CN108795369A - silicone sealant and preparation method thereof - Google Patents
silicone sealant and preparation method thereof Download PDFInfo
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- CN108795369A CN108795369A CN201810689753.6A CN201810689753A CN108795369A CN 108795369 A CN108795369 A CN 108795369A CN 201810689753 A CN201810689753 A CN 201810689753A CN 108795369 A CN108795369 A CN 108795369A
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- Prior art keywords
- silicone sealant
- parts
- plasticizer
- filler
- preparation
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The present invention proposes a kind of silicone sealant and preparation method thereof, according to the number of parts by weight, including following components：1~10 part of 0.1~3 part of 30~50 parts of 15~25 parts of 45~60 parts of polydiorganosiloxanepolyurea, plasticizer, filler, crosslinking agent, coupling agent containing active end group and 0.1~3 part of catalyst；The plasticizer is mainly prepared by methylchlorosilane and white oil.Preparation method：1) polydiorganosiloxanepolyurea containing active end group is dehydrated with filler, base-material is obtained after being cooled to room temperature；2) plasticizer, crosslinking agent, coupling agent and catalyst are added into base-material, is stirred under vacuum, you can obtains silicone sealant.The silicone sealant has good ageing-resistant performance and adhesive property.
Description
Technical field
The invention belongs to sealing material technical fields for building, and in particular to a kind of silicone sealant and preparation method thereof.
Background technology
Silicone sealant have the characteristics that excellent heatproof, it is weather-proof, anti-aging, be not cracked, antidetonation and moisture-proof, building,
Electronic apparatus, automobile, field of aerospace are widely used.The widely used construction sealing materials of silicone sealant material, however
The silicone sealant of general low elongation cannot meet the requirement of the height displacement ability of concrete joint, with concrete itself
Adhesive property it is bad, be easy drawing crack, to make sealing function lose, and maintenance cost is excessively high again.
Domestic patent provides a kind of preparation method of neutral stone material glue, and modulus is more than 0.4MPa, is applied to concrete
When the sealing of seam, it is easy cracking.Also there are the preparation method of the low modulus silicone sealant of patent disclosure, but such sealing rubber moulding
Amount is too low, is restricted in use, and also undesirable to the adhesive property of concrete.
Invention content
The present invention proposes that a kind of silicone sealant, the silicone sealant have good ageing-resistant performance and adhesive property.
The technical proposal of the invention is realized in this way：
A kind of silicone sealant, according to the number of parts by weight, including following components：
30~50 parts of 15~25 parts of 45~60 parts of polydiorganosiloxanepolyurea, plasticizer, filler, crosslinking agent containing active end group
0.1~3 part of 0.1~3 part, 1~10 part of coupling agent and catalyst；The plasticizer is mainly prepared by methylchlorosilane and white oil
It arrives.
Preferably, the preparation method of the plasticizer is：
It weighs the methylchlorosilane of 60~70wt% and 30~40wt% white oils is mixed to get mix monomer, mix monomer oil
Bath is warming up to 50~60 DEG C, and under the conditions of inert gas shielding, stannous octoate and ethylene glycol is added, reacts 1~2h, then cools down
It is handled again with concentrated hydrochloric acid to room temperature, then with alkali neutralization to neutrality, filtered fluid is obtained by filtration, filtered fluid is dried.
Preferably, the addition of the stannous octoate is the 1~3% of mix monomer quality, the addition of the ethylene glycol
It is the 4~8% of mix monomer quality.
Preferably, the polydiorganosiloxanepolyurea containing active end group is α, alpha, omega-dihydroxy polydimethyl siloxane.
Preferably, the filler be aerosil and gas-phase silica mixture, the aerosil with
The mass ratio of the gas-phase silica is 8~12:1.
Preferably, the crosslinking agent is the mixture of ethyl orthosilicate and methyltriethoxysilane.
Preferably, the coupling agent is gamma-aminopropyl-triethoxy-silane, γ-(2,3- the third oxygen of epoxy) propyl trimethoxy
Base silane, γ-(methacryloxypropyl) propyl trimethoxies silicon, N- (β-aminoethyl)-gamma-aminopropyl-triethoxy silicon and double
At least one of (γ-trimethoxy-silylpropyl) amine.
