CN110317421B - Fireproof sealing material and preparation method thereof - Google Patents
Fireproof sealing material and preparation method thereof Download PDFInfo
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- CN110317421B CN110317421B CN201910633231.9A CN201910633231A CN110317421B CN 110317421 B CN110317421 B CN 110317421B CN 201910633231 A CN201910633231 A CN 201910633231A CN 110317421 B CN110317421 B CN 110317421B
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Abstract
The invention belongs to the technical field and provides a novel fireproof sealing material and a preparation method thereof. A novel fireproof sealing material comprises the following components in parts by weight: 20-50 parts of resin, 3-10 parts of carbon black, 5-75 parts of expanded graphite, 0.2-3 parts of nano antimony trioxide, 0.5-15 parts of brominated flame retardant, 0.2-7 parts of phosphorus flame retardant, 0.05-5 parts of dicumyl peroxide, 1-10 parts of compatilizer, 0.5-7 parts of synergist, 0.01-40 parts of plasticizer, 0.02-3 parts of lubricant, 2-10 parts of stabilizer, 0.1-2 parts of antioxidant, 0.1-1 part of silane coupling agent and 0.5-5 parts of inorganic hydroxide flame retardant. Through the technical scheme, the problem that the fireproof sealing material in the prior art is low in fireproof and flame-retardant performance is solved.
Description
Technical Field
The invention belongs to the technical field of fireproof sealing materials, and relates to a fireproof sealing material and a preparation method thereof.
Background
During the construction of a building, a large number of building pipelines, such as air-conditioning pipelines, smoke-exhaust-preventing pipelines, water supply and drainage pipelines, heating and power pipelines, ventilating pipelines, gas pipelines, oil pipes and other process pipelines, transversely penetrate between a floor slab and bodies. The pipelines pass through holes formed in walls and floors, or gaps between floors and walls and between walls are all paths for fire propagation. In addition, some gaps are reserved for ensuring the normal use of fire doors, fire windows, fire valves and fire-proof rolling shutters in buildings. Without effective blocking of these holes or gaps, in the event of a fire, these holes or gaps would create a smoky effect and a difference in fire pressure across the holes or gaps, causing the fire to spread gradually in adjacent rooms, compromising the life and property of other fire zones.
At present, the fireproof sealing material is generally adopted at home and abroad to block openings or holes formed when various penetrations penetrate through walls or floors, the volume of the fireproof sealing material expands firstly and then hardens under the action of high temperature and flame to form a hard microporous fire-retardant carbon layer, the heat-insulating layer has good heat-insulating property and plays roles in fire-retardant smoke blocking and heat insulation, and meanwhile, the expanded fire-retardant carbon layer can completely fill the holes left after the ablation of combustible materials such as cable insulating skins and the like, so that the fireproof plugging is thoroughly and effectively achieved.
The existing fireproof sealing material has poor flame retardant effect and uneven raw material mixing, so that the material has low structural stability and poor fireproof flame retardance.
Disclosure of Invention
The invention provides a novel fireproof sealing material and a preparation method thereof, and solves the problem that the fireproof sealing material in the prior art is low in fireproof and flame-retardant properties.
The technical scheme of the invention is realized as follows:
a novel fireproof sealing material comprises the following components in parts by weight:
20-50 parts of resin, 3-10 parts of carbon black, 5-75 parts of expanded graphite, 0.2-3 parts of nano antimony trioxide, 0.5-15 parts of brominated flame retardant, 0.2-7 parts of phosphorus flame retardant, 0.05-5 parts of dicumyl peroxide, 1-10 parts of compatilizer, 0.5-7 parts of synergist, 0.01-40 parts of plasticizer, 0.02-3 parts of lubricant, 2-10 parts of stabilizer, 0.1-2 parts of antioxidant, 0.1-1 part of silane coupling agent and 0.5-5 parts of inorganic hydroxide flame retardant.
