CN115304918B - Low-density solid rocket engine heat-proof material and preparation method thereof - Google Patents

Low-density solid rocket engine heat-proof material and preparation method thereof Download PDF

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CN115304918B
CN115304918B CN202210963808.4A CN202210963808A CN115304918B CN 115304918 B CN115304918 B CN 115304918B CN 202210963808 A CN202210963808 A CN 202210963808A CN 115304918 B CN115304918 B CN 115304918B
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parts
solid rocket
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powder
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CN115304918A (en
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陈海亚
肖勇
黄赓乔
向世平
周超
马雪松
周晓斌
鲁明涛
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Hubei Hangju Technology Co ltd
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
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    • C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes
    • C08J2383/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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Abstract

The invention provides a low-density solid rocket engine heat-proof material and a preparation method thereof, wherein the low-density solid rocket engine heat-proof material comprises the following components in parts by weight: 100 parts of base material, 10-40 parts of reinforcing filler, 10-40 parts of ablation-resistant filler, 10-40 parts of structural filler, 1-5 parts of tackifying auxiliary agent, 1-40 parts of heat insulation filler and 50-70 parts of solvent; the structural filler includes hard fibrous filler and pulp filler. The low-density solid rocket engine heat-proof material has a simple production process, and the prepared material has a three-phase structure, extremely low density and excellent heat insulation performance. The hard fiber plays a role in enhancing the three-dimensional performance in the material, the pulp fiber plays a role in enhancing the two-dimensional plane, can resist cracking, particularly avoids deep splitting, and utilizes the swelling property of the pulp fiber to form an air phase, thereby greatly reducing the overall density of the material and enabling the density to reach 0.3-0.4g/cm 3 。

Description

Low-density solid rocket engine heat-proof material and preparation method thereof
Technical Field
The invention relates to the technical field of heat-proof and heat-proof materials, in particular to a low-density solid rocket engine heat-proof material and a preparation method thereof.
Background
When the aircraft flies at a high speed in the atmosphere, the high-speed airflow is compressed on the outer surface of the aircraft, a large amount of kinetic energy is converted into heat energy, and the temperature of the airflow is increased sharply, so that the outer surface of the aircraft must be thermally protected. Currently, there have been many studies on heat insulation materials for aircraft.
The patent CN 109266212A proposes a low-density high-performance heat-proof coating, which adopts silicon rubber to fill glass hollow spheres and gas-phase white carbon black, has the characteristics of low density, low heat conductivity coefficient and the like, but the density of the series of heat-proof materials is 0.5-0.7g/cm 3 The heat conductivity coefficient is less than or equal to 0.14W/(m.k), and the density and the heat conductivity coefficient of the coating material cannot be further reduced due to the limitation of the density and the added parts of the hollow microspheres, so that the improvement of the performance and the application field of the coating material are limited.
The patent CN109294238A proposes a light high-elastic ablation-resistant heat-insulating material and a preparation method thereof, wherein the material consists of heat-vulcanized silicone rubber, boron phenolic resin, hexamethylenetetramine, white carbon black, hydroxyl silicone oil, light ablation-resistant filler, vulcanizing agent, mesitylene and fiber, and has good elasticity and ablation resistance, but higher density of 0.6-0.8/cm through mixing, plasticating, banburying, segmented repeated foaming and vulcanization molding 3 The molding process is relatively complex, high-temperature foaming is required to be carried out through multiple sections (90 ℃,150 ℃,170 ℃ and 190 ℃), the requirement on equipment is high, and the energy consumption is high.
Patent CN109796772a proposes a flexible ablation-resistant composite material of an air source micro-foaming carbon layer, which consists of silicon rubber, fiber, white carbon black, an air source substance, a curing agent and a catalyst, is molded at room temperature, has good ablation resistance, but has a thermal conductivity coefficient of 0.18-0.29W/(m·k) and poor heat insulation performance.
