CN114410274A - Flame-retardant silicone sealant for hollow glass and preparation method thereof - Google Patents
Flame-retardant silicone sealant for hollow glass and preparation method thereof Download PDFInfo
- Publication number
- CN114410274A CN114410274A CN202210229699.3A CN202210229699A CN114410274A CN 114410274 A CN114410274 A CN 114410274A CN 202210229699 A CN202210229699 A CN 202210229699A CN 114410274 A CN114410274 A CN 114410274A
- Authority
- CN
- China
- Prior art keywords
- flame
- parts
- component
- retardant
- silicone sealant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 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 72
- 239000003063 flame retardant Substances 0.000 title claims abstract description 71
- 239000004590 silicone sealant Substances 0.000 title claims abstract description 31
- 239000011521 glass Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000006229 carbon black Substances 0.000 claims abstract description 38
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 37
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 19
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 16
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 16
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 239000007822 coupling agent Substances 0.000 claims abstract description 6
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 76
- 238000003756 stirring Methods 0.000 claims description 67
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 11
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- 239000011787 zinc oxide Substances 0.000 claims description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- 241000872198 Serjania polyphylla Species 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000002715 modification method Methods 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- MMGVVYCBXBYXRR-UHFFFAOYSA-L 2-acetyl-3-oxobutanoate;dibutyltin(2+) Chemical compound CCCC[Sn+2]CCCC.CC(=O)C(C(C)=O)C([O-])=O.CC(=O)C(C(C)=O)C([O-])=O MMGVVYCBXBYXRR-UHFFFAOYSA-L 0.000 claims 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 abstract description 11
- 229940083037 simethicone Drugs 0.000 abstract description 11
- 239000000565 sealant Substances 0.000 abstract description 7
- 238000005303 weighing Methods 0.000 description 36
- 238000004898 kneading Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 14
- 239000000463 material Substances 0.000 description 6
- 238000004381 surface treatment Methods 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 3
- 239000012796 inorganic flame retardant Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- BRUFYILNWNCKJT-UHFFFAOYSA-N 3-acetylpentane-2,4-dione;dibutyltin Chemical compound CCCC[Sn]CCCC.CC(=O)C(C(C)=O)C(C)=O BRUFYILNWNCKJT-UHFFFAOYSA-N 0.000 description 2
- KAHCSMBMOWVIMH-UHFFFAOYSA-N C(CCC)[Sn]CCCC.C(C)(=O)C(C(=O)OCC)C(C)=O Chemical compound C(CCC)[Sn]CCCC.C(C)(=O)C(C(=O)OCC)C(C)=O KAHCSMBMOWVIMH-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a flame-retardant silicone sealant for hollow glass and a preparation method thereof, wherein the sealant comprises a component A and a component B, the component A comprises alpha, omega-dihydroxy polydimethylsiloxane, a flame-retardant filler and a reinforcing filler, the component B comprises simethicone, a cross-linking agent, a coupling agent and a catalyst, the flame-retardant filler is prepared from silane coupling agent modified whiskers, the reinforcing filler is prepared from silane coupling agent modified white carbon black, and the component A and the component B are mixed according to a certain proportion to obtain the sealant.
Description
Technical Field
The invention relates to the technical field of sealing materials, in particular to a flame-retardant silicone sealant for hollow glass and a preparation method thereof.
Background
The silicone sealant has excellent high and low temperature resistance, insulating property, severe environment resistance and other properties, and has good adhesion to most base materials, so that the silicone sealant is widely applied to various application fields.
However, with the continuous development of the technology, the requirement of people on the fireproof and flame retardant performance of the sealant is higher and higher, the conventional flame retardant component is added into the silicone sealant, although the flame retardant performance of the silicone sealant can be improved, the addition of the flame retardant component can also directly influence the original performance of the silicone sealant, for example, when the flame retardant performance of the silicone sealant is improved by adopting an inorganic flame retardant filler, the addition amount of the inorganic flame retardant filler is generally larger, the addition of a large amount of the inorganic flame retardant filler can directly influence the adhesion performance between high molecular materials in the silicone sealant, and meanwhile, due to the difference of material properties, the materials are difficult to achieve good uniformity during mixing, and finally influence the mechanical performance of the cured sealant.
