ablative coating,
Heat will be penetrated while consumption of calorie is absorbed in the form of strong infra-red radiation to be transmitted into surrounding medium, so as to further carry
The anti-thermal effect of height combination coating.
The purpose of the present invention is achieved through the following technical solutions：
In a first aspect, the present invention provides a kind of anti-heat insulating coat of silicon rubber base, including heat insulating coat, radiation coating and ablation
Coating；The heat insulating coat is arranged on substrate surface, and the radiation coating is arranged between heat insulating coat and ablative coating；
The heat insulating coat, radiation coating and ablative coating are silicon rubber base coating；The radiation coating is by penetrating
The heat of ablative coating carries out in-situ ceramic reaction；Polyparaphenylene Benzo-dioxazole fibre is distributed with the ablative coating
Dimension.
Preferably, the thickness of the ablative coating is 0.1mm~2mm.0.1mm is that can be formed after ablative coating sprays one time
The limiting value of uniform liquid film, and penetrate shortage of heat if coating layer thickness is more than 2mm and reacted with starting ceramic in radiation coating.
Preferably, the thickness of the radiation coating is 0.1mm~5mm.0.1mm is that can be formed after radiation coating sprays one time
The limiting value of uniform liquid film, and if radiation coating thickness more than 5mm, coating can produce sagging phenomenon, and surface quality is bad.
Preferably, the thickness of the heat insulating coat is 0.1mm~5mm.Heat insulating coat select the reason for thickness range with
Radiation coating is identical.
Preferably, the heat insulating coat includes each component of following quality parts ratio：Lighting thermal insulating filling, surface treatment
Agent, white carbon, methyl silicone rubber rubber, tetraethyl orthosilicate, dibutyl tin laurate, toluene quality parts ratio for (5~
25)：2：20：100：3：1：200.In above-mentioned heat insulating coat each component, rise main effect of heat insulation be lighting thermal insulating filling and
Surface conditioning agent, wherein, thermal conductivity on the one hand can be reduced from lighting thermal insulating filling, improves the heat-insulated effect of heat insulating coat
Fruit, heat insulating coat density on the other hand can be reduced, improve heat insulating coat utilization ratio (the heat-insulated effect that unit mass coating reaches
Fruit).And the compatibility of lighting thermal insulating filling and methyl silicone rubber matrix can be improved from surface conditioning agent, improve lighting
Dispersing uniformity of the thermal insulating filling in methyl silicone rubber matrix.Other components are commercially available methyl silicone rubber rubber and its reinforcement
Agent, curing agent, catalysts and solvents.
Methyl silicone rubber rubber can not use phenyl siloxane rubber rubber to substitute in the heat insulating coat of the present invention, and reason is phenyl silicon
Remaining carbon is more than methyl silicone rubber rubber remaining carbon when rubber is thermally decomposed, and carbon is the good conductor of heat, the increase meeting of remaining carbon
Reduce the effect of heat insulation of heat insulating coat.In addition, the phenyl siloxane rubber rubber in ablative coating can not be replaced with methyl silicone rubber rubber
In generation, reason is better than methyl silicone rubber for the heat endurance of phenyl siloxane rubber, favourable to the heat endurance of ablative coating.And radiation applies
Phenyl siloxane rubber rubber in layer can not use methyl silicone rubber rubber to substitute, and reason is the carbon residue that phenyl siloxane rubber is thermally decomposed
It is one of raw material in ceramic reaction, and methyl silicone rubber is thermally decomposed caused remaining carbon deficiency.
Preferably, the lighting thermal insulating filling in hollow glass micro-ball, hollow phenolic aldehyde microballoon, cork powder one
Kind.Above-mentioned filler is hollow or porous type low-density light filler.
