CN102408722B - Novel bi-component dealcoholization type silicon rubber sealant and preparation method thereof - Google Patents
Novel bi-component dealcoholization type silicon rubber sealant and preparation method thereof Download PDFInfo
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- CN102408722B CN102408722B CN 201110303287 CN201110303287A CN102408722B CN 102408722 B CN102408722 B CN 102408722B CN 201110303287 CN201110303287 CN 201110303287 CN 201110303287 A CN201110303287 A CN 201110303287A CN 102408722 B CN102408722 B CN 102408722B
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000004589 rubber sealant Substances 0.000 title abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 12
- 229910001868 water Inorganic materials 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 30
- 239000004945 silicone rubber Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- -1 polydimethylsiloxane Polymers 0.000 claims description 19
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 18
- 229910021485 fumed silica Inorganic materials 0.000 claims description 18
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 18
- 239000012763 reinforcing filler Substances 0.000 claims description 16
- 239000000565 sealant Substances 0.000 claims description 15
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000012975 dibutyltin dilaurate Substances 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
- 239000000413 hydrolysate Substances 0.000 claims description 9
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 8
- 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 claims description 8
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 8
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 229940083037 simethicone Drugs 0.000 claims description 8
- 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 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- BTXXTMOWISPQSJ-UHFFFAOYSA-N 4,4,4-trifluorobutan-2-one Chemical compound CC(=O)CC(F)(F)F BTXXTMOWISPQSJ-UHFFFAOYSA-N 0.000 claims description 6
- BQACOLQNOUYJCE-FYZZASKESA-N Abietic acid Natural products CC(C)C1=CC2=CC[C@]3(C)[C@](C)(CCC[C@@]3(C)C(=O)O)[C@H]2CC1 BQACOLQNOUYJCE-FYZZASKESA-N 0.000 claims description 6
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 6
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 6
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000194 fatty acid Substances 0.000 claims description 6
- 229930195729 fatty acid Natural products 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 6
- QUVMSYUGOKEMPX-UHFFFAOYSA-N 2-methylpropan-1-olate;titanium(4+) Chemical compound [Ti+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] QUVMSYUGOKEMPX-UHFFFAOYSA-N 0.000 claims description 5
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 5
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 5
- XQBCVRSTVUHIGH-UHFFFAOYSA-L [dodecanoyloxy(dioctyl)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCCCCCC)(CCCCCCCC)OC(=O)CCCCCCCCCCC XQBCVRSTVUHIGH-UHFFFAOYSA-L 0.000 claims description 5
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 5
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims 2
- 229910007161 Si(CH3)3 Inorganic materials 0.000 claims 1
- 230000002411 adverse Effects 0.000 abstract description 3
- 229920013730 reactive polymer Polymers 0.000 abstract description 3
- 238000004132 cross linking Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 238000001723 curing Methods 0.000 description 8
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 7
- 238000012360 testing method Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000013008 moisture curing Methods 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Novel bi-component dealcoholization type silicon rubber sealant and preparation method thereof, wherein component A itself is single-component dealcoholization type silicon rubber and can offer a final strength value equal to the mixture of component A and component B, and has a good storage stability. The component B contains water, wherein the water can be directly added in free-state way and carried on the filler material; the component B also contains reactive polymer which can be activated by contacting with the catalyst of the component A, and perform quick cross-linking reaction with the cross-linking agent in the component A at the same time, the advantages of the invention are as follows: on one hand, the invention solves the shortcoming that the single-component silicon rubber has bigger reliance on the temperature and humidity of the environment; on the other hand, the invention accelerates the curing and reduces sensibility of the bi-component system to the mix error and measurement error at the same time. The ratios of the component A and component B in the bi-component system can vary in a large range without producing adverse effect to the final strength.
Description
Technical Field
The invention relates to a novel two-component dealcoholized silicone rubber sealant and a preparation method thereof. The novel double-component silicon rubber overcomes the defect that single-component silicon rubber has large dependence on environment temperature and humidity, and reduces sensitivity of a double-component system to mixing errors and metering errors while accelerating curing. The double-component silicon rubber can be widely used for bonding and encapsulating various electronic and electrical elements, can play a role in protection such as moisture prevention, corrosion prevention, insulation and the like, and is particularly suitable for encapsulating and bonding parts which require rapid and deep vulcanization.
