CN109852260A - A kind of organic silicon pressure-sensitive adhesive and preparation method thereof - Google Patents
A kind of organic silicon pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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- CN109852260A CN109852260A CN201910041848.1A CN201910041848A CN109852260A CN 109852260 A CN109852260 A CN 109852260A CN 201910041848 A CN201910041848 A CN 201910041848A CN 109852260 A CN109852260 A CN 109852260A
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Abstract
The invention discloses a kind of organic silicon pressure-sensitive adhesive and preparation method thereof, which includes the component of following mass fraction: 30-60 parts of hydroxy vinyl based compound;40-70 parts of silane coupling agent containing vinyl;1-2 parts of catalyst;Preparation method are as follows: the hydroxy vinyl based compound, vinyl silanes, catalyst of formula ratio are added in reaction kettle, starts stirring, is heated to 80 DEG C of reaction 2h;90 DEG C of reaction 2h are then heated to, 1h is finally vacuumized at 90 DEG C, stops heating, is cooled to room temperature;Of the invention organic silicon pressure-sensitive adhesive fitting simple glass plate or armorplate glass after high temperature and humidity is handled without degumming, aggravated without peeling force the problem of, using effect is preferable, and preparation process is simple, and raw material is cheap and easy to get, it is easy to accomplish industrialized production.
Description
Technical field
The present invention relates to organic pressure-sensitive gel technical field more particularly to a kind of organic silicon pressure-sensitive adhesive and its preparation sides
Method.
Background technique
Organic pressure-sensitive gel is generally referred to the pressure sensitive adhesive based on organosilicon polymer, or by Organosiliconpolymermodified modified
Acrylic acid and organic-silicon-modified rubber pressure-sensitive adhesive.Compared with traditional acrylate pressure-sensitive adhesive, rubber pressure-sensitive adhesive, it has
There are the performances such as excellent chemical-resistant resistance, water-fast, oil resistant, solvent resistant, high temperature resistant, low temperature resistant, resistance to thermal degradation, resistance to oxidation degradation,
And can with a variety of difficult viscous such as not surface treated polyolefin (BOPP, PET, PE) fluoroplastics of material, polyimides with
And polycarbonate etc. is glued.Wide range of applications, as transformer immersion oil glass adhesive tape, wiring board punching protection, baking vanish are protected
Protect pressure-sensitive gummed paper, the bonding of cell phone lines plate, mobile phone key bonding, high-temperature insulation adhesive tape, mica pressure sensitive film, mobile TV machine screen
Curtain protective film, heat-resistant polyimide adhesive tape etc., over time, the application field of organic pressure-sensitive gel expands rapidly
Exhibition.
But existing organic silicon pressure-sensitive adhesive, adhesive force have limitation, especially attaching element glass high temperature and humidity
Afterwards, it is easy to appear the phenomenon that peeling force aggravates even degumming, about problems rarer document report both at home and abroad.
It is main former that Chinese patent CN108048031A, which discloses one kind by vinyl polysiloxane and hydrogeneous MQ silicone resin,
Expect the organic pressure-sensitive gel of synthesis, which has preferable just glutinous and peeling force, but adhesive force is declined after boiling, shadow
It rings and uses.
Therefore, a kind of fitting simple glass plate or armorplate glass are needed after high temperature and humidity is handled without degumming, without stripping
The organic silicon pressure-sensitive adhesive aggravated from power solves the above problems.
Summary of the invention
Shortcoming present in view of the above technology, the purpose of the present invention is to provide a kind of organic silicon pressure-sensitive adhesives
And preparation method thereof, which is bonded simple glass plate or the armorplate glass nothing after high temperature and humidity is handled
Degumming, without peeling force aggravate the problem of, using effect is more preferable, and preparation process is simple, and raw material is cheap and easy to get, it is easy to accomplish industry
Metaplasia produces.
To achieve the above object, technical scheme is as follows.
A kind of organic silicon pressure-sensitive adhesive, the organic silicon pressure-sensitive adhesive are by the material of the component of following mass fraction
Hybrid reaction is made:
30-60 parts of hydroxy vinyl based compound;
40-70 parts of silane coupling agent containing vinyl;
1-2 parts of catalyst.
It is bonded by hydroxy vinyl based compound with the combination of the silane coupling agent containing vinyl, organic silicon pressure-sensitive adhesive
Simple glass plate or armorplate glass after high temperature and humidity is handled without degumming, aggravated without peeling force the problem of, using effect compared with
It is good.
Further, the hydroxy vinyl based compound is pentaerythritol triallyl ether, two allyl of trimethylolpropane
Any one in base ether, trimethyolol propane monoallyl ether or any combination.