How to provide a silicone sealant which can improve the flame retardant property of the silicone sealant and simultaneously can not influence the mechanical property of the silicone sealant is a technical problem which needs to be solved urgently.
Disclosure of Invention
In view of the above, the invention provides a flame-retardant silicone sealant for hollow glass with excellent flame retardant property and mechanical property and a preparation method thereof.
The technical scheme of the invention is realized as follows: the invention provides a flame-retardant silicone sealant for hollow glass, which comprises a component A and a component B, wherein the component A comprises the following components in parts by weight:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane
30-50 parts of flame-retardant filler
30-50 parts of reinforcing filler
The component B comprises the following components in parts by weight:
on the basis of the technical scheme, preferably, when in use, the component A and the component B are mixed according to the mass ratio of (11-16): 1, mixing uniformly for use.
On the basis of the technical scheme, preferably, the flame-retardant filler is one or a mixture of more of aluminum oxide whiskers, magnesium oxide whiskers and tetrapod-like zinc oxide whiskers which are subjected to modification treatment by a silane coupling agent.
On the basis of the above technical solution, preferably, the preparation method of the flame retardant filler comprises: mixing the whisker to be modified with a silane coupling agent and xylene, keeping the temperature at 20-30 ℃ in a kneader, mixing and stirring at the stirring speed of 100-200rpm for 10-20min to obtain a mixed solution, heating the mixed solution to 90-100 ℃, mixing and stirring at the stirring speed of 600-700rpm for 30-40min, filtering and drying to obtain the flame-retardant filler.
Based on the above technical solution, preferably, the length of the alumina whisker and the magnesia whisker is 15 to 25 μm, and the length of the needle body of the tetrapod-like zinc oxide whisker is 15 to 25 μm.
Still further preferably, the whiskers: silane coupling agent: the mass ratio of the dimethylbenzene is 1: (0.1-0.2): (2-5).
On the basis of the above technical scheme, preferably, the reinforcing filler is white carbon black subjected to surface modification, and the surface modification method of the white carbon black comprises the following steps: after mixing the white carbon black with the silane coupling agent and ethanol, keeping the temperature at 50-60 ℃ in a kneader, mixing and stirring at the stirring speed of 300-400rpm for 20-30min, filtering and drying to obtain the surface modified white carbon black.
On the basis of the above technical scheme, preferably, the white carbon black: silane coupling agent: the mass ratio of ethanol is 1: (0.1-0.2): (2-5).
On the basis of the technical scheme, preferably, the cross-linking agent is one of methyltrimethoxysilane, methyltriethoxysilane and vinyltrimethoxysilane.
Based on the above technical scheme, preferably, the coupling agent is one of KH540, KH550, KH560 and KH 570.
On the basis of the technical scheme, preferably, the catalyst is one of dibutyltin diacetate, dibutyltin diacetyl acetone and dibutyltin ethyl diacetylacetate.
The invention also provides a preparation method of the flame-retardant silicone sealant for hollow glass, which comprises the following steps: uniformly mixing alpha, omega-dihydroxy polydimethylsiloxane with the flame-retardant filler and the reinforcing filler respectively, and then performing vacuum defoaming to obtain a component A; then uniformly mixing the dimethyl silicone oil, the cross-linking agent, the coupling agent and the catalyst, and performing vacuum defoaming to obtain a component B.
On the basis of the technical scheme, preferably, after alpha, omega-dihydroxy polydimethylsiloxane is respectively uniformly mixed with the flame-retardant filler and the reinforcing filler, kneading treatment is carried out for 10-30min at the vacuum degree of-0.08-0.1 MPa and the temperature of 20-30 ℃ to obtain the component A, and then the simethicone, the cross-linking agent, the coupling agent and the catalyst are uniformly mixed, kneading treatment is carried out for 20-40min at the vacuum degree of-0.08-0.1 MPa and the temperature of 20-30 ℃ to obtain the component B.
