CN115707754A - Fireproof flame-retardant expandable sealant and preparation method thereof - Google Patents
Fireproof flame-retardant expandable sealant and preparation method thereof Download PDFInfo
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- CN115707754A CN115707754A CN202110947930.8A CN202110947930A CN115707754A CN 115707754 A CN115707754 A CN 115707754A CN 202110947930 A CN202110947930 A CN 202110947930A CN 115707754 A CN115707754 A CN 115707754A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 26
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000000565 sealant Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000004590 silicone sealant Substances 0.000 claims abstract description 31
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 14
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 13
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 13
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 13
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 13
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 13
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920002050 silicone resin Polymers 0.000 claims abstract description 13
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 12
- 239000012188 paraffin wax Substances 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000000945 filler Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 28
- 239000006185 dispersion Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000009924 canning Methods 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 10
- HEXHLHNCJVXPNU-UHFFFAOYSA-N 2-(trimethoxysilylmethyl)butane-1,4-diamine Chemical compound CO[Si](OC)(OC)CC(CN)CCN HEXHLHNCJVXPNU-UHFFFAOYSA-N 0.000 claims description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 9
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000012257 stirred material Substances 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 abstract description 5
- 229910052736 halogen Inorganic materials 0.000 abstract description 4
- 150000002367 halogens Chemical class 0.000 abstract description 4
- 239000002341 toxic gas Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- 239000011863 silicon-based powder Substances 0.000 description 5
- 229920001971 elastomer Polymers 0.000 description 3
- 239000003566 sealing material Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
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- Sealing Material Composition (AREA)
Abstract
The invention discloses a fireproof flame-retardant expandable sealant and a preparation method thereof, and solves the technical problems of poor flame-retardant performance, high use hazard, and low extension and expansion of the conventional silicone sealant. The invention comprises the following components in parts by weight: 15-40 parts of alpha, omega-dihydroxy polydimethylsiloxane, 2-18 parts of 201 methyl silicone oil, 20-40 parts of expanded graphite, 5-10 parts of paraffin, 3-8 parts of melamine, 2-6 parts of ammonium polyphosphate, 4-10 parts of methyl phenyl silicone resin, 10-70 parts of filler, 2-10 parts of cross-linking agent, 0.2-2 parts of silane coupling agent and 0.5-3 parts of catalyst. The invention has simple structure, scientific and reasonable design and convenient use, adopts the silicone sealant which has strong flame retardance, does not contain halogen elements, has strong ductility and expansion, has wider application range, stronger safety performance and lower production cost, and the expanded graphite can enhance the volume of the silicone sealant and reduce the flow of air and toxic gas in a sealing way.
Description
Technical Field
The invention belongs to the technical field of high polymer sealing materials, and particularly relates to a fireproof flame-retardant expandable silicone sealant and a preparation method thereof.
Background
A fire door is a door that can meet the requirements of fire stability, integrity and thermal insulation within a certain period of time. It is a fire-proof partition with certain fire resistance, which is arranged in fire-proof subareas, evacuation staircases, vertical shafts and the like. The fire door has the functions of a common door and also has the functions of preventing the fire from spreading and the smoke from diffusing, and can prevent the fire from spreading within a certain time to ensure the evacuation of people.
In order to ensure the sealing performance between the installation door frame and the wall body of the fireproof door, the joint of the installation door frame and the wall body needs to be filled with a sealing glue, and at present, a silicone sealing glue is generally adopted. The silicone sealant has the characteristics of excellent weather aging resistance, ultraviolet stability, pressure resistance, shock resistance, moisture resistance, high and low temperature resistance, no tearing and cracking in severe weather environments and the like. Although the common silicone sealant has certain flame retardance, the problems of unqualified flame retardance and poor storage stability generally exist. In order to improve the flame retardant property, a bromine compound is commonly used as an organic flame retardant, aluminum hydroxide and the like are used as inorganic flame retardants, but when the bromine compound is combusted, carcinogenic substances are easily generated, and the surface polarity of magnesium hydroxide and the like is high, the mechanical processing property is poor, so that the elasticity and displacement of the silicone sealant are seriously influenced. In addition, the low ductility and low expansion of silicone sealants can make them somewhat limited.
