CN116834395B - Ablation-resistant heat-insulating composite heat-insulating layer structure and forming method - Google Patents

Ablation-resistant heat-insulating composite heat-insulating layer structure and forming method Download PDF

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CN116834395B
CN116834395B CN202311123577.7A CN202311123577A CN116834395B CN 116834395 B CN116834395 B CN 116834395B CN 202311123577 A CN202311123577 A CN 202311123577A CN 116834395 B CN116834395 B CN 116834395B
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layer
ablation
heat
ethylene propylene
diene monomer
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CN116834395A (en
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秦锋
马俊
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Shaanxi Pulimei Material Technology Co ltd
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Shaanxi Pulimei Material Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/14—Layered products comprising a layer of natural or synthetic rubber comprising synthetic rubber copolymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/02—Layered products comprising a layer of natural or synthetic rubber with fibres or particles being present as additives in the layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B32B37/1018—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure using only vacuum
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    • B32—LAYERED PRODUCTS
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1284—Application of adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • 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
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02K—JET-PROPULSION PLANTS
    • F02K9/00—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof
    • F02K9/08—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof using solid propellants
    • F02K9/32—Constructional parts; Details not otherwise provided for
    • F02K9/34—Casings; Combustion chambers; Liners thereof
    • F02K9/346—Liners, e.g. inhibitors
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/04—Cellulosic plastic fibres, e.g. rayon
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    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/106—Carbon fibres, e.g. graphite fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/304—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
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    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc

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Abstract

The application provides an ablation-resistant heat-insulating composite heat-insulating layer structure and a forming method, wherein the ablation-resistant heat-insulating composite heat-insulating layer structure comprises the following components: a surface layer bonded to the grain liner, the surface layer being an ethylene propylene diene monomer rubber insulating layer having a high elongation for releasing propellant stress; the ablation layer is arranged on the inner side of the surface layer, is a carbon fiber reinforced ethylene propylene diene monomer rubber heat insulation layer and is used for resisting high-temperature high-pressure high-combustion-speed airflow interfaces generated in the working process of the propellant and particle scouring in the propellant; the heat insulation layer is arranged on the inner side of the ablation layer and is used for transmitting heat flow received by the interface of the ablation layer. The material has oxyacetylene line ablation rate of not more than 0.03mm/s and density of 1.1g/cm 3 ～1.2 g/cm 3 The tensile strength is not less than 10MPa, and the bonding strength with the ethylene propylene diene monomer rubber heat insulation layer is not less than 5MPa.

Description

Ablation-resistant heat-insulating composite heat-insulating layer structure and forming method
Technical Field
The application belongs to the technical field of ablation-resistant materials, and is applied to rocket engine propellers, in particular relates to an ablation-resistant heat-insulation composite heat-insulation layer structure and a forming method.
Background
Carbon fiber has been widely used in the field of solid rocket engine combustion chamber heat insulating layer materials due to its excellent ablation resistance, and particularly in the back end enclosure of the combustion chamber and the parts with serious ablation, the carbon fiber composite material or the composite heat insulating layer plays an important role in the structural integrity of the product. In the publication No. CN107057197A named as 'a carbon fiber reinforced ethylene propylene diene monomer rubber material and a preparation method', a heat insulation layer material of the chopped fiber reinforced ethylene propylene diene monomer rubber is provided, and is formed by rubber mixing and processing, so that the heat insulation layer material is unreliable relative to a working condition with serious ablation; in publication number CN 105837956A named as an anti-ablation material of carbon fiber reinforced ethylene propylene diene monomer and a preparation method, an ethylene propylene diene monomer heat insulation layer taking carbon fiber woven cloth or carbon fiber knitted cloth as a reinforcement is provided, so that the anti-ablation and anti-scouring performance of the heat insulation layer is effectively improved, but because the fiber is made of polyacrylonitrile carbon fiber, the modulus is high, the forming process is complex, in practical application, bulges are easy to generate due to the material, and a certain interface risk exists.
In GBJ2909-1997, the specification of carbon fiber/phenolic aldehyde-nitrile rubber material, a composite material which takes viscose fiber carbon fiber as a reinforcement body and takes phenolic resin and nitrile rubber as a matrix is proposed, and the composite material is also widely applied to a heat insulation layer structure of a solid rocket engine, but needs to be used in combination with other rubber heat insulation layers, the processing specification of the product is only 3mm and 5mm, the shape is generally rectangular sheet-shaped, in actual use, the product needs to be subjected to secondary cutting processing and forming, the cost waste is easy to be caused, the process is complex, the consistency is poor, the matrix specificity and the bonding strength with ethylene propylene diene monomer rubber are also low, the vulcanization process also needs to be subjected to at least secondary vulcanization forming (CN 109058661A is an interlayer composite heat insulation layer structure and a manufacturing method), the processing cost is high, and the permanent storage performance of the product is still to be further examined. In addition, because of the composite insulation layer structure, there are easily uneven stress release due to differences in hardness and elongation of each material, and excessive or unreasonable use of the insulation layer material, thereby wasting resources.
