CN115449225A - Light low-smoke fireproof heat-insulation silicon rubber material and preparation method thereof - Google Patents
Light low-smoke fireproof heat-insulation silicon rubber material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a light low-smoke fireproof heat-insulating silicone rubber material and a preparation method thereof, wherein the light low-smoke fireproof heat-insulating silicone rubber material comprises the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 30-50 parts of reinforcing filler, 40-60 parts of compounded porcelain filler, 20-50 parts of compounded fluxing agent, 30-50 parts of hollow ceramic microspheres, 15-30 parts of compounded flame-retardant smoke suppressant, 0.5-1.5 parts of crosslinking agent and 1-3 parts of silane coupling agent. According to the invention, the silicon rubber composite material with low density and excellent fireproof and heat-insulating properties is prepared by adopting specific components and proportions, when an airplane is on fire, the heat transfer is isolated, the further ablation can be effectively resisted, the damage caused by the fact that high-temperature flame or gas in a fire area enters other areas is prevented, airborne equipment and personnel can be effectively protected, and the flight safety of the airplane is ensured.
Description
Technical Field
The invention belongs to the technical field of special rubber, and particularly relates to a light low-smoke fireproof heat-insulating silicon rubber material and a preparation method thereof.
Background
The fireproof sealing material has very important application in the field of aviation, is mainly used in potential ignition areas of airplanes, including engine nacelles, hangers, APU cabins and other parts, has the function of fireproof sealing when the airplanes catch fire, and is vital to protecting airborne personnel and equipment and improving the flight safety of the airplanes. The requisite flight control systems, engine mounts and other flight structures located in a designated fire zone or in the vicinity of a fire that may be affected by the fire must be made of or shielded from a fire-resistant material to withstand the effects of the fire as required by the CCAR-25 airworthiness regulations. According to the definition of AC 20-135: fire protection (Fireproproof) refers to a material or structure that can perform the function required by a design when it is exposed to a flame of 2000F + -150F for 15 minutes.
In the field of aviation in China, researchers also carry out related research work, and the Chinese invention patent CN200910062254.5 fireproof silicone rubber composite material and the preparation method thereof are formed by hot-pressing and compounding 4 layers of silicone rubber fireproof isolation layer, silicone rubber flame-retardant cooling layer, silicone rubber anti-ablation layer and body silicone rubber layerThe flame is sprayed and burned at 1100 +/-50 ℃ for 15min, a sample with the thickness of 8mm is not burned through, the temperature of the back fire surface is lower than 400 ℃, but the flame-retardant rubber material is compounded by a plurality of layers of rubber materials, the molding process is complex, the fireproof function can be realized only when the flame-retardant rubber material reaches the higher thickness, and the application range of the flame-retardant rubber material is limited. The existing fireproof rubber material is generally high in specific gravity (mostly 1.4 g/cm) due to the addition of a large amount of flame-retardant filler 3 Above), the smog volume is big, still remains to promote in aspects such as structural integrity after the ignition, heat-proof quality, etc. to the fire prevention under some special operating mode of aircraft thermal-insulated and sealed requirement, can not satisfy completely yet.
Disclosure of Invention
The invention provides a light low-smoke fireproof heat-insulating silicone rubber material and a preparation method thereof, which have the advantages of low density, low smoke toxicity, excellent fireproof heat-insulating property and capability of meeting the fireproof sealing requirement of an airplane. In order to achieve the purpose, the technical scheme of the invention is as follows:
the light low-smoke fireproof heat-insulating silicon rubber material comprises the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 30-50 parts of reinforcing filler, 40-60 parts of compounded porcelain filler, 20-50 parts of compounded fluxing agent, 30-50 parts of hollow ceramic microspheres, 15-30 parts of compounded flame-retardant smoke suppressant, 0.5-1.5 parts of crosslinking agent and 1-3 parts of silane coupling agent.
Furthermore, the vinyl mole fraction content of the methyl vinyl silicone rubber is 0.13-0.18%.
Furthermore, the reinforcing filler is fumed silica, and dimethyl dichlorosilane is adopted for surface treatment, so that the particle size is 10-50 nm.
Further, the composite ceramic filler comprises sericite powder and silicon micropowder which are compounded according to the mass ratio of 1-2.
Further, the compound fluxing agent comprises two kinds of low-melting-point glass powder which are compounded, wherein the melting points of the two kinds of low-melting-point glass powder are respectively 500-600 ℃ and 700-800 ℃, and the two kinds of low-melting-point glass powder are compounded according to the mass ratio of 1.
