CN107760194B - 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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- CN107760194B CN107760194B CN201710944900.5A CN201710944900A CN107760194B CN 107760194 B CN107760194 B CN 107760194B CN 201710944900 A CN201710944900 A CN 201710944900A CN 107760194 B CN107760194 B CN 107760194B
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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 present invention provides a kind of anti-heat insulating coats of silicon rubber base and preparation method thereof, including heat insulating coat, radiation coating and ablative coating；In substrate surface, the radiation coating is arranged between heat insulating coat and ablative coating for the heat insulating coat setting；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 in the ablative coating.Made Preparation Method includes preparing ablative coating, radiation coating and heat insulating coat.Compared with the prior art, the invention has the following beneficial effects: the mechanical properties that ablative coating is improved using polyparaphenylene benzo dioxazole fiber, high radiation coating is prepared for by in-situ ceramicization reaction, it successfully solves silicon rubber base thermal protective coating mechanical property and the relatively low drawback of anti-heat-proof quality, there is wide application prospect in thermal protections fields such as rocket delivery, missile armament body structure surfaces.
Description
Technical field
The present invention relates to field of material technology, and in particular, to a kind of anti-heat insulating coat of silicon rubber base and preparation method thereof.
Background technique
3350 boosting module tail portion of high thrust carrier rocket is by more engine wake effects, and hot-fluid is high in short-term on surface, needs
Thermal protection processing is carried out to boosting module aluminum alloy surface, to guarantee its structural-load-carrying capacity.Coating is due to its convenient construction, matter
Amount consistency is good and becomes 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, structure is complicated disposably to make in extreme hot-fluid environment
It promotes the use of on rocket surface；And insulating moulding coating is usually using polyurethane or epoxy resin as matrix, intolerant to ablation, therefore single function
The thermal protective coating of energy has been unable to satisfy high-heat environment condition to the growing urgent need of efficient anti-thermal technology.
Currently, reaction in-situ constructs one layer in the prior art there is not yet having among ablative coating and heat insulating coat
The report of the anti-heat insulating coat of silicon rubber base of radiation coating presoma.
Summary of the invention
For the deficiency of simple function thermal protective coating in the prior art, it is anti-that the object of the present invention is to provide a kind of silicon rubber bases
Heat insulating coat and preparation method thereof.The mechanical property that ablative coating is improved using polyparaphenylene benzo dioxazole fiber, is being burnt
One layer of radiation presoma coating is constructed among erosion resisting coating and heat insulating coat, carries out ceramic using the heat for penetrating ablative coating,
Heat will be penetrated in the form of strong infra-red radiation while absorbing consumption of calorie to be emitted in surrounding medium, to further mention
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；In substrate surface, the radiation coating is arranged between heat insulating coat and ablative coating for the heat insulating coat setting；
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；It is fine that polyparaphenylene benzo dioxazole is distributed in the ablative coating
Dimension.
Preferably, the ablative coating with a thickness of 0.1mm~2mm.0.1mm is that can be formed after ablative coating sprays one time
The limiting value of uniform liquid film, and shortage of heat is penetrated if coating layer thickness is more than 2mm to start ceramic in radiation coating and react.
Preferably, the radiation coating with a thickness of 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 is more than 5mm, coating can generate sagging phenomenon, and surface quality is bad.
Preferably, the heat insulating coat with a thickness of 0.1mm~5mm.Heat insulating coat select the reason of thickness range with
Radiation coating is identical.
Preferably, the heat insulating coat includes each component of following mass parts ratio: lighting thermal insulating filling, surface treatment
Agent, white carbon black, methyl silicone rubber raw rubber, ethyl orthosilicate, dibutyl tin dilaurate, toluene mass parts ratio be (5~
25): 2:20:100:3:1:200.In above-mentioned heat insulating coat each component, rise main heat insulation be lighting thermal insulating filling and
Surface treating agent, wherein select lighting thermal insulating filling on the one hand can reduce thermal conductivity, improve the heat-insulated effect of heat insulating coat
On the other hand fruit can reduce heat insulating coat density, improve heat insulating coat utilization efficiency (the heat-insulated effect that unit mass coating reaches
Fruit).And select surface treating agent that can improve the compatibility of lighting thermal insulating filling Yu methyl silicone rubber matrix, improve lighting
Dispersing uniformity of the thermal insulating filling in methyl silicone rubber matrix.Other components are commercially available methyl silicone rubber raw rubber and its reinforcement
Agent, curing agent, catalysts and solvents.