As known from the existing heat protection technology, the existing methods for reducing the density of the heat protection material mainly comprise the following two methods: 1. reducing the material density by adding a low density filler; 2. foaming the material by adding a foaming agent reduces the density of the material. The method for reducing the density of the material by adding the low-density filler is limited by the mechanical property of the material and the density of the filler, and the density of the material cannot be further reduced; the foaming process of the material is greatly affected by temperature by adding the foaming agent to ensure that the appearance surface of the material is difficult to control and the consistency of the material performance is difficult to be effectively ensured, and in addition, the high-temperature vulcanized foaming material has the defect of complex process. Therefore, there is a need to further develop a low-density heat insulating material with simple process and controllable shape surface.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a low-density solid rocket engine heat-proof material and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows: the low-density solid rocket engine heat-resistant material comprises the following components in parts by weight:
100 parts of base material, 10-40 parts of reinforcing filler, 10-40 parts of ablation-resistant filler, 10-40 parts of structural filler, 1-5 parts of tackifying auxiliary agent, 1-40 parts of heat insulation filler and 50-70 parts of solvent;
the structural filler comprises a hard fiber filler and a pulp filler.
Further, the hard fiber filler comprises one or more of silicon carbide whisker, ceramic fiber, aramid fiber, glass fiber, carbon fiber, mullite fiber quartz fiber, polyimide fiber and polyphenylene benzodioxazole fiber.
Further, the pulp filler comprises one or more of aramid pulp, polyimide pulp and polyphenylene benzodioxazole pulp.
Further, the mass ratio of the hard fiber filler to the pulp filler is (3-5): 1
Further, the base material comprises silicone rubber/silicone resin, and further preferably comprises one or more of phenyl silicone rubber, phenyl silicone resin, methyl silicone rubber, methyl silicone resin, ethyl silicone rubber, ethyl silicone resin, phenylene silicone rubber, phenylene silicone resin, phenylene ether silicone rubber, phenylene ether silicone resin, fluorine silicone rubber and fluorine silicone resin.
Further, the reinforcing filler comprises one or more of white carbon black, light calcium carbonate, silica micropowder, organic montmorillonite, polyvinyl polysiloxane and nano alumina;
the anti-ablation filler comprises one or more of zirconia powder, alumina powder, quartz powder, mullite powder, ferric oxide powder, zinc oxide powder, silicon carbide powder and aramid powder; the size of the anti-ablative filler is preferably 300-600 mesh.
Further, the tackifying assistant comprises one or more of silane coupling agent, silicon-boron siloxane, titanate coupling agent and aluminate coupling agent.
Further, the heat insulation filler comprises one or more of cork powder, aerogel powder, hollow glass beads, phenolic hollow microspheres and silicone microspheres, and the size of the heat insulation filler is preferably 600-1200 meshes;
the solvent comprises one or more of n-hexane, n-heptane, ethyl acetate, butyl acetate, toluene and xylene.
Further, the diameter of the hard fiber filler is 2-20 mu m, and the length-diameter ratio is (10-50): 1.
The invention also provides a preparation method of the low-density solid rocket engine heat-proof material, which is characterized by comprising the following steps of:
s1, weighing base materials, reinforcing fillers, anti-ablation fillers, structural fillers and tackifying assistants according to mass, and mixing to obtain a mixed material;
s2, weighing the mixing materials and the heat-insulating filler according to mass, and uniformly stirring to obtain a heat-proof material;
s3, forming the obtained heat-resistant material by blade coating (a small amount of solvent is required for blade coating so as to be convenient for blade coating as a standard) or diluting the heat-resistant material into a diluted material by using the solvent and then spraying the diluted material for forming; curing at room temperature.
