CN102127389A - High-solid-content high-temperature-resistant organic-silicone pressure-sensitive adhesive and preparation method thereof - Google Patents
High-solid-content high-temperature-resistant organic-silicone pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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- CN102127389A CN102127389A CN 201110004600 CN201110004600A CN102127389A CN 102127389 A CN102127389 A CN 102127389A CN 201110004600 CN201110004600 CN 201110004600 CN 201110004600 A CN201110004600 A CN 201110004600A CN 102127389 A CN102127389 A CN 102127389A
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Abstract
The invention discloses a high-solid-content high-temperature-resistant organic-silicone pressure-sensitive adhesive which is prepared by reacting the following components in percentage by weight: 25.0-40.0% of organic silicone rubber, 25.0-40.0% of MQ organic silicone resin, 0.05-5.00% of catalyst and 30.0-40.0% of solvent. The organic-silicone pressure-sensitive adhesive disclosed by the invention can resist high temperature (250-280 DEG C), and the solid content of the organic-silicone pressure-sensitive adhesive is up to 65-70%; and compared with the silanol condensed type high-temperature-resistant organic-silicone pressure-sensitive adhesive system in the existing market, the VOC (volatile organic compound) content of the organic-silicone pressure-sensitive adhesive disclosed by the invention is obviously lowered, and the organic-silicone pressure-sensitive adhesive disclosed by the invention has better environmental protection performance.
Description
Technical field
The present invention relates to a kind of organic pressure-sensitive gel and preparation method thereof, more particularly, the present invention relates to high temperature resistant organic pressure-sensitive gel of a kind of high solids content and preparation method thereof.
Background technology
Organic pressure-sensitive gel is the extraordinary pressure sensitive adhesive of a class high-quality high-grade in the pressure sensitive adhesive family.At present, the organic pressure-sensitive gel system that is adapted at using under the high temperature severe condition is silanol condensed type organic silicon pressure sensitive adhesive.For example, in printed circuit board (PCB) (PCB) manufacturing processed gold-plated, hot blast is smooth and the wave soldering operation in all need to use masking tape, require these adhesive tapes (250 ℃～280 ℃) under hot environment not only will bond closely knit with PCB, and it is residual not allow glue during tape stripping, has only silanol condensed type organic silicon pressure sensitive adhesive can satisfy this requirement at present.
Silanol condensed type organic silicon pressure sensitive adhesive is made up of organo-silicone rubber, MQ silicone resin, organic solvent and other additive etc. usually.The organic solvent that uses generally is toluene or dimethylbenzene, and its solid content is generally 40%～50%, has a large amount of volatile organic compounds (VOC) to discharge in coating process.These materials not only cause the comparison serious environmental to pollute, and human beings'health is caused bigger harm.Therefore, solid content, the reduction VOC value that how to improve the solvent-type organosilicon pressure sensitive adhesive put on the outstanding position.Solid content claims non-volatile part content again, is meant that product dry the mass percent that back remainder accounts for total amount under prescribed condition.So-called high solids content is meant solid content generally more than 60%, is that 40%～50% silanol condensed type organic silicon pressure sensitive adhesive system is compared with traditional solid content, can reduce the VOC value significantly.
Summary of the invention
The object of the present invention is to provide high temperature resistant organic pressure-sensitive gel of a kind of high solids content and preparation method thereof.
The objective of the invention is to be achieved through the following technical solutions:
The high temperature resistant organic pressure-sensitive gel of a kind of high solids content is prepared from by following component reaction by weight percentage:
Organo-silicone rubber 25.0～40.0%;
MQ silicone resin 25.0～40.0%;
Catalyzer 0.05～5.00%;
Solvent 30.0～40.0%.
Organo-silicone rubber of the present invention is to be the linear polydimethylsiloxane of end group with the hydroxyl.For high solids content and the high temperature resistant requirement of satisfying organic pressure-sensitive gel of the present invention, necessary choose reasonable organo-silicone rubber, crucial have 2 points: (1) molecular weight: the molecular weight of organo-silicone rubber should be moderate, the too low pressure sensitive adhesive that can not guarantee of molecular weight has good snappiness, cohesive strength and low mobility, molecular weight is too high to make then that product viscosity is too big, solid content is low, therefore, the present invention selects the organo-silicone rubber of molecular weight between 200,000～500,000; (2) hydroxy radical content: organo-silicone rubber will have certain hydroxy radical content, so as with MQ silicone resin generation condensation reaction, the selected hydroxy radical content scope of the present invention is 0.3%～1.5%.
