CN104497332A - Release film and preparation method thereof - Google Patents
Release film and preparation method thereof Download PDFInfo
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- CN104497332A CN104497332A CN201410742980.2A CN201410742980A CN104497332A CN 104497332 A CN104497332 A CN 104497332A CN 201410742980 A CN201410742980 A CN 201410742980A CN 104497332 A CN104497332 A CN 104497332A
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- toluene
- release film
- parting agent
- diluting solvent
- ethylene glycol
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Abstract
The invention discloses a release film and a preparation method thereof. According to the release film, BOPET film is used as a base membrane and is coated with a release agent layer, wherein the release agent layer is prepared from reactant monomers, an initiator and toluene; the reactant monomers include the following components in percentage by weight: 20-30 percent of an organosilicone monomer containing vinyl, 30-40 percent of acrylic acid, 8-15 percent of methacrylate or methyl methacrylate, 10-20 percent of ethyl acrylate or butyl acrylate, 5-10 percent of styrene and 4-10 percent of iso-butyl methacrylate. The release film has the advantages of high surface tension, moderate release force, excellent residual adhesion rate and the like.
Description
Technical field
The present invention relates to high-molecular coating Material Field, particularly relate to a kind of release film and preparation method thereof.
Background technology
Along with the develop rapidly of national economy, organosilicon barrier film is sharply rising at the consumption of industry-by-industry.Although have the manufacturer of a lot of release film domestic, the release film great majority produced are all low-end products, and its cleanliness factor, planarization and the index such as antistatic all do not reach the service requirements of the industry such as electronics and cross cutting.The demand of high-end product then can only rely on import, and particularly at the release film of electron trade application, the serious development constraining China's relevant industries, the release film price of import is high, and delivery cycle is long makes demestic user deeply disturbed.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, provide a kind of release film and preparation method thereof in the present invention, be intended to the peeling force solving existing domestic release film, the indexs such as mist degree and remaining adhesion rate do not reach the problem of the service requirements of electron trade.
Technical scheme of the present invention is as follows:
A kind of release film, wherein, described release film comprises BOPET film, described BOPET film is coated with a parting agent layer;
Wherein, described parting agent layer, its raw material composition comprises reactant monomer, initiator and toluene;
Described reactant monomer, according to mass percent, comprises following component:
Organosilicon performed polymer:
Organosilane monomer 20% ~ 30% containing vinyl;
Acrylate monomer:
Vinylformic acid 30% ~ 40%; Methyl acrylate or methyl methacrylate 8% ~ 15%; Ethyl propenoate or butyl acrylate 10% ~ 20%; Vinylbenzene 5% ~ 10%; Propenoic acid, 2-methyl, isobutyl ester 4% ~ 10%;
Described initiator comprises one or more in dilauroyl peroxide, benzoyl peroxide, dicumyl peroxide, and the consumption of initiator is the 1.0wt% ~ 2.5wt% of reactant monomer quality.
Described release film, wherein, described parting agent layer, its raw material composition also comprises solidifying agent and diluting solvent;
Wherein, described solidifying agent is aziridine CX-100, and consumption accounts for 3% ~ 5% of vinylformic acid quality;
The mass ratio of parting agent and diluting solvent is 1.0:2.0 ~ 3.8; Diluting solvent comprise in ethylene glycol monomethyl ether and toluene one or both.
Described release film, wherein, the diluting solvent used is ethylene glycol monomethyl ether and toluene, and parting agent, consumption mass ratio between ethylene glycol monomethyl ether and toluene are 1.0:0 ~ 0.8:2.0 ~ 3.0
Described release film, wherein, described organosilicon performed polymer is vinyl triacetoxy siloxanes.
A preparation method for release film as above, wherein, comprises the following steps:
The toluene of whole organosilicon performed polymers, part and the initiator of part are joined in reactor;
Acrylic ester monomer, remaining initiator and toluene are mixed to make and adds liquid;
Reactor starts and stirs and heat, and when being heated to 85 DEG C ± 2 DEG C, add liquid described at the uniform velocity dripping in the reactor, time for adding controls at 2 ~ 4h; Be warming up to 92 DEG C ± 2 DEG C after dropping terminates, insulation 3 ~ 4h, to be triggered dose be exhausted after, cooling, discharging, obtain described parting agent;
Described parting agent is coated in described BOPET film.
