CN105950041A - Release film having excellent peelability - Google Patents
Release film having excellent peelability Download PDFInfo
- Publication number
- CN105950041A CN105950041A CN201610059877.7A CN201610059877A CN105950041A CN 105950041 A CN105950041 A CN 105950041A CN 201610059877 A CN201610059877 A CN 201610059877A CN 105950041 A CN105950041 A CN 105950041A
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- China
- Prior art keywords
- mould release
- release membrance
- resin
- layer
- thickness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J101/00—Adhesives based on cellulose, modified cellulose, or cellulose derivatives
- C09J101/08—Cellulose derivatives
- C09J101/26—Cellulose ethers
- C09J101/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/201—Adhesives in the form of films or foils characterised by their carriers characterised by the release coating composition on the carrier layer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/748—Releasability
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2367/00—Polyesters, e.g. PET, i.e. polyethylene terephthalate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/20—Presence of organic materials
- C09J2400/22—Presence of unspecified polymer
- C09J2400/225—Presence of unspecified polymer in the release coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
Abstract
The present invention provides a release film excellent in peelability. The release film has a small peeling force, which is not liable to increase with a lapse of time even in a state that the release film adheres to an adhesive layer; the transfer of a silicone component to the adhesive layer is less, and the adhesive force of the adhesive layer to which the film adheres is not reduced. The release film excellent in peelability is characterized in that a release agent layer (4) having a thickness of 0.4 to 2 [mu]m and containing a silicone-based release agent is provided on one surface of a base film (1), and an adhesive resin layer (2) containing inorganic fine particles and/or polymer particles as fine particles (3) are arranged on the other surface of the base film; the fine particles (3), the adhesive resin layer (2) and the release agent layer (4) satisfy the following conditions (1) and (2): (1) the volume reference average particle size of the fine particles (3) is more than twice the thickness of the release agent layer (4); (2) the thickness of the adhesive resin layer (2) is in the range of 25 to 60% of the volume reference average particle size of the fine particles (3).
Description
Technical field
The present invention relates to the surface protection for various adhesive articles or the object with cohesive
Mould release membrance.More specifically, relating to the mould release membrance that fissility is excellent, its peeling force is little, i.e.
Making the state fitting in adhesive phase to pass through the time, peeling force is also difficult to become big and organic
Silicon (silicone) composition is few to the transfer of adhesive phase, thus without the binding agent reducing laminating
The bonding force of layer.
Background technology
For a long time, mould release membrance (sometimes referred to as stripping film) is used for various uses.The widest
General for: manufacture the various ceramic electronic unit such as multilayer ceramic capacitor, ceramic substrate time
The molding mould release membrance of the raw cook (green sheet) used;Manufacture polaroid, light filter,
The mould release membrance used for optical part with adhesive phase used during flat faced display etc.;For touch-control
The adhesive phase of the optical member adhering that panel component or optics are fitted each other is used
Mould release membrance etc..
Use when manufacturing the various ceramic electronic unit such as multilayer ceramic capacitor, ceramic substrate
Raw cook carries out filming along with miniaturization and the high capacity of multilayer ceramic capacitor.This
Outward, when raw cook is peeled off from mould release membrance, in the case of the peeling force of mould release membrance is big,
Raw cook is damaged, therefore seeks the mould release membrance that peeling force compared with the past is little.
On the other hand, as constituting the Polarizer of parts of liquid crystal display, polarizer etc.
In optics, employ mutual for optics or optics and miscellaneous part laminating
Adhesive phase and for protecting the mould release membrance of this adhesive phase.
For the mould release membrance of this purposes along with the maximization of display, the optics such as Polarizer
And the becoming large-sized of mould release membrance, it also is able to greatly easily peel off even if needing to peel off area.Therefore,
Seek the mould release membrance that peeling force compared with the past is little.Additionally, for the structure for making contact panel
Become the adhesive phase used for optical part that parts, optics are fitted each other, along with flat board
The slimming of PC, tablet terminal, contact panel etc., uses the adhesive phase that cohesiveness is weak,
Even the difference of height making film adhesive layer also be able to follow optics (such as, is used for moving
The framework printing (frame printing) of the glass cover-plate (cover glass) etc. of dynamic terminal
Difference of height etc.).But, in the case of the adhesive phase that use cohesiveness is weak, if mould release membrance
Peeling force excessive, adhesive phase the most used for optical part can deform, and therefore seeks compared with the past
The mould release membrance that peeling force is little.
So, in shaping mould release membrance and the various optic with adhesive phase of ceramic green sheet
In part mould release membrance, seek the mould release membrance that peeling force compared with the past is little.With above-mentioned situation for the back of the body
Scape, in patent documentation 1, it is proposed that using the mould release membrance of solidification silicon, described solidification silicon contains
The most only there is the organosilicon of a vinyl.
Additionally, in patent documentation 2, it is proposed that following mould release membrance, in a face of polyester film
On be applied with the anti-sedimentary of oligomer, it has containing solvent-free class additive reaction curing type
The release layer of organosilicon, adhesive tape peeling force is below 15mN/cm, and silicone composition
It is more than 90% that transitivity evaluates bonding rate.
Further, in patent documentation 3, it is proposed that a kind of mould release membrance, it is for using without official
The polydimethylsiloxane that can roll into a ball etc. are without gently peeling off composition (light peeling
Component) addition reaction-type organosilicon, applies 20 hours in the environment of 50~65 DEG C
The mould release membrance of above heat treatment, the peeling force of acrylic adhesives be 0.15N/50mm with
Under, remaining bonding rate is more than 90%.
