CN112322040A - Organic silicon heat insulation layer for engine and preparation method thereof - Google Patents
Organic silicon heat insulation layer for engine and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses an organic silicon heat insulation layer for an engine and a preparation method thereof, wherein the raw materials of the organic silicon heat insulation layer comprise: the heat-vulcanized two-component liquid silicone rubber serving as a matrix raw material, powdery ablation-resistant filler, density-reducing filler, antioxidant, coolant, phosphorus flame retardant and fiber filler; the powdery ablation-resistant filler is zirconium silicide and holmium trioxide, the density-reducing filler is phenolic hollow microspheres, the antioxidant is boron carbide, the coolant is basic magnesium carbonate, the phosphorus flame retardant is FR-103 flame retardant, and the fiber filler is phenolic fibers and high silica fibers. The invention can prepare the organic silicon heat insulation layer for the engine, which has ablation resistance, good mechanical property, low heat conduction, low density and low glass transition temperature.
Description
Technical Field
The invention relates to a heat insulation layer for an engine, which is suitable for heat protection of various engines, is particularly suitable for heat protection of a combustion chamber of a ramjet engine which works for a long time and has severe working conditions, and can be widely applied to the fields of spaceflight, aviation, weapons, ships and the like.
Background
The heat insulating layer material of the engine can be generally divided into three types according to the molecular structure, namely a silicon-based heat insulating layer, a carbon-based heat insulating layer and an organic polymer-based heat insulating layer. The carbon-based heat insulation layer material has excellent ablation resistance and scouring resistance, but the density is high, so that the negative weight of the engine is increased; the thermal conductivity is very high, and the purpose of heat insulation cannot be achieved by single use; the engine housing cannot be integrally molded, the engine housing needs to be manufactured into a block in advance and then molded on the inner surface of the engine housing by adopting a paving and bonding method, so that the connection and the sealing performance of the engine housing are poor, and the most fatal defects are large difficulty in processing and assembly, long manufacturing period and extremely high manufacturing cost.
The organic polymer-based heat insulation layer has low manufacturing cost, density and heat conductivity, but has low carbon forming strength and poor ablation resistance and erosion resistance, and can not meet the requirement of missile weapon engine development on heat protection.
In comparison, the silicon-based heat insulation layer integrates the advantages of the carbon-based heat insulation layer and the organic polymer-based heat insulation layer, has excellent ablation resistance and scouring resistance, and has the advantages of low density, low heat conduction, integral forming, low manufacturing cost, short period and the like, so that the silicon-based heat insulation layer is always used as a preferred material for the heat insulation layer of the engine by domestic and foreign heat protection workers.
The research work of silicon-based heat-insulating materials in units such as weapons 204 institute, space four schools 42 institute, 46 institute and the like in China from the last 90 years has achieved considerable results at present. The technical research on the high-efficiency organic silicon heat-insulating layer developed during the 'eleven-five' period of the weapon 204 successfully passes the general assembly acceptance in 2010, the ablative performance of the developed silicon-based heat-insulating layer reaches the domestic leading, and the solid ramjet engine runs the flight test assessment in 300 seconds for the first time in China; with the development of the technology of the ramjet engine, higher requirements are provided for the mechanical property, the density, the heat conduction, the long storage life and the glass transition temperature of the formula, and the existing formula technology cannot cover a plurality of excellent properties, so that the improvement of the mechanical property of the heat-insulating layer, the extension of the storage life, the reduction of the density, the heat conduction and the glass transition temperature (below minus 55 ℃) become the research direction of the formula of the heat-insulating layer of the new-generation engine.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides the organic silicon heat insulation layer for the engine, which has the advantages of ablation resistance, good mechanical property, low heat conduction, low density and low glass transition temperature, and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a silicone heat insulating layer for an engine, the silicone heat insulating layer being made of a raw material comprising: the heat-vulcanized two-component liquid silicone rubber serving as a base raw material, powdery ablation-resistant filler, density-reducing filler, antioxidant, coolant, phosphorus flame retardant and fiber filler.
The invention also comprises the following technical characteristics:
specifically, the powdery ablation-resistant filler is zirconium silicide and holmium trioxide, the density-reducing filler is phenolic hollow microspheres, the antioxidant is boron carbide, the coolant is basic magnesium carbonate, the phosphorus flame retardant is FR-103 flame retardant, and the fiber filler is phenolic fibers and high silica fibers.