Disclosure of Invention
Accordingly, the present application is directed to a composite heat insulating layer structure with ablation resistance and thermal insulation and a molding method thereof.
The technical scheme adopted by the application is as follows:
an ablation resistant thermal insulation composite thermal insulation layer structure comprising:
a surface layer bonded to the grain liner, the surface layer being an ethylene propylene diene monomer rubber insulating layer having a high elongation for releasing propellant stress;
the ablation layer is arranged on the inner side of the surface layer, is a carbon fiber reinforced ethylene propylene diene monomer rubber heat insulation layer and is used for resisting high-temperature high-pressure high-combustion-speed airflow interfaces generated in the working process of the propellant and particle scouring in the propellant;
the heat insulation layer is arranged on the inner side of the ablation layer and is used for transmitting heat flow received by the interface of the ablation layer.
Further, the heat insulation layer is prepared from an ethylene propylene diene monomer heat insulation base material with the heat conductivity smaller than 0.15W/mK and the hardness larger than 85.
Further, the ablation layer is made of an ethylene propylene diene monomer rubber material reinforced by viscose.
Further, the surface layer is an ethylene propylene diene monomer rubber heat insulation layer with the elongation percentage being more than 500%.
Further, the viscose fiber reinforced ethylene propylene diene monomer rubber material is prepared according to the following method:
step 1) preparation of ethylene propylene diene monomer rubber heat insulation material: weighing materials required for preparing the ethylene propylene diene monomer rubber heat insulation material according to a proportion, and mixing and molding on an internal mixer or an open rubber mixing mill;
step 2) preparation of ethylene propylene diene monomer solution: the ethylene propylene diene monomer rubber heat insulation material is sliced on an open mill, and the thickness is not more than 1mm; then cutting into fragments, putting the fragments into a container, and pouring a set amount of solvent for dissolution, wherein the dissolution mass ratio is as follows: film= (5-10): 1;
step 3) mixing: immersing carbon fiber into the dissolved ethylene propylene diene monomer solution in a container, uniformly stirring, and airing for 12-24 hours.
Further, the ethylene propylene diene monomer rubber heat insulation material comprises the following components in parts by weight: 80-85 parts of ethylene propylene diene monomer, 4-8 parts of zinc oxide, 1.5-2 parts of stearic acid, 1-2 parts of an anti-aging agent, 1.5-2 parts of a silane coupling agent, 1-2 parts of a plasticizer, 5-8 parts of aluminum hydroxide and 1-2 parts of a vulcanizing agent.
Further, the silane coupling agent adopts KH-570 brand silane coupling agent.
Further, the plasticizer adopts one of dioctyl sebacate and 3, 4-diaminobenzene sulfonic acid.
Further, the solvent is one of cyclohexane, n-butanol and toluene.
The application also provides a forming method of the ablation-resistant heat-insulating composite heat-insulating layer structure, which is applied to the preparation of the ablation-resistant heat-insulating composite heat-insulating layer structure and comprises the following steps:
1) Blasting sand on the end socket of the combustion chamber shell: blowing sand on the bonding surface of the rear sealing head of the combustion chamber shell, wherein the sand blasting adopts brown fused alumina or quartz sand with 20-24 meshes, and the air pressure is 0.5-0.7 MPa; then dedusting, cleaning the bonding surface by using ethyl acetate, and brushing a surface adhesive on the bonding surface after airing;
2) Preforming a heat insulation layer and a surface layer: filling an ethylene propylene diene monomer rubber heat insulation base material on a flat vulcanizing machine by adopting a die, and pressing a heat insulation layer; wiping the pressed bonding surface of the heat insulation layer with ethyl acetate, and airing for standby, wherein the heat conductivity of the heat insulation layer is less than 0.15W/mK, and the hardness is more than 85; filling an ethylene propylene diene monomer rubber heat insulation base material into a mold to prepare a surface layer, wiping a pressed surface layer bonding surface with ethyl acetate, and airing for standby, wherein the extensibility of the surface layer is more than 500%;
3) Preforming an ablation layer: weighing the viscose fiber reinforced ethylene propylene diene monomer rubber material with a set proportion, preheating the material in an oven at 85-100 ℃ for 15-20 min, then filling the material into a molding die cavity which is preheated to 85-100 ℃ on a hydraulic press, uniformly filling the material for a plurality of times to ensure that the viscose fiber reinforced ethylene propylene diene monomer rubber material is uniformly paved in the die cavity, then closing the die, preheating for 30-40 min, pressurizing for 8-12 MPa, pressing the die in place, maintaining the pressure, preserving the heat for 60-80 min, and naturally cooling to room temperature; ejecting and demolding the preformed ablation layer through a hydraulic press to obtain the ablation layer;
4) Surface treatment: brushing adhesive on the bonding surface of the back sealing head, the bonding surface of the heat insulation layer, the bonding surface of the ablation layer and the bonding surface of the surface layer of the combustion chamber shell respectively, and airing for later use;