In patent documentation 1~3, all propose peeling force little and do not reduce the binding agent of laminating
The mould release membrance of the bonding force of layer.But, in the mould release membrance described in patent documentation 1, owing to making
With the solidification silicon containing the organosilicon the most only with a vinyl, if vinyl is anti-
Should be incomplete, the organosilicon the most only with a vinyl shifts to adhesive phase, therefore worries
The bonding force of adhesive phase reduces.
Additionally, for the mould release membrance described in patent documentation 2, be provided with the anti-sedimentary of oligomer,
Different from existing mould release membrance.But, owing to employing the additive reaction curing type of solvent-free class
Organosilicon, for stripping performance, fall into the category of existing mould release membrance.
Further, the mould release membrance described in patent documentation 3 is for by making without gently peeling off composition
The mould release membrance of light separation of addition reaction-type organosilicon ripening (aging).At this
In the case of, though being light stripping, it is possible to do not reduced the bonding force of the adhesive phase of laminating
Mould release membrance, but it is difficult to further reduce peeling force.
Additionally, the mould release membrance described in patent documentation 4 is, make in polyester film containing regulation particle diameter
The organosilicon peel ply of inert particle (inert particle) be formed as the release of specific thickness
Film.By the inert particle of regulation particle diameter is joined in organosilicon peel ply, solve and made
When machine silicon peel ply thickens produce adhesion (blocking) (when being roll by release film roll,
The back side of mould release membrance bonding, the phenomenon that cannot smoothly wind doubtful with peel ply).But, by
In inert particle, organosilicon peel ply becomes discontinuous, if solvent contact, then has solvent-saturated
The possibility that inert particle and the interface of organosilicon, organosilicon come off.Additionally, due to the addition of grain
The inert particle that footpath is bigger than organosilicon peel ply thickness, at the table that mould release membrance is used for adhesive phase
In the case of the protection of face, inert particle may be attached to adhesive phase side, makes adhesive phase
Bonding force reduce.
Prior art literature
Patent documentation
Patent documentation 1: JP 2008-265227 publication
Patent documentation 2: JP 2012-136612 publication
Patent documentation 3: JP 2006-007689 publication
Patent documentation 4: JP 2013-208897 publication
Summary of the invention
The technical problem to be solved in the present invention
The technical problem of the present invention is the mould release membrance providing fissility excellent, and its peeling force is little,
Even if passing through the time to fit in the state of adhesive phase, peeling force is also difficult to become big, and has
Machine silicon composition is few to the transfer of adhesive phase, thus without the bonding of the adhesive phase reducing laminating
Power.
Solve the technological means of technical problem
Having carried out conscientiously studying to solve above-mentioned problem, result specify that, in order to not reduce
The bonding force of adhesive phase, needs to employ silicone mould release and (sometimes referred to as peels off
Agent) mould release membrance become organosilicon to the adhesive phase few mould release membrance of transfer.Even if additionally,
Employ organosilicon in the case of the adhesive phase few silicone mould release of transfer, to making stripping
Diminishing from power and study, result also specify that, by making the thickness of parting agent layer be specific
More than thickness, it is possible to make peeling force diminish.But specify that, become at the thickness making parting agent layer
In the case of thickness, mould release membrance being wound into roll, parting agent layer is at the back side fitting in mould release membrance
Time stick together, mould release membrance cannot become roll by rollback smoothly.For the base material film of mould release membrance at it
In manufacturing process, even if not sticking together to make base material film be wound into roll, make base material
Film carries out film forming containing lubricant particle.Therefore, at the back side of mould release membrance, base material film
Although surface has a concaveconvex structure, but thickening by the thickness that makes parting agent layer, and parting agent layer is filled out
The concaveconvex structure having buried base material film surface is considered as the reason sticked together.
Additionally, carried out conscientiously studying to taking into account the fissility method with resistance to adhesive, it is thus possible to
Enough complete the present invention.Even if the present invention employ silicone ingredients to adhesive phase transfer few
In the case of mould release, in order to reduce peeling force, the thickness making parting agent layer is more than 0.4 μm.
Additionally, the technological thought of the present invention is, in order to prevent the adhesion of parting agent layer and the mould release membrance back side,
By on the face contrary with parting agent layer at base material film, formed and be consistent with the thickness of parting agent layer
The concaveconvex shape of the surface roughness closed, thus take into account fissility and resistance to adhesive.
In order to solve described technical problem, the present invention provides a kind of mould release membrance, it is characterised in that
A face of base material film is provided with thickness be 0.4~2 μm containing silicone mould release
Parting agent layer, is provided with containing inorganic particles and/or polymer particles on the other surface as micro-
The adhesive resin layer of grain, described microgranule, described adhesive resin layer and described parting agent layer are full
Foot 2 times that volume reference mean diameter is described parting agent layer thickness of (1) described microgranule with
On, and the thickness of (2) described adhesive resin layer is in the volume reference average particle of described microgranule
In the range of the 25~60% of footpath.
Described inorganic particles be preferably selected from by silicon dioxide, calcium carbonate, calcium phosphate, barium sulfate,
More than one in the inorganic particle group that Kaolin, glass dust, Talcum are constituted.Additionally, institute
State polymer particles to be preferably selected from by silicone resin, acrylic resin, polyamide-based
Resin, polyester resin, polythylene resin, polypropylene-based resin, polystyrene resins,
More than one in the macromolecule resin granule group that epoxylite is constituted.
Additionally, described base material film is preferably polyester resin film.
