CN108276923A - A kind of UV visbreakings composition, UV visbreaking films and preparation method thereof - Google Patents
A kind of UV visbreakings composition, UV visbreaking films and preparation method thereof Download PDFInfo
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- CN108276923A CN108276923A CN201810105862.9A CN201810105862A CN108276923A CN 108276923 A CN108276923 A CN 108276923A CN 201810105862 A CN201810105862 A CN 201810105862A CN 108276923 A CN108276923 A CN 108276923A
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- visbreakings
- crosslinking agent
- ester
- visbreaking
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- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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- 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
- C09J2465/00—Presence of polyphenylene
- C09J2465/005—Presence of polyphenylene 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
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- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to protection technical field of membrane, more particularly, to a kind of UV visbreakings composition, UV visbreaking films and preparation method thereof.The UV visbreakings composition is mainly made of the following raw material by weight percentage：Acrylate pressure-sensitive adhesive resin 20% 50%, polyfunctionality oligomer and/or polyfunctional monomer 1% 30%, crosslinking agent 0.3% 2%, thermal initiator 0.1% 5%, photoinitiator 0.5% 5% and solvent 25% 60%.The UV visbreakings film includes the substrate layer being bonded successively, UV anti-adhesive layers and release film layer, wherein the UV anti-adhesive layers are to be coated on base material layer surface by the UV visbreakings composition, and drying curing obtains.There is the UV visbreakings composition excellent bonding force, UV pre-irradiations to have high adhesion, and peeling force is high, has low adhesion power after UV irradiations, UV peeling forces are low, and residue glue is not stayed after long-time storage.
Description
Technical field
The present invention relates to protection technical field of membrane, more particularly, to a kind of UV visbreakings composition, UV visbreakings film and its preparation
Method.
Background technology
In semiconductor process, when carrying out semiconductor crystal wafer cutting, polishing, to reduce silicon thin layer defect concentration, often
It is often used wafer cutting visbreaking protective film.Visbreaking protective film refers to that bonding force is strong when in use, and in later stage stripping process, it glues
Resultant force weakens to remove.
Visbreaking protective film currently on the market is mostly UV visbreaking protective films, refers to having high adhesion power in UV pre-irradiations,
Adhesion is good, and bonding force is decreased obviously after UV irradiations, is easily peeled off.Cut for wafer on domestic market and pick technique etc.
The UV visbreakings glue of protection is mostly based on Japan, Taiwan, and domestic UV visbreakings glue is also several to be promoted in research and development, but performance is not yet complete
Stablize.For current UV visbreakings protective film generally after storage about 3 months, the small molecule in glue-line can move to film surface, though
Then bonding force becomes smaller after UV irradiates when the phase removes, but the small molecule of adhesive layer can remain in by fitting body surface, give
It is polluted by fitting object.
In view of this, special propose the present invention.
Invention content
The first object of the present invention is to provide a kind of UV visbreakings composition have excellent bonding force in UV pre-irradiations,
Bonding force, which declines to a great extent, after UV irradiations is easily peeled off, and storage time is long, and residue glue is not stayed after long-time storage.
The second object of the present invention is to provide a kind of UV visbreakings film, and the UV visbreakings film has excellent in UV pre-irradiations
Bonding force, bonding force, which declines to a great extent, after UV irradiations is easily peeled off, and residue glue is not stayed after long-time storage.
Another object of the present invention is to provide a kind of preparation method of the UV visbreakings film, the preparation method operative employees
Skill is simple, favorable repeatability.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme：
A kind of UV visbreakings composition, is mainly made of the following raw material by weight percentage：
Acrylate pressure-sensitive adhesive resin 20%-50%, polyfunctionality oligomer and/or polyfunctional monomer 1%-30%,
Crosslinking agent 0.3%-2%, thermal initiator 0.1%-5%, photoinitiator 0.5%-5% and solvent 25%-60%.
Preferably, the UV visbreakings composition, is mainly made of the following raw material by weight percentage：
Acrylate pressure-sensitive adhesive resin 40%-50%, polyfunctionality oligomer and/or polyfunctional monomer 5%-20%,
Crosslinking agent 1%-2%, thermal initiator 1%-3%, photoinitiator 3%-5% and solvent 35%-60%.