Preferably, the surface conditioning agent is selected from gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl three
One kind in methoxy silane, γ-(methacryloxy) propyl trimethoxy silicane.Above-mentioned three kinds of surface conditioning agents are
One end is that three alkoxy grp other ends are short aliphatic chain functional group (aminopropyl, glycidyl ether oxygen propyl, methacryloxypropyl
Base propyl group) silane coupler, caused hydroxyl can be bonded with lighting filler surface hydroxyl after alkoxy grp hydrolysis, and another
The short aliphatic chain functional group at end has splendid compatibility with nonpolar methyl silicone rubber, so as to improve lighting filler in first
Dispersiveness in base silicone rubber matrix.
Preferably, the radiation coating includes each component of following quality parts ratio：Mica, silicon powder, white carbon, phenyl
Raw-silastic continuously, curing agent, dibutyl tin laurate, the mass fraction ratio of toluene are (15~30)：(5~10)：20：100：
3：1：200.Mica, silicon powder are the primary raw materials of ceramic reaction in said components, and phenyl siloxane rubber is except the basic film forming of offer
Outside the cementation of material, carbon residue caused by its thermal decomposition is also one of ceramic reaction；Other groups are commercially available reinforcing agent, solidification
Agent, catalysts and solvents.
Preferably, in radiation coating, the mass fraction of silicon is 30%~50% in the phenyl siloxane rubber rubber.If phenyl
The mass fraction of silicon is less than 30% in raw-silastic continuously, shows phenyl group content height, then is thermally decomposed caused remaining carbon mistake
It can cause to generate the low easy efflorescence of ceramics strength more, radiation ceramic layer can not be formed heat is transmitted into surrounding medium；If phenyl
The mass fraction of silicon is higher than 50% in raw-silastic continuously, and surface phenyl collection mass contg is low, then is thermally decomposed caused remaining carbon not
Foot, ceramic reaction raw materials deficiency, can not equally form radiation ceramic layer.Methyl silicone rubber rubber and ablation in heat insulating coat
Influence of the silicon mass content of phenyl siloxane rubber rubber to respective coatings is smaller in coating.
Preferably, the curing agent is tetraethyl orthosilicate, positive silicic acid propyl ester, MTES, the ethoxy of phenyl three
One kind in base silane, phenyltrimethoxysila,e.Above-mentioned curing agent is dealcoholized cold curing agent, is given birth in the curing process
Into alcohols material can gradually from solidification crosslinking silicon rubber in spread effusion.
Preferably, the ablative coating includes each component of following quality parts ratio：Polyparaphenylene Benzo-dioxazole is fine
Dimension, surface modifier, iron oxide, calcium carbonate, white carbon, phenyl siloxane rubber rubber, tetraethyl orthosilicate, di lauric dibutyl
Tin, the quality parts ratio of toluene are (1~10)：(0.5~2)：(1~5)：30：20：100：3：1：200.
Preferably, the length of the polyparaphenylene Benzo-dioxazole fiber is 0.1~1 centimetre.If fibre length is less than
0.1 centimetre, then its reinforcing effect unobvious to silicon rubber；If fibre length is more than 1 centimetre, fiber is easy in whipping process
It is not easy to disperse into knot, and spray gun discharging opening is also easily blocked in spraying process.
Preferably, the surface modifier is the phosphate compounds of the substituted radical containing 5~18 carbon atom chain lengths.
If phosphate compounds substituent length is less than 5 carbon atoms, whole compound nonpolar action is weak, with phenyl siloxane rubber
The poor compatibility of nonpolar polysiloxane molecule chain in matrix；If phosphate compounds substituent length is more than 18 carbon originals
Son, then whole compound polarity effect is weak, poor with the pbo fiber surface action with polar group, causes fiber surface modification to be made
Use unobvious.