5) And (3) assembling: firstly, sticking a heat insulation layer on the surface of a shell, aligning up and down, and pressing in place; similarly, the ablation layer and the surface layer are respectively stuck at the corresponding positions; after the heat insulation layer, the ablation layer and the surface layer are inspected to be stuck in place, wrapping the whole part by using a separation film and a vacuum bag;
6) And (3) forming: placing the wrapped parts into a vulcanizing tank, vacuumizing to be not more than-0.098 MPa, observing for 30-40 min without pressure drop, and indicating that the sealing is perfect; then heating and pressurizing in a vulcanizing tank for molding; the temperature is set as follows: heating the room temperature to 85-100 ℃ for 2-3 h, then preserving heat for 1-2 h, heating to 100-140 ℃ for 2-3 h, preserving heat for 1-2 h, heating to 140-180 ℃ for 2-3 h, and naturally cooling the room temperature after the heat preservation is finished; the pressure is set as follows: the pressure rises at 0.03MPa/min, after heating and starting, the pressure is increased to 1.1MPa, and then the temperature is maintained until the room temperature is reached;
7) And (3) checking: after the forming is finished, the tooling is disassembled, the vulcanized part is taken out, whether the appearance is good or not is checked, the thickness is measured, and whether the bonding interface is debonded or not is checked by ultrasonic flaw detection.
The application realizes co-vulcanization with the same matrix of the ethylene propylene diene monomer rubber heat insulation layer, realizes chemical crosslinking at the interface, solves the quality hidden trouble of poor interfacial adhesion of the composite heat insulation layer, reduces the modulus of the carbon fiber material, and greatly reduces the stress of the carbon fiber ethylene propylene diene monomer composite heat insulation layer in the long-term storage process.
The material has oxyacetylene line ablation rate of not more than 0.03mm/s and density of 1.1g/cm 3 ～1.2 g/cm 3 The tensile strength is not less than 10MPa, and the bonding strength with the ethylene propylene diene monomer rubber heat insulation layer is not less than 5MPa.
Drawings
FIG. 1 is a schematic structural view of an ablation-resistant heat-insulating composite heat-insulating layer structure in the application;
FIG. 2 is a schematic view of a portion of the structure of the ablation-resistant and thermally insulating composite insulation layer of the present application mounted to a propeller.
Detailed Description
The present application will now be described in detail with reference to the drawings and the specific embodiments thereof, wherein the exemplary embodiments and descriptions of the present application are provided for illustration of the application and are not intended to be limiting.
Example 1:
the application aims to research an ablation-resistant material which can replace carbon fiber woven cloth to strengthen an ethylene propylene diene monomer rubber heat insulation layer, a carbon wool board and the like, so as to improve the process applicability of the carbon fiber/ethylene propylene diene monomer rubber composite heat insulation layer, process the carbon fiber/ethylene propylene diene monomer rubber composite heat insulation layer structural member meeting the design requirements according to the design structural requirements, reduce the processing waste of the material, reduce the vulcanization forming process and time of the heat insulation layer, improve the production efficiency on the basis of ensuring the reliability of the ablation-resistant performance, and reduce the production cost. Meanwhile, according to the material characteristics, a heat insulation structure with high reliability is designed, and the ablation and heat prevention integrated functional application of the heat insulation layer in the combustion chamber of the solid rocket engine is realized.
Referring to fig. 1, the ablation-resistant heat-insulating composite heat-insulating layer structure mainly comprises a surface layer, an ablation layer and a heat-insulating layer, wherein the surface layer is an ethylene propylene diene monomer rubber heat-insulating layer with high elongation and mainly aims at being adhered to a grain lining to release propellant stress; the ablation layer is a carbon fiber reinforced ethylene propylene diene monomer rubber heat insulation layer and has the main functions of resisting high temperature, high pressure and high combustion speed and particle scouring in the working process of the propellant; the heat insulating layer is used for heat flow transmission of the ablation layer, has the characteristics of low heat conductivity and high hardness, and is characterized by combining system stress effectiveness, ablative property and heat insulation.
Specifically, the application provides an ablation-resistant heat-insulating composite heat-insulating layer structure, which comprises the following components:
a surface layer bonded to the grain liner, the surface layer being an ethylene propylene diene monomer rubber insulating layer having a high elongation for releasing propellant stress;
the ablation layer is arranged on the inner side of the surface layer, is a carbon fiber reinforced ethylene propylene diene monomer rubber heat insulation layer and is used for resisting high-temperature high-pressure high-combustion-speed airflow interfaces generated in the working process of the propellant and particle scouring in the propellant;
the heat insulation layer is arranged on the inner side of the ablation layer and is used for transmitting heat flow received by the interface of the ablation layer.
