CN108841180B - Water-based silicon rubber ceramizable composite material and preparation method and application thereof - Google Patents
Water-based silicon rubber ceramizable composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a water-based silicon rubber ceramizable composite material, which comprises the following raw materials: water-based nano silicon rubber, a graphene oxide/calcium oxide composite material, EVA resin, a flame retardant, vitrified powder, nano silicon dioxide and an antioxidant; the flame retardant is one or more of a nano-scale magnesium hydroxide flame retardant, a PP flame retardant, a CPE flame retardant, a fabric coating adhesive flame retardant and a water-based paint flame retardant; the ceramic powder is composed of mineral filler and one of low-melting-point glass powder, ceramic whiskers and boron compounds; the ceramic whisker is one or more of potassium titanate, zinc oxide and aluminum borate; the antioxidant is one or more of trioctyl ester, tridecyl ester, diphenylamine, dihydroquinoline and other compounds and derivatives or polymers thereof. The material has excellent performances in aging resistance, freeze-thaw resistance and the like, and has a self-cleaning function; can form inorganic hollow ceramic material, and effectively protect the internal material from being damaged by fire and high temperature.
Description
Technical Field
The invention relates to the technical field of thermal protection composite materials, in particular to a water-based silicon rubber ceramizable composite material.
Background
The porcelainized polymer matrix composite (Ceramifiable Polymers Composites) is a fireproof material which has the performance at normal temperature which is not different from that of the common composite, but can be converted into a high-temperature resistant ceramic heat-insulating layer when being burnt at high temperature, and compared with the traditional flame-retardant fireproof material, the porcelainized polymer matrix composite has the following remarkable characteristics: (1) the ceramic polymer matrix composite can be converted into a ceramic protective layer during high-temperature combustion, the ceramic layer has a compact structure and relatively objective mechanical strength, can prevent the internal polymer from continuing thermal cracking, and can prevent water vapor and combustible gas from permeating into the interior, so that the internal material is protected from being directly burned by fire, and the ceramic polymer matrix composite is an active fireproof material; (2) the ceramifiable polymer-based composite material does not need to be added with traditional flame retardants such as halogen and the like, and volatile matters generated after thermal decomposition are nontoxic and harmless CO2And H2O, thereby generating no toxic gas and toxic smoke in the case of fire and avoiding secondary damage to people caused by fire smoke.
Chinese patent CN1973019A discloses a fire-resistant ceramifying composition comprising a mineral silicate, at least one inorganic phosphate forming a liquid phase at a temperature not exceeding 800 ℃, a polymer-based composition comprising at least 50% by weight of an organic polymer. The fireproof ceramic composition is used for manufacturing fire-resistant cables, polyurethane foams and the like. The disadvantage of this patent is that the resulting ceramic is of poor strength and requires high temperatures for ceramic formation. Chinese patent CN1320556C discloses a fire resistant cable comprising at least one conductor and at least one fire resistant coating, wherein the fire resistant coating comprises at least one organic polymer having a burning temperature in the range between a minimum temperature T1 and a maximum temperature T2; chinese patent No. 101404189B discloses a fast ceramic fire-resistant cable material and its preparation method, wherein the cable material is prepared by blending and extruding ethylene-vinyl acetate copolymer EVA, linear low-density polyethylene LLDPE, ceramic-forming filler, fire retardant, antioxidant, lubricant and coupling agent, and the cable material can be vitrified within 10 minutes at 750 ℃ and higher, and the porcelainizing material can ensure the normal operation of the line at 950 ℃ for more than 90 minutes, the disadvantage of the patent is the poor strength of the formed ceramic, the porcelain forming requires high temperature, and the mechanical property of the cable material is poor. Chinese patent CN104650441A discloses a flame-retardant polymer composite material capable of being ceramized based on polyolefin or based on thermoplastic polyurethane elastomer, which comprises the following components in parts by weight: 30-40 parts of polyolefin resin or thermoplastic polyurethane elastomer, 25-45 parts of porcelain forming filler, 20-30 parts of halogen-free flame retardant, 1-5 parts of synergistic flame retardant, 1-3 parts of plasticizer, 0.5-2 parts of antioxidant and 0.02-0.15 part of cross-linking agent, wherein the porcelain forming filler comprises low-softening-point glass powder and silicate mineral filler. This patent suffers from the following disadvantages: the addition of a large amount of porcelain forming filler leads to the remarkable reduction of the tensile strength, the tearing strength and the elongation at break of the composite material, and can not meet the mechanical property requirements of cables and optical cables on insulating or sheathing materials. The composite material disclosed by the patent can generate large toxic smoke during combustion, and is extremely not beneficial to escape of people in case of fire; when the polyolefin elastomer is burnt, a large amount of toxic smoke is released, so that people are hindered from escaping or poisoned and died directly.
