CN101580688B - Dual-component silicone sealant formula used for construction and preparation thereof - Google Patents
Dual-component silicone sealant formula used for construction and preparation thereof Download PDFInfo
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- CN101580688B CN101580688B CN2009101079842A CN200910107984A CN101580688B CN 101580688 B CN101580688 B CN 101580688B CN 2009101079842 A CN2009101079842 A CN 2009101079842A CN 200910107984 A CN200910107984 A CN 200910107984A CN 101580688 B CN101580688 B CN 101580688B
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Abstract
The invention relates to a dual-component silicone sealant used for construction and having stable storage, excellent physical performances and faster curing speed. The dual-component silicone sealantused for construction comprises an A component and a B component, and the mass parts of all the components are as follows: A component: basic polymer: 50-150 parts, plasticizer: 0.1-20 parts, filler:50-150 parts, and MQ silicon resin: 0.1-50 parts; and B component: end-alkoxy polysiloxane: 0-100 parts, dimethyl silicone oil: 0-100 parts, pigment: 0.1-50 parts, filler: 0.1-100 parts, cross-linking agent: 0.5-80 parts, coupling agent: 0.5-80 parts, and catalyst: 0.001-10 parts. When in use, the mass ratio of the two components is that A:B is equal to 7-13:1.
Description
Technical field:
The invention belongs to the room temperature silicone sealant, be specifically related to the neutral silicone sealant of a kind of two-pack, especially a kind of shelf-stable, physicals brilliance, curing speed two-component building silicone sealant faster that relates to.
Background technology:
Silicone sealant has superior UV resistant and atmospheric aging, can keep not chapping in 30 years in severe environment such as sunlight, rain, snow and seasonal climate conversion, does not become fragile, the superior endurance quality of stay-in-grade and wide temperature range have 50% characteristics such as displacement capacity.A large amount of employings along with the superior and large-scale skeleton construction of prefabricated, the high stratification of building industry, building internal and external ornament and finishing cause the performance requriements and the consumption of building sealant more and more higher.
The bi-component silicone seal gum is faster than single component curing speed, and curing time is short, and curing speed can utilize the ratio of A, B component to adjust flexibly.Provide a kind of electronic-grade bicomponent normal temperature moisture solidification silicone sealant as ZL200510100904.2, owing to contain linking agent in the A component, if filler without processed, then contains moisture and can cause A component deficiency storage period in the filler; If filler is through processed, then the curing speed of system has considerable influence.
At present country there are strict requirements to tensile strength, modulus and the maximum, force elongation of structural silicone adhesive.So will be not only up to specification but also guarantee the silicone sealant of use properties and effect, be the difficult problem that an industrial silicon ketone seal gum is produced.
Summary of the invention:
A kind of two-component building silicone sealant that the present invention invents in order to solve above-mentioned prior art problem just.
Prescription:
A kind of two-component building silicone sealant includes A component and B component, and described each constituent mass is constructed as follows:
The A component:
Base polymer: 50～150 parts;
Softening agent: 0.1～20 part;
Filler: 50～150 parts;
MQ silicone resin: 0.1～50 part;
The B component:
End alkoxyl group polysiloxane: 0～100 part;
Dimethyl silicone oil: 0～100 part;
Pigment: 0.1～50 part;
Filler: 0.1～100 part;
Linking agent: 0.5～80 part;
Coupling agent: 0.5～80 part;
Catalyzer: 0.001～10 part.
Two constituent masses ratio: A: B=7～13: 1 during use.
Described A component and B component constitute can also for:
The A component:
Base polymer: 50～150 parts;
Softening agent: 0.1～10 part;
Filler: 50～150 parts;
MQ silicone resin: 0.1～20 part;
The B component:
End alkoxyl group polysiloxane: 0～50 part;
Dimethyl silicone oil: 0～50 part;
Pigment: 0.1～30 part;
Filler: 0.1～30 part;
Linking agent: 0.5～50 part;
Coupling agent: 0.5～50 part;
Catalyzer: 0.01～5 part.
