CN101134887A - Autocatalysis cross-linking organosilicon seal glue and method for making same - Google Patents
Autocatalysis cross-linking organosilicon seal glue and method for making same Download PDFInfo
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- CN101134887A CN101134887A CNA2007100298345A CN200710029834A CN101134887A CN 101134887 A CN101134887 A CN 101134887A CN A2007100298345 A CNA2007100298345 A CN A2007100298345A CN 200710029834 A CN200710029834 A CN 200710029834A CN 101134887 A CN101134887 A CN 101134887A
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Abstract
The present invention discloses one kind of self-catalysis cross-linked silicone sealing glue and its preparation process. The self-catalysis cross-linked silicone sealing glue contains alpha, omega-dihydroxy polysiloxane as main component, alpha-amidomethyl trialkoxy silane as the cross-linking agent, stuffing and diluent. It has simple preparation process without need of added catalyst, fast curing speed, low cost and other advantages. It is suitable for adhering and sealing energy-saving lamp and vehicle lamp.
Description
Technical field
The present invention relates to a kind of autocatalysis cross-linking organosilicon seal glue and manufacture method thereof, be applicable to the adhering and sealing of energy-saving lamp, car light.
Background technology
Domestic and international widely used condensed type organic silicon seal gum and tackiness agent adopt organic tin salt, titanium complex at present, and it is big to have toxicity, the shortcoming of reversion under the cross-linked rubber high temperature.For example patent ZL01107167.2 (neutral silicone seal gum and manufacture method thereof) adopts dibutyl tin laurate, dibutyltin diacetate or stannic oxide acetyl triethyl complex compound; The catalyzer that ZL01803341.5 (organosiloxane composition) introduces is the acetylacetic ester of titanium or zirconium.And add-on type organosilicon sealant and tackiness agent adopt platinum group catalyst, not only cost an arm and a leg, and cause poisoning of catalyst easily.
Summary of the invention
For addressing the above problem, the purpose of this invention is to provide a kind of autocatalysis cross-linking organosilicon seal glue, its toxicity is low, superior performance, price is lower.
Another object of the present invention provides the manufacture method of above-mentioned autocatalysis cross-linking organosilicon seal glue, and its technology is simple, need not extra catalyst.
The object of the present invention is achieved like this: a kind of autocatalysis cross-linking organosilicon seal glue is characterized in that containing following component:
Base glue α, the alpha, omega-dihydroxy polysiloxane;
Linking agent α-aminomethyl trialkoxy silane;
Filler and thinner.
The preparation method of above-mentioned autocatalysis cross-linking organosilicon seal glue is characterized in that may further comprise the steps:
(1) with α, alpha, omega-dihydroxy polysiloxane 100 mass parts, filler 60-120 mass parts mix to stir, and progressively is warming up to 110-120 ℃, be-0.080 in vacuum tightness～-the 0.095MPa condition under, vacuum hydro-extraction 45-60 minute, it was standby to be cooled to room temperature;
(2) under the room temperature with the α-aminomethyl trialkoxy silane of 1.2-4.0 mass parts and the thinner wiring solution-forming of 60-100 mass parts, add α, in the alpha, omega-dihydroxy polysiloxane mixture vacuum tightness-0.080～-mixed discharging 10-20 minute under the 0.095MPa.
Self cure single component autocatalysis cross-linking organosilicon seal glue of the present invention, simplified manufacturing process does not need extra catalyst; Avoid with the big organotin catalysts of toxicity and easily make the xanthochromic titanium complex of product, do not occur the reversion phenomenon under the cross-linked rubber high temperature; Sealing glue solidifying speed is fast, and cured properties is better than existing catalytic type organosilicon sealant; Need not the more expensive gas-phase silica of price and make reinforced filling.
Embodiment
The present invention is a kind of autocatalysis cross-linking organosilicon seal glue, contains: basic glue α, alpha, omega-dihydroxy polysiloxane 100 mass parts, linking agent α-aminomethyl trialkoxy silane 1.2-4.0 mass parts, filler 60-120 mass parts, thinner 60-100 mass parts.
Preferably, α, the alpha, omega-dihydroxy polysiloxane is selected α for use, alpha, omega-dihydroxy polydimethyl siloxane, α, poly-di-ethyl siloxane of alpha, omega-dihydroxy or α, a kind of in the poly-diphenyl siloxane of alpha, omega-dihydroxy, the equal molecular mass of its relative number is 10,000 to 60,000, and preferred value is 10,000 to 30,000.α-aminomethyl trialkoxy silane general formula is R
1NHCH
2Si (OR)
3, R
2NR
3CH
2Si (OR)
3Or NH
2R
4NHCH
2Si (OR)
3, wherein R is a kind of in the alkyl of C1 to C4; R
1A kind of in the alkyl of C4 to C10, the cycloalkyl group; R
2Or R
3A kind of in the alkyl of C3 to C10, R
4Be the alkyl of C2-C10, a kind of in the cycloalkyl group of C4-C8 or the phenyl.Described filler is one or more compound in nano-calcium carbonate, wollastonite, diatomite or the kaolin.Described thinner is normal hexane or normal heptane.