Compared with the prior art, the flame-retardant silicone sealant for hollow glass has the following beneficial effects:
(1) according to the invention, the silane coupling agent modified magnesium oxide, aluminum oxide or zinc oxide whisker is used as a flame retardant component, so that the flame retardant effect is good, and the influence on the mechanical strength of the silicone sealant is small;
(2) furthermore, the white carbon black subjected to surface modification by silane and ethanol is used as a reinforcing filler, so that the intermolecular acting force of the polyorganosiloxane is improved, the mechanical strength of the sealant body is also improved, the white carbon black subjected to surface modification has better dispersion performance and surface performance, and the problem of weakening the acting force between the filler and the silicone rubber due to the addition of the flame-retardant filler can be solved.
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 obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
Preparing a flame-retardant filler:
respectively weighing 1 part of alumina whisker with the length of 15-25 mu m, 0.1 part of silane coupling agent KH540 and 2 parts of dimethylbenzene, uniformly mixing, keeping the temperature in a kneader at 20-30 ℃ and the stirring speed of 100rpm, mixing and stirring for 10min to obtain a mixed solution, heating the mixed solution to 90 ℃, mixing and stirring at the stirring speed of 600rpm for 30min, filtering and drying to obtain the flame-retardant filler.
Preparing a reinforcing filler:
respectively weighing 1 part of white carbon black, 0.1 part of silane coupling agent KH540 and 2 parts of ethanol, uniformly mixing, keeping the temperature at 50 ℃ in a kneader, stirring at the stirring speed of 300rpm, mixing and stirring for 20min, filtering, and drying to obtain the surface-treated white carbon black.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 30 parts of flame-retardant filler and 30 parts of surface-treated white carbon black, uniformly mixing, and kneading at 20-30 ℃ for 10min under the vacuum degree of-0.08 MPa to obtain the component A.
Respectively weighing 10 parts of simethicone, 5 parts of methyltrimethoxysilane, 2 parts of silane coupling agent KH540 and 0.1 part of dibutyltin diacetate, uniformly mixing, and kneading at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ for 20min to obtain the component B.
Example 2
Preparing a flame-retardant filler:
respectively weighing 1 part of magnesium oxide whisker with the length of 15-25 mu m, 0.2 part of silane coupling agent KH550 and 3 parts of dimethylbenzene, uniformly mixing, keeping the temperature in a kneader at 20-30 ℃ and the stirring speed of 200rpm, mixing and stirring for 20min to obtain a mixed solution, heating the mixed solution to 100 ℃, mixing and stirring at the stirring speed of 700rpm for 40min, filtering and drying to obtain the flame-retardant filler.
Preparing a reinforcing filler:
respectively weighing 1 part of white carbon black, 0.2 part of silane coupling agent KH550 and 3 parts of ethanol, uniformly mixing, keeping the temperature at 60 ℃ in a kneader, stirring at the stirring speed of 400rpm, mixing and stirring for 30min, filtering, and drying to obtain the surface-treated white carbon black.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 40 parts of flame-retardant filler and 40 parts of white carbon black subjected to surface treatment, uniformly mixing, and kneading for 20min at the vacuum degree of-0.09 MPa and the temperature of 20-30 ℃ to obtain the component A.
Respectively weighing 10 parts of dimethyl silicone oil, 10 parts of methyl triethoxysilane, 3 parts of silane coupling agent KH550 and 0.5 part of dibutyltin diacetyl acetone, uniformly mixing, and kneading at the temperature of 20-30 ℃ and the vacuum degree of-0.09 MPa for 30min to obtain the component B.
Example 3
Preparing a flame-retardant filler:
respectively weighing 1 part of tetrapod-shaped zinc oxide whisker with the needle body length of 15-25 mu m, 0.2 part of silane coupling agent KH560 and 4 parts of dimethylbenzene, uniformly mixing, keeping the temperature of 20-30 ℃ in a kneader and stirring at the speed of 200rpm, mixing and stirring for 20min to obtain a mixed solution, heating the mixed solution to 100 ℃, mixing and stirring at the speed of 700rpm for 40min, filtering and drying to obtain the flame-retardant filler.