Therefore, the invention provides a fireproof and flame-retardant expandable silicone sealant and a preparation method thereof, solves the technical problems of poor flame retardant property, high use hazard, and low extension and expansion of the conventional silicone sealant, adopts the silicone sealant which has strong flame retardancy, does not contain halogen elements, has strong extensibility and expansion, has wider application range, stronger safety performance and lower production cost, and can enhance the volume of the silicone sealant, seal and reduce the flow of air and toxic gases.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the fireproof flame-retardant expandable silicone sealant and the preparation method thereof are provided, and the technical problems of poor flame-retardant performance, high use hazard and low extension and expansion of the conventional silicone sealant are solved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the fireproof flame-retardant expandable silicone sealant comprises the following components in parts by weight:
further, the filler is one or more of calcium carbonate, activated clay, silica micropowder, talcum powder and diatomite.
Further, the filler is silicon micropowder.
Further, the cross-linking agent is any one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane and phenyltrimethoxysilane.
Further, the crosslinking agent is vinyltrimethoxysilane.
Further, the silane coupling agent is any one or more of gamma-aminopropyltriethoxysilane, beta-aminoethyl-gamma-aminopropyltrimethoxysilane, bis (gamma-trimethoxysilylpropyl) amine and glycidoxypropyltrimethoxysilane.
Further, the silane coupling agent is beta-aminoethyl-gamma-aminopropyltrimethoxysilane.
Further, the catalyst is any one or more of isopropyl titanate, butyl titanate, dibutyltin dilaurate and dibutyltin diacetate.
Further, the catalyst is butyl titanate.
A preparation method of a fireproof flame-retardant expandable silicone sealant comprises the following steps:
step 1, adding alpha, omega-dihydroxy polydimethylsiloxane, 201 methyl silicone oil, paraffin, melamine, ammonium polyphosphate, methyl phenyl silicone resin and filler into a vacuum kneading machine according to parts by weight, keeping the temperature at 100-130 ℃, and dehydrating and blending for 1-2 hours under the vacuum degree of-0.1 to-0.03 MPa to obtain a mixed base material;
step 2, grinding the mixed base material obtained in the step 1 in a three-roll grinder for 2 times to obtain a ground base material;
3, transferring the ground base material obtained in the step 2 into a high-speed dispersion stirring kettle, and cooling to room temperature to obtain a cooled base material;
step 4, adding expanded graphite, a cross-linking agent and a silane coupling agent into the cooling base material in the high-speed dispersing and stirring kettle in the step 3 at room temperature, and stirring for 1.5 hours under the conditions that the vacuum degree is-0.1 to-0.03 MPa and the rotating speed is 200rpm to obtain a mixed stirring object;
and 5, adding a catalyst into the mixed stirred material obtained in the step 4, stirring for 1h under the conditions that the vacuum degree is-0.1 to-0.03 MPa and the rotating speed is 250rpm, discharging and canning to obtain the silicone sealant.
Compared with the prior art, the invention has the following beneficial effects:
the invention has simple structure, scientific and reasonable design and convenient use, solves the technical problems of poor flame retardant property, high use hazard and low extension and expansion of the existing silicone sealant, adopts the silicone sealant which has strong flame retardance, does not contain halogen elements, has strong extensibility and expansion, has wider use range, stronger safety performance and lower production cost, and the expanded graphite can enhance the volume of the silicone sealant and reduce the flow of air and toxic gas in a sealing way.
