CN115819982A - Flame-retardant ceramic liquid silicone rubber foam material and preparation method and application thereof - Google Patents
Flame-retardant ceramic liquid silicone rubber foam material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of high polymer material fire prevention, and particularly relates to a flame-retardant ceramic liquid silicone rubber foam material and a preparation method and application thereof. The flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises a foaming component and a crosslinking component, has excellent flame-retardant performance, and has the advantages of flat product surface, no cracking, no toxicity, no odor and no open fire in the combustion process, stable product high-temperature size, capability of forming a ceramic state at a low temperature and good ceramic forming effect. Compared with the traditional flame-retardant material, the flame-retardant ceramic liquid silicone rubber foam material prepared by the invention has the advantages of small combustion smoke amount, no toxicity, no harm, low production cost, simple preparation process, wide application prospect, and can be used in the fields of buildings, new energy automobiles, transportation and aerospace.
Description
Technical Field
The invention belongs to the technical field of high polymer material fire prevention, and particularly relates to a flame-retardant ceramic liquid silicone rubber foam material and a preparation method and application thereof.
Background
The silicon rubber foam has the characteristics of high resilience, sound insulation, shock absorption, heat preservation, low density, no toxic gas release in the using process and the like, and is widely applied to the fields of buildings, new energy automobiles, transportation, aerospace and the like.
Although the silicon-oxygen main chain of the silicon rubber foam substrate enables the silicon-oxygen main chain to have better high-temperature resistance than a carbon chain, pure silicon rubber foam does not have a flame-retardant effect at room temperature, and flame spread is easily caused after ignition; and it leaves only a pile of loose silica powder after high temperature ablation, and cannot continue to provide basic mechanical properties to buildings or equipment. The flame-retardant porcelainized silicon rubber foam keeps the characteristics of the silicon rubber foam at room temperature and plays a role in isolating heat transfer; and a firm ceramic body structure can be formed after high-temperature ablation, the original shape is kept to a greater extent, heat transfer is isolated, flame spread is prevented, and the high-strength mechanical property ensures that the support material is not easy to collapse.
Chinese patent CN 113831738A discloses a preparation method of flame-retardant silicone rubber foam, and the product obtained by the method has a certain flame-retardant effect, but cannot form a firm ceramic body structure after high-temperature ablation.
Chinese patent CN 115073921A discloses a preparation process of a silicon rubber foam coated with a ceramic flame-retardant coating, and the obtained silicon rubber foam has strong flame-retardant property, but the silicon rubber foam is prepared by adopting supercritical carbon dioxide, so that the production cost is high, and the silicon rubber foam is difficult to produce on a large scale.
Disclosure of Invention
The invention aims to provide a flame-retardant ceramic liquid silicone rubber foam material, and a preparation method and application thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a flame-retardant ceramic liquid silicone rubber foam material, which comprises a foaming component and a crosslinking component;
the foaming component comprises the following raw materials in parts by mass:
the crosslinking component comprises the following raw materials in parts by mass:
the mass ratio of the foaming component to the crosslinking component is 1.
Preferably, the platinum catalyst is a platinum-vinylsiloxane complex; the Pt content of the platinum-vinyl siloxane complex is 300-3000 ppm.
Preferably, the vinyl silicone oil is vinyl-terminated polydimethylsiloxane; the apparent viscosity of the vinyl silicone oil is 100-15000 mPa.s at 25 ℃; the content of vinyl groups in the vinyl silicone oil is 0.09-0.3 wt%.
Preferably, the hydroxyl silicone oil is monohydroxy silicone oil or dihydroxy silicone oil; the hydroxyl content of the hydroxyl silicone oil is 4-20 wt%.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.2-1.6 wt%.
Preferably, the flame retardant filler comprises Al (OH) 3 、Mg(OH) 2 MgO and Al 2 O 3 One or more of the above;
the ceramic filler is one or more of mica, kaolin, low-melting-point glass powder, montmorillonite and silica micropowder; the softening point temperature of the low-melting-point glass powder is 500-800 ℃.