Furthermore, the hollow ceramic microspheres are of thin-wall hollow structures, the chemical components of the hollow ceramic microspheres comprise silicon dioxide and aluminum oxide, the melting point of the hollow ceramic microspheres is 1600-1800 ℃, and the average particle size of the hollow ceramic microspheres isThe diameter is 60-100 mu m, and the bulk density is 0.25-0.45 g/cm 3 。
Further, the compound flame-retardant smoke suppressant comprises a platinum flame retardant and Al (OH) 3 And molybdenum oxide.
Further, the cross-linking agent is 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane or dicumyl peroxide.
Furthermore, the silane coupling agent is vinyl triethoxysilane.
The preparation method of the light low-smoke fireproof heat-insulation silicon rubber material comprises the following steps:
taking methyl vinyl silicone rubber and reinforcing filler, and uniformly mixing; adding a compounded ceramic filler, a compounded fluxing agent and a compounded flame-retardant smoke suppressant, and mixing uniformly; adding a cross-linking agent, and uniformly mixing; adding the hollow ceramic microspheres, and uniformly mixing to obtain a mixed rubber material; the roller temperature in each mixing process is not higher than 50 ℃;
naturally standing the mixed rubber material for more than 24 hours at room temperature;
pressing the parked rubber material into a semi-finished rubber sheet;
hot-pressing and vulcanizing for 15-25 min at 150-170 ℃ and 10-15 MPa to obtain a hot-pressing and vulcanizing molded product;
and (3) placing the hot-pressed vulcanized molded product at room temperature for more than 16 hours.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the silicon rubber composite material with low density and excellent fireproof and heat-insulating properties is prepared by adopting specific components and proportions, when an airplane is on fire, heat transfer is isolated, further ablation can be effectively resisted, high-temperature flame or gas in a fire area is prevented from entering other areas to cause harm, airborne equipment and personnel can be effectively protected, and the flight safety of the airplane is ensured.
2. The invention takes methyl vinyl silicone rubber as a base material, sericite powder/silicon micropowder complexing system as a ceramic filler, and glass powder with different melting points is compounded with a fluxing agent to prepare the porcelainized fireproof silicone rubber composite material with low smoke, good porcelainizing effect and excellent fireproof performance.
3. The invention greatly reduces the material proportion, reduces the heat conduction and improves the fireproof and heat-insulating properties by applying the hollow ceramic microspheres with the characteristics of light weight, high strength, wear resistance, low heat conduction, high temperature resistance, flame retardance and the like.
4. The invention uses platinum flame retardant and Al (OH) 3 The flame-retardant smoke-suppressing system compounded by molybdenum oxide greatly improves the flame-retardant performance of the material and reduces the smoke density.
Of course, not all of the advantages described above need to be achieved at the same time in practicing the various aspects of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that drawings of other embodiments can be obtained according to the drawings without creative efforts.
FIG. 1 is a photograph of a burned surface of a rubber material produced in example 1 of the present invention;
FIG. 2 is a photograph of a burned surface of the rubber material prepared in comparative example 1 of the present invention;
FIG. 3 is a photograph of a burned surface of the rubber material prepared in comparative example 2 of the present invention;
fig. 4 is a graph comparing the thermal insulation performance of example 1 of the present invention with that of comparative example 3.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully hereinafter with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
In the description of this patent, it is to be understood that the terms "center," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings for the convenience of describing the patent and for the simplicity of description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the patent.
In the description of this patent, it is noted that unless otherwise specifically stated or limited, the terms "mounted," "connected," and "disposed" are to be construed broadly and can include, for example, fixedly connected, disposed, detachably connected, disposed, or integrally connected and disposed. The specific meaning of the above terms in this patent may be understood by those of ordinary skill in the art as appropriate. The present invention will be described in detail below with reference to the accompanying drawings and examples.
