CN101560372A - Method for preparing one-step molding organic silicon self-adhesive pressure sensitive adhesive - Google Patents
Method for preparing one-step molding organic silicon self-adhesive pressure sensitive adhesive Download PDFInfo
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- CN101560372A CN101560372A CNA2009100383826A CN200910038382A CN101560372A CN 101560372 A CN101560372 A CN 101560372A CN A2009100383826 A CNA2009100383826 A CN A2009100383826A CN 200910038382 A CN200910038382 A CN 200910038382A CN 101560372 A CN101560372 A CN 101560372A
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Abstract
The invention discloses a method for preparing a one-step molding organic silicon self-adhesive pressure sensitive adhesive. The method is characterized by comprising the following steps: firstly, preparing materials by the following compositions according to the parts by weight: methyl vinyl silicone rubber:white carbon black:silicon micropowder:hydroxyl silicon oil:pressure sensitive adhesive resin:methyl silicone oil=(10-90) parts:(1-50) parts:(10-50) parts:(0.1-3) parts:(4-40) parts:(10-90) parts; secondly, adding the compositions into a reactor which is provided with a stainless steel stirring paddle, a motor and a heating system; thirdly, mixing the methyl vinyl silicone rubber, the pressure sensitive adhesive resin and the methyl silicone oil at normal temperature to be heated to banburying for 1 to 3 hours; finally, pumping for 0.5 to 2 hours, and discharging. The method has the advantages of simple process, environmental protection, wide production application and the like.
Description
Technical field
The present invention relates to chemical technology field, more particularly relate to a kind of preparation method of organic silicon self-adhesive pressure sensitive adhesive.
Background technology
At present, organosilicon material is the novel material project of country's " 95 " " 15 " emphasis research and development, and in recent years, many R﹠D institutions and enterprise constantly organized human and material resources, and this brand-new material is developed, studied and applies.Organo-silicone rubber has insulation, waterproof, anti-salt fog, properties such as nontoxic, no burn into is high temperature resistant, low temperature, anti-marquis, so material is used widely in fields such as space flight, electric power, building, communication, electrical equipment, automatization, chemical industry, metallurgy, automobile making, medicine instrument and weaving.The complete processing of existing organic pressure-sensitive gel all is on original base material, coating, the baking of carrying out one or many with pressure-sensitive adhesive form, product performance are general, not enough environmental protection, after losing viscosity during use, can't recover, cause waste, and if things go on like this, easily environment is caused a large amount of pollutions.
Summary of the invention
Purpose of the present invention is exactly in order to solve the deficiency of prior art, and a kind of organic pressure-sensitive gel and the once shaped preparation method thereof with good cohesive force, performance index excellence who provides.
The present invention adopts following technical solution to realize above-mentioned purpose:
The preparation method of one-step molding organic silicon self-adhesive pressure sensitive adhesive is characterized in that, its preparation method's step is; At first, proportion ingredient by following component, in weight part ratio, methyl vinyl silicone rubber: white carbon black: silicon powder: hydroxy silicon oil: pressure sensitive adhesive portions of resin methyl-silicone oil=(10～90) part: (1～50) part: (10～50) part: (0.1～3) part: (4～40) part: (10～90) part; Add above-mentioned batching then in the reactor of being furnished with stainless steel stirring arm, motor and heating system, mix under the normal temperature of will preparing burden, the banburying 1～3 hour that heats up was again found time 0.5～2 hour at last, and discharging gets final product, and drop temperature is controlled at more than 150 ℃.
Described methyl vinyl silicone rubber is that contents of ethylene is 0.01～0.24%, and molecular weight is 45～700,000.
Described white carbon black is that specific surface area (BET method) is 200 ± 25m
2/ g, average primary particle diameter are the thermal silica of 12～14Nm.
Described silicon powder is general filler level silicon powder.
Described hydroxy silicon oil is that hydroxy radical content is 5～12% silicone oil.
Described pressure sensitive adhesive resin is a methyl MQ resin, and the M/Q ratio is 0.5～1.2.
Described methyl-silicone oil is that viscosity is 5000～200000CS.
The beneficial effect that the present invention adopts above-mentioned technical solution to reach is:
One, the organic pressure-sensitive gel of prepared of the present invention is to add the organosilicon binding agent in organosilicon material is produced, make it fully contact, react with base material, has good cohesive force after the base material sulfuration, and the organic pressure-sensitive gel that this method is produced uses the back to descend as viscosity, after the available tap water flushing, viscosity is recovered as before.