Methyl silicone rubber raw rubber cannot be substituted with phenyl siloxane rubber raw rubber in heat insulating coat of the invention, and reason is phenyl silicon
Remaining carbon is greater than methyl silicone rubber raw rubber remaining carbon when rubber is thermally decomposed, and carbon is the good conductor of heat, the increase meeting of remaining carbon
Reduce the heat insulation of heat insulating coat.In addition, the phenyl siloxane rubber raw rubber in ablative coating cannot be replaced with methyl silicone rubber raw rubber
In generation, reason is that the thermal stability of phenyl siloxane rubber is better than methyl silicone rubber, advantageous to the thermal stability of ablative coating.And radiation applies
Phenyl siloxane rubber raw rubber in layer can not be substituted with methyl silicone rubber raw rubber, and reason is the carbon residue that phenyl siloxane rubber is thermally decomposed
It is one of the raw material in ceramic reaction, and the remaining carbon that methyl silicone rubber is generated by thermal decomposition is insufficient.
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 treating agent is selected from gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl three
One of methoxy silane, γ-(methacryloxy) propyl trimethoxy silicane.Above-mentioned three kinds of surface treating 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) silane coupling agent, the hydroxyl that generates can be bonded with lighting filler surface hydroxyl after alkoxy grp hydrolysis, and another
The short aliphatic chain functional group at end and nonpolar methyl silicone rubber have splendid compatibility, to improve lighting filler in first
Dispersibility in base silicone rubber matrix.
Preferably, the radiation coating includes each component of following mass parts ratio: mica, silicon powder, white carbon black, phenyl
Raw-silastic continuously, curing agent, dibutyl tin dilaurate, toluene mass fraction ratio be (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 substance, the carbon residue that thermal decomposition generates 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 raw rubber.If phenyl
The mass fraction of silicon is lower than 30% in raw-silastic continuously, shows the remaining carbon mistake that phenyl group content is high, then is generated by thermal decomposition
It will lead to more and generate the low easy dusting of ceramics strength, radiation ceramic layer can not be formed, heat is emitted in 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 not by the remaining carbon of thermal decomposition generation
Foot, ceramic reaction raw materials are insufficient, can not equally form radiation ceramic layer.Methyl silicone rubber raw rubber and ablation in heat insulating coat
Influence of the silicon mass content of phenyl siloxane rubber raw rubber to respective coatings is smaller in coating.
Preferably, the curing agent is ethyl orthosilicate, positive silicic acid propyl ester, methyltriethoxysilane, three ethoxy of phenyl
One of base silane, phenyltrimethoxysila,e.Above-mentioned curing agent is dealcoholized cold curing agent, is given birth in the curing process
At alcohols material can gradually from solidify crosslinking silicon rubber in spread evolution.
Preferably, the ablative coating includes each component of following mass parts ratio: polyparaphenylene benzo dioxazole is fine
Dimension, surface modifier, iron oxide, calcium carbonate, white carbon black, phenyl siloxane rubber raw rubber, ethyl orthosilicate, di lauric dibutyl
Tin, toluene mass parts ratio be (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 it is unobvious to the reinforcing effect of silicon rubber；If fibre length is greater than 1 centimetre, fiber is easy in whipping process
It is not easy to disperse at knot, and is also easy blocking spray gun discharge port in spraying process.
Preferably, the surface modifier is the phosphate compounds of the substituent group containing 5~18 carbon atom chain lengths.
If less than 5 carbon atoms of phosphate compounds substituent group length, entire compound nonpolar action is weak, with phenyl siloxane rubber
The poor compatibility of nonpolar polysiloxane molecule chain in matrix；If phosphate compounds substituent group length is greater than 18 carbon originals
Son, then entire compound polarity effect is weak, poor with the pbo fiber surface action with polar group, and fiber surface modification is caused to be made
With unobvious.