Preparing a reinforcing filler:
respectively weighing 1 part of white carbon black, 0.2 part of silane coupling agent KH560 and 4 parts of ethanol, uniformly mixing, keeping the temperature at 60 ℃ in a kneader, stirring at the stirring speed of 400rpm, mixing and stirring for 30min, filtering, and drying to obtain the surface-treated white carbon black.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 50 parts of flame-retardant filler and 50 parts of surface-treated white carbon black, uniformly mixing, and kneading at 20-30 ℃ for 20min under the vacuum degree of-0.1 MPa to obtain the component A.
Respectively weighing 10 parts of simethicone, 15 parts of vinyl trimethoxy silane, 4 parts of silane coupling agent KH560 and 1 part of ethyl diacetylacetate dibutyl tin, uniformly mixing, and kneading at 20-30 ℃ for 30min under the vacuum degree of-0.09 MPa to obtain the component B.
Example 4
Preparing a flame-retardant filler:
respectively weighing 0.5 part of magnesium oxide whisker with the length of 15-25 mu m, 0.5 part of tetrapod-like zinc oxide whisker with the needle-like body with the length of 15-25 mu m, 0.2 part of silane coupling agent KH570 and 5 parts of dimethylbenzene, uniformly mixing, keeping the temperature of 20-30 ℃ in a kneader and the stirring speed of 200rpm, mixing and stirring for 20min to obtain a mixed solution, heating the mixed solution to 100 ℃, mixing and stirring for 40min at the stirring speed of 700rpm, filtering and drying to obtain the flame-retardant filler.
Preparing a reinforcing filler:
respectively weighing 1 part of white carbon black, 0.2 part of silane coupling agent KH570 and 5 parts of ethanol, uniformly mixing, keeping the temperature at 60 ℃ in a kneader, stirring at the stirring speed of 400rpm, mixing and stirring for 30min, filtering, and drying to obtain the surface-treated white carbon black.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 40 parts of flame-retardant filler and 40 parts of white carbon black subjected to surface treatment, uniformly mixing, and kneading for 20min at the vacuum degree of-0.1 MPa and the temperature of 20-30 ℃ to obtain the component A.
Respectively weighing 10 parts of simethicone, 10 parts of vinyl trimethoxy silane, 5 parts of silane coupling agent KH570 and 0.5 part of dibutyltin diacetate, uniformly mixing, and kneading at the temperature of 20-30 ℃ and the vacuum degree of-0.1 MPa for 30min to obtain the component B.
Example 5
Preparing a flame-retardant filler:
respectively weighing 0.5 part of alumina whisker with the length of 15-25 mu m, 0.5 part of magnesium oxide whisker with the length of 15-25 mu m, 0.2 part of silane coupling agent KH570 and 5 parts of dimethylbenzene, uniformly mixing, keeping the temperature of 20-30 ℃ in a kneader and the stirring speed of 200rpm, mixing and stirring for 20min to obtain a mixed solution, heating the mixed solution to 100 ℃, mixing and stirring for 40min at the stirring speed of 700rpm, filtering and drying to obtain the flame-retardant filler.
Preparing a reinforcing filler:
respectively weighing 1 part of white carbon black, 0.2 part of silane coupling agent KH570 and 5 parts of ethanol, uniformly mixing, keeping the temperature at 60 ℃ in a kneader, stirring at the stirring speed of 400rpm, mixing and stirring for 30min, filtering, and drying to obtain the surface-treated white carbon black.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 40 parts of flame-retardant filler and 40 parts of white carbon black subjected to surface treatment, uniformly mixing, and kneading for 20min at the vacuum degree of-0.1 MPa and the temperature of 20-30 ℃ to obtain the component A.
Respectively weighing 10 parts of simethicone, 10 parts of vinyl trimethoxy silane, 5 parts of silane coupling agent KH570 and 0.5 part of dibutyltin diacetate, uniformly mixing, and kneading at the temperature of 20-30 ℃ and the vacuum degree of-0.1 MPa for 30min to obtain the component B.
Comparative example 1
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 30 parts of alumina whisker with the length of 15-25 mu m and 30 parts of white carbon black, uniformly mixing, and kneading for 10min at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ to obtain the component A.
