CN105086927B - A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive and preparation method thereof - Google Patents
A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive and preparation method thereof Download PDFInfo
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- CN105086927B CN105086927B CN201510481078.4A CN201510481078A CN105086927B CN 105086927 B CN105086927 B CN 105086927B CN 201510481078 A CN201510481078 A CN 201510481078A CN 105086927 B CN105086927 B CN 105086927B
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Abstract
The invention discloses a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, in parts by weight, including following components：20 60 parts of vinyldimethicone, α, 20 50 parts alkoxy end-capped ω of dimethyl silicone polymer, 30 50 parts of hexamethyl cyclotrisiloxane, 20 30 parts of MQ organic siliconresins, 15 30 parts of PAMA, 5 15 parts of polyborosiloxane, 25 parts of nano boron carbide, 13 parts of nano-silicon nitride, 0.5 1.5 parts of crosslinking agent, 12 parts of dispersant.The invention also discloses the preparation method of the organic pressure-sensitive gel.The pressure sensitive adhesive cementitiousness is strong, with good chemical inertness, long service life, while having prominent moisture-proof and electrical property, high and low temperature resistance is excellent, tasteless, nontoxic, and preparation method is simple, economic and environment-friendly.
Description
Technical field：
The present invention relates to pressure sensitive adhesive technical field, a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive is specifically related to.
Background technology：
The demand of pressure sensitive adhesive was always maintained at faster growth rate in recent years, and the development of high-performance special pressure sensitive adhesive is particularly
Rapidly, produce and sell and be persistently substantially increased, in the world as sales volume highest pressure sensitive adhesive kind.But in China,
By technical restriction, its application is far below world level, the continuous improvement with performance, it is contemplated that the growth of such pressure sensitive adhesive is still
To be most fast；And traditional strap pressure sensitive adhesive increasess slowly, profit is gradually because market is already ripe and approaches to saturation
It is low.
Organic pressure-sensitive gel is a kind of new tool adhesive with broad prospects for development, and it not only must with pressure sensitive adhesive
The good adhesion strength and tack of palpus, also with many unique performances：(1) have to high energy and low energy surface material good
Good adhesiveness, therefore it is to untreated difficult adhesion material, such as polytetrafluoroethylene (PTFE), polyimides, makrolon have compared with
Good adhesive property；(2) there is prominent high and low temperature resistance, its adhesion strength is remained in that under high temperature and low temperature and flexible
Property；(3) there is good chemical inertness, long service life, while having prominent moisture-proof and electrical property；(4) have certain
Liquid permeable and biologically inert.While with scientific progress, also Novel adhesive is carried in electric field
Go out higher more rigorous actual requirement, especially its resistance to elevated temperatures is of interest by many professionals and researcher,
The temperature classification of existing organic pressure-sensitive gel can not meet the requirement of practical application, it is necessary to be modified to it.
Chinese patent (201110006971.3) discloses a kind of solvent-free organic silicon pressure sensitive adhesive, including end group is alkenyl
Dimethyl silicone polymer, end group be hydroxyl dimethyl silicone polymer, MQ resins, polyisobutene, diluent, crosslinking agent and platinum
Catalyst.The organic pressure-sensitive gel, it is nontoxic with good tack, long-lasting, but its poor heat resistance, and catalyst adopts
With platinum, production cost height.
The content of the invention：
It is an object of the invention to provide a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, its cementitiousness is strong, has
Good chemical inertness, long service life, while having prominent moisture-proof and electrical property, high and low temperature resistance is excellent, tasteless,
It is nontoxic.
It is a further object to provide the preparation method of the organic pressure-sensitive gel.
To achieve the above object, the present invention uses following technical scheme：
A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, in parts by weight, including following components：
20-60 parts of vinyldimethicone,
α, ω-alkoxy end-capped 20-50 parts of dimethyl silicone polymer,
30-50 parts of hexamethyl cyclotrisiloxane,
20-30 parts of MQ organic siliconresins,
15-30 parts of PAMA,
5-15 parts of polyborosiloxane,
2-5 parts of nano boron carbide, 1-3 parts of nano-silicon nitride,
0.5-1.5 parts of crosslinking agent, 1-2 parts of dispersant.
