CN103642452A - Method for preparing silicone sealant - Google Patents
Method for preparing silicone sealant Download PDFInfo
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- CN103642452A CN103642452A CN201310615283.6A CN201310615283A CN103642452A CN 103642452 A CN103642452 A CN 103642452A CN 201310615283 A CN201310615283 A CN 201310615283A CN 103642452 A CN103642452 A CN 103642452A
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- silicone sealant
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- 239000004590 silicone sealant Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 35
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 16
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 239000003921 oil Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 5
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000003292 glue Substances 0.000 claims description 52
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 26
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 25
- 229910000077 silane Inorganic materials 0.000 claims description 23
- 238000002360 preparation method Methods 0.000 claims description 21
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 18
- 239000004593 Epoxy Substances 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 17
- 239000001301 oxygen Substances 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 17
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 17
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 16
- 229920002554 vinyl polymer Polymers 0.000 claims description 16
- 229920002545 silicone oil Polymers 0.000 claims description 15
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 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 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 241000276489 Merlangius merlangus Species 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 6
- -1 polydimethylsiloxane Polymers 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000006229 carbon black Substances 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 238000004898 kneading Methods 0.000 abstract 1
- 239000002562 thickening agent Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 15
- 150000004756 silanes Chemical class 0.000 description 14
- 241001417490 Sillaginidae Species 0.000 description 10
- 238000005703 Whiting synthesis reaction Methods 0.000 description 10
- 229920001296 polysiloxane Polymers 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 239000004902 Softening Agent Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 239000000565 sealant Substances 0.000 description 4
- 239000013464 silicone adhesive Substances 0.000 description 4
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 229920005601 base polymer Polymers 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 1
- 239000004589 rubber sealant Substances 0.000 description 1
- 238000013040 rubber vulcanization Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method for preparing silicone sealant. The method comprises the following steps: adding alpha,omega-dyhydroxy polydimethylsiloxane, filler and dimethyl silicon oil into a vacuum kneading machine, vacuuming, heating and mixing for 2-5 hours; stopping heating, introducing nitrogen to change the vacuum state, adding a silane coupling agent, mixing for 0.5-1 hour at the vacuum degree of -0.06 to -0.1Mpa, introducing nitrogen to change the vacuum state; sealing and cooling to room temperature, subsequently transferring into a stirring machine, adding a cross-linking agent, a thickening agent and a catalyst, vacuuming, and uniformly stirring and mixing so as to obtain the silicone sealant. According to a product of the silicone sealant, the addition amount of the filler is increased, the product stability and the surface smoothness are improved, the thixotropy and the deep curing are also improved, the curing homogeneity is good, the tensile strength, the elasticity and the cohesiveness are greatly improved, expensive white carbon black can be replaced, the filling amount is large, the curing time is short, the construction efficiency is improved, the process is simple and feasible, the production cost is low, and good economic benefits and social benefits are achieved.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of silicone sealant, particularly a kind of preparation method of silicone sealant.
Background technology
Silicone sealant is to take a kind of sealing material that hydroxy-end capped polysiloxane makes as base-material, belong to silicone based product, after first curing cross-linked process is the moisture in linking agent contact atmosphere, there is rapidly hydrolysis reaction in the functional group of hydrolyzable, generates silanol.The Si-OH base of its silanol and 107 glue
si-OH base is sent out condensation reaction, forms three-dimensional netted Si-O-Si skeleton structure, becomes elastomerics.Silicone sealant is easy to use, cured glue body volumetric shrinkage is little, good airproof performance, its bonding force is strong, and tensile strength is large, and there is good ageing resistance, resistant of high or low temperature, resistance to electrical insulating property, flexible resistance, weathering resistance etc., be widely used in the new high-tech industry fields such as building, automobile, machinery, electronics, weaving, using value is very high.In recent years, China's silicone sealant industry has been stepped into development motorway.
Single-component silicone fluid sealant can be divided into three kinds of high-modulus, middle modulus and low modulus according to the size of modulus after solidifying completely.Middle modulus silicone sealant 100% stress at definite elongation is 0.4～0.6MPa, and maximum tensile stress is 0.75～2.0MPa, maximum elongation rate 300～750%.Middle modulus silicone sealant purposes is wider, is also one of seal gum that in silicone sealant, consumption is maximum, and it both can be used as general bonding, also can make the special bondings such as structural.
