CN115449225B - Light low-smoke fireproof heat-insulating silicon rubber material and preparation method thereof - Google Patents
Light low-smoke fireproof heat-insulating silicon rubber material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a light low-smoke fireproof heat-insulating silicon rubber material and a preparation method thereof, wherein 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 compound ceramic filler, 20-50 parts of compound fluxing agent, 30-50 parts of hollow ceramic microbeads, 15-30 parts of compound flame-retardant smoke suppressant, 0.5-1.5 parts of cross-linking agent and 1-3 parts of silane coupling agent. According to the invention, the silicone rubber composite material with low density and excellent fireproof and heat-insulating properties is prepared by adopting specific compositions and proportions, so that when an aircraft fires, 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 aircraft 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 silicone rubber material and a preparation method thereof.
Background
The fireproof sealing material has very important application in the aviation field, is mainly used in potential ignition areas of an aircraft, comprises parts such as an engine nacelle, a hanging part, an APU cabin and the like, plays a role in fireproof sealing when the aircraft is in fire, and is important for protecting airborne personnel and equipment and improving the flight safety of the aircraft. The requisite flight control systems, engine mounts and other flight structures within a designated fire zone or in the vicinity of a fire that may be affected by the firing of the fire zone, must be manufactured from or otherwise shielded from fire resistant materials to withstand the effects of the fire as required by the CCAR-25 airworthiness provisions. According to the definition of AC 20-135: fire protection (Fireprof) refers to the impact of a material or structure for 15 minutes in a flame of 2000 DEG F.+ -.150 DEG F, which is capable of performing the function required by the design.
Related research work is also carried out in the aviation field in China, and a scientific research personnel develop a Chinese invention patent CN200910062254.5 fireproof silicon rubber composite material and a preparation method thereof, wherein the composite material is formed by compounding 4 layers of materials including a silicon rubber fireproof isolation layer, a silicon rubber flame-retardant cooling layer, a silicon rubber ablation-resistant layer and a body silicon rubber layer in a hot pressing manner, flame is sprayed at 1100+/-50 ℃ for 15min, a sample with the thickness of 8mm is not burnt through, the backfire surface temperature is lower than 400 ℃, the composite material is formed by compounding a plurality of layers of rubber materials, the molding process is complex, the fireproof function can be achieved only by reaching a higher thickness, and the application range is limited. The existing fireproof rubber material is generally added with a large amount of flame retardant filler, so that the specific gravity is large (mostly 1.4g/cm 3 Above), the smoke amount is large, the structural integrity, the heat insulation performance and the like of the burned aircraft are still to be improved, and the requirements on fire prevention, heat insulation and sealing under certain special working conditions of the aircraft are not completely met.
Disclosure of Invention
The invention provides a light low-smoke fireproof heat-insulating silicon rubber material and a preparation method thereof, which have low density, low smoke toxicity and excellent fireproof heat-insulating performance and meet the fireproof sealing requirement of an airplane. In order to achieve the above 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 compound ceramic filler, 20-50 parts of compound fluxing agent, 30-50 parts of hollow ceramic microbeads, 15-30 parts of compound flame-retardant smoke suppressant, 0.5-1.5 parts of cross-linking agent and 1-3 parts of silane coupling agent.
Further, the vinyl molar fraction content of the methyl vinyl silicone rubber is 0.13-0.18%.
Further, the reinforcing filler is fumed silica, dimethyl dichlorosilane is adopted for surface treatment, and the particle size is 10 nm-50 nm.
Further, the compounded ceramic filler comprises sericite powder and silicon micropowder according to the mass ratio of 1:1-2:1.
Further, the compound fluxing agent comprises two low-melting-point glass powders, wherein the melting points of the two low-melting-point glass powders are respectively 500-600 ℃, 700-800 ℃, and the two low-melting-point glass powders are compounded according to the mass ratio of 1:2-2:1.
Further, the hollow ceramic microbeads are of thin-wall hollow structures, the chemical components of the hollow ceramic microbeads comprise silicon dioxide and aluminum oxide, the melting point of the hollow ceramic microbeads is 1600-1800 ℃, the average particle size 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 (3) compounding molybdenum oxide.
Further, the cross-linking agent is selected from 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane or dicumyl peroxide.
Further, the silane coupling agent is vinyl triethoxysilane.