During preparation, at first with α, alpha, omega-dihydroxy polysiloxane 100 mass parts, filler 60-120 mass parts mix to stir, and progressively is warming up to 110-120 ℃, is-0.080 to-0.095MPa condition in vacuum tightness, and vacuum hydro-extraction 45-60 minute, it was standby to be cooled to room temperature.Then under the room temperature with the α-aminomethyl trialkoxy silane of 1.2-4.0 mass parts and the thinner wiring solution-forming of 60-100 mass parts, add α, in the alpha, omega-dihydroxy polysiloxane mixture planetary mixer vacuum tightness-0.080～-mixed discharging can behind the vacuum removal lower-molecular substance 10-20 minute under the 0.095MPa.Above-mentioned stirring can be adopted vacuum planetary mixer or static mixer.
Below come by specific embodiment that the present invention is described further, but the present invention is not limited to this specific examples.
Embodiment 1
With 100 parts of α, alpha, omega-dihydroxy polydimethyl siloxane, 60 parts of nano-calcium carbonates be in vacuum tightness-0.095, mix under 110 ℃ of the temperature, and vacuum hydro-extraction 45 minutes, cool to room temperature, the gained epoxy glue is standby.
With 1.25 parts n-Butyl Amine 99 Union carbide A-162s and 60 parts of normal hexane wiring solution-formings, under normal temperature, vacuum tightness-0.095MPa, mixed 15 minutes with above-mentioned epoxy glue, make the sealing sizing material and pour in the dark 4 millimeters tetrafluoroethylene mould, solidify under the room temperature and press GB/T13477-1992 Test method for building sealants regulation mensuration mechanical properties of vulcanizate after 7 days.
Adopt 80 * 10 * 3mm, inject batten, gluing overlap joint, the shearing resistance of pressing GB/T13477-92 tackiness agent tensile shear strength test organosilicon sealant through PE, the PP of sander surface coarsening.
Adopt 200 * 25 * 0.05mm duralumin sheet, press the stripping strength that GB/T2791-1995 tackiness agent T peeling strength test method is measured organosilicon sealant; Chuck segregation rate 100mm/min.
The thermal stability determination of seal gum carries out on the TG209C of NETZSCH company type thermal gravimetric analyzer, 10 ℃/min of temperature rise rate, N
2Atmosphere.
Every performance of seal gum is as shown in table 1.
Embodiment 2
Adopt 1.38 parts hexahydroaniline Union carbide A-162 to make linking agent, all the other are with application example 1, and every performance of seal gum is as shown in table 1.
Embodiment 3
Adopt 1.53 parts Di-n-Butyl Amine Union carbide A-162 to make linking agent, all the other are with application example 1, and every performance of seal gum is as shown in table 1.
Embodiment 4
Adopt 1.18 parts quadrol Union carbide A-162 to make linking agent, all the other are with application example 1, and every performance of seal gum is as shown in table 1.
Embodiment 5
Adopt 1.46 parts hexanediamine Union carbide A-162 to make linking agent, all the other are with application example 1, and every performance of seal gum is as shown in table 1.
Embodiment 6
Adopt 1.38 parts diethylenetriamine Union carbide A-162 to make linking agent, all the other are with application example 1, and every performance of seal gum is as shown in table 1.
Embodiment 7
Adopt 1.83 parts tetraethylene pentamine Union carbide A-162 to make linking agent, all the other are with application example 1, and every performance of seal gum is as shown in table 1.
Embodiment 8
At first with 100 parts of α, alpha, omega-dihydroxy gathers di-ethyl siloxane, and 100 parts of wollastonites are at vacuum tightness-0.080MPa, mix under 120 ℃ of the temperature, and vacuum hydro-extraction 50 minutes, cool to room temperature, the gained epoxy glue is standby.Then with 3.66 parts tetraethylene pentamine Union carbide A-162 and 100 parts of normal heptane wiring solution-formings and above-mentioned epoxy glue at normal temperatures-mixed 10 minutes under the 0.080MPa vacuum tightness.