The existing insulation and sheath materials for cables and optical cables only have a flame retardant function, and a few materials have low smoke characteristics. Insulating and sheathing materials for ceramifiable cables and optical cables have also become a hot point of research and development. However, materials which have flame retardant, low smoke and ceramic functions and can comprehensively overcome the negative influence on escape of people caused by burning of cables and optical cables have not been provided, and reports are rarely made. Therefore, the development of a composite material integrating heat resistance, flame retardance, low smoke and ceramic functions is urgently needed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a water-based silicon rubber ceramizable composite material and a preparation method and application thereof. By adding the water-based nano silicon rubber and the graphene oxide/calcium oxide composite material, the porcelainized composite material has excellent performances in the aspects of aging resistance, freeze thawing resistance and the like, has a self-cleaning function, can form an inorganic hollow ceramic material, and has the advantages of insulation, heat insulation, fire insulation, water resistance, earthquake resistance, small thermal weight loss and the like.
The invention provides a water-based silicon rubber ceramizable composite material which comprises the following raw materials in parts by weight: 60-80 parts of water-based nano silicon rubber, 0.1-5 parts of graphene oxide/calcium oxide composite material, 15-20 parts of EVA resin, 5-10 parts of flame retardant, 20-40 parts of vitrified powder, 1-5 parts of nano silicon dioxide and 1-5 parts of antioxidant; the flame retardant is one or more of a nano-scale magnesium hydroxide flame retardant, a high-purity industrial-grade modified magnesium hydroxide flame retardant, a magnesium hydroxide composite flame retardant, an aluminum hydroxide flame retardant, a modified aluminum hydroxide flame retardant, light magnesium oxide, an unsaturated resin flame retardant, a silicone rubber flame retardant, a polyamide flame retardant, a PE flame retardant, a PP flame retardant, a CPE flame retardant, a fabric coating glue flame retardant, a water-based paint flame retardant and an oil-based paint flame retardant; the ceramic powder is composed of mineral filler and one or more of low-melting-point glass powder, ceramic whiskers, alumina-silicon composite nanotubes and boron compounds, and the ceramic whiskers are one or more of potassium titanate, zinc oxide and aluminum borate; the antioxidant is one or more of compounds such as trioctyl ester, tridecyl ester, tridodecyl alcohol ester, trihexadecyl alcohol ester, 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) thioether, tetra [ beta- (3, 5-tertiary butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, didodecyl alcohol ester, ditetradecyl alcohol ester, dioctadecyl alcohol ester, diphenylamine, p-phenylenediamine, dihydroquinoline and derivatives or polymers thereof.
As a further improvement of the invention, the preparation method of the water-based nano silicone rubber comprises the following steps: dissolving vinyl silicone rubber in a diluent, stirring and reacting for 5-7h at 70 ℃, cooling to 45 ℃, removing the solvent by evaporation under reduced pressure, adding a compound emulsifier and distilled water, continuing to react for 2-3h, adjusting the HLB value, neutralizing with glacial acetic acid, and adding an organic silicone rubber curing agent for curing at 80-100 ℃ to obtain the water-based nano silicone rubber.
As a further development of the invention, the diluent is a solvent containing C ═ C functional groups.
As a further improvement of the invention, the organic silicon rubber curing agent is a peroxy initiator.
As a further improvement of the invention, the compound emulsifier is a compound of a cationic emulsifier and a nonionic emulsifier, wherein the cationic emulsifier is an alkyl quaternary ammonium salt emulsifier.
As a further improvement of the invention, the HLB value is adjusted to 11-15.
As a further improvement of the invention, the preparation method of the graphene oxide/calcium oxide composite material comprises the following steps: dissolving graphene oxide and calcium hydroxide in water, adding a coupling agent, stirring and reacting for 5-7h at 80 ℃ in a nitrogen atmosphere, stopping the reaction, dissolving with distilled water, recrystallizing with acetone-petroleum ether, separating out a precipitate, filtering, collecting the precipitate, and drying to obtain the graphene oxide/calcium oxide composite material.
As a further improvement of the invention, the volume ratio of the acetone to the petroleum ether is 1 (3-5).