As the preferred of above-mentioned technical proposal, a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, in parts by weight, bag
Include following components：
50 parts of vinyldimethicone,
α, ω-alkoxy end-capped 35 parts of dimethyl silicone polymer,
40 parts of hexamethyl cyclotrisiloxane,
28 parts of MQ organic siliconresins,
15 parts of PAMA,
10 parts of polyborosiloxane,
3 parts of nano boron carbide, 2 parts of nano-silicon nitride,
1 part of crosslinking agent, 1.5 parts of dispersant.
As the preferred of above-mentioned technical proposal, in the MQ organic siliconresins, M/Q is 0.7-0.9.
As the preferred of above-mentioned technical proposal, the particle size of the nano boron carbide is 10-20nm.
As the preferred of above-mentioned technical proposal, the density of the nano-silicon nitride is 1.5-2.5g/cm3, Mohs' hardness is
9-9.5, particle size is 10-20nm.
As the preferred of above-mentioned technical proposal, the crosslinking agent is MTMS, gamma-aminopropyl-triethoxy
One in silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane
Plant or a variety of mixing.
As the preferred of above-mentioned technical proposal, the dispersant be trimethyl silicane alkoxy esters of silicon acis, esters of silicon acis coupling agent,
One or more mixing in connection boric acid pinacol ester.
A kind of preparation method of inorganic nano-filler modified organic silicon pressure sensitive adhesive, comprises the following steps：
(1) MQ organic siliconresins are prepared；
(2) the MQ organic siliconresins and vinyldimethicone, α for preparing step (1), ω-alkoxy end-capped
Dimethyl silicone polymer, hexamethyl cyclotrisiloxane, polyborosiloxane, PAMA be uniformly mixed, turn
Move at autoclave, 80-100 DEG C, mix 1-2h, obtain blend glue stuff；
(3) nano boron carbide is continuously added in the blend glue stuff obtained to step (2), it is nano-silicon nitride, crosslinking agent, scattered
Agent, is uniformly mixed, ultrasound 2-3h under 500-1000W power, at 150-160 DEG C, solidifies 1-2h, obtains inorganic nano-filler
Modified organic silicon pressure sensitive adhesive.
As the preferred of above-mentioned technical proposal, ultrasonic power described in step (2) is 800W, and the ultrasonic time is
1.5h。
Compared with prior art, the invention has the advantages that：
(1) the product non-volatility solvent, nontoxic, tasteless, is conducive to environmental protection；
(2) present invention adds polyborosiloxane, introduces boron atom, significantly during organic pressure-sensitive gel is prepared
The adhesive property of organic pressure-sensitive gel is improved, its peel strength is also effectively improved；
(3) addition of PAMA, substantially increases the degree of cross linking of pressure sensitive adhesive, so that its adhesive property is significantly
Improve, with excellent resistance to elevated temperatures；
(4) nano boron carbide, nano-silicon nitride have a higher heat resistance, good stability, and it passes through dispersant, stable
It is present in organic pressure-sensitive gel, is improved its heat resistance.
Embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solution
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, with parts by weight, including following components：
20 parts of vinyldimethicone,
α, ω-alkoxy end-capped 20 parts of dimethyl silicone polymer,
30 parts of hexamethyl cyclotrisiloxane,
20 parts of MQ organic siliconresins, 15 parts of PAMA,
5 parts of polyborosiloxane, 2 parts of nano boron carbide, 1 part of nano-silicon nitride,
0.5 part of crosslinking agent, 1 part of dispersant.
Its preparation method comprises the following steps：
(1) MQ organic siliconresins are prepared；
(2) the MQ organic siliconresins and vinyldimethicone, α for preparing step (1), ω-alkoxy end-capped
Dimethyl silicone polymer, hexamethyl cyclotrisiloxane, polyborosiloxane, PAMA be uniformly mixed, turn
Move at autoclave, 80 DEG C, mix 1h, obtain blend glue stuff；
(3) nano boron carbide is continuously added in the blend glue stuff obtained to step (2), it is nano-silicon nitride, crosslinking agent, scattered
Agent, is uniformly mixed, ultrasound 2h under 500W power, at 150 DEG C, solidifies 1h, obtains inorganic nano-filler modified organic silicon pressure
Quick glue.