Embodiment 9
At first with 100 parts of α, alpha, omega-dihydroxy gathers diphenyl siloxane, and 80 parts of diatomite are at vacuum tightness-0.090MPa, mix under 115 ℃ of the temperature, and vacuum hydro-extraction 60 minutes, cool to room temperature, the gained epoxy glue is standby.Then with 1.93 parts diethylenetriamine Union carbide A-162 and 80 parts of normal heptane wiring solution-formings and above-mentioned epoxy glue at normal temperatures-mixed 20 minutes under the 0.090MPa vacuum tightness.
For the performance of the organosilicon sealant that contrasts autocatalysis cross-linking organosilicon seal glue of the present invention and extra catalyst better, it is as follows that the spy does reference examples: reference examples 1
Adopt 100 parts of α, alpha, omega-dihydroxy polydimethyl siloxane, 60 parts of nano-calcium carbonates, 0.89 part Union carbide A-162,0.005 part of dibutyl tin laurate is made catalyzer, and manufacture method is with application example 1, and every performance of seal gum is as shown in table 1.Reference examples 2
Adopt 0.005 part of titanium complex (peach of immortality chemical plant, Hubei product) to make catalyzer, all the other are with reference examples 1, and every performance of seal gum is as shown in table 1.
From every performance comparison of table 1 seal gum as can be known, the performance of autocatalysis cross-linking organosilicon seal glue is better than catalytic crosslinking type organosilicon sealant.
Every performance comparison of table 1 seal gum
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Reference examples 1 | Reference examples 2 | |
| The set time/hrs cross-linked rubber tensile strength (MPa) cross-linked rubber elongation at break (%) seal gum shearing resistance PE-PE (MPa) PP-PP seal gum stripping strength (N/mm) thermal weight loss 2% temperature (℃) thermal weight loss 50% temperature (℃) | ?8 1.264 695.3 0.2915 0.3408 3.053 372 542 | 8 1.388 751.7 0.3044 0.3501 3.039 377 547 | 6.5 1.334 722.5 0.3099 0.3454 3.220 430 567 | 7 1.375 772.3 0.3140 0.3578 3.170 434 578 | 7 1.435 700.3 0.3115 0.3618 3.214 420 565 | 6 1.466 730.0 0.3231 0.3662 3.549 459 600 | 5.5 1.478 710.6 0.3191 0.3645 3.286 428 612 | 48 1.180 623.2 0.1946 0.2152 1.573 264 482 | 42 1.169 665.5 0.2080 0.2203 1.596 256 464 |
Claims (10)
1. autocatalysis cross-linking organosilicon seal glue is characterized in that containing following component:
Base glue α, the alpha, omega-dihydroxy polysiloxane;
Linking agent α-aminomethyl trialkoxy silane;
Filler and thinner.
2. autocatalysis cross-linking organosilicon seal glue according to claim 1 is characterized in that containing following proportioning component:
Base glue α, alpha, omega-dihydroxy polysiloxane 100 mass parts;
Linking agent α-aminomethyl trialkoxy silane 1.2-4.0 mass parts;
Filler 60-120 mass parts;
Thinner 60-100 mass parts.
3. autocatalysis cross-linking organosilicon seal glue according to claim 1 and 2, it is characterized in that: described α, the alpha, omega-dihydroxy polysiloxane is α, alpha, omega-dihydroxy polydimethyl siloxane, α, poly-di-ethyl siloxane of alpha, omega-dihydroxy or α, a kind of in the poly-diphenyl siloxane of alpha, omega-dihydroxy, the equal molecular mass of its relative number is 10,000 to 60,000.
4. autocatalysis cross-linking organosilicon seal glue according to claim 1 and 2 is characterized in that: described α-aminomethyl trialkoxy silane general formula is R
1NHCH
2Si (OR)
3, R
2NR
3CH
2Si (OR)
3Or NH
2R
4NHCH
2Si (OR)
3
5. autocatalysis cross-linking organosilicon seal glue according to claim 4 is characterized in that: described α-aminomethyl trialkoxy silane, and wherein R is a kind of in the alkyl of C1 to C4; R
1A kind of in the alkyl of C4 to C10, the cycloalkyl group; R
2Or R
3A kind of in the alkyl of C3 to C10, R
4Be the alkyl of C2-C10, a kind of in the cycloalkyl group of C4-C8 or the phenyl.
6. autocatalysis cross-linking organosilicon seal glue according to claim 1 and 2 is characterized in that: described filler is one or more compound in nano-calcium carbonate, wollastonite, diatomite or the kaolin.
7. autocatalysis cross-linking organosilicon seal glue according to claim 1 and 2 is characterized in that: described thinner is normal hexane or normal heptane.