Two constituent masses ratio: A: B=8～13: 1 during use.
Described A component and B component constitute can also for:
The A component:
Base polymer: 100 parts;
Softening agent: 5 parts;
Filler: 100 parts;
MQ silicone resin: 10 parts;
The B component:
End alkoxyl group polysiloxane: 25 parts;
Dimethyl silicone oil: 25 parts;
Pigment: 15 parts;
Filler: 2 parts;
Linking agent: 25 parts;
Coupling agent: 23 parts;
Catalyzer: 0.1～0.5 part.
Two constituent masses ratio: A: B=8～13: 1 during use.
Wherein said base polymer is: α, alpha, omega-dihydroxy polydimethyl siloxane (I).Described end alkoxyl group polysiloxane is α, ω-methyl dimethoxy oxygen base siloxy end-blocking polydimethylsiloxane or (II) at least a in α, ω-trimethoxy siloxy end-blocking polydimethylsiloxane (III).Described softening agent is a monoalkoxy end-blocking polydimethylsiloxane, comprises that dimethyl silicone oil, dimethyl methoxy base siloxy end-blocking polydimethylsiloxane (IV), methyl dimethoxy oxygen base siloxy end-blocking polydimethylsiloxane (V) or trimethoxy siloxy end-blocking polydimethylsiloxane (VI) are at least a.Described filler is that lime carbonate, white carbon black, silicon powder, wilkinite or talcum powder are at least a.Described linking agent is methyltrimethoxy silane, ethyl trimethoxy silane, vinyltrimethoxy silane, tetraethoxy, just the silicic acid propyl ester is at least a.Described coupling agent is that γ-An Bingjisanyiyangjiguiwan, γ-(2, the 3-glycidoxy) propyl trimethoxy silicane, N-β-aminoethyl-γ-An Bingjisanjiayangjiguiwan, r-chloropropyl trimethoxyl silane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane are at least a.Described catalyzer is at least a in the acetylacetone chelate of ethyl acetoacetate chelate, isopropyl titanate of dibutyl tin dilaurate, isopropyl titanate, tetrabutyl titanate, isopropyl titanate.
Preparation technology:
The A component:
Base polymer, softening agent, MQ silicone resin and filler are added in the vacuum kneader, vacuum tightness is-0.04～-0.1MPa, mediated 1～10 hour, make basic glue, grind with three-roller again, moving into vacuum removal bubble in the high-speed mixer then, vacuum tightness is-0.04～-0.1MPa, be distributed into the A component at last;
The B component:
(1) catalyst mixture: coupling agent, catalyzer are placed reactor, find time to stir, and temperature is risen to 60 ℃～100 ℃ reactions 1～4 hour, make catalyst mixture;
(2) mill base: softening agent, filler, pigment are added in the vacuum kneader, vacuum tightness be-0.04～-0.1MPa, temperature is 80 ℃～150 ℃, mediates 1～10 hour, with the three-roller grinding, makes mill base again;
(3) at room temperature, mill base, end alkoxyl group polysiloxane, linking agent and catalyst mixture being added in the high speed dispersor, find time to stir, vacuum tightness be-0.04～-0.1MPa, rotating speed is 50～1000rpm, churning time is preservation after 15～120 minutes.
Preserve respectively after A component, B component are produced, wait when using to be mixed in proportion, can adopt the two-pack adhesive supplier of specialty.
The present invention compared with prior art has following advantage:
1) curing speed is very fast, and curing speed can be adjusted by the ratio of A, B component.
2) shelf-stable.Do not contain linking agent, coupling agent, catalyzer etc. in the A component; Filler in the B component is through processed.
3) physicals brilliance, especially maximum, force elongation, high-low temperature resistant and immersion cohesiveness aspect.