The invention is prepared by the composite reaction of alpha, omega-dihydroxy polydimethylsiloxane, 201 methyl silicone oil, expanded graphite, paraffin melamine, ammonium polyphosphate, methyl phenyl silicone resin, filler, a crosslinking agent, a silane coupling agent and a catalyst, wherein the added melamine, ammonium polyphosphate and methyl phenyl silicone resin ensure that the silicone sealant has flame retardancy and self-extinguishing property, and the flame retardant property is far superior to that of the existing sealant. The silicone sealant disclosed by the invention has the advantages of good physical properties, large elasticity, larger stretchable length, higher safety in the actual use process and wider application range; meanwhile, no halogen is added, so that the paint is non-toxic, healthy and environment-friendly, and the use safety is enhanced. In addition, the expanded graphite is used as one of the raw materials, and the volume of the expanded graphite can be rapidly expanded at high temperature to block gaps and prevent flame and toxic gas from overflowing.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without any inventive step, are within the scope of the present invention.
The invention examines the influence of the selection of each component on the flame retardant property and the physical property of the fireproof silicone sealant through a large number of experiments, wherein the surface drying time detection method refers to the national standard GB/T13477 building sealing material test method, part 5: measuring the surface dry time;
the hardness detection method is referred to the national standard GB/T531 test method for pressing hardness of vulcanized rubber or thermoplastic rubber, part 1: shore durometer (shore hardness); the method for detecting the displacement capability is referred to national standard ASTMC719 test method for the adhesiveness and cohesive force of elastic joint sealing material under cyclic motion conditions;
tensile strength and elongation at break: testing according to the national standard GB/T528-2009, wherein the thickness of the prepared rubber plate is 2.0mm +/-0.25 mm, the length of the prepared rubber plate is not less than 25mm +/-0.25 mm, and the number of each group of cut samples is not less than 5;
and (3) determining the flame retardant property by an oxygen index method: measuring according to the national standard GB/T10707-2008; the prepared rubber plate sample has the length of 80-150mm, the width of 6.5 +/-0.25 mm and the thickness of 3 +/-0.25 mm. 20 samples of each panel were prepared and the test data for each panel was averaged.
Example one
Adding 15 parts of alpha, omega-dihydroxy polydimethylsiloxane, 2 parts of 201 methyl silicone oil, 5 parts of paraffin, 3 parts of melamine, 2 parts of ammonium polyphosphate, 4 parts of methyl phenyl silicone resin and 10 parts of silicon powder into a vacuum kneader, keeping the temperature at 100 ℃, dehydrating and blending for 2 hours under the vacuum degree of-0.1 MPa, grinding for 2 times by a three-roll grinder, transferring into a high-speed dispersion stirring kettle, cooling to room temperature to obtain a base material, adding 20 parts of expanded graphite, 2 parts of vinyl trimethoxy silane and 0.2 part of silane coupling agent beta-aminoethyl-gamma-aminopropyl trimethoxy silane into the high-speed dispersion stirring kettle at room temperature, mixing with the base material, stirring for 1.5 hours under the conditions of the vacuum degree of-0.1 MPa and the rotation speed of 200rpm, then adding 0.5 part of butyl titanate, stirring for 1 hour under the conditions of the vacuum degree of-0.1 MPa and the rotation speed of 250rpm, discharging and canning to obtain the silicone sealant.
Example two
Adding 20 parts of alpha, omega-dihydroxy polydimethylsiloxane, 6 parts of 201 methyl silicone oil, 6 parts of paraffin, 4 parts of melamine, 3 parts of ammonium polyphosphate, 5 parts of methyl phenyl silicone resin and 40 parts of silicon micropowder into a vacuum kneader, maintaining the temperature at 120 ℃, dehydrating and blending for 1 hour under the vacuum degree of-0.05 MPa, grinding for 2 times by a three-roll grinder, transferring into a high-speed dispersion stirring kettle, cooling to room temperature to obtain a base material, adding 25 parts of expanded graphite, 5 parts of vinyl trimethoxy silane and 0.5 part of silane coupling agent beta-aminoethyl-gamma-aminopropyl trimethoxy silane into the high-speed dispersion stirring kettle at room temperature, mixing with the base material, stirring for 1.5 hours under the conditions of the vacuum degree of-0.05 MPa and the rotation speed of 200rpm, then adding 1 part of butyl titanate, stirring for 1 hour under the conditions of the vacuum degree of-0.05 MPa and the rotation speed of 250rpm, discharging and canning to obtain the silicone sealant.