A light low-smoke fireproof heat-insulation silicon rubber material comprises the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber, wherein the vinyl content of the methyl vinyl silicone rubber is 0.13-0.18%;
30-50 parts of reinforcing filler, wherein the reinforcing filler is fumed silica, and is subjected to surface treatment by using dimethyldichlorosilane, and the particle size is 10-50 nm;
40-60 parts of a ceramic filler, wherein the ceramic filler is prepared by compounding sericite powder and silicon micropowder according to the proportion of 1;
20-50 parts of a compound fluxing agent, wherein the compound fluxing agent is prepared by compounding two kinds of low-melting-point glass powder with different melting points (500-600 ℃ and 700-800 ℃) according to the proportion of 1;
30-50 parts of hollow ceramic microspheres, wherein the hollow ceramic microspheres are in a thin-wall hollow structure, mainly comprise silicon dioxide and aluminum oxide, have a melting point of 1600-1800 ℃, an average particle size of 60-100 mu m and a bulk density of 0.25-0.45 g/cm 3 ；
15-30 parts of compound flame-retardant smoke suppressant, wherein the compound flame-retardant smoke suppressant consists of a platinum flame retardant, al (OH) 3 and molybdenum oxide according to a certain proportion;
0.5-1.5 parts of cross-linking agent, wherein the cross-linking agent refers to one of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane or dicumyl peroxide;
1-3 parts of silane coupling agent, wherein the silane coupling agent is vinyl triethoxysilane (A151).
A preparation method of a light low-smoke fireproof heat-insulation silicon rubber material specifically comprises the following steps:
s1, uniformly mixing methyl vinyl silicone rubber and a reinforcing material, adding a porcelain forming filler, a fluxing agent and a flame-retardant smoke suppressant, uniformly mixing, adding a crosslinking agent, uniformly mixing, adding hollow ceramic microspheres, and uniformly mixing to obtain a mixed rubber material, wherein the roll temperature in the whole mixing process is not higher than 50 ℃;
specifically, step S1 includes the following substeps:
s101, using a double-roller open mill to adjust the roller spacing to a required value, adding methyl vinyl silicone rubber for mixing, gradually and slowly adding fumed silica, and continuously mixing for 2-3 min after the fumed silica is added and uniformly mixed visually;
step S102, sequentially adding a porcelain forming filler, a fluxing agent and a flame-retardant smoke suppressant, and continuously mixing for 2-3 min after the porcelain forming filler, the fluxing agent and the flame-retardant smoke suppressant are visually and uniformly mixed after the porcelain forming filler, the fluxing agent and the flame-retardant smoke suppressant are added;
step S103, adding a cross-linking agent 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, and mixing for 3-5 min.
Step S104: adjusting the gap between the two rollers to be larger, adding the hollow ceramic microspheres, mixing uniformly by visual inspection after the addition is finished, and then continuing to mix for 2-3 min, and discharging the slices;
s2, naturally standing the rubber material for more than 24 hours at room temperature;
s3, pressing the parked rubber material into a semi-finished rubber sheet product with a certain thickness;
s4, carrying out hot-press vulcanization for 15-25 min at the temperature of 150-170 ℃ and under the pressure of 10-15 MPa to obtain a hot-press vulcanization molded product;
and S5, placing the hot-press vulcanization molded product at room temperature for more than 16 hours to finally obtain the light low-smoke fireproof heat-insulating silicon rubber material.
The following describes in detail the embodiments of the formulation of the present invention by way of table 1:
TABLE 1 basic recipe of inventive and comparative examples
The above examples and comparative examples were subjected to multiple sets of performance tests to obtain:
(1) By adopting specific composition and proportion, the compounding and performance optimization of the fireproof silicone rubber material are carried out, the silicone rubber material with low density, low smoke toxicity and excellent fireproof and heat-insulating properties is prepared, the material can be used for preparing a fireproof sealing element of an airplane, the sealing element is subjected to a fireproof test at 1093 +/-66 ℃ for 15min according to the AC20-135 standard, and the sealing element is free from burning through and back burning.
(2) The material has excellent mechanical property, fireproof and heat-insulating properties, good rebound resilience and sealing property, and the specific gravity of the material is 1.15-1.25 g/cm 3 The tensile strength is 6.2-7.0 MPa, the elongation at break is 300-360 percent, the compression permanent deformation is 16-18 percent when the material is compressed for 70 hours at 150 ℃, and the heat flow density is not lower than 10.6W/cm at 1093 +/-66 ℃ according to the AC20-135 test standard 2 ) And then, a fire test is carried out for 15min, the sample of 6mm is not burnt through, and the temperature of the back fire surface is not higher than 200 ℃. The tensile strength and the elongation at break of the material are tested according to GB/T532, and the specific gravity is tested according to GB/T533.