Further, the heat insulation layer is prepared from an ethylene propylene diene monomer heat insulation base material with the heat conductivity smaller than 0.15W/mK and the hardness larger than 85.
Further, the ablation layer is made of an ethylene propylene diene monomer rubber material reinforced by viscose.
Further, the surface layer is an ethylene propylene diene monomer rubber heat insulation layer with the elongation percentage being more than 500%.
Further, the viscose fiber reinforced ethylene propylene diene monomer rubber material is prepared according to the following method:
step 1) preparation of ethylene propylene diene monomer rubber heat insulation material: weighing materials required for preparing the ethylene propylene diene monomer rubber heat insulation material according to a proportion, and mixing and molding on an internal mixer or an open rubber mixing mill;
step 2) preparation of ethylene propylene diene monomer solution: the ethylene propylene diene monomer rubber heat insulation material is sliced on an open mill, and the thickness is not more than 1mm; then cutting into fragments, placing into a container, pouring a set amount of solvent for dissolution, wherein the dissolution mass ratio is that: film= (5-10): 1;
step 3) mixing: immersing carbon fiber into the dissolved ethylene propylene diene monomer solution in a container, uniformly stirring, and airing for 12-24 hours.
Further, the ethylene propylene diene monomer rubber heat insulation material comprises the following components in parts by weight: 80-85 parts of ethylene propylene diene monomer, 4-8 parts of zinc oxide, 1.5-2 parts of stearic acid, 1-2 parts of an anti-aging agent, 1.5-2 parts of a silane coupling agent, 1-2 parts of a plasticizer, 5-8 parts of aluminum hydroxide and 1-2 parts of a vulcanizing agent.
In the above, zinc oxide is used as a vulcanization active agent and a reinforcing agent in vulcanization of the ethylene propylene diene monomer rubber heat insulation material, and aluminum hydroxide is used as an inorganic flame retardant additive, so that the ethylene propylene diene monomer rubber heat insulation material achieves a good flame retardant effect; the vulcanizing agent is dicumyl peroxide vulcanizing agent, and the silane coupling agent is KH-570 brand silane coupling agent; the plasticizer adopts one of dioctyl sebacate and 3, 4-diaminobenzene sulfonic acid. The application realizes co-vulcanization with the same matrix of the ethylene propylene diene monomer rubber heat insulation layer, realizes chemical crosslinking at the interface, solves the quality hidden trouble of poor interfacial adhesion of the composite heat insulation layer, reduces the modulus of the carbon fiber material, and greatly reduces the stress of the carbon fiber ethylene propylene diene monomer composite heat insulation layer in the long-term storage process.
Further, the solvent is one of cyclohexane, n-butanol and toluene.
Example 2:
the application also provides a forming method of the ablation-resistant heat-insulating composite heat-insulating layer structure, which is applied to the preparation of the ablation-resistant heat-insulating composite heat-insulating layer structure and comprises the following steps:
1) Blasting sand on the end socket of the combustion chamber shell: blowing sand on the bonding surface of the rear sealing head of the combustion chamber shell, wherein 20-mesh brown fused alumina or quartz sand is adopted for sand blasting, and the air pressure is 0.5 MPa; then dedusting, cleaning the bonding surface by using ethyl acetate, and brushing a surface adhesive on the bonding surface after airing;
2) Preforming a heat insulation layer and a surface layer: filling an ethylene propylene diene monomer rubber heat insulation base material on a flat vulcanizing machine by adopting a die, and pressing a heat insulation layer; wiping the pressed bonding surface of the heat insulation layer with ethyl acetate, and airing for standby, wherein the heat conductivity of the heat insulation layer is less than 0.15W/mK, and the hardness is more than 85; filling an ethylene propylene diene monomer rubber heat insulation base material into a mold to prepare a surface layer, wiping a pressed surface layer bonding surface with ethyl acetate, and airing for standby, wherein the extensibility of the surface layer is more than 500%;
3) Preforming an ablation layer: weighing a set proportion of the viscose fiber reinforced ethylene propylene diene monomer rubber material, preheating the material in an oven at 85 ℃ for 15min, then filling the material into a forming die cavity which is preheated to 85 ℃ on a hydraulic press, uniformly filling the material for multiple times to ensure that the viscose fiber reinforced ethylene propylene diene monomer rubber material is uniformly laid in the die cavity, closing the die, preheating the material for 30min, pressurizing the material for 8MPa, pressing the die in place, maintaining the pressure and preserving the heat for 60min, and naturally cooling the material to room temperature; ejecting and demolding the preformed ablation layer through a hydraulic press to obtain the ablation layer;
4) Surface treatment: brushing adhesive on the bonding surface of the back sealing head, the bonding surface of the heat insulation layer, the bonding surface of the ablation layer and the bonding surface of the surface layer of the combustion chamber shell respectively, and airing for later use;
5) And (3) assembling: firstly, sticking a heat insulation layer on the surface of a shell, aligning up and down, and pressing in place; similarly, the ablation layer and the surface layer are respectively stuck at the corresponding positions; after the heat insulation layer, the ablation layer and the surface layer are inspected to be stuck in place, wrapping the whole part by using a separation film and a vacuum bag;
6) And (3) forming: placing the wrapped parts into a vulcanizing tank, vacuumizing to be not more than-0.098 MPa, observing for 30min without pressure drop, and indicating that the sealing is perfect; then heating and pressurizing in a vulcanizing tank for molding; the temperature is set as follows: heating the room temperature to 85 ℃ for 2 hours, then preserving heat for 1 hour, heating to 100 ℃ for 2 hours, preserving heat for 1-2 hours, heating to 140 ℃ for 2-3 hours, preserving heat for 2 hours, and naturally cooling the room temperature after the heat preservation is finished; the pressure is set as follows: the pressure rises at 0.03MPa/min, after heating and starting, the pressure is increased to 1.1MPa, and then the temperature is maintained until the room temperature is reached;
7) And (3) checking: after the forming is finished, the tooling is disassembled, the vulcanized part is taken out, whether the appearance is good or not is checked, the thickness is measured, and whether the bonding interface is debonded or not is checked by ultrasonic flaw detection.