Respectively weighing 10 parts of simethicone, 5 parts of methyltrimethoxysilane, 2 parts of silane coupling agent KH540 and 0.1 part of dibutyltin diacetate, uniformly mixing, and kneading at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ for 20min to obtain the component B.
Comparative example 2
Preparing a flame-retardant filler:
respectively weighing 1 part of alumina whisker with the length of 15-25 mu m, 0.1 part of silane coupling agent KH540 and 2 parts of dimethylbenzene, uniformly mixing, keeping the temperature in a kneader at 20-30 ℃ and the stirring speed of 100rpm, mixing and stirring for 10min to obtain a mixed solution, heating the mixed solution to 90 ℃, mixing and stirring at the stirring speed of 600rpm for 30min, filtering and drying to obtain the flame-retardant filler.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 30 parts of flame retardant filler and 30 parts of white carbon black, uniformly mixing, and kneading for 10min at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ to obtain the component A.
Respectively weighing 10 parts of simethicone, 5 parts of methyltrimethoxysilane, 2 parts of silane coupling agent KH540 and 0.1 part of dibutyltin diacetate, uniformly mixing, and kneading at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ for 20min to obtain the component B.
Comparative example 3
Preparing a reinforcing filler:
respectively weighing 1 part of white carbon black, 0.1 part of silane coupling agent KH540 and 2 parts of ethanol, uniformly mixing, keeping the temperature at 50 ℃ in a kneader, stirring at the stirring speed of 300rpm, mixing and stirring for 20min, filtering, and drying to obtain the surface-treated white carbon black.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 30 parts of alumina whisker with the length of 15-25 mu m and 30 parts of white carbon black subjected to surface treatment, uniformly mixing, and kneading for 10min at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ to obtain the component A.
Respectively weighing 10 parts of simethicone, 5 parts of methyltrimethoxysilane, 2 parts of silane coupling agent KH540 and 0.1 part of dibutyltin diacetate, uniformly mixing, and kneading at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ for 20min to obtain the component B.
The A, B components prepared in the above examples and comparative examples are uniformly mixed according to the mass ratio of 11:1 to prepare adhesive tapes, rubber plates and I-shaped parts, and the flame retardant property, Shore A hardness, tensile strength, elongation at break and tear strength are respectively tested, and the results are shown in the following table:
| grouping | Oxygen index | Shore A hardness | Tensile strength | Elongation at break | Tear strength |
| Example 1 | 33％ | 42 degree | 3.4MPa | 160％ | 12.6KN/m |
| Example 2 | 34％ | 42 degree | 3.4MPa | 160％ | 12.8KN/m |
| Example 3 | 34％ | 43 degree | 3.5MPa | 160％ | 12.7KN/m |
| Example 4 | 36％ | 44 degree | 3.7MPa | 180％ | 13.8KN/m |
| Example 5 | 35％ | 43 degree | 3.4MPa | 160％ | 12.8KN/m |
| Comparative example 1 | 30％ | 41 degree | 2.6MPa | 120％ | 9.5KN/m |
| Comparative example 2 | 32％ | 42 degree | 2.8MPa | 130％ | 10.2KN/m |
| Comparative example 3 | 31％ | 42 degree | 2.7MPa | 130％ | 10.4KN/m |
The data of the above examples show that the silicone sealant prepared by the technical scheme of the invention has good flame retardant property, and meanwhile, the preparation method of the flame retardant filler and the reinforcing filler adopted in the invention enables the silicone sealant corresponding to the invention to overcome the problem of mechanical property reduction caused by adding conventional flame retardant filler, on the contrary, the obtained sealant still has good tensile strength and tear strength, and particularly when magnesium oxide whiskers and tetrapod-like zinc oxide whiskers are adopted as the base material of the modified flame retardant filler, the performances of the obtained sealant are optimal, and compared with the conventional method that single magnesium oxide whiskers or single tetrapod-like zinc oxide whiskers are adopted, the silicone sealant has better flame retardant property and mechanical property.