EXAMPLE III
Adding 18 parts of alpha, omega-dihydroxy polydimethylsiloxane, 12 parts of 201 methyl silicone oil, 7 parts of paraffin, 5 parts of melamine, 3 parts of ammonium polyphosphate, 5 parts of methyl phenyl silicone resin and 50 parts of silicon micropowder into a vacuum kneader, keeping the temperature at 120 ℃, dehydrating and blending for 1 hour under the vacuum degree of-0.05 MPa, grinding for 2 times by a three-roll grinder, transferring into a high-speed dispersion stirring kettle, cooling to room temperature to obtain a base material, adding 28 parts of expanded graphite, 6 parts of methyl trimethoxy silane and 1 part of gamma-aminopropyl triethoxysilane into the high-speed dispersion stirring kettle at room temperature, mixing with the base material, stirring for 1.5 hours under the conditions of the vacuum degree of-0.05 MPa and the rotating speed of 200rpm, then adding 1 part of dibutyltin diacetate, stirring for 1 hour under the conditions of the vacuum degree of-0.05 MPa and the rotating speed of 250rpm, discharging and canning to obtain the silicone sealant.
Example four
Adding 25 parts of alpha, omega-dihydroxy polydimethylsiloxane, 10 parts of 201 methyl silicone oil, 8 parts of paraffin, 5 parts of melamine, 4 parts of ammonium polyphosphate, 6 parts of methyl phenyl silicone resin and 60 parts of silicon powder into a vacuum kneader, keeping the temperature at 130 ℃, dehydrating and blending for 1 hour under the vacuum degree of minus 0.06MPa, grinding for 2 times by a three-roll grinder, transferring into a high-speed dispersion stirring kettle, cooling to room temperature to obtain a base material, adding 30 parts of expanded graphite, 6 parts of vinyl trimethoxy silane and 1 part of silane coupling agent beta-aminoethyl-gamma-aminopropyl trimethoxy silane into the high-speed dispersion stirring kettle at room temperature, mixing with the base material, stirring for 1.5 hours under the conditions of the vacuum degree of minus 0.06MPa and the rotation speed of 200rpm, then adding 1.5 parts of butyl titanate, discharging and canning after stirring for 1 hour under the conditions of the vacuum degree of minus 0.06MPa and the rotation speed of 250rpm, thus obtaining the silicone sealant.
EXAMPLE five
Adding 30 parts of alpha, omega-dihydroxy polydimethylsiloxane, 8 parts of 201 methyl silicone oil, 9 parts of paraffin, 6 parts of melamine, 5 parts of ammonium polyphosphate, 7 parts of methyl phenyl silicone resin and 70 parts of silicon powder into a vacuum kneader, maintaining the temperature at 110 ℃, dehydrating and blending for 1 hour under the vacuum degree of-0.03 MPa, grinding for 2 times by a three-roll grinder, transferring into a high-speed dispersion stirring kettle, cooling to room temperature to obtain a base material, adding 30 parts of expanded graphite, 8 parts of vinyl trimethoxy silane and 1.5 parts of beta-aminoethyl-gamma-aminopropyl trimethoxy silane into the high-speed dispersion stirring kettle at room temperature, mixing with the base material, stirring for 1.5 hours under the conditions of the vacuum degree of-0.03 MPa and the rotation speed of 200rpm, then adding 2 parts of butyl titanate, stirring for 1 hour under the conditions of the vacuum degree of-0.03 MPa and the rotation speed of 250rpm, discharging and canning to obtain the silicone sealant.