Additionally, the present invention provides a kind of laminated film, it has at least one face of resin molding
It is laminated with the laminate of adhesive phase or single adhesive phase and described mould release membrance, by by institute
State mould release membrance to fit in via described parting agent layer and form on the surface of described adhesive phase.
Invention effect
In accordance with the invention it is possible to provide the shaping mould release membrance for ceramic green sheet, various have
The mould release membrance that the fissility of the optics of adhesive phase is excellent.Additionally, the present invention can provide
The mould release membrance that a kind of fissility is excellent, its mould release membrance peeling force is little, even if to fit in binding agent
The state of layer passed through the time, and peeling force is also difficult to become big, and silicone ingredients is to adhesive phase
Transfer few, the most do not reduce the bonding force of the adhesive phase of laminating.
Additionally, the mould release membrance of the present invention will not reduce the bonding force of the adhesive phase of laminating, and by
Even if not sticking together and successfully rollback in roll can be wound as, thus take into account excellence
Fissility and resistance to adhesive, value industrially is big, thus its industrial value is very big.
Accompanying drawing explanation
Fig. 1 is the sectional view of an example of the mould release membrance schematically showing the present invention;
Fig. 2 is the cross section of the example of the 1st embodiment of the laminated film schematically showing the present invention
Figure;
Fig. 3 is the cross section of the example of the 2nd embodiment of the laminated film schematically showing the present invention
Figure.
Description of reference numerals
1 is base material film, and 2 is adhesive resin layer, and 3 is inorganic particles or polymer particles, 4
For parting agent layer, 5 is mould release membrance, and 6 is adhesive phase, and 7 is blooming, 8 be blooming with
The laminate of adhesive phase, 9 is optical bonding sheet, and 10 is adhesive blooming.
Detailed description of the invention
Hereinafter the suitable embodiment of the present invention is illustrated.
Fig. 1 is the sectional view of an example of the mould release membrance schematically showing the present invention, at base material film 1
A face on be formed with adhesive resin layer 2, the opposing face of base material film 1 has been formed
Machine silicon class parting agent layer 4.
In this adhesive resin layer 2, as tissue adhesion with microgranule 3 containing inorganic particles and/
Or polymer particles.
In the mould release membrance 5 of the present invention, as long as the resin molding as base material film 1 selects according to purposes
Select, polyester resin film, polyamide resin, polyimide resin film can be listed, gather
Olefin resin film, polyvinyl chloride resin film, polystyrene resin film, acrylic resin film, second
Acid ester resin film, polyphenylene sulfide resin adipose membrane etc..
Wherein, in terms of the characteristic such as optical characteristics, heat-resistant quality or in price, outward appearance taste
Etc. from the point of view of aspect, be suitably polyester resin film.As polyester resin, can list poly-to benzene two
Formic acid glycol ester, PEN, polyethylene glycol isophthalate are right with poly-
The copolymer of PET, polybutylene terephthalate (PBT) etc..Among this,
From the point of view of cost or optical characteristics, particularly preferred polyethylene terephthalate
(PET).If in addition from the standpoint of optical characteristics, preferably uniaxial tension product or
The optics polyethylene terephthalate of biaxial stretching product.
Additionally, as required, it is also possible to apply on the surface of base material film 1 to put via plasma
Electricity or the easy bonding process such as the surface modification of corona discharge, coating anchor coating agent.
The thickness of base material film 1 has no particular limits, if the operation being considered as mould release membrance 5 is held
Easily degree or mould release membrance 5 is wound into roll, the thickness of base material film 1 is preferably 10~200 μm
Left and right.
In the present invention, even if the thickness of the parting agent layer containing silicone mould release is carried out
Thicken, on the surface contrary with parting agent layer of base material film 1, formed and meet mould release thickness
The concaveconvex structure of surface roughness of degree, makes parting agent layer not send out when fitting in the back side of mould release membrance
Raw adhesion.Forming concaveconvex structure on the surface of base material film 1 is by will be containing as tissue adhesion
Be coated with the inorganic particles of microgranule 3 and/or the adhesive resin layer 2 of polymer particles and
Formed.
As serving as inorganic particles and/or the polymer particles of tissue adhesion microgranule 3, can enumerate
Go out the inorganic particles as inorganic compound microgranule, micro-as the polymer of macromolecule resin microgranule
Grain.Inorganic particles and polymer particles can use any of which, the most also can be same by both
Time use.Inorganic particles be preferably selected from by silicon dioxide, calcium carbonate, calcium phosphate, barium sulfate,
More than one in the inorganic particle group that Kaolin, glass dust, Talcum are constituted.Additionally, it is poly-
Compound microgranule be preferably selected from by silicone resin, acrylic resin, polyamide-based resin,
Polyester resin, polythylene resin, polypropylene-based resin, polystyrene resins, epoxy
More than one in the macromolecule resin granule group that resinoid is constituted.
There is no particular limitation for the shape of microgranule 3, spherical, bar-shaped, flakey, hemispherical,
Lens-shaped, mushroom, irregularly shaped etc., due to the spherical or shape of almost spherical
Easily show tissue adhesion performance, be therefore more suitable for.
As volume reference mean diameter, the particle diameter of microgranule 3 is preferably the thickness of parting agent layer 4
More than 2 times.If the volume reference mean diameter of microgranule 3 is less than the thickness of parting agent layer 4
2 times, then there is the possibility that tissue adhesion performance reduces.The volume reference mean diameter of microgranule 3 be from
More than 2 times of the thickness of type oxidant layer 4, then be obtained in that tissue adhesion performance.The volume of microgranule 3
The upper limit of benchmark mean diameter is not specially constructed problem, but puts down in the volume reference making microgranule 3
In the case of all particle diameter becomes greatly, the thickness making adhesive resin layer 2 is needed to thicken, thus cost
Increase.Therefore, the volume reference mean diameter of microgranule 3 preferably controls the thickness to parting agent layer 4
About 10 times of degree.Additionally, according to volume reference mean diameter, bulky granule effect
Greatly, though the little granule of volume be mixed into wherein affect the least, therefore, if at least some of
Grain has the particle diameter of more than 2 times of parting agent layer 4 thickness, it becomes possible to obtain tissue adhesion performance.