It is highly preferred that the surface modifier is two (2- (methylacryloyl epoxide) ethyl) phosphoric acid or castor-oil plant oleophosphoric acid
Ester.Two (2- (methylacryloyl epoxide) ethyl) phosphoric acid or the semipolar phosphate groups part of castor oil phosphate ester with pole
Property group pbo fiber surface produce esterification and the strong interaction such as hydrogen bond, (methylacryloyl epoxide) ethyl and castor simultaneously
Aliphatic chain in sesame oil has fabulous compatibility with the polysiloxane molecule chain in phenyl siloxane rubber matrix, so as to improve PBO
The interface binding power of fiber and phenyl siloxane rubber matrix.
Further, as shown in Fig. 2 the structure of the ablative coating is not wound between pbo fiber independently uniformly to divide
Be dispersed in phenyl siloxane rubber matrix (Fig. 2 is left), and have layer of surface modifying agent on pbo fiber surface (Fig. 2 is right).Because surface is modified
The semipolar phosphate groups part of agent produces the strong interactions such as esterification and hydrogen bond with the pbo fiber surface with polar group,
The aliphatic chain in (methylacryloyl epoxide) ethyl and castor oil has fabulous compatibility with phenyl siloxane rubber matrix simultaneously,
The interface binding power of pbo fiber and phenyl siloxane rubber matrix can be improved, so as to be greatly improved the mechanical strength of ablative coating.And
Pbo fiber is high-temperature resistant special fiber, and the introducing of pbo fiber can improve the high temperature resistant thermal protective performance of ablative coating.
Second aspect, the present invention provide a kind of preparation method of the anti-heat insulating coat of silicon rubber base, comprised the following steps：
S1, with solvent will be sprayed-on substrate surface wiped clean, by lighting thermal insulating filling, surface conditioning agent, white carbon,
Methyl silicone rubber rubber, tetraethyl orthosilicate, dibutyl tin laurate, toluene press quality parts ratio (5~25)：2：20：100：
3：1：200 uniformly mixing, are filtered by 30~40 mesh filter screens after mixing, filtrate are sprayed at into substrate surface, obtains heat insulating coat；
S2, mica, silicon powder, white carbon, phenyl siloxane rubber rubber, curing agent, dibutyl tin laurate, toluene pressed
Mass fraction ratio (15~30)：(5~10)：20：100：3：1：200 uniformly mixing, are filtered after mixing by 30~40 mesh filter screens,
Filtrate is sprayed to the surface for the heat insulating coat that step S1 is obtained, obtains radiation coating；
S3, by polyparaphenylene Benzo-dioxazole fiber, surface modifier, iron oxide, calcium carbonate, white carbon, phenyl silicon
Rubber raw rubber, tetraethyl orthosilicate, dibutyl tin laurate, toluene press quality parts ratio (1~10)：(0.5~2)：(1~5)：
30：20：100：3：1：200 uniformly mixing, are filtered by 30~40 mesh filter screens after mixing, filtrate are sprayed at into what step S2 was obtained
The surface of radiation coating, obtains ablative coating.
, can not will may be mixed miscellaneous in coating preparation process if screen specification is less than 30 mesh in above-mentioned filtration step
Matter particulate matter filters out, and causing impurity to be finally sprayed into product surface influences coating surface quality；If screen specification is higher than 40 mesh,
Then easily pbo fiber is filtered out, causes the content of coating ingredients inaccurate.
Preferably, for above-mentioned S1 into S3 steps, the filter screen is wire netting；The spraying uses spray gun with 0.5MPa pressure
Power is sprayed filtrate.
Compared with prior art, the present invention has following beneficial effect：
1st, it is compound using polyparaphenylene Benzo-dioxazole fiber and phenyl siloxane rubber, changed in compound preparation process with surface
Property agent improve the interface cohesion of polyparaphenylene Benzo-dioxazole fiber and phenyl siloxane rubber matrix and act on, applied so as to improve ablation
The mechanical property of layer.Such as using other fibers with silicon rubber is compound can not reach same effect, such as the stretching of aramid fiber
Intensity (2.82GPa) is only the half of polyparaphenylene Benzo-dioxazole tensile strength of fiber (5.80GPa), mechanics enhancing effect
It is bad；And carbon fiber T800 tensile strength is also only 5.49GPa, and carbon fiber T800 density is 1.81g/cm3 higher than poly-
To the 1.54g/cm3 of phenylene Benzo-dioxazole fibre density, it is unfavorable for the lighting of coating.