Preferably, the catalyst is dibutyl tin dilaurate or dibutyl tin acetate.
It is a further object to provide a kind of preparation methods of silicone sealant, include the following steps：
1) according to proportioning weigh polydiorganosiloxanepolyurea containing active end group, plasticizer, filler, crosslinking agent, coupling agent and
Catalyst is spare；
2) polydiorganosiloxanepolyurea containing active end group is dehydrated with filler, base-material is obtained after being cooled to room temperature；
3) plasticizer, crosslinking agent, coupling agent and catalyst are added into base-material, is stirred under vacuum, you can
Obtain silicone sealant.
Preferably, it is 0.075~0.095MPa that the vacuum condition of the step 3), which is vacuum degree,.
Beneficial effects of the present invention
Plasticizer in the silicone sealant of the present invention is mainly prepared by methylchlorosilane and white oil, by tradition
White oil be modified processing, the permeability phenomenon of white oil product before the plasticizer of acquisition avoids, while making silicone seal
Glue elongation at break reaches 500~600%.
The construction materials such as silicone sealant provided by the invention and concrete have excellent caking property, weatherability
Can be good, good water-proof effect can be applied in than relatively rugged environment.
Specific implementation mode
Embodiment 1
A kind of silicone sealant, according to the number of parts by weight, including following components：
α, 53 parts of alpha, omega-dihydroxy polydimethyl siloxane, 20 parts of plasticizer, 40 parts of filler, 2 parts of crosslinking agent, γ-aminopropyl
1.6 parts of 7 parts of triethoxysilane and dibutyl tin dilaurate.Filler is the mixing of aerosil and gas-phase silica
The mass ratio of object, aerosil and gas-phase silica is 12:1.Crosslinking agent is ethyl orthosilicate and methyl triethoxy
The mixture of silane.
The preparation method of plasticizer is：
It weighs the methylchlorosilane of 65wt% and 35wt% white oils is mixed to get mix monomer, mix monomer oil bath is warming up to
60 DEG C, under the conditions of inert gas shielding, stannous octoate and ethylene glycol is added, reacts 1h, then cools to room temperature again with dense salt
Acid processing, then with alkali neutralization to neutrality, filtered fluid is obtained by filtration, filtered fluid is dried.The addition of stannous octoate
It is the 2% of mix monomer quality, the addition of the ethylene glycol is the 6% of mix monomer quality.
The preparation method of silicone sealant：
1) α, alpha, omega-dihydroxy polydimethyl siloxane, plasticizer, filler, crosslinking agent, γ-aminopropyl are weighed according to proportioning
Triethoxysilane and dibutyl tin dilaurate are spare；
2) by α, alpha, omega-dihydroxy polydimethyl siloxane is dehydrated with filler, and base-material is obtained after being cooled to room temperature；
3) plasticizer, crosslinking agent, gamma-aminopropyl-triethoxy-silane and dibutyl tin dilaurate are added into base-material,
It is stirred under conditions of vacuum degree is 0.075~0.095MPa, you can obtain silicone sealant.
Embodiment 2
A kind of silicone sealant, according to the number of parts by weight, including following components：
α, 45 parts of alpha, omega-dihydroxy polydimethyl siloxane, 15 parts of plasticizer, 50 parts of filler, 0.1 part of crosslinking agent, γ-ammonia third
0.1 part of 1 part of ethyl triethoxy silicane alkane and dibutyl tin dilaurate.Filler is the mixing of aerosil and gas-phase silica
The mass ratio of object, aerosil and gas-phase silica is 9:1.Crosslinking agent is ethyl orthosilicate and methyltriethoxy silane
The mixture of alkane.