It is highly preferred that the surface modifier is two (2- (methylacryloyl oxygroup) ethyl) phosphoric acid or castor-oil plant oleophosphoric acid
Ester.Two (2- (methylacryloyl oxygroup) ethyl) phosphoric acid or the semipolar phosphate groups part of castor oil phosphate ester with pole
Property group pbo fiber surface generate esterification and the strong interactions such as hydrogen bond, (methylacryloyl oxygroup) ethyl and castor simultaneously
The polysiloxane molecule chain in aliphatic chain and phenyl siloxane rubber matrix in sesame oil has fabulous compatibility, 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
It is dispersed in phenyl siloxane rubber matrix (Fig. 2 is left), and has layer of surface modifying agent on pbo fiber surface (Fig. 2 is right).Because surface is modified
The semipolar phosphate groups part of agent generates the strong interactions such as esterification and hydrogen bond with the pbo fiber surface with polar group,
The aliphatic chain in (methylacryloyl oxygroup) ethyl and castor oil and phenyl siloxane rubber matrix have fabulous compatibility simultaneously,
The interface binding power of pbo fiber Yu phenyl siloxane rubber matrix can be improved, to be greatly improved the mechanical strength of ablative coating.And
Pbo fiber is high-temperature resistant special fiber, and the high temperature resistant thermal protective performance of ablative coating can be improved in the introducing of pbo fiber.
Second aspect, the present invention provide a kind of preparation method of anti-heat insulating coat of silicon rubber base, include the following steps:
S1, substrate surface wiped clean will be sprayed-on with solvent, by lighting thermal insulating filling, surface treating agent, white carbon black,
Methyl silicone rubber raw rubber, ethyl orthosilicate, dibutyl tin dilaurate, toluene press mass parts ratio (5~25): 2:20:100:
3:1:200 is uniformly mixed, and is filtered after mixing by 30~40 mesh filter screens, filtrate is sprayed at substrate surface, obtains heat insulating coat；
S2, mica, silicon powder, white carbon black, phenyl siloxane rubber raw rubber, curing agent, dibutyl tin dilaurate, toluene are pressed
Mass fraction ratio (15~30): (5~10): 20:100:3:1:200 is uniformly mixed, and is 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 black, phenyl silicon
Rubber raw rubber, ethyl orthosilicate, dibutyl tin dilaurate, toluene press mass parts ratio (1~10): (0.5~2): (1~5):
30:20:100:3:1:200 is uniformly mixed, and is filtered after mixing by 30~40 mesh filter screens, filtrate is sprayed at what step S2 was obtained
The surface of radiation coating, obtains ablative coating.
It, can not will may be mixed miscellaneous in coating preparation process if screen specification is lower 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, leads to the content inaccuracy of coating ingredients.
Preferably, for above-mentioned S1 into S3 step, the strainer is metal mesh；The spraying uses spray gun with the pressure of 0.5MPa
Power sprays filtrate.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, 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, to improve ablation painting
The mechanical property of layer.Such as using other fibers with silicon rubber is compound cannot 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 reinforcing effect
It is bad；And the tensile strength of carbon fiber T800 is also only 5.49GPa, and the density of carbon fiber T800 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.
2, high radiation coating is prepared for by in-situ ceramicization reaction using the heat for penetrating ablative coating, is consumed absorbing
Subsequent arrival heat will be penetrated heat in the form of strong infra-red electromagnetic wave radiation and be emitted to ring by the ceramics generated while heat
In the medium of border, to further increase the anti-thermal effect of combination coating.Successfully solves silicon rubber base thermal protective coating mechanical property
The relatively low drawback with anti-heat-proof quality, before the thermal protections fields such as rocket delivery, missile armament body structure surface have and are widely applied
Scape.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the structural schematic diagram of the anti-heat insulating coat of silicon rubber base of the present invention；
Fig. 2 is the structural schematic diagram of ablative coating in the present invention.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to the present invention
Protection scope.
