CN112625318A - Environment-friendly ablation-resistant rubber type heat-insulating layer and preparation method thereof - Google Patents
Environment-friendly ablation-resistant rubber type heat-insulating layer and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an environment-friendly ablation-resistant rubber type heat-insulating layer, which is prepared by taking nitrile rubber as a main material, introducing novel heat-resistant fibers and resin, and mixing the materials in a certain weight part ratio, wherein all the raw materials are green and environment-friendly. The raw materials are mixed through the working procedures to prepare rubber compound, and the environment-friendly ablation-resistant rubber type heat insulation layer is obtained. Compared with the prior art, the environment-friendly ablation-resistant heat-insulating layer has excellent ablation performance, good bonding performance of each interface and high tensile strength and elongation at break. The heat insulating layer can be applied to the field of heat insulating layer materials in solid rocket engines.
Description
Technical Field
The invention belongs to the technical field of thermal protection materials, and particularly relates to an environment-friendly ablation-resistant rubber type heat insulation layer and a preparation method thereof.
Background
The heat insulation layer of the solid rocket engine is a non-metal heat insulation protective material positioned between the inner surface of the shell and the propellant, when the solid rocket engine works, the heat insulation layer absorbs heat and decomposes to take away part of heat, and simultaneously forms a carbonization layer to resist scouring and ablation of high-temperature gas, so that the heat generated by the high-temperature gas is delayed to be transferred to the shell, the shell is prevented from reaching the temperature which endangers the structural integrity of the shell, and the normal work of the engine is ensured. At present, the internal and external heat insulation materials mainly comprise two types, one is a flexible material taking rubber as a matrix, and the other is a rigid material taking resin as a matrix, wherein the flexible material is commonly a nitrile rubber heat insulation layer, an ethylene propylene diene monomer heat insulation layer, a silicon rubber heat insulation layer and a blended rubber heat insulation layer.
The flexible material is widely applied to the aspect of heat insulation in the solid rocket motor due to good process performance, low density, low heat conductivity and the like. However, the flexible material alone cannot form a high-strength carbonized layer after carbonization, which results in the thermal insulation material being not resistant to erosion by air flow, and therefore, it is necessary to add ablation-resistant fibers, flame retardants, heat-resistant resins, etc., to improve the integrity and firmness of the carbonized layer and reduce the ablation rate. The ablation-resistant fiber mainly includes inorganic fibers such as asbestos fiber, glass fiber, and carbon fiber, and organic fibers such as aramid fiber, phenol fiber, aramid fiber, and polyimide fiber. At present, aramid fiber and polyimide fiber are widely applied to heat-insulating materials due to the advantages of high strength, low density, high temperature resistance, good chemical stability and the like. The flame retardants are mainly classified into organic and inorganic types, wherein the organic flame retardants mainly comprise organic halogen flame retardants, organic phosphorus flame retardants and organic silicon flame retardants; the inorganic flame retardant mainly comprises aluminum hydroxide, magnesium hydroxide, ammonium polyphosphate and the like. The zinc borate is a novel environment-friendly flame retardant, has the characteristics of high thermal stability, small specific gravity, good dispersibility and the like, and is widely applied as an efficient flame retardant. The ablation-resistant resin has been used for a composite material of a solid rocket engine nozzle due to excellent heat resistance and high char formation, has a certain application value in ablation materials, and is one of important materials for improving the quality of a heat-insulating layer carbon layer. The currently widely used resins mainly include phenolic resins, boron phenolic resins, polyphenylene sulfide resins, benzoxazine resins and silicone resins.
At present, nitrile rubber heat insulation layers are developed for a long time in China and have a plurality of perfect formulas, but most nitrile rubber heat insulation layers contain toxic and harmful substances, most nitrile rubber heat insulation layers are reported to adopt asbestos fibers as flame retardant fiber agents in the last century, and since the asbestos fibers are carcinogens and are gradually replaced by other fibers, people who write on Gunn and the like report that halogen-antimony containing flame retardants are used, aramid fibers replace the asbestos fibers, and the formula of the ablation-resistant nitrile rubber heat insulation layers is developed; li Yinni et al reported that boron phenolic resin/phenolic fiber can replace asbestos to prepare nitrile-based insulation layer material. The Wangming super-grade adopts silicone resin and pps resin to improve the ablation property of the nitrile rubber heat-insulating layer, but the elongation at break of the heat-insulating layer is lower. Meanwhile, with the development of a solid propulsion technology, higher requirements are put forward on the ablation performance of an inner heat-insulating layer, and related reports of an environment-friendly ablation-resistant nitrile rubber heat-insulating layer with excellent mechanical properties are not seen at present.