EXAMPLE six
Adding 35 parts of alpha, omega-dihydroxy polydimethylsiloxane, 7 parts of 201 methyl silicone oil, 10 parts of paraffin, 7 parts of melamine, 4 parts of ammonium polyphosphate, 8 parts of methyl phenyl silicone resin and 65 parts of silicon micropowder into a vacuum kneader, keeping the temperature at 110 ℃, dehydrating and blending for 1 hour under the vacuum degree of-0.03 MPa, grinding for 2 times by a three-roll grinder, transferring into a high-speed dispersion stirring kettle, cooling to room temperature to obtain a base material, then adding 30 parts of expanded graphite, 6 parts of phenyl trimethoxy silane and 2 parts of bis (gamma-trimethoxysilylpropyl) amine into the high-speed dispersion stirring kettle at room temperature, mixing with the base material, stirring for 1.5 hours under the conditions of the vacuum degree of-0.03 MPa and the rotation speed of 200rpm, then adding 2 parts of isopropyl titanate, stirring for 1 hour under the conditions of the vacuum degree of-0.03 MPa and the rotation speed of 250rpm, discharging and canning to obtain the sealant.
EXAMPLE seven
Adding 35 parts of alpha, omega-dihydroxy polydimethylsiloxane, 7 parts of 201 methyl silicone oil, 8 parts of paraffin, 7 parts of melamine, 4 parts of ammonium polyphosphate, 8 parts of methyl phenyl silicone resin and 65 parts of silicon powder into a vacuum kneader, maintaining the temperature at 110 ℃, dehydrating and blending for 1 hour under the vacuum degree of-0.03 MPa, grinding for 2 times by a three-roll grinder, transferring into a high-speed dispersion stirring kettle, cooling to room temperature to obtain a base material, adding 35 parts of expanded graphite, 6 parts of phenyltrimethoxysilane and 2 parts of bis (gamma-trimethoxysilylpropyl) amine into the high-speed dispersion stirring kettle at room temperature, mixing with the base material, stirring for 1.5 hours under the conditions of the vacuum degree of-0.03 MPa and the rotation speed of 200rpm, then adding 2 parts of dibutyltin diacetate, stirring for 1 hour under the conditions of the vacuum degree of-0.03 MPa and the rotation speed of 250rpm, discharging and canning to obtain the silicone sealant.
Example eight
Adding 40 parts of alpha, omega-dihydroxy polydimethylsiloxane, 18 parts of 201 methyl silicone oil, 8 parts of paraffin, 8 parts of melamine, 6 parts of ammonium polyphosphate, 10 parts of methyl phenyl silicone resin and 80 parts of silicon powder into a vacuum kneader, maintaining the temperature at 120 ℃, dehydrating and blending for 1 hour under the vacuum degree of-0.07 MPa, grinding for 2 times by a three-roll grinder, transferring into a high-speed dispersion stirring kettle, cooling to room temperature to obtain a base material, adding 40 parts of expanded graphite, 10 parts of vinyl trimethoxy silane and 2 parts of beta-aminoethyl-gamma-aminopropyl trimethoxy silane into the high-speed dispersion stirring kettle at room temperature, mixing with the base material, stirring for 1.5 hours under the conditions of the vacuum degree of-0.07 MPa and the rotation speed of 200rpm, then adding 3 parts of butyl titanate, stirring for 1 hour under the conditions of the vacuum degree of-0.07 MPa and the rotation speed of 250rpm, discharging and canning to obtain the silicone sealant.
Finally, it should be noted that: the above embodiments are only preferred embodiments of the present invention to illustrate the technical solutions of the present invention, but not to limit the technical solutions, and certainly not to limit the patent scope of the present invention; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention; that is, the technical problems to be solved by the present invention are still consistent with the present invention, and all the modifications or changes made without substantial meaning in the spirit and scope of the present invention should be included in the protection scope of the present invention; in addition, the technical scheme of the invention is directly or indirectly applied to other related technical fields, and the technical scheme of the invention is included in the patent protection scope of the invention.