Specific embodiment:
Embodiment 1:
The A component:
Base polymer: 50～150 parts;
Softening agent: 0.1～20 part;
Filler: 50～150 parts;
MQ silicone resin: 0.1～50 part;
The B component:
End alkoxyl group polysiloxane: 0～100 part;
Dimethyl silicone oil: 0～100 part;
Pigment: 0.1～50;
Filler: 0.1～100 part;
Linking agent: 0.5～80 part;
Coupling agent: 0.5～80 part;
Catalyzer: 0.001～10 part.
Two constituent masses ratio: A: B=7～13: 1 during use
Embodiment 2:
The A component:
Base polymer: 50～150 parts;
Softening agent: 0.1～10 part;
Filler: 50～150 parts;
MQ silicone resin: 0.1～20 part;
The B component:
End alkoxyl group polysiloxane: 0～50 part;
Dimethyl silicone oil: 0～50 part;
Pigment: 0.1～30;
Filler: 0.1～30 part;
Linking agent: 0.5～50 part;
Coupling agent: 0.5～50 part;
Catalyzer: 0.01～5 part.
Two constituent masses ratio: A: B=8～13: 1 during use
Embodiment 3
The A component:
Base polymer: 100 parts;
Softening agent: 5 parts;
Filler: 100 parts;
MQ silicone resin: 10 parts;
The B component:
End alkoxyl group polysiloxane: 25 parts;
Dimethyl silicone oil: 25 parts;
Pigment: 15 parts;
Filler: 2 parts;
Linking agent: 25 parts;
Coupling agent: 23 parts;
Catalyzer: 0.1～0.5 part.
Two constituent masses ratio: A: B=8～13: 1 during use
In the foregoing description 1～3, described base polymer is: α, alpha, omega-dihydroxy polydimethyl siloxane (I).Described end alkoxyl group polysiloxane is α, ω-methyl dimethoxy oxygen base siloxy end-blocking polydimethylsiloxane or (II) at least a in α, ω-trimethoxy siloxy end-blocking polydimethylsiloxane (III).Described softening agent is a monoalkoxy end-blocking polydimethylsiloxane, comprises that dimethyl silicone oil, dimethyl methoxy base siloxy end-blocking polydimethylsiloxane (IV), methyl dimethoxy oxygen base siloxy end-blocking polydimethylsiloxane (V) or trimethoxy siloxy end-blocking polydimethylsiloxane (VI) are at least a.Described filler is that lime carbonate, white carbon black, silicon powder, wilkinite or talcum powder are at least a.Described linking agent is methyltrimethoxy silane, ethyl trimethoxy silane, vinyltrimethoxy silane, tetraethoxy, just the silicic acid propyl ester is at least a.Described coupling agent is that γ-An Bingjisanyiyangjiguiwan, γ-(2, the 3-glycidoxy) propyl trimethoxy silicane, N-β-aminoethyl-γ-An Bingjisanjiayangjiguiwan, r-chloropropyl trimethoxyl silane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane are at least a.Described catalyzer is at least a in the acetylacetone chelate of ethyl acetoacetate chelate, isopropyl titanate of dibutyl tin dilaurate, isopropyl titanate, tetrabutyl titanate, isopropyl titanate.
Embodiment 4:
Formula for a product is as follows:
The A component:
α, alpha, omega-dihydroxy polydimethyl siloxane (I): 100 parts
Dimethyl silicone oil: 5 parts
Lime carbonate: 100 parts
MQ silicone resin: 10 parts
The B component:
End trimethoxy polydimethylsiloxane: 25 parts
Dimethyl silicone oil: 25 parts
Carbon black: 15 parts
Gas-phase silica: 2 parts
Methyltrimethoxy silane: 5 parts
Tetraethoxy: 10 parts
Positive silicic acid propyl ester: 10 parts
γ-An Bingjisanyiyangjiguiwan: 15 parts
γ-(2, the 3-glycidoxy) propyl trimethoxy silicane: 8 parts
Dibutyl tin dilaurate: 0.1 part
Two constituent masses ratio: A: B=13: 1 during use
Embodiment 5:
Replace end trimethoxy polydimethylsiloxane (consumption that is dimethyl silicone oil is 50 parts) with dimethyl silicone oil in the B component, the addition of all the other compositions and preparation technology are identical with embodiment 4.