Specifically, the feed is prepared from the following raw materials in percentage by mass: 36.36-38.06% of heat-vulcanized two-component liquid silicone rubber, 14.80-14.87% of zirconium silicide, 9.16-9.45% of holmium trioxide, 4.27-4.64% of phenolic hollow microspheres, 7.96-8.38% of boron carbide, 6.60-6.77% of basic magnesium carbonate, 11.65-12.12% of phosphorus flame retardant, 2.97-3.03% of phenolic fibers and 4.45-4.47% of high silica fibers.
Specifically, the feed is prepared from the following raw materials in percentage by mass: 37.18 percent of heat-vulcanized two-component liquid silicone rubber, 14.87 percent of zirconium silicide, 9.29 percent of holmium trioxide, 4.46 percent of phenolic hollow microspheres, 8.18 percent of boron carbide, 6.69 percent of basic magnesium carbonate, 11.90 percent of phosphorus flame retardant, 2.97 percent of phenolic fibers and 4.46 percent of high silica fibers.
Specifically, the phenolic aldehyde hollow microsphere has the particle size of 0.4mm and the wall thickness of 40 microns.
Specifically, the length of the phenolic fiber is 3 mm-4 mm.
Specifically, the length of the high silica fiber is 7 mm-8 mm.
A preparation method of an organic silicon heat insulating layer for an engine comprises the following steps:
step 1, weighing the following components according to the formula: the heat-vulcanized double-component silicone rubber comprises heat-vulcanized double-component liquid silicone rubber, zirconium silicide, holmium trioxide, phenolic aldehyde hollow microspheres, boron carbide, basic magnesium carbonate, a phosphorus flame retardant, phenolic fibers and high silica fibers; the component A and the component B in the heat-vulcanized two-component liquid silicone rubber are equal in quantity; putting the component A in the heat-vulcanized two-component liquid silicone rubber, zirconium silicide, holmium trioxide, phenolic aldehyde hollow microspheres, boron carbide, basic magnesium carbonate, a phosphorus flame retardant, phenolic fibers and high silica fibers into a speed-adjustable multifunctional mixer, and mixing and stirring for 30-60 minutes; adding the component B in the heat-vulcanized two-component liquid silicone rubber, and continuously stirring for 10-15 minutes to form a heat insulation layer rubber material with good uniformity;
step 2, performing oil removal and sand blasting surface treatment on the inner wall of the engine shell, and then brushing and adhering a transition coating; after the transition coating is completely dried, forming the heat insulation layer rubber material obtained in the step 1 on the engine shell by using a heat insulation layer forming machine, and then heating and vulcanizing at high temperature; and demolding after the heat insulating layer is completely cured to finish the preparation of the heat insulating layer.
Compared with the prior art, the invention has the beneficial technical effects that:
1. the organic silicon heat insulating layer for the engine has good mechanical property: the tensile strength is more than or equal to 8MPa at the temperature of 20 ℃;
2. the invention reduces the density of the heat insulating layer and effectively lightens the startingA negative weight; the density is less than or equal to 1.08g/cm at 20 DEG C3；
3. The invention reduces the heat conductivity coefficient of the heat insulating layer, further effectively protects the engine shell when the engine works, and the heat conductivity coefficient is less than or equal to 0.18W/M.K at 20 ℃;
4. the invention greatly reduces the vitrification temperature of the heat insulating layer, improves the aging performance, and increases the long-term storage life, and the vitrification temperature is less than or equal to-57.2 ℃;
5. the invention has simple process, reduces the molding period and ensures the molding quality.
Detailed Description
The invention discloses an organic silicon heat insulation layer for an engine and a preparation method thereof, wherein the raw materials of the organic silicon heat insulation layer comprise: the heat-vulcanized two-component liquid silicone rubber serving as a base raw material, powdery ablation-resistant filler, density-reducing filler, antioxidant, coolant, phosphorus flame retardant and fiber filler.
The powdery ablation-resistant filler is zirconium silicide and holmium trioxide, the density-reducing filler is phenolic hollow microspheres, the antioxidant is boron carbide, the coolant is basic magnesium carbonate, the phosphorus flame retardant is FR-103 flame retardant, and the fibrous filler is phenolic fibers and high silica fibers.
The composite material is prepared from the following raw materials in percentage by mass: 36.36-38.06% of heat-vulcanized two-component liquid silicone rubber, 14.80-14.87% of zirconium silicide, 9.16-9.45% of holmium trioxide, 4.27-4.64% of phenolic hollow microspheres, 7.96-8.38% of boron carbide, 6.60-6.77% of basic magnesium carbonate, 11.65-12.12% of phosphorus flame retardant, 2.97-3.03% of phenolic fibers and 4.45-4.47% of high silica fibers.