Disclosure of Invention
The invention aims to overcome the defects and provide an environment-friendly ablation-resistant rubber type heat-insulating layer and a preparation method thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides an environment-friendly ablation-resistant rubber heat-insulating layer which comprises the following raw materials in parts by weight:
the heat-resistant fiber is one or a combination of more than one of aramid chopped fiber and polyimide chopped fiber, and is preferably terpene phenolic resin.
The resin is one or more of terpene phenolic resin, disproportionated rosin glycerin resin, rosin glycerin resin or hydrogenated rosin glycerin resin.
Further, the silicon dioxide is general silicon dioxide powder sold in the market, and comprises a precipitation method and a gas phase preparation method for silicon dioxide.
Further, the metal oxide is zinc oxide powder.
Furthermore, the heat-resistant fiber is a combination of aramid chopped fiber and polyimide chopped fiber, and in the combination of the aramid chopped fiber and the polyimide chopped fiber, the mass percentage of the polyimide chopped fiber is 40-100%.
Further, the flame retardant is one or a combination of more than one of antimony trioxide or zinc borate.
Further, the anti-aging agent is N- (1, 3-dimethylbutyl) -N' -phenyl-p-phenylenediamine; the vulcanization accelerator is one or more of 2-thiol benzothiazole or N-cyclohexyl-2-benzothiazole sulfonamide; the vulcanizing agent is sulfur powder.
Further, the plasticizer is chlorinated liquid paraffin; the plasticizer includes, but is not limited to, chlorinated liquid paraffin-42 and chlorinated liquid paraffin-52.
Furthermore, the single filament number of the heat-resistant fiber is 1.0-2.0dtex, and the length is 2-6 mm.
The preparation method of the environment-friendly ablation-resistant rubber heat-insulating layer comprises the following steps:
(1) at room temperature, sequentially adding nitrile rubber, silicon dioxide, metal oxide, heat-resistant fiber, a flame retardant, a resin plasticizer and an anti-aging agent according to a proportion, and then carrying out open milling or banburying to obtain a rubber compound;
(2) adding a vulcanization accelerator and a vulcanizing agent into the rubber compound, mixing, thinning and uniformly discharging the mixture to obtain a sheet;
(3) and (3) vulcanizing and molding the rubber compound obtained in the step (2) to obtain the environment-friendly ablation-resistant nitrile rubber type heat-insulating layer.
Further, in the step (3), the temperature for vulcanizing and molding the rubber compound is 140-180 ℃, and the time is 15-90 min.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides a novel formula for preparing a nitrile rubber type heat-insulating layer, which is characterized in that terpene phenolic resin, disproportionated rosin glycerin resin, rosin glycerin resin or hydrogenated rosin glycerin resin are introduced for the first time, and aramid chopped fiber or polyimide chopped fiber is used as heat-resistant fiber, so that the ablation resistance of the nitrile rubber type heat-insulating layer is obviously improved, and the nitrile rubber type heat-insulating layer has higher elongation at break.
(2) The carbonized layer obtained under the condition of oxyacetylene ablation has high strength, is firmly attached to the base material and has no shedding phenomenon.
(3) All raw materials of the formula of the nitrile rubber type heat insulation layer are green and environment-friendly, and do not contain harmful substances such as asbestos, halogen and the like.
Drawings
FIG. 1 is a photograph of the morphology of a sample obtained in example 4 of the present invention before and after ablation with oxyacetylene;
FIG. 2 is a scanning electron micrograph of a sample carbonized layer obtained in example 4 of the present invention.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The invention relates to an environment-friendly ablation-resistant rubber heat-insulating layer which is prepared from the following raw materials in parts by mass:
nitrile rubber: 100-102;
silicon dioxide: 8-15 parts of;
3-10 parts of metal oxide;
8-20 parts of heat-resistant fibers;
20-40 parts of flame retardant;
8-15 parts of resin;
5-15 parts of plasticizer;
0.5-2 parts of anti-aging agent;
0.5-2 parts of vulcanization accelerator;
1-5 parts of a vulcanizing agent;
the heat-resistant fiber is one or more of aramid chopped fiber or polyimide chopped fiber; the resin is one or more of commercially available terpene phenolic resin, disproportionated rosin glycerin resin, rosin glycerin resin or hydrogenated rosin glycerin resin, preferably terpene phenolic resin.
