CN115785892A - Silicone rubber sealant and preparation method thereof - Google Patents
Silicone rubber sealant and preparation method thereof Download PDFInfo
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- CN115785892A CN115785892A CN202211399472.XA CN202211399472A CN115785892A CN 115785892 A CN115785892 A CN 115785892A CN 202211399472 A CN202211399472 A CN 202211399472A CN 115785892 A CN115785892 A CN 115785892A
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- 239000000565 sealant Substances 0.000 title claims abstract description 45
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 37
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title description 5
- 229920002545 silicone oil Polymers 0.000 claims abstract description 44
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 31
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 24
- 229920000570 polyether Polymers 0.000 claims abstract description 24
- 229920001971 elastomer Polymers 0.000 claims abstract description 20
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 20
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 16
- 239000000945 filler Substances 0.000 claims abstract description 16
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 239000003086 colorant Substances 0.000 claims abstract description 5
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 5
- 238000004898 kneading Methods 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000006229 carbon black Substances 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- BTXFTCVNWMNXKH-UHFFFAOYSA-N NC1=CC=CC=C1.CCO[Si](C)(OCC)OCC Chemical compound NC1=CC=CC=C1.CCO[Si](C)(OCC)OCC BTXFTCVNWMNXKH-UHFFFAOYSA-N 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- IXQMGECVDWVOFK-UHFFFAOYSA-N dichloromethyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C(Cl)Cl IXQMGECVDWVOFK-UHFFFAOYSA-N 0.000 claims description 10
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 8
- BZQKBFHEWDPQHD-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-[2-(2,3,4,5,6-pentabromophenyl)ethyl]benzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br BZQKBFHEWDPQHD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 229910021485 fumed silica Inorganic materials 0.000 claims description 7
- 235000011837 pasties Nutrition 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 5
- FIAXCDIQXHJNIX-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-ethylbenzene Chemical compound CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br FIAXCDIQXHJNIX-UHFFFAOYSA-N 0.000 claims description 4
- FMWLUWPQPKEARP-UHFFFAOYSA-N bromodichloromethane Chemical compound ClC(Cl)Br FMWLUWPQPKEARP-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 125000004435 hydrogen atom Polymers [H]* 0.000 claims 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- 239000010690 paraffinic oil Substances 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 229920001296 polysiloxane Polymers 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 150000004756 silanes Chemical class 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 7
- 230000009974 thixotropic effect Effects 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000005662 Paraffin oil Substances 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- 229920002367 Polyisobutene Polymers 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229940083037 simethicone Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 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 description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 2
- 229940008841 1,6-hexamethylene diisocyanate Drugs 0.000 description 1
- RLTQHDXGJNBSEC-UHFFFAOYSA-N CCCC(=O)CC(=O)OC(C)C.CCCC(=O)CC(=O)OC(C)C Chemical compound CCCC(=O)CC(=O)OC(C)C.CCCC(=O)CC(=O)OC(C)C RLTQHDXGJNBSEC-UHFFFAOYSA-N 0.000 description 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- WIEGKKSLPGLWRN-UHFFFAOYSA-N ethyl 3-oxobutanoate;titanium Chemical compound [Ti].CCOC(=O)CC(C)=O WIEGKKSLPGLWRN-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 1
- 239000004589 rubber sealant Substances 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 239000012945 sealing adhesive Substances 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to a silicone rubber sealant, comprising: 90-120 parts of hydroxyl-terminated polydimethylsiloxane, 8-14 parts of plasticizer, 8-15 parts of extending filler, 3-5 parts of polyether modified hydrogen-containing silicone oil, 12-20 parts of low-density filler, 12-18 parts of thixotropic agent, 0.5-1.5 parts of colorant and 8-10 parts of polyfunctional group silane coupling agent system. The polydimethylsiloxane chain segment forms orientation on the surface, so that the thixotropy of the sealant is endowed. In addition, the modification of the hydrogen-containing silicone oil introduces a polyether chain segment which can be dissolved in rubber components, and after the polyether modified hydrogen-containing silicone oil is added, a layer of polysiloxane film can be formed on the surfaces of rubber and air, so that the influence of internal flow caused by surface tension change in the drying process on the surface can be reduced, the thixotropy of the surface is further improved, and the sealing quality is good. The added multifunctional silane coupling agent catalytic system is formed by copolymerizing three silanes with different structures, and excellent bonding universality and good curing speed can be obtained by matching various functional groups of different types.