Preferably, the composition is prepared from the following raw materials in percentage by mass: 37.18 percent of heat-vulcanized two-component liquid silicone rubber, 14.87 percent of zirconium silicide, 9.29 percent of holmium trioxide, 4.46 percent of phenolic hollow microspheres, 8.18 percent of boron carbide, 6.69 percent of basic magnesium carbonate, 11.90 percent of phosphorus flame retardant, 2.97 percent of phenolic fibers and 4.46 percent of high silica fibers.
The particle size of the phenolic aldehyde hollow microsphere is 0.4mm, and the wall thickness is 40 microns.
The length of the phenolic fiber is 3 mm-4 mm.
The length of the high silica fiber is 7 mm-8 mm.
A preparation method of an organic silicon heat insulating layer for an engine comprises the following steps:
step 1, weighing the following components according to the formula: the heat-vulcanized double-component silicone rubber comprises heat-vulcanized double-component liquid silicone rubber, zirconium silicide, holmium trioxide, phenolic aldehyde hollow microspheres, boron carbide, basic magnesium carbonate, a phosphorus flame retardant, phenolic fibers and high silica fibers; the component A and the component B in the heat-vulcanized two-component liquid silicone rubber are equal in quantity; putting the component A in the heat-vulcanized two-component liquid silicone rubber, zirconium silicide, holmium trioxide, phenolic aldehyde hollow microspheres, boron carbide, basic magnesium carbonate, a phosphorus flame retardant, phenolic fibers and high silica fibers into a speed-adjustable multifunctional mixer, and mixing and stirring for 30-60 minutes; adding the component B in the heat-vulcanized two-component liquid silicone rubber, and continuously stirring for 10-15 minutes to form a heat insulation layer rubber material with good uniformity;
step 2, performing oil removal and sand blasting surface treatment on the inner wall of the engine shell, and then brushing and adhering a transition coating; after the transition coating is completely dried, forming the heat insulation layer rubber material obtained in the step 1 on the engine shell by using a heat insulation layer forming machine, and then heating and vulcanizing at high temperature; and demolding after the heat insulating layer is completely cured to finish the preparation of the heat insulating layer.
The present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention fall within the protection scope of the present invention.
Example 1:
the present embodiment discloses a silicone heat insulating layer for an engine and a method for manufacturing the same, wherein the silicone heat insulating layer comprises the following raw materials: the heat-vulcanized two-component liquid silicone rubber serving as a base raw material, powdery ablation-resistant filler, density-reducing filler, antioxidant, coolant, phosphorus flame retardant and fiber filler.
The powdery ablation-resistant filler is zirconium silicide and holmium trioxide, the density-reducing filler is phenolic hollow microspheres, the antioxidant is boron carbide, the coolant is basic magnesium carbonate, the phosphorus flame retardant is FR-103 flame retardant, and the fibrous filler is phenolic fibers and high silica fibers.
The composite material is prepared from the following raw materials in percentage by mass: 37.18 percent of heat-vulcanized two-component liquid silicone rubber (A/B), 14.87 percent of zirconium silicide, 9.29 percent of holmium trioxide, 4.46 percent of phenolic hollow microspheres, 8.18 percent of boron carbide, 6.69 percent of basic magnesium carbonate, 11.90 percent of phosphorus flame retardant, 2.97 percent of phenolic fibers and 4.46 percent of high silica fibers.
The particle size of the phenolic aldehyde hollow microsphere is 0.4mm, and the wall thickness is 40 microns.
The length of the phenolic fiber is 3 mm-4 mm.
The length of the high silica fiber is 7 mm-8 mm.
The preparation method of the organic silicon heat insulation layer for the engine comprises the following steps:
step 1, weighing the following components according to the formula: the heat-vulcanized double-component silicone rubber comprises heat-vulcanized double-component liquid silicone rubber, zirconium silicide, holmium trioxide, phenolic aldehyde hollow microspheres, boron carbide, basic magnesium carbonate, a phosphorus flame retardant, phenolic fibers and high silica fibers; the component A and the component B in the heat-vulcanized two-component liquid silicone rubber are equal in quantity; putting the component A in the heat-vulcanized two-component liquid silicone rubber, zirconium silicide, holmium trioxide, phenolic aldehyde hollow microspheres, boron carbide, basic magnesium carbonate, a phosphorus flame retardant, phenolic fibers and high silica fibers into a speed-adjustable multifunctional mixer, and mixing and stirring for 30 minutes; then adding the component B in the heat-vulcanized two-component liquid silicone rubber, and continuously stirring for 10 minutes to form a heat-insulating layer rubber material with good uniformity;
step 2, performing oil removal and sand blasting surface treatment on the inner wall of the engine shell, and then brushing and adhering a transition coating; after the transition coating is completely dried, forming the heat insulation layer rubber material obtained in the step 1 on the engine shell by using a heat insulation layer forming machine, and then heating and vulcanizing at high temperature; and demolding after the heat insulating layer is completely cured to finish the preparation of the heat insulating layer.