As a further improvement of the invention, the preparation method comprises the following steps:
(1) drying the ceramic powder, the flame retardant, the nano silicon dioxide and the antioxidant in an oven at 60 ℃ for 5-10 h;
(2) uniformly mixing water-based nano silicon rubber emulsion, a graphene oxide/calcium oxide composite material, EVA resin, vitrified powder, a flame retardant, nano silicon dioxide and an antioxidant in a double roller;
(3) adding silicone oil into the double-roller to be mixed uniformly;
(4) granulating the mixed materials at 220 ℃ and 12Mpa, cold cutting, and drying at 70-80 ℃ for 1-2h to obtain the product.
The invention further protects the application of the water-based silicone rubber ceramifiable composite material in flame-retardant wires, cables and optical cables.
The invention has the following beneficial effects:
1. the material has excellent performances in aging resistance, freeze-thaw resistance and the like, and has a self-cleaning function;
2. when the material is subjected to flameless high temperature of more than 300 ℃ and flame ablation of more than 500 ℃, the material can be converted into an inorganic hollow ceramic material, and the formed special ceramic material has the advantages of insulation, heat insulation, fire insulation, water isolation, shock resistance, small thermal weight loss and the like, and can effectively protect the internal material from being damaged by big fire and high temperature.
Drawings
Fig. 1 is a preparation process diagram of water-based nano silicone rubber.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the embodiments described are only some representative embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Example 1 preparation of Water-based Silicone rubber ceramifiable composite
The raw materials comprise: 60 parts of water-based nano silicon rubber, 0.1 part of graphene oxide/calcium oxide composite material, 15 parts of EVA resin, 5 parts of nano magnesium hydroxide flame retardant, 10 parts of low-melting-point glass powder, 5 parts of ceramic whisker, 5 parts of mineral filler, 1 part of nano silicon dioxide, 1 part of tri (dodecyl) ester and tri (hexadecyl) ester;
preparation of water-based nano silicone rubber: dissolving vinyl silicone rubber in n-octene, stirring at 70 ℃ for 5h, cooling to 45 ℃, removing the solvent by evaporation under reduced pressure, adding a compound emulsifier and distilled water, continuing to react for 2h, adjusting the HLB value to 11, neutralizing with glacial acetic acid, adding a benzoyl peroxide curing agent, and curing at 80 ℃ to obtain water-based nano silicone rubber with the yield of 77%;
preparing a graphene oxide/calcium oxide composite material: dissolving graphene oxide and calcium hydroxide in water, adding a coupling agent, stirring and reacting for 5 hours at 80 ℃ in a nitrogen atmosphere, stopping the reaction, dissolving the mixture in distilled water, recrystallizing the mixture with acetone-petroleum ether (volume ratio is 1:3), separating out a precipitate, filtering, collecting the precipitate, and drying to obtain a graphene oxide/calcium oxide composite material, wherein the yield is 72%;
preparation of the water-based silicone rubber ceramizable composite material:
(1) drying low-melting-point glass powder, ceramic whiskers, mineral fillers, a nano-scale magnesium hydroxide flame retardant, nano-silica, tridodecyl alcohol ester and trihexadecyl alcohol ester in an oven at 60 ℃ for 5 hours;
(2) uniformly mixing water-based nano silicon rubber emulsion, a graphene oxide/calcium oxide composite material, EVA resin, low-melting-point glass powder, ceramic whiskers, a mineral filler, a nano magnesium hydroxide flame retardant, nano silicon dioxide, tri (dodecyl) ester, tri (hexadecyl) ester and nano silicon dioxide in double rollers;
(3) adding silicone oil into the double-roller to be mixed uniformly;
(4) the mixed materials are granulated and cold cut at 220 ℃ and 12Mpa, and then dried for 1h at 70 ℃ to obtain the product with the yield of 79 percent.