Compared with the prior art, the invention has the following beneficial effects:
(1) Unlike traditional heat insulating material with matrix resin and stuffing, the present invention creates one kind of three-phase structure comprising matrix resin, stuffing and stuffing, and has further lowered material density. In the traditional heat-proof and insulating material technology, pulp filler can play a good role in reinforcing and ablation resistance, but because of a special hairiness structure and strong oil absorption, the spraying manufacturability is poor, and the curing shrinkage rate of a material obtained by spraying is large, so that the pulp filler is not used for spraying and forming the heat-proof and insulating material. The invention improves the spraying manufacturability of the material by controlling the addition amount of the pulp filler, simultaneously, the invention utilizes the oil absorption of the pulp filler to fully expand the material to absorb the solvent, and the hard fiber filler is added to form a space skeleton in the material, thereby inhibiting the deformation caused by the volatilization of the solvent when the material is solidified, and forming a gap by the volatilization of the solvent in the material solidification process, so that the material forms a three-phase structure consisting of an organic phase (matrix material), an inorganic phase (filler) and an air phase (gap), and the density of the material is reduced. Specifically, the hard fiber plays a role in strengthening the three-dimensional body in the material, the pulp fiber plays a role in strengthening the two-dimensional plane, can resist cracking, particularly avoids deep splitting, and utilizes the swelling property of the pulp fiber to form an air phase, thereby greatly reducing the overall density of the material and enabling the density to reach 0.3-0.4g/cm 3 。
(2) The molding process is simple. The invention takes room temperature solidified silicon rubber/silicon resin as a matrix material, adopts a spray coating/blade coating mode for forming, does not need heating and pressurizing equipment, can accurately control the thickness of the material, and has a flat surface.
Drawings
FIG. 1 is a photograph of a material sample prepared in example 1 of the present invention after testing under certain wind tunnel test conditions.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, but the scope of the present invention is not limited by these examples.
The terms "comprising," "including," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
Where an amount, mass percent, or other value or parameter is expressed as a range, preferred range, or as a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Example 1
A preparation method of a low-density solid rocket engine heat-resistant material comprises the following steps:
weighing 800g of methyl silicone resin, 200g of white carbon black, 100g of wollastonite (namely ceramic fiber), 200g of aramid powder, 100g of carbon fiber, 30g of aramid pulp and 20g of silane coupling agent, and placing the mixture on an open mill for mixing for 20min to obtain a mixed material. 250g of glass hollow microspheres and 500g of butyl acetate are added into the mixed material, and the mixture is stirred and dispersed for 20min by using a dispersing machine of 500 r/min. Adding hydrogen-containing silicone oil cross-linking agent (curing agent), forming by spray coating process, and curing at room temperature for 7 days to obtain the low-density solid rocket engine heat-proof material with a three-phase structure.
Example 2
A preparation method of a low-density solid rocket engine heat-resistant material comprises the following steps:
weighing 800g of phenyl silicone rubber, 200g of light calcium carbonate, 100g of wollastonite, 200g of alumina powder, 100g of glass fiber, 30g of polyimide pulp and 20g of titanate coupling agent, and placing the materials on an open mill for mixing for 20min to obtain a mixed material. To the kneaded material, 250g of cork powder and 500g of n-hexane were added, and the mixture was stirred and dispersed for 20 minutes using a dispersing machine 500 r/min. Adding hydrogen-containing silicone oil cross-linking agent (curing agent), forming by spray coating process, and curing at room temperature for 7 days to obtain the low-density solid rocket engine heat-proof material with a three-phase structure.
Example 3
A preparation method of a low-density solid rocket engine heat-resistant material comprises the following steps:
weighing 800g of fluorine silicon resin, 200g of white carbon black, 100g of wollastonite, 200g of polyphenylene benzodioxazole fiber, 100g of carbon fiber, 30g of polyimide pulp and 20g of silicon-boron siloxane, and placing the materials on an open mill for mixing for 20min to obtain a mixed material. 250g of phenolic aldehyde hollow microspheres and 500g of butyl acetate are added into the mixed material, and the mixed material is stirred and dispersed for 20min by using a dispersing machine of 500 r/min. Adding hydrogen-containing silicone oil cross-linking agent (curing agent), forming by blade coating process, and curing at room temperature for 7 days to obtain the low-density solid rocket engine heat-proof material with three-phase structure.