The surface layer of the prepared material is an ethylene propylene diene monomer rubber heat insulation layer with high elongation, and the main function of the material is to bond with a grain lining and release the stress of a propellant; the ablation layer is a carbon fiber reinforced ethylene propylene diene monomer rubber heat insulation layer and has the main functions of resisting high temperature, high pressure and high combustion speed and particle scouring in the working process of the propellant; the heat insulating layer is used for heat flow transmission of the ablation layer, has the characteristics of low heat conductivity and high hardness, and is characterized by combining system stress effectiveness, ablative property and heat insulation.
The application realizes co-vulcanization with the same matrix of the ethylene propylene diene monomer rubber heat insulation layer, realizes chemical crosslinking at the interface, solves the quality hidden trouble of poor interfacial adhesion of the composite heat insulation layer, reduces the modulus of the carbon fiber material, and greatly reduces the stress of the carbon fiber ethylene propylene diene monomer composite heat insulation layer in the long-term storage process.
The material has oxyacetylene line ablation rate of not more than 0.03mm/s and density of 1.1g/cm 3 ～1.2 g/cm 3 The tensile strength is not less than 10MPa, and the bonding strength with the ethylene propylene diene monomer rubber heat insulation layer is not less than 5MPa.
Example 3:
the application also provides a forming method of the ablation-resistant heat-insulating composite heat-insulating layer structure, which is applied to the preparation of the ablation-resistant heat-insulating composite heat-insulating layer structure and comprises the following steps:
1) Blasting sand on the end socket of the combustion chamber shell: blowing sand on the bonding surface of the rear sealing head of the combustion chamber shell, wherein 24-mesh brown fused alumina or quartz sand is adopted for sand blasting, and the air pressure is 0.7MPa; then dedusting, cleaning the bonding surface by using ethyl acetate, and brushing a surface adhesive on the bonding surface after airing;
2) Preforming a heat insulation layer and a surface layer: filling an ethylene propylene diene monomer rubber heat insulation base material on a flat vulcanizing machine by adopting a die, and pressing a heat insulation layer; wiping the pressed bonding surface of the heat insulation layer with ethyl acetate, and airing for standby, wherein the heat conductivity of the heat insulation layer is less than 0.15W/mK, and the hardness is more than 85; filling an ethylene propylene diene monomer rubber heat insulation base material into a mold to prepare a surface layer, wiping a pressed surface layer bonding surface with ethyl acetate, and airing for standby, wherein the extensibility of the surface layer is more than 500%;
3) Preforming an ablation layer: weighing a set proportion of the viscose fiber reinforced ethylene propylene diene monomer rubber material, preheating the material in a baking oven at 100 ℃ for 20min, then filling the material into a forming die cavity which is preheated to 100 ℃ on a hydraulic press, uniformly filling the material for multiple times to ensure that the viscose fiber reinforced ethylene propylene diene monomer rubber material is uniformly laid in the die cavity, then closing the die, preheating the material for 40min, pressurizing the material for 12MPa, pressing the die in place, maintaining the pressure and preserving the heat for 80min, and naturally cooling the material to room temperature; ejecting and demolding the preformed ablation layer through a hydraulic press to obtain the ablation layer;
4) Surface treatment: brushing adhesive on the bonding surface of the back sealing head, the bonding surface of the heat insulation layer, the bonding surface of the ablation layer and the bonding surface of the surface layer of the combustion chamber shell respectively, and airing for later use;
5) And (3) assembling: firstly, sticking a heat insulation layer on the surface of a shell, aligning up and down, and pressing in place; similarly, the ablation layer and the surface layer are respectively stuck at the corresponding positions; after the heat insulation layer, the ablation layer and the surface layer are inspected to be stuck in place, wrapping the whole part by using a separation film and a vacuum bag;
6) And (3) forming: placing the wrapped parts into a vulcanizing tank, vacuumizing to be not more than-0.098 MPa, observing for 40min without pressure drop, and indicating that the sealing is perfect; then heating and pressurizing in a vulcanizing tank for molding; the temperature is set as follows: heating from room temperature to 100 ℃ for 3 hours, then preserving heat for 2 hours, then heating to 140 ℃ for 3 hours, preserving heat for 2 hours, then heating to the temperature for 3 hours, preserving heat for 3 hours, and naturally cooling to room temperature after the heat preservation is finished; the pressure is set as follows: the pressure rises at 0.03MPa/min, after heating and starting, the pressure is increased to 1.1MPa, and then the temperature is maintained until the room temperature is reached;
7) And (3) checking: after the forming is finished, the tooling is disassembled, the vulcanized part is taken out, whether the appearance is good or not is checked, the thickness is measured, and whether the bonding interface is debonded or not is checked by ultrasonic flaw detection.