The preparation method of the light low-smoke fireproof heat-insulating silicone rubber material comprises the following steps:
taking methyl vinyl silicone rubber and reinforcing filler, and uniformly mixing; adding a compound ceramic filler, a compound fluxing agent and a compound flame-retardant smoke suppressant, and uniformly mixing; adding a cross-linking agent, and uniformly mixing; adding hollow ceramic microspheres, and uniformly mixing to obtain a mixed sizing material; the roller temperature in each mixing process is not higher than 50 ℃;
naturally standing the mixed sizing material for more than 24 hours at room temperature;
pressing the parked glue stock into a semi-finished film;
hot-press vulcanization is carried out for 15 to 25 minutes at the temperature of 150 to 170 ℃ and the pressure of 10 to 15MPa to obtain a hot-press vulcanization molding 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 silicone rubber composite material with low density and excellent fireproof and heat-insulating properties is prepared by adopting specific compositions and proportions, so that when an aircraft fires, 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 aircraft is ensured.
2. The invention uses methyl vinyl silicone rubber as a base material, and a sericite powder/silicon micropowder compound system is a porcelain-forming filler, and glass powders with different melting points are compounded with fluxing agents to prepare the porcelain-forming fireproof silicone rubber composite material with low smoke, good porcelain-forming effect and excellent fireproof performance.
3. The hollow ceramic microbeads with the characteristics of light weight, high strength, wear resistance, low heat conduction, high temperature resistance, flame retardance and the like are applied, so that the specific gravity of the material is greatly reduced, the heat conduction is reduced, and the fireproof heat insulation performance is improved.
4. The invention uses platinum flame retardant and Al (OH) 3 And the molybdenum oxide compounded flame-retardant smoke-suppressing system greatly improves the flame retardant property of the material and reduces the smoke density.
It is, of course, not necessary for all of the above advantages to be achieved simultaneously in the practice of the various aspects of the invention.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other embodiments of the drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a photograph of the fire surface of the rubber material prepared in example 1 of the present invention after ablation;
FIG. 2 is a photograph of the fire surface after ablation of the rubber material prepared in comparative example 1 of the present invention;
FIG. 3 is a photograph of the fire surface after ablation of the rubber material prepared in comparative example 2 of the present invention;
FIG. 4 is a graph showing the heat insulating properties of example 1 of the present invention and comparative example 3.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. The drawings illustrate preferred embodiments of the invention. 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 should be understood that the terms "center," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate describing the patent and simplify the description, and do not indicate or imply that the devices or elements being referred to must have a particular orientation, be configured and operated in a particular orientation, and are therefore not to be construed as limiting the patent.
In the description of this patent, it should be noted that, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "disposed" are to be construed broadly, and may be fixedly connected, disposed, detachably connected, disposed, or integrally connected, disposed, for example. The specific meaning of the terms in this patent will be understood by those of ordinary skill in the art as the case may be. The present invention will be described in detail with reference to the accompanying drawings and examples.
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, 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 dimethyl dichlorosilane is adopted for surface treatment, and the particle size is 10-50 nm;
40-60 parts of compound porcelain filler, wherein the compound porcelain filler is composed of sericite powder and silica micropowder according to the proportion of 1:1-2:1;
20-50 parts of compound fluxing agent, wherein the compound fluxing agent is formed by compounding two low-melting-point glass powders with different melting points (500-600 ℃ and 700-800 ℃) according to a ratio of 1:2-2:1;
30-50 parts of hollow ceramic microbeads which are of thin-wall hollow structure, mainly comprise silicon dioxide and aluminum oxide, have a melting point of 1600-1800 ℃, have an average particle size of 60-100 mu m and have 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 platinum flame retardant, al (OH) 3 and molybdenum oxide according to a certain proportion;
0.5 to 1.5 parts of cross-linking agent, wherein the cross-linking agent refers to one of 2, 5-dimethyl-2, 5-bis (tertiary butyl peroxy) hexane or dicumyl peroxide;
1-3 parts of a silane coupling agent, wherein the silane coupling agent is vinyltriethoxysilane (A151).
The preparation method of the light low-smoke fireproof heat-insulating silicone rubber material specifically comprises the following steps:
s1, taking methyl vinyl silicone rubber and a reinforcing material, uniformly mixing, adding a ceramic-forming filler, a fluxing agent and a flame-retardant smoke suppressant, uniformly mixing, adding a cross-linking agent, uniformly mixing, adding hollow ceramic microspheres, and uniformly mixing to obtain a mixed rubber material, wherein the roller temperature in the whole mixing process is not higher than 50 ℃;
specifically, step S1 includes the following sub-steps:
s101, adjusting the roll gap to a required value by using a double-roll mill, adding methyl vinyl silicone rubber for mixing, gradually and slowly adding fumed silica, and continuously mixing for 2-3 min after visual observation and uniform mixing are completed after the addition;
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 visual observation and uniform mixing are carried out after the porcelain-forming filler, the fluxing agent and the flame-retardant smoke suppressant are added;
step S103, adding a cross-linking agent of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, and mixing for 3-5 min.