Comparative example 4
Preparing a flame-retardant filler:
respectively weighing 1 part of alumina whisker with the length of 5-15 mu m, 0.1 part of silane coupling agent KH540 and 2 parts of dimethylbenzene, uniformly mixing, keeping the temperature in a kneader at 20-30 ℃ and the stirring speed of 100rpm, mixing and stirring for 10min to obtain a mixed solution, heating the mixed solution to 90 ℃, mixing and stirring at the stirring speed of 600rpm for 30min, filtering and drying to obtain the flame-retardant filler.
Preparing a reinforcing filler:
respectively weighing 1 part of white carbon black, 0.1 part of silane coupling agent KH540 and 2 parts of ethanol, uniformly mixing, keeping the temperature at 50 ℃ in a kneader, stirring at the stirring speed of 300rpm, mixing and stirring for 20min, filtering, and drying to obtain the surface-treated white carbon black.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 30 parts of flame-retardant filler and 30 parts of surface-treated white carbon black, uniformly mixing, and kneading at 20-30 ℃ for 10min under the vacuum degree of-0.08 MPa to obtain the component A.
Respectively weighing 10 parts of simethicone, 5 parts of methyltrimethoxysilane, 2 parts of silane coupling agent KH540 and 0.1 part of dibutyltin diacetate, uniformly mixing, and kneading at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ for 20min to obtain the component B.
Comparative example 5
Preparing a flame-retardant filler:
respectively weighing 1 part of alumina whisker with the length of 25-35 mu m, 0.1 part of silane coupling agent KH540 and 2 parts of dimethylbenzene, uniformly mixing, keeping the temperature in a kneader at 20-30 ℃ and the stirring speed of 100rpm, mixing and stirring for 10min to obtain a mixed solution, heating the mixed solution to 90 ℃, mixing and stirring at the stirring speed of 600rpm for 30min, filtering and drying to obtain the flame-retardant filler.
Preparing a reinforcing filler:
respectively weighing 1 part of white carbon black, 0.1 part of silane coupling agent KH540 and 2 parts of ethanol, uniformly mixing, keeping the temperature at 50 ℃ in a kneader, stirring at the stirring speed of 300rpm, mixing and stirring for 20min, filtering, and drying to obtain the surface-treated white carbon black.
Respectively weighing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 30 parts of flame-retardant filler and 30 parts of surface-treated white carbon black, uniformly mixing, and kneading at 20-30 ℃ for 10min under the vacuum degree of-0.08 MPa to obtain the component A.
Respectively weighing 10 parts of simethicone, 5 parts of methyltrimethoxysilane, 2 parts of silane coupling agent KH540 and 0.1 part of dibutyltin diacetate, uniformly mixing, and kneading at the vacuum degree of-0.08 MPa and the temperature of 20-30 ℃ for 20min to obtain the component B.
The A, B components prepared in comparative example 4 and comparative example 5 were mixed uniformly at a mass ratio of 11:1 to prepare a rubber strip, a rubber sheet, and an i-shaped member. Then, corresponding performance tests are carried out, and the results are as follows:
| grouping | Oxygen index | Shore A hardness | Tensile strength | Elongation at break | Tear strength |
| Comparative example 4 | 33％ | 36 degree | 2.2MPa | 230％ | 12.4KN/m |
| Comparative example 5 | 33％ | 45 degree | 3.8MPa | 90％ | 13.2KN/m |
It can be seen from the comparative example data that the mechanical properties are greatly affected when the whisker length of the substrate of the flame retardant filler is changed, while the flame retardant properties are not greatly affected by the change of the material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. The flame-retardant silicone sealant for hollow glass is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by weight:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane
30-50 parts of flame-retardant filler
30-50 parts of reinforcing filler
The component B comprises the following components in parts by weight:
2. the flame-retardant silicone sealant for hollow glass according to claim 1, wherein the flame-retardant filler is one or a mixture of more of aluminum oxide whiskers, magnesium oxide whiskers and tetrapod-like zinc oxide whiskers, which are modified with a silane coupling agent.