Description
Technical Field
The invention relates to the technical field of silicone rubber, in particular to a silicone rubber sealant and a preparation method thereof.
Background
The single-component silicone rubber sealant is prepared by taking silicone rubber as a basic raw material, adding a filler and a cross-linking agent and matching. The single-component silicone rubber sealant has excellent adhesion to most base materials, excellent electrical insulation and chemical stability, good adhesion to various metal and non-metal materials and no corrosion. Is particularly suitable for the industries of electronic appliances, photovoltaics and the like. However, because the molecular weight of RTV silicone rubber is lower, the prepared sealant is easy to flow, namely, the thixotropy is poorer. In the application process of the silicone rubber sealant, when the silicone rubber sealant is operated on a vertical surface and a face upwards, the sealant is easy to receive the action of gravity, and the sealant overflows from the bottom surface of a structural member and drips to cause incomplete sealing and loss of effect. In the prior art, the thixotropy which is a process factor influencing the quality of the application process of the silicone rubber sealant is not paid sufficient attention. The thixotropy index directly influences the sealing effect and is related to the quality problem of the sealing application process.
The prior patents CN104513645, CN113956840, CN112300749, CN108624274, etc. disclose various silicone rubber sealants and preparation methods, but most of them use calcium carbonate systems as main material, and have poor thixotropic properties and are easy to sag, resulting in poor quality in application process. Therefore, the improvement of the thixotropy of the single-component silicon rubber sealant is particularly important for the application of the sealant.
Disclosure of Invention
In order to overcome the defects of the prior art, in particular to solve the problem that the conventional sealant in the prior art is poor in thixotropy and easy to sag, the invention provides a single-component silicone rubber sealant with excellent thixotropy.
In order to realize the purpose, the technical scheme provided by the invention is as follows: a silicone rubber sealant comprising by weight: 90-120 parts of hydroxyl-terminated polydimethylsiloxane, 8-14 parts of plasticizer, 8-15 parts of extending filler, 3-5 parts of polyether modified hydrogen-containing silicone oil, 12-20 parts of low-density filler, 12-18 parts of thixotropic agent, 0.5-1.5 parts of colorant and 8-10 parts of polyfunctional group silane coupling agent system.
Further, the number average molecular weight of the hydroxyl-terminated polydimethylsiloxane is between 1000 and 10000, and the dynamic viscosity is 100 to 10000cp at 25 ℃;
further, the synthesis method of the polyether modified hydrogen-containing silicone oil comprises the following steps: mixing allyl polyether and ethyl hydrogen-containing silicone oil, adding a catalyst, and reacting in an inert gas atmosphere to obtain polyether modified hydrogen-containing silicone oil;
the catalyst can adopt chloroplatinic acid, and the dosage of the catalyst is 0.2 to 0.4 percent of the total mass of the allyl polyether and the ethyl hydrogen-containing silicone oil; preferably, the allyl polyether and the ethyl hydrogen silicone oil are mixed according to a ratio of 1: (0.8-1.2), more preferably 1:1.
further, in the synthetic reaction of the modified hydrogen-containing silicone oil, the reaction temperature is controlled to be 80-100 ℃, and the reaction time is 4-6 hours.
Further, the multifunctional silane coupling agent system comprises one or more of ethyl orthosilicate, dichloromethyl triethoxysilane, aniline methyl triethoxysilane, aminopropyl triethoxysilane or their derivatives.
Further, the plasticizer includes one or more of paraffin oil, simethicone, naphthene base oil or derivatives thereof.
Further, the extending filler comprises one or more of pentabromoethylbenzene, dichlorobromomethane, decabromodiphenylethane, or derivatives thereof.
Further, the low-density filler comprises one or more of hollow glass microspheres, diatomite, activated calcium carbonate, fumed silica, carbon black or derivatives thereof.
The invention also provides a preparation method of the silicone rubber sealant, which is characterized by comprising the following steps:
s1, stirring and kneading hydroxyl-terminated polydimethylsiloxane, a plasticizer, an incremental filler, modified silicone oil, a low-density filler, a thixotropic agent and a colorant, then starting a vacuum pump to remove residual moisture, and continuously and uniformly kneading to obtain a pasty rubber material;
and S2, cooling the paste rubber prepared in the step S1, adding a polyfunctional silane coupling agent system, filling inert gas, and continuously kneading under a normal pressure state to prepare the silicone rubber sealing agent.