As a further technical scheme, the paint comprises the following components in parts by weight:
25-40 parts of resin, 5-8 parts of carbon black, 15-55 parts of expanded graphite, 0.5-2 parts of nano antimony trioxide, 5-13 parts of brominated flame retardant, 1.5-3.5 parts of phosphorus flame retardant, 1-2 parts of dicumyl peroxide, 2-5 parts of compatilizer, 1-5 parts of synergist, 0.05-20 parts of plasticizer, 0.5-2 parts of lubricant, 2.5-8 parts of stabilizer, 0.1-0.5 part of antioxidant, 0.2-0.5 part of silane coupling agent and 1-3.5 parts of inorganic hydroxide flame retardant.
As a further technical scheme, the paint comprises the following components in parts by weight:
33 parts of resin, 6 parts of carbon black, 30 parts of expanded graphite, 1.5 parts of nano antimony trioxide, 9 parts of brominated flame retardant, 2.5 parts of phosphorus flame retardant, 1.5 parts of dicumyl peroxide, 3 parts of compatilizer, 2 parts of synergist, 10 parts of plasticizer, 1.2 parts of lubricant, 5 parts of stabilizer, 0.3 part of antioxidant, 0.3 part of silane coupling agent and 2.5 parts of inorganic hydroxide flame retardant.
According to a further technical scheme, the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine, wherein the mass ratio of the sulfydryl chitosan to the sulfydryl graphene to the polyethyleneimine is 3:5: 2.
As a further technical scheme, the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8.
As a further technical scheme, the resin is one or more of polyvinyl chloride resin, ethylene-vinyl acetate copolymer resin, polyethylene resin, polystyrene resin, styrene-acrylonitrile resin, acrylonitrile-butadiene-styrene resin, styrene-maleic anhydride copolymer resin, acrylonitrile-styrene-acrylate copolymer resin, methacrylate-butadiene-styrene resin, methyl methacrylate-acrylonitrile-butadiene-styrene resin and polyphenyl ether resin.
As a further technical scheme, the carbon black is conductive nano carbon black with the particle size of 15nm, the particle size of the expanded graphite is 30-100 meshes, and the particle size of the nano antimony trioxide is 24-35nm and a specific surface area of 54-90 m2/g。
As a further technical scheme, the bromine flame retardant is one or more of hexabromocyclododecane, tetrabromobisphenol A, tetrabromobisphenol allyl ether and decabromodiphenyl ether, the phosphorus flame retardant is one or more of triphenyl phosphate, cresyldiphenyl phosphate, diphenyl isopropyl phenyl phosphate, tricresyl phosphate, trixylenyl phosphate and resorcinol bis (diphenyl phosphate), and the inorganic hydroxide flame retardant is aluminum hydroxide and/or magnesium hydroxide.
As a further technical scheme, the plasticizer is mineral oil or dioctyl phthalate, the lubricant is low-molecular polyethylene wax, the stabilizer is a calcium-zinc stabilizer, the silane coupling agent is gamma-aminopropyl triethoxysilane or 3-aminopropyl triethoxysilane, and the antioxidant is antioxidant 1010 or antioxidant 168.
A preparation method of a novel fireproof sealing material comprises the following steps:
s1, weighing the components according to the formula of the novel fireproof sealing material for later use;
s2, heating and melting the resin, adding the plasticizer, the lubricant, the stabilizer, the antioxidant and the silane coupling agent, and uniformly mixing to obtain a first component;
s3, uniformly mixing carbon black, expanded graphite, nano antimony trioxide, diisotoluene peroxide brominated flame retardant, phosphorus flame retardant and inorganic hydroxide flame retardant to obtain a second component;
s4, mixing the first component obtained in the step S2 and the second component obtained in the step S3, adding a compatilizer and a synergist, and uniformly mixing to obtain a mixed material;
and S5, calendering and molding the mixed material obtained in the step S4, and cooling to obtain the novel fireproof sealing material.
The working principle and the beneficial effects of the invention are as follows:
1. in the invention, the resin is adopted as a raw material, is matched with other components in the formula and is compatible with each other, so that the prepared fireproof sealing material has good fireproof heat-insulating property, fireproof and smoke-proof properties, the limit oxygen index is up to 52.8, the flame-retardant grade is up to V-0 grade, the fire-retardant limit is up to 4h, the smoke-proof time is up to 80min, and the fireproof sealing material has good expansion performance, can not automatically combust when being used for a fireproof door, a fireproof window and a fireproof separation member, can automatically expand to fill gaps at the sealing parts of the fireproof door, the fireproof window, the fireproof separation member and the like, can block the air circulation of two spaces, effectively prevents the harm of thick smoke, toxic gas and hot gas at the early stage of fire to human bodies in the smoke-proof time, plays a good role of preventing the penetration of flame and smoke, effectively controls the spread of fire, and prevents the expansion of the disaster, the safety performance of the fireproof door, the fireproof window, the fireproof separating member and the like is improved, and the fireproof door is suitable for popularization and use.