The UV visbreaking compositions that the present invention is prepared by above-mentioned raw materials have excellent bonding force, UV pre-irradiations tool
There is high adhesion, peeling force is high, has low adhesion power after UV irradiations, and UV peeling forces are low, add thermal initiator in the composition,
Small molecule can be consumed in UV visbreaking composition maturing process, the residual of small molecule is reduced, small molecule is avoided to move to glue-line table
Face and cause peeling force to increase, cohesive force reduces, the phenomenon that causing residue glue, to extend storage time.The polyfunctionality is low
Polymers and/or polyfunctional monomer itself generate cross-linking reaction after UV irradiates, and larger volume contraction is generated after cross-linking reaction to be made
Fold is generated between the UV visbreakings composition and adherend body surface face, the big position of fold generates micropore, makes UV visbreaking groups
It closes contact area between object and adherend body surface face to reduce, to realize that visbreaking acts on.
Acrylate pressure-sensitive adhesive resin, under smaller active force, you can firm bonding force is formed, without other
Means can be closely bonded with adherend.
Preferably, the thermal initiator is free radical thermal initiator.It is furthermore preferred that the free radical thermal initiator included
It is one or more in peroxide initiator, azo compound thermal initiator, redox thermal initiator.It is further preferred that institute
It includes azodiisobutyronitrile (AIBN), azobisisoheptonitrile (ABVN), dilauroyl peroxide, peroxidating to state free radical thermal initiator
It is one or more in dibenzoyl, isopropyl benzene hydroperoxide, cyclohexanone peroxide, tert-butyl hydroperoxide etc..
Preferably, the acrylate pressure-sensitive adhesive resin is solvent-type acrylic ester pressure-sensitive adhesive.It is furthermore preferred that described
The molecular weight of acrylate pressure-sensitive adhesive resin is 100,000-200 ten thousand.It is further preferred that the solvent-type acrylic ester pressure-sensitive
The solid content of stick is 25%-60%, viscosity 300cps-20000cps.
Preferably, the polyfunctionality oligomer includes aliphatic urethane acrylate oligomer and epoxy acrylate
One or both of oligomer.
Preferably, the polyfunctional monomer includes pentaerythritol tetraacrylate, double pentaerythritol C5 methacrylate, two
Six acrylate of pentaerythrite, trimethylolpropane trimethacrylate, dipentaerythritol hexaacrylate, trimethylolpropane tris
Acrylate, ethoxyquin trimethylolpropane trimethacrylate, trimethylol-propane trimethacrylate, methacrylic acid-
2- hydroxy methacrylates, acrylamide, dimethacrylate -1,6-HD ester, diacrylate -1,6-HD ester, diacrylate
Glycol ester, diacrylate triethyleneglycol ester, diacrylate tripropylene glycol ester, diacrylate are to neopentyl glycol ester, trihydroxy methyl third
Alkane triacrylate, trihydroxy methyl pentane trimethyl acrylic ester, trimethylolpropane pentaerythritol triacrylate, the third oxidation
In neopentylglycol diacrylate, ethoxyquin 1,6 hexanediol diacrylate and three (2- acrylyl oxy-ethyls) isocyanuric acid esters
It is one or more.
Preferably, the crosslinking agent includes one in isocyanates crosslinking agent, amine cross-linking agent, aziridines crosslinking agent
Kind is a variety of, preferably isocyanates crosslinking agent.
Preferably, the isocyanates crosslinking agent include isophorone diisocyanate, hexamethylene diisocyanate,
One in dicyclohexyl methyl hydride diisocyanate, benzene dimethylene diisocyanate and tetramethylxylylene diisocyanate
Kind is a variety of.It is furthermore preferred that the crosslinking agent is hexamethylene diisocyanate, preferably N3390 (Beyer Co., Ltd) crosslinking agent.
Preferably, the amine cross-linking agent includes in diethylenetriamines, trien and hexamethylenetetramine
It is one or more.