Performance testing of the insulation layer material of this example
The engine test of the embodiment:
the experimental conditions are as follows: the temperature is about 1800 ℃, the oxygen enrichment rate is 17%, the air flow rate is 600mm/s, the heat insulating layer of the invention is successfully examined by 315 seconds engine tests, and the residual shell is complete.
Example 2:
the present embodiment discloses a silicone heat insulating layer for an engine and a method for manufacturing the same, wherein the silicone heat insulating layer comprises the following raw materials: the heat-vulcanized two-component liquid silicone rubber serving as a base raw material, powdery ablation-resistant filler, density-reducing filler, antioxidant, coolant, phosphorus flame retardant and fiber filler.
The powdery ablation-resistant filler is zirconium silicide and holmium trioxide, the density-reducing filler is phenolic hollow microspheres, the antioxidant is boron carbide, the coolant is basic magnesium carbonate, the phosphorus flame retardant is FR-103 flame retardant, and the fibrous filler is phenolic fibers and high silica fibers.
The composite material is prepared from the following raw materials in percentage by mass: 38.06% of heat-vulcanized two-component liquid silicone rubber (A/B), 14.80% of zirconium silicide, 9.16% of holmium trioxide, 4.27% of phenolic hollow microspheres, 7.96% of boron carbide, 6.60% of basic magnesium carbonate, 11.65% of phosphorus flame retardant, 3.03% of phenolic fibers and 4.47% of high silica fibers.
The particle size of the phenolic aldehyde hollow microsphere is 0.4mm, and the wall thickness is 40 microns.
The length of the phenolic fiber is 3 mm-4 mm.
The length of the high silica fiber is 7 mm-8 mm.
The preparation method and condition parameters of the organic silicon heat insulating layer for the engine in the embodiment are the same as those of the embodiment 1.
Performance test of the insulating layer of this example
The engine test of the embodiment: the experimental conditions were the same as in example 1. The accumulated time of the heat insulating layer of the invention is 156 seconds after the ramjet engine experiment, and the heat insulating layer shell is complete.
Example 3:
the present embodiment discloses a silicone heat insulating layer for an engine and a method for manufacturing the same, wherein the silicone heat insulating layer comprises the following raw materials: the heat-vulcanized two-component liquid silicone rubber serving as a base raw material, powdery ablation-resistant filler, density-reducing filler, antioxidant, coolant, phosphorus flame retardant and fiber filler.
The powdery ablation-resistant filler is zirconium silicide and holmium trioxide, the density-reducing filler is phenolic hollow microspheres, the antioxidant is boron carbide, the coolant is basic magnesium carbonate, the phosphorus flame retardant is FR-103 flame retardant, and the fibrous filler is phenolic fibers and high silica fibers.
The composite material is prepared from the following raw materials in percentage by mass: 36.36% of heat-vulcanized two-component liquid silicone rubber (A/B), 14.80% of zirconium silicide, 9.45% of holmium trioxide, 4.64% of phenolic hollow microspheres, 8.38% of boron carbide, 6.77% of basic magnesium carbonate, 12.12% of phosphorus flame retardant, 3.03% of phenolic fibers and 4.45% of high silica fibers.
The particle size of the phenolic aldehyde hollow microsphere is 0.4mm, and the wall thickness is 40 microns.
The length of the phenolic fiber is 3 mm-4 mm.
The length of the high silica fiber is 7 mm-8 mm.
The preparation method of the organic silicon heat insulating layer for the engine is the same as that of the embodiment 1.
Performance test of the insulating layer of this example
The engine test of the embodiment: the experimental conditions were the same as in example 1. The time of the heat insulating layer of the invention accumulated by the ramjet engine test is 245 seconds, and the heat insulating layer casing is complete.
Claims (8)
1. A silicone heat insulating layer for an engine, characterized in that the raw material of the silicone heat insulating layer comprises: the heat-vulcanized two-component liquid silicone rubber serving as a base raw material, powdery ablation-resistant filler, density-reducing filler, antioxidant, coolant, phosphorus flame retardant and fiber filler.