2. According to the invention, a bromine flame retardant, a phosphorus flame retardant and an inorganic hydroxide flame retardant are matched with each other, so that the prepared fireproof sealing material has good flame retardant performance, the addition of the nano antimony trioxide and the dicumyl peroxide plays a role in flame retardant synergism, the flame retardant performance of the fireproof sealing material is further improved, the flame retardant grade of the prepared fireproof sealing material reaches V-0 level through compounding of various components, the addition of the silane coupling agent couples the resin with carbon black, expanded graphite, mercaptographene, aminopropyl isobutyl silsesquioxane, hollow glass microspheres and the like to form a stable crosslinking system, the melting point of the resin is improved, and the fireproof and smoke-proof performance of the fireproof sealing material is further improved. In the preparation process of the fireproof sealing material, the phosphorus flame retardant is matched with the plasticizer, so that the adhesion effect of the resin and other components in the formula is improved, and the processing performance of the fireproof sealing material is improved.
3. According to the invention, the compatibility and the dispersibility of the resin and other components in the formula are increased by adding the compatilizer, so that the components in the formula are mixed more uniformly, the stability of the fireproof sealing material is improved, the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine, the mass ratio of the sulfydryl chitosan to the sulfydryl graphene is 3:5:2, a disulfide bond is formed by matching the sulfydryl chitosan and the sulfydryl graphene, the disulfide bond is combined with a resin matrix, the melting point of the resin is improved, the space structure of a mixed system is stabilized, the structure of the fireproof sealing material is more stable, the polyethyleneimine is matched with the sulfydryl chitosan, the binding power of the mixed system is improved, the components in the formula are combined more stably, and the thermal stability and the durability of the sealing material are further improved.
4. In the invention, the synergist is added, so that the fireproof and heat-insulating properties and the fireproof and smoke-proof properties of the fireproof sealing material are improved. The synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1:8, the aminopropyl isobutyl silsesquioxane is introduced into a resin system in a way that organic active group amino in a molecular structure of the aminopropyl isobutyl silsesquioxane reacts with reactive sulfydryl, olefin and the like in a formula, so that the prepared fireproof sealing material has good thermal stability and high flame retardance, and silicon dioxide formed after the aminopropyl isobutyl silsesquioxane is heated and decomposed reacts with the hollow glass microspheres to form a porous hard ceramic substance, so that heat is isolated, and the fireproof and heat-insulating properties of the fireproof sealing material are further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
20 parts of resin, 3 parts of carbon black, 5 parts of expanded graphite, 0.2 part of nano antimony trioxide, 0.5 part of brominated flame retardant, 0.2 part of phosphorus flame retardant, 0.05 part of dicumyl peroxide, 1 part of compatilizer, 0.5 part of synergist, 0.01 part of plasticizer, 0.02 part of lubricant, 2 parts of stabilizer, 0.1 part of antioxidant, 0.1 part of silane coupling agent and 0.5 part of inorganic hydroxide flame retardant,
wherein the resin is polyvinyl chloride resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the brominated flame retardant is hexabromocyclododecaneDioxane; the phosphorus flame retardant is triphenyl phosphate; the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine in a mass ratio of 3:5: 2; the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8; the inorganic hydroxide flame retardant is aluminum hydroxide; the plasticizer is mineral oil; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is antioxidant 1010;
the preparation method comprises the following steps:
s1, weighing the components according to the formula for later use;
s2, heating and melting the resin, adding the plasticizer, the lubricant, the stabilizer, the antioxidant and the silane coupling agent, and uniformly mixing to obtain a first component;
s3, uniformly mixing carbon black, expanded graphite, nano antimony trioxide, diisotoluene peroxide brominated flame retardant, phosphorus flame retardant and inorganic hydroxide flame retardant to obtain a second component;
s4, mixing the first component obtained in the step S2 and the second component obtained in the step S3, adding a compatilizer and a synergist, and uniformly mixing to obtain a mixed material;
and S5, calendering and molding the mixed material obtained in the step S4, and cooling to obtain the novel fireproof sealing material.