The surface layer of the prepared material is an ethylene propylene diene monomer rubber heat insulation layer with high elongation, and the main function of the material is to bond with a grain lining and release the stress of a propellant; the ablation layer is a carbon fiber reinforced ethylene propylene diene monomer rubber heat insulation layer and has the main functions of resisting high temperature, high pressure and high combustion speed and particle scouring in the working process of the propellant; the heat insulating layer is used for heat flow transmission of the ablation layer, has the characteristics of low heat conductivity and high hardness, and is characterized by combining system stress effectiveness, ablative property and heat insulation.
The application realizes co-vulcanization with the same matrix of the ethylene propylene diene monomer rubber heat insulation layer, realizes chemical crosslinking at the interface, solves the quality hidden trouble of poor interfacial adhesion of the composite heat insulation layer, reduces the modulus of the carbon fiber material, and greatly reduces the stress of the carbon fiber ethylene propylene diene monomer composite heat insulation layer in the long-term storage process.
The material has oxyacetylene line ablation rate of not more than 0.03mm/s and density of 1.1g/cm 3 ～1.2 g/cm 3 The tensile strength is not less than 10MPa, and the bonding strength with the ethylene propylene diene monomer rubber heat insulation layer is not less than 5MPa.
Example 4:
the application also provides a forming method of the ablation-resistant heat-insulating composite heat-insulating layer structure, which is applied to the preparation of the ablation-resistant heat-insulating composite heat-insulating layer structure and comprises the following steps:
1) Blasting sand on the end socket of the combustion chamber shell: blowing sand on the bonding surface of the rear sealing head of the combustion chamber shell, wherein 22-mesh brown fused alumina or quartz sand is adopted for sand blasting, and the air pressure is 0.6MPa; then dedusting, cleaning the bonding surface by using ethyl acetate, and brushing a surface adhesive on the bonding surface after airing;
2) Preforming a heat insulation layer and a surface layer: filling an ethylene propylene diene monomer rubber heat insulation base material on a flat vulcanizing machine by adopting a die, and pressing a heat insulation layer; wiping the pressed bonding surface of the heat insulation layer with ethyl acetate, and airing for standby, wherein the heat conductivity of the heat insulation layer is less than 0.15W/mK, and the hardness is more than 85; filling an ethylene propylene diene monomer rubber heat insulation base material into a mold to prepare a surface layer, wiping a pressed surface layer bonding surface with ethyl acetate, and airing for standby, wherein the extensibility of the surface layer is more than 500%;
3) Preforming an ablation layer: weighing a set proportion of the viscose fiber reinforced ethylene propylene diene monomer rubber material, preheating the material in a baking oven at 90 ℃ for 18min, then filling the material into a forming die cavity which is preheated to 90 ℃ on a hydraulic press, uniformly filling the material for multiple times to ensure that the viscose fiber reinforced ethylene propylene diene monomer rubber material is uniformly laid in the die cavity, closing the die, preheating for 35min, pressurizing for 10MPa, pressing the die in place, maintaining the pressure, preserving the heat for 60-80 min, and naturally cooling to room temperature; ejecting and demolding the preformed ablation layer through a hydraulic press to obtain the ablation layer;
4) Surface treatment: brushing adhesive on the bonding surface of the back sealing head, the bonding surface of the heat insulation layer, the bonding surface of the ablation layer and the bonding surface of the surface layer of the combustion chamber shell respectively, and airing for later use;
5) And (3) assembling: firstly, sticking a heat insulation layer on the surface of a shell, aligning up and down, and pressing in place; similarly, the ablation layer and the surface layer are respectively stuck at the corresponding positions; after the heat insulation layer, the ablation layer and the surface layer are inspected to be stuck in place, wrapping the whole part by using a separation film and a vacuum bag;
6) And (3) forming: placing the wrapped parts into a vulcanizing tank, vacuumizing to be not more than-0.098 MPa, observing for 35min without pressure drop, and indicating that the sealing is perfect; then heating and pressurizing in a vulcanizing tank for molding; the temperature is set as follows: heating from room temperature to 90 ℃ for 2.5h, then preserving heat for 1.5h, heating to 120 ℃ for 2.5h, preserving heat for 1.5h, heating to 160 ℃ for 2.5h, preserving heat for 2.5h, and naturally cooling to room temperature after the heat preservation is finished; the pressure is set as follows: the pressure rises at 0.03MPa/min, after heating and starting, the pressure is increased to 1.1MPa, and then the temperature is maintained until the room temperature is reached;
7) And (3) checking: after the forming is finished, the tooling is disassembled, the vulcanized part is taken out, whether the appearance is good or not is checked, the thickness is measured, and whether the bonding interface is debonded or not is checked by ultrasonic flaw detection.