Embodiment 1
The present embodiment is related to a kind of anti-heat insulating coat of silicon rubber base, and 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-ball, 2g
Gamma-aminopropyl-triethoxy-silane, 20g white carbon black, 100g methyl silicone rubber raw rubber, 3g ethyl orthosilicate, 1g tin dilaurate two
Butyl tin and 200g toluene are mixed, with 30~40 mesh metal mesh filters after stirring, with spray gun with the pressure of 0.5MPa
Filtrate is sprayed at substrate surface, obtains silicon rubber base heat insulating coat, heat insulating coat thickness control is 5mm；
(2) by 15g mica, 5g silicon powder, 20g white carbon black, 100g silicon mass fraction be 33% phenyl siloxane rubber raw rubber,
3g ethyl orthosilicate, 1g dibutyl tin dilaurate and 200g toluene are mixed, with 30~40 mesh metal meshes after stirring
Filtering, is sprayed at step (1) for filtrate with the pressure of 0.5MPa with spray gun and obtains heat insulating coat surface, obtain heat insulating coat substrate
Radiation coating, radiation coating thickness control be 2.5mm；
(3) the polyparaphenylene benzo dioxazole fiber by 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 carbon black, 100g phenyl siloxane rubber raw rubber, 3g ethyl orthosilicate, 1g
Dibutyl tin dilaurate 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 the pressure of 0.5MPa
Control is 1.5mm, obtains the silicon rubber base that ablative coating, radiation coating, heat insulating coat are followed successively by by outer surface to substrate sequence
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 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 microballoon, 2g
γ-(methacryloxy) propyl trimethoxy silicane, 20g white carbon black, 100g methyl silicone rubber raw rubber, the positive silicic acid second of 3g
Ester, 1g dibutyl tin dilaurate and 200g toluene are mixed, and with 30~40 mesh metal mesh filters after stirring, use spray gun
Filtrate is sprayed at substrate surface with the pressure of 0.5MPa, obtains silicon rubber base heat insulating coat, heat insulating coat thickness control is
0.1mm；
(2) by 30g mica, 8g silicon powder, 2g white carbon black, 100g silicon mass fraction be 42% phenyl siloxane rubber raw rubber,
3g positive silicic acid propyl ester, 1g dibutyl tin dilaurate and 200g toluene are mixed, with 30~40 mesh metal meshes after stirring
Filtering, is sprayed at step (1) for filtrate with the pressure of 0.5MPa with spray gun and obtains heat insulating coat surface, obtain heat insulating coat substrate
Radiation coating, radiation coating thickness control be 5mm；
(3) polyparaphenylene benzo dioxazole fiber, 2g castor oil phosphate ester, 5g that 5g length is 0.5 centimetre are aoxidized
Iron, 30g calcium carbonate, 20g white carbon black, 100g phenyl siloxane rubber raw rubber, 3g ethyl orthosilicate, 1g dibutyl tin dilaurate and
200g toluene is mixed, and with 30~40 mesh metal mesh filters after stirring, is sprayed filtrate with the pressure of 0.5MPa with spray gun
It is applied to the radiation coating surface for the heat insulating coat substrate that step (2) obtains, ablative coating thickness control is 2mm, is obtained by appearance
Face to substrate sequence 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 preparation method is as follows:
(1) substrate surface wiped clean will be sprayed-on by dipping acetone with degreasing veil, by 5g cork powder, 2g γ-shrink
Glycerol ether oxygen propyl trimethoxy silicane, 20g white carbon black, 100g methyl silicone rubber raw rubber, 3g ethyl orthosilicate, 1g tin dilaurate
Dibutyl tin and 200g toluene are mixed, with 30~40 mesh metal mesh filters after stirring, with spray gun with the pressure of 0.5MPa
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) by 25g mica, 10g silicon powder, 20g white carbon black, the phenyl siloxane rubber life that 100g silicon mass fraction is 30%
Glue, 3g phenyltrimethoxysila,e, 1g dibutyl tin dilaurate and 200g toluene are mixed, with 30~40 after stirring
Filtrate is sprayed at step (1) with the pressure of 0.5MPa with spray gun and obtains heat insulating coat surface, obtained heat-insulated by mesh metal mesh filter
The radiation coating of coated substrate, heat insulating coat thickness control are 0.1mm；
(3) the polyparaphenylene benzo dioxazole fiber by 10g length for 0.7 centimetre, the (2- (methacryl of 1.0g bis-
Base oxygroup) ethyl) phosphoric acid, 1g iron oxide, 30g calcium carbonate, 20g white carbon black, 100g phenyl siloxane rubber raw rubber, the positive silicic acid second of 3g
Ester, 1g dibutyl tin dilaurate 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 the pressure of 0.5MPa, ablative coating is thick
Degree control is 2mm, obtains the silicon rubber base that ablative coating, radiation coating, heat insulating coat are followed successively by by outer surface to substrate sequence
Anti- heat insulating coat.