Further, the kneading temperature is controlled at 110-130 ℃ in the step S1; in the step S2, the kneading temperature is controlled to be 40-50 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) The polydimethylsiloxane chain segment forms orientation on the surface, so that the sealing adhesive is endowed with thixotropy. The modified hydrogen-containing silicone oil is modified, the polyether chain segment is introduced and can be dissolved in the rubber component, and after the modified hydrogen-containing silicone oil is added, a layer of polysiloxane film can be formed on the surfaces of rubber and air, so that the influence of internal flow caused by surface tension change in the drying process on the surfaces can be reduced, the thixotropy of the surfaces can be further improved, and the sealing quality is good.
(2) The polysiloxane polymer adopted by the invention has physiological inertia, good chemical stability, electrical insulation and weather resistance. The addition of the low-density filler reduces the density of the sealant, so that the whole dispersion is more uniform, the thixotropy of the sealant is improved, and the sealant does not sag.
(3) The multifunctional silane coupling agent catalyst system added into the silicone rubber sealant can obtain excellent bonding universality and good curing speed. The silane coupling agent system is formed by copolymerizing three silanes with different structures, contains groups such as chloro groups, anilino groups, alkyl groups, multi-alkoxy groups and the like, is matched with various functional groups of different types after being added, and the multi-alkoxy groups can quickly generate crosslinking reaction with base glue in the presence of a small amount of water vapor, so that the deep curing speed of a product is improved.
(4) The product of the invention has excellent bonding and sealing performance, and can realize good bonding and sealing for various universal metal and plastic base materials. In addition, the product of the invention also has good deep curing performance, can shorten the curing time and improve the production efficiency, and can be applied to occasions requiring high-efficiency sealing assembly and other occasions requiring rapid curing.
Detailed Description
The present invention is illustrated below by way of specific examples, which are provided primarily for the purpose of illustrating the principles, features and advantages of the invention, and are not to be construed as limited to the examples described below, which may be further modified without departing from the principles of the experiment.
Example 1:
100 parts of hydroxyl-terminated polydimethylsiloxane, 10 parts of dimethyl silicone oil, 8 parts of decabromodiphenylethane, 4 parts of modified silicone oil, 15 parts of hollow glass microspheres, 15 parts of fumed silica, 1 part of carbon black, 1 part of ethyl orthosilicate, 4 parts of dichloromethyl triethoxysilane, 2 parts of aniline methyl triethoxysilane and 2 parts of aminopropyl triethoxysilane.
(1) Modification of hydrogen-containing silicone oil: in a four-neck flask equipped with a thermometer, stirrer, spherical condenser, the ratio of 1: adding allyl polyether and ethyl hydrogen-containing silicone oil according to the mass ratio of 1, controlling the reaction temperature to be 93 ℃ under the protection of nitrogen, adding chloroplatinic acid, reacting for 6 hours, cooling, and discharging to obtain the polyether modified hydrogen-containing silicone oil.
(2) Adding hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil, decabromodiphenylethane, polyether modified hydrogen-containing silicone oil, hollow glass beads, white carbon black and carbon black into a material cavity of a vacuum kneading machine, adjusting the rotating speed of blades of the kneading machine, stirring and kneading, starting a vacuum pump, maintaining the temperature at 110 ℃, removing residual moisture, and continuously and uniformly kneading to obtain a paste-shaped rubber material;
(3) And cooling the paste rubber material prepared in the step to 50 ℃, adding tetraethoxysilane, dichloromethyl triethoxysilane, aniline methyl triethoxysilane and aminopropyl triethoxysilane, introducing nitrogen, continuously kneading under a normal pressure state, and uniformly dispersing liquid components in a paste rubber material system to prepare the silicone rubber sealant.
Example 2:
110 parts of hydroxyl-terminated polydimethylsiloxane, 12 parts of naphthenic oil, 10 parts of decabromodiphenylethane, 5 parts of dichlorobromomethane, 5 parts of polyether modified hydrogen-containing silicone oil, 10 parts of hollow glass beads, 10 parts of fumed silica, 1 part of carbon black, 1 part of ethyl orthosilicate, 3 parts of dichloromethyl triethoxysilane, 1.2 parts of aniline methyl triethoxysilane and 1.8 parts of methyl triethoxysilane.