Comparative example 1
A preparation method of a solid rocket engine heat-proof material comprises the following steps:
weighing 800g of methyl silicone resin, 200g of white carbon black, 100g of wollastonite, 200g of aramid fiber powder and 20g of silane coupling agent, and placing the mixture on an open mill for mixing for 20min to obtain a mixed material. 250g of glass hollow microspheres and 500g of butyl acetate are added into the mixed material, and the mixture is stirred and dispersed for 20min by using a dispersing machine of 500 r/min. Adding hydrogen-containing silicone oil cross-linking agent (curing agent), forming by spray coating process, and curing at room temperature for 7 days to obtain the solid rocket engine heat-proof material with a 'two-phase' structure.
Comparative example 2
A preparation method of a solid rocket engine heat-proof material comprises the following steps:
weighing 800g of methyl silicone resin, 200g of white carbon black, 100g of wollastonite, 200g of aramid powder, 100g of carbon fiber and 20g of silane coupling agent, and placing the mixture on an open mill for mixing for 20min to obtain a mixed material. 250g of glass hollow microspheres and 500g of butyl acetate are added into the mixed material, and the mixture is stirred and dispersed for 20min by using a dispersing machine of 500 r/min. Adding hydrogen-containing silicone oil cross-linking agent (curing agent), forming by spray coating process, and curing at room temperature for 7 days to obtain the solid rocket engine heat-proof material.
Comparative example 3
A preparation method of a solid rocket engine heat-proof material comprises the following steps:
weighing 800g of methyl silicone resin, 200g of white carbon black, 100g of wollastonite, 200g of aramid powder, 30g of aramid pulp and 20g of silane coupling agent, and placing the mixture on an open mill for mixing for 20min to obtain a mixed material. 250g of glass hollow microspheres and 500g of butyl acetate are added into the mixed material, and the mixture is stirred and dispersed for 20min by using a dispersing machine of 500 r/min. Adding hydrogen-containing silicone oil cross-linking agent (curing agent), adopting spray coating process to make formation, curing at room temperature for 7 days so as to obtain the invented engine heat-resisting material.
Comparative example 4
A preparation method of a solid rocket engine heat-proof material comprises the following steps:
weighing 800g of hydroxyl-terminated methyl silicone resin, 200g of white carbon black, 100g of wollastonite, 200g of aramid fiber powder and 20g of silane coupling agent, and placing the mixture on an open mill for mixing for 20min to obtain a mixing material. 250g of glass hollow microspheres are added into the mixed materials, and the mixed materials are stirred and dispersed for 20min by using a dispersing machine of 500 r/min. Adding hydrogen-containing silicone oil cross-linking agent (curing agent), forming by blade coating process, naturally foaming at room temperature, and curing at room temperature for 7 days to obtain the foaming type low-density solid rocket engine heat-proof material.
The performance of the solid rocket engine heat-resistant material prepared by the above examples and comparative examples is tested, and the specific table is shown below:
from the test results of the specific examples and the comparative examples, the low-density solid rocket motor heat-resistant material with the three-phase structure has extremely low density (0.37 g/cm) 3 Left and right) and good ablation resistance, the phenyl silicone rubber is used for replacing the methyl silicone resin in the embodiment 2 to improve the elongation at break of the material, and the ablation-resistant filler is replaced in the embodiment 3 to improve the ablation resistance of the material to a certain extent.
Comparative example 1 does not add structural filler, the obtained material has a 'two-phase structure', and from the aspect of performance test results, the material has higher density and poorer ablation resistance.
In comparative example 2, the pulp structural filler was not added, and from the results of performance test, the density of the material was reduced to some extent by the effect of the fiber structural filler, but the effect was not obvious.