Preferably, the white carbon black is fumed white carbon black; the specific surface area of the white carbon black is 135-440 m 2 /g。
The invention also provides a preparation method of the flame-retardant ceramic liquid silicone rubber foam material, which comprises the following steps:
mixing vinyl silicone oil, hydroxyl silicone oil, a platinum catalyst, white carbon black, a flame-retardant filler and a ceramic filler to obtain a foaming component;
mixing vinyl silicone oil, hydrogen-containing silicone oil, white carbon black, flame-retardant filler and ceramic filler to obtain a cross-linking component;
mixing the foaming component and the crosslinking component, and vulcanizing and foaming to obtain the flame-retardant ceramic liquid silicone rubber foam material;
the order of preparation of the foaming component and the crosslinking component is not required.
Preferably, the temperature of the vulcanization foaming is 50-200 ℃, and the time of the vulcanization foaming is 5-120 min.
The invention also provides application of the flame-retardant ceramic liquid silicone rubber foam material prepared by the preparation method in the scheme or in the fields of buildings, new energy automobiles, transportation and aerospace.
The invention provides a flame-retardant ceramic liquid silicone rubber foam material. The flame-retardant filler in the flame-retardant ceramic liquid silicone rubber foam material can generate a strong endothermic thermal decomposition reaction under a high temperature condition (more than 200 ℃), and a large amount of crystal water can be released in the reaction process, so that the overall temperature of a reaction system is greatly reduced; the ceramic filler in the flame-retardant ceramic liquid silicone rubber foam material is melted at a relatively low temperature, permeates into the main chain of the flame-retardant ceramic liquid silicone rubber foam material and the holes formed by the decomposition of the flame-retardant filler, and forms eutectic with silicon dioxide powder decomposed in the flame-retardant ceramic liquid silicone rubber foam material, so that the phase structure of a system is changed, and a harder ceramic body is formed. The flame-retardant ceramic liquid silicone rubber foam material provided by the invention has excellent flame-retardant performance and ceramic performance, most of the flame-retardant filler and the ceramic filler are not required to be modified, the price is low, the production cost is low, the surface of a product is flat and free of cracking after high-temperature ablation, the combustion process is nontoxic and odorless, the high-temperature size is stable, a ceramic body can be formed at a lower temperature (500-550 ℃), the three-point bending strength of the ceramic body is high, and the mechanical performance is excellent. Compared with the traditional flame-retardant material, the flame-retardant ceramic liquid silicone rubber foam material prepared by the invention has the advantages of small combustion smoke amount, high residual rate, no toxicity and no harm.
The invention also provides a preparation method of the flame-retardant ceramic liquid silicone rubber foam material. The preparation method provided by the invention has simple steps, is easy to operate and is beneficial to industrial production.
The invention also provides application of the flame-retardant ceramic liquid silicone rubber foam material prepared by the preparation method in the scheme or in the fields of buildings, new energy automobiles, transportation and aerospace. The flame-retardant ceramic liquid silicone rubber foam material provided by the invention has excellent ceramic effect and flame-retardant property, and is low in production cost and wide in application prospect.
Detailed Description
The invention provides a flame-retardant ceramic liquid silicone rubber foam material, which comprises a foaming component and a crosslinking component;
the foaming component comprises the following raw materials in parts by mass:
the crosslinking component comprises the following raw materials in parts by mass:
the mass ratio of the foaming component to the crosslinking component is 1.
Unless otherwise specified, the starting materials used in the present invention are commercially available.
The foaming component of the flame-retardant ceramic liquid silicone rubber foam material comprises 100 parts by mass of vinyl silicone oil. In the present invention, the vinyl silicone oil is preferably vinyl-terminated polydimethylsiloxane; the vinyl silicone oil preferably has an apparent viscosity at 25 ℃ of 100 to 15000 mPas, more preferably 3500 to 10000 mPas, and even more preferably 6000 to 9000 mPas; the vinyl silicone oil preferably contains 0.09 to 0.30wt% of vinyl groups, more preferably 0.09 to 0.20wt%, and still more preferably 0.10 to 0.15wt%. The main component of the flame-retardant ceramic liquid silicone rubber foam material is vinyl silicone oil.