Further, the silica is commercially available general-purpose fine silica powder, including but not limited to precipitation method and gas phase preparation silica.
Further, the metal oxide is commercially available zinc oxide powder.
Furthermore, the heat-resistant fiber is a combination of aramid chopped fiber and polyimide chopped fiber, and in the combination of the aramid chopped fiber and the polyimide chopped fiber, the mass percentage of the polyimide chopped fiber is 40-100%.
Further, the flame retardant is one or more of antimony trioxide or zinc borate.
Further, the anti-aging agent is N- (1, 3-dimethylbutyl) -N' -phenyl-p-phenylenediamine; the vulcanization accelerator is one or more of 2-thiol benzothiazole or N-cyclohexyl-2-benzothiazole sulfonamide; the vulcanizing agent is sulfur powder.
Further, the plasticizer is a commercially available chlorinated liquid paraffin, including but not limited to chlorinated liquid paraffin-42 and chlorinated liquid paraffin-52.
Furthermore, the single filament number of the heat-resistant fiber is 1.0-2.0dtex, and the length is 2-6 mm.
A preparation method of an environment-friendly ablation-resistant rubber type heat insulating layer comprises the following steps:
(1) at room temperature, sequentially adding nitrile rubber, silicon dioxide, metal oxide, heat-resistant fiber, flame retardant, resin and plasticizer in proportion, and then carrying out open milling or banburying to obtain a rubber compound; specifically, under the working condition of room temperature, nitrile rubber, silicon dioxide, metal oxide, heat-resistant fiber, flame retardant, resin, plasticizer and anti-aging agent are sequentially added into a double-roller open mill according to a certain proportion and are mixed uniformly; or gradually adding the filler into an internal mixer for uniformly mixing.
(2) Adding an anti-aging agent, a vulcanization accelerator and a vulcanizing agent into the rubber compound, mixing, thinning and uniformly discharging to obtain a sheet;
(3) and (3) vulcanizing and molding the rubber compound obtained in the step (2) to obtain the environment-friendly ablation-resistant nitrile rubber type heat-insulating layer.
Further, in the step (3), the temperature for vulcanizing and molding the rubber compound is 140-180 ℃, and the time is 15-90 min.
In the examples, the amounts not specifically described are parts by mass.
The nitrile rubber is NBR3604 of Lanzhou petrochemical company in China, the acrylonitrile content is 36-40%, and the Mooney viscosity is 40-65.
Example 1
Under the working condition of room temperature, 100 parts of nitrile rubber, 10 parts of silicon dioxide, 5 parts of zinc oxide, 8 parts of polyimide fiber, 4 parts of aramid fiber, 10 parts of antimony trioxide, 20 parts of zinc borate, 8 parts of terpene phenolic resin, 9 parts of chlorinated paraffin CP52 (chlorinated liquid paraffin-52) and 1 part of anti-aging agent 4020(N- (1, 3-dimethylbutyl) -N' -phenyl-p-phenylenediamine) are sequentially added into a double-roll open mill to be uniformly mixed, and finally, 2 parts of sulfur powder and 0.8 part of vulcanization accelerator M (2-thiol benzothiazole) are added to be uniformly mixed and thinned, and then the sheet is obtained. And vulcanizing the mixture for 40 minutes at 160 ℃ in a flat vulcanizing machine for molding to obtain the environment-friendly ablation-resistant nitrile rubber type heat insulating layer.
Ablation rate of oxyacetylene wire: 0.082mm/s, tensile strength: 8.22 MPa; elongation at break: 616.7 percent.
Example 2
Under the working condition of room temperature, 100 parts of nitrile rubber, 10 parts of silicon dioxide, 3 parts of zinc oxide, 6 parts of polyimide fiber, 4 parts of aramid fiber, 30 parts of zinc borate, 10 parts of disproportionated rosin glycerol resin, 10 parts of chlorinated paraffin CP52 (chlorinated liquid paraffin-52) and 40201 parts of anti-aging agent are sequentially added into a double-roll milling machine for uniform mixing, finally 2 parts of sulfur powder and 0.8 part of vulcanization accelerator M (2-thiol benzothiazole) are added, and the mixture is mixed, thinned and uniformly mixed and discharged. And vulcanizing the mixture for 40 minutes at 160 ℃ in a flat vulcanizing machine for molding to obtain the environment-friendly ablation-resistant nitrile rubber type heat insulating layer.