(3) Through a mica powder/silicon micropowder compounded ceramic forming system and two different melting point glass powder compounded system fluxing agents, the temperature gradient design of the two fluxing agents is adopted, the ceramic conversion rate is improved, the strength of an ablated ceramic layer is enhanced, the prepared fireproof heat-insulating silicon rubber has excellent fireproof performance, a flame at 1093 +/-66 ℃ is subjected to a fireproof test for 15min, a 6mm sample is not burnt through, and the ablated ceramic layer is complete in structure. Meanwhile, the smoke density of the ceramic material prepared by compounding mica powder/silicon micropowder into a ceramic system material is obviously lower than that of the mica powder used as a ceramic filler singly when the smoke density of the ceramic material prepared by compounding the mica powder/silicon micropowder is recorded in detail in the following table 2. Referring to fig. 1, the sample is not burnt through after ablation in the embodiment 1 of the invention, no crack is generated on the fire surface, and the ceramic layer structure is complete; referring to fig. 2, comparative example 1 exhibited more cracks to the fire face after ablation; referring to fig. 3, comparative example 2 had cracks to the fire face after ablation.
TABLE 2 measurement of smoke density of fire-resistant silicone rubber
| Sample(s) | Test time, s | Maximum time, s | The maximum smoke density value of the smoke is obtained, 4 Dm |
| comparative example 5 | 240 | 240 | 116 |
| Example 1 | 240 | 240 | 85 |
(4) Referring to Table 3 below, the use of hollow ceramic microspheres in a flame-retardant silicone rubber greatly reduces the specific gravity of the material (from 1.38 g/cm) by comparison of example 1 and comparative example 3 3 The temperature is reduced to 1.17g/cm 3 ). Referring to fig. 4, the flame of 1093 ℃ ± 66 ℃ is subjected to a fire test for 15min for the example 1 and the comparative example 3, and the highest temperature of the back of the sample of the example 1 is reduced from 206 ℃ to 135 ℃, so that the fire-proof and heat-insulating properties of the material are greatly improved; at the same timeThe compatibility of the hollow ceramic microspheres and the ablated ceramic layer is good, and the ablated ceramic layer has a complete structure.
TABLE 3 specific gravity test of fire-resistant silicone rubber
| Sample(s) | Specific gravity, g/cm 3 |
| Example 1 | 1.17 |
| Comparative example 3 | 1.38 |
(5) Referring to tables 4 and 5 below, example 1 and comparative example 4 were compared by platinum flame retardant, al (OH) 3 The smoke density and the smoke toxicity of the material are greatly reduced, and the smoke density and the toxicity requirements of civil aircrafts are met. The smoke density test standard is HB6577-2014, and the smoke toxicity test standard is HB7066-2014.
Table 4 smoke density test of fire-resistant silicone rubber
| Sample(s) | Test time, s | Time of maximum value, s | The maximum smoke density value of the smoke is obtained, 4 Dm |
| comparative example 4 | 240 | 240 | 123 |
| Example 1 | 240 | 240 | 85 |
TABLE 5 Smoke toxicity test for fire-retardant silicone rubber
| Number of | CO | HCN | HF | HCl | SO 2 | NOX |
| Comparative example 4 | 113 | 12 | 3 | 3 | 0 | 15 |
| Example 1 | 83 | 9 | 0 | 3 | 0 | 4 |
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. Numerous simple deductions, modifications or substitutions may also be made by those skilled in the art in light of the present teachings.
Claims (10)
1. The light low-smoke fireproof heat-insulation silicon rubber material is characterized by comprising the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 30-50 parts of reinforcing filler, 40-60 parts of compounded porcelain filler, 20-50 parts of compounded fluxing agent, 30-50 parts of hollow ceramic microspheres, 15-30 parts of compounded flame-retardant smoke suppressant, 0.5-1.5 parts of crosslinking agent and 1-3 parts of silane coupling agent.
2. The light low-smoke fireproof heat-insulating silicon rubber material as claimed in claim 1, wherein the vinyl mole fraction content of the methyl vinyl silicone rubber is 0.13-0.18%.
3. The light low-smoke fireproof heat-insulating silicone rubber material as claimed in claim 1 or 2, wherein the reinforcing filler is fumed silica, and dimethyl dichlorosilane is used for surface treatment, and the particle size is 10nm to 50nm.
4. The light low-smoke fireproof heat-insulating silicone rubber material as claimed in claim 3, wherein the composite ceramic filler comprises sericite powder and silica micropowder in a mass ratio of 1.