Based on the mass parts of the vinyl silicone oil in the foaming component, the foaming component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 5-30 parts of hydroxyl silicone oil, preferably 5-15 parts, and more preferably 15-20 parts; the hydroxyl silicone oil is preferably monohydroxy silicone oil or dihydroxy silicone oil; the monohydroxy silicone oil is preferably polydimethyl monohydroxy siloxane; the hydroxyl content of the hydroxyl silicone oil is preferably 4 to 20wt%, and more preferably 5 to 15wt%; the hydroxyl group content of the monohydroxy silicone oil is preferably 5 to 13wt%, more preferably 7 to 10wt%.
Based on the mass parts of the vinyl silicone oil in the foaming component, the foaming component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 0.02-3.0 parts of platinum catalyst, preferably 0.1-2.0 parts, and more preferably 0.5-1.0 part; the platinum catalyst is preferably a platinum-vinylsiloxane complex; the content of Pt in the platinum-vinylsiloxane complex is preferably 300 to 3000ppm, more preferably 300 to 3000ppm.
Based on the mass parts of the vinyl silicone oil in the foaming component, the foaming component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 1-20 parts of white carbon black, preferably 1-16 parts, more preferably 2-10 parts, and further preferably 5-8 parts; the white carbon black is preferably fumed white carbon black; the specific surface area of the white carbon black is preferably 135-440 m 2 (ii) g, more preferably 150 to 220m 2 /g。
Based on the mass parts of the vinyl silicone oil in the foaming component, the foaming component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 10-80 parts of flame-retardant filler, preferably 10-40 parts, and more preferably 20-40 parts; the flame-retardant filler preferably comprises Al (OH) 3 、Mg(OH) 2 MgO and Al 2 O 3 More preferably Mg (OH) 2 And Al (OH) 3 Compounding flame-retardant filler. In a particular embodiment of the invention, when the flame-retardant filler is Mg (OH) 2 And Al (OH) 3 When compounded with flame retardant fillers, the Mg (OH) 2 And Al (OH) 3 The mass ratio of (b 1).
Based on the mass parts of the vinyl silicone oil in the foaming component, the foaming component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 10-80 parts of ceramic filler, preferably 10-50 parts, and more preferably 30-50 parts; the ceramic filler is preferably one or more of mica, kaolin, low-melting-point glass powder, montmorillonite and silica micropowder, and more preferably a compound ceramic filler of mica, silica micropowder and low-melting-point glass powder. In a specific embodiment of the present invention, when the ceramifying filler is a mica, silica powder and low-melting glass powder compounded ceramifying filler, the mass ratio of the mica, silica powder and low-melting glass powder is preferably 5.
The cross-linking component of the flame-retardant ceramic liquid silicone rubber foam material comprises 100 parts by mass of vinyl silicone oil; the vinyl silicone oil is preferably vinyl-terminated polydimethylsiloxane; the apparent viscosity of the vinyl silicone oil at 25 ℃ is preferably 100 to 15000 mPas, more preferably 3500 to 10000 mPas; the content of the vinyl functional group in the vinyl silicone oil is preferably 0.09 to 0.30wt%, and more preferably 0.09 to 0.20wt%.
Based on the mass part of the vinyl silicone oil in the crosslinking component, the crosslinking component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 10-30 parts of hydrogen-containing silicone oil, preferably 10-20 parts, and more preferably 15 parts; the hydrogen content of the hydrogen-containing silicone oil is preferably 0.2 to 1.6wt%, and more preferably 0.6 to 1.6wt%.
Based on the mass parts of the vinyl silicone oil in the crosslinking component, the crosslinking component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 1-20 parts of white carbon black, preferably 5-15 parts; the white carbon black is preferably fumed silica; the specific surface area of the white carbon black is preferably 135-440 m 2 (ii) g, more preferably 150 to 220m 2 (ii) in terms of/g. The surface of the untreated white carbon black has a large amount of hydroxyl groups, and the agglomeration phenomenon can be generated by directly adding the hydroxyl groups.