Embodiment 4
The present embodiment is related to a kind of anti-heat insulating coat of silicon rubber base, and 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-ball, 2g
Gamma-aminopropyl-triethoxy-silane, 20g white carbon black, 100g methyl silicone rubber raw rubber, 3g ethyl orthosilicate, 1g tin dilaurate two
Butyl tin and 200g toluene are mixed, with 30~40 mesh metal mesh filters after stirring, with spray gun with the pressure of 0.5MPa
Filtrate is sprayed at substrate surface, obtains silicon rubber base heat insulating coat, heat insulating coat thickness control is 0.5mm；
(2) by 15g mica, 7g silicon powder, 20g white carbon black, 100g silicon mass fraction be 50% phenyl siloxane rubber raw rubber,
3g ethyl orthosilicate, 1g dibutyl tin dilaurate and 200g toluene are mixed, with 30~40 mesh metal meshes after stirring
Filtering, is sprayed at step (1) for filtrate with the pressure of 0.5MPa with spray gun and obtains heat insulating coat surface, obtain heat insulating coat substrate
Radiation coating, radiation coating thickness control be 1mm；
(3) the polyparaphenylene benzo dioxazole fiber by 3g length for 0.1 centimetre, the (2- (methylacryloyl of 1.5g bis-
Oxygroup) ethyl) phosphoric acid, 2g iron oxide, 30g calcium carbonate, 20g white carbon black, 100g phenyl siloxane rubber raw rubber, 3g ethyl orthosilicate,
1g dibutyl tin dilaurate 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 the pressure of 0.5MPa
Control is 0.1mm, obtains the silicon rubber base that ablative coating, radiation coating, heat insulating coat are followed successively by by outer surface to substrate sequence
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 preparation method and embodiment 1 are almost the same, difference
Be in: do not spray ablative coating, obtain the silicon rubber base for being followed successively by radiation coating, heat insulating coat by outer surface to substrate sequence
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 preparation method and embodiment 1 are almost the same, difference
Be in: do not spray radiation coating, obtain the silicon rubber base for being followed successively by ablative coating, heat insulating coat by outer surface to substrate sequence
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 preparation method and embodiment 1 are almost the same, difference
Be in: do not spray heat insulating coat, obtain the silicon rubber base for being followed successively by ablative coating, radiation coating by outer surface to substrate sequence
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 preparation method and embodiment 1 are almost the same, difference
Be in: in step (3), using aramid fiber replace polyparaphenylene benzo dioxazole fiber.
Comparative example 5
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and preparation method and embodiment 1 are almost the same, difference
Be in: in step (3), using tributyl phosphate surface modifier replace two (2- (methylacryloyl oxygroup) ethyl) phosphorus
Acid.
Comparative example 6
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and preparation method and embodiment 1 are almost the same, difference
Be in: in step (1), using phenyl siloxane rubber raw rubber replace the methyl silicone rubber raw rubber.
Comparative example 7
This comparative example is related to a kind of anti-heat insulating coat of silicon rubber base, and preparation method and embodiment 1 are almost the same, difference
Be in: in step (2), in the phenyl siloxane rubber raw rubber mass fraction of silicon be 65%.