EXAMPLE 2 preparation of Water-based Silicone rubber ceramifiable composite
The raw materials comprise: 80 parts of water-based nano silicon rubber, 5 parts of graphene oxide/calcium oxide composite material, 20 parts of EVA resin, 10 parts of unsaturated resin flame retardant, 10 parts of alumina-silicon composite nanotube, 20 parts of boron compound, 10 parts of mineral filler, 5 parts of nano silicon dioxide and 5 parts of 2, 6-tertiary butyl-4-methylphenol;
preparation of water-based nano silicone rubber: dissolving vinyl silicone rubber in isooctene, stirring at 70 ℃ for 7h, cooling to 45 ℃, removing the solvent by evaporation under reduced pressure, adding a compound emulsifier and distilled water, continuing to react for 3h, adjusting the HLB value to 15, neutralizing with glacial acetic acid, adding a benzoyl peroxide curing agent, and curing at 100 ℃ to obtain water-based nano silicone rubber with the yield of 82%;
preparing a graphene oxide/calcium oxide composite material: dissolving graphene oxide and calcium hydroxide in water, adding a coupling agent, stirring and reacting for 7 hours at 80 ℃ in a nitrogen atmosphere, stopping the reaction, dissolving the mixture in distilled water, recrystallizing the mixture with acetone-petroleum ether (volume ratio is 1:5), separating out a precipitate, filtering, collecting the precipitate, and drying to obtain a graphene oxide/calcium oxide composite material, wherein the yield is 80%;
preparation of the water-based silicone rubber ceramizable composite material:
(1) drying unsaturated resin flame retardant, alumina-silicon composite nanotube, boron compound, mineral filler, nano-silica and 2, 6-tertiary butyl-4-methylphenol in an oven at 60 ℃ for 10 hours;
(2) uniformly mixing water-based nano silicon rubber emulsion, a graphene oxide/calcium oxide composite material, EVA resin, an unsaturated resin flame retardant, an alumina-silicon composite nanotube, a boron compound, a mineral filler, nano silicon dioxide, 2, 6-tertiary butyl-4-methylphenol and nano silicon dioxide in a double-roller;
(3) adding silicone oil into the double-roller to be mixed uniformly;
(4) the mixed materials are granulated and cold cut at 220 ℃ and 12Mpa, and then dried for 2h at 80 ℃ to obtain the product, wherein the yield is 85%.
EXAMPLE 3 preparation of Water-based Silicone rubber ceramifiable composite
The raw materials comprise: 70 parts of water-based nano silicon rubber, 3 parts of graphene oxide/calcium oxide composite material, 17 parts of EVA resin, 7 parts of PP flame retardant, 5 parts of low-melting-point glass powder, 15 parts of alumina-silicon composite nanotube, 10 parts of mineral filler, 3 parts of nano silicon dioxide, 1 part of bistetradecanol ester and bistearyl alcohol ester and 1 part of diphenylamine;
preparation of water-based nano silicone rubber: dissolving vinyl silicone rubber in n-undecylene, stirring at 70 ℃ for 6 hours, cooling to 45 ℃, removing the solvent by evaporation under reduced pressure, adding a compound emulsifier and distilled water, continuing to react for 2.5 hours, adjusting the HLB value to 13, neutralizing with glacial acetic acid, adding a benzoyl peroxide curing agent, and curing at 80 ℃ to obtain the water-based nano silicone rubber, wherein the yield is 89%;
preparing a graphene oxide/calcium oxide composite material: dissolving graphene oxide and calcium hydroxide in water, adding a coupling agent, stirring and reacting for 6 hours at 80 ℃ in a nitrogen atmosphere, stopping the reaction, dissolving the mixture in distilled water, recrystallizing the mixture with acetone-petroleum ether (volume ratio is 1:4), separating out a precipitate, filtering, collecting the precipitate, and drying to obtain a graphene oxide/calcium oxide composite material, wherein the yield is 92%;
preparation of the water-based silicone rubber ceramizable composite material:
(1) drying PP flame retardant, low-melting-point glass powder, alumina-silicon composite nanotubes, mineral filler, nano-silica, bistetradecanol ester, bistearyl alcohol ester and diphenylamine in an oven at 60 ℃ for 8 hours;
(2) uniformly mixing water-based nano silicon rubber emulsion, a graphene oxide/calcium oxide composite material, EVA (ethylene vinyl acetate) resin, a PP (polypropylene) flame retardant, low-melting-point glass powder, an alumina-silicon composite nanotube, a mineral filler, nano silicon dioxide, ditetradecanol ester and dioctadecyl ester, diphenylamine and nano silicon dioxide in a double rod;
(3) adding silicone oil into the double-roller to be mixed uniformly;
(4) the mixed materials are granulated and cold cut at 220 ℃ and 12Mpa, and then dried for 1.5h at 75 ℃ to obtain the product, wherein the yield is 90%.
Comparative example 1 patent ZL 201210145780.X "ceramifiable carbon-based Polymer composite and Process for its preparation"
(1) Soaking 30 parts of high silica glass fiber, 20 parts of potassium feldspar powder, 20 parts of diatomite and 2 parts of boron nitride ceramic powder into 2 parts of high-temperature coupling agent M302 for 30 minutes, and then preserving heat for 3 hours in an oven at 80 ℃; the particle size of the feldspar powder is 800-1000 meshes, the particle size of the diatomite is 800-1000 meshes, and the particle size of the boron nitride ceramic powder is 800-1000 meshes;
(2) dissolving 100 parts of barium phenolic resin by using absolute ethyl alcohol, adding the feldspar powder, the diatomite and the boron nitride ceramic powder which are obtained in the step (1) and treated by the coupling agent, and uniformly stirring to prepare a gum dipping solution; then soaking the high silica glass fiber into the dipping solution to prepare a pre-dipping cloth;
(3) after the presoaked cloth is dried, cutting, placing on a hot press, and press-molding at 200 deg.C and 1.5Mpa for 4h to obtain the ceramic carbon-based polymer composite material.