Example 2
50 parts of resin, 10 parts of carbon black, 75 parts of expanded graphite, 3 parts of nano antimony trioxide, 15 parts of a brominated flame retardant, 7 parts of a phosphorus flame retardant, 5 parts of dicumyl peroxide, 10 parts of a compatilizer, 7 parts of a synergist, 40 parts of a plasticizer, 3 parts of a lubricant, 10 parts of a stabilizer, 2 parts of an antioxidant, 1 part of a silane coupling agent and 5 parts of an inorganic hydroxide flame retardant,
wherein the resin is ethylene-vinyl acetate copolymer resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the brominated flame retardant is tetrabromobisphenol A; the phosphorus flame retardant is diphenyl cresyl phosphate; the compatilizer is sulfhydryl chitosanThe mass ratio of the mercapto graphene to the polyethyleneimine is 3:5: 2; the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8; the inorganic hydroxide flame retardant is magnesium hydroxide; the plasticizer is dioctyl phthalate; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is 3-aminopropyl triethoxysilane; the antioxidant is antioxidant 168;
the preparation method is the same as that of example 1.
Example 3
25 parts of resin, 5 parts of carbon black, 15 parts of expanded graphite, 0.5 part of nano antimony trioxide, 5 parts of brominated flame retardant, 1.5 parts of phosphorus flame retardant, 1 part of dicumyl peroxide, 2 parts of compatilizer, 1 part of synergist, 0.05 part of plasticizer, 0.5 part of lubricant, 2.5 parts of stabilizer, 0.1 part of antioxidant, 0.2 part of silane coupling agent and 1 part of inorganic hydroxide flame retardant;
wherein the resin is polyethylene resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the brominated flame retardant is tetrabromobisphenol allyl ether; the phosphorus flame retardant is diphenyl isopropyl phenyl phosphate; the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine in a mass ratio of 3:5: 2; the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8; the inorganic hydroxide flame retardant is aluminum hydroxide; the plasticizer is mineral oil; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is antioxidant 1010;
the preparation method is the same as that of example 1.
Example 4
40 parts of resin, 8 parts of carbon black, 55 parts of expanded graphite, 2 parts of nano antimony trioxide, 13 parts of a brominated flame retardant, 3.5 parts of a phosphorus flame retardant, 2 parts of dicumyl peroxide, 5 parts of a compatilizer, 5 parts of a synergist, 20 parts of a plasticizer, 2 parts of a lubricant, 8 parts of a stabilizer, 0.5 part of an antioxidant, 0.5 part of a silane coupling agent and 3.5 parts of an inorganic hydroxide flame retardant;
wherein the resin is polystyrene resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the bromine flame retardant is decabromodiphenyl ether; the phosphorus flame retardant is tricresyl phosphate; the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine in a mass ratio of 3:5: 2; the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8; the inorganic hydroxide flame retardant is aluminum hydroxide; the plasticizer is dioctyl phthalate; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is 3-aminopropyl triethoxysilane; the antioxidant is antioxidant 1010;
the preparation method is the same as that of example 1.
Example 5
33 parts of resin, 6 parts of carbon black, 30 parts of expanded graphite, 1.5 parts of nano antimony trioxide, 9 parts of brominated flame retardant, 2.5 parts of phosphorus flame retardant, 1.5 parts of dicumyl peroxide, 3 parts of compatilizer, 2 parts of synergist, 10 parts of plasticizer, 1.2 parts of lubricant, 5 parts of stabilizer, 0.3 part of antioxidant, 0.3 part of silane coupling agent and 2.5 parts of inorganic hydroxide flame retardant,
wherein the resin is styrene-acrylonitrile resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the brominated flame retardant is hexabromocyclododecane; the phosphorus flame retardant is tri (xylene) phosphate; the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine in a mass ratio of 3:5: 2; the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8; the inorganic hydroxide flame retardant is aluminum hydroxide; the plasticizer is mineral oil; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is antioxidant 1010;
the preparation method is the same as that of example 1.