Ablation rate of oxyacetylene wire: 0.096mm/s, tensile strength: 9.28 MPa; elongation at break: 641.2 percent.
Example 3
Under the working condition of room temperature, 100 parts of nitrile rubber, 10 parts of silicon dioxide, 8 parts of zinc oxide, 10 parts of polyimide fiber, 8 parts of antimony trioxide, 20 parts of zinc borate, 9 parts of rosin glycerol resin, 10 parts of chlorinated paraffin CP42 (chlorinated liquid paraffin-42) and 40201 parts of anti-aging agent are added into a double-roll mill for mixing uniformly, finally 2 parts of sulfur powder and 0.8 part of vulcanization accelerator M (2-thiol benzothiazole) are added, mixing and passing uniformly are carried out, and sheets are obtained. And vulcanizing the mixture for 40 minutes at 160 ℃ in a flat vulcanizing machine for molding to obtain the environment-friendly ablation-resistant nitrile rubber type heat insulating layer.
Ablation rate of oxyacetylene wire: 0.091mm/s, tensile strength: 8.18 MPa; elongation at break: 521.6 percent.
Example 4
Under the working condition of room temperature, 100 parts of nitrile rubber, 10 parts of silicon dioxide, 5 parts of zinc oxide, 8 parts of polyimide fiber, 4 parts of aramid fiber, 30 parts of zinc borate, 10 parts of terpene phenolic resin, 10 parts of chlorinated paraffin CP42 (chlorinated liquid paraffin-42) and 10 parts of anti-aging agent 40201 are added into a double-roll mill for mixing uniformly, finally 2 parts of sulfur powder and 1 part of vulcanization accelerator CZ (N-cyclohexyl-2-benzothiazole sulfenamide) are added, mixing and passing uniformly are carried out, and sheets are obtained. And vulcanizing the mixture for 40 minutes at 160 ℃ in a flat vulcanizing machine for molding to obtain the environment-friendly ablation-resistant nitrile rubber type heat insulating layer.
Ablation rate of oxyacetylene wire: 0.076mm/s, tensile strength: 7.88 MPa; elongation at break: 584.7 percent. FIG. 1 is a photograph of the morphology of the sample before and after ablation with oxyacetylene, which shows that the carbonized layer on the surface of the ablated sample is complete and smooth, the surface of the carbonized layer has no cracking phenomenon, and the carbonized layer is tightly bonded with the base material; fig. 2 is a scanning electron microscope image of the obtained sample carbonization layer, the carbonization layer has a uniform porous structure, and no obvious cracks are formed in the carbonization layer, which shows that the carbonization layer has a complete structure and is not easy to fall off under the oxyacetylene ablation condition, and the carbonization layer can fully play a role in heat insulation in the ablation process.
Comparative example 1
100 parts of nitrile rubber, 30 parts of silicon dioxide, 6 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of stearic acid, 30 parts of silicon resin, 10 parts of PPS resin, 10 parts of aramid fiber and 7 parts of carbon black are milled to be uniformly mixed under the working condition of room temperature, and finally 2 parts of sulfur, 0.5 part of 2-mercaptobenzothiazole and 1.5 parts of tetramethyl thiuram disulfide are added, mixed, thinned and uniformly mixed, and the mixture is taken out. And vulcanizing the mixture at 160 ℃ in a flat vulcanizing machine for 40 minutes to form the heat insulating layer of the comparative example.
Ablation rate of oxyacetylene wire: 0.078mm/s, tensile strength: 7.56 MPa; elongation at break: 267.7 percent.
Compared with the examples 1-4, although the oxyacetylene ablation rate and tensile strength of the heat-insulating layer of the comparative example are equivalent to those of the heat-insulating layers of the examples 1-4, the difference of the elongation at break is large, and the good mechanical property of the heat-insulating layer is difficult to ensure.
Comparative example 2
100 parts of nitrile rubber, 10 parts of silicon dioxide, 5 parts of zinc oxide, 2 parts of stearic acid, 10 parts of boron phenolic resin, 8 parts of polyimide fiber, 20 parts of zinc borate, 10 parts of antimony trioxide, 4210 parts of chlorinated paraffin CP, and 40201 parts of anti-aging agent are milled to be uniformly mixed under the working condition of room temperature, finally 2 parts of sulfur and 0.5 part of vulcanization accelerator M are added, and the mixture is mixed, thinned and uniformly discharged. And vulcanizing the mixture at 160 ℃ in a flat vulcanizing machine for 40 minutes to form the heat insulating layer of the comparative example.