Further, the silane coupling agent containing vinyl is vinyltrimethoxysilane, vinyl triethoxyl
Silane, allyltrimethoxysilanis, methyl allyl acyloxypropyl trimethoxysilane, methacryloxypropyl triethoxy
Any one in silane or any combination.
Further, the catalyst is butyl titanate, any one in isopropyl titanate.
The present invention also provides a kind of preparation methods of organic silicon pressure-sensitive adhesive, comprising the following steps:
Step 1: the hydroxy vinyl based compound, vinyl silanes, catalyst of formula ratio are added in reaction kettle, started
Stirring, is heated to 60-90 DEG C of reaction 1h or more;
Step 2: then heating to 80-100 DEG C of reaction 1h or more, be finally maintained at 80-100 DEG C and vacuumize 0.5h or more,
Then stop heating, be cooled to room temperature.
Further, the hydroxy vinyl based compound is pentaerythritol triallyl ether, two allyl of trimethylolpropane
Any one in base ether, trimethyolol propane monoallyl ether or any combination.
Further, the silane coupling agent containing vinyl is vinyltrimethoxysilane, vinyl triethoxyl
Silane, allyltrimethoxysilanis, methyl allyl acyloxypropyl trimethoxysilane, methacryloxypropyl triethoxy
Any one in silane or any combination.
Further, the catalyst is butyl titanate, any one in isopropyl titanate.
Hydroxy vinyl based compound in a kind of organic silicon pressure-sensitive adhesive provided by the invention can provide hydroxyl and second
Alkenyl, medium vinyl can react with the containing hydrogen silicone oil in silica gel, promote it is bonding with silica gel, hydroxyl with it is silane coupled
Ester exchange reaction occurs under the catalysis of titanate esters for the alkoxy in agent to forming uniform compound, the alcoxyl in the compound
Base can generate adhesive effect with substrate, and so that it will not degumming, the vinyl in silane coupling agent can also be with containing in silica gel
Hydrogen silicone oil reacts, and inhibits climbing for peeling force, so organic silicon pressure-sensitive adhesive fitting simple glass plate or steel
Change glass plate after high temperature and humidity is handled without degumming, without peeling force aggravate the problem of, using effect is preferable;It is provided by the invention
Preparation process is simple, and raw material is cheap and easy to get, it is easy to accomplish industrialized production.
Specific embodiment
In order to which the purpose of the present invention, technical solution and beneficial effect is more clearly understood, the present invention is carried out further
It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
To achieve the above object, the present invention provides a kind of organic silicon pressure-sensitive adhesive, and the organic silicon pressure-sensitive adhesive is
It is made of the material hybrid reaction of the component of following mass fraction:
30-60 parts of hydroxy vinyl based compound;
40-70 parts of silane coupling agent containing vinyl;
1-2 parts of catalyst.
In the present invention, organic silicon pressure-sensitive adhesive fitting simple glass plate or armorplate glass are by high temperature and humidity
The problem of after reason without degumming, without peeling force exacerbation, using effect is preferable.
In the present embodiment, hydroxy vinyl based compound is pentaerythritol triallyl ether, two allyl of trimethylolpropane
Any one in base ether, trimethyolol propane monoallyl ether or any combination.
In the present embodiment, the silane coupling agent containing vinyl is vinyltrimethoxysilane, vinyl triethoxyl
Silane, allyltrimethoxysilanis, methyl allyl acyloxypropyl trimethoxysilane, methacryloxypropyl triethoxy
Any one in silane or any combination.
In the present embodiment, catalyst is butyl titanate, any one in isopropyl titanate.
The present invention also provides a kind of preparation methods of organic silicon pressure-sensitive adhesive, comprising the following steps:
Step 1: the hydroxy vinyl based compound, vinyl silanes, catalyst of formula ratio are added in reaction kettle, started
Stirring, is heated to 60-90 DEG C of reaction 1h or more;
Step 2: then heating to 80-100 DEG C of reaction 1h or more, be finally maintained at 80-100 DEG C and vacuumize 0.5h or more,
Then stop heating, be cooled to room temperature.
Compared with prior art, a kind of organic silicon pressure-sensitive adhesive fitting simple glass plate or tempering glass provided by the invention
Glass plate after high temperature and humidity is handled without degumming, without peeling force aggravate the problem of, using effect is preferable;Preparation provided by the invention
Simple process, raw material are cheap and easy to get, it is easy to accomplish industrialized production.
Organic silicon pressure-sensitive adhesive of the invention and preparation method thereof is carried out specifically below in conjunction with specific embodiment
It is bright.