2nd, high radiation coating is prepared for by in-situ ceramicization reaction using the heat for penetrating ablative coating, consumed absorbing
Follow-up arrival heat will be penetrated heat in the form of strong infra-red electromagnetic wave radiation and be transmitted into ring by the ceramics generated while heat
In the medium of border, so as to further improve the anti-thermal effect of combination coating.Successfully solves silicon rubber base thermal protective coating mechanical property
With anti-heat-proof quality it is relatively low the drawbacks of, the thermal protection fields such as rocket delivery, missile armament body structure surface have extensively using before
Scape.
Brief description of the drawings
The detailed description made by reading with reference to the following drawings to non-limiting example, further feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the structural representation of the anti-heat insulating coat of silicon rubber base of the present invention；
Fig. 2 is the structural representation of ablative coating in the present invention.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, some changes and improvements can also be made.These belong to the present invention
Protection domain.
Embodiment 1
The present embodiment is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method is as follows：
(1) to dip acetone with degreasing veil will be sprayed-on substrate surface wiped clean, by 10g hollow glass micro-balls, 2g
Gamma-aminopropyl-triethoxy-silane, 20g white carbons, 100g methyl silicone rubbers rubber, 3g tetraethyl orthosilicates, 1g tin dilaurates two
Butyl tin and 200g toluene are mixed, with 30~40 mesh metal mesh filters after stirring, with spray gun with 0.5MPa pressure
Filtrate is sprayed at substrate surface, obtains silicon rubber base heat insulating coat, heat insulating coat thickness control is 5mm；
(2) by 15g micas, 5g silicon powders, 20g white carbons, 100g silicon mass fraction be 33% phenyl siloxane rubber rubber,
3g tetraethyl orthosilicates, 1g dibutyl tin laurates and 200g toluene are mixed, with 30~40 mesh wire nettings after stirring
Filtering, is sprayed at step (1) by filtrate with 0.5MPa pressure with spray gun and obtains heat insulating coat surface, obtain heat insulating coat substrate
Radiation coating, radiation coating thickness control is 2.5mm；
(3) by polyparaphenylene Benzo-dioxazole fiber of the 1g length for 1 centimetre, (2- (the methylacryloyl oxygen of 0.5g bis-
Base) ethyl) phosphoric acid, 2g iron oxide, 30g calcium carbonate, 20g white carbons, 100g phenyl siloxane rubbers rubber, 3g tetraethyl orthosilicates, 1g
Dibutyl tin laurate and 200g toluene are mixed, with 30~40 mesh metal mesh filters after stirring, with spray gun with
Filtrate is sprayed at the radiation coating surface for the heat insulating coat substrate that step (2) obtains, ablative coating thickness by 0.5MPa pressure
Control as 1.5mm, obtain being followed successively by the silicon rubber base of ablative coating, radiation coating, heat insulating coat by outer surface to base material order
Anti- heat insulating coat.As shown in Figure 1.