Oxyacetylene ablation rate: 0.154 mm/s. Comparison with examples 1-4 shows that the use of commercially available terpene phenolic resins, disproportionated rosin glycerol resins, rosin glycerol resins or hydrogenated rosin glycerol resins in the formulations of the present invention is effective in reducing the oxyacetylene ablation rate of the thermal insulation layer.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (10)
1. An environment-friendly ablation-resistant rubber heat-insulating layer is characterized by comprising the following raw materials in parts by mass:
the heat-resistant fiber is one or a combination of more than one of aramid chopped fiber or polyimide chopped fiber;
the resin is one or more of terpene phenolic resin, disproportionated rosin glycerin resin, rosin glycerin resin or hydrogenated rosin glycerin resin.
2. The environment-friendly ablation-resistant rubber heat-insulating layer as claimed in claim 1, wherein the silica is a fine silica powder, and the preparation comprises a precipitation method and a gas phase preparation of silica.
3. The environmentally friendly ablation resistant rubber-type thermal insulation layer of claim 1 wherein said metal oxide is zinc oxide powder.
4. The environment-friendly ablation-resistant rubber heat-insulating layer as claimed in claim 1, wherein the heat-resistant fiber is a combination of aramid chopped fiber and polyimide chopped fiber, and the mass percentage of the polyimide chopped fiber in the combination is 40-100%.
5. The environment-friendly ablation-resistant rubber type heat-insulating layer as claimed in claim 1, wherein the flame retardant is one or more of antimony trioxide and zinc borate.
6. The environmentally friendly ablation-resistant rubber-type thermal insulation layer of claim 1, wherein the antioxidant is N- (1, 3-dimethylbutyl) -N' -phenyl-p-phenylenediamine; the vulcanization accelerator is one or more of 2-thiol benzothiazole or N-cyclohexyl-2-benzothiazole sulfonamide; the vulcanizing agent is sulfur powder.
7. The environmentally friendly ablation resistant rubber-type thermal insulation layer of claim 1 wherein the plasticizer is chlorinated liquid paraffin; the plasticizer is chlorinated liquid paraffin-42 or chlorinated liquid paraffin-52.
8. The environment-friendly ablation-resistant rubber-type thermal insulation layer as claimed in claim 1, wherein the heat-resistant fiber has a filament fineness of 1.0 to 2.0dtex and a length of 2 to 6 mm.
9. The method for preparing the environment-friendly ablation-resistant rubber type heat insulating layer according to any one of claims 1 to 8, which is characterized by comprising the following steps:
(1) at room temperature, sequentially adding nitrile rubber, silicon dioxide, metal oxide, heat-resistant fiber, a flame retardant, a resin plasticizer and an anti-aging agent according to a proportion, and then carrying out open milling or banburying to obtain a rubber compound;
(2) adding a vulcanization accelerator and a vulcanizing agent into the rubber compound, mixing, thinning and uniformly discharging the mixture to obtain a sheet;
(3) and (3) vulcanizing and molding the rubber compound obtained in the step (2) to obtain the environment-friendly ablation-resistant nitrile rubber type heat-insulating layer.
10. The method for preparing the environment-friendly ablation-resistant rubber type heat insulating layer as claimed in claim 9, wherein in the step (3), the temperature for vulcanizing and molding the rubber compound is 140-180 ℃ and the time is 15-90 min.
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| CN114230879A (en) * | 2022-01-05 | 2022-03-25 | 开滦（集团）有限责任公司 | Flame-retardant ablation-resistant butyronitrile heat-insulating material and preparation method thereof |
| CN114230879B (en) * | 2022-01-05 | 2023-09-12 | 开滦（集团）有限责任公司 | Flame-retardant ablation-resistant nitrile-butadiene heat-insulating material and preparation method thereof |
| CN115572420A (en) * | 2022-09-28 | 2023-01-06 | 上海航天化工应用研究所 | Cross-linked interpenetrating network structure nitrile rubber-heat-resistant resin heat-insulating material and preparation method thereof |
| CN115572420B (en) * | 2022-09-28 | 2023-12-12 | 上海航天化工应用研究所 | Nitrile rubber-heat-resistant resin heat-insulating material with cross-linked interpenetrating network structure and preparation method thereof |
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