If the resin microgranule 3 for adhesive resin layer 2 disperses and is attached at base material film 1,
Then there is no particular limitation.Include, for example out polyester resin, acrylic resin, poly-ammonia
Esters resin, alkyd based resin, silicone resin, cellulosic resin, polyvinyl alcohol,
Silanes coating agent, silicates coating agent etc..
Resin for adhesive resin layer 2 can be aqueous, non-aqueous (solvent borne) or
No-solvent type.The thickness of adhesive resin layer 2 is preferably in the volume reference mean diameter of microgranule 3
25~60% in the range of.If the thickness of adhesive resin layer 2 is less than the volume base of microgranule 3
The 25% of quasi-mean diameter, then the anchor force (anchoring force) of microgranule 3 declines, micro-
Grain 3 becomes easily to come off.If additionally, the thickness of adhesive resin layer 2 exceedes the volume of microgranule
The 60% of benchmark mean diameter, can produce the problems such as tissue adhesion performance reduces, cost price is high,
The most preferred.
Microgranule 3 is mixed in the resin forming adhesive resin layer 2, coats on base material film 1.
A part (top) for microgranule 3 (does not has the portion of microgranule 3 than the thickness of adhesive resin layer 2
The average thickness divided) prominent.The upper face of microgranule 3 relatively can be attached with bonding by unfertile land
The resin of agent resin bed 2, or can also be non-cohesive.
In terms of the adhesion preventing mould release membrance, it is important that microgranule 3, adhesive resin layer 2 and
Parting agent layer 4 meets following two conditions:
(1) more than 2 times of the thickness that volume reference mean diameter is parting agent layer 4 of microgranule 3;
(2) thickness of adhesive resin layer 2 is in the volume reference mean diameter of microgranule 3
In the range of 25~60%.
For the microgranule 3 mixing in adhesive resin, process for dispersing, according to adhesive resin
And the kind of microgranule uses known method to carry out.If microgranule is readily dispersed in binding agent
System in resin, uses the manual utensil stirrings such as scoop (spatula) to mix.Even if
In adhesive resin, scattered combination or easy scattered system it is difficult to, in bonding for microgranule
Agent resin and microgranule be substantial amounts of in the case of, it is possible to use homogenizer (homogenizer)
Or the disperser such as mixer for well-distribution (homomixer) carries out dispersion mixing.Additionally, except micro-
Outside grain and adhesive resin, it is also possible to be added as needed on surfactant, coloring agent, resist
The anti-fouling agents such as the lubricant such as electrostatic agent, paraffin, organosilicon or fluorine, levelling agent, firming agent, anti-
Rotten agent etc..
As long as being formed the bonding containing microgranule 3 of the adhesive resin layer 2 containing microgranule 3
Agent is resin-coated to be arranged at base material film 1.There is no particular limitation for coating process, only
Will be according to the viscosity of the adhesive resin containing microgranule 3, coating weight, from known coating process
In select.As an example, can list Meyer rod (meyer bar) method, notch board method,
Inverse roller method, air knife method, multistage roller method etc..
The solidification (curing) of the adhesive resin layer 2 containing microgranule 3 or cure
(solidifying) as long as carrying out according to the kind of adhesive resin.Such as, can enter
Go and remove solvent or water etc. by heat drying, irradiated by ultraviolet or electron beam irradiation etc. is made
Adhesive resin solidification etc..
As the mould release for parting agent layer 4, silicone mould release can be listed.Organic
In silicon class mould release, can list addition reaction-type, condensation reaction type, cationic polymerization type,
The known silicone mould release such as radical polymerization mould assembly (radical polymerization type).
, include, for example out in commercially available product as addition reaction-type silicone mould release
KS-776A、KS-776L、KS-847、KS-847T、KS-779H、KS-837、KS-778、
KS-830、KS-774、KS-3565、X-62-2829、KS-3650、KNS-3051、
KNS-320A, KNS-316, KNS-3002, X-62-1387 (SHIN-ETSU HANTOTAI's chemical industry (strain)
System), SRX-211, SRX-345, SRX-357, SD7333, SD7220, SD7223,
LTC-300B、LTC-350G、LTC-310、LTC-750A、SP-7025、SP-7248S、
SP-7015, SP-7259, LTC-1006L, LTC-1056L (Dow Corning Toray (strain)
System), TPR-6722, TPR-6721, TPR-6702, TPR-6700, TPR-6600, SL6625
(Momentive Performance Materials society system) etc..As condensation reaction type
In commercially available product, include, for example out SRX-290, SYLOFF-23 (Dow Corning
Toray (strain) makes), YSR-3022 (Momentive Performance Materials society system)
Deng.In the product commercially available as cationic polymerization type, include, for example out TPR-6501,
TPR-6502、TPR-6500、UV9300、VU9315、UV9430(Momentive
Performance Materials society system), X62-7622, X-62-7660, X-62-7655 (letter
More chemical industry (strain) system) etc..As radical polymerization mould assembly in commercially available product, example
As KF-2005, X62-7205 (SHIN-ETSU HANTOTAI's chemical industry (strain) system) etc. can be listed.As
Silicone ingredients, to the few mould release of transfer of adhesive phase, can list and not contain light stripping and add
Add composition (without the organosilicon of the organo-functional group participating in additive reaction, such as, poly dimethyl
Siloxanes etc.) silicone mould release.