Embodiment 1
Step 1: by 30 parts of pentaerythritol triallyl ethers, 70 parts of vinyltrimethoxysilanes and 1 part of butyl titanate
It is added in reaction kettle, starts stirring, be heated to 80 DEG C of reaction 2h;
Step 2: then heating to 90 DEG C of reaction 2h, and 1h is finally vacuumized at 90 DEG C, stops heating, is cooled to room temperature, and surveys
It is as shown in table 1 to try performance.
Embodiment 2
Step 1: by 50 parts of pentaerythritol triallyl ethers, 50 parts of vinyltrimethoxysilanes and 1 part of butyl titanate
It is added in reaction kettle, starts stirring, be heated to 80 DEG C of reaction 2h;
Step 2: then heating to 90 DEG C of reaction 2h, and 1h is finally vacuumized at 90 DEG C, stops heating, is cooled to room temperature, and surveys
It is as shown in table 1 to try performance.
Embodiment 3
Step 1: by 60 parts of pentaerythritol triallyl ethers, 40 parts of vinyltrimethoxysilanes and 2 parts of butyl titanates
It is added in reaction kettle, starts stirring, be heated to 80 DEG C of reaction 2h;
Step 2: then heating to 90 DEG C of reaction 2h, and 1h is finally vacuumized at 90 DEG C, stops heating, is cooled to room temperature, and surveys
It is as shown in table 1 to try performance.
Embodiment 4
Step 1: by 40 parts of pentaerythritol triallyl ethers, 60 parts of vinyltrimethoxysilanes and 1 part of butyl titanate
It is added in reaction kettle, starts stirring, be heated to 80 DEG C of reaction 2h;
Step 2: then heating to 90 DEG C of reaction 2h, and 1h is finally vacuumized at 90 DEG C, stops heating, is cooled to room temperature, and surveys
It is as shown in table 1 to try performance.
Embodiment 5
Step 1: by 50 parts of pentaerythritol triallyl ethers, 50 parts of vinyltrimethoxysilanes and 2 parts of butyl titanates
It is added in reaction kettle, starts stirring, be heated to 80 DEG C of reaction 2h;
Step 2: then heating to 90 DEG C of reaction 2h, and 1h is finally vacuumized at 90 DEG C, stops heating, is cooled to room temperature, and surveys
It is as shown in table 1 to try performance.
Embodiment 6
Step 1: by 50 parts of pentaerythritol triallyl ethers, 50 parts of vinyltrimethoxysilanes and 1 part of butyl titanate
It is added in reaction kettle, starts stirring, be heated to 60 DEG C of reaction 2h;
Step 2: then heating to 80 DEG C of reaction 2h, and 1h is finally vacuumized at 80 DEG C, stops heating, is cooled to room temperature, and surveys
It is as shown in table 1 to try performance.
Embodiment 7
Step 1: by 60 parts of pentaerythritol triallyl ethers, 40 parts of vinyltrimethoxysilanes and 2 parts of butyl titanates
It is added in reaction kettle, starts stirring, be heated to 90 DEG C of reaction 2h;
Step 2: then heating to 100 DEG C of reaction 2h, and 1h is finally vacuumized at 100 DEG C, stops heating, is cooled to room temperature,
Test performance is as shown in table 1.
By organic silicon pressure-sensitive adhesive obtained by above-described embodiment 1-7 with KL-2610B (Kang Libangke in the prior art
The silica gel glue of skill Co., Ltd) quality 1% addition, be added 20% ethyl acetate, 1% Pt4000 (Kang Libang science and technology
The platinum water of Co., Ltd), it after mixing evenly, is coated in the PET base material of 50 μ thickness, 140 DEG C solidify 1 minute.After solidification
PET protection film is cut into breadth 25mm, and the test bars of long 100mm are attached in element glass, places after twenty minutes, test removing
Power is denoted as peeling force 1, the results are shown in Table 1;In addition the test-strips being attached in element glass are placed in high temperature and humidity case, 85
DEG C, under conditions of 85%RH, 5d is tested, after taking-up, is placed 20 minutes, is tested peeling force, be denoted as peeling force 2, see whether to take off
Glue the results are shown in Table 1.Comparative example is the product that organic silicon pressure-sensitive adhesive of the invention is not added.
Table 1 is the test performance parameter comparison table of embodiment 1-7 and comparative example
As shown in Table 1, for organic silicon pressure-sensitive adhesive of the invention after synthesis, the vinyl and alkoxy included can
To play bonding effect, and the use of vinyl alkoxy silane to pressure sensitive adhesive and substrate well, largely inhibit
Climbing for peeling force, so the use of the organic silicon pressure-sensitive adhesive can be guarantee adhesive force under conditions of, peeling force warp
After crossing high temperature and humidity test, it there is no and climb, satisfy the use demand well.