3. The flame-retardant silicone sealant for hollow glass according to claim 2, wherein the preparation method of the flame-retardant filler comprises: mixing the whisker to be modified with a silane coupling agent and xylene, keeping the temperature at 20-30 ℃ in a kneader, mixing and stirring at the stirring speed of 100-200rpm for 10-20min to obtain a mixed solution, heating the mixed solution to 90-100 ℃, mixing and stirring at the stirring speed of 600-700rpm for 30-40min, filtering and drying to obtain the flame-retardant filler.
4. The flame retardant silicone sealant for hollow glass according to claim 2, wherein the alumina whiskers and the magnesia whiskers have a length of 15 to 25 μm, and the tetrapod-like zinc oxide whiskers have a needle body length of 15 to 25 μm.
5. The flame-retardant silicone sealant for hollow glass according to claim 1, wherein the reinforcing filler is white carbon black subjected to surface modification, and the surface modification method of the white carbon black comprises the following steps: after mixing the white carbon black with the silane coupling agent and ethanol, keeping the temperature at 50-60 ℃ in a kneader, mixing and stirring at the stirring speed of 300-400rpm for 20-30min, filtering and drying to obtain the surface modified white carbon black.
6. The flame retardant silicone sealant for hollow glass according to claim 1, wherein said crosslinking agent is one of methyltrimethoxysilane, methyltriethoxysilane and vinyltrimethoxysilane.
7. The flame-retardant silicone sealant for hollow glass according to claim 1, wherein the coupling agent is one of KH540, KH550, KH560 and KH 570.
8. The flame retardant silicone sealant for hollow glass according to claim 1, wherein the catalyst is one of dibutyltin diacetate, dibutyltin diacetylacetonate and dibutyltin diacetylacetate.
9. The process for preparing the flame retardant silicone sealant for hollow glass according to any one of claims 1 to 8, comprising the steps of: uniformly mixing alpha, omega-dihydroxy polydimethylsiloxane with the flame-retardant filler and the reinforcing filler respectively, and then performing vacuum defoaming to obtain a component A; then uniformly mixing the dimethyl silicone oil, the cross-linking agent, the coupling agent and the catalyst, and performing vacuum defoaming to obtain a component B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210229699.3A CN114410274A (en) | 2022-03-10 | 2022-03-10 | Flame-retardant silicone sealant for hollow glass and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210229699.3A CN114410274A (en) | 2022-03-10 | 2022-03-10 | Flame-retardant silicone sealant for hollow glass and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114410274A true CN114410274A (en) | 2022-04-29 |
Family
ID=81264562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210229699.3A Pending CN114410274A (en) | 2022-03-10 | 2022-03-10 | Flame-retardant silicone sealant for hollow glass and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114410274A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115491165A (en) * | 2022-10-19 | 2022-12-20 | 杭州之江新材料有限公司 | Flame-retardant silicone adhesive for hollow glass and preparation method thereof |
| CN117070186A (en) * | 2023-10-18 | 2023-11-17 | 山东景茂新材料有限公司 | Preparation method of alcohol type silicone sealant |
| CN118064076A (en) * | 2024-04-24 | 2024-05-24 | 山东沃赛新材料科技有限公司 | Flame-retardant temperature-resistant antibacterial mildew-proof beautifying trimming adhesive and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH061911A (en) * | 1992-04-19 | 1994-01-11 | Sekiyu Sangyo Kasseika Center | Composite material |
| CN107446509A (en) * | 2017-08-03 | 2017-12-08 | 合肥隆延科技有限公司 | UV (ultraviolet) curing silicone sealant and preparation method thereof |
| CN107459804A (en) * | 2017-08-16 | 2017-12-12 | 宜宾天原集团股份有限公司 | Toughened and reinforced poly (arylene ether nitrile) composite material of inorganic crystal whisker and preparation method thereof |
| CN112239644A (en) * | 2020-09-07 | 2021-01-19 | 广州凌玮科技股份有限公司 | Silicone adhesive with good heat conduction effect and preparation method thereof |
-
2022
- 2022-03-10 CN CN202210229699.3A patent/CN114410274A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH061911A (en) * | 1992-04-19 | 1994-01-11 | Sekiyu Sangyo Kasseika Center | Composite material |
