CN107353854A - A kind of OCA optical cements and OCA optical adhesive films - Google Patents
A kind of OCA optical cements and OCA optical adhesive films Download PDFInfo
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- CN107353854A CN107353854A CN201710575394.7A CN201710575394A CN107353854A CN 107353854 A CN107353854 A CN 107353854A CN 201710575394 A CN201710575394 A CN 201710575394A CN 107353854 A CN107353854 A CN 107353854A
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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
- C09J133/04—Homopolymers or copolymers of esters
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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
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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
- C09J7/00—Adhesives in the form of films or foils
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C09J2433/00—Presence of (meth)acrylic polymer
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- Adhesives Or Adhesive Processes (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention belongs to optical cement field, more particularly to a kind of OCA optical cements and OCA optical adhesive films.OCA optical cements provided by the invention in terms of parts by weight, including：10~40 parts of saturation polyacrylate containing crosslinkable groups；20~40 parts of oligomer containing unsaturated bond；20~40 parts of diluent；0.5~5 part of light trigger；0.1~2 part of crosslinking agent.The present invention obtains the OCA optical cements of excellent performance, OCA optical cements coating wetability is excellent, and it is not in shrinkage cavity to be coated on base material by the way that the constituent of optical cement is in optimized selection；The OCA optical adhesive films being prepared by the optical cement have higher viscosity, and are bonded on display material and are not easy cull, and glued membrane has preferable fissility.Present invention also offers a kind of OCA optical adhesive films, the OCA optical adhesive films by above-mentioned OCA optical cements it is coated and solidification after formed, there is higher sticky and preferable fissility.
Description
Technical field
The invention belongs to optical cement field, more particularly to a kind of OCA optical cements and OCA optical adhesive films.
Background technology
OCA (Optical Clear Adhesive) optical adhesive film is without the two-sided fitting of base-material made of OCA optical cements
Adhesive tape, have the characteristics that water white transparency, light transmission rate are high, adhesive strength is high.OCA optical adhesive films can be applied to according to thickness difference
Different fields, it is mainly used in the cementing of transparent optical element in Electronic Paper, projection screen, display, camera lens, touch-screen.
Development is told with electronic product industry in recent years, the market demand of OCA optical cements rises year by year, has wide
Wealthy development prospect.But existing OCA optical cements in the prevalence of wetability it is poor the problem of, so as to cause to be coated on base
Easily there is shrinkage cavity when OCA glued membranes are prepared on material, reduce the yields of OCA glued membranes.In addition, the OCA that existing OCA optical cements are formed
Also there is the problem of viscosity and poor fissility for glue optical film, it is difficult to meets the requirement of high-precision end electronic product.
The content of the invention
In view of this, it is provided by the invention it is an object of the invention to provide a kind of OCA optical cements and OCA optical adhesive films
OCA optical cements coating wetability is excellent, and the glued membrane prepared by the OCA optical cements has higher viscosity and preferably peeled off
Property.
The invention provides a kind of OCA optical cements, in terms of parts by weight, including following components：
Crosslinkable groups in the saturation polyacrylate containing crosslinkable groups are included in amino, hydroxyl and carboxyl
It is one or more；
The oligomer containing unsaturated bond includes urethane acrylate, polyisoprene, polyethylene, acroleic acid esterification
One or more in polyacrylic acid, epoxy acrylate and polybutadiene acrylic acid ester；
The diluent includes butyl acrylate, hydroxyethyl methacrylate, isobornyl acrylate, isooctyl acrylate
Ester, tetrahydrofurfuryl acrylic acid, hexylene glycol double methyl methacrylate, double contracting propane diols double methacrylates, ethoxylated bisphenol A double third
Olefin(e) acid ester, polyethyleneglycol diacrylate, neopentyl glycol ethoxy-c epoxide double methacrylate, trimethylolpropane tris (methyl)
Acrylate, the amylalcohol triacrylate of season four, three (2- ethoxys) isocyanurate triacrylates, the amylalcohol tetrapropylene acid of season four
One or more in ester, the acrylate of dipentaerythrite five, triethyleneglycol divinylether and butyl vinyl ether.
Preferably, the number-average molecular weight of the saturation polyacrylate containing crosslinkable groups is 8000~12000.
Preferably, the number-average molecular weight of the oligomer containing unsaturated bond is 1000~5000.
Preferably, the light trigger include 2,2- diethoxy acetophenones, acetophenone, propiophenone, benzophenone, fluorenes,
Benzaldehyde, anthraquinone, carbazole, 3- methyl acetophenones, 4- methyl acetophenones, 4- methoxyacetophenones, to diacetyl benzene, 3-
Methoxy benzophenone, 2,4,6- tri-methyl benzophenones, polymerization (2- hydroxy-2-methyls -1- (4- (1- methyl second
Alkenyl) phenyl) acetone), 4- allyl benzenes ethyl ketone, camphorquinone, 2,4,6- trimethyl benzoyl diphenyl bases phosphine oxide, 4- first
The chloro- 4 '-benzyl benzophenone of base benzophenone, 4-, 2- hydroxy-2-methyl -1- phenyl -1- acetone, benzoyl,
Benzoyl methyl ether, benzoin butyl ether, double (4- dimethylaminophenyls) ketone, benzyl methoxyl group ketal, o-toluic acid
Ester, benzil dimethyl ketal, methyl benzoylformate, double (trichloromethyl) -6- styryl s- triazines, 2- (naphthalene -1- bases) -
Double (the trichloromethyl)-s- triazines of 4,6-, double (the trichloromethyl)-s- triazines of 2- (4- methoxynaphthalene -1- bases) -4,6-, 2-4- trichlorines
One or more in methyl (piperonyl) -6- triazines and 2-4- trichloromethyls (4 '-methoxyl-styrene) -6- triazines.