Claims (10)
1. The fireproof flame-retardant expandable sealant is characterized by comprising the following components in parts by weight:
2. a fire retardant expandable sealant in accordance with claim 1, wherein: the filler is one or more of calcium carbonate, active clay, silica micropowder, talcum powder and diatomite.
3. A fire retardant expandable sealant according to claim 2, wherein: the filler is silicon micropowder.
4. A fire retardant expandable sealant according to claim 1, wherein: the cross-linking agent is any one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane and phenyltrimethoxysilane.
5. A fire retardant expandable sealant according to claim 4, wherein: the cross-linking agent is vinyl trimethoxy silane.
6. A fire retardant expandable sealant in accordance with claim 1, wherein: the silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, beta-aminoethyl-gamma-aminopropyltrimethoxysilane, bis (gamma-trimethoxysilylpropyl) amine and glycidoxypropyltrimethoxysilane.
7. The sealant of claim 6, wherein: the silane coupling agent is beta-aminoethyl-gamma-aminopropyltrimethoxysilane.
8. A fire retardant expandable sealant according to claim 1, wherein: the catalyst is one or more of isopropyl titanate, butyl titanate, dibutyltin dilaurate and dibutyltin diacetate.
9. A fire retardant expandable sealant according to claim 8, wherein: the catalyst is butyl titanate.
10. A method of preparing a fire retardant expandable sealant according to any one of claims 1-9, comprising the steps of:
step 1, adding alpha, omega-dihydroxy polydimethylsiloxane, 201 methyl silicone oil, paraffin, melamine, ammonium polyphosphate, methyl phenyl silicone resin and filler into a vacuum kneader according to parts by weight, keeping the temperature at 100-130 ℃, and dehydrating and blending for 1-2 hours under the vacuum degree of-0.1-0.03 MPa to obtain a mixed base material;
step 2, grinding the mixed base material obtained in the step 1 in a three-roll grinder for 2 times to obtain a ground base material;
3, transferring the grinding base material obtained in the step 2 into a high-speed dispersion stirring kettle, and cooling to room temperature to obtain a cooling base material;
step 4, adding expanded graphite, a cross-linking agent and a silane coupling agent into the cooling base material in the high-speed dispersing and stirring kettle in the step 3 at room temperature, and stirring for 1.5 hours under the conditions that the vacuum degree is-0.1 to-0.03 MPa and the rotating speed is 200rpm to obtain a mixed stirring object;
and 5, adding a catalyst into the mixed stirred material obtained in the step 4, stirring for 1h under the conditions that the vacuum degree is-0.1 to-0.03 MPa and the rotating speed is 250rpm, discharging and canning to obtain the silicone sealant.
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| CN202110947930.8A CN115707754A (en) | 2021-08-18 | 2021-08-18 | Fireproof flame-retardant expandable sealant and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964846A (en) * | 2012-12-19 | 2013-03-13 | 吴孟怀 | Thermal-expansion fireproof puddle |
| CN104388041A (en) * | 2014-12-01 | 2015-03-04 | 公安部四川消防研究所 | High-performance fireproof silicone sealant and preparation method thereof |
| CN109456599A (en) * | 2018-10-12 | 2019-03-12 | 浙江研和新材料股份有限公司 | A kind of fire prevention expansion and fire-retardant expansion combination sealing adhesive tape |
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2021
- 2021-08-18 CN CN202110947930.8A patent/CN115707754A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964846A (en) * | 2012-12-19 | 2013-03-13 | 吴孟怀 | Thermal-expansion fireproof puddle |
| CN104388041A (en) * | 2014-12-01 | 2015-03-04 | 公安部四川消防研究所 | High-performance fireproof silicone sealant and preparation method thereof |
| CN109456599A (en) * | 2018-10-12 | 2019-03-12 | 浙江研和新材料股份有限公司 | A kind of fire prevention expansion and fire-retardant expansion combination sealing adhesive tape |
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