Based on the mass parts of the vinyl silicone oil in the crosslinking component, the crosslinking component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 1-80 parts of flame-retardant filler, preferably 10-40 parts, and more preferably 20-40 parts; the flame-retardant filler preferably comprises Al (OH) 3 、Mg(OH) 2 MgO and Al 2 O 3 More preferably Mg (OH) 2 And Al (OH) 3 Compounding flame-retardant filler. In a particular embodiment of the invention, when the flame-retardant filler is Mg (OH) 2 And Al (OH) 3 When compounded with flame retardant fillers, the Mg (OH) 2 And Al (OH) 3 Is preferably 1.
Based on the mass parts of the vinyl silicone oil in the crosslinking component, the crosslinking component of the flame-retardant ceramic liquid silicone rubber foam material provided by the invention comprises 10-80 parts of ceramic filler, preferably 10-50 parts, and more preferably 30-50 parts; the ceramic filler preferably comprises one or more of mica, kaolin, diatomite, silica micropowder and low-melting-point glass powder, and more preferably is a compound ceramic filler of mica, silica micropowder and low-melting-point glass powder; the softening point temperature of the low-melting-point glass powder is preferably 500 to 800 ℃, more preferably 600 to 700 ℃, and further preferably 750 ℃. In a specific embodiment of the present invention, when the ceramifying filler is a mica, silica powder and low-melting glass powder compounded ceramifying filler, the mass ratio of the mica, silica powder and low-melting glass powder is preferably 5.
In the present invention, the mass ratio of the foaming component to the crosslinking component is preferably 1.1 to 1, more preferably 1.
The invention also provides a preparation method of the flame-retardant ceramic liquid silicone rubber foam material, which comprises the following steps:
mixing vinyl silicone oil, hydroxyl silicone oil, a platinum catalyst, white carbon black, a flame-retardant filler and a ceramic filler to obtain a foaming component;
mixing vinyl silicone oil, hydrogen-containing silicone oil, white carbon black, flame-retardant filler and ceramic filler to obtain a crosslinking component;
mixing the foaming component and the crosslinking component, and vulcanizing and foaming to obtain the flame-retardant ceramic liquid silicone rubber foam material;
the order of preparation of the foaming component and the crosslinking component is not required.
The foaming component is obtained by mixing vinyl silicone oil, hydroxyl silicone oil, platinum catalyst, white carbon black, flame-retardant filler and ceramic filler (marked as first mixing). In the present invention, the relative degree of vacuum of the first mixing is preferably-0.2 to-0.4 MPa, more preferably-0.2 MPa, and the present invention controls the relative degree of vacuum of the first mixing within the above range, which can prevent the introduction of a large amount of bubbles due to stirring; the first mixing preferably comprises low-speed pre-stirring (denoted as first low-speed pre-stirring) and high-speed dispersing (denoted as first high-speed dispersing) which are sequentially carried out; the rotating speed of the first low-speed pre-stirring is preferably 15-30 rpm, more preferably 20-25 rpm, and the time of the first low-speed pre-stirring is preferably 5-60 min, more preferably 10-40 min; the first low-speed pre-stirring is preferably carried out in a planetary stirrer; the rotation speed of the first high-speed dispersion is preferably 500-1200 rpm, more preferably 700-1000 rpm, and the time of the first high-speed dispersion is preferably 5-50 min, more preferably 10-30 min; the first high-speed dispersion is preferably carried out in a high-speed disperser. The invention pre-stirs the mixed raw materials at low speed in a relatively vacuum environment, disperses the raw materials at high speed and can ensure the compatibility and the dispersibility between the rubber and the filler.