Single-component silicone fluid sealant can be divided into two kinds of Aci-Jel and neutral gums according to character, and because the cementability of sealing neutral silicone resin is not as acetic acid type, thereby formula often adds silane coupling agent to carry out modification tackify.Silane coupling agent is one to have the silicoorganic compound of two kinds of different chemical character functional groups roughly the same time, it is as the tackifier of silicone sealant for building, be used for improving the adhesiveproperties to material surface, can also improve the wettability of colloid, make itself and adherend fully bonding, thereby raising bonding strength, and improve shock resistance, stripping strength of glue etc.
The development of sealing neutral silicone resin series product is well afoot also, a lot of products are put on market, not only meet the ever-increasing demand of construction industry, and promoted double glazing, glass curtain wall, out-hung panel and metal frame adhesive structure etc. to build the development of product innovation, new texture, new technology.The leading manufacturing enterprise of domestic silicone building sealant has carried out the research and development of series product on the basis of pilot scale production technology of introducing national organosilicon engineering center neutral silicone building sealant, obtains impressive achievement.
Patent CN 102443375 A disclose a kind of preparation method of one-component oxime transparent silicone adhesive, before it is characterized in that tackifier and catalyzer are placed on to aerosil, add preparation, wherein used more cheap white oil as softening agent, colloid modulus is reduced, easy oil impregnate, some bonding substrates is brought to pollution, and reduced cohesiveness etc.
Patent CN 103072216 A disclose continuous production method and the device of a kind of acidity and neutral transparent silicone seal gum, by 107 glue, the first auxiliary agent, white oil and silicon oil quantitative feed mix, disperse and vacuumize after obtain mixing with white carbon black again after liquid material, two screw machines have wherein been used, equipment power consumption is larger, the white oil adding can reduce adhesive property, and some base material is had to pollution.
Patent CN 102898838 A disclose a kind of nano modification electronics silicone adhesive and preparation method thereof, its preparation method is that polymkeric substance and softening agent are first added in vacuum planetary mixer, and then add successively filler and various auxiliary agent to make, this patent of invention is directly at the various materials of planet stirrer for mixing, not heating, cause course of processing filler can not disperse well in polymkeric substance, the silicone adhesive colloid of preparation is not evenly with fine and smooth.
Patent CN 101570680 A disclose a kind of high-temperature resistant and expediting setting dealcoholized type room temperature vulcanized silicone rubber adhesive and preparation method thereof, wherein by hydroxyl-terminated injecting two methyl siloxane, after aerosil and titanium dioxide premix, add hydroxyl treatment agent, tackifier, catalyzer and linking agent make, the filler that this patent of invention is selected is aerosil and titanium dioxide, in the course of processing, be prone to base-material retrogradation situation, and surface drying excessive velocities, in glue, easily produce bubble, space, it is just completely curing that glue does not penetrate into substrate surface completely, so there will be not good state with substrate bonding, and filler is expensive, cost is higher.
Patent CN 101768361 A disclose a kind of method that improves room temperture rubber vulcanization mechanical property, and in 80～140 ℃, by α, alpha, omega-dihydroxy polydimethyl siloxane and filler and titanic acid ester are carried out vacuum hydro-extraction and stirred after 0.5～3h as base-material.This invention, by siloxanes and the direct hybrid reaction of titanic acid ester, causes the generation on viscosity peak, and impact generates the overall performance of rubber.
Patent CN 102417732 A disclose a kind of preparation method of silicone adhesive, the premix in screw extrusion press by 107 silicon rubber base-materials and linking agent wherein, add again filler to mix, finally add softening agent, coupling agent, catalyzer to vacuumize dispersion, mixing, stir and degassed making.Another patent CN 101565596 A disclose a kind of neutral silicone weather resistant glue formula and preparation technology thereof, patent CN 102757647 A disclose a kind of single-component catalysis dealcoholizing-type RTV silicon rubber sealant and preparation method thereof, these patented technologies all by base polymer and filler in vacuum kneader after blend dehydration, at room temperature, linking agent, thickening material and softening agent are added in high speed dispersor to vacuumize to stir with base glue and make.