Background
Room temperature vulcanized silicone rubber (RTV for short) is a type of silicone rubber which can be vulcanized at room temperature without heating, develops rapidly since the coming out of the 60 s, is widely used in the industries such as electronics, electrics, automobiles, buildings and the like, and brings a new opportunity for the development of RTV silicone rubber due to the rise of the photovoltaic industry in recent years. RTV silicone rubbers can be classified into two types, one-component and two-component, depending on the packaging.
The single-component RTV silicone rubber is generally preferred by users due to the convenience of use, because no mixing error or metering error occurs during use. However, the single-component RTV silicone rubber is cured from the outside to the inside, and is difficult to completely cure when the curing depth is more than a certain thickness, and the use of the single-component RTV silicone rubber is severely limited due to the relatively slow curing rate. Another disadvantage of single-component RTV silicone rubbers is their great dependence of the curing rate on the climate, i.e. their curing rate is not only dependent on the ambient temperature but also to a greater extent on the ambient atmospheric humidity, which is very low, in particular during the winter months, so that deep-layer curing is very slow.
The major advantage of the two-component RTV silicone rubber is its deep level of cure, and conventional two-component adhesive systems, which package the base rubber separately from the cross-linking agent, catalyst, etc. and mix them in a certain proportion before use, have the disadvantage that they are very sensitive to mixing errors, so that ideal cure and performance can only be achieved when the two components are mixed thoroughly in the correct stoichiometric ratio.
Disclosure of Invention
The object of the present invention is to provide a novel two-component system which allows mixing errors and metering errors in use, solves the problem of sensitivity of the two components to mixing errors and metering errors, and which can vary the ratio between component a and component B over a wide range without adversely affecting the final strength.
In order to achieve the purpose of the invention, the invention providesA novel two-component dealcoholized silicone rubber sealant comprises A, B following two components:
the component A comprises the following components:
A1100 parts of alpha, omega-dihydroxy polydimethylsiloxane having the molecular structural formulaHO[(CH3) 2 SiO] n H，n=300～1500；
A210-30 parts of simethicone, the molecular structural formula of which is (CH 3 ) 3 SiO[(CH3) 2 SiO] n Si(CH 3 ) 3 ，n=50～230；
A33-8 parts of dealcoholization type crosslinking agent
A41-5 parts of silane coupling agent
A510-100 parts of reinforcing filler
A6Catalyst 0.1-0.6 part
The component B comprises the following components:
B1100 parts of alpha, omega-dihydroxy polydimethylsiloxane having the molecular structural formulaHO[(CH3) 2 SiO] n H，n=300～1500；
B21-2 parts of a surfactant, namely selecting nonylphenol polyoxyethylene ether;
B3.8-15 parts of deionized water with the chemical formula of H2O；
B410-100 parts of reinforcing filler, which is at least one or a combination of a plurality of fillers selected from fumed silica and light calcium carbonate;
wherein the volume mixing ratio of A, B is 20: 1 to 2: 1, wherein 4: 1 and mixing.
A is described3Dealcoholization type crosslinking agent selected from at least one or more of methyltrimethoxysilane, vinyl trimethoxysilane, ethyl orthosilicate and partial hydrolysate thereof;
a is described4The silane coupling agent is at least one or a combination of a plurality of gamma-aminopropyl trimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma- (methacryloyloxy) propyl trimethoxysilane, gamma-mercaptopropyl trimethoxysilane and gamma-urea propyl trimethoxysilane;
a is described5Reinforcing filler, at least one or the combination of two fillers of fumed silica and light calcium carbonate is selected;
a is described6The moisture curing catalyst is at least one of dibutyltin dilaurate, dioctyltin dilaurate, stannous octoate, tetrabutyl titanate, tetraisobutyl titanate and tetraisopropyl titanate;
b is1The viscosity of the alpha, omega-dihydroxypolydimethylsiloxane is 1000-50000mpa.s at 25 ℃, and the preferred viscosity is 3000 mpa.s;
b is4The surface of the gas phase white carbon black is modified by dimethyl dichlorosilane or hexamethyldisilazane, and the light calcium carbonate is treated by fatty acid and abietic acid surface modifiers.