Example 6
33 parts of resin, 6 parts of carbon black, 30 parts of expanded graphite, 1.5 parts of nano antimony trioxide, 9 parts of brominated flame retardant, 2.5 parts of phosphorus flame retardant, 1.5 parts of dicumyl peroxide, 3 parts of compatilizer, 2 parts of synergist, 10 parts of plasticizer, 1.2 parts of lubricant, 5 parts of stabilizer, 0.3 part of antioxidant, 0.3 part of silane coupling agent and 2.5 parts of inorganic hydroxide flame retardant,
wherein the resin is styrene-maleic anhydride copolymer resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the brominated flame retardant is hexabromocyclododecane; the phosphorus flame retardant is resorcinol bis (diphenyl phosphate); the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine in a mass ratio of 3:5: 2; the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8; the inorganic hydroxide flame retardant is aluminum hydroxide; the plasticizer is mineral oil; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is antioxidant 1010;
the preparation method is the same as that of example 1.
Comparative example 1
33 parts of resin, 6 parts of carbon black, 30 parts of expanded graphite, 1.5 parts of nano antimony trioxide, 9 parts of brominated flame retardant, 2.5 parts of phosphorus flame retardant, 1.5 parts of dicumyl peroxide, 3 parts of compatilizer, 2 parts of synergist, 10 parts of plasticizer, 1.2 parts of lubricant, 5 parts of stabilizer, 0.3 part of antioxidant, 0.3 part of silane coupling agent and 2.5 parts of inorganic hydroxide flame retardant,
wherein the resin is styrene-maleic anhydride copolymer resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the brominated flame retardant is hexabromocyclododecane; the phosphorus flame retardant is resorcinol bis (diphenyl phosphate); the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8; the inorganic hydroxide flame retardant is aluminum hydroxide; the plasticizer is mineralAn oil; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is antioxidant 1010;
the preparation method is the same as that of example 1 except that the compatilizer in step S4 is deleted.
Comparative example 2
33 parts of resin, 6 parts of carbon black, 30 parts of expanded graphite, 1.5 parts of nano antimony trioxide, 9 parts of brominated flame retardant, 2.5 parts of phosphorus flame retardant, 1.5 parts of dicumyl peroxide, 3 parts of compatilizer, 10 parts of plasticizer, 1.2 parts of lubricant, 5 parts of stabilizer, 0.3 part of antioxidant, 0.3 part of silane coupling agent and 2.5 parts of inorganic hydroxide flame retardant,
wherein the resin is styrene-maleic anhydride copolymer resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the brominated flame retardant is hexabromocyclododecane; the phosphorus flame retardant is resorcinol bis (diphenyl phosphate); the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine in a mass ratio of 3:5: 2; the plasticizer is mineral oil; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is antioxidant 1010;
the preparation method is the same as that of example 1 except that the synergist in step S4 is removed.
Comparative example 3
33 parts of resin, 6 parts of carbon black, 30 parts of expanded graphite, 1.5 parts of nano antimony trioxide, 9 parts of brominated flame retardant, 2.5 parts of phosphorus flame retardant, 3 parts of compatilizer, 2 parts of synergist, 10 parts of plasticizer, 1.2 parts of lubricant, 5 parts of stabilizer, 0.3 part of antioxidant and 0.3 part of silane coupling agent,
wherein the resin is styrene-maleic anhydride copolymer resin; the carbon black is conductive nano carbon black with the particle size of 15 nm; the particle size of the expanded graphite is 30-100 meshes; the particle size of the nano antimony trioxide is 24-35 nm, and the specific surface area is 54-90 m2(ii)/g; the brominated flame retardant is hexabromocyclododecane; the phosphorus flame retardant is resorcinol bis (bis)Phenyl phosphate ester); the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine in a mass ratio of 3:5: 2; the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8; the plasticizer is mineral oil; the lubricant is low molecular polyethylene wax; the stabilizer is calcium zinc stabilizer; the silane coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is antioxidant 1010;
the preparation method is the same as that of example 1 except that the diisotoluene peroxide and the inorganic hydroxide flame retardant in step S3 are removed.