In more than existing, in the making method of silicone sealant, all do not have in base glue and first base polymer, filler and coupling agent are heated and vacuumize premix, then add each auxiliary agent to prepare the method for silicone sealant when the room temperature in base glue.Through retrieval, relevant document is also there are no adopting this method to prepare the report of silicone sealant.
Summary of the invention
The present invention seeks to overcome the deficiency of more above-mentioned technology, provide a kind of and in base glue, utilize that waste heat adds that silane coupling agent prepares that cohesiveness is strong, good stability, base adhesive capacity are less and controlled, easy and simple to handle, power consumption less, the preparation method of modulus silicone sealant in low cost with low cost.
Concrete technical scheme of the present invention is as follows:
A preparation method for silicone sealant, comprises following steps:
(1) by α, alpha, omega-dihydroxy polydimethyl siloxane, filler, dimethyl silicone oil add in vacuum kneader, vacuumize and add hot milling 2～5h;
(2) stop heating, pass into nitrogen and remove vacuum, add appropriate silane coupling agent, mixing 0.5～1h obtains base glue, and it is-0.06～-0.1MPa that mixing process keeps vacuum tightness;
(3) pass into nitrogen and remove vacuum, move into stirrer in after the base glue sealing obtaining is cooled to room temperature in step (2), add linking agent, tackifier, catalyzer, vacuumize, be uniformly mixed and make single-component ketoxime removing type silicone sealant.
α described in above step (1), alpha, omega-dihydroxy polydimethyl siloxane viscosity is more than one in 10000～300000cP; Described filler is to be 20～35m through surface treatment specific surface area
2the active nano-calcium carbonate of/g and a small amount of coarse whiting; Described dimethyl-silicon oil viscosity is more than one in 350～12500cP; Described a small amount of coarse whiting is active nano-calcium carbonate used 5～35%;
Above-described α, the quality proportioning of alpha, omega-dihydroxy polydimethyl siloxane, filler, methyl-silicone oil is 100: 80～150: 0.05～8;
It is 70～140 ℃ that vacuumizing described in above step (1) adds thermal control temperature, and vacuum tightness is-0.06～-0.1MPa.
Silane coupling agent described in above step (2) comprises more than one in γ-aminopropyl triethoxysilane, γ-(2.3-epoxy the third oxygen) propyl trimethoxy silicane, composite dry silane, vinyl tributyl ketoximyl silane, its consumption is α, 0.02～2.00% of alpha, omega-dihydroxy polydimethyl siloxane and filler total mass.
Stirrer described in above step (3) is high speed dispersion planetary mixer, mixing speed 100～1000r/min, churning time 30～120min; Described vacuumize that to control vacuum tightness be-0.06～-0.1MPa.
Linking agent described in above step (3) is methyl tributanoximo silane; Described tackifier be vinyl tributyl ketoximyl silane, γ-aminopropyl triethoxysilane and γ-(2.3-epoxy the third oxygen) propyl trimethoxy silicane more than one; Described catalyzer is wherein a kind of of dibutyl tin laurate and stannous octoate.
The quality proportioning of the linking agent described in above step (3), tackifier, catalyzer is 10:1～4:0.05～0.15.
Advantage of the present invention and beneficial effect:
1, the present invention can regulate and control base adhesive capacity by change silane coupling agent add-on in base glue, particularly add composite dry silane, not only can improve the addition of filler, increase product stability and surface smoothness, and thixotropy and deep layer are solidified and also had remarkable help, curing homogeneity is good, and product tensile strength, elasticity and cohesiveness power are significantly improved.
2, the present invention replaces expensive white carbon black with surface treated nano-calcium carbonate, and loading level is large, and the products solidifying time obviously accelerates, and can improve operating efficiency.