The invention also provides a preparation method of the novel two-component dealcoholized silicone rubber sealant, which consists of A, B two components, wherein the volume ratio of A, B two components is from 20: 1 to 2: 1, wherein 4: 1, mixing;
of component AThe preparation method comprises the following steps: mixing A in a certain proportion1、A2Uniformly mixing and de-bubbling N under the condition that the vacuum degree is-0.095 to-0.1 MPa2Adding A in turn under protection3Component A4Component A5Component A and6the components are added each time and stirred for 20min under the condition that the vacuum degree is-0.095 to-0.1 MPa, and finally the component A similar to single-component dealcoholized silicon rubber can be prepared;
the preparation method of the component B comprises the following steps: mixing B in a certain proportion1、B2Uniformly mixing and de-bubbling N under the condition that the vacuum degree is-0.095 to-0.1 MPa2Adding B in turn under protection3、B4The component is added each time and stirred for 20min under the condition that the vacuum degree is-0.095 to-0.1 MPa, and finally the component B can be prepared;
wherein,
A1100 parts of alpha, omega-dihydroxypolydimethylsiloxane；
A210-30 parts of simethicone；
A33-8 parts of dealcoholization type crosslinking agent
A41-5 parts of silane coupling agent
A510-100 parts of reinforcing filler
A6Catalyst 0.1-0.6 part
B1100 parts of alpha, omega-dihydroxypolydimethylsiloxane；
B21-2 parts of a surfactant, namely selecting nonylphenol polyoxyethylene ether;
B3.8-15 parts of deionized water;
B410-100 parts of reinforcing filler, and at least one or a combination of several fillers selected from fumed silica and light calcium carbonate.
A is described3A dealcoholization type cross-linking agent,selecting at least one or a combination of several of methyltrimethoxysilane, vinyl trimethoxysilane, ethyl orthosilicate and partial hydrolysate thereof;
a is described4The silane coupling agent is at least one or a combination of a plurality of gamma-aminopropyl trimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma- (methacryloyloxy) propyl trimethoxysilane, gamma-mercaptopropyl trimethoxysilane and gamma-urea propyl trimethoxysilane;
a is described5Reinforcing filler, at least one or the combination of two fillers of fumed silica and light calcium carbonate is selected;
a is described6The moisture curing catalyst is at least one of dibutyltin dilaurate, dioctyltin dilaurate, stannous octoate, tetrabutyl titanate, tetraisobutyl titanate and tetraisopropyl titanate;
b is1The viscosity of the alpha, omega-dihydroxypolydimethylsiloxane is 1000-50000mpa.s at 25 ℃, and the preferred viscosity is 3000 mpa.s;
b is4The surface of the gas phase white carbon black is modified by dimethyl dichlorosilane or hexamethyldisilazane, and the light calcium carbonate is treated by fatty acid and abietic acid surface modifiers.
The component A can also be prepared by the following specific steps: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000mpa.s at 25 ℃ and 20 parts of simethicone with viscosity of 500mpa.s are mixed uniformly under the condition of vacuum degree of-0.095 to-0.1 MPa for defoaming. Adding 4 parts of vinyl trimethoxy silane under the protection of nitrogen, stirring for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1MPa to carry out end capping reaction, adding 4 parts of partial hydrolysate of ethyl orthosilicate under the protection of nitrogen, and stirring for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1 MPa; adding a mixture of 2 parts of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane and 2 parts of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane under the protection of nitrogen, and stirring for 20min under the condition that the vacuum degree is-0.095 to-0.1 MPa; under the protection of nitrogen, 5 parts of fumed silica and 50 parts of light calcium carbonate are sequentially added, and stirring and dispersion are carried out under the condition that the vacuum degree is-0.095 to-0.1 MPa until the mixture is uniform and has no particles; adding 0.4 part of dibutyltin dilaurate under the protection of nitrogen, and stirring for 20min under the condition of vacuum degree of-0.095 to-0.1 MPa to obtain glue;
the component B can also be prepared by adopting the following specific steps: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 3000mpa.s at 25 ℃ and 1 part of nonylphenol polyoxyethylene ether are mixed uniformly under the condition of vacuum degree of-0.095 to-0.1 MPa to remove bubbles. 10 portions of deionized water is added under the protection of nitrogen and stirred for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1 MPa. Under the protection of nitrogen, 3 parts of fumed silica and 40 parts of light calcium carbonate are sequentially added, and stirring and dispersion are carried out under the condition that the vacuum degree is-0.095 to-0.1 MPa until uniform particle-free glue discharging is realized.