The following performance tests were performed on the fireproof sealing materials prepared in examples 1 to 6 and comparative examples 1 to 3:
1. combustion performance: testing according to a vertical method specified in GB/T2408-2008 'determination horizontal method and vertical method of plastic combustion performance', and testing the combustion performance of a sample;
2. fire resistance: testing the fire resistance of a sample according to a test method specified in GB23864-2009 fireproof plugging material 6.16;
3. expansion performance: testing the fire resistance of a sample according to a test method specified in GB23864-2009 fireproof plugging material 6.14 expansion performance;
the test results are given in the following table:
as can be seen from the above table, compared with the fireproof sealing materials prepared in comparative examples 1 to 3, the fireproof sealing materials prepared in examples 1 to 6 of the present invention have better fireproof and heat insulating properties and fireproof and smoke-proof properties, the limited oxygen index is as high as 52.8, the flame retardant rating reaches V-0, the fire resistance limit reaches 4h, the smoke-proof time is as high as 80min, and the fireproof sealing materials have good expansion properties, so that after the fireproof sealing materials prepared in examples 1 to 6 of the present invention are used for fireproof doors, fireproof windows, and fireproof partition members, when a fire occurs, the fireproof sealing materials do not burn by themselves, and can automatically expand to fill gaps at the sealing positions of the fireproof doors, the fireproof windows, the fireproof partition members, and the like, block air circulation in two spaces, effectively prevent the harm of early-stage dense smoke, toxic gas and hot gas of the fire to human body in the smoke-proof time, and have a good effect of preventing the penetration of flame and smoke, and effectively control the spread of fire, prevent the expansion of disaster, be fit for using widely.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The fireproof sealing material is characterized by comprising the following components in parts by weight:
20-50 parts of resin, 3-10 parts of carbon black, 5-75 parts of expanded graphite, 0.2-3 parts of nano antimony trioxide, 0.5-15 parts of brominated flame retardant, 0.2-7 parts of phosphorus flame retardant, 0.05-5 parts of dicumyl peroxide, 1-10 parts of compatilizer, 0.5-7 parts of synergist, 0.01-40 parts of plasticizer, 0.02-3 parts of lubricant, 2-10 parts of stabilizer, 0.1-2 parts of antioxidant, 0.1-1 part of silane coupling agent and 0.5-5 parts of inorganic hydroxide flame retardant;
the compatilizer is a mixture of sulfydryl chitosan, sulfydryl graphene and polyethyleneimine in a mass ratio of 3:5: 2;
the synergist is a mixture of aminopropyl isobutyl silsesquioxane and hollow glass microspheres in a mass ratio of 1: 8.
2. The fireproof sealing material of claim 1, which is composed of the following components in parts by weight:
25-40 parts of resin, 5-8 parts of carbon black, 15-55 parts of expanded graphite, 0.5-2 parts of nano antimony trioxide, 5-13 parts of brominated flame retardant, 1.5-3.5 parts of phosphorus flame retardant, 1-2 parts of dicumyl peroxide, 2-5 parts of compatilizer, 1-5 parts of synergist, 0.05-20 parts of plasticizer, 0.5-2 parts of lubricant, 2.5-8 parts of stabilizer, 0.1-0.5 part of antioxidant, 0.2-0.5 part of silane coupling agent and 1-3.5 parts of inorganic hydroxide flame retardant.
3. The fireproof sealing material of claim 1, which is composed of the following components in parts by weight:
33 parts of resin, 6 parts of carbon black, 30 parts of expanded graphite, 1.5 parts of nano antimony trioxide, 9 parts of brominated flame retardant, 2.5 parts of phosphorus flame retardant, 1.5 parts of dicumyl peroxide, 3 parts of compatilizer, 2 parts of synergist, 10 parts of plasticizer, 1.2 parts of lubricant, 5 parts of stabilizer, 0.3 part of antioxidant, 0.3 part of silane coupling agent and 2.5 parts of inorganic hydroxide flame retardant.