| CN107446509A (en) * | 2017-08-03 | 2017-12-08 | 合肥隆延科技有限公司 | UV (ultraviolet) curing silicone sealant and preparation method thereof |
| CN107459804A (en) * | 2017-08-16 | 2017-12-12 | 宜宾天原集团股份有限公司 | Toughened and reinforced poly (arylene ether nitrile) composite material of inorganic crystal whisker and preparation method thereof |
| CN112239644A (en) * | 2020-09-07 | 2021-01-19 | 广州凌玮科技股份有限公司 | Silicone adhesive with good heat conduction effect and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 山西省化工研究所: "《增强塑料：细观结构与力学性能》" * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115491165A (en) * | 2022-10-19 | 2022-12-20 | 杭州之江新材料有限公司 | Flame-retardant silicone adhesive for hollow glass and preparation method thereof |
| CN115491165B (en) * | 2022-10-19 | 2023-08-18 | 杭州之江新材料有限公司 | Flame-retardant silicone adhesive for hollow glass and preparation method thereof |
| CN117070186A (en) * | 2023-10-18 | 2023-11-17 | 山东景茂新材料有限公司 | Preparation method of alcohol type silicone sealant |
| CN117070186B (en) * | 2023-10-18 | 2023-12-26 | 山东景茂新材料有限公司 | Preparation method of alcohol type silicone sealant |
| CN118064076A (en) * | 2024-04-24 | 2024-05-24 | 山东沃赛新材料科技有限公司 | Flame-retardant temperature-resistant antibacterial mildew-proof beautifying trimming adhesive and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114410274A (en) | Flame-retardant silicone sealant for hollow glass and preparation method thereof | |
| CN111087958A (en) | Room-temperature fast-curing epoxy adhesive and preparation method thereof | |
| CN103709763A (en) | Low-compression permanent deformation silicone rubber composition and preparation method thereof | |
| CN103408948B (en) | A kind of rubber combination and application thereof | |
| CN108314990B (en) | High-strength high-temperature-resistant silicone sealant and preparation method thereof | |
| CN111718486A (en) | Thixotropic agent and two-component silicone sealant containing same | |
| CN110387128B (en) | Self-adhesive single-component addition type silicone rubber and preparation method thereof | |
| CN104693805A (en) | Low-viscosity and high-strength transparent organic silicon compound as well as preparation method and application thereof | |
| CN116162439A (en) | Preparation method of polydopamine modified polysiloxane organic silica gel film | |
| CN115011246A (en) | High-strength wear-resistant organic silicon protective coating and preparation method thereof | |
| JP3763334B2 (en) | Method for producing rubber composition and rubber composition | |
| CN112251165B (en) | Special prime coat-free platinum vulcanizing agent for combination of metal substrate and silica gel and preparation method thereof | |
| CN113980470A (en) | Single-component high-transparency ketoxime-removing room-temperature vulcanized silicone rubber | |
| CN111117481B (en) | Addition type organic silicon liquid coating material and preparation method and application thereof | |
| CN111662511A (en) | High-resilience high-strength thermoplastic vulcanized elastomer material and preparation method thereof | |
| CN115926472B (en) | High-hardness high-performance liquid silicone rubber and preparation method thereof | |
| CN115584064B (en) | Variable modulus damping rubber material and preparation method and application thereof | |
| CN112111157A (en) | Novel guanidine salt antibacterial mildew-proof silicone rubber and preparation method thereof | |
| CN106318268A (en) | Adhesive capable of enhancing adhesion between chloroprene rubber and polyester lines and preparation method thereof | |
| CN113549330B (en) | High-strength easy-demolding mold silica gel and preparation method thereof | |
| CN115109326A (en) | High-damping high-durability composite rubber | |
| KR102399677B1 (en) | Ultra-high temperature silicone rubber gasket composition with improved durability and preparing method thereof | |
| KR101717183B1 (en) | A cylinder head module including gasket of cylinder head cover module | |
| CN114456602B (en) | Silicone rubber impression material for precision die | |
| CN114836041B (en) | Composite insulator rubber compound and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220429 |
|
| RJ01 | Rejection of invention patent application after publication |