The preparation method of described release film, wherein, specifically comprises the following steps the process that described parting agent is coated in described BOPET film:
By the parting agent of gained and diluting solvent blended, simultaneously add solidifying agent in proportion, be diluted to coating fluid, use reticulate pattern formula coating machine to be evenly coated in BOPET film, dry;
Described solidifying agent is aziridine CX-100, and consumption accounts for 3% ~ 5% of vinylformic acid quality;
The mass ratio of parting agent and diluting solvent is 1.0:2.0 ~ 3.8; Diluting solvent comprise in ethylene glycol monomethyl ether and toluene one or both.
The preparation method of described release film, wherein, the diluting solvent used is ethylene glycol monomethyl ether and toluene; Parting agent, consumption mass ratio 1.0:0 ~ 0.8:2.0 ~ 3.0 between ethylene glycol monomethyl ether and toluene.
Beneficial effect: release film provided by the present invention take BOPET film as basement membrane, and at BOPET film coating parting agent, described parting agent is the acrylate modified silicone resin containing vinyl.The advantages such as release film of the present invention has higher surface tension, and peeling force is moderate, and remaining adhesion rate is excellent.
Embodiment
The invention provides a kind of release film and preparation method thereof, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Release film provided by the present invention, is take BOPET film as basement membrane, described BOPET film is coated with a parting agent layer.
Wherein, described parting agent layer, its raw material composition comprises reactant monomer, initiator and toluene;
Described reactant monomer, according to mass percent, comprises following component:
Organosilicon performed polymer:
Organosilane monomer 20% ~ 30% containing vinyl;
Acrylate monomer:
Vinylformic acid 30% ~ 40%; Methyl acrylate or methyl methacrylate 8% ~ 15%; Ethyl propenoate or butyl acrylate 10% ~ 20%; Vinylbenzene 5% ~ 10%; Propenoic acid, 2-methyl, isobutyl ester 4% ~ 10%;
Described initiator comprise dilauroyl peroxide, benzoyl peroxide, dicumyl peroxide etc. one or more, the consumption of initiator is about the 1.0wt% ~ 2.5wt% of reactant monomer quality;
Described parting agent employs the organosilicon preformed polymer with vinyl in building-up process, can directly pass through the method for radical polymerization with acrylic ester monomer copolymerization; And organosilyl Self-emulsifying properties, in non-polar solvent system, silicone segments easily occurs curling, defines emulsion particle.Preferably, have employed vinyl triacetoxy siloxanes in the present invention, solid content is 30wt%.
The amount ranges of described toluene is 1.5 to 2.0 times of reactant monomer quality.The effect of toluene is solvent, makes the solid content of reaction monomers remain on 20-40% when reacting.
Described parting agent layer, its raw material composition also comprises solidifying agent and diluting solvent;
Wherein, described solidifying agent is aziridine CX-100, and consumption accounts for 3% ~ 5% of vinylformic acid quality.Solidifying agent aziridine is added in parting agent, curing reaction is there is after film, make film inside form cross-linked network, thus improve the over-all properties of film, also inhibits film forming while improving stripping strength and solvent resistance after, organosilicon preformed polymer molecule is to the migration on surface.
The mass ratio of parting agent and diluting solvent is 1.0:2.0 ~ 3.8.The diluting solvent used comprise in ethylene glycol monomethyl ether and toluene one or both.The diluting solvent used is ethylene glycol monomethyl ether and toluene two kinds, and particularly, each constituent mass ratio is parting agent: ethylene glycol monomethyl ether: toluene 1.0:0 ~ 0.8:2.0 ~ 3.0.