Step S104: the gap between the two rollers is enlarged, hollow ceramic microbeads are added, and after the hollow ceramic microbeads are visually mixed uniformly after the hollow ceramic microbeads are added, the mixing is continued for 2-3 min, and the hollow ceramic microbeads are sliced;
s2, naturally standing the sizing material for more than 24 hours at room temperature;
s3, pressing the parked sizing material into a semi-finished film product with a certain thickness;
s4, hot-press vulcanization is carried out for 15 to 25 minutes at the temperature of 150 to 170 ℃ and the pressure of 10 to 15MPa, so as to obtain a hot-press vulcanization molding product;
and S5, placing the hot-pressed vulcanized molded product for more than 16 hours at room temperature, and finally obtaining the light low-smoke fireproof heat-insulating silicone rubber material.
The following details the embodiment of the proportioning scheme of the present invention through table 1:
table 1 basic formulations of inventive examples and comparative examples
The above examples and comparative examples were subjected to a plurality of performance tests to obtain:
(1) By adopting specific composition and proportion, the fireproof silicone rubber material is compounded and performance is optimized, the silicone rubber material with low density, low smoke toxicity and excellent fireproof and heat-insulating performance is prepared, the material can be used for preparing an aircraft fireproof sealing member, the sealing member is subjected to a fireproof test of 15min at 1093+/-66 ℃ according to an AC20-135 standard, and the sealing member is not burnt through and has no back combustion.
(2) The material has excellent mechanical property, fireproof and heat insulating performance, good rebound resilience and sealing performance, 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%, the compression set is 16-18% after compression for 70h at 150 ℃, and the flame (the heat flux density is not less than 10.6W/cm) at 1093+/-66 ℃ according to the AC20-135 test standard 2 ) The fire resistance test is carried out for 15min, the 6mm sample is not burnt through, and the temperature of the backfire surface is not higher than 200 ℃. The tensile strength and the elongation at break of the material were measured according to GB/T532 and the specific gravity according to GB/T533.
(3) The ceramic forming system compounded by mica powder/silica micropowder and the fluxing agent of the glass powder compounding system with two different melting points are adopted, the ceramic conversion rate of the ceramic forming system is improved, the strength of the ceramic layer after ablation is enhanced through the temperature gradient design of the two fluxing agents, the prepared fireproof heat-insulating silicone rubber has excellent fireproof performance, a fireproof test is carried out for 15min at 1093+/-66 ℃, a 6mm sample is not burnt through, and the ceramic layer after ablation has complete structure. Meanwhile, the smoke density of the invention of the embodiment 1 and the comparative example 5 is recorded in detail in the following table 2, and the smoke density of the ceramic system material compounded by mica powder/silicon micropowder is obviously lower than that of the ceramic system material compounded by using the mica powder alone. Referring to FIG. 1, the sample of the invention in example 1 is not burnt out after ablation, has no crack on fire surface, and has complete ceramic layer structure; referring to fig. 2, comparative example 1 has more cracks on the fire surface after ablation; referring to fig. 3, comparative example 2 was ablated to crack the fire surface.
TABLE 2 Smoke density test of fireproof Silicone rubber
| Sample of | Test time s | Maximum time, s | The value of the maximum smoke density is calculated, 4 Dm |
| comparative example 5 | 240 | 240 | 116 |
| Example 1 | 240 | 240 | 85 |
(4) By comparison of example 1 and comparative example 3, see Table 3 below, the use of hollow ceramic microbeads in flame-retardant silicone rubber greatly reduced the specific gravity of the material (from 1.38g/cm 3 Down to 1.17g/cm 3 ). Referring to FIG. 4, a fire test was performed for 15 minutes on flames of 1093+ -66 ℃ in example 1 and comparative example 3, and the highest temperature of the back of the sample of example 1 was reduced from 206 ℃ to 135 ℃, thus the fire-proof and heat-insulating properties of the material were greatly improved in the invention; meanwhile, the hollow ceramic microbeads have good compatibility with the ceramic layer after ablation, and the ceramic layer after ablation has complete structure.