Embodiment 2
The present embodiment is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method is as follows：
(1) substrate surface wiped clean will be sprayed-on by dipping acetone with degreasing veil, by 20g hollow phenolic aldehyde microballoons, 2g
γ-(methacryloxy) propyl trimethoxy silicane, 20g white carbons, 100g methyl silicone rubbers rubber, the positive silicic acid second of 3g
Ester, 1g dibutyl tin laurates and 200g toluene are mixed, and with 30~40 mesh metal mesh filters after stirring, use spray gun
Filtrate is sprayed at by substrate surface with 0.5MPa pressure, obtains silicon rubber base heat insulating coat, heat insulating coat thickness control is
0.1mm；
(2) by 30g micas, 8g silicon powders, 2g white carbons, 100g silicon mass fraction be 42% phenyl siloxane rubber rubber,
3g positive silicic acid propyl esters, 1g dibutyl tin laurates and 200g toluene are mixed, with 30~40 mesh wire nettings after stirring
Filtering, is sprayed at step (1) by filtrate with 0.5MPa pressure with spray gun and obtains heat insulating coat surface, obtain heat insulating coat substrate
Radiation coating, radiation coating thickness control is 5mm；
(3) polyparaphenylene Benzo-dioxazole fiber, 2g castor oil phosphate esters, 5g that 5g length is 0.5 centimetre are aoxidized
Iron, 30g calcium carbonate, 20g white carbons, 100g phenyl siloxane rubbers rubber, 3g tetraethyl orthosilicates, 1g dibutyl tin laurates and
200g toluene is mixed, and with 30~40 mesh metal mesh filters after stirring, is sprayed filtrate with 0.5MPa pressure with spray gun
The radiation coating surface for the heat insulating coat substrate that step (2) obtains is applied to, ablative coating thickness control is 2mm, is obtained by appearance
Face to base material order is followed successively by the anti-heat insulating coat of silicon rubber base of ablative coating, radiation coating, heat insulating coat.
Embodiment 3
The present embodiment is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method is as follows：
(1) substrate surface wiped clean will be sprayed-on by dipping acetone with degreasing veil, by 5g corks powder, 2g γ-shrink
Glycerine ether oxygen propyl trimethoxy silicane, 20g white carbons, 100g methyl silicone rubbers rubber, 3g tetraethyl orthosilicates, 1g tin dilaurates
Dibutyl tin and 200g toluene are mixed, with 30~40 mesh metal mesh filters after stirring, with spray gun with 0.5MPa pressure
Filtrate is sprayed at substrate surface by power, obtains silicon rubber base heat insulating coat, and heat insulating coat thickness control is 2.5mm；
(2) 25g micas, 10g silicon powders, 20g white carbons, the phenyl siloxane rubber that 100g silicon mass fraction is 30% are given birth to
Glue, 3g phenyltrimethoxysila,es, 1g dibutyl tin laurates and 200g toluene are mixed, with 30~40 after stirring
Mesh metal mesh filter, filtrate is sprayed at by step (1) with 0.5MPa pressure with spray gun and obtains heat insulating coat surface, is obtained heat-insulated
The radiation coating of coated substrate, heat insulating coat thickness control are 0.1mm；
(3) by polyparaphenylene Benzo-dioxazole fiber of the 10g length for 0.7 centimetre, the (2- (methacryls of 1.0g bis-
Base epoxide) ethyl) phosphoric acid, 1g iron oxide, 30g calcium carbonate, 20g white carbons, 100g phenyl siloxane rubbers rubber, the positive silicic acid second of 3g
Ester, 1g dibutyl tin laurates and 200g toluene are mixed, and with 30~40 mesh metal mesh filters after stirring, use spray gun
Filtrate is sprayed to the radiation coating surface for the heat insulating coat substrate that step (2) obtains with 0.5MPa pressure, ablative coating is thick
Degree control is 2mm, obtains being followed successively by the silicon rubber base of ablative coating, radiation coating, heat insulating coat by outer surface to base material order
Anti- heat insulating coat.