For the silicone mould release of the mould release membrance of the present invention, can be used alone one, also
Multiple Cultivar mixtures can be used.In addition it is also possible to add silane coupler, antistatic additive,
Composition beyond the silicone mould releases such as wettability modifying agent, as long as considering fissility, painting
Cloth, curable etc. determine.The coating of mould release can be carried out by known method,
There is no particular limitation, can list Meyer rod method, notch board method, inverse roller method, air knife method, many
Level roller method etc..The curing of silicone mould release can list be heating and curing, ultraviolet solid
Change, electronic beam curing, heating irradiate the methods such as use simultaneously, according to silicone with ultraviolet
The kind of mould release selects suitable method.Parting agent layer containing silicone mould release
The thickness of 4 for example, 0.4~2 μm.If the thickness of parting agent layer 4 is less than 0.4 μm, peeling force
Easily become big.Additionally, the upper limit of the thickness of parting agent layer 4 is not specially constructed problem, make
In the case of the thickness of parting agent layer 4 increases, in the volume reference mean diameter increasing microgranule 3
While, need the thickness making adhesive resin layer 2 to thicken, thus cost up.Therefore,
The thickness of parting agent layer 4 preferably controls to 2 μm.
Made when the mould release membrance 5 of the present invention being used at the various ceramic electronic unit of manufacture
Raw cook molding release sheet in the case of, raw cook be scattered in by ceramic particle organic
The coating of the serosity of solvent, it is dried and is formed.This for protecting raw cook purposes
In mould release membrance 5, for parting agent layer 4, it is desirable to solvent resistance.The parting agent layer 4 of the present invention
Due to without microgranule 3, be silicone mould release will not discontinuously, solvent resistance the best
Parting agent layer 4, it is possible to be suitably used for protecting the purposes of raw cook.Additionally, be not limited to raw cook,
Can be suitably used for protecting conductor paste, insulating paste etc. to be dispersed with the film of various powder body, contain
The purposes on the surface of the film of solvent.
Fig. 2 is the cross section of the example of the 1st embodiment of the laminated film schematically showing the present invention
Figure.The adhesive blooming 10 of Fig. 2 is to be used for protecting lamination by the mould release membrance 5 of the present invention
In the purposes of the adhesive phase 6 on blooming 7.On the mould release membrance 5 of the present invention of Fig. 1,
It is fitted with blooming 7 via adhesive phase 6.The manufacturer of this adhesive blooming 10
Method can be coating solvent type adhesive on mould release membrance 5, after drying, and blooming 7 of fitting.
In this mould release membrance 5 for protecting the purposes of adhesive phase 6, for parting agent layer 4,
Require solvent resistance.The parting agent layer 4 of the present invention due to without microgranule 3, be silicone from
Type agent will not discontinuously, the best parting agent layer 4 of solvent resistance, it is possible to be suitably used for protecting
Protect in the purposes of adhesive phase 6.Laminate containing adhesive phase 6 can be containing 1 or 2
Individual above resin molding and 1 or the adhesive phase of more than 2.For example, it is also possible at optics
The two sides of film 7 arranges adhesive phase 6, mould release membrance 5 of fitting on each adhesive phase 6.As
Other manufacture method, it is also possible to be that a face of blooming 7 is provided with adhesive phase 6
On laminate 8, mould release membrance 5 of fitting.Or, it is possible to after coating non-solvent adhesive,
Between mould release membrance 5 and blooming 7, adhesive phase 6 is made to solidify by light or heat etc..
Additionally, the example of the 2nd embodiment that Fig. 3 is the laminated film schematically showing the present invention
Sectional view.The optical bonding sheet 9 of Fig. 3 is for contact panel parts, the patch of optics
On the adhesive phase 6 closed, the mould release membrance 5 of the laminating present invention is to protect this adhesive phase 6.Light
Learning bonding sheet 9 is the form that two panels mould release membrance 5 clamps adhesive phase 6.At this optical bonding
In the manufacture method of sheet 9, generally, a piece of mould release membrance 5 is coated with, is dried solvent-borne type bonding
After agent, fit with another sheet mould release membrance 5.This for protecting the purposes of adhesive phase 6
In mould release membrance 5, for parting agent layer 4, it is desirable to solvent resistance.The parting agent layer 4 of the present invention
Due to without microgranule 3, be silicone mould release will not discontinuously, solvent resistance the best
Parting agent layer 4, it is possible to be suitably used in the purposes of protection adhesive phase 6.
Binding agent for adhesive phase 6 can be aqueous, non-aqueous (solvent borne) or nothing
Solvent-borne type.As binding agent, acrylic adhesives, silicone binding agent, rubber-like are viscous
Mixture, polyurethane binding etc..Acrylic adhesives the transparency, have excellent weather resistance,
So preferably.
Resin molding for laminated film is not limited to blooming 7, as long as being that opaque resin molding is
Can.As blooming, light polarizing film, phase retardation film, antireflection film, anti-dazzle can be listed
(anti-glare) film, ultraviolet-absorbing film, infrared absorbing film, optical compensation films, blast
Film, high grade of transparency film etc..
Embodiment
Hereinafter, by embodiment, the present invention is specifically described.