Release film provided by the present invention is basement membrane with BOPET film, the advantages such as BOPET film has good heat resistance, and mechanical strength is high, profile pattern is good.And described parting agent adopts acrylate modified silicone resin, while raising organosilyl surface tension force, also increase organosilicon to the sticking power of BOPET film.By adopting the organosilane monomer containing vinyl, organosilicon ratio can be controlled well, making the medium range that the peeling force of modified organic silicon release film controls; Compare with grafting modifying silicone resin, the existence of vinyl can increase substantially the ratio of acrylate in copolymerization product, further increases organosilyl solvability, improves the homogeneity after coating.Release film provided by the present invention, the advantages such as have higher surface tension, peeling force is moderate, and remaining adhesion rate is excellent.
The preparation method of described release film is also provided in the present invention, specifically comprises the following steps:
In proportion the toluene of whole organosilicon performed polymers, part and the initiator of part are joined in reactor;
Acrylic ester monomer, remaining initiator and toluene are mixed to make and adds liquid, store for future use;
Start stirring, during reacting by heating still to 85 DEG C ± 2 DEG C, liquid will be added and at the uniform velocity add reactor by dripping tank, time for adding controls at 2 ~ 4h, drips after terminating and is warming up to 92 DEG C ± 2 DEG C, insulation 3 ~ 4h, to be triggered dose be exhausted after, cooling, discharging, obtain polymer emulsion, be described parting agent;
By the parting agent of gained and diluting solvent blended, simultaneously add solidifying agent in proportion, be diluted to coating fluid, use reticulate pattern formula coating machine to be evenly coated in BOPET film, dry, obtain water white release film.
Wherein, the initiator of described part refers to and accounts for 20% ~ 45% of formulation weight; The toluene of described part refers to and accounts for 50% ~ 65% of formulation weight.
Oven temperature 80 ~ 160 DEG C, it is 160 DEG C that baking oven adopts gradient increased temperature top temperature to control.It is 60 ~ 80m/min that surface covered controls.
Preferably, first carry out corona treatment to BOPET film before coating, the surface tension after corona treatment is not less than 38 dyne.First corona treatment is carried out to BOPET film before coating, the surface tension of BOPET film can be improved, increase the sticking power of parting agent.
According to GB/T 25256-2010 requirement, the method of dyne water is adopted to measure described release film surface tension, and the peeling force of described release film and remaining adhesion rate are measured, measuring result finds that described in gained, release film has higher surface tension, the advantages such as peeling force is moderate, and remaining adhesion rate is excellent.Wherein, peel test force adopts TESA7457 adhesive tape to test peeling force, adopts Nitto31B adhesive tape to measure remnants adhesion rate.
Below in conjunction with embodiment, the present invention is further described.
Embodiment one
By formula by organosilicon performed polymer 3.0kg, benzoyl peroxide 0.06kg, toluene 18.0kg joins in reactor.Take vinylformic acid 4.0kg, butyl acrylate 1.2kg, methyl methacrylate 1.0kg, Propenoic acid, 2-methyl, isobutyl ester 0.5kg, vinylbenzene 0.6kg, benzoyl peroxide 0.14kg, and toluene 12.0kg mix after be mixed with and add liquid, seal for subsequent use.
Reacting by heating still also starts stirring, stir speed (S.S.) is 600r/min, during reacting by heating still to 85 DEG C ± 2 DEG C, to add liquid and at the uniform velocity add reactor by dripping tank, time for adding controls at 2h, drips after terminating and is warming up to 92 DEG C ± 2 DEG C, insulation 4h, to be triggered dose be exhausted after, cooling, discharging, obtain polymer emulsion.
Embodiment two
By formula by organosilicon performed polymer 2.5kg, benzoyl peroxide 0.06kg, and toluene 18kg joins in reactor.Take vinylformic acid 4.0kg, methyl acrylate 1.3kg, butyl acrylate 1.50kg, Propenoic acid, 2-methyl, isobutyl ester 0.6kg, vinylbenzene 0.8kg, be mixed with after benzoyl peroxide 0.14kg and toluene 12.0kg mixes and add liquid, seal for subsequent use.