4. The fire-resistant sealing material according to claim 1, wherein the resin is one or more of a polyvinyl chloride resin, an ethylene-vinyl acetate copolymer resin, a polyethylene resin, a polystyrene resin, a styrene-acrylonitrile resin, an acrylonitrile-butadiene-styrene resin, a styrene-maleic anhydride copolymer resin, an acrylonitrile-styrene-acrylate copolymer resin, a methacrylate-butadiene-styrene resin, a methyl methacrylate-acrylonitrile-butadiene-styrene resin, and a polyphenylene ether resin.
5. The fireproof sealing material of claim 1, wherein the carbon black is conductive nano carbon black with a particle size of 15nm, the expanded graphite particle size is 30-100 mesh, the nano antimony trioxide particle size is 24-35 nm, and the specific surface area is 54-90 m2/g。
6. The fire-retardant sealing material of claim 1 wherein said bromine-based flame retardant is one or more selected from hexabromocyclododecane, tetrabromobisphenol A, tetrabromobisphenol allyl ether, decabromodiphenyl ether, said phosphorus-based flame retardant is one or more selected from triphenyl phosphate, cresyldiphenyl phosphate, diphenylisopropyl phenyl phosphate, tricresyl phosphate, trixylenyl phosphate, resorcinol bis (diphenyl phosphate), and said inorganic hydroxide flame retardant is aluminum hydroxide and/or magnesium hydroxide.
7. The fireproof sealing material of claim 1, wherein the plasticizer is mineral oil or dioctyl phthalate, the lubricant is low molecular polyethylene wax, the stabilizer is calcium zinc stabilizer, the silane coupling agent is gamma-aminopropyl triethoxysilane or 3-aminopropyl triethoxysilane, and the antioxidant is antioxidant 1010 or antioxidant 168.
8. The preparation method of the fireproof sealing material is characterized by comprising the following steps of:
s1, weighing the components for later use according to the formula of the fireproof sealing material in any one of claims 1 to 7;
s2, heating and melting the resin, adding the plasticizer, the lubricant, the stabilizer, the antioxidant and the silane coupling agent, and uniformly mixing to obtain a first component;
s3, uniformly mixing carbon black, expanded graphite, nano antimony trioxide, dicumyl peroxide, a brominated flame retardant, a phosphorus flame retardant and an inorganic hydroxide flame retardant to obtain a second component;
s4, mixing the first component obtained in the step S2 and the second component obtained in the step S3, adding a compatilizer and a synergist, and uniformly mixing to obtain a mixed material;
and S5, calendering and molding the mixed material obtained in the step S4, and cooling to obtain the fireproof sealing material.
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| KR101381933B1 (en) * | 2013-02-21 | 2014-04-07 | 홍성산업 주식회사 | A flame retardant composite panel having light weight |
| CN104194177A (en) * | 2014-08-14 | 2014-12-10 | 韩志才 | Novel expandable polystyrene (EPS) functional material |
| CN107236273A (en) * | 2017-06-19 | 2017-10-10 | 魏科峰 | A kind of PC/ABS plastic alloys of halogen-free flameproof and preparation method thereof |
| CN108203525A (en) * | 2018-01-02 | 2018-06-26 | 佛山市南海崇泰防火材料有限公司 | A kind of inflatable fire resistant flexible material and its application |
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| KR100463171B1 (en) * | 2002-08-13 | 2004-12-23 | 주식회사 엘지화학 | Rubber-modified styrene resin composition |
| CN106380770A (en) * | 2016-08-26 | 2017-02-08 | 青岛海尔新材料研发有限公司 | Flame-retardant styrene resin composition and preparation method thereof |
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| KR101381933B1 (en) * | 2013-02-21 | 2014-04-07 | 홍성산업 주식회사 | A flame retardant composite panel having light weight |
| CN104194177A (en) * | 2014-08-14 | 2014-12-10 | 韩志才 | Novel expandable polystyrene (EPS) functional material |
| CN107236273A (en) * | 2017-06-19 | 2017-10-10 | 魏科峰 | A kind of PC/ABS plastic alloys of halogen-free flameproof and preparation method thereof |
| CN108203525A (en) * | 2018-01-02 | 2018-06-26 | 佛山市南海崇泰防火材料有限公司 | A kind of inflatable fire resistant flexible material and its application |
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