(mould release membrance of embodiment 1)
7.5 weight portion ethyl celluloses (DOW Chemical society system, business is put in beaker
The name of an article: ETHOCEL (registered trade mark) 100FP), 0.0375 weight portion mean diameter (body
Long-pending benchmark mean diameter) it is the silicone particulate polymer resin (Momentive of 2 μm
Performance Materials society system, trade name: Tospearl (registered trade mark) 120), 92.5
50/50 mixed solvent of parts by weight of toluene/ethyl acetate also mixes, and stirs molten to ethyl cellulose
Solve, make coating.Then, thickness 50 μm, one side sided corona treatment polyester film corona not
On process face, the thickness being made dried adhesive resin by the coating of Meyer rod method is 1.0 μm
After, use the heated air circulation type exsiccator of 120 DEG C to heat 1 minute, set on one face
There is the polyester film of surface unevenness profile.Then, it is provided with concaveconvex shape at obtained polyester film
Face opposing face (sided corona treatment face) on, by Meyer rod method be coated with relative to 30 weight
Part addition reaction-type silicone release agent (Dow Corning Toray society system, trade name:
LTC-1056L) 1 weight portion platinum catalyst (Dow Corning Toray society system, commodity are mixed
Name: SRX212 CATALYST), 70 parts by weight of toluene/ethyl acetate 50/50 mixing molten
The mixed coating of agent, making dried thickness is 1.0 μm, and using design temperature is 120 DEG C
Heated air circulation type exsiccator heat 1 minute, obtain the mould release membrance of embodiment 1.
(confirmation of adhesive)
In embodiment 1, change adhesive resin layer (ethyl cellulose) and parting agent layer
Thickness and the kind of silicone particulate polymer resin, obtain manufacturing the mould release membrance of example 1~12,
Additionally, the manufacture example 5 that described embodiment 1 is table 1.
The mould release membrance of the manufacture example 1~12 for obtaining, to parting agent layer and adhesive resin layer
Carry out confirming experiment with or without adhesion and with or without coming off of microgranule.
(with or without the confirmation of adhesion)
Make the sample that 3 mould release membrances are overlapping, be sandwiched two panels corrosion resistant plate (SUS304)
Between.On this sample, to apply 20g/cm2{0.196N/cm2The state of load,
23 DEG C, place 24 hours in the environment of 50%RH.Then, take out 3 overlapping from
Type film, by confirming adhesion state with hands strip off mould release membrance piecewise.Light without adhesion, mould release membrance
Under easy-peel for adhesive good (zero), mould release membrance exist when peeling off a little resistance for adhesive
The worst (Δ), mould release membrance peel off time exist notable resistance for adhesive bad (×).
(with or without the confirmation of particles from getting loose)
With non-woven fabrics (fiber society of Asahi Chemical Industry bemcot (registered trade mark) M-1) with 200
Loaded state entering containing fine-grained adhesive resin coated face mould release membrance executed by g counterweight
Row once reciprocal wiping.Then, the part wiped across sample with laser microscope is observed.
To measure at 10 at the residual of microgranule and the number at the place that comes off, coming off less than 30% of microgranule
For good (zero), microgranule come off be more than 30% for bad (×).
(result of validation test)
The result of validation test is as shown in table 1.
[table 1]
Knowable to the result of the validation test shown in table 1, as parting agent layer and adhesive resin
The condition that layer does not sticks together, the thickness of parting agent layer becomes the thickest, then need adhesive resin
The surface roughness (concavo-convex) of layer is the biggest.Additionally, from the result of the validation test shown in table 1,
The condition not sticked together as parting agent layer and adhesive resin layer, obtains following microgranule (nothing
Machine microgranule or polymer particles) the pass of thickness of volume reference mean diameter and parting agent layer
The thickness of system and adhesive resin layer is relative to microgranule (inorganic particles or polymer particles)
The relation of mean diameter:
I the mean diameter of () microgranule is more than 2 times of the thickness of parting agent layer;
(ii) thickness of adhesive resin layer is less than 75% relative to the mean diameter of microgranule.
On the other hand, as not making microgranule from the bar come off containing fine-grained adhesive resin layer
Part, needs the thickness making the adhesive resin layer of the mean diameter relative to microgranule to thicken.By table
The result of the validation test shown in 1 derive following, do not make microgranule from containing fine-grained bonding
The thickness of the adhesive resin layer come off in agent resin bed:
(iii) thickness of adhesive resin layer is more than 25% relative to the mean diameter of microgranule.
Additionally, in the result of the validation test shown in table 1, by manufacturing example 6 and manufacturing example
The comparison of 7 understands, for condition (ii), as long as the thickness of adhesive resin layer is relative to micro-
The volume reference mean diameter of grain is less than 60%, then parting agent layer is not sent out with adhesive resin layer
Raw adhesion.
That is, according to the result of the validation test shown in table 1, as parting agent layer and binding agent tree
Condition and microgranule that lipid layer does not sticks together do not come off from containing fine-grained adhesive resin layer
Condition, obtain following condition:
(1) mean diameter of microgranule is more than 2 times of thickness of parting agent layer;
(2) thickness of adhesive resin layer is in 25~the scope of 60% of the mean diameter of microgranule
In.
(embodiment 2)
In addition to the thickness of parting agent layer is set to 0.4 μm, with side same as in Example 1
Formula makes the mould release membrance of embodiment 2.
(embodiment 3)
In addition to the thickness of parting agent layer is set to 0.5 μm, with side same as in Example 1
Formula makes the mould release membrance of embodiment 3.