The surface layer of the prepared material is an ethylene propylene diene monomer rubber heat insulation layer with high elongation, and the main function of the material is to bond with a grain lining and release the stress of a propellant; the ablation layer is a carbon fiber reinforced ethylene propylene diene monomer rubber heat insulation layer and has the main functions of resisting high temperature, high pressure and high combustion speed and particle scouring in the working process of the propellant; the heat insulating layer is used for heat flow transmission of the ablation layer, has the characteristics of low heat conductivity and high hardness, and is characterized by combining system stress effectiveness, ablative property and heat insulation.
The application realizes co-vulcanization with the same matrix of the ethylene propylene diene monomer rubber heat insulation layer, realizes chemical crosslinking at the interface, solves the quality hidden trouble of poor interfacial adhesion of the composite heat insulation layer, reduces the modulus of the carbon fiber material, and greatly reduces the stress of the carbon fiber ethylene propylene diene monomer composite heat insulation layer in the long-term storage process.
The material has oxyacetylene line ablation rate of not more than 0.03mm/s and density of 1.1g/cm 3 ～1.2 g/cm 3 The tensile strength is not less than 10MPa, and the bonding strength with the ethylene propylene diene monomer rubber heat insulation layer is not less than 5MPa.
Example 5:
in addition to examples 2 to 4, in step 6), the vulcanization molding of the component can be performed by the following method, and the vulcanization molding of the component can be performed by the air bag press molding. Temperature parameters: the room temperature is heated to 85 ℃ through 2 hours, then is kept for 1 hour, then is heated to 120 ℃ through 2 hours, is kept for 1 hour, is heated to 160 ℃ through 2 hours, is kept for 2 hours, and is naturally cooled to the room temperature after the heat preservation is finished. Pressure parameters: after the heating is started, the pressure is increased to 0.9MPa within 5min, and then the temperature is maintained until the temperature reaches the room temperature.
The foregoing has described in detail the embodiments of the present application, and specific embodiments have been employed to illustrate the principles and implementations of the embodiments of the present application, the above description of the embodiments being only useful for aiding in the understanding of the principles of the embodiments of the present application; meanwhile, as for those skilled in the art, according to the embodiments of the present application, there are variations in the specific embodiments and the application scope, and the present description should not be construed as limiting the present application.

Claims (4)

1. Ablation-resistant heat-insulating composite heat-insulating layer structure, which is characterized by comprising:
a surface layer bonded to the grain liner, the surface layer being an ethylene propylene diene monomer rubber insulating layer having a high elongation for releasing propellant stress;
the ablation layer is arranged on the inner side of the surface layer and is used for resisting the high-temperature high-pressure high-combustion-speed airflow interface generated in the working process of the propellant and particle scouring in the propellant;
the heat insulation layer is arranged on the inner side of the ablation layer and is used for transmitting heat flow received by the interface of the ablation layer;
the ablation layer is made of an ethylene propylene diene monomer rubber material reinforced by viscose;
the viscose fiber reinforced ethylene propylene diene monomer rubber material is prepared by the following method:
the viscose yarn reinforced ethylene propylene diene monomer rubber material is used for replacing carbon fiber woven cloth reinforced ethylene propylene diene monomer rubber heat insulation layer and carbon wool board ablation-resistant material;
step 1) preparation of ethylene propylene diene monomer rubber heat insulation material: weighing materials required for preparing the ethylene propylene diene monomer rubber heat insulation material according to a proportion, and mixing and molding on an internal mixer or an open rubber mixing mill;
step 2) preparation of ethylene propylene diene monomer solution: the ethylene propylene diene monomer rubber heat insulation material is sliced on an open mill, and the thickness is not more than 1mm; then cutting into fragments, placing into a container, pouring a set amount of solvent for dissolution, wherein the dissolution mass ratio is that: film= (5-10): 1;
step 3) mixing: immersing carbon fibers into the dissolved ethylene propylene diene monomer rubber solution in a container, uniformly stirring, and airing for 12-24 hours;
the ethylene propylene diene monomer rubber heat insulation material comprises the following components in parts by weight: 80-85 parts of ethylene propylene diene monomer, 4-8 parts of zinc oxide, 1.5-2 parts of stearic acid, 1-2 parts of anti-aging agent, 1.5-2 parts of silane coupling agent, 1-2 parts of plasticizer, 5-8 parts of aluminum hydroxide and 1-2 parts of vulcanizing agent;