Compared with the prior art, the invention has the following beneficial effects:
the novel double-component dealcoholized silicone rubber sealant has the advantages that the defect that single-component silicone rubber has large dependence on environment temperature and humidity is overcome, and the sensitivity of a double-component system to mixing errors and metering errors is reduced while the curing is accelerated. The component A of the present invention can provide a final strength value comparable to that of a mixture of the component A and the component B, and is excellent in storage stability. The component B contains water, the water can be directly added in a free state or carried on a filler material, the component B also contains a reactive polymer, and the reactive polymer can be activated by a catalyst of the component A and simultaneously can perform a rapid crosslinking reaction with a crosslinking agent in the component A under the promotion of the water of the component B. Thus, the ratio of the two-component system to component A and component B can be varied over a wide range without adversely affecting the final strength.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific embodiments below.
The invention relates to a novel two-component dealcoholized silicone rubber sealant and a preparation method thereof, and is characterized in that the silicone rubber sealant comprises A, B two components, wherein the volume mixing ratio of A, B is 20: 1 to 2: 1.
1) the component A comprises the following components in parts by weight:
A1100 parts of alpha, omega-dihydroxypolydimethylsiloxane
A210-30 parts of simethicone
A33-8 parts of dealcoholization type crosslinking agent
A41-5 parts of silane coupling agent
A510-100 parts of reinforcing filler
A6Catalyst 0.1-0.6 part
A is described1 The component is alpha, omega-dihydroxy polydimethylsiloxane with the molecular structural formulaHO[(CH3) 2 SiO] n H，n = 300-1500, and the alpha, omega-dihydroxy polydimethylsiloxane having a viscosity of 1000-50000mpa.s, preferably 20000mpa.s at 25 ℃.
A is described2The component is dimethyl silicone oil with the molecular structural formula(CH 3 ) 3 SiO[(CH3) 2 SiO] n Si(CH 3 ) 3 N = 50-230, and the viscosity is 50-500mpa.s at 25 ℃, and the dimethyl silicone oil with the viscosity of 500mpa.s is preferred.
A is described3The component is dealcoholization type cross-linking agent, which is selected from at least one or a combination of methyl trimethoxy silane, vinyl trimethoxy silane, ethyl orthosilicate and partial hydrolysate thereof. Preference is given toA combination of vinyltrimethoxysilane and an ethyl orthosilicate partial hydrolysate.
A is described4The component is a silane coupling agent which is selected from at least one or a combination of a plurality of gamma-aminopropyl trimethoxy silane, N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma- (methacryloyloxy) propyl trimethoxy silane, gamma-mercaptopropyl trimethoxy silane and gamma-urea propyl trimethoxy silane. A combination of N- (. beta. -aminoethyl) -gamma-aminopropyltrimethoxysilane and gamma- (2, 3-glycidoxy) propyltrimethoxysilane is preferred.
A is described5The components are reinforcing fillers, and at least one or the combination of a plurality of fillers in fumed silica and light calcium carbonate is selected. The surface of the fumed silica is generally modified by dimethyldichlorosilane or hexamethyldisilazane, and the light calcium carbonate is generally treated by surface modifiers such as fatty acid, abietic acid and the like.
A is described6The component is moisture curing catalyst, and at least one of dibutyltin dilaurate, dioctyltin dilaurate, stannous octoate, tetrabutyl titanate, tetraisobutyl titanate and tetraisopropyl titanate is selected. Dibutyltin dilaurate is preferred.
The preparation method of the component A comprises the following steps: mixing A in a certain proportion1、A2Uniformly mixing and de-bubbling N under the condition that the vacuum degree is-0.095 to-0.1 MPa2Adding A in turn under protection3Component A4Component A5Component A and6after each addition, the components are stirred for 20min under the condition that the vacuum degree is-0.095 to-0.1 MPa, and finally the component A similar to the single-component dealcoholized silicone rubber can be prepared.