Embodiment 2
A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, with parts by weight, including following components：
60 parts of vinyldimethicone,
α, ω-alkoxy end-capped 50 parts of dimethyl silicone polymer,
50 parts of hexamethyl cyclotrisiloxane,
30 parts of MQ organic siliconresins, 30 parts of PAMA,
15 parts of polyborosiloxane, 5 parts of nano boron carbide, 3 parts of nano-silicon nitride,
1.5 parts of crosslinking agent, 2 parts of dispersant.
Its preparation method comprises the following steps：
(1) MQ organic siliconresins are prepared；
(2) the MQ organic siliconresins and vinyldimethicone, α for preparing step (1), ω-alkoxy end-capped
Dimethyl silicone polymer, hexamethyl cyclotrisiloxane, polyborosiloxane, PAMA be uniformly mixed, turn
Move at autoclave, 100 DEG C, mix 2h, obtain blend glue stuff；
(3) nano boron carbide is continuously added in the blend glue stuff obtained to step (2), it is nano-silicon nitride, crosslinking agent, scattered
Agent, is uniformly mixed, ultrasound 3h under 1000W power, at 160 DEG C, solidifies 2h, obtains inorganic nano-filler modified organic silicon pressure
Quick glue.
Embodiment 3
A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, with parts by weight, including following components：
30 parts of vinyldimethicone,
α, ω-alkoxy end-capped 30 parts of dimethyl silicone polymer,
35 parts of hexamethyl cyclotrisiloxane,
22 parts of MQ organic siliconresins, 18 parts of PAMA,
7 parts of polyborosiloxane, 3 parts of nano boron carbide, 1.5 parts of nano-silicon nitride,
0.7 part of crosslinking agent, 1.2 parts of dispersant.
Its preparation method comprises the following steps：
(1) MQ organic siliconresins are prepared；
(2) the MQ organic siliconresins and vinyldimethicone, α for preparing step (1), ω-alkoxy end-capped
Dimethyl silicone polymer, hexamethyl cyclotrisiloxane, polyborosiloxane, PAMA be uniformly mixed, turn
Move at autoclave, 85 DEG C, mix 1.2h, obtain blend glue stuff；
(3) nano boron carbide is continuously added in the blend glue stuff obtained to step (2), it is nano-silicon nitride, crosslinking agent, scattered
Agent, is uniformly mixed, ultrasound 2.2h under 600W power, at 155 DEG C, solidifies 1.2h, obtains inorganic nano-filler modification organic
Silicon pressure sensitive adhesive.
Embodiment 4
A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, with parts by weight, including following components：
40 parts of vinyldimethicone,
α, ω-alkoxy end-capped 35 parts of dimethyl silicone polymer,
38 parts of hexamethyl cyclotrisiloxane,
24 parts of MQ organic siliconresins, 20 parts of PAMA,
9 parts of polyborosiloxane, 3.5 parts of nano boron carbide, 1.8 parts of nano-silicon nitride,
0.9 part of crosslinking agent, 1.4 parts of dispersant.
Its preparation method comprises the following steps：
(1) MQ organic siliconresins are prepared；
(2) the MQ organic siliconresins and vinyldimethicone, α for preparing step (1), ω-alkoxy end-capped
Dimethyl silicone polymer, hexamethyl cyclotrisiloxane, polyborosiloxane, PAMA be uniformly mixed, turn
Move at autoclave, 90 DEG C, mix 1.4h, obtain blend glue stuff；
(3) nano boron carbide is continuously added in the blend glue stuff obtained to step (2), it is nano-silicon nitride, crosslinking agent, scattered
Agent, is uniformly mixed, ultrasound 2.4h under 700W power, at 150 DEG C, solidifies 1.4h, obtains inorganic nano-filler modification organic
Silicon pressure sensitive adhesive.