Two, preparation method of the present invention is fairly simple, adopts the production technique of general rubber unvulcanizate, and the system temperature of reaction is being carried out below 150 ℃; Production cost is low, environment friendly and pollution-free, the organic pressure-sensitive gel finished product viscosity of making is good, the height of anti-resistance to spalling the, every performance index are good, can be widely used in fields such as space flight, electric power, building, communication, electrical equipment, automatization, chemical industry, metallurgy, automobile making, medicine instrument and weavings.
Embodiment
Embodiment 1
The method that the present invention prepares organic silicon self-adhesive pressure sensitive adhesive is, at first in the reactor of being furnished with stainless steel agitator, motor and heating system, add 40 parts of methyl vinyl silicone rubbers, 8 parts of white carbon blacks, 30 parts of silicon powders, 2 parts of hydroxy silicon oils, 10 parts of pressure sensitive adhesive resins mix under 10 parts of normal temperature of methyl-silicone oil, are warming up to 150 ℃ of banburyings 2 hours again; Found time at last 1 hour, discharging promptly obtains self-adhesive.Methyl vinyl silicone rubber in the described raw material is that contents of ethylene is 0.2%, and molecular weight is 600,000; This white carbon black is that specific surface area (BET method) is 200 ± 25m
2/ g, average primary particle diameter are the thermal silica of 12～14Nm; This silicon powder is the silicon powder of general filler level, and hydroxy silicon oil is that hydroxy radical content is 7% silicone oil; This pressure sensitive adhesive resin is a methyl MQ resin, and the M/Q ratio is 0.5～1.2; Methyl-silicone oil is that viscosity is 50000CS.
Embodiment 2～4
Compare with embodiment 1, the Production Flow Chart of embodiment 2～4 is identical with it.The proportioning of each component and reaction times and temperature see Table 1 among each embodiment.
Table 1 set of dispense ratio and reaction times and thermometer
| Methyl vinyl silicone rubber | White carbon black | Silicon powder | Hydroxy silicon oil | The pressure sensitive adhesive resin | Methyl-silicone oil | Temperature of reaction/℃ | Reaction times/h | |
| Embodiment 2 | 30 | 5 | 40 | 1 | 14 | 10 | 150 | 1.5 |
| Embodiment 3 | 50 | 8 | 20 | 0.6 | 6.4 | 15 | 150 | 2 |
| Embodiment 4 | 25 | 4 | 45 | 2 | 4 | 20 | 150 | 2 |
The product of the present invention that embodiment 1 method is obtained carries out sulfidization molding with two 2,5 vulcanizing agents by heating and pressurizing, carries out performance test according to following standard, sees Table 2, and its sulfide reason mechanical property meets the requirement of table 2.
Table 2 physical and mechanical properties
Annotate: specimen size: long 130mm, wide 90mm, thick 2mm
The self-adhesion performance test:
Place the film of sulfidization molding vertical glass to stick, bubble is drained, after static 5 minutes, 20 cigarettes boxes that the 60g counterweight is housed are attached on the self-adhesion film, compress, handle unclamps after 10 seconds, picks up counting, and does not come off in setting-up time.
The present invention is not limited to the foregoing description, more than shown only be preferred embodiment of the present invention, can not limit the present invention's interest field with this, therefore the equivalent variations of being done according to the present patent application claim still belongs to the scope that the present invention is contained.
Claims (8)
1, the preparation method of one-step molding organic silicon self-adhesive pressure sensitive adhesive is characterized in that, its preparation method's step is; At first, proportion ingredient by following component, in weight part ratio, methyl vinyl silicone rubber: white carbon black: silicon powder: hydroxy silicon oil: pressure sensitive adhesive portions of resin methyl-silicone oil=(10～90) part: (1～50) part: (10～50) part: (0.1～3) part: (4～40) part: (10～90) part; In the reactor of being furnished with stainless steel stirring arm, motor and heating system, add above-mentioned batching then, methyl vinyl silicone rubber, white carbon black, silicon powder and hydroxy silicon oil, pressure sensitive adhesive resin, methyl-silicone oil are mixed at normal temperatures, banburying 1～3 hour again heats up, found time at last 0.5～2 hour, discharging gets final product, and drop temperature is controlled at more than 150 ℃.
According to the preparation method of the described one-step molding organic silicon self-adhesive pressure sensitive adhesive of claim 1, it is characterized in that 2, the contents of ethylene of described methyl vinyl silicone rubber is 0.01～0.24%, molecular weight is 45～700,000.
According to the preparation method of the described one-step molding organic silicon self-adhesive pressure sensitive adhesive of claim 1, it is characterized in that 3, described white carbon black is the surface-area 200 ± 25m than BET method
2/ g, average primary particle diameter are the thermal silica of 12～14Nm.
According to the preparation method of the described one-step molding organic silicon self-adhesive pressure sensitive adhesive of claim 1, it is characterized in that 4, described silicon powder is general filler level silicon powder.