Product preparation process:
The A component:
Base polymer, softening agent, MQ silicone resin and filler are added in the vacuum kneader, and vacuum tightness is-0.098MPa to mediate 2 hours, make basic glue, grind with three-roller again, move into vacuum removal bubble in the high-speed mixer then, vacuum tightness is-0.098MPa to be distributed into the A component at last.
The B component:
1) catalyst mixture: with γ-An Bingjisanyiyangjiguiwan, γ-(2, the 3-glycidoxy) propyl trimethoxy silicane and dibutyl tin dilaurate place reactor, find time to stir, and temperature is risen to 80 ℃ of reactions 2 hours, make catalyst mixture.
2) mill base: dimethyl silicone oil, gas-phase silica, carbon black are added in the vacuum kneader, and vacuum tightness is-0.098MPa that temperature is 120 ℃, mediates 3 hours, grinds with three-roller again, makes mill base.
3) at room temperature, mill base, end trimethoxy polydimethylsiloxane, methyltrimethoxy silane, tetraethoxy, positive silicic acid propyl ester and catalyst mixture are added in the high speed dispersor, find time to stir, vacuum tightness is-0.098MPa, rotating speed is 500rpm, and churning time is 60 minutes.
Using method: be mixed in proportion the back and use, can adopt professional adhesive supplier.A: B=7～13: 1 is preferred 13: 1.
Below by this product and national standard and some this product of currently available products compare test data declaration effects:
Comparative example 1:
Do not contain the MQ silicone resin in the A component, the addition of all the other compositions and preparation technology are identical with embodiment 4.
Comparative example 2:
Cancel dimethyl silicone oil in the A component, cancellation dimethyl silicone oil and end trimethoxy polydimethylsiloxane in the B component.The addition of all the other compositions and preparation technology are identical with embodiment 4.
The performance perameter contrast
It is GB16776-2005 " structural silicone sealant for building " that last table adopts national examination criteria.
Can draw to draw a conclusion from last table data:
(1) product performance brilliance of the present invention can reach and partial properties surmounts national standard.
(2) adopt the MQ silicone resin as reinforced filling, can effectively improve the aspect performances such as physicals own, particularly elongation at break, high-low temperature resistant and immersion cohesiveness of product.
(3) interpolation holds the trimethoxy polydimethylsiloxane that the physicals of system is improved in the prescription.
More than be that a kind of dual-component silicone sealant formula used for construction provided by the present invention and preparation and using method thereof are described in detail, used specific case herein prescription of the present invention and preparation technology thereof are set forth, above embodiment just is used for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, part in specific embodiments and applications all can change.In sum, this description should not be construed as limitation of the present invention.
Claims (7)
1. a two-component building silicone sealant includes A component and B component, it is characterized in that described each constituent mass is constructed as follows:
The A component:
Base polymer: 50～150 parts;
Softening agent: 0.1～20 part;
Filler: 50～150 parts;
MQ silicone resin: 0.1～50 part;
The B component:
End alkoxyl group polysiloxane: 0～100 part;
Dimethyl silicone oil: 0～100 part;
Pigment: 0.1～50 part;
Filler: 0.1～100 part;
Linking agent: 0.5～80 part;
Coupling agent: 0.5～80 part;
Catalyzer: 0.001～10 part;
Two constituent masses ratio: A: B=7～13: 1 during use;
Described base polymer is: α, alpha, omega-dihydroxy polydimethyl siloxane (I);
Described end alkoxyl group polysiloxane is at least a in α, ω-methyl dimethoxy oxygen base siloxy end-blocking polydimethylsiloxane (II) or α, the ω-trimethoxy siloxy end-blocking polydimethylsiloxane (III);
Described softening agent is that dimethyl silicone oil, dimethyl methoxy base siloxy end-blocking polydimethylsiloxane (IV), methyl dimethoxy oxygen base siloxy end-blocking polydimethylsiloxane (V) or trimethoxy siloxy end-blocking polydimethylsiloxane (VI) are at least a.