Embodiment 4
The present embodiment is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method is as follows：
(1) to dip acetone with degreasing veil will be sprayed-on substrate surface wiped clean, by 25g hollow glass micro-balls, 2g
Gamma-aminopropyl-triethoxy-silane, 20g white carbons, 100g methyl silicone rubbers rubber, 3g tetraethyl orthosilicates, 1g tin dilaurates two
Butyl tin and 200g toluene are mixed, with 30~40 mesh metal mesh filters after stirring, with spray gun with 0.5MPa pressure
Filtrate is sprayed at substrate surface, obtains silicon rubber base heat insulating coat, heat insulating coat thickness control is 0.5mm；
(2) by 15g micas, 7g silicon powders, 20g white carbons, 100g silicon mass fraction be 50% phenyl siloxane rubber rubber,
3g tetraethyl orthosilicates, 1g dibutyl tin laurates and 200g toluene are mixed, with 30~40 mesh wire nettings after stirring
Filtering, is sprayed at step (1) by filtrate with 0.5MPa pressure with spray gun and obtains heat insulating coat surface, obtain heat insulating coat substrate
Radiation coating, radiation coating thickness control is 1mm；
(3) by polyparaphenylene Benzo-dioxazole fiber of the 3g length for 0.1 centimetre, the (2- (methylacryloyls of 1.5g bis-
Epoxide) ethyl) phosphoric acid, 2g iron oxide, 30g calcium carbonate, 20g white carbons, 100g phenyl siloxane rubbers rubber, 3g tetraethyl orthosilicates,
1g dibutyl tin laurates and 200g toluene are mixed, with 30~40 mesh metal mesh filters after stirring, with spray gun with
Filtrate is sprayed at the radiation coating surface for the heat insulating coat substrate that step (2) obtains, ablative coating thickness by 0.5MPa pressure
Control as 0.1mm, obtain being followed successively by the silicon rubber base of ablative coating, radiation coating, heat insulating coat by outer surface to base material order
Anti- heat insulating coat.
Comparative example 1
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method and embodiment 1 are basically identical, difference
Be in：Ablative coating is not sprayed, obtains being followed successively by the silicon rubber base of radiation coating, heat insulating coat by outer surface to base material order
Anti- heat insulating coat.
Comparative example 2
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method and embodiment 1 are basically identical, difference
Be in：Radiation coating is not sprayed, obtains being followed successively by the silicon rubber base of ablative coating, heat insulating coat by outer surface to base material order
Anti- heat insulating coat.
Comparative example 3
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method and embodiment 1 are basically identical, difference
Be in：Heat insulating coat is not sprayed, obtains being followed successively by the silicon rubber base of ablative coating, radiation coating by outer surface to base material order
Anti- heat insulating coat.
Comparative example 4
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method and embodiment 1 are basically identical, difference
Be in：In step (3), polyparaphenylene Benzo-dioxazole fiber is replaced using aramid fiber.
Comparative example 5
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method and embodiment 1 are basically identical, difference
Be in：In step (3), two (2- (methylacryloyl epoxide) ethyl) phosphorus are replaced using tributyl phosphate surface modifier
Acid.
Comparative example 6
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method and embodiment 1 are basically identical, difference
Be in：In step (1), the methyl silicone rubber rubber is replaced using phenyl siloxane rubber rubber.
Comparative example 7
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and its preparation method and embodiment 1 are basically identical, difference
Be in：In step (2), the mass fraction of silicon is 65% in the phenyl siloxane rubber rubber.
Performance test
Using the standard testing coating densities of QJ 990.13, using the standard testing thermal conductivities of GB/T 10295, using GB/T
The various embodiments described above and each comparative example are tested by 1040.2 standard testing coating tensile strengths and elongation at break, test
As a result it is as shown in table 1 below：
Table 1
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or change within the scope of the claims, this not shadow
Ring the substantive content of the present invention.In the case where not conflicting, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (10)
1. a kind of anti-heat insulating coat of silicon rubber base, it is characterised in that including heat insulating coat, radiation coating and ablative coating；It is described
Heat insulating coat is arranged on substrate surface, and the radiation coating is arranged between heat insulating coat and ablative coating；
The heat insulating coat, radiation coating and ablative coating are silicon rubber base coating；The radiation coating is by penetrating ablation
The heat of coating carries out in-situ ceramic reaction；Polyparaphenylene Benzo-dioxazole fiber is distributed with the ablative coating.