3, the present invention first heats base glue base polymer, filler and coupling agent to vacuumize premix, then carries out crosslinking reaction, technique simple possible, and production cost is low, has good economic benefit and social benefit.
embodiment:
Below by specific embodiment, the present invention is done further and set forth, by the α of viscosity 10000～300000cP, alpha, omega-dihydroxy polydimethyl siloxane, specific surface area are 20～35m
2the active nano-calcium carbonate filler of/g and quality are that the coarse whiting of active nano-calcium carbonate 5～35%, the quality proportioning that viscosity is 350～12500cP dimethyl silicone oil add in vacuum kneader by 100: 80～150: 0.05～8, controlling temperature is 70～140 ℃, and vacuum tightness is the mixing 2～5h of-0.06～-0.1MPa, stop heating, pass into nitrogen and remove vacuum, add α, 0.02～2.00% γ-aminopropyl triethoxysilane, γ-(2.3-epoxy the third oxygen) propyl trimethoxy silicane, composite dry silane, vinyl tributyl ketoximyl silane silane coupling agent of alpha, omega-dihydroxy polydimethyl siloxane and filler total mass, mixing 0.5～1h obtains base glue, and it is-0.06～-0.1MPa that mixing process keeps vacuum tightness, pass into nitrogen and remove vacuum, after being cooled to room temperature, the sealing of base glue moves in high speed dispersion planetary mixer, adding quality is the methyl tributanoximo silane linking agent of base glue 2～6%, quality is the vinyl tributyl ketoximyl silane of base glue 0.2～1.5%, γ-aminopropyl triethoxysilane and γ-(2.3-epoxy the third oxygen) propyl trimethoxy silicane tackifier, quality is dibutyl tin laurate or the stannous octoate catalyst of base glue 0.04～0.15%, rotating speed 100～1000r/min, churning time 30～120min, controlling vacuum tightness is that-0.06～-0.1MPa vacuumizes, be uniformly mixed and make single-component ketoxime removing type silicone sealant, specific embodiment is as follows:
embodiment 1
By the α of 50000cP, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes, specific surface area are 35m
24 parts of 120 parts of the active nano-calcium carbonates of/g, 15 parts of coarse whitings and 8000cP dimethyl silicone oils add in vacuum kneader, material temperature is controlled at 75 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, add 0.1 part of γ-aminopropyl triethoxysilane, mixing 0.5h makes base glue; After being cooled to room temperature, the sealing of base glue moves in planetary mixer, add successively 8 parts of methyl tributanoximo silanes, 1 part of vinyl tributyl ketoximyl silane, 0.5 part of γ-aminopropyl triethoxysilane and γ-0.25 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, 0.1 part of dibutyl tin laurate, vacuumize and stir 60min, vacuum keep-0.1MPa with base glue.
embodiment 2
By the α of 80000cP, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes, specific surface area are 30m
25 parts of 115 parts of the active nano-calcium carbonates of/g, 13 parts of coarse whitings and 5000cP dimethyl silicone oils add in vacuum kneader, material temperature is controlled at 80 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, add 0.1 part of γ-aminopropyl triethoxysilane, γ-0.05 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, mixing 0.5h makes base glue; After the sealing of base glue is cooled to room temperature, move in planetary mixer, add successively 7 parts of methyl tributanoximo silanes, 1 part of vinyl tributyl ketoximyl silane, 0.08 part of dibutyl tin laurate, vacuumize and stir 60min, vacuum keep-0.1MPa with base glue.
embodiment 3
By the α of 100000cP, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes, specific surface area are 25m
27 parts of 105 parts of the active nano-calcium carbonates of/g, 11 parts of coarse whitings and 2000cP dimethyl silicone oils add in vacuum kneader, and material temperature is controlled at 130 ℃, and vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, add 1 part, composite dry silane, mixing 0.5h makes base glue; After the sealing of base glue is cooled to room temperature, move in planetary mixer, add successively 6 parts of methyl tributanoximo silanes, 1.5 parts of γ-aminopropyl triethoxysilanes, 0.12 part of dibutyl tin laurate, vacuumize and stir 60min, vacuum keep-0.1MPa with base glue.
embodiment 4
By the α of 150000cP, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes, specific surface area are 23m
28 parts of 100 parts of the active nano-calcium carbonates of/g, 9 parts of coarse whitings and 850cP dimethyl silicone oils add in vacuum kneader, material temperature is controlled at 70 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, add 0.05 part of vinyl tributyl ketoximyl silane, mixing 0.5h makes base glue; After being cooled to room temperature, the sealing of base glue moves in planetary mixer, add successively 5 parts of methyl tributanoximo silanes, 1.65 parts of γ (2.3-epoxy the third oxygen) propyl trimethoxy silicanes, 0.1 part of stannous octoate, vacuumize and stir 60min, vacuum keep-0.08MPa with base glue.