2) The component B comprises the following components:
B1100 parts of alpha, omega-dihydroxypolydimethylsiloxane
B2.1-2 parts of surfactant
B38-15 parts of deionized water
B410-100 parts of reinforcing filler
B is1 The component is alpha, omega-dihydroxy polydimethylsiloxane with the molecular structural formulaHO[(CH3) 2 SiO] n H，n = 300-1500, and the alpha, omega-dihydroxy polydimethylsiloxane having a viscosity of 1000-50000mpa.s, preferably 3000mpa.s at 25 ℃.
B is2The component is surfactant, and nonylphenol polyoxyethylene ether is selected
B is3The component is deionized water with a chemical formula of H2O
B is4The components are reinforcing fillers, and at least one or the combination of a plurality of fillers in fumed silica and light calcium carbonate is selected. The surface of the fumed silica is generally modified by dimethyldichlorosilane or hexamethyldisilazane, and the light calcium carbonate is generally treated by surface modifiers such as fatty acid, abietic acid and the like.
The preparation method of the component B comprises the following steps: mixing B in a certain proportion1、B2Uniformly mixing and de-bubbling N under the condition that the vacuum degree is-0.095 to-0.1 MPa2Adding B in turn under protection3、B4The component is added each time and stirred for 20min under the condition that the vacuum degree is-0.095 to-0.1 MPa, and finally the component B can be prepared.
Example (b):
100 parts of alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000mpa.s at 25 ℃ and 20 parts of simethicone with viscosity of 500mpa.s are mixed uniformly under the condition of vacuum degree of-0.095 to-0.1 MPa for defoaming. Adding 4 parts of vinyl trimethoxy silane under the protection of nitrogen, stirring for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1MPa to carry out end capping reaction, adding 4 parts of partial hydrolysate of ethyl orthosilicate under the protection of nitrogen, and stirring for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1 MPa. Adding a mixture of 2 parts of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane and 2 parts of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane into the mixture under the protection of nitrogen, and stirring the mixture for 20min under the condition that the vacuum degree is between-0.095 and-0.1 MPa. Under the protection of nitrogen, 5 parts of fumed silica and 50 parts of light calcium carbonate are sequentially added, and stirring and dispersion are carried out under the condition that the vacuum degree is-0.095 to-0.1 MPa until the mixture is uniform and has no particles. And (3) under the protection of nitrogen, rapidly adding 0.4 part of dibutyltin dilaurate, and stirring for 20min under the condition of vacuum degree of-0.095 to-0.1 MPa to obtain the component A.
100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 3000mpa.s at 25 ℃ and 1 part of nonylphenol polyoxyethylene ether are mixed uniformly under the condition of vacuum degree of-0.095 to-0.1 MPa to remove bubbles. 10 portions of deionized water is added under the protection of nitrogen and stirred for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1 MPa. And under the protection of nitrogen, sequentially adding 3 parts of fumed silica and 40 parts of light calcium carbonate, and stirring and dispersing under the condition that the vacuum degree is-0.095 to-0.1 MPa until the components are uniform, no particles are produced, and thus obtaining the component B.
The a-component silicone rubber sealant prepared in the examples and two-component 4: 1. 10: 1, preparing a sample wafer with the thickness of about 2mm by using a mold with the thickness of about 2mm, curing for 14 days at the temperature of 23 +/-2 ℃ and the humidity of 50 +/-5%, cutting the sample wafer into a dumbbell shape by using a special cutter, testing the hardness according to GB/T531, and testing the tensile strength and the elongation at break according to GB/T528. From the test data, it can be seen that the surface drying time of the two-component mixture is shortened compared with that of the single-component A, and the mixing ratio is 4: 1 and 10: the mechanical properties (tensile strength, elongation at break and hardness) of 1 are not much different from those of the single component A, and the insensitivity to the mixing proportion is reflected.