Preferably, the photoinitiator includes 2- isopropyl thioxanthones (ITX), 1- hydroxycyclohexyl phenyl ketones
(184), 2- hydroxy-methyls phenyl third, benzoin dimethylether (651), benzophenone (BP), 2- methyl-1s-(4- methylthio phenyls
Base) -2- morpholinyl -1- acetone (907), 2,4,6- (trimethylbenzoyl)-diphenyl phosphine oxide (TPO), alkane -1- ketone
(1173), one or more in DR-575, preferably 2,4,6- (trimethylbenzoyl)-diphenyl phosphine oxides (TPO).
Preferably, the solvent include acetone, cyclohexanone, ethyl acetate, butyl acetate, butanone, methanol, ethyl alcohol, propyl alcohol,
Isopropanol, isobutanol, n-butanol, methylisobutylketone, isophorone, toluene, dimethylbenzene, propylene glycol monomethyl ether, dipropylene glycol methyl ether
In one or more, preferably butanone.
The method of the UV visbreakings composition is not unique, above-mentioned raw materials can be mixed evenly in proportion and subtract to get UV
Tacking compositions.It is preferred that mixing time is 1-5h, more preferably 2h.
The present invention also provides a kind of UV visbreakings films, including substrate layer, UV anti-adhesive layers and the release film layer being bonded successively,
In, the UV anti-adhesive layers are to be coated on base material layer surface by the UV visbreakings composition, and drying curing obtains.
Preferably, the base material is PET.It is furthermore preferred that the thickness of the substrate layer is 50-150 μm, preferably 75-125 μ
M, more preferably 100 μm.
Preferably, the thickness of the UV anti-adhesive layers is 10-30 μm, preferably 15-25 μm, more preferably 20 μm.
Preferably, the release film layer is PET release film layers, and preferred thickness is 20-50 μm, preferred off-type force range
For 10-100gf.
The present invention also provides a kind of preparation methods of the UV visbreakings film, include the following steps：
UV visbreaking compositions are coated on base material layer surface, release film layer is bonded on UV visbreaking compositions after preliminary drying, it is ripe
Change, obtains the UV visbreakings film.
Preferably, the preliminary drying dries 1-5min under the conditions of being included in 100 ± 10 DEG C, is preferably dried under the conditions of 100 DEG C
2min。
Preferably, the cooking conditions are to cure 20-30h under the conditions of 60 ± 10 DEG C, are preferably cured for 24 hours at 60 DEG C.
Compared with prior art, beneficial effects of the present invention are：
(1) UV visbreaking compositions of the invention have excellent bonding force in UV pre-irradiations, up to 1850gf, are shone in UV
It penetrates rear bonding force and declines to a great extent and be easily peeled off；The UV visbreakings composition storage time is long, and residue glue is not stayed after long-time storage；
(2) the UV visbreakings film that UV visbreakings composition using the present invention obtains has excellent bonding force in UV pre-irradiations,
Bonding force, which declines to a great extent, after UV irradiations is easily peeled off, and residue glue is not stayed after long-time storage；
(3) the preparation method operating procedure of UV visbreakings film of the present invention is simple, and production efficiency is high, favorable repeatability.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, other drawings may also be obtained based on these drawings.
Fig. 1 is a kind of structural schematic diagram of the UV visbreaking films of specific implementation mode of the present invention.
Reference numeral：
1- substrate layers；2-UV anti-adhesive layers；3- release film layers.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with the drawings and specific embodiments, but
Be it will be understood to those of skill in the art that it is following described embodiments are some of the embodiments of the present invention, rather than it is whole
Embodiment is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained without making creative work, belongs to guarantor of the present invention
The range of shield.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same
Or production firm person is not specified in instrument, is the conventional products that can be obtained by commercially available purchase.
In the description of the present invention, it should be noted that term "center", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for the description present invention and simplify description, do not indicate or imply the indicated device or element must have a particular orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for description purposes only, and is not understood to indicate or imply relative importance.