8. the preparation method of an autocatalysis cross-linking organosilicon seal glue is characterized in that may further comprise the steps:
(1) with α, alpha, omega-dihydroxy polysiloxane 100 mass parts, filler 60-120 mass parts are mixed, and are warming up to 110-120 ℃, stir to-0.095MPa condition for-0.080 in vacuum tightness, and vacuum hydro-extraction 45-60 minute, it was standby to be cooled to room temperature;
(2) under the room temperature with the α-aminomethyl trialkoxy silane of 1.2-4.0 mass parts and the thinner wiring solution-forming of 60-100 mass parts, the α that adds step (1), in the alpha, omega-dihydroxy polysiloxane mixture vacuum tightness-0.080～-mixed discharging 10-20 minute under the 0.095MPa.
9. the preparation method of autocatalysis cross-linking organosilicon seal glue according to claim 8 is characterized in that: described stirring employing vacuum planetary mixer or static mixer.
10. the preparation method of autocatalysis cross-linking organosilicon seal glue according to claim 8 is characterized in that: remove lower-molecular substance earlier before the described discharging can.
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| CNB2007100298345A CN100572487C (en) | 2007-08-22 | 2007-08-22 | Autocatalysis cross-linking organosilicon seal glue and preparation method thereof |
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|---|---|---|---|
| CNB2007100298345A CN100572487C (en) | 2007-08-22 | 2007-08-22 | Autocatalysis cross-linking organosilicon seal glue and preparation method thereof |
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|---|---|
| CN101134887A true CN101134887A (en) | 2008-03-05 |
| CN100572487C CN100572487C (en) | 2009-12-23 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665623B (en) * | 2009-10-15 | 2011-07-06 | 成都拓利化工实业有限公司 | Double-component addition self-adhesive silicon rubber |
| CN105802236A (en) * | 2016-04-06 | 2016-07-27 | 苏州甫众塑胶有限公司 | Expansion joint sealing material and preparation method thereof |
| CN106366278A (en) * | 2016-08-30 | 2017-02-01 | 江苏创景科技有限公司 | Synthesis method of alpha type silane terminated polyurethane |
| CN106634803A (en) * | 2016-11-14 | 2017-05-10 | 山东大学 | Autocatalytic and dealcoholized room-temperature vulcanized silicone rubber and preparation method thereof |
| WO2018134124A1 (en) | 2017-01-17 | 2018-07-26 | Akzo Nobel Coatings International B.V. | Foul release coating composition, substrate coated with such coating composition, and use of such coating composition |
| WO2020011839A1 (en) | 2018-07-13 | 2020-01-16 | Akzo Nobel Coatings International B.V. | Tie-coat composition |
| CN113943546A (en) * | 2021-10-28 | 2022-01-18 | 济南汉斯曼时代技术有限公司 | Two-component silicone pouring sealant for electrical components and preparation method thereof |
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2007
- 2007-08-22 CN CNB2007100298345A patent/CN100572487C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665623B (en) * | 2009-10-15 | 2011-07-06 | 成都拓利化工实业有限公司 | Double-component addition self-adhesive silicon rubber |
| CN105802236A (en) * | 2016-04-06 | 2016-07-27 | 苏州甫众塑胶有限公司 | Expansion joint sealing material and preparation method thereof |
| CN106366278A (en) * | 2016-08-30 | 2017-02-01 | 江苏创景科技有限公司 | Synthesis method of alpha type silane terminated polyurethane |
| CN106634803A (en) * | 2016-11-14 | 2017-05-10 | 山东大学 | Autocatalytic and dealcoholized room-temperature vulcanized silicone rubber and preparation method thereof |
| WO2018134124A1 (en) | 2017-01-17 | 2018-07-26 | Akzo Nobel Coatings International B.V. | Foul release coating composition, substrate coated with such coating composition, and use of such coating composition |
| KR20190098261A (en) * | 2017-01-17 | 2019-08-21 | 아크조노벨코팅스인터내셔널비.브이. | Antifouling coating compositions, substrates coated with such coating compositions, and uses of such coating compositions |
| KR102289888B1 (en) | 2017-01-17 | 2021-08-13 | 아크조노벨코팅스인터내셔널비.브이. | Antifouling coating compositions, substrates coated with such coating compositions, and uses of such coating compositions |
| WO2020011839A1 (en) | 2018-07-13 | 2020-01-16 | Akzo Nobel Coatings International B.V. | Tie-coat composition |
| CN113943546A (en) * | 2021-10-28 | 2022-01-18 | 济南汉斯曼时代技术有限公司 | Two-component silicone pouring sealant for electrical components and preparation method thereof |
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|---|---|
| CN100572487C (en) | 2009-12-23 |
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