Test example 1 general preparation test
The results are shown in Table 1.
As can be seen from the table above, the aging resistance, stain resistance, heat conductivity and the like of the water-based silicone rubber ceramifiable composite material prepared by the embodiment of the invention are obviously superior to those of the ceramifiable carbon-based polymer composite material prepared by the comparative example.
Claims (1)
1. The water-based silicone rubber ceramizable composite material is characterized by comprising the following raw materials in parts by weight: 60-80 parts of water-based nano silicon rubber, 0.1-5 parts of graphene oxide/calcium oxide composite material, 15-20 parts of EVA resin, 5-10 parts of flame retardant, 20-40 parts of vitrified powder, 1-5 parts of nano silicon dioxide and 1-5 parts of antioxidant; the flame retardant is one or more of a nano-scale magnesium hydroxide flame retardant, a high-purity industrial-grade modified magnesium hydroxide flame retardant, a magnesium hydroxide composite flame retardant, an aluminum hydroxide flame retardant, a modified aluminum hydroxide flame retardant, light magnesium oxide, an unsaturated resin flame retardant, a silicone rubber flame retardant, a polyamide flame retardant, a PE flame retardant, a PP flame retardant, a CPE flame retardant, a fabric coating glue flame retardant, a water-based paint flame retardant and an oil-based paint flame retardant; the ceramic powder is composed of mineral filler and one or more of low-melting-point glass powder, ceramic whiskers, alumina-silicon composite nanotubes and boron compounds, and the ceramic whiskers are one or more of potassium titanate, zinc oxide and aluminum borate; the antioxidant is one or more of trioctyl ester, tridecyl ester, tridodecyl alcohol, trihexadecyl alcohol, 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) thioether, tetra [ beta- (3, 5-tertiary butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, didodecyl alcohol ester, ditetradecyl alcohol ester, dioctadecyl alcohol ester, diphenylamine, p-phenylenediamine and dihydroquinoline; the preparation method of the water-based nano silicone rubber comprises the following steps: dissolving vinyl silicone rubber in a diluent, stirring and reacting for 5-7h at 70 ℃, cooling to 45 ℃, removing the solvent by evaporation under reduced pressure, adding a compound emulsifier and distilled water, continuing to react for 2-3h, adjusting the HLB value, neutralizing with glacial acetic acid, and adding an organic silicone rubber curing agent for curing at 80-100 ℃ to obtain water-based nano silicone rubber; the diluent is a solvent containing C = C functional groups; the organic silicon rubber curing agent is a peroxy initiator; the compound emulsifier is formed by compounding a cationic emulsifier and a nonionic emulsifier, wherein the cationic emulsifier is an alkyl quaternary ammonium salt emulsifier; the HLB value is adjusted to 11-15; the preparation method of the graphene oxide/calcium oxide composite material comprises the following steps: dissolving graphene oxide and calcium hydroxide in water, adding a coupling agent, stirring and reacting for 5-7h at 80 ℃ in a nitrogen atmosphere, stopping the reaction, dissolving with distilled water, recrystallizing with acetone-petroleum ether, separating out a precipitate, filtering, collecting the precipitate, and drying to obtain a graphene oxide/calcium oxide composite material; the volume ratio of the acetone to the petroleum ether is 1 (3-5); the water-based silicon rubber ceramizable composite material is prepared by the following method:
(1) drying the ceramic powder, the flame retardant, the nano silicon dioxide and the antioxidant in an oven at 60 ℃ for 5-10 h;
(2) uniformly mixing water-based nano silicon rubber emulsion, a graphene oxide/calcium oxide composite material, EVA resin, vitrified powder, a flame retardant, nano silicon dioxide and an antioxidant in a double roller;
(3) adding silicone oil into the double-roller to be mixed uniformly;
(4) granulating and cold cutting the mixed materials at 220 ℃ and 12Mpa, and drying at 70-80 ℃ for 1-2h to obtain a product; the water-based silicone rubber ceramifiable composite material is applied to flame-retardant wires, cables and optical cables.
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