UV visbreakings composition of the present invention, is mainly made of the following raw material by weight percentage：
Acrylate pressure-sensitive adhesive resin 20%-50%, polyfunctionality oligomer and/or polyfunctional monomer 1%-30%,
Crosslinking agent 0.3%-2%, thermal initiator 0.1%-5%, photoinitiator 0.5%-5% and solvent 25%-60%.
In a kind of preferred embodiment of the present invention, the thermal initiator is free radical thermal initiator.It is furthermore preferred that
The free radical thermal initiator includes one in peroxide initiator, azo compound thermal initiator, redox thermal initiator
Kind is a variety of.It is further preferred that the free radical thermal initiator includes azodiisobutyronitrile (AIBN), azobisisoheptonitrile
(ABVN), dilauroyl peroxide, dibenzoyl peroxide, isopropyl benzene hydroperoxide, cyclohexanone peroxide, tert-butyl hydroperoxide
It is one or more in.
Using specific thermal initiator, remaining small molecule can be effectively facilitated in composition maturing process and continues to polymerize
And be gradually consumed, it reduces the residual of small molecule and extends storage time, not residue glue.
In a kind of preferred embodiment of the present invention, the acrylate pressure-sensitive adhesive resin is solvent-type acrylic ester
Pressure-sensitive adhesive.It is furthermore preferred that the molecular weight of the acrylate pressure-sensitive adhesive resin is 100,000-200 ten thousand.It is further preferred that
The solid content of the solvent-type acrylic ester pressure-sensitive adhesive is 25%-60%, viscosity 300cps-20000cps.
Using specific acrylate pressure-sensitive adhesive resin, the bonding force of the UV visbreakings composition is helped to improve, is improved
Peeling force.
In a kind of preferred embodiment of the present invention, the polyfunctionality oligomer includes aliphatic polyurethane propylene
One or both of acid esters oligomer and epoxy acrylate oligomer；The polyfunctional monomer includes pentaerythrite 4 third
Olefin(e) acid ester, double pentaerythritol C5 methacrylate, dipentaerythritol hexaacrylate, trimethylolpropane trimethacrylate, two seasons
Penta tetrol, six acrylate, trimethylolpropane trimethacrylate, ethoxyquin trimethylolpropane trimethacrylate, trihydroxy methyl
Propane trimethyl acrylic ester, methacrylic acid -2- hydroxy methacrylates, acrylamide, dimethacrylate -1,6-HD ester,
Diacrylate -1,6-HD ester, ethylene glycol diacrylate, diacrylate triethyleneglycol ester, diacrylate tripropylene glycol ester, two
Acrylic acid is to neopentyl glycol ester, trimethylolpropane trimethacrylate, trihydroxy methyl pentane trimethyl acrylic ester, trihydroxy methyl
Propane pentaerythritol triacrylate, third oxidation neopentylglycol diacrylate, ethoxyquin 1,6 hexanediol diacrylate and
It is one or more in three (2- acrylyl oxy-ethyls) isocyanuric acid esters.
Using specific polyfunctionality oligomer and/or polyfunctional monomer, during polymerizing curable, crosslinking is improved
Degree increases bonding force, to improve the peeling resistance before the UV processing of UV visbreaking compositions；And the combination of UV visbreakings can be reduced
The small molecule of object remains.
In a kind of preferred embodiment of the present invention, the crosslinking agent includes isocyanates crosslinking agent, amine friendship
Join agent, one or more in aziridines crosslinking agent, preferably isocyanates crosslinking agent.
In a kind of preferred embodiment of the present invention, the isocyanates crosslinking agent includes two isocyanide of isophorone
Acid esters, hexamethylene diisocyanate, dicyclohexyl methyl hydride diisocyanate, benzene dimethylene diisocyanate and durol
It is one or more in dimethylene diisocyanate.It is furthermore preferred that the crosslinking agent is hexamethylene diisocyanate, preferably
For N3390 (Beyer Co., Ltd) crosslinking agent.The amine cross-linking agent includes diethylenetriamines, trien and six methines
It is one or more in tetramine.
Using specific crosslinking agent, the crosslinking curing between each raw material is peomoted, fully improves gained UV visbreakings combination
The bonding force of object, peeling resistance.