The crosslinking component is obtained by mixing vinyl silicone oil, hydrogen-containing silicone oil, white carbon black, flame-retardant filler and ceramic filler (marked as second mixing). In the present invention, the relative degree of vacuum of the second mixing is preferably-0.2 to-0.4 MPa, more preferably-0.2 MPa, and the present invention controls the relative degree of vacuum of the second mixing within the above range, which can prevent the introduction of a large amount of bubbles due to stirring; the second mixing preferably comprises low-speed pre-stirring (denoted as second low-speed pre-stirring) and high-speed dispersion (denoted as second high-speed dispersion) which are sequentially carried out; the rotation speed of the second low-speed pre-stirring is preferably 15-30 rpm, more preferably 20-25 rpm, and the time of the second low-speed pre-stirring is preferably 5-60 min, more preferably 10-40 min; the second low-speed pre-stirring is preferably carried out in a planetary stirrer; the rotation speed of the second high-speed dispersion is preferably 500-1200 rpm, more preferably 700-1000 rpm, and the time of the second high-speed dispersion is preferably 5-50 min, more preferably 10-30 min; the second high speed dispersion is preferably carried out in a high speed disperser. The invention pre-stirs the mixed material at low speed in a relative vacuum environment, disperses the material at high speed and can ensure the compatibility and the dispersibility between the sizing material and the filler. In the present invention, after the foaming component and the crosslinking component are prepared, it is preferably stored at room temperature.
The foaming component and the crosslinking component are mixed (marked as third mixing) and then vulcanized and foamed to obtain the flame-retardant ceramic liquid silicone rubber foam material. In the present invention, the temperature of the third mixing is preferably 0 to 40 ℃, more preferably 0 to 30 ℃; the third mixing equipment is preferably an A and B rubber mixing machine; the temperature of the vulcanization foaming is preferably 50-200 ℃, more preferably 60-180 ℃, and further preferably 80-150 ℃, and the vulcanization foaming time is preferably 5-120 min, more preferably 5-60 min, and further preferably 10-40 min; the equipment for vulcanizing foaming is preferably a tunnel furnace.
The invention also provides application of the flame-retardant ceramic liquid silicone rubber foam material prepared by the preparation method in the scheme or in the fields of buildings, new energy automobiles, transportation and aerospace.
In order to further illustrate the present invention, the following examples are given as illustrative embodiments of the present invention and should not be construed as limiting the scope of the present invention.
Example 1
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and Al (OH) 3 And a compounded ceramic filler (mica, silicon powder and low-melting-point glass powder in a mass ratio of 5Mixing for 30min, and mixing in a high-speed disperser at 500rpm for 20min to obtain foaming component;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 And a compounded ceramic filler (mica, silicon powder and low-melting glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.8, then performing calendering molding, placing in a tunnel furnace, setting the temperature at 150 ℃, and performing vulcanization foaming for 30min to obtain the flame-retardant ceramic liquid silicone rubber foam material.
Example 2
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and Al (OH) 3 、Mg(OH) 2 And compoundingThe ceramic filler (mica, silica powder and low-melting glass powder in a mass ratio of 5;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 And a compounded ceramic filler (mica, silicon powder and low-melting glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.5, then performing calendering molding, placing in a tunnel furnace, setting the temperature at 150 ℃, and performing vulcanization foaming for 30min to obtain the flame-retardant ceramic liquid silicone rubber foam material.
Example 3
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming component, the vinyl-terminated polydimethylsiloxane and the polydimethyl monohydroxy are mixedSiloxanes, platinum-vinylsiloxane complexes, fumed silica, al (OH) 3 And a compounded ceramic filler (mica, silica powder and low-melting glass powder in a mass ratio of 5;
according to the material composition of the crosslinking components, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 And a compound ceramic filler (mica, silicon powder and low-melting glass powder in a mass ratio of 5;
and (2) mixing the foaming component and the crosslinking component in a bi-component glue mixer according to the mass ratio of 1.
Example 4
The flame-retardant ceramic liquid silicone rubber foam material comprises the following foaming components in parts by weight:
the flame-retardant ceramic liquid silicone rubber foam material comprises the following crosslinking components in parts by weight:
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of foaming components, the vinyl-terminated polydimethylsiloxane, the polydimethylsiloxane monohydroxy, the platinum-vinyl siloxane complex, the fumed silica and the Al 2 O 3 And a compounded ceramic filler (mica, silica powder and low-melting glass powder in a mass ratio of 5;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and the Al 2 OH 3 And a compounded ceramic filler (mica, silica powder and low-melting glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.