As preferred embodiment a kind of, MQ silicone resin of the present invention is prepared from by following component reaction by weight percentage:
Water glass 15.0%～30.0%; Hexamethyldisiloxane 10.0%～25.0%;
3,5-dimethylphenyl chlorosilane 1.00%～10.0%; Concentrated hydrochloric acid 0.20%～3.00%;
Alcohol mixture 30.0%～50.0%; Deionized water 10.0%～25.0%.
Wherein, the Q group of the synthetic MQ silicone resin of described water glass conduct, the condensation that under lesser temps and acidic conditions, can self be hydrolyzed, condensation also can be hydrolyzed with the siloxanes of M group; Described hexamethyldisiloxane is as the M group of synthetic MQ silicone resin, can with the condensation that is hydrolyzed of Q group, carry out end-blocking for the MQ silicone resin provides methyl, so that the molecular weight and the solvability of control product; Described 3,5-dimethylphenyl chlorosilane is as the functional group of synthetic MQ silicone resin, the condensation that is hydrolyzed of main and Q group, for the MQ silicone resin provides functionalized phenyl, can improve the high temperature use properties of MQ silicone resin, also can increase the solubility property of product in organic solvent; Described concentrated hydrochloric acid is that concentration is the hydrochloric acid of 35wt%～37wt%, and it mainly provides acid carrying out with the catalytic hydrolysis condensation reaction; Described alcohol mixture is the mixture of Virahol and propyl carbinol, and both weight ratios are 3: 1～1: 1, and it is used for dissolving raw material and product as reaction medium; Described deionized water is mainly used in to described hydrolysis-condensation reaction hydroxyl is provided.
The preparation method of above-mentioned MQ silicone resin is: add deionized water, concentrated hydrochloric acid, alcohol mixture and hexamethyldisiloxane in reactor, under agitation condition, drip water glass and 3,5-dimethylphenyl chlorosilane simultaneously, the dropping time was controlled at 20～60 minutes, and temperature of reaction is controlled at 25 ℃～40 ℃; Dropwise the back and continue reaction 0.5～1 hour down, be warmed up to 50 ℃～60 ℃ insulation reaction 0.5～1 hour then at 25 ℃～40 ℃; At last product is carried out spraying drying, washing and oven dry and handle, promptly obtain described MQ silicone resin.
MQ silicone resin of the present invention is the silicone of structure height cladodification, and it is by the organosilane monomer R of simple function group (M group)
3SiO
1/2Organosilane monomer SiO with four-functional group (Q group)
4/2Hydrolytic condensation forms.The MQ silicone resin has complicated three-dimensional ball-type structure, have two kinds of different chain links, organic chain link wherein can improve the consistency of organo-silicone rubber and play viscosifying action, and the siloxanes chain link has strengthening action to organo-silicone rubber, can improve the cohesive strength of pressure sensitive adhesive.The selection key of MQ silicone resin has 4 points: (1) consistency: have good consistency with selected organo-silicone rubber, could guarantee that prepared organic pressure-sensitive gel has good comprehensive performances and high solids content; (2) M/Q is than (mol ratio of M group and Q group): suitable M/Q ratio is 0.6～0.9, and M/Q＜0.6 is poor with the consistency of organo-silicone rubber, and M/Q＞0.9 cohesive strength is too poor; (3) hydroxy radical content: hydroxy radical content can influence the degree of itself and organo-silicone rubber reaction and organic pressure-sensitive gel to the adhesive power of base material and bonding strength etc., and the selected hydroxy radical content scope of the present invention is 1%～4%; (4) phenyl content: contain an amount of phenyl in the MQ silicone resin, can improve its thermotolerance greatly, the selected phenyl content scope of the present invention is 3%～15%.
Catalyzer of the present invention is the organic tin compound, comprises dibutyl tin laurate, two lauric acid dioctyl tins, dibutyltin diacetate and stannous octoate etc., and it mainly acts on is condensation reaction between catalysis organo-silicone rubber and the MQ silicone resin.
Solvent of the present invention is preferably the mixture of dimethylbenzene and N-Methyl pyrrolidone (NMP), and wherein, the content of NMP in organic pressure-sensitive gel of the present invention is preferably 3%～10%.Dimethylbenzene is the good solvent of organo-silicone rubber and MQ silicone resin, and NMP can form hydrogen bond with hydroxyl, and the existence of an amount of NMP can reduce the interaction between the organo-silicone rubber molecule, thereby can improve the solid content of product greatly.