In a kind of preferred embodiment of the present invention, the photoinitiator include 2- isopropyl thioxanthones (ITX),
1- hydroxycyclohexyl phenyl ketones (184), 2- hydroxy-methyls phenyl third, benzoin dimethylether (651), benzophenone (BP), 2-
Methyl-1-(4- methyl mercaptos phenyl)-2- morpholinyl-1- acetone (907), 2,4,6- (trimethylbenzoyl)-diphenyl oxidation
It is one or more in phosphine (TPO), alkane -1- ketone (1173), DR-575, preferably 2,4,6- (trimethylbenzoyl)-hexichol
Base phosphine oxide (TPO).
In a kind of preferred embodiment of the present invention, the solvent includes acetone, cyclohexanone, ethyl acetate, acetic acid
Butyl ester, butanone, methanol, ethyl alcohol, propyl alcohol, isopropanol, isobutanol, n-butanol, methylisobutylketone, isophorone, toluene, diformazan
It is one or more in benzene, propylene glycol monomethyl ether, dipropylene glycol methyl ether, preferably butanone.
Fig. 1 is a kind of UV visbreaking membrane structure diagrams of specific implementation mode of the present invention, and the UV visbreakings film includes successively
Substrate layer 1, UV anti-adhesive layers 2 and the release film layer 3 of fitting.Wherein, the UV anti-adhesive layers are to be coated on base by UV visbreaking compositions
Material layer surface, drying curing obtain.
In a kind of preferred embodiment of the present invention, the base material is PET, and the thickness of the substrate layer is 50-150
μm, preferably 75-125 μm, more preferably 100 μm.
In a kind of preferred embodiment of the present invention, the thickness of the UV anti-adhesive layers is 10-30 μm, preferably 15-
25 μm, more preferably 20 μm.
In a kind of preferred embodiment of the present invention, the release film layer is preferably PET release film layers, preferred thick
Degree is 20-50 μm, preferred off-type force ranging from 10-100gf.
Embodiment 1
UV visbreaking compositions described in the present embodiment, raw material composition are as follows：
40g acrylic pressure sensitive gum resins (production firm：Shanghai Toyo Ink Manufacturing Co., Ltd, model：
STS0119OP), 20g polyfunctionalities oligomer (production firm：Chemical drug chemical industry (Wuxi) Co., Ltd, model：UX-8620W)、
1g crosslinking agents (production firm：Bayer A.G, model：N3390), 1g azobisisoheptonitrile, 5g 2,4,6- (trimethylbenzenes
Formoxyl)-diphenyl phosphine oxide (TPO), 33g butanone.
Wherein, the average molecular weight of the STS0119OP is 600,000, solid content 25%, viscosity 10000cps.It is described
UX-8620W is aliphatic urethane acrylate oligomer.
Embodiment 2
UV visbreaking compositions described in the present embodiment, raw material composition are as follows：
40g acrylic pressure sensitive gum resins (production firm：Shanghai Toyo Ink Manufacturing Co., Ltd, model：
STS0119OP), 20g polyfunctionalities oligomer (production firm：Chemical drug chemical industry (Wuxi) Co., Ltd, model：UX-8620W)、
1g crosslinking agents (production firm：Bayer A.G, model：N3390), 1.5g azobisisoheptonitrile, 5g 2,4,6- (trimethyls
Benzoyl)-diphenyl phosphine oxide (TPO), 32.5g butanone.
Embodiment 3
UV visbreaking compositions described in the present embodiment, raw material composition are as follows：
40g acrylic pressure sensitive gum resins (production firm：Shanghai Toyo Ink Manufacturing Co., Ltd, model：
STS0119OP), 20g polyfunctionalities oligomer (production firm：Chemical drug chemical industry (Wuxi) Co., Ltd, model：UX-8620W)、
1g crosslinking agents (production firm：Bayer A.G, model：N3390), 2g azobisisoheptonitrile, 5g 2,4,6- (trimethylbenzenes
Formoxyl)-diphenyl phosphine oxide (TPO), 32g butanone.