(embodiment 4)
Weighing 7.5 weight account polyethylene alcohol (Kuraray society system, trade name: POVAL 203),
92.5 weight portion ion exchange water.In beaker, add ion exchange water, be heated up to 80 DEG C of left sides
After the right side, add polyvinyl alcohol while stirring, continue stirring to polyvinyl alcohol and be completely dissolved.Cold
But to after room temperature, add 0.0375 weight portion volume reference mean diameter be 2.7 μm without fixed
Shape silicon dioxide (silysia society of Fuji system, trade name: sylysia (registered trade mark) 310P),
It is stirred mixing by homogenizer dispersed to silicon dioxide, makes containing fine-grained bonding
Agent cold coating.
Then, on the sided corona treatment face that thickness is 50 μm, two sides sided corona treatment polyester film,
It is coated with the adhesive resin coating prepared by Meyer rod method, makes dried adhesive resin
Thickness be 1 μm, use design temperature be 120 DEG C heated air circulation type exsiccator heat 3 points
Clock, is provided with the polyester film of surface unevenness profile on one face.Then, poly-obtain
Added by the coating mixing of Meyer rod method on the opposing face (sided corona treatment face) of the concaveconvex shape of ester film
Become response type silicone release agent (trade name of 18 weight portion Dow Corning Toray societies:
LTC-1056L, the trade name of 40 chemical industry societies of weight portion SHIN-ETSU HANTOTAI: KS-847T), 1 weight
Amount part platinum catalyst (Dow Corning Toray society system, trade name: SRX212
CATALYST) coating, after 50/50 mixed solvent of 42 parts by weight of toluene/ethyl acetate,
Making dried thickness is 1.0 μm, and the heated air circulation type using design temperature to be 120 DEG C is dried
Device heats 1 minute, obtains the mould release membrance of embodiment 4.
(comparative example 1)
In addition to the thickness of parting agent layer is set to 0.2 μm, with side same as in Example 1
Formula makes the mould release membrance of comparative example 1.
(comparative example 2)
Except the dried thickness of adhesive resin layer (ethyl cellulose) is set to 1.5 μm
In addition, the mould release membrance of comparative example 2 is made in the same manner as example 1.Additionally, compare
Example 2 is the manufacture example 7 of table 1.
(comparative example 3)
On the sided corona treatment face that thickness is 50 μm, one side sided corona treatment polyester film, by stepping
The addition reaction-type silicone release agent that rod method coating is the most exfoliated relative to 5 weight portions
(Dow Corning Toray society system, trade name: SRX-357) is mixed with 0.05 weight portion
Platinum catalyst (Dow Corning Toray society system, trade name: SRX212CATALYST),
The mixed coating of 50/50 mixed solvent of 95 parts by weight of toluene/ethyl acetate, makes to be dried
After thickness be 0.2 μm, use design temperature be 120 DEG C heated air circulation type exsiccator heating
1 minute, obtain the mould release membrance of comparative example 3.
(comparative example 4)
Relative to 30 weight portion addition reaction-type silicone release agent (Dow Corning Toray
Society's system, trade name: LTC-1056L), mix 1 weight portion platinum catalyst (Dow Corning
Toray society system, trade name: SRX212), 70 parts by weight of toluene/ethyl acetate 50/50 mix
Bonding solvent, in the coating of mixing, adding 0.0375 weight portion volume reference mean diameter is
Silicone particulate polymer resin (the Momentive Performance Materials of 2 μm
Society's system, trade name: TOSPEARL (registered trade mark) 120), stirring mixing, make containing
The silicone release agent coating of microgranule.At the one side sided corona treatment polyester film that thickness is 50 μm
On sided corona treatment face, the coating prepared by the coating of Meyer rod method, make the dried thickness be
1.0 μm, the heated air circulation type exsiccator using design temperature to be 120 DEG C heats 1 minute,
Mould release membrance to comparative example 4.
For the mould release membrance obtained in embodiment 1~4 and comparative example 1~4, carry out various mensuration,
Validation test.Confirmation method with or without adhesion is described above.In addition test method is as follows
Described.
(mensuration of peeling force)
Surface laminating polyester binding adhesive tape (day east electrician strain formula meeting in the parting agent layer of mould release membrance
Society's system, trade name: polyester tape No.31B), at 20g/cm2{0.196N/cm2Negative
Under load, after carrying out ripening in 20 hours with 70 DEG C, use desk type accurate universal testing machine (Shimadzu
Make institute society system, Autograph (registered trade mark)), measure with peeling rate 300mm/ minute,
Peel strength when peel angle 180 ° is peeled off is as peeling force (mN/50mm).
(mensuration of remaining bonding rate)
The adhesive tape that mould release membrance after testing from above-mentioned (mensuration of peeling force) with roller peels
Adherend (corrosion resistant plate) is crimped, 23 DEG C, place 1 in the environment of 55%RH
After hour, use desk type accurate universal testing machine (society of Shimadzu Seisakusho Ltd. system, Autograph (note
Volume trade mark)), measure with peeling rate 300mm/ minute, peel angle 180 ° from this adherend
Peeling force during stripping is as remaining bonding force.
In addition, similarly measure untapped adhesive tape is crimped on the quilt of identical material
Peeling force when peeling off on viscous thing is as benchmark bonding force.
Remaining bonding rate is calculated by formula (residual adhesion)/(benchmark bonding force) × 100 (%).
(confirmation of the attaching of parting agent layer)
Parting agent layer by the mould release membrance after above-mentioned (mensuration of peeling force) being tested by finger belly
Surface carry out 3 strong wipings after, with the part of visualization wiping.By being visually confirmed to be
Come off from base material film with or without parting agent layer, be assessed as (zero) almost without what parting agent layer came off,
Parting agent layer has come off a little to be assessed as (△), what parting agent layer significantly came off be assessed as (×).