The preparation method of organic pressure-sensitive gel of the present invention is: add solvent, MQ silicone resin and organo-silicone rubber in reactor by weight percentage, slowly drip catalyzer after being warming up to 130 ℃～135 ℃, dropwised in 1～3 hour, continue reaction 1～2 hour down at 130 ℃～150 ℃ then, promptly obtain organic pressure-sensitive gel of the present invention after the cooling.
The present invention is by choose reasonable organo-silicone rubber and silicone resin raw material, and adopt NMP as solvent, make the prepared organic silicon pressure sensitive adhesive can high temperature resistant (250 ℃～280 ℃), and its solid content is up to 65%～70%, with solid content in the market is that 40%～50% the high temperature resistant organic pressure-sensitive gel system of silanol condensed type is compared, reduce the VOC value significantly, had the more superior feature of environmental protection.
Embodiment
Embodiment one:
In reactor, add 290 kilograms of dimethylbenzene, 40 kilograms of NMP, 310 kilograms of MQ silicone resins and 350 kilograms of organo-silicone rubbers, slowly drip 10 kilograms of dibutyl tin laurates after being warming up to 130 ℃～135 ℃, dropwised in 2 hours, continue reaction 2 hours down at 130 ℃～150 ℃ then, promptly obtain organic pressure-sensitive gel of the present invention after the cooling.
Embodiment two:
In reactor, add 300 kilograms of dimethylbenzene, 35 kilograms of NMP, 350 kilograms of MQ silicone resins and 300 kilograms of organo-silicone rubbers, slowly drip 15 kilograms of dibutyltin diacetates after being warming up to 130 ℃～135 ℃, dropwised in 2 hours, continue reaction 2 hours down at 130 ℃～150 ℃ then, promptly obtain organic pressure-sensitive gel of the present invention after the cooling.
Embodiment three:
In reactor, add 300 kilograms of dimethylbenzene, 50 kilograms of NMP, 340 kilograms of MQ silicone resins and 290 kilograms of organo-silicone rubbers, slowly drip 20 kilogram of two lauric acid dioctyl tin after being warming up to 130 ℃～135 ℃, dropwised in 2 hours, continue reaction 2 hours down at 130 ℃～150 ℃ then, promptly obtain organic pressure-sensitive gel of the present invention after the cooling.
Claims (10)
1. high temperature resistant organic pressure-sensitive gel of high solids content is prepared from by following component reaction by weight percentage:
Organo-silicone rubber 25.0～40.0%;
MQ silicone resin 25.0～40.0%;
Catalyzer 0.05～5.00%;
Solvent 30.0～40.0%.
2. organic pressure-sensitive gel according to claim 1 is characterized in that: described organo-silicone rubber is to be the linear polydimethylsiloxane of end group with the hydroxyl, and its molecular weight is 200,000～500,000, and its hydroxy radical content is 0.3%～1.5%.
3. organic pressure-sensitive gel according to claim 1 is characterized in that, described MQ silicone resin is prepared from by following component reaction by weight percentage:
Water glass 15.0%～30.0%;
Hexamethyldisiloxane 10.0%～25.0%;
3,5-dimethylphenyl chlorosilane 1.00%～10.0%;
Concentrated hydrochloric acid 0.20%～3.00%;
Alcohol mixture 30.0%～50.0%;
Deionized water 10.0%～25.0%.
4. organic pressure-sensitive gel according to claim 3 is characterized in that: described alcohol mixture is the mixture of Virahol and propyl carbinol, and both weight ratios are 3: 1～1: 1.
5. organic pressure-sensitive gel according to claim 3 is characterized in that: in the described MQ silicone resin, hydroxy radical content is 1～4%, and phenyl content is 3～15%.
6. organic pressure-sensitive gel according to claim 1 is characterized in that: in the described MQ silicone resin, the mol ratio of M group and Q group is 0.6～0.9.
7. organic pressure-sensitive gel according to claim 1 is characterized in that: described catalyzer is the organic tin catalyzer.
8. organic pressure-sensitive gel according to claim 7 is characterized in that: described organic tin catalyzer comprises dibutyl tin laurate, two lauric acid dioctyl tins, dibutyltin diacetate and stannous octoate.
9. organic pressure-sensitive gel according to claim 1 is characterized in that: described solvent is the mixture of dimethylbenzene and N-Methyl pyrrolidone; The content of described N-Methyl pyrrolidone in described organic pressure-sensitive gel is 3%～10%.