Embodiment 4
UV visbreaking compositions described in the present embodiment, raw material composition are as follows：
40g acrylic pressure sensitive gum resins (production firm：Shanghai Toyo Ink Manufacturing Co., Ltd, model：
STS0119OP), 20g polyfunctionalities oligomer (production firm：Chemical drug chemical industry (Wuxi) Co., Ltd, model：UX-8620W)、
1g crosslinking agents (production firm：Bayer A.G, model：N3390), 2.5g azobisisoheptonitrile, 5g 2,4,6- (trimethyls
Benzoyl)-diphenyl phosphine oxide (TPO), 31.5g butanone.
Embodiment 5
UV visbreaking compositions described in the present embodiment, raw material composition are as follows：
40g acrylic pressure sensitive gum resins (production firm：Shanghai Toyo Ink Manufacturing Co., Ltd, model：
STS0119OP), 20g polyfunctionalities oligomer (production firm：Chemical drug chemical industry (Wuxi) Co., Ltd, model：UX-8620W)、
1g crosslinking agents (production firm：Bayer A.G, model：N3390), 2,4,6- (trimethyls of 0.2g azodiisobutyronitriles, 3g
Benzoyl)-diphenyl phosphine oxide (TPO), 35.8g butanone.
Embodiment 6
UV visbreaking compositions described in the present embodiment, raw material composition are as follows：
50g acrylic pressure sensitive gum resins (production firm：Shanghai Toyo Ink Manufacturing Co., Ltd, model：
STS0119OP), 5g polyfunctionalities oligomer (production firm：Chemical drug chemical industry (Wuxi) Co., Ltd, model：UX-8620W)、
0.3g crosslinking agents (production firm：Bayer A.G, model：N3390), the 2- isopropyl sulphur of 5g dilauroyl peroxides, 0.5g
Miscellaneous anthrone (ITX), 39.2g isopropanol.
Embodiment 7
UV visbreaking compositions described in the present embodiment, raw material composition are as follows：
20g acrylic pressure sensitive gum resins (production firm：Shanghai Toyo Ink Manufacturing Co., Ltd, model：
STS0119OP), 30g pentaerythritol tetraacrylates, 2g crosslinking agents (production firm：Bayer A.G, model：N3390)、
The toluene of 1g tert-butyl hydroperoxide, the 1- hydroxycyclohexyl phenyl ketones (184) of 5g, 42g.
Embodiment 8
UV visbreaking compositions described in the present embodiment, raw material composition are as follows：
20g acrylic pressure sensitive gum resins (production firm：Shanghai Toyo Ink Manufacturing Co., Ltd, model：
STS0119OP), 15g polyfunctionalities oligomer (production firm：Chemical drug chemical industry (Wuxi) Co., Ltd, model：UX-8620W)、
1g crosslinking agents (production firm：Bayer A.G, model：N3390), 3g azobisisoheptonitrile, 1g 2- hydroxy-methyl phenyl
The third, the propylene glycol monomethyl ether of 60g.
Embodiment 9
The preparation method of UV visbreaking compositions described in embodiment 1-8, includes the following steps：
Each component is put in proportion into reaction kettle, 1-5h is stirred, preferably stirs 2h to get to the UV visbreakings group
Close object.
The present embodiment additionally provides a kind of UV visbreakings that the UV visbreaking compositions using described in embodiment 1-8 are prepared
Film, the UV visbreakings film, including the substrate layer, UV anti-adhesive layers and the release film layer that are bonded successively, the UV anti-adhesive layers are by described
UV visbreaking compositions are coated on the formation of base material layer surface, and the release film layer fits in UV anti-adhesive layers；Wherein, the UV visbreakings
Layer is to be coated on base material layer surface by the UV visbreakings composition, and drying curing obtains.The base material is PET, thickness 50-
150 μm, preferably 100 μm.The thickness of the UV anti-adhesive layers is 10-30 μm, preferably 20 μm.