The preparation method of plasticizer is：
It weighs the methylchlorosilane of 60wt% and 40wt% white oils is mixed to get mix monomer, mix monomer oil bath is warming up to
55 DEG C, under the conditions of inert gas shielding, stannous octoate and ethylene glycol is added, reacts 1.6h, then cools to room temperature again with dense
HCl treatment, then with alkali neutralization to neutrality, filtered fluid is obtained by filtration, filtered fluid is dried.The addition of stannous octoate
Amount is the 1% of mix monomer quality, and the addition of the ethylene glycol is the 4% of mix monomer quality.
The preparation method of silicone sealant is substantially the same manner as Example 1, the difference is that each component and content.
Embodiment 3
A kind of silicone sealant, according to the number of parts by weight, including following components：
α, 60 parts of alpha, omega-dihydroxy polydimethyl siloxane, 25 parts of plasticizer, 30 parts of filler, 1.7 parts of crosslinking agent, γ-(first
Base acryloyl-oxy) 3 parts of 10 parts of propyl trimethoxy silicon and dibutyl tin acetate.Filler is aerosil and gas phase hard charcoal
The mass ratio of black mixture, aerosil and gas-phase silica is 10:1.Crosslinking agent is ethyl orthosilicate and methyl
The mixture of triethoxysilane.
The preparation method of plasticizer is：
It weighs the methylchlorosilane of 70wt% and 30wt% white oils is mixed to get mix monomer, mix monomer oil bath is warming up to
50 DEG C, under the conditions of inert gas shielding, stannous octoate and ethylene glycol is added, reacts 2h, then cools to room temperature again with dense salt
Acid processing, then with alkali neutralization to neutrality, filtered fluid is obtained by filtration, filtered fluid is dried.The addition of stannous octoate
It is the 3% of mix monomer quality, the addition of the ethylene glycol is the 5% of mix monomer quality.
The preparation method of silicone sealant is substantially the same manner as Example 1, the difference is that each component and content.
Embodiment 4
A kind of silicone sealant, according to the number of parts by weight, including following components：
α, 55 parts of alpha, omega-dihydroxy polydimethyl siloxane, 18 parts of plasticizer, 35 parts of filler, 2.3 parts of crosslinking agent, γ-(first
Base acryloyl-oxy) 2 parts of 4 parts of propyl trimethoxy silicon and dibutyl tin acetate.Filler is aerosil and gas phase hard charcoal
The mass ratio of black mixture, aerosil and gas-phase silica is 8:1.Crosslinking agent is ethyl orthosilicate and methyl three
The mixture of Ethoxysilane.
The preparation method of plasticizer is：
It weighs the methylchlorosilane of 68wt% and 32wt% white oils is mixed to get mix monomer, mix monomer oil bath is warming up to
58 DEG C, under the conditions of inert gas shielding, stannous octoate and ethylene glycol is added, reacts 1.2h, then cools to room temperature again with dense
HCl treatment, then with alkali neutralization to neutrality, filtered fluid is obtained by filtration, filtered fluid is dried.The addition of stannous octoate
Amount is the 2% of mix monomer quality, and the addition of the ethylene glycol is the 8% of mix monomer quality.
The preparation method of silicone sealant is substantially the same manner as Example 1, the difference is that each component and content.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of silicone sealant, which is characterized in that according to the number of parts by weight, including following components：
30~50 parts of 15~25 parts of 45~60 parts of polydiorganosiloxanepolyurea, plasticizer, filler, crosslinking agent 0.1 containing active end group
0.1~3 part of~3 parts, 1~10 part of coupling agent and catalyst；The plasticizer is mainly prepared by methylchlorosilane and white oil.
2. silicone sealant according to claim 1, which is characterized in that the preparation method of the plasticizer is：
It weighs the methylchlorosilane of 60~70wt% and 30~40wt% white oils is mixed to get mix monomer, mix monomer oil bath liter
Temperature is to 50~60 DEG C, and under the conditions of inert gas shielding, stannous octoate and ethylene glycol is added, reacts 1~2h, is subsequently cooled to room
The processing of Wen Zaiyong concentrated hydrochloric acids, then with alkali neutralization to neutrality, filtered fluid is obtained by filtration, filtered fluid is dried.