10. the preparation method of the described organic pressure-sensitive gel of claim 1, it is characterized in that may further comprise the steps: in reactor, add solvent, MQ silicone resin and organo-silicone rubber by weight percentage, slowly drip catalyzer after being warming up to 130 ℃～135 ℃, dropwised in 1～3 hour, continue reaction 1～2 hour down at 130 ℃～150 ℃ then, promptly obtain organic pressure-sensitive gel of the present invention after the cooling.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104232008A (en) * | 2014-08-26 | 2014-12-24 | 安徽神舟飞船胶业有限公司 | Polysiloxane pressure-sensitive adhesive formula and preparation technique thereof |
| CN105968359A (en) * | 2016-06-08 | 2016-09-28 | 成都大蓉新材料有限责任公司 | Hydroxyl resin for organic silicon-coated material and preparation method of hydroxyl resin |
| CN106010237A (en) * | 2016-06-08 | 2016-10-12 | 成都大蓉新材料有限责任公司 | Organosilicone coating material and preparation method thereof |
| CN108084903A (en) * | 2017-12-16 | 2018-05-29 | 宁波六麦新材料科技有限公司 | A kind of two-sided shading rubber belt of high-low temperature resistant of high purification anti-pollution |
| CN108520851A (en) * | 2018-05-07 | 2018-09-11 | 丁爱琴 | A kind of logical device side wall etching machine using refractory seals new material |
| 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 |
| CN110734739A (en) * | 2019-09-19 | 2020-01-31 | 宜宾天原集团股份有限公司 | Preparation method of organic silicon pressure-sensitive adhesives |
| CN113956837A (en) * | 2021-10-22 | 2022-01-21 | 万华化学集团股份有限公司 | Non-stop printing high-anchorage organic silicon pressure-sensitive adhesive, preparation method and application thereof |
| CN113956833A (en) * | 2021-09-23 | 2022-01-21 | 万华化学集团股份有限公司 | Organic silicon pressure-sensitive adhesive for anti-fingerprint glass, preparation method and application thereof |
| CN114316268A (en) * | 2021-12-09 | 2022-04-12 | 湖北晟特新材料有限公司 | Organic silicon resin and preparation method thereof, mica tape adhesive and preparation method thereof |
| CN114656921A (en) * | 2022-03-31 | 2022-06-24 | 兰州金睿合新材料科技有限责任公司 | Organic silicon pressure-sensitive adhesive and preparation method thereof |
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| US7687591B2 (en) * | 2003-03-17 | 2010-03-30 | Dow Corning Corporation | Solventless silicone pressure sensitive adhesives with improved high temperature cohesive strength |
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Cited By (14)
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| CN104232008A (en) * | 2014-08-26 | 2014-12-24 | 安徽神舟飞船胶业有限公司 | Polysiloxane pressure-sensitive adhesive formula and preparation technique thereof |
| CN105968359A (en) * | 2016-06-08 | 2016-09-28 | 成都大蓉新材料有限责任公司 | Hydroxyl resin for organic silicon-coated material and preparation method of hydroxyl resin |
| CN106010237A (en) * | 2016-06-08 | 2016-10-12 | 成都大蓉新材料有限责任公司 | Organosilicone coating material and preparation method thereof |
| CN108084903A (en) * | 2017-12-16 | 2018-05-29 | 宁波六麦新材料科技有限公司 | A kind of two-sided shading rubber belt of high-low temperature resistant of high purification anti-pollution |
| CN108520851A (en) * | 2018-05-07 | 2018-09-11 | 丁爱琴 | A kind of logical device side wall etching machine using refractory seals new material |
| 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 |
| 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 |
| WO2019237601A1 (en) * | 2018-06-15 | 2019-12-19 | 歌尔股份有限公司 | Organosilicon pressure sensitive adhesive and preparation method therefor, composite film structure, vibration film, and sound generating 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 |
| CN110734739A (en) * | 2019-09-19 | 2020-01-31 | 宜宾天原集团股份有限公司 | Preparation method of organic silicon pressure-sensitive adhesives |
| CN113956833A (en) * | 2021-09-23 | 2022-01-21 | 万华化学集团股份有限公司 | Organic silicon pressure-sensitive adhesive for anti-fingerprint glass, preparation method and application thereof |
| CN113956837A (en) * | 2021-10-22 | 2022-01-21 | 万华化学集团股份有限公司 | Non-stop printing high-anchorage organic silicon pressure-sensitive adhesive, preparation method and application thereof |
| CN114316268A (en) * | 2021-12-09 | 2022-04-12 | 湖北晟特新材料有限公司 | Organic silicon resin and preparation method thereof, mica tape adhesive and preparation method thereof |
| CN114656921A (en) * | 2022-03-31 | 2022-06-24 | 兰州金睿合新材料科技有限责任公司 | Organic silicon pressure-sensitive adhesive and preparation method thereof |
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