Specifically, the preparation method of the UV visbreakings film includes the following steps：
The UV visbreaking compositions that embodiment 1-8 is obtained are respectively coated to the PET film (production firm in 100 μ m-thicks：East is beautiful
Company, model：PY-2 on), it is placed in preliminary drying 2min in 100 DEG C of baking ovens, fitting release film is put into 60 on UV visbreaking compositions surface
It is cured for 24 hours in DEG C baking oven, obtains the UV visbreakings film.Wherein, the coating thickness of UV visbreaking compositions is adjusted according to actual demand,
In the present embodiment, thickness is 20 μm after keeping UV visbreaking compositions dry.
Comparative example 1
A kind of UV visbreakings film is prepared with reference to the preparation method of the embodiment of the present invention 9, is combined using the UV visbreakings of embodiment 1
Object, difference lies in do not add thermal initiator in UV visbreaking compositions.
Experimental example 1
For the performance of the UV visbreaking compositions of each embodiment of comparative illustration, method described in embodiment 9 will be used with reality
Apply UV visbreakings film that the UV visbreaking compositions described in a 1-8 are prepared and comparative example 1 (respectively number be 1,2,3,4,5,6,
7, it 8 and 9) is tested for the property, each UV visbreakings film is stored 1 month, 2 months, 3 months, 4 months, 5 months and 6 months, test
(UV irradiation intensities are 230mW/cm for its UV pre-irradiations peeling force and UV irradiations2, irradiation time is that 5-10s (is when test
Whether there are residue glue, test result to be shown in Table 1 after 8s)).
The performance test results for the UV visbreaking films that 1 difference UV visbreaking compositions of table are prepared
As seen from the above table, UV visbreakings composition of the invention has excellent bonding force in UV pre-irradiations, after UV irradiations
Bonding force, which declines to a great extent, to be easily peeled off, and residue glue is not stayed after long-time storage.That thermal initiator is not added in comparative example 1,
Peeling force is quickly increased with the extension of storage time, and storage starts residue glue phenomenon occur after three months, the main reason is that small
Molecular migration causes peeling force to increase the reduction with cohesive force and causes residue glue phenomenon to film surface.With in the present embodiment
The increase of thermal initiator dosage, storage stability is higher and higher, but when dosage is excessive, peeling force rapid decrease, the present invention's
In amount ranges, storage stability can be improved while ensureing peeling force.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that：Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement；And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of UV visbreakings composition, which is characterized in that be mainly made of the following raw material by weight percentage：
Acrylate pressure-sensitive adhesive resin 20%-50%, polyfunctionality oligomer and/or polyfunctional monomer 1%-30%, crosslinking
Agent 0.3%-2%, thermal initiator 0.1%-5%, photoinitiator 0.5%-5% and solvent 25%-60%.
2. UV visbreakings composition according to claim 1, which is characterized in that the thermal initiator is free radical thermal initiation
Agent；
Preferably, the free radical thermal initiator includes that peroxide initiator, azo compound thermal initiator, redox heat are drawn
It sends out one or more in agent；
Preferably, the free radical thermal initiator includes azodiisobutyronitrile (AI BN), azobisisoheptonitrile (ABVN), peroxide
Change one kind in lauroyl, dibenzoyl peroxide, isopropyl benzene hydroperoxide, cyclohexanone peroxide, tert-butyl hydroperoxide etc.
Or it is a variety of.
3. UV visbreakings composition according to claim 1 or 2, which is characterized in that the acrylate pressure-sensitive adhesive resin is
Solvent-type acrylic ester pressure-sensitive adhesive；
Preferably, the molecular weight of the acrylate pressure-sensitive adhesive resin is 100,000-200 ten thousand；
Preferably, the solid content of the solvent-type acrylic ester pressure-sensitive adhesive is 25%-60%, viscosity 300cps-
20000cps。
4. UV visbreakings composition according to claim 1 or 2, which is characterized in that the polyfunctionality oligomer includes fat
One or both of fat race urethane acrylate oligomer and epoxy acrylate oligomer；
Preferably, the polyfunctional monomer includes pentaerythritol tetraacrylate, double pentaerythritol C5 methacrylate, two seasons penta
Six acrylate of tetrol, trimethylolpropane trimethacrylate, dipentaerythritol hexaacrylate, trimethylolpropane tris propylene
Acid esters, ethoxyquin trimethylolpropane trimethacrylate, trimethylol-propane trimethacrylate, methacrylic acid -2- hydroxyls
Base ethyl ester, acrylamide, dimethacrylate -1,6-HD ester, diacrylate -1,6-HD ester, diacrylate second two
Alcohol ester, diacrylate triethyleneglycol ester, diacrylate tripropylene glycol ester, diacrylate are to neopentyl glycol ester, trimethylolpropane tris
Acrylate, trihydroxy methyl pentane trimethyl acrylic ester, trimethylolpropane pentaerythritol triacrylate, the third oxidation new penta
One in omega-diol diacrylate, ethoxyquin 1,6 hexanediol diacrylate and three (2- acrylyl oxy-ethyls) isocyanuric acid esters
Kind is a variety of.