3. silicone sealant according to claim 2, which is characterized in that the addition of the stannous octoate is mix monomer
The 1~3% of quality, the addition of the ethylene glycol are the 4~8% of mix monomer quality.
4. silicone sealant according to claim 1, which is characterized in that the polydiorganosiloxanepolyurea containing active end group
For α, alpha, omega-dihydroxy polydimethyl siloxane.
5. silicone sealant according to claim 1, which is characterized in that the filler is that aerosil and gas phase are white
The mass ratio of the mixture of carbon black, the aerosil and the gas-phase silica is 8~12:1.
6. silicone sealant according to claim 1, which is characterized in that the crosslinking agent is ethyl orthosilicate and methyl three
The mixture of Ethoxysilane.
7. silicone sealant according to claim 1, which is characterized in that the coupling agent is gamma-aminopropyl-triethoxy
Silane, γ-(the third oxygen of 2,3- epoxies) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxies silicon, N- (β-
Aminoethyl) at least one of-gamma-aminopropyl-triethoxy silicon and bis- (γ-trimethoxy-silylpropyl) amine.
8. silicone sealant according to claim 1, which is characterized in that the catalyst be dibutyl tin dilaurate or
Person's dibutyl tin acetate.
9. the preparation method of silicone sealant as described in claim 1, which is characterized in that include the following steps：
1) polydiorganosiloxanepolyurea, plasticizer, filler, crosslinking agent, coupling agent and catalysis containing active end group are weighed according to proportioning
Agent is spare；
2) polydiorganosiloxanepolyurea containing active end group is dehydrated with filler, base-material is obtained after being cooled to room temperature；
3) plasticizer, crosslinking agent, coupling agent and catalyst are added into base-material, is stirred under vacuum, you can obtains
Silicone sealant.
10. the preparation method of silicone sealant according to claim 9, which is characterized in that the vacuum item of the step 3)
Part is that vacuum degree is 0.075~0.095MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810689753.6A CN108795369A (en) | 2018-06-28 | 2018-06-28 | silicone sealant and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810689753.6A CN108795369A (en) | 2018-06-28 | 2018-06-28 | silicone sealant and preparation method thereof |
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| CN108795369A true CN108795369A (en) | 2018-11-13 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101293978A (en) * | 2008-06-12 | 2008-10-29 | 南京工业大学 | Sericite modified ultraviolet resistant polymer master batch and composite material |
| CN107353869A (en) * | 2017-07-17 | 2017-11-17 | 四川建筑职业技术学院 | It is a kind of to be used to emulate acid silicone adhesive of dinosaurs handicraft and preparation method thereof |
| CN107384304A (en) * | 2017-08-03 | 2017-11-24 | 合肥隆延科技有限公司 | Silicone sealant and preparation method thereof |
| CN107384303A (en) * | 2017-08-03 | 2017-11-24 | 合肥隆延科技有限公司 | Silicone sealant that steam-preventing passes through and preparation method thereof |
| US20180016400A1 (en) * | 2015-03-17 | 2018-01-18 | Henkel Ag & Co. Kgaa | Curable Silicone Compositions |
-
2018
- 2018-06-28 CN CN201810689753.6A patent/CN108795369A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101293978A (en) * | 2008-06-12 | 2008-10-29 | 南京工业大学 | Sericite modified ultraviolet resistant polymer master batch and composite material |
| US20180016400A1 (en) * | 2015-03-17 | 2018-01-18 | Henkel Ag & Co. Kgaa | Curable Silicone Compositions |
| CN107353869A (en) * | 2017-07-17 | 2017-11-17 | 四川建筑职业技术学院 | It is a kind of to be used to emulate acid silicone adhesive of dinosaurs handicraft and preparation method thereof |
| CN107384304A (en) * | 2017-08-03 | 2017-11-24 | 合肥隆延科技有限公司 | Silicone sealant and preparation method thereof |
| CN107384303A (en) * | 2017-08-03 | 2017-11-24 | 合肥隆延科技有限公司 | Silicone sealant that steam-preventing passes through and preparation method thereof |
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Application publication date: 20181113 |
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