Embodiment 5
A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, with parts by weight, including following components：
45 parts of vinyldimethicone,
α, ω-alkoxy end-capped 40 parts of dimethyl silicone polymer,
40 parts of hexamethyl cyclotrisiloxane,
26 parts of MQ organic siliconresins, 25 parts of PAMA,
11 parts of polyborosiloxane, 4 parts of nano boron carbide, 2 parts of nano-silicon nitride,
1.1 parts of crosslinking agent, 1.6 parts of dispersant.
Its preparation method comprises the following steps：
(1) MQ organic siliconresins are prepared；
(2) the MQ organic siliconresins and vinyldimethicone, α for preparing step (1), ω-alkoxy end-capped
Dimethyl silicone polymer, hexamethyl cyclotrisiloxane, polyborosiloxane, PAMA be uniformly mixed, turn
Move at autoclave, 80 DEG C, mix 1.6h, obtain blend glue stuff；
(3) nano boron carbide is continuously added in the blend glue stuff obtained to step (2), it is nano-silicon nitride, crosslinking agent, scattered
Agent, is uniformly mixed, ultrasound 2.6h under 800W power, at 155 DEG C, solidifies 1.6h, obtains inorganic nano-filler modification organic
Silicon pressure sensitive adhesive.
Embodiment 6
A kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, with parts by weight, including following components：
55 parts of vinyldimethicone,
α, ω-alkoxy end-capped 45 parts of dimethyl silicone polymer,
45 parts of hexamethyl cyclotrisiloxane,
28 parts of MQ organic siliconresins, 25 parts of PAMA,
13 parts of polyborosiloxane, 4.5 parts of nano boron carbide, 2.8 parts of nano-silicon nitride,
1.3 parts of crosslinking agent, 1.8 parts of dispersant.
Its preparation method comprises the following steps：
(1) MQ organic siliconresins are prepared；
(2) the MQ organic siliconresins and vinyldimethicone, α for preparing step (1), ω-alkoxy end-capped
Dimethyl silicone polymer, hexamethyl cyclotrisiloxane, polyborosiloxane, PAMA be uniformly mixed, turn
Move at autoclave, 90 DEG C, mix 1.8h, obtain blend glue stuff；
(3) nano boron carbide is continuously added in the blend glue stuff obtained to step (2), it is nano-silicon nitride, crosslinking agent, scattered
Agent, is uniformly mixed, ultrasound 2.8h under 900W power, at 160 DEG C, solidifies 1.8h, obtains inorganic nano-filler modification organic
Silicon pressure sensitive adhesive.
Performance test is carried out to the organic pressure-sensitive gel that the present invention is provided below.
(1) tack
Tested according to GB/T 4852-2002；
(2) viscosity is held
Tested according to GB/T 4851-1998；
(3) 180 ° of peel strengths
Tested according to GB/T 2792-1998.
Table 1
From the point of view of table 1, the organic pressure-sensitive gel that provides of the present invention has excellent adhesive property and peel strength.
Claims (8)
1. a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive, it is characterised in that in parts by weight, including following components：
20-60 parts of vinyldimethicone,
α, ω-alkoxy end-capped 20-50 parts of dimethyl silicone polymer,
30-50 parts of hexamethyl cyclotrisiloxane,
20-30 parts of MQ organic siliconresins,
15-30 parts of PAMA,
5-15 parts of polyborosiloxane,
2-5 parts of nano boron carbide, 1-3 parts of nano-silicon nitride,
0.5-1.5 parts of crosslinking agent, 1-2 parts of dispersant；
Its preparation method comprises the following steps：
(1) MQ organic siliconresins are prepared；
(2) the MQ organic siliconresins and vinyldimethicone, α for preparing step (1), ω's-alkoxy end-capped is poly-
Dimethyl siloxane, hexamethyl cyclotrisiloxane, polyborosiloxane, PAMA are uniformly mixed, and are transferred to
Autoclave, at 80-100 DEG C, mixes 1-2h, obtains blend glue stuff；
(3) nano boron carbide, nano-silicon nitride, crosslinking agent, dispersant are continuously added in the blend glue stuff obtained to step (2),
It is uniformly mixed, ultrasound 2-3h under 500-1000W power, at 150-160 DEG C, solidifies 1-2h, obtain inorganic nano-filler and change
Property organic pressure-sensitive gel.