Example 5
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxanePolydimethylmonohydroxysiloxane, platinum-vinylsiloxane complex, fumed silica, al (OH) 3 Placing MgO and a compound ceramic filler (mica, silicon powder and low-melting-point glass powder with the mass ratio of 5;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 Placing MgO and a compound ceramic filler (mica, silicon powder and low-melting-point glass powder with the mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.
Example 6
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and Al (OH) 3 、Al 2 O 3 And a compounded ceramic filler (mica, silica powder and low-melting glass powder in a mass ratio of 5;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 、Al 2 O 3 And a compounded ceramic filler (mica, silicon powder and low-melting-point glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.
Example 7
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and compound flame-retardant filler (Mg (OH) 2 And Al (OH) 3 ) And a compounded ceramic filler (mica, silicon powder and low-melting-point glass powder in a mass ratio of 5;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and the compound flame-retardant filler (Mg (OH) 2 And Al (OH) 3 ) And a compounded ceramic filler (mica, silicon powder and low-melting-point glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.
Example 8
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming components, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and compound flame-retardant filler (Mg (OH) 2 And Al (OH) 3 )、Al 2 O 3 And a compounded ceramic filler (mica, silica powder and low-melting glass powder in a mass ratio of 5;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and the compound flame-retardant filler (Mg (OH) 2 And Al (OH) 3 )、Al 2 O 3 And a compounded ceramic filler (mica, silicon powder and low-melting-point glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.
Example 9
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and Al (OH) 3 H300 and a compound ceramic filler (mica, silicon powder and low-melting-point glass powder in a mass ratio of 5;
according to the material composition of the crosslinking components, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 H300 and a compound ceramic filler (mica, silicon powder and low-melting-point glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.35, then performing calendering molding, placing in a tunnel furnace, setting the temperature at 120 ℃, and curing and foaming for 25min to obtain the flame-retardant ceramic liquid silicone rubber foam material.
Example 10
The foaming components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (in parts by weight):
the cross-linking components of the flame-retardant ceramic liquid silicone rubber foam material are as follows (by weight portions):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the flame-retardant ceramic liquid silicone rubber foam material in the embodiment comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and Al (OH) 3 And a compounded ceramic filler (mica, silica powder and low-melting glass powder in a mass ratio of 5;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 And a compounded ceramic filler (mica, silica powder and low-melting glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a bi-component rubber mixing machine according to the mass ratio of 1.
Comparative example 1
The foaming components of the liquid silicone rubber foam are as follows (by weight portion):
the crosslinking components of the liquid silicone rubber foam are as follows (in parts by weight):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the liquid silicone rubber foam material in the comparative example comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and Al (OH) 3 Placing in a planetary stirrer with rotation speed of 20rpm, mixing for 30min, and mixing in a high speed disperser at rotation speed of 750rpm for 10min to obtain foaming component;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 Placing in a planetary stirrer with rotation speed of 20rpm, mixing for 30min, and mixing in a high speed disperser at rotation speed of 750rpm for 10min to obtain crosslinking component;
mixing the foaming component and the crosslinking component in a two-component rubber mixing machine according to the mass ratio of 1, then performing calendering molding, placing in a tunnel furnace, setting the temperature at 100 ℃, and performing vulcanization foaming for 30min to obtain the liquid silicone rubber foam material.
Comparative example 2
The foaming components of the liquid silicone rubber foam are as follows (by weight portion):
the crosslinking components of the liquid silicone rubber foam are as follows (in parts by weight):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the liquid silicone rubber foam material in the comparative example comprises the following steps:
according to the material composition of the foaming component, putting vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and compound ceramic filler (mica, silica powder and low-melting glass powder with the mass ratio of 5;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 And a compounded ceramic filler (mica, silicon powder and low-melting-point glass powder in a mass ratio of 5;
mixing the foaming component and the crosslinking component in a two-component rubber mixing machine according to the mass ratio of 1.