TABLE 1
| Test items | Component A | 4: 1 mixing | 10: 1 mixing |
| Surface drying time/min | 29 | 18 | 17 |
| hardness/A | 33 | 35 | 32 |
| Tensile strength/MPa | 1.9 | 1.9 | 1.8 |
| Elongation at break/% | 595 | 550 | 580 |
The above-mentioned embodiments are intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (1)
1. The two-component dealcoholized silicone rubber sealant is characterized by comprising the following A, B components in parts by weight:
the component A comprises the following components:
A1100 parts of alpha, omega-dihydroxy polydimethylsiloxane having the molecular structural formula HO [ (CH)3)2SiO]nH，n=300～1500；
A210-30 parts of simethicone, the molecular structural formula of which is (CH)3)3SiO[(CH3)2SiO]n Si(CH3)3，n=50～230；
A33-8 parts of dealcoholization type crosslinking agent;
A41-5 parts of a silane coupling agent;
A510-100 parts of reinforcing filler;
A60.1-0.6 parts of catalyst;
2) the component B comprises the following components:
B1100 parts of alpha, omega-dihydroxy polydimethylsiloxane having the molecular structural formula HO [ (CH)3)2SiO]nH，n=300～1500；
B21-2 parts of a surfactant, namely selecting nonylphenol polyoxyethylene ether;
B3.8-15 parts of deionized water with the chemical formula of H2O；
B410-100 parts of reinforcing filler, which is at least one or a combination of a plurality of fillers selected from fumed silica and light calcium carbonate;
wherein the volume mixing ratio of A, B is 20: 1 to 2: 1.
2. the silicone rubber sealant according to claim 1, wherein said a is3Dealcoholization type crosslinking agent selected from at least one or more of methyltrimethoxysilane, vinyl trimethoxysilane, ethyl orthosilicate and partial hydrolysate thereof;
a is described4The silane coupling agent is at least one or a combination of a plurality of gamma-aminopropyl trimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, gamma- (methacryloyloxy) propyl trimethoxysilane, gamma-mercaptopropyl trimethoxysilane and gamma-urea propyl trimethoxysilane;
a is described5Reinforcing filler, at least one or the combination of two fillers of fumed silica and light calcium carbonate is selected;
a is described6The catalyst is selected from dibutyltin dilaurate, dioctyltin dilaurate, stannous octoate, tetrabutyl titanate, tetraisobutyl titanate and tetraisopropyl titanateAt least one of (1);
b is1The viscosity of the alpha, omega-dihydroxy polydimethylsiloxane at 25 ℃ is 1000-;
b is4The surface of the gas phase white carbon black is modified by dimethyl dichlorosilane or hexamethyldisilazane, and the light calcium carbonate is treated by fatty acid and abietic acid surface modifiers.
3. The silicone rubber sealant according to claim 2, wherein the A, B has a volume mixing ratio of 4: 1; b is1The viscosity of the alpha, omega-dihydroxy polydimethylsiloxane was 3000mpa.s at 25 ℃.
4. A method of preparing the two-component dealcoholized silicone rubber sealant according to any of claims 1 to 3, wherein said silicone rubber sealant consists of A, B two components;
the preparation method of the component A comprises the following steps: mixing A in a certain proportion1、A2Uniformly mixing under the vacuum condition of-0.095 to-0.1 MPa for removing bubbles, and N2Adding A in turn under protection3Component A4Component A5Component A and6the component A can be prepared by stirring the components for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1MPa in each adding;
the preparation method of the component B comprises the following steps: mixing B in a certain proportion1、B2Uniformly mixing and de-bubbling under the condition that the vacuum degree is between 0.095 and 0.1MPa, and N2Adding B in turn under protection3、B4The component is added each time and stirred for 20min under the condition that the vacuum degree is-0.095 to-0.1 MPa, and finally the component B is prepared;
wherein,
A1100 parts of alpha, omega-dihydroxy polydimethylsiloxane;
A210-30 parts of simethicone;
A33-8 parts of dealcoholization type crosslinking agent;
A41-5 parts of a silane coupling agent;
A510-100 parts of reinforcing filler;
A60.1-0.6 parts of catalyst;
B1alpha, omega-dihydroxyl poly100 parts of dimethyl siloxane;
B21-2 parts of a surfactant, namely selecting nonylphenol polyoxyethylene ether;
B3.8-15 parts of deionized water;
B410-100 parts of reinforcing filler, and at least one or a combination of several fillers selected from fumed silica and light calcium carbonate.