embodiment 5
By the α of 20000cP, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes, specific surface area are 20m
21 part of 135 parts of the active nano-calcium carbonates of/g, 16 parts of coarse whitings and 12500cP dimethyl silicone oil add in vacuum kneader, material temperature is controlled at 90 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, add γ-0.05 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, mixing 0.5h makes base glue; After being cooled to room temperature, the sealing of base glue moves in planetary mixer, add successively 9 parts of methyl tributanoximo silanes, 1.5 parts of vinyl tributyl ketoximyl silanes, 0.45 part of γ-aminopropyl triethoxysilane, 0.08 part of stannous octoate, vacuumize and stir 60min, vacuum keep-0.1MPa with base glue.
embodiment 6
By the α of 350000cP, the α of 30 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 10000cP, 70 parts of alpha, omega-dihydroxy polydimethyl siloxanes, specific surface area are 20m
20.5 part of 90 parts of the active nano-calcium carbonates of/g, 25 parts of coarse whitings and 350cP dimethyl silicone oil add in vacuum kneader, material temperature is controlled at 70 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, add 0.05 part of vinyl tributyl ketoximyl silane, γ-0.05 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, mixing 0.5h makes base glue; After being cooled to room temperature, the sealing of base glue moves in planetary mixer, add successively 4.5 parts of methyl tributanoximo silanes, 1.58 parts of γ-aminopropyl triethoxysilanes and γ-0.2 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, 0.06 part of stannous octoate, vacuumize and stir 60min, vacuum keep-0.1MPa with base glue.
embodiment 7
By the α of 250000cP, the α of 30 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 20000cP, 70 parts of alpha, omega-dihydroxy polydimethyl siloxanes,, specific surface area is 22m
22.5 parts of 100 parts of the active nano-calcium carbonates of/g, 18 parts of coarse whitings and 500cP dimethyl silicone oils add in vacuum kneader, material temperature is controlled at 75 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, add 0.05 part of vinyl tributyl ketoximyl silane, 0.5 part of mixing 0.5h of composite dry silane makes base glue; After being cooled to room temperature, the sealing of base glue moves in planetary mixer, add successively 5.5 parts of methyl tributanoximo silanes, 2.0 parts of γ-aminopropyl triethoxysilanes and γ-0.25 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, 0.05 part of dibutyl tin laurate, vacuumize and stir 60min, vacuum keep-0.1MPa with base glue.
embodiment 8
By the α of 150000cP, the α of 30 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 50000cP, 70 parts of alpha, omega-dihydroxy polydimethyl siloxanes,, specific surface area is 24m
22.5 parts of 110 parts of the active nano-calcium carbonates of/g, 14 parts of coarse whitings and 600cP dimethyl silicone oils add in vacuum kneader, material temperature is controlled at 70 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, 0.05 part of vinyl tributyl ketoximyl silane, 0.1 part of mixing 0.5h of γ-aminopropyl triethoxysilane makes base glue; After being cooled to room temperature, the sealing of base glue moves in planetary mixer, add successively 6 parts of methyl tributanoximo silanes, 1.5 parts of vinyl tributyl ketoximyl silanes, 0.5 part of γ-aminopropyl triethoxysilane and γ-0.35 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, 0.07 part of stannous octoate, vacuumize and stir 60min, vacuum keep-0.09MPa with base glue.
embodiment 9
By the α of 100000cP, the α of 30 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 80000cP, 70 parts of alpha, omega-dihydroxy polydimethyl siloxanes, specific surface area are 28m
23.5 parts of 110 parts of the active nano-calcium carbonates of/g, 12 parts of coarse whitings and 5000cP dimethyl silicone oils add in vacuum kneader, material temperature is controlled at 90 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, 0.1 part of γ-aminopropyl triethoxysilane, 0.5 part, composite dry silane, mixing 0.5h makes base glue; After being cooled to room temperature, the sealing of base glue moves in planetary mixer, add successively 7.5 parts of methyl tributanoximo silanes, 1.8 parts of vinyl tributyl ketoximyl silanes, 0.6 part of γ-aminopropyl triethoxysilane and γ-0.3 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, 0.06 part of dibutyl tin laurate, vacuumize and stir 60min, vacuum keep-0.1MPa with base glue.