the molding method of the ablation-resistant heat-insulating composite heat-insulating layer structure comprises the following steps:
1) Blasting sand on the end socket of the combustion chamber shell: blowing sand on the bonding surface of the rear sealing head of the combustion chamber shell, wherein the sand blasting adopts brown fused alumina or quartz sand with 20-24 meshes, and the air pressure is 0.5-0.7 MPa; then dedusting, cleaning the bonding surface by using ethyl acetate, and brushing a surface adhesive on the bonding surface after airing;
2) Preforming a heat insulation layer and a surface layer: filling an ethylene propylene diene monomer rubber heat insulation base material on a flat vulcanizing machine by adopting a die, and pressing a heat insulation layer; wiping the pressed bonding surface of the heat insulation layer with ethyl acetate, and airing for standby, wherein the heat conductivity of the heat insulation layer is less than 0.15W/mK, and the hardness is more than 85; filling an ethylene propylene diene monomer rubber heat insulation base material into a mold to prepare a surface layer, wiping a pressed surface layer bonding surface with ethyl acetate, and airing for standby, wherein the extensibility of the surface layer is more than 500%;
3) Preforming an ablation layer: weighing the viscose fiber reinforced ethylene propylene diene monomer rubber material with a set proportion, preheating the material in an oven at 85-100 ℃ for 15-20 min, then filling the material into a molding die cavity which is preheated to 85-100 ℃ on a hydraulic press, uniformly filling the material for a plurality of times to ensure that the viscose fiber reinforced ethylene propylene diene monomer rubber material is uniformly paved in the die cavity, then closing the die, preheating for 30-40 min, pressurizing for 8-12 MPa, pressing the die in place, maintaining the pressure, preserving the heat for 60-80 min, and naturally cooling to room temperature; ejecting and demolding the preformed ablation layer through a hydraulic press to obtain the ablation layer;
4) Surface treatment: brushing adhesive on the bonding surface of the back sealing head, the bonding surface of the heat insulation layer, the bonding surface of the ablation layer and the bonding surface of the surface layer of the combustion chamber shell respectively, and airing for later use;
5) And (3) assembling: firstly, sticking a heat insulation layer on the surface of a shell, aligning up and down, and pressing in place; similarly, the ablation layer and the surface layer are respectively stuck at the corresponding positions; after the heat insulation layer, the ablation layer and the surface layer are inspected to be stuck in place, wrapping the whole part by using a separation film and a vacuum bag;
6) And (3) forming: placing the wrapped parts into a vulcanizing tank, vacuumizing to be not more than-0.098 MPa, observing for 30-40 min without pressure drop, and indicating that the sealing is perfect; then heating and pressurizing in a vulcanizing tank for molding; the temperature is set as follows: raising the temperature to 85-100 ℃ from room temperature for 2-3 h, then preserving heat for 1-2 h, raising the temperature to 100-140 ℃ for 2-3 h, preserving heat for 1-2 h, raising the temperature to 140-180 ℃ for 2-3 h, and naturally cooling to room temperature after the heat preservation is finished; the pressure is set as follows: the pressure rises at 0.03MPa/min, after heating and starting, the pressure is increased to 1.1MPa, and then the pressure is maintained until the temperature is reduced to the room temperature;
7) And (3) checking: after the forming is finished, the tooling is disassembled, the vulcanized part is taken out, whether the appearance is good or not is checked, the thickness is measured, and whether the bonding interface is debonded or not is checked by ultrasonic flaw detection.
2. The ablation-resistant heat-insulating composite heat-insulating layer structure according to claim 1, wherein the silane coupling agent is KH-570 brand silane coupling agent.
3. The ablation-resistant heat-insulating composite heat-insulating layer structure according to claim 1, wherein the plasticizer is one of dioctyl sebacate and 3, 4-diaminobenzenesulfonic acid.
4. The ablation-resistant thermal insulation composite thermal insulation layer structure according to claim 1, wherein the solvent is one of cyclohexane, n-butanol and toluene.
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CN111086298A (en) * 2019-12-31 2020-05-01 武汉理工大学 Variable-density ethylene propylene diene monomer rubber heat-insulating functional material and preparation method thereof
CN115898695A (en) * 2023-03-09 2023-04-04 陕西普利美材料科技有限公司 Heat insulation layer structure of solid rocket engine combustion chamber and bonding method thereof

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KR20150004454A (en) * 2013-07-02 2015-01-13 주식회사 한화 Rubber Composition added Carbon Fabric for solid rocket motor insulation
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