5. The method for preparing a silicone rubber sealant according to claim 4, wherein said A is3Dealcoholization type crosslinking agent selected from at least one or more of methyltrimethoxysilane, vinyl trimethoxysilane, ethyl orthosilicate and partial hydrolysate thereof;
a is described4The silane coupling agent is at least one or a combination of a plurality of gamma-aminopropyl trimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma- (methacryloyloxy) propyl trimethoxysilane, gamma-mercaptopropyl trimethoxysilane and gamma-urea propyl trimethoxysilane;
a is described5Reinforcing filler, at least one or the combination of two fillers of fumed silica and light calcium carbonate is selected;
a is described6The catalyst is at least one of dibutyltin dilaurate, dioctyltin dilaurate, stannous octoate, tetrabutyl titanate, tetraisobutyl titanate and tetraisopropyl titanate;
b is1The viscosity of the alpha, omega-dihydroxy polydimethylsiloxane at 25 ℃ is 3000 mpa.s;
b is4The surface of the gas phase white carbon black is modified by dimethyl dichlorosilane or hexamethyldisilazane, and the light calcium carbonate is treated by fatty acid and abietic acid surface modifiers.
6. The preparation method of the silicone rubber sealant according to claim 5, wherein the component A is prepared by the following specific steps: uniformly mixing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000mpa.s at 25 ℃ and 20 parts of simethicone with viscosity of 500mpa.s under the condition of vacuum degree of-0.095 to-0.1 MPa, and removing bubbles; adding 4 parts of vinyl trimethoxy silane under the protection of nitrogen, stirring for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1MPa for end capping reaction, adding 4 parts of partial hydrolysate of ethyl orthosilicate under the protection of nitrogen, and stirring for 20min under the condition of vacuum degree of minus 0.095 to minus 0.1 MPa; adding a mixture of 2 parts of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane and 2 parts of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane under the protection of nitrogen, and stirring for 20min under the condition that the vacuum degree is-0.095 to-0.1 MPa; under the protection of nitrogen, sequentially adding 5 parts of fumed silica and 50 parts of light calcium carbonate, and stirring and dispersing under the vacuum degree of-0.095 to-0.1 MPa until the mixture is uniform and has no particles; adding 0.4 part of dibutyltin dilaurate under the protection of nitrogen, and stirring for 20min under the condition of vacuum degree of-0.095 to-0.1 MPa to obtain a glue;
the component B is prepared by the following specific steps: uniformly mixing 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 3000mpa.s at 25 ℃ and 1 part of nonylphenol polyoxyethylene ether under the condition of vacuum degree of-0.095 to-0.1 MPa, and defoaming; adding 10 parts of deionized water under the protection of nitrogen, and stirring for 20min under the vacuum degree of-0.095 to-0.1 MPa; and sequentially adding 3 parts of fumed silica and 40 parts of light calcium carbonate under the protection of nitrogen, and stirring and dispersing under the vacuum degree of-0.095 to-0.1 MPa until particles are uniformly discharged.
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| CN103805136A (en) * | 2013-12-11 | 2014-05-21 | 常熟市希诺包装制品有限公司 | Sealant |
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| CN104194195A (en) * | 2014-07-29 | 2014-12-10 | 安徽九子山塑业有限公司 | Flame-retardant high-reinforcement filler for PVC tubes and preparation method of flame-retardant high-reinforcement filler |
| CN106867443A (en) * | 2015-12-10 | 2017-06-20 | 江苏天辰新材料股份有限公司 | A kind of dealcoholysis condensed type double-component room temperature vulcanized silicone rubber building sealant and preparation method thereof |
| CN106221241A (en) * | 2016-08-31 | 2016-12-14 | 江苏天辰新材料股份有限公司 | A kind of medical dual composition addition type liquid silastic and preparation method thereof |
| CN108570304A (en) * | 2017-03-14 | 2018-09-25 | 北京天山新材料技术有限公司 | A kind of two-component silicone rubber bonding agent of wet and heat ageing resistant and preparation method thereof |
| CN110982448B (en) * | 2019-12-24 | 2021-02-02 | 广州市白云化工实业有限公司 | Tackifier, dealcoholized RTV (room temperature vulcanized) silicone rubber and preparation method thereof |
| CN111910165A (en) * | 2020-07-20 | 2020-11-10 | 上海空间电源研究所 | Exposed metal protection liquid and protection method in PECVD (plasma enhanced chemical vapor deposition) process |
| CN112063359A (en) * | 2020-07-29 | 2020-12-11 | 广东美的厨房电器制造有限公司 | Adhesive composition and bonding method |
| CN118240523B (en) * | 2024-04-27 | 2024-09-10 | 佛山市普力达科技有限公司 | Quick-curing variegated alcohol type silica gel and preparation method thereof |
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