In comparative example 3, no fibrous structural filler is added, and from the result of performance test, only pulp structural filler is added, so that the material has obvious shrinkage deformation in the curing process, the effect of reducing the density of the material is not obvious, and the ablation resistance is not good.
From the performance test results of comparative example 4, the density of the material is reduced by a foaming method, the performance of the material obtained by using a spraying process is unstable, the foaming process is difficult to control by using a blade coating process, and the appearance surface of the obtained material is uneven and has poor mechanical property and ablation resistance.
It should be noted that the above embodiments are merely illustrative of the present invention and not limiting, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The low-density solid rocket engine heat-proof material is characterized by comprising the following components in parts by weight:
100 parts of base material, 10-40 parts of reinforcing filler, 10-40 parts of ablation-resistant filler, 10-40 parts of structural filler, 1-5 parts of tackifying auxiliary agent, 1-40 parts of heat insulation filler and 50-70 parts of solvent;
the structural filler comprises a hard fiber filler and a pulp filler;
the mass ratio of the hard fiber filler to the pulp filler is (3-5): 1.
2. A low density solid rocket motor thermal protection material as recited in claim 1, wherein said hard fiber filler comprises one or more of silicon carbide whiskers, ceramic fibers, aramid fibers, glass fibers, carbon fibers, mullite fibers, quartz fibers, polyimide fibers, and polyphenylene benzobisoxazole fibers.
3. A low density solid rocket motor thermal protection material as recited in claim 1, wherein said pulp filler comprises one or more of aramid pulp, polyimide pulp, and polyphenylene benzodioxazole pulp.
4. A low density solid rocket motor thermal protection material as recited in claim 1, wherein said base material comprises one or more of phenyl silicone rubber, phenyl silicone resin, methyl silicone rubber, methyl silicone resin, ethyl silicone rubber, ethyl silicone resin, phenylene silicone rubber, phenylene silicone resin, fluorosilicone rubber, fluorosilicone resin.
5. A low density solid rocket engine thermal protection material as recited in claim 1, wherein said reinforcing filler comprises one or more of white carbon black, light calcium carbonate, silica micropowder, organo montmorillonite, polyvinyl polysiloxane, nano alumina;
the anti-ablation filler comprises one or more of zirconia powder, alumina powder, quartz powder, mullite powder, ferric oxide powder, zinc oxide powder, silicon carbide powder and aramid powder; the size of the anti-ablation filler is 300-600 meshes.
6. A low density solid rocket engine thermal protection material according to claim 1, wherein said adhesion promoting additive comprises one or more of silane coupling agent, silicon-boron-siloxane, titanate coupling agent, aluminate coupling agent.
7. A low density solid rocket engine thermal protection material according to claim 1, wherein said thermal insulation filler comprises one or more of cork powder, aerogel powder, hollow glass microspheres, phenolic hollow microspheres, silicone microspheres, said thermal insulation filler having a size of 600-1200 mesh;
the solvent comprises one or more of n-hexane, n-heptane, ethyl acetate, butyl acetate, toluene and xylene.
8. A low density solid rocket motor thermal protection material according to claim 1, wherein said hard fiber filler has a diameter of 2-20 μm and an aspect ratio of (10-50): 1.
9. A method of preparing a low density solid rocket motor thermal protection material as recited in any one of claims 1-8, comprising the steps of:
s1, weighing base materials, reinforcing fillers, anti-ablation fillers, structural fillers and tackifying assistants according to mass, and mixing to obtain a mixed material;
s2, weighing the mixing materials, the heat insulation filler and the solvent according to mass, and uniformly stirring to obtain a heat-proof material;
s3, forming the obtained heat-resistant material by blade coating or spraying; curing at room temperature.
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CN109852238A (en) * 2019-01-09 2019-06-07 上海交通大学 A kind of sprayable resistance to ablative coatings of silicon rubber base lightweight and its application
CN111138973A (en) * 2019-12-31 2020-05-12 湖北航聚科技有限公司 Heat insulating material in solid rocket engine and preparation method and application thereof
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