embodiment 10
By the α of 80000cP, the α of 60 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 10000cP, 40 parts of alpha, omega-dihydroxy polydimethyl siloxanes, specific surface area are 33m
20.05 part of 120 parts of the active nano-calcium carbonates of/g, 5 parts of coarse whitings and 1500cP dimethyl silicone oil add in vacuum kneader, material temperature is controlled at 95 ℃, vacuum tightness is-0.1MPa, after mixing 3h, stop heating, pass into nitrogen and remove vacuum, add 0.5 part, composite dry silane, γ-0.05 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, mixing 0.5h makes base glue; After being cooled to room temperature, the sealing of base glue moves in planetary mixer, add successively 6.5 parts of methyl tributanoximo silanes, 2.2 parts of vinyl tributyl ketoximyl silanes, 0.45 part of γ-aminopropyl triethoxysilane and γ-0.35 part of (2.3-epoxy the third oxygen) propyl trimethoxy silicane, 0.09 part of stannous octoate, vacuumize and stir 60min, vacuum keep-0.1MPa with base glue.
Above embodiment experimental result is carried out to Performance Detection by GB GB/T13477-2002, and result is as table 1.
Table 1: the experimental result of modulus silicone sealant in this low cost
Claims (8)
1. a preparation method for silicone sealant, is characterized in that: comprise following steps:
(1) by α, alpha, omega-dihydroxy polydimethyl siloxane, filler, dimethyl silicone oil add in vacuum kneader, vacuumize and add hot milling 2～5h;
(2) stop heating, pass into nitrogen and remove vacuum, add appropriate silane coupling agent, mixing 0.5～1h obtains base glue, and it is-0.06～-0.1MPa that mixing process keeps vacuum tightness;
(3) pass into nitrogen and remove vacuum, move into stirrer in after the base glue sealing obtaining is cooled to room temperature in step (2), add linking agent, tackifier, catalyzer, vacuumize, be uniformly mixed and make single-component ketoxime removing type silicone sealant.
2. the preparation method of a kind of silicone sealant according to claim 1, is characterized in that: the α described in step (1), and alpha, omega-dihydroxy polydimethyl siloxane viscosity is more than one in 10000～300000cP; Described filler is to be 20～35m through surface treatment specific surface area
2the active nano-calcium carbonate of/g and a small amount of coarse whiting; Described dimethyl-silicon oil viscosity is more than one in 350～12500cP; Described a small amount of coarse whiting is active nano-calcium carbonate used 5～35%.
3. the preparation method of a kind of silicone sealant according to claim 1, is characterized in that: described α, the quality proportioning of alpha, omega-dihydroxy polydimethyl siloxane, filler, methyl-silicone oil is 100: 80～150: 0.05～8.
4. the preparation method of a kind of silicone sealant according to claim 1, is characterized in that: it is 70～140 ℃ that vacuumizing described in step (1) adds thermal control temperature, and vacuum tightness is-0.06～-0.1MPa.
5. the preparation method of a kind of silicone sealant according to claim 1, it is characterized in that: the silane coupling agent described in step (2) comprises more than one in γ-aminopropyl triethoxysilane, γ-(2.3-epoxy the third oxygen) propyl trimethoxy silicane, composite dry silane, vinyl tributyl ketoximyl silane, its consumption is α, 0.02～2.00% of alpha, omega-dihydroxy polydimethyl siloxane and filler total mass.
6. the preparation method of a kind of silicone sealant according to claim 1, is characterized in that: the stirrer described in step (3) is high speed dispersion planetary mixer mixing speed 100～1000r/min, churning time 30～120min; Described vacuumize that to control vacuum tightness be-0.06～-0.1MPa.
7. the preparation method of a kind of silicone sealant according to claim 1, is characterized in that: the linking agent described in step (3) is methyl tributanoximo silane; Described tackifier be vinyl tributyl ketoximyl silane, γ-aminopropyl triethoxysilane and γ-(2.3-epoxy the third oxygen) propyl trimethoxy silicane more than one; Described catalyzer is wherein a kind of of dibutyl tin laurate and stannous octoate.
8. the preparation method of a kind of silicone sealant according to claim 1, is characterized in that: the quality proportioning of the linking agent described in step (3), tackifier, catalyzer is 10:1～4:0.05～0.15.
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