5. The light low-smoke fireproof heat-insulating silicone rubber material as claimed in claim 4, wherein the compound fluxing agent comprises two low-melting-point glass powders which are compounded at the melting points of 500-600 ℃ and 700-800 ℃ respectively, according to the mass ratio of 1-2.
6. The light low-smoke fireproof heat-insulating silicon rubber material as claimed in claim 5, wherein the hollow ceramic microspheres are thin-walled hollow structures, the chemical components of the hollow ceramic microspheres comprise silicon dioxide and aluminum oxide, the melting point of the hollow ceramic microspheres is 1600-1800 ℃, the average particle size of the hollow ceramic microspheres is 60-100 μm, and the bulk density of the hollow ceramic microspheres is 0.25-0.45 g/cm 3 。
7. The light low-smoke fireproof heat-insulating silicone rubber material as claimed in claim 6, wherein the compounded flame-retardant smoke suppressant comprises platinum flame retardant, al (OH) 3 And molybdenum oxide.
8. The light low-smoke fireproof heat-insulating silicone rubber material as claimed in claim 7, wherein the cross-linking agent is 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane or dicumyl peroxide.
9. The lightweight low-smoke fire-proof heat-insulating silicon rubber material as claimed in claim 8, wherein the silane coupling agent is vinyltriethoxysilane.
10. The preparation method of the light low-smoke fireproof heat-insulation silicon rubber material is characterized by comprising the following steps of:
taking methyl vinyl silicone rubber and reinforcing filler, and uniformly mixing; adding a compounded ceramic filler, a compounded fluxing agent and a compounded flame-retardant smoke suppressant, and mixing uniformly; adding a cross-linking agent, and uniformly mixing; adding the hollow ceramic microspheres, and uniformly mixing to obtain a mixed rubber material; the roller temperature in each mixing process is not higher than 50 ℃;
naturally standing the mixed rubber material for more than 24 hours at room temperature;
pressing the parked rubber material into a semi-finished rubber sheet;
hot-pressing and vulcanizing for 15-25 min at 150-170 ℃ and 10-15 MPa to obtain a hot-pressing and vulcanizing molded product;
and (3) placing the hot-pressed vulcanized molded product at room temperature for more than 16 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232577A (en) * | 2022-08-01 | 2022-10-25 | 科建高分子材料（上海）股份有限公司 | Fireproof butyl rubber and application thereof in multilayer composite fireproof coiled material |
| CN115850977A (en) * | 2022-12-21 | 2023-03-28 | 蚌埠壹石通聚合物复合材料有限公司 | Normal-temperature heat-conducting and high-temperature flame-retardant heat-insulating silicone rubber and preparation method thereof |
| CN116218234A (en) * | 2023-04-17 | 2023-06-06 | 应急管理部四川消防研究所 | Ceramic fireproof plugging module and preparation method thereof |
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| WO2013029382A1 (en) * | 2011-08-29 | 2013-03-07 | 深圳市沃尔核材股份有限公司 | Ceramic silicon rubber and preparation method therefor |
| CN104817844A (en) * | 2015-05-19 | 2015-08-05 | 西北橡胶塑料研究设计院有限公司 | Fireproof heat-insulation silicon rubber and preparation method thereof |
| CN108943920A (en) * | 2018-05-24 | 2018-12-07 | 沪如科技南京有限公司 | A kind of high temperature resistant heat insulation rubber composite belt and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115232577A (en) * | 2022-08-01 | 2022-10-25 | 科建高分子材料（上海）股份有限公司 | Fireproof butyl rubber and application thereof in multilayer composite fireproof coiled material |
| CN115850977A (en) * | 2022-12-21 | 2023-03-28 | 蚌埠壹石通聚合物复合材料有限公司 | Normal-temperature heat-conducting and high-temperature flame-retardant heat-insulating silicone rubber and preparation method thereof |
| CN115850977B (en) * | 2022-12-21 | 2023-10-20 | 蚌埠壹石通聚合物复合材料有限公司 | Silicon rubber with normal-temperature heat conduction, high-temperature flame retardance and heat insulation and preparation method thereof |
| CN116218234A (en) * | 2023-04-17 | 2023-06-06 | 应急管理部四川消防研究所 | Ceramic fireproof plugging module and preparation method thereof |
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| CN115449225B (en) | 2023-07-25 |
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