Reacting by heating still also starts stirring, stir speed (S.S.) is 600r/min, during reacting by heating still to 85 DEG C ± 2 DEG C, to add liquid and at the uniform velocity add reactor by dripping tank, time for adding controls at 2h, drips after terminating and is warming up to 92 DEG C ± 2 DEG C, insulation 4h, to be triggered dose be exhausted after, cooling, discharging, obtain polymer emulsion.
Embodiment three
Take polymer emulsion 1.0kg in embodiment one, ethylene glycol monomethyl ether 0.2kg and toluene 3.0kg is blended, adds solidifying agent 0.005kg simultaneously, is diluted to coating fluid, reticulate pattern formula coating machine is used evenly to be coated in BOPET film, surface covered 65m/min, oven temperature 80 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 120 DEG C, obtain water white release film.The peeling force measuring gained is 36.3g/25mm, remaining adhesion rate 97%, mist degree 6.2%.
Embodiment four
Take polymer emulsion 1.0kg in embodiment two, ethylene glycol monomethyl ether 0.2kg and toluene 3.0kg is blended, adds solidifying agent 0.005kg simultaneously, is diluted to coating fluid, reticulate pattern formula coating machine is used evenly to be coated in BOPET film, surface covered 65m/min, oven temperature 80 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 120 DEG C, obtain water white release film.The peeling force measuring gained is 14.2g/25mm, remaining adhesion rate 97%, mist degree 8.5%.
In sum, described release film provided by the present invention, by adopting acrylate modified silicone resin as parting agent, while raising organosilyl surface tension force, also increases organosilicon to the sticking power of BOPET film.By adopting the organosilane monomer containing vinyl, organosilicon ratio can be controlled well, making the medium range that the peeling force of modified organic silicon release film controls; Compare with grafting modifying silicone resin, the existence of vinyl can increase substantially the ratio of acrylate in copolymerization product, further increases organosilyl solvability, improves the homogeneity after coating.Release film of the present invention, the advantages such as have higher surface tension, peeling force is moderate, and remaining adhesion rate is excellent.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (7)
1. a release film, is characterized in that, described release film comprises BOPET film, described BOPET film is coated with a parting agent layer;
Wherein, described parting agent layer, its raw material composition comprises reactant monomer, initiator and toluene;
Described reactant monomer, according to mass percent, comprises following component:
Organosilicon performed polymer:
Organosilane monomer 20% ~ 30% containing vinyl;
Acrylate monomer:
Vinylformic acid 30% ~ 40%; Methyl acrylate or methyl methacrylate 8% ~ 15%; Ethyl propenoate or butyl acrylate 10% ~ 20%; Vinylbenzene 5% ~ 10%; Propenoic acid, 2-methyl, isobutyl ester 4% ~ 10%;
Described initiator comprises one or more in dilauroyl peroxide, benzoyl peroxide, dicumyl peroxide, and the consumption of initiator is the 1.0wt% ~ 2.5wt% of reactant monomer quality.
2. release film according to claim 1, is characterized in that, described parting agent layer, and its raw material composition also comprises solidifying agent and diluting solvent;
Wherein, described solidifying agent is aziridine CX-100, and consumption accounts for 3% ~ 5% of vinylformic acid quality;
The mass ratio of parting agent and diluting solvent is 1.0:2.0 ~ 3.8; Diluting solvent comprise in ethylene glycol monomethyl ether and toluene one or both.
3. release film according to claim 2, is characterized in that, the diluting solvent used is ethylene glycol monomethyl ether and toluene, and parting agent, consumption mass ratio between ethylene glycol monomethyl ether and toluene are 1.0:0 ~ 0.8:2.0 ~ 3.0.
4. release film according to claim 1, is characterized in that, described organosilicon performed polymer is vinyl triacetoxy siloxanes; The BOPET film mist degree selected is not more than 1%.