Performance test
Using 990.13 standard testing coating density of QJ, using 10295 standard testing thermal conductivity of GB/T, using GB/T
1040.2 standard testing coating tensile strengths and elongation at break, test the various embodiments described above and each comparative example, test
As a result as shown in table 1 below:
Table 1
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (7)
1. a kind of anti-heat insulating coat of silicon rubber base, which is characterized in that including heat insulating coat, radiation coating and ablative coating；It is described
Heat insulating coat setting is arranged between heat insulating coat and ablative coating in substrate surface, the radiation 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 in the ablative coating；
The heat insulating coat includes each component of following mass parts ratio: lighting thermal insulating filling, surface treating agent, white carbon black,
Methyl silicone rubber raw rubber, ethyl orthosilicate, dibutyl tin dilaurate, toluene mass parts ratio be (5~25): 2:20:
100:3:1:200；
The radiation coating includes each component of following mass parts ratio: mica, silicon powder, white carbon black, phenyl siloxane rubber raw rubber,
Curing agent, dibutyl tin dilaurate, toluene mass fraction ratio be (15~30): (5~10): 20:100:3:1:200；
The ablative coating includes each component of following mass parts ratio: polyparaphenylene benzo dioxazole fiber, surface are modified
Agent, iron oxide, calcium carbonate, white carbon black, phenyl siloxane rubber raw rubber, ethyl orthosilicate, dibutyl tin dilaurate, toluene quality
Portion rate is (1~10): (0.5~2): (1~5): 30:20:100:3:1:200.
2. the anti-heat insulating coat of silicon rubber base according to claim 1, which is characterized in that the lighting thermal insulating filling is selected from
One of hollow glass micro-ball, hollow phenolic aldehyde microballoon, cork powder.
3. the anti-heat insulating coat of silicon rubber base according to claim 1, which is characterized in that the surface treating agent is selected from γ-
Aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxy) propyl three
One of methoxy silane.
4. the anti-heat insulating coat of silicon rubber base according to claim 1, which is characterized in that silicon in the phenyl siloxane rubber raw rubber
Mass fraction be 30%~50%.
5. the anti-heat insulating coat of silicon rubber base according to claim 1, which is characterized in that the curing agent is positive silicic acid second
One of ester, positive silicic acid propyl ester, methyltriethoxysilane, phenyl triethoxysilane, phenyltrimethoxysila,e.
6. the anti-heat insulating coat of silicon rubber base according to claim 1, which is characterized in that the surface modifier be containing 5~
The phosphate compounds of the substituent group of 18 carbon atom chain lengths.
7. a kind of preparation method of the anti-heat insulating coat of silicon rubber base according to claim 1-6, which is characterized in that
Include the following steps:
S1, it will be sprayed-on substrate surface wiped clean with solvent, by lighting thermal insulating filling, surface treating agent, white carbon black, methyl
Raw-silastic continuously, ethyl orthosilicate, dibutyl tin dilaurate, toluene press mass 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 substrate surface, obtains heat insulating coat；
S2, mica, silicon powder, white carbon black, phenyl siloxane rubber raw rubber, curing agent, dibutyl tin dilaurate, toluene are pressed into quality
Score ratio (15~30): (5~10): 20:100:3:1:200 is uniformly mixed, and is filtered, will be filtered by 30~40 mesh filter screens after mixing
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 black, phenyl siloxane rubber
Raw rubber, ethyl orthosilicate, dibutyl tin dilaurate, toluene press mass parts ratio (1~10): (0.5~2): (1~5): 30:
20:100:3:1:200 is uniformly mixed, and is filtered after mixing by 30~40 mesh filter screens, filtrate is sprayed at the spoke that step S2 is obtained
The surface for penetrating coating, obtains ablative coating.
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| CN109161331B (en) * | 2018-07-27 | 2021-08-31 | 上海交通大学 | Ceramic spiral fiber reinforced silicon rubber light ablation-resistant heat-insulating coating and application thereof |
| CN109266212A (en) * | 2018-09-07 | 2019-01-25 | 西安宙通新材料科技有限公司 | A kind of low density and high performance thermal protective coating |
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| CN111500155A (en) * | 2020-06-01 | 2020-08-07 | 郑林义 | Modified cork composite material |
| CN115895435B (en) * | 2022-10-11 | 2023-11-03 | 航天特种材料及工艺技术研究所 | High-performance heat-insulating paint, coating and preparation method thereof |
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| JP4005009B2 (en) * | 2003-09-17 | 2007-11-07 | 信越化学工業株式会社 | Silicone rubber composition for wire coating |
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