(1) Modification of hydrogen-containing silicone oil: in a four-neck flask equipped with a thermometer, stirrer, spherical condenser, the ratio of 1: adding allyl polyether and ethyl hydrogen-containing silicone oil according to the mass ratio of 0.8, controlling the reaction temperature at 90 ℃ under the protection of nitrogen, adding chloroplatinic acid, reacting for 6 hours, cooling, and discharging to obtain the polyether modified hydrogen-containing silicone oil.
(2) Adding hydroxyl-terminated polydimethylsiloxane, naphthenic oil, decabromodiphenylethane, dichlorobromomethane, polyether modified hydrogen-containing silicone oil, hollow glass beads, white carbon black and carbon black into a material cavity of a vacuum kneading machine, adjusting the rotating speed of blades of the kneading machine, stirring and kneading, starting a vacuum pump, maintaining the temperature at 110 ℃, removing residual moisture, and continuously and uniformly kneading to obtain a pasty rubber material;
(3) And cooling the paste rubber material prepared in the step to 40 ℃, adding tetraethoxysilane, dichloromethyl triethoxysilane, aniline methyl triethoxysilane and methyl triethoxysilane, introducing nitrogen, continuously kneading under a normal pressure state, and uniformly dispersing liquid components in a paste rubber material system to prepare the silicone rubber sealant.
Example 3
120 parts of hydroxyl-terminated polydimethylsiloxane, 8 parts of paraffin oil, 15 parts of pentabromoethylbenzene, 5 parts of polyether modified hydrogen-containing silicone oil, 10 parts of diatomite, 6 parts of activated calcium carbonate, 2 parts of ethyl orthosilicate, 3 parts of dichloromethyl triethoxysilane, 2 parts of aniline methyl triethoxysilane and 3 parts of aminopropyl triethoxysilane.
(1) Modification of hydrogen-containing silicone oil: in a four-neck flask equipped with a thermometer, stirrer, spherical condenser, the ratio of 1: and 1.2, adding allyl polyether and ethyl hydrogen-containing silicone oil, controlling the reaction temperature at 95 ℃ under the protection of nitrogen, adding chloroplatinic acid, reacting for 6 hours, cooling, and discharging to obtain the polyether modified hydrogen-containing silicone oil.
(2) Adding hydroxyl-terminated polydimethylsiloxane, paraffin oil, pentabromoethyl benzene, polyether modified hydrogen-containing silicone oil, diatomite, white carbon black and carbon black into a material cavity of a vacuum kneading machine, adjusting the rotating speed of blades of the kneading machine, stirring and kneading, starting a vacuum pump, maintaining the temperature at 110 ℃, removing residual moisture, and continuously and uniformly kneading to obtain a pasty rubber material;
(3) Cooling the paste rubber material prepared in the above steps to 45 ℃, adding tetraethoxysilane, dichloromethyl triethoxysilane, aniline methyl triethoxysilane and aminopropyl triethoxysilane, introducing nitrogen gas, continuously kneading under normal pressure, and uniformly dispersing liquid components in the paste rubber material system to obtain the silicone rubber sealant.
Comparative example 1
The sealant was prepared according to the method of patent CN 108624274:
(1) Aminopropyl trimethoxysilane, gamma-glycidoxypropyl trimethoxysilane and 1,6-hexamethylene diisocyanate in a molar ratio of 1:2:2, mixing and reacting for 110h at 50 ℃ to obtain the tackifier.
(2) Putting 100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane, 10 parts by weight of simethicone, 120 parts by weight of nano calcium carbonate and 8 parts by weight of white slurry into a high-speed dispersion planetary machine for stirring, simultaneously heating to 120 ℃, and carrying out vacuum dehydration for 3 hours under-0.1 MPa to obtain a dehydrated mixed material; and then cooling the mixed material to below 50 ℃, adding 8 parts by weight of methyltrimethoxysilane and 6 parts by weight of ethyl acetoacetate titanium compound, uniformly stirring under a vacuum condition, adding 0.5 part by weight of tackifier, continuously and uniformly stirring under the vacuum condition, and discharging to obtain the dealcoholized silicone rubber sealant.