The above is only several preferred embodiments of the invention, are not intended to limit the invention, it is all in spirit of the invention and
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within principle.
Claims (8)
1. a kind of organic silicon pressure-sensitive adhesive, it is characterised in that the organic silicon pressure-sensitive adhesive is by the group of following mass fraction
The material hybrid reaction divided is made:
30-60 parts of hydroxy vinyl based compound;
40-70 parts of silane coupling agent containing vinyl;
1-2 parts of catalyst.
2. organic silicon pressure-sensitive adhesive according to claim 1, it is characterised in that the hydroxy vinyl based compound is season
Penta tetrol triallyl ether, trimethylolpropane allyl ether, any one in trimethyolol propane monoallyl ether
Or any combination.
3. organic silicon pressure-sensitive adhesive according to claim 1, it is characterised in that the silane coupling agent containing vinyl
For vinyltrimethoxysilane, vinyltriethoxysilane, allyltrimethoxysilanis, methacryloxypropyl three
Any one in methoxy silane, methacryloxypropyl triethoxysilane or any combination.
4. organic silicon pressure-sensitive adhesive according to claim 1, it is characterised in that the catalyst is butyl titanate, titanium
Any one in isopropyl propionate.
5. a kind of preparation method of organic silicon pressure-sensitive adhesive, it is characterised in that the following steps are included:
Step 1: the hydroxy vinyl based compound, vinyl silanes, catalyst of formula ratio being added in reaction kettle, stirring is started,
It is heated to 60-90 DEG C of reaction 1h or more;
Step 2: 80-100 DEG C of reaction 1h or more is then heated to, 80-100 DEG C is finally maintained at and vacuumizes 0.5h or more, then
Stop heating, is cooled to room temperature.
6. the preparation method of organic silicon pressure-sensitive adhesive according to claim 5, it is characterised in that the hydroxyvinyl
Compound is pentaerythritol triallyl ether, in trimethylolpropane allyl ether, trimethyolol propane monoallyl ether
Any one or any combination.
7. the preparation method of organic silicon pressure-sensitive adhesive according to claim 5, it is characterised in that described containing vinyl
Silane coupling agent is vinyltrimethoxysilane, vinyltriethoxysilane, allyltrimethoxysilanis, metering system
Any one in monomethacryloxypropyl trimethoxy silane, methacryloxypropyl triethoxysilane or any combination.
8. the preparation method of organic silicon pressure-sensitive adhesive according to claim 5, it is characterised in that the catalyst is titanium
Any one in sour four butyl esters, isopropyl titanate.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113845861A (en) * | 2021-09-30 | 2021-12-28 | 苏州世华新材料科技股份有限公司 | Low-climbing organic silicon protective film and preparation method thereof |
CN114539947A (en) * | 2022-03-22 | 2022-05-27 | 浙江新安化工集团股份有限公司 | Diluent, organic silicon pressure-sensitive adhesive and preparation method thereof |
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CN103965479A (en) * | 2013-01-31 | 2014-08-06 | 成都硅田科技有限公司 | Preparation method of polymer precursor bridged polysilsesquioxane silane-coupling agent |
CN105131669A (en) * | 2015-08-13 | 2015-12-09 | 岳胜武 | One-component treatment agent for treating PC adhesion addition type silicone rubber, and preparation method thereof |
CN109054725A (en) * | 2018-06-28 | 2018-12-21 | 深圳市康利邦科技有限公司 | A kind of one-component heat cure glue that temperature tolerance is good |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102994004A (en) * | 2012-11-29 | 2013-03-27 | 华南理工大学 | Reinforcing addition type liquid silicone rubber bonding accelerant and preparation method and application thereof |
CN103965479A (en) * | 2013-01-31 | 2014-08-06 | 成都硅田科技有限公司 | Preparation method of polymer precursor bridged polysilsesquioxane silane-coupling agent |
CN105131669A (en) * | 2015-08-13 | 2015-12-09 | 岳胜武 | One-component treatment agent for treating PC adhesion addition type silicone rubber, and preparation method thereof |
CN109054725A (en) * | 2018-06-28 | 2018-12-21 | 深圳市康利邦科技有限公司 | A kind of one-component heat cure glue that temperature tolerance is good |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113845861A (en) * | 2021-09-30 | 2021-12-28 | 苏州世华新材料科技股份有限公司 | Low-climbing organic silicon protective film and preparation method thereof |
CN114539947A (en) * | 2022-03-22 | 2022-05-27 | 浙江新安化工集团股份有限公司 | Diluent, organic silicon pressure-sensitive adhesive and preparation method thereof |
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Application publication date: 20190607 |