According to the preparation method of the described one-step molding organic silicon self-adhesive pressure sensitive adhesive of claim 1, it is characterized in that 5, described hydroxy silicon oil is that hydroxy radical content is 5～12% silicone oil.
According to the preparation method of the described one-step molding organic silicon self-adhesive pressure sensitive adhesive of claim 1, it is characterized in that 6, described pressure sensitive adhesive resin is a methyl MQ resin, the M/Q ratio is 0.3～2.
According to the preparation method of the described one-step molding organic silicon self-adhesive pressure sensitive adhesive of claim 1, it is characterized in that 7, described methyl-silicone oil is that viscosity is 1000～200000CS.
According to the preparation method of the described one-step molding organic silicon self-adhesive pressure sensitive adhesive of claim 1, it is characterized in that 8, the described intensification banburying time is 2 hours; Evacuated time is 1 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910038382 CN101560372B (en) | 2009-04-02 | 2009-04-02 | Method for preparing one-step molding organic silicon self-adhesive pressure sensitive adhesive |
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| CN 200910038382 CN101560372B (en) | 2009-04-02 | 2009-04-02 | Method for preparing one-step molding organic silicon self-adhesive pressure sensitive adhesive |
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| CN101560372A true CN101560372A (en) | 2009-10-21 |
| CN101560372B CN101560372B (en) | 2012-12-12 |
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| CN 200910038382 Expired - Fee Related CN101560372B (en) | 2009-04-02 | 2009-04-02 | Method for preparing one-step molding organic silicon self-adhesive pressure sensitive adhesive |
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Cited By (15)
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| CN101805520A (en) * | 2010-03-19 | 2010-08-18 | 东莞市宏达新材料有限公司 | Silicone self-adhesive formula and preparation method |
| CN102127389A (en) * | 2011-01-11 | 2011-07-20 | 广东达美新材料有限公司 | High-solid-content high-temperature-resistant organic-silicone pressure-sensitive adhesive and preparation method thereof |
| WO2012094885A1 (en) * | 2011-01-13 | 2012-07-19 | 深圳市森日有机硅材料有限公司 | Solventless silicone pressure sensitive adhesive and preparation method thereof |
| WO2013002843A2 (en) * | 2011-06-30 | 2013-01-03 | Trennel Incorporation | Self-adhesive silicone rubber compositions and articles comprising same |
| CN103361022A (en) * | 2012-04-09 | 2013-10-23 | 泰科电子(上海)有限公司 | Silicon rubber sealing mortar used for middle-high voltage cable accessory and cable accessory |
| CN104449439A (en) * | 2013-09-17 | 2015-03-25 | 河北联合大学 | High self-adhesive silicone rubber belt as well as preparation and application of high self-adhesive silicone rubber belt |
| CN105153995A (en) * | 2015-07-28 | 2015-12-16 | 深圳市安品有机硅材料有限公司 | Heat-conductive silicone rubber bonding composition, heat-conductive silicone rubber bonding sheet material and application thereof |
| CN105295826A (en) * | 2015-11-24 | 2016-02-03 | 刘志辉 | High temperature resistant silica gel pressure sensitive adhesive |
| CN106753091A (en) * | 2016-12-09 | 2017-05-31 | 德阳力久云智知识产权运营有限公司 | A kind of organic silicon adhesive containing Terpene styron and preparation method thereof |
| CN106753195A (en) * | 2016-11-23 | 2017-05-31 | 成都拓利科技股份有限公司 | A kind of organic pressure-sensitive gel and pressure sensitive adhesive adhesive tape or film |
| CN107699186A (en) * | 2017-10-09 | 2018-02-16 | 南京图艾生物医药科技有限公司 | A kind of modified medical grade silicon rubber pressure sensitive adhesive and preparation method thereof |
| CN108774488A (en) * | 2018-06-15 | 2018-11-09 | 歌尔股份有限公司 | Organic silicon pressure sensitive adhesive and preparation method thereof, structure of composite membrane, vibrating diaphragm and sound-producing device |
| CN109021915A (en) * | 2018-06-15 | 2018-12-18 | 歌尔股份有限公司 | Organic silicon pressure sensitive adhesive and preparation method thereof, structure of composite membrane, vibrating diaphragm and sounding device |
| CN109111746A (en) * | 2018-08-14 | 2019-01-01 | 江苏天辰新材料股份有限公司 | A kind of preparation method of low-shrinkage silicon rubber |