2. two-component building silicone sealant according to claim 1, it is characterized in that described A component and B component constitute can also for:
The A component:
Base polymer: 50～150 parts;
Softening agent: 0.1～10 part;
Filler: 50～150 parts;
MQ silicone resin: 0.1～20 part;
The B component:
End alkoxyl group polysiloxane: 0～50 part;
Dimethyl silicone oil: 0～50 part;
Pigment: 0.1～30 part;
Filler: 0.1～30 part;
Linking agent: 0.5～50 part;
Coupling agent: 0.5～50 part;
Catalyzer: 0.01～5 part;
Two constituent masses ratio: A: B=8～13: 1 during use.
3. two-component building silicone sealant according to claim 2, it is characterized in that described A component and B component constitute can also for:
The A component:
Base polymer: 100 parts;
Softening agent: 5 parts;
Filler: 100 parts;
MQ silicone resin: 10 parts;
The B component:
End alkoxyl group polysiloxane: 25 parts;
Dimethyl silicone oil: 25 parts;
Pigment: 15 parts;
Filler: 2 parts;
Linking agent: 25 parts;
Coupling agent: 23 parts;
Catalyzer: 0.1～0.5 part;
Two constituent masses ratio: A: B=8～13: 1 during use.
4. two-component building silicone sealant according to claim 1 is characterized in that described filler is that lime carbonate, white carbon black, silicon powder, wilkinite or talcum powder are at least a.
5. two-component building silicone sealant according to claim 1 is characterized in that described linking agent is methyltrimethoxy silane, ethyl trimethoxy silane, vinyltrimethoxy silane, tetraethoxy, just the silicic acid propyl ester is at least a; Described coupling agent is that γ-An Bingjisanyiyangjiguiwan, γ-(2, the 3-glycidoxy) propyl trimethoxy silicane, N-β-aminoethyl-γ-An Bingjisanjiayangjiguiwan, r-chloropropyl trimethoxyl silane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane are at least a.
6. two-component building silicone sealant according to claim 1 is characterized in that described catalyzer is at least a in the acetylacetone chelate of ethyl acetoacetate chelate, isopropyl titanate of dibutyl tin dilaurate, isopropyl titanate, tetrabutyl titanate, isopropyl titanate.
7. a two-component building as claimed in claim 1 is characterized in that described technology comprises the different manufacture crafts of A, B two components with the preparation technology of silicone sealant:
The A component:
Base polymer, softening agent, MQ silicone resin and filler are added in the vacuum kneader, vacuum tightness is-0.04～-0.1MPa, mediated 1～10 hour, make basic glue, grind with three-roller again, moving into vacuum removal bubble in the high-speed mixer then, vacuum tightness is-0.04～-0.1MPa, be distributed into the A component at last;
The B component:
(1) catalyst mixture: coupling agent, catalyzer are placed reactor, find time to stir, and temperature is risen to 60 ℃～100 ℃ reactions 1～4 hour, make catalyst mixture;
(2) mill base: dimethyl silicone oil, filler, pigment are added in the vacuum kneader, vacuum tightness be-0.04～-0.1MPa, temperature is 80 ℃～150 ℃, mediates 1～10 hour, with the three-roller grinding, makes mill base again;
(3) at room temperature, mill base, end alkoxyl group polysiloxane, linking agent and catalyst mixture being added in the high speed dispersor, find time to stir, vacuum tightness be-0.04～-0.1MPa, rotating speed is 50～1000rpm, churning time is preservation after 15～120 minutes;
(4) preserve respectively after A component, B component are produced, be mixed in proportion the back during use and use.
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| CN2009101079842A CN101580688B (en) | 2009-06-12 | 2009-06-12 | Dual-component silicone sealant formula used for construction and preparation thereof |
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| CN101580688B true CN101580688B (en) | 2011-07-13 |
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2009
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