TABLE 3 specific gravity test of fireproof Silicone rubber
| Sample of | Specific gravity, g/cm 3 |
| Example 1 | 1.17 |
| Comparative example 3 | 1.38 |
(5) See belowTables 4 and 5 compare example 1 with comparative example 4 by platinum flame retardant, al (OH) 3 The smoke density and the smoke toxicity of the material are greatly reduced, and the requirements of the smoke density and the toxicity of civil aircraft 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 of | Test time s | Maximum time, s | The value of the maximum smoke density is calculated, 4 Dm |
| comparative example 4 | 240 | 240 | 123 |
| Example 1 | 240 | 240 | 85 |
Table 5 fire-resistant silicone rubber smoke toxicity test
| Numbering device | 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 foregoing description of the invention has been presented for purposes of illustration and description, and is not intended to be limiting. Several simple deductions, modifications or substitutions may also be made by a person skilled in the art to which the invention pertains, based on the idea of the invention.
Claims (6)
1. The light low-smoke fireproof heat-insulating silicone 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 ceramic filler, 20-50 parts of compounded fluxing agent, 30-50 parts of hollow ceramic microbeads, 15-30 parts of compounded flame-retardant smoke suppressant, 0.5-1.5 parts of cross-linking agent and 1-3 parts of silane coupling agent;
the compounded ceramic filler comprises sericite powder and silicon micropowder according to the mass ratio of 1:1-2:1;
the compound fluxing agent comprises two low-melting-point glass powders, wherein the melting points of the two low-melting-point glass powders are 500-600 ℃ and 700-800 ℃ respectively, and the two low-melting-point glass powders are compounded according to the mass ratio of 1:2-2:1;
the hollow ceramic microbeads are of a thin-wall hollow structure, the chemical components of the hollow ceramic microbeads comprise silicon dioxide and aluminum oxide, the melting point of the hollow ceramic microbeads ranges from 1600 ℃ to 1800 ℃, the average particle size of the hollow ceramic microbeads ranges from 60 mu m to 100 mu m, and the stacking density of the hollow ceramic microbeads ranges from 0.25 g/cm to 0.45g/cm 3 ;
The compound flame-retardant smoke suppressant comprises a platinum flame retardant and Al (OH) 3 And (3) compounding molybdenum oxide.
2. The light low smoke, fire-resistant and heat-insulating silicone rubber material according to claim 1, wherein the vinyl molar fraction content of the methyl vinyl silicone rubber is 0.13-0.18%.
3. The light low-smoke fireproof heat-insulating silicon rubber material according to claim 1 or 2, wherein the reinforcing filler is fumed silica, and the surface treatment is carried out by adopting dimethyl dichlorosilane, and the particle size is 10-50 nm.
4. The light low smoke fireproof heat insulation silicone rubber material according to claim 3, wherein the cross-linking agent is 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane or dicumyl peroxide.
5. The light low smoke fireproof heat insulation silicone rubber material according to claim 4, wherein the silane coupling agent is vinyl triethoxysilane.
6. The light, low smoke, fire resistant and heat insulating silicone rubber material according to claim 1, wherein the method for preparing said rubber material comprises the steps of:
taking methyl vinyl silicone rubber and reinforcing filler, and uniformly mixing; adding a compound ceramic filler, a compound fluxing agent and a compound flame-retardant smoke suppressant, and uniformly mixing; adding a cross-linking agent, and uniformly mixing; adding hollow ceramic microspheres, and uniformly mixing to obtain a mixed sizing material; the roller temperature in each mixing process is not higher than 50 ℃;
naturally standing the mixed sizing material for more than 24 hours at room temperature;
pressing the parked glue stock into a semi-finished film;
hot-press vulcanization is carried out for 15 to 25 minutes at the temperature of 150 to 170 ℃ and the pressure of 10 to 15MPa to obtain a hot-press vulcanization molding product;
and (3) placing the hot-pressed vulcanized molded product at room temperature for more than 16 hours.
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| CN102964836B (en) * | 2011-08-29 | 2014-07-30 | 深圳市沃尔核材股份有限公司 | Ceramicized silicon rubber, preparation method and application |
| CN104817844B (en) * | 2015-05-19 | 2018-02-16 | 西北橡胶塑料研究设计院有限公司 | Fire-proof and thermal-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 |
| CN109082122B (en) * | 2018-06-13 | 2021-06-11 | 上海陛升新材料科技有限公司 | Normal-temperature heat conduction-high-temperature heat insulation ceramizable high polymer material and preparation method thereof |
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