(confirmation of the solvent resistance of parting agent layer)
Use non-woven fabrics (the fiber society of Asahi Chemical Industry bemcot (registered trade mark) being soaked with ethyl acetate
M-1), the parting agent layer of mould release membrance is carried out one executing loaded state with the counterweight of 200g
Secondary reciprocal wiping.Then, by the parting agent layer with visualization mould release membrance, confirm mould release membrance
The solvent resistance of parting agent layer.With being visually confirmed to be the surface of parting agent layer, outward appearance is unconverted
It is assessed as (zero), what mould release came off be assessed as (×).
(mensuration, the result of validation test)
The various mensuration of mould release membrance that obtain in embodiment 1~4 and comparative example 1~4, confirmation
The result of test is as shown in table 2.
[table 2]
(summary)
The mould release membrance peeling force of embodiment 1~4 is the least, and remaining bonding rate demonstrates the highest
Numerical value.Additionally, the parting agent layer of the mould release membrance of embodiment 1~4 is not sent out with adhesive resin layer
Raw adhesion, the attaching of silicone mould release, solvent resistance are the best.In contrast,
The mould release membrance of the comparative example 1 that the thickness of parting agent layer is thin is peeling the knot of weight (peeling force is big)
Really.Additionally, the concavo-convex little (bonding containing fine-grained adhesive resin layer of mould release rear side
The thickness of agent resin bed is big relative to the ratio of the mean diameter of microgranule) the mould release membrance of comparative example 2
There occurs adhesion, peeling force also becomes big.It is coated with normally used light stripping with common coating weight
The overburden ratio embodiment 1~4 of the mould release membrance of the comparative example 3 of type organosilicon is the heaviest, and produces remnants
The result that bonding rate is to be differed from.Containing fine-grained comparative example 4 in silicone mould release
The peeling force of mould release membrance, remaining bonding rate also have a good result, but the attaching of parting agent layer
Property and solvent resistance are bad result.
Claims (4)
1. the mould release membrance that a fissility is excellent, it is characterised in that in a face of base material film
Be provided with thickness be 0.4~2 μm, parting agent layer containing silicone mould release, at another
Face is provided with containing as the inorganic particles of microgranule and/or the adhesive resin of polymer particles
Layer, described microgranule, described adhesive resin layer and described parting agent layer meet following condition (1)
And (2):
(1) the 2 of the thickness that volume reference mean diameter is described parting agent layer of described microgranule
More than Bei;
(2) thickness of described adhesive resin layer is in the volume reference mean diameter of described microgranule
25~60% in the range of.
The mould release membrance that fissility the most according to claim 1 is excellent, it is characterised in that
Described inorganic particles for select free silicon dioxide, calcium carbonate, calcium phosphate, barium sulfate, Kaolin,
More than one in the inorganic particle group that glass dust, Talcum are constituted, described polymer particles is
Select free silicone resin, acrylic resin, polyamide-based resin, polyester resin,
Polythylene resin, polypropylene-based resin, polystyrene resins, epoxylite are constituted
Macromolecule resin granule group in more than one.
The mould release membrance that fissility the most according to claim 1 and 2 is excellent, wherein, institute
Stating base material film is polyester resin film.
4. a laminated film, it has and is laminated with binding agent at least one face of resin molding
The laminate of layer or single adhesive phase and according to according to any one of claims 1 to 3
The mould release membrance that fissility is excellent, by mould release membrance excellent for described fissility via described parting agent layer
The surface fitting in described adhesive phase forms.
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CN106498800A (en) * | 2016-11-04 | 2017-03-15 | 张日龙 | A kind of glassine paper and preparation method thereof |
CN110944840A (en) * | 2017-08-24 | 2020-03-31 | 东洋纺株式会社 | Release film for producing ceramic green sheet |
CN111267451A (en) * | 2018-12-04 | 2020-06-12 | 南亚塑胶工业股份有限公司 | Release film for high-capacity multilayer ceramic capacitor and method for producing same |
CN111748278A (en) * | 2020-07-07 | 2020-10-09 | 浙江洁美电子科技股份有限公司 | Release agent for quickly stripping OCA (optical clear adhesive) and release film containing same |
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CN109627876A (en) * | 2018-12-05 | 2019-04-16 | 香洋新材料(江苏)有限公司 | A kind of thermal transfer mould release and preparation method thereof for digital printing |
CN112917867A (en) * | 2021-03-14 | 2021-06-08 | 山东胜通光学材料科技有限公司 | Preparation method of base film for release film of ceramic capacitor |
KR20240046519A (en) | 2022-08-05 | 2024-04-09 | 미쯔비시 케미컬 주식회사 | release film |
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CN111748278A (en) * | 2020-07-07 | 2020-10-09 | 浙江洁美电子科技股份有限公司 | Release agent for quickly stripping OCA (optical clear adhesive) and release film containing same |
Also Published As
Publication number | Publication date |
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CN105950041B (en) | 2020-07-14 |
JP2016165825A (en) | 2016-09-15 |
KR101836212B1 (en) | 2018-03-08 |
JP6147284B2 (en) | 2017-06-14 |
KR101987643B1 (en) | 2019-06-11 |
TW201639703A (en) | 2016-11-16 |
TWI681875B (en) | 2020-01-11 |
KR20180026696A (en) | 2018-03-13 |
TWI778311B (en) | 2022-09-21 |
KR20160110082A (en) | 2016-09-21 |
TW202010812A (en) | 2020-03-16 |
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