Comparative example 2
The sealant was prepared according to the method of patent CN 113956840: alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 6000mpa.s and dimethyl silicone oil with the viscosity of 500mpa.s are selected according to the following components in proportion:
A. 100 parts of alpha, omega-dihydroxy dimethyl silicone polymer
B. End-capping reagent 1.8 parts
C. 0.05 part of trifluoromethanesulfonic acid
D. 10 parts of dimethyl silicone oil
E. 100 portions of calcium carbonate and 12 portions of fumed silica
F. 4 parts of vinyl trimethoxy silane
G. 0.8 part of gamma-aminoethyl aminopropyltrimethoxysilane
H. 0.8 part of tetraisopropyl titanate
General formula (N) 2 Adding A, B, C with the viscosity and the parts into a reaction kettle under protection, stirring for 18min at room temperature, then stirring for 10 min under the vacuum condition of-0.1 MPa to remove micromolecules, adding D, E, stirring for 30 min under the vacuum condition of-0.1 MPa, uniformly mixing, sequentially adding F, G, H, and stirring for 30 min under the vacuum condition of-0.1 MPa until bubbles are uniformly removed, thus obtaining the dealcoholized room temperature vulcanized silicone rubber sealant.
Comparative example 3
The sealant was prepared according to the method of patent CN 104513645: alpha, omega-divinyl dimethyl silicone with the viscosity of 5000mpa & s, dimethyl silicone oil with the viscosity of 100mpa & s, silane modified polyisobutylene with the molecular weight of 10000 and vinyl siloxane chelate of chloroplatinic acid are selected as platinum catalysts, and the specific component proportion is as follows:
A. 100 parts of alpha, omega-divinyl polydimethylsiloxane;
B. 6 parts of hydrido trimethoxy silane;
C. 1.5 parts of a platinum catalyst;
D. 10 parts of dimethyl silicone oil;
E. 25 parts of silane modified polyisobutylene;
F. 5 parts of vinyl trimethoxy silane;
G. 1.5 parts of aminopropyl trimethoxy silane;
H. 80 parts of calcium carbonate and 8 parts of fumed silica;
I. 3 parts of diisopropyl bis (ethyl acetoacetate) titanate.
N 2 Adding A, B, C into the reaction kettle under protection, stirring uniformly, heating to 50 ℃, and adding N 2 Continuously stirring for reaction for 5 hours under protection, then stirring for 30-60 minutes under the vacuum condition of-0.1 MPa to remove small molecules, cooling to below 40 ℃, adding the D, E, H component, stirring for 30 minutes under the vacuum condition of-0.1 MPa to be uniformly mixed, then sequentially adding the F, G, I component, and stirring for 30 minutes under the vacuum condition of-0.1 MPa respectively until uniform bubbles are not generated.
Comparative example 4
100 parts of hydroxyl-terminated polydimethylsiloxane, 10 parts of dimethyl silicone oil, 8 parts of decabromodiphenylethane, 4 parts of modified silicone oil, 15 parts of hollow glass microspheres, 15 parts of fumed silica, 1 part of carbon black, 1 part of ethyl orthosilicate, 4 parts of dichloromethyl triethoxysilane, 2 parts of aniline methyl triethoxysilane and 2 parts of aminopropyl triethoxysilane.
(2) Adding hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil (unmodified), decabromodiphenylethane, modified silicone oil, hollow glass microspheres, white carbon black and carbon black into a material cavity of a vacuum kneading machine, adjusting the rotating speed of blades of the kneading machine, stirring and kneading, starting a vacuum pump, maintaining the temperature at 110 ℃, removing residual moisture, and continuously and uniformly kneading to obtain a pasty rubber material;
(3) And cooling the paste rubber material prepared in the step to 50 ℃, adding tetraethoxysilane, dichloromethyl triethoxysilane, aniline methyl triethoxysilane and aminopropyl triethoxysilane, introducing nitrogen, continuously kneading under a normal pressure state, and uniformly dispersing liquid components in a paste rubber material system to prepare the silicone rubber sealant.
Thixotropic index was determined by comparative testing of product properties using the thixotropic ring method for the silicone rubber sealants of the above examples and comparative examples, wherein the thixotropic index is expressed as the ratio of the viscosity of 5.6 r min to the viscosity of 65r/min in the non-newtonian fluid such as an adhesive, namely: it = η 5.6/η 65.
TABLE 1 thixotropic index data for examples and comparative examples
| Performance of | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Thixotropic index | 3.6 | 3.2 | 3.5 | 2 | 1.8 | 2 | 2.2 |
TABLE 2 thixotropic index data adhesion data for examples and comparative examples
As can be seen from tables 1 to 2, the silicone rubber sealant provided in embodiments 1 to 3 of the present invention has excellent adhesion, and the thixotropy is greatly improved compared with similar products in the market, thereby solving the problem of poor quality in the application process due to poor thixotropy and easy sagging in the prior art.