| CN115521719A (en) * | 2022-09-19 | 2022-12-27 | 厦门华天华电子有限公司 | PET (polyethylene terephthalate) substrate coated with silicic acid gel micro-adhesive protective film and using method thereof |
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| US5290885A (en) * | 1992-12-30 | 1994-03-01 | Dow Corning Corporation | Unsaturated organic adduct of an organohydrogenpolysiloxane as an improved crosslinking agent for silicone pressure-sensitive adhesives |
| CN1109084C (en) * | 2000-08-24 | 2003-05-21 | 李世荣 | Process for preparing sealing adhesive tape of colour butyl rubber |
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| CN101805520A (en) * | 2010-03-19 | 2010-08-18 | 东莞市宏达新材料有限公司 | Silicone self-adhesive formula and preparation method |
| CN102127389A (en) * | 2011-01-11 | 2011-07-20 | 广东达美新材料有限公司 | High-solid-content high-temperature-resistant organic-silicone pressure-sensitive adhesive and preparation method thereof |
| CN102127389B (en) * | 2011-01-11 | 2012-10-10 | 广东达美新材料有限公司 | High-solid-content high-temperature-resistant organic-silicone pressure-sensitive adhesive and preparation method thereof |
| WO2012094885A1 (en) * | 2011-01-13 | 2012-07-19 | 深圳市森日有机硅材料有限公司 | Solventless silicone pressure sensitive adhesive and preparation method thereof |
| WO2013002843A2 (en) * | 2011-06-30 | 2013-01-03 | Trennel Incorporation | Self-adhesive silicone rubber compositions and articles comprising same |
| WO2013002843A3 (en) * | 2011-06-30 | 2013-02-28 | Trennel Incorporation | Self-adhesive silicone rubber compositions and articles comprising same |
| CN103361022A (en) * | 2012-04-09 | 2013-10-23 | 泰科电子(上海)有限公司 | Silicon rubber sealing mortar used for middle-high voltage cable accessory and cable accessory |
| CN103361022B (en) * | 2012-04-09 | 2015-01-28 | 泰科电子(上海)有限公司 | Silicon rubber sealing mortar used for middle-high voltage cable accessory and cable accessory |
| CN104449439A (en) * | 2013-09-17 | 2015-03-25 | 河北联合大学 | High self-adhesive silicone rubber belt as well as preparation and application of high self-adhesive silicone rubber belt |
| CN105153995B (en) * | 2015-07-28 | 2017-11-28 | 深圳市安品有机硅材料有限公司 | Heat-conducting silicon rubber adhesive composition, heat-conducting silicon rubber adhesive sheet and its application |
| CN105153995A (en) * | 2015-07-28 | 2015-12-16 | 深圳市安品有机硅材料有限公司 | Heat-conductive silicone rubber bonding composition, heat-conductive silicone rubber bonding sheet material and application thereof |
| CN105295826A (en) * | 2015-11-24 | 2016-02-03 | 刘志辉 | High temperature resistant silica gel pressure sensitive adhesive |
| CN106753195A (en) * | 2016-11-23 | 2017-05-31 | 成都拓利科技股份有限公司 | A kind of organic pressure-sensitive gel and pressure sensitive adhesive adhesive tape or film |
| CN106753195B (en) * | 2016-11-23 | 2020-07-14 | 成都拓利科技股份有限公司 | Organic silicon pressure-sensitive adhesive and pressure-sensitive adhesive tape or film |
| CN106753091A (en) * | 2016-12-09 | 2017-05-31 | 德阳力久云智知识产权运营有限公司 | A kind of organic silicon adhesive containing Terpene styron and preparation method thereof |
| CN107699186A (en) * | 2017-10-09 | 2018-02-16 | 南京图艾生物医药科技有限公司 | A kind of modified medical grade silicon rubber pressure sensitive adhesive and preparation method thereof |
| CN108774488A (en) * | 2018-06-15 | 2018-11-09 | 歌尔股份有限公司 | Organic silicon pressure sensitive adhesive and preparation method thereof, structure of composite membrane, vibrating diaphragm and sound-producing device |
| CN109021915A (en) * | 2018-06-15 | 2018-12-18 | 歌尔股份有限公司 | Organic silicon pressure sensitive adhesive and preparation method thereof, structure of composite membrane, vibrating diaphragm and sounding device |
| WO2019237696A1 (en) * | 2018-06-15 | 2019-12-19 | 歌尔股份有限公司 | Organosilicon pressure-sensitive adhesive and preparation method thereof, composite film structure, diaphragm, and sound generating device |
| CN109111746A (en) * | 2018-08-14 | 2019-01-01 | 江苏天辰新材料股份有限公司 | A kind of preparation method of low-shrinkage silicon rubber |
| CN115521719A (en) * | 2022-09-19 | 2022-12-27 | 厦门华天华电子有限公司 | PET (polyethylene terephthalate) substrate coated with silicic acid gel micro-adhesive protective film and using method thereof |
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