5. UV visbreakings composition according to claim 1 or 2, which is characterized in that the crosslinking agent includes isocyanates
It is one or more in crosslinking agent, amine cross-linking agent, aziridines crosslinking agent；
Preferably, the crosslinking agent is isocyanates crosslinking agent；
Preferably, the isocyanates crosslinking agent includes isophorone diisocyanate, hexamethylene diisocyanate, two rings
One kind in hexyl methane diisocyanate, benzene dimethylene diisocyanate and tetramethylxylylene diisocyanate or
It is a variety of；
It is furthermore preferred that the crosslinking agent is hexamethylene diisocyanate.
6. UV visbreakings composition according to claim 1 or 2, which is characterized in that the photoinitiator includes 2- isopropyls
Thioxanthone, 1- hydroxycyclohexyl phenyl ketones, 2- hydroxy-methyls phenyl third, benzoin dimethylether, benzophenone, 2- methyl-
1- (4- methyl mercaptos phenyl) -2- morpholinyl -1- acetone, 2,4,6- (trimethylbenzoyl)-diphenyl phosphine oxide, alkane -1- ketone,
It is one or more in DR-575；
Preferably, the photoinitiator is 2,4,6- (trimethylbenzoyl)-diphenyl phosphine oxides.
7. UV visbreakings composition according to claim 1 or 2, which is characterized in that the solvent include acetone, cyclohexanone,
Ethyl acetate, butyl acetate, butanone, methanol, ethyl alcohol, propyl alcohol, isopropanol, isobutanol, n-butanol, methylisobutylketone, different Fo Er
It is one or more in ketone, toluene, dimethylbenzene, propylene glycol monomethyl ether, dipropylene glycol methyl ether；
Preferably, the solvent is butanone.
8. a kind of UV visbreakings film, which is characterized in that including substrate layer, UV anti-adhesive layers and the release film layer being bonded successively；
Wherein, the UV anti-adhesive layers are to be coated on base material layer surface by any one of the claim 1-7 UV visbreakings compositions, are dried
What dry curing obtained.
9. UV visbreakings film according to claim 8, which is characterized in that the base material is PET；
Preferably, the thickness of the substrate layer is 50-150 μm；
Preferably, the thickness of the UV anti-adhesive layers is 10-30 μm.
10. the preparation method of the UV visbreaking films described in claim 8 or 9, which is characterized in that include the following steps：
UV visbreaking compositions are coated on base material layer surface, release film layer is bonded on UV visbreaking compositions after preliminary drying, cures, obtains
To the UV visbreakings film；
Preferably, 1-5mi n are dried under the conditions of the preliminary drying is included in 100 ± 10 DEG C；
It is furthermore preferred that the preliminary drying is to dry 2mi n under the conditions of 100 DEG C；
Preferably, the cooking conditions are to cure 20-30h under the conditions of 60 ± 10 DEG C；
It is furthermore preferred that the cooking conditions are to be cured for 24 hours at 60 DEG C.
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Address after: 215311 Dongping Road 399, Bacheng Town, Kunshan City, Suzhou City, Jiangsu Province Applicant after: Suzhou Chengbang Dayi Material Technology Co., Ltd. Address before: 215000 Dongping Road 399, Bacheng Industrial Zone, Suzhou City, Jiangsu Province Applicant before: Suzhou City-State Dali Material Technology Co., Ltd. |
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Application publication date: 20180713 |