2. the anti-heat insulating coat of silicon rubber base according to claim 1, it is characterised in that the heat insulating coat includes following matter
Measure each component of portion rate：Lighting thermal insulating filling, surface conditioning agent, white carbon, methyl silicone rubber rubber, tetraethyl orthosilicate,
Dibutyl tin laurate, the quality parts ratio of toluene are (5~25)：2：20：100：3：1：200.
3. the anti-heat insulating coat of silicon rubber base according to claim 2, it is characterised in that the lighting thermal insulating filling is selected from
One kind in hollow glass micro-ball, hollow phenolic aldehyde microballoon, cork powder.
4. the anti-heat insulating coat of silicon rubber base according to claim 2, it is characterised in that the surface conditioning agent be selected from γ-
Aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxy) propyl group three
One kind in methoxy silane.
5. the anti-heat insulating coat of silicon rubber base according to claim 1, it is characterised in that the radiation coating includes following matter
Measure each component of portion rate：Mica, silicon powder, white carbon, phenyl siloxane rubber rubber, curing agent, dibutyl tin laurate, first
The mass fraction ratio of benzene is (15~30)：(5~10)：20：100：3：1：200.
6. the anti-heat insulating coat of silicon rubber base according to claim 5, it is characterised in that silicon in the phenyl siloxane rubber rubber
Mass fraction be 30%~50%.
7. the anti-heat insulating coat of silicon rubber base according to claim 5, it is characterised in that the curing agent is positive silicic acid second
One kind in ester, positive silicic acid propyl ester, MTES, phenyl triethoxysilane, phenyltrimethoxysila,e.
8. the anti-heat insulating coat of silicon rubber base according to claim 1, it is characterised in that the ablative coating includes following matter
Measure each component of portion rate：Polyparaphenylene Benzo-dioxazole fiber, surface modifier, iron oxide, calcium carbonate, white carbon, benzene
Base raw-silastic continuously, tetraethyl orthosilicate, dibutyl tin laurate, the quality parts ratio of toluene are (1~10)：(0.5~2)：
(1~5)：30：20：100：3：1：200.
9. the anti-heat insulating coat of silicon rubber base according to claim 8, it is characterised in that the surface modifier be containing 5~
The phosphate compounds of the substituted radical of 18 carbon atom chain lengths.
10. a kind of preparation method of anti-heat insulating coat of silicon rubber base according to claim any one of 1-9, its feature exist
In comprising the following steps：
S1, with solvent substrate surface wiped clean will be sprayed-on, by lighting thermal insulating filling, surface conditioning agent, white carbon, methyl
Raw-silastic continuously, tetraethyl orthosilicate, dibutyl tin laurate, toluene press quality parts ratio (5~25)：2：20：100：3：1：
200 uniformly mixing, are filtered by 30~40 mesh filter screens after mixing, filtrate are sprayed at into substrate surface, obtains heat insulating coat；
S2, mica, silicon powder, white carbon, phenyl siloxane rubber rubber, curing agent, dibutyl tin laurate, toluene pressed into quality
Score ratio (15~30)：(5~10)：20：100：3：1：200 uniformly mixing, are filtered by 30~40 mesh filter screens after mixing, will filtered
Liquid is sprayed at the surface for the heat insulating coat that step S1 is obtained, and obtains radiation coating；
S3, by polyparaphenylene Benzo-dioxazole fiber, surface modifier, iron oxide, calcium carbonate, white carbon, phenyl siloxane rubber
Rubber, tetraethyl orthosilicate, dibutyl tin laurate, toluene press quality parts ratio (1~10)：(0.5~2)：(1~5)：30：
20：100：3：1：200 uniformly mixing, are filtered after mixing by 30~40 mesh filter screens, and filtrate is sprayed at into the spoke that step S2 obtains
The surface of coating is penetrated, obtains ablative coating.
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