5. a preparation method for release film as claimed in claim 1, is characterized in that, comprises the following steps:
The toluene of whole organosilicon performed polymers, part and the initiator of part are joined in reactor;
Acrylic ester monomer, remaining initiator and toluene are mixed to make and adds liquid;
Reactor starts and stirs and heat, and when being heated to 85 ± 2 DEG C DEG C, add liquid described at the uniform velocity dripping in the reactor, time for adding controls at 2 ~ 4h; Be warming up to 92 ± 2 DEG C DEG C after dropping terminates, insulation 3 ~ 4h, to be triggered dose be exhausted after, cooling, discharging, obtain described parting agent;
Described parting agent is coated in described BOPET film.
6. the preparation method of release film according to claim 5, is characterized in that, the process that described parting agent is coated in described BOPET film is specifically comprised the following steps:
By the parting agent of gained and diluting solvent blended, simultaneously add solidifying agent in proportion, be diluted to coating fluid, use reticulate pattern formula coating machine to be evenly coated in BOPET film, dry;
Described solidifying agent is aziridine CX-100, and consumption accounts for 3% ~ 5% of vinylformic acid quality;
The mass ratio of parting agent and diluting solvent is 1.0:2.0 ~ 3.8; Diluting solvent comprise in ethylene glycol monomethyl ether and toluene one or both.
7. the preparation method of release film according to claim 6, is characterized in that, the diluting solvent used is ethylene glycol monomethyl ether and toluene; Parting agent, consumption mass ratio 1.0:0 ~ 0.8:2.0 ~ 3.0 between ethylene glycol monomethyl ether and toluene.
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| CN201410742980.2A CN104497332B (en) | 2014-12-05 | 2014-12-05 | A kind of mould release membrance and preparation method thereof |
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| CN201410742980.2A CN104497332B (en) | 2014-12-05 | 2014-12-05 | A kind of mould release membrance and preparation method thereof |
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Cited By (6)
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| CN106220880A (en) * | 2016-07-29 | 2016-12-14 | 苏州睿利斯电子材料科技有限公司 | A kind of light off-type force Anti-static release liner |
| CN106273937A (en) * | 2016-07-29 | 2017-01-04 | 苏州睿利斯电子材料科技有限公司 | A kind of PET mould release membrance for base material of aluminizing |
| CN109280449A (en) * | 2017-07-19 | 2019-01-29 | 天津市利好卫生材料有限公司 | A kind of painting silicon release film |
| CN109320749A (en) * | 2018-09-28 | 2019-02-12 | 苏州市星辰科技有限公司 | A kind of normal temperature cure silicon systems release film and preparation method thereof |
| CN109422889A (en) * | 2017-07-19 | 2019-03-05 | 天津市利好卫生材料有限公司 | Apply silicon release film |
| CN110157030A (en) * | 2019-06-05 | 2019-08-23 | 四川羽玺电子科技有限公司 | A kind of preparation process of release film |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220880A (en) * | 2016-07-29 | 2016-12-14 | 苏州睿利斯电子材料科技有限公司 | A kind of light off-type force Anti-static release liner |
| CN106273937A (en) * | 2016-07-29 | 2017-01-04 | 苏州睿利斯电子材料科技有限公司 | A kind of PET mould release membrance for base material of aluminizing |
| CN109280449A (en) * | 2017-07-19 | 2019-01-29 | 天津市利好卫生材料有限公司 | A kind of painting silicon release film |
| CN109422889A (en) * | 2017-07-19 | 2019-03-05 | 天津市利好卫生材料有限公司 | Apply silicon release film |
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| CN109320749A (en) * | 2018-09-28 | 2019-02-12 | 苏州市星辰科技有限公司 | A kind of normal temperature cure silicon systems release film and preparation method thereof |
| CN110157030A (en) * | 2019-06-05 | 2019-08-23 | 四川羽玺电子科技有限公司 | A kind of preparation process of release film |
| CN110157030B (en) * | 2019-06-05 | 2021-11-19 | 四川羽玺电子科技有限公司 | Preparation process of release film |
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| CN104497332B (en) | 2017-09-29 |
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