2. The silicone heat insulation layer of claim 1, wherein the powdery ablation-resistant filler is zirconium silicide and holmium trioxide, the density-reducing filler is phenolic hollow microspheres, the antioxidant is boron carbide, the coolant is basic magnesium carbonate, the phosphorus flame retardant is FR-103 flame retardant, and the fibrous filler is phenolic fibers and high silica fibers.
3. The silicone heat insulating layer for an engine according to claim 2, characterized by being made from the following raw materials in percentage by mass: 36.36-38.06% of heat-vulcanized two-component liquid silicone rubber, 14.80-14.87% of zirconium silicide, 9.16-9.45% of holmium trioxide, 4.27-4.64% of phenolic hollow microspheres, 7.96-8.38% of boron carbide, 6.60-6.77% of basic magnesium carbonate, 11.65-12.12% of phosphorus flame retardant, 2.97-3.03% of phenolic fibers and 4.45-4.47% of high silica fibers.
4. The silicone heat insulating layer for an engine according to claim 3, which is made from the following raw materials in percentage by mass: 37.18 percent of heat-vulcanized two-component liquid silicone rubber, 14.87 percent of zirconium silicide, 9.29 percent of holmium trioxide, 4.46 percent of phenolic hollow microspheres, 8.18 percent of boron carbide, 6.69 percent of basic magnesium carbonate, 11.90 percent of phosphorus flame retardant, 2.97 percent of phenolic fibers and 4.46 percent of high silica fibers.
5. The silicone heat insulating layer for an engine according to claim 3, wherein the phenolic hollow microspheres have a particle size of 0.4mm and a wall thickness of 40 μm.
6. The silicone heat insulating layer for an engine according to claim 3, wherein the phenolic fiber has a length of 3mm to 4 mm.
7. The heat-insulating silicone layer for an engine according to claim 3, wherein the length of the high-silica fiber is 7mm to 8 mm.
8. The preparation method of the organic silicon heat insulation layer for the engine is characterized by comprising the following steps:
step 1, weighing the following components according to the formula: the heat-vulcanized double-component silicone rubber comprises heat-vulcanized double-component liquid silicone rubber, zirconium silicide, holmium trioxide, phenolic aldehyde hollow microspheres, boron carbide, basic magnesium carbonate, a phosphorus flame retardant, phenolic fibers and high silica fibers; the component A and the component B in the heat-vulcanized two-component liquid silicone rubber are equal in quantity; putting the component A in the heat-vulcanized two-component liquid silicone rubber, zirconium silicide, holmium trioxide, phenolic aldehyde hollow microspheres, boron carbide, basic magnesium carbonate, a phosphorus flame retardant, phenolic fibers and high silica fibers into a speed-adjustable multifunctional mixer, and mixing and stirring for 30-60 minutes; adding the component B in the heat-vulcanized two-component liquid silicone rubber, and continuously stirring for 10-15 minutes to form a heat insulation layer rubber material with good uniformity;
step 2, performing oil removal and sand blasting surface treatment on the inner wall of the engine shell, and then brushing and adhering a transition coating; after the transition coating is completely dried, forming the heat insulation layer rubber material obtained in the step 1 on the engine shell by using a heat insulation layer forming machine, and then heating and vulcanizing at high temperature; and demolding after the heat insulating layer is completely cured to finish the preparation of the heat insulating layer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115488019A (en) * | 2022-08-31 | 2022-12-20 | 山西北方兴安化学工业有限公司 | Preparation process of solid rocket engine combustion chamber inner wall heat insulation coating |
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| CN111171721A (en) * | 2020-01-22 | 2020-05-19 | 西安近代化学研究所 | Ceramizable ablation-resistant coating and preparation method thereof |
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| GB1066294A (en) * | 1963-04-01 | 1967-04-26 | Kurt Herberts | Process relating to fire-protective coating compositions |
| CN105111935A (en) * | 2015-09-02 | 2015-12-02 | 航天材料及工艺研究所 | High-temperature-resistant and high-radiation-resistant thermal control coating and preparation method thereof |
| CN107686559A (en) * | 2017-09-29 | 2018-02-13 | 西安近代化学研究所 | A kind of engine composite adiabatic layer |
| CN110819228A (en) * | 2019-11-29 | 2020-02-21 | 北京理工大学 | Heat-insulation ablation-resistant maintainable repair agent and coating dual-purpose slurry, preparation method and application |
| CN111171721A (en) * | 2020-01-22 | 2020-05-19 | 西安近代化学研究所 | Ceramizable ablation-resistant coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115488019A (en) * | 2022-08-31 | 2022-12-20 | 山西北方兴安化学工业有限公司 | Preparation process of solid rocket engine combustion chamber inner wall heat insulation coating |
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