2. a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive as claimed in claim 1, it is characterised in that with parts by weight
Meter, including following components：
50 parts of vinyldimethicone,
α, ω-alkoxy end-capped 35 parts of dimethyl silicone polymer,
40 parts of hexamethyl cyclotrisiloxane,
28 parts of MQ organic siliconresins,
15 parts of PAMA,
10 parts of polyborosiloxane,
3 parts of nano boron carbide, 2 parts of nano-silicon nitride,
1 part of crosslinking agent, 1.5 parts of dispersant.
3. a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive as claimed in claim 1, it is characterised in that the MQ is organic
In silicones, M/Q is 0.7-0.9.
4. a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive as claimed in claim 1, it is characterised in that the nano-sized carbon
The particle size for changing boron is 10-20nm.
5. a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive as claimed in claim 1, it is characterised in that the nanometer nitrogen
The density of SiClx is 1.5-2.5g/cm3, Mohs' hardness is 9-9.5, and particle size is 10-20nm.
6. a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive as claimed in claim 1, it is characterised in that the crosslinking agent
For MTMS, gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-
One or more mixing in (methacryloxypropyl) propyl trimethoxy silicane.
7. a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive as claimed in claim 1, it is characterised in that the dispersant
For the one or more mixing in trimethyl silicane alkoxy esters of silicon acis, esters of silicon acis coupling agent, connection boric acid pinacol ester.
8. a kind of inorganic nano-filler modified organic silicon pressure sensitive adhesive as claimed in claim 1, it is characterised in that in step (2)
The ultrasonic power is 800W, and the ultrasonic time is 1.5h.
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| CN106701012B (en) * | 2017-01-11 | 2020-10-02 | 广州天赐有机硅科技有限公司 | Light-weight heat-conducting organic silicon pouring sealant base rubber material, composition and preparation method of light-weight heat-conducting organic silicon pouring sealant base rubber material |
| CN111171753A (en) * | 2020-02-17 | 2020-05-19 | 宁国市千洪电子有限公司 | Double-sided adhesive tape convenient to wind and preparation method thereof |
| CN113265222B (en) * | 2021-05-27 | 2023-03-17 | 河南守真电子科技有限公司 | Polymer moisture-proof fireproof plugging composite material and use method thereof |
| CN113528078A (en) * | 2021-07-09 | 2021-10-22 | 深圳市哈深智材科技有限公司 | Pressure-sensitive conductive slurry and preparation method and application thereof |
| CN113801627A (en) * | 2021-11-01 | 2021-12-17 | 苏州达同新材料有限公司 | Organic silicon adhesive sealant and preparation method thereof |
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|---|---|---|---|---|
| CN1431255A (en) * | 2003-01-28 | 2003-07-23 | 南京师范大学 | Luminous nano composite material and its preparing method |
| CN101302421A (en) * | 2008-05-29 | 2008-11-12 | 海龙艾默生（镇江）能源科技有限公司 | Elastic fireproof sealant and preparation thereof |
| CN104031603A (en) * | 2014-05-26 | 2014-09-10 | 中科院广州化学有限公司 | High-heat-conductivity boroheteropolysiloxane potting adhesive and preparation method thereof |
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| US20140005304A1 (en) * | 2012-07-02 | 2014-01-02 | Baker Hughes Incorporated | Nanocomposite and method of making the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431255A (en) * | 2003-01-28 | 2003-07-23 | 南京师范大学 | Luminous nano composite material and its preparing method |
| CN101302421A (en) * | 2008-05-29 | 2008-11-12 | 海龙艾默生（镇江）能源科技有限公司 | Elastic fireproof sealant and preparation thereof |
| CN104031603A (en) * | 2014-05-26 | 2014-09-10 | 中科院广州化学有限公司 | High-heat-conductivity boroheteropolysiloxane potting adhesive and preparation method thereof |
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