Claims (10)
1. A silicone rubber sealant characterized by comprising by weight: 90-120 parts of hydroxyl-terminated polydimethylsiloxane, 8-14 parts of plasticizer, 8-15 parts of incremental filler, 3-5 parts of polyether modified hydrogen-containing silicone oil, 12-20 parts of low-density filler, 12-18 parts of thixotropic agent, 0.5-1.5 parts of colorant and 8-10 parts of polyfunctional silane coupling agent system.
2. The silicone rubber sealant according to claim 1, wherein the hydroxyl terminated polydimethylsiloxane has a number average molecular weight of 1000 to 10000 and a kinematic viscosity of 100 to 10000cp at 25 ℃.
3. The silicone rubber sealant according to claim 1, wherein the polyether-modified hydrogen-containing silicone oil is synthesized by the following method: mixing allyl polyether and ethyl hydrogen-containing silicone oil, adding a catalyst, and reacting in an inert gas atmosphere to obtain the polyether modified hydrogen-containing silicone oil.
4. The silicone rubber sealant according to claim 1, wherein in the synthesis reaction of the polyether-modified hydrogen-containing silicone oil, the reaction temperature is controlled to be 80-100 ℃ and the reaction time is controlled to be 4-6 hours.
5. The silicone rubber sealant according to claim 1, wherein the multifunctional silane coupling agent system comprises one or more of ethyl orthosilicate, dichloromethyl triethoxysilane, aniline methyl triethoxysilane, aminopropyl triethoxysilane, or derivatives thereof.
6. The silicone rubber sealant according to claim 1, wherein the plasticizer comprises one or more of paraffinic oil, dimethylsilicone oil, naphthenic oil, or derivatives thereof.
7. The silicone rubber sealant according to claim 1, wherein the extending filler comprises one or more of pentabromoethylbenzene, dichlorobromomethane, decabromodiphenylethane, or derivatives thereof.
8. The silicone rubber sealant according to claim 1, wherein the low-density filler comprises one or more of hollow glass microspheres, diatomaceous earth, activated calcium carbonate, fumed silica, carbon black, or derivatives thereof.
9. The method for producing the silicone rubber sealant according to any one of claims 1 to 8, characterized by comprising the steps of:
s1, stirring and kneading hydroxyl-terminated polydimethylsiloxane, a plasticizer, an incremental filler, modified silicone oil, a low-density filler, a thixotropic agent and a colorant, then starting a vacuum pump to remove residual moisture, and continuously and uniformly kneading to obtain a pasty rubber material;
and S2, cooling the pasty rubber material prepared in the step S1, adding a polyfunctional group silane coupling agent system, filling inert gas, and continuously kneading under a normal pressure state to prepare the silicone rubber sealant.
10. The method for producing a silicone rubber sealant according to claim 9, wherein the kneading temperature in step S1 is controlled at 110 to 130 ℃; in the step S2, the kneading temperature is controlled to be 40-50 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163908A (en) * | 2017-07-18 | 2017-09-15 | 杭州之江有机硅化工有限公司 | One kind is used for automobile lamp and assembles sealed two-component silicone rubber sealant and preparation method thereof |
| CN111718486A (en) * | 2020-06-22 | 2020-09-29 | 湖北回天新材料股份有限公司 | Thixotropic agent and two-component silicone sealant containing same |
| CN113337122A (en) * | 2021-06-28 | 2021-09-03 | 湖南航天三丰科工有限公司 | Dealcoholized room temperature curing silicone rubber with ultra-long storage life and preparation method thereof |
| CN113429928A (en) * | 2021-06-21 | 2021-09-24 | 湖南航天三丰科工有限公司 | Self-curing silicone rubber composite material and preparation process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163908A (en) * | 2017-07-18 | 2017-09-15 | 杭州之江有机硅化工有限公司 | One kind is used for automobile lamp and assembles sealed two-component silicone rubber sealant and preparation method thereof |
| CN111718486A (en) * | 2020-06-22 | 2020-09-29 | 湖北回天新材料股份有限公司 | Thixotropic agent and two-component silicone sealant containing same |
| CN113429928A (en) * | 2021-06-21 | 2021-09-24 | 湖南航天三丰科工有限公司 | Self-curing silicone rubber composite material and preparation process thereof |
| CN113337122A (en) * | 2021-06-28 | 2021-09-03 | 湖南航天三丰科工有限公司 | Dealcoholized room temperature curing silicone rubber with ultra-long storage life and preparation method thereof |
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