Comparative example 3
The foaming components of the liquid silicone rubber foam are as follows (by weight portion):
the crosslinking components of the liquid silicone rubber foam are as follows (in parts by weight):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the liquid silicone rubber foam material in the comparative example comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and Al (OH) 3 Placing in a planetary stirrer with rotation speed of 20rpm, mixing for 30min, and mixing in a high speed disperser at rotation speed of 750rpm for 10min to obtain foaming component;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 Placing in a planetary stirrer with rotation speed of 20rpm, mixing for 30min, and mixing in a high speed disperser at rotation speed of 750rpm for 10min to obtain crosslinking component;
mixing the foaming component and the crosslinking component in a two-component rubber mixing machine according to the mass ratio of 1.
Comparative example 4
The foaming components of the liquid silicone rubber foam are as follows (by weight portion):
the crosslinking components of the liquid silicone rubber foam are as follows (in parts by weight):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the liquid silicone rubber foam material in the comparative example comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane and polydimethylmonohydroxysiloxanePlatinum-vinylsiloxane complex, fumed silica and Al (OH) 3 Placing in a planetary stirrer with rotation speed of 20rpm, mixing for 30min, and mixing in a high speed disperser at rotation speed of 750rpm for 10min to obtain foaming component;
according to the material composition of the crosslinking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil, the fumed silica and Al (OH) 3 Placing in a planetary stirrer with rotation speed of 20rpm, mixing for 30min, and mixing in a high speed disperser at rotation speed of 750rpm for 10min to obtain crosslinking component;
mixing the foaming component and the crosslinking component in a two-component rubber mixing machine according to the mass ratio of 1, then performing calendering molding, placing in a tunnel furnace, setting the temperature at 130 ℃, and curing and foaming for 30min to obtain the silicone rubber foam material.
Comparative example 5
The foaming components of the liquid silicone rubber foam are as follows (by weight portion):
the crosslinking components of the liquid silicone rubber foam are as follows (in parts by weight):
the mass ratio of the foaming component to the crosslinking component is 1.
The preparation method of the liquid silicone rubber foam material in the comparative example comprises the following steps:
according to the material composition of the foaming component, vinyl-terminated polydimethylsiloxane, polydimethylsiloxane monohydroxy, platinum-vinyl siloxane complex, fumed silica and Al (OH) 3 Placing in a planetary stirrer with rotation speed of 20rpm, mixing for 30min, and mixing in a high speed disperser at rotation speed of 750rpm for 10min to obtain foaming component;
according to the material composition of the cross-linking component, the vinyl-terminated polydimethylsiloxane, the hydrogen-containing silicone oil and the gas phase method are carried outWhite carbon black and Al (OH) 3 Placing in a planetary stirrer with rotation speed of 20rpm, mixing for 30min, and then mixing in a high-speed disperser with rotation speed of 750rpm for 10min to obtain a crosslinking component;
mixing the foaming component and the crosslinking component in a two-component rubber mixing machine according to the mass ratio of 1, then performing calendering molding, placing in a tunnel furnace, setting the temperature at 130 ℃, and curing and foaming for 30min to obtain the liquid silicone rubber foam material.
The properties of the foams prepared in examples 1 to 10 according to the invention and comparative examples 1 to 5 were tested by the following methods: the tensile strength is tested according to GB/T6344-2008; the 25% compressive strength was tested according to GB/T7757-2009; the oxygen index is determined according to the national standard GB/T2408-2009; the vertical combustion is tested according to the national standard GB/T8333-2008; the three-point bending strength is tested according to GB/T6569-2006, and the mass residual rate is as follows: placing the sample in a tube furnace for ablation, wherein the heating rate is 10 ℃/min, and taking out the sample after the temperature is 800 ℃;
mass residual ratio = final sample mass/starting sample mass;
the results are shown in Table 1.
TABLE 1 Properties of the foams prepared in examples 1 to 10 and comparative examples 1 to 5
As can be seen from Table 1, compared with example 10, in comparative example 1, only the flame retardant filler is added, the product only reaches the threshold of the flame retardant material, the residual bulk strength is too low, and a ceramic body structure cannot be formed; in the comparative example 2, only the compound ceramic filler is added, so that the product cannot provide flame retardant performance at room temperature; compared with the prior art, the flame-retardant filler and the mica powder are added in the comparative example 3, so that the product has a flame-retardant effect, but a ceramic body structure cannot be formed; compared with the prior art, the flame-retardant filler and the glass powder are added in the comparative example 4, so that the product has both flame retardant property and porcelain forming property, but has poor porcelain forming effect and basic mechanical property, and cannot meet the actual use; in comparative example 5, the flame-retardant filler and the silica powder were added, but the product had poor flame retardancy and low residual strength. It can be seen that the liquid silicone rubber foams finally prepared in comparative examples 1-5 all have significantly reduced flame retardant properties and low residual body strength. The flame-retardant ceramic liquid silicone rubber foam material prepared in the embodiments 1 to 10 of the invention has excellent basic mechanical properties; when the flame retardant effect is ensured, the product forms a ceramic state after high-temperature ablation, the ceramic forming effect is good, the ablation strength is high, the residual rate is high, and the performance requirement of the flame retardant fireproof material is met.
The embodiment shows that the flame-retardant ceramic liquid silicone rubber foam material provided by the invention has excellent comprehensive mechanical properties, excellent flame-retardant property, low production cost, good ceramic forming effect and wide application prospect in the fields of buildings, new energy automobiles, transportation, aerospace and the like, and can form a ceramic body at the same time, and the ceramic body can be formed at relatively low temperature.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (10)
1. A flame-retardant ceramic liquid silicone rubber foam material comprises a foaming component and a crosslinking component;
the foaming component comprises the following raw materials in parts by mass:
the crosslinking component comprises the following raw materials in parts by mass:
the mass ratio of the foaming component to the crosslinking component is 1.
2. The flame retardant ceramified liquid silicone rubber foam according to claim 1, wherein the platinum catalyst is a platinum-vinylsiloxane complex; the Pt content of the platinum-vinyl siloxane complex is 300-3000 ppm.
3. The flame retardant ceramified liquid silicone rubber foam according to claim 1, wherein the vinyl silicone oil is a vinyl terminated polydimethylsiloxane; the apparent viscosity of the vinyl silicone oil at 25 ℃ is 100-15000 mPa & s; the content of vinyl groups in the vinyl silicone oil is 0.09-0.3 wt%.
4. The flame-retardant ceramified liquid silicone rubber foam according to claim 1, wherein the hydroxy silicone oil is a monohydroxy silicone oil or a bishydroxy silicone oil; the hydroxyl content of the hydroxyl silicone oil is 4-20 wt%.
5. The flame-retardant ceramified liquid silicone rubber foam according to claim 1 or 3, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.2 to 1.6wt%.
6. The flame retardant ceramified liquid silicone rubber foam according to claim 1, wherein the flame retardant filler comprises Al (OH) 3 、Mg(OH) 2 MgO and Al 2 O 3 One or more of the above;
the ceramic filler is one or more of mica, kaolin, low-melting-point glass powder, montmorillonite and silica micropowder; the softening point temperature of the low-melting-point glass powder is 500-800 ℃.
7. The flame-retardant ceramized liquid silicone rubber foam material according to claim 1, wherein the white carbon black is fumed white carbon black; the specific surface area of the white carbon black is 135-440 m 2 /g。
8. A process for the preparation of a flame-retardant ceramized liquid silicone rubber foam according to any one of claims 1 to 7 comprising the steps of:
mixing vinyl silicone oil, hydroxyl silicone oil, a platinum catalyst, white carbon black, a flame-retardant filler and a ceramic filler to obtain a foaming component;
mixing vinyl silicone oil, hydrogen-containing silicone oil, white carbon black, flame-retardant filler and ceramic filler to obtain a crosslinking component;
mixing the foaming component and the crosslinking component, and vulcanizing and foaming to obtain the flame-retardant ceramic liquid silicone rubber foam material;
the order of preparation of the foaming component and the crosslinking component is not required.
9. The preparation method of claim 8, wherein the temperature of the vulcanization foaming is 50-200 ℃, and the vulcanization foaming time is 5-120 min.
10. Use of the flame-retardant ceramized liquid silicone rubber foam according to any one of claims 1 to 7 or the flame-retardant ceramized liquid silicone rubber foam obtained by the preparation method according to any one of claims 8 to 9 in the fields of construction, new energy automobiles, transportation and aerospace.
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