Preferably, the crosslinking agent is included in polynary amine crosslinker, isocyanate crosslinking and aziridines crosslinking agent
It is one or more.
Preferably, in addition to light stabilizer and antioxidant.
Preferably, the light stabilizer includes 4,4 '-butylidene double (the 6- tert-butyl group -3- methylphenols), poly- (dipropyls two
Alcohol) phenyl phosphites, 2- ethylhexyls diphenylphosphite, 4,6- double (octylsulfo methyl)-O- cresols, 1,3,5- tri-
Methyl -2,4,6- three (3,5- di-tert-butyl-4-hydroxyl benzyls) benzene, octadecyl -3- (3,5- di-tert-butyl-hydroxy phenyls)
Propionic ester, triethylene glycol-bis- (3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester, 2,2- di-2-ethylhexylphosphine oxides (4- methyl -6- (1-
Methylcyclohexyl)-phenol), diphenylisodecyl base ester, the isodecyl base ester of phosphorous acid three, diphenylethyllene pentaerythrite two
Phosphite ester, double (2,4- di-tert-butyl-phenyls) pentaerythritol diphosphites, double (4,6- DI-tert-butylphenol compounds), hexa-methylene
Double [3- (3,5- di-tert-butyl-hydroxy phenyls) propionic esters], three (2,4- di-tert-butyl-phenyls) phosphite esters, it is double (1,2,2,
6,6- pentamethyl -4- piperidyls) sebacate, (2,2,6,6- tetramethyl -4- piperidyls) sebacate and double-(1- octyloxies -
2,2,6,6- tetramethyl -4- piperidyls) one or more in sebacate；
The antioxidant includes Hexaethyl Asia phosphoric triamide, dialkyl phosphite, tri iso octyl phosphorite, thio
One or more in phosphoryl disulfide, 1,2- diphenylisobenzofurans and triphenyl phosphorus.
The invention provides a kind of OCA optical adhesive films, it is prepared in accordance with the following methods：
Optical cement described in any one of claim 1~7 is coated and solidified successively, obtains OCA optical adhesive films.
Preferably, the step of solidification specifically includes：Ultra-violet curing is first carried out, then carries out heat cure.
Preferably, the UV energy of the ultra-violet curing is 1500~3000mJ/cm2；The temperature of the heat cure is
90~200 DEG C, the time of the heat cure is 1~10min.
Compared with prior art, the invention provides a kind of OCA optical cements and OCA optical adhesive films.OCA provided by the invention
Optical cement is in terms of parts by weight, including following components：10~40 parts of saturation polyacrylate containing crosslinkable groups；Containing unsaturation
20~40 parts of the oligomer of key；20~40 parts of diluent；0.5~5 part of light trigger；0.1~2 part of crosslinking agent；It is described to contain and hand over
Crosslinkable groups in the saturation polyacrylate of symbasis group include the one or more in amino, hydroxyl and carboxyl；It is described to contain
The oligomer of unsaturated bond includes urethane acrylate, polyisoprene, polyethylene, acroleic acid esterification polyacrylic acid, epoxy
One or more in acrylate and polybutadiene acrylic acid ester；The diluent includes butyl acrylate, methacrylic acid
It is hydroxyl ethyl ester, isobornyl acrylate, isooctyl acrylate, tetrahydrofurfuryl acrylic acid, hexylene glycol double methyl methacrylate, double
Contracting propane diols double methacrylate, ethoxylated bisphenol A double methacrylates, polyethyleneglycol diacrylate, neopentyl glycol ethoxy-c
Epoxide double methacrylate, trimethylolpropane tris (methyl) acrylate, the amylalcohol triacrylate of season four, three (2- ethoxys) are different
Cyanate triacrylate, the amylalcohol tetraacrylate of season four, the acrylate of dipentaerythrite five, triethyleneglycol divinylether
With the one or more in butyl vinyl ether.The present invention is carried out excellent by the constituent to optical cement and the content of each composition
Change selection, obtain the OCA optical cements of excellent performance, OCA optical cements coating wetability is excellent, and being coated on base material to go out
Existing shrinkage cavity；The OCA optical adhesive films being prepared by the optical cement have higher viscosity, and are not easy on fitting display material residual
Glue, glued membrane have preferable fissility.Present invention also offers a kind of OCA optical adhesive films, and the OCA optical adhesive films are by above-mentioned OCA
Optical cement it is coated and solidification after formed, there is higher sticky and preferable fissility.In optimization technique provided by the invention
In scheme, the OCA optical cements after coating are solidified by the way of ultra-violet curing and heat cure successively, further carried
The viscosity and fissility of solidified glue film are risen.Test result indicates that OCA optical cements provided by the invention are coated on mould release membrance not
Shrink, without shrinkage cavity, the peeling force ＞ 900gf of OCA optical adhesive films made of the optical cement, not cull after stripping.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
The invention provides a kind of OCA optical cements, in terms of parts by weight, including following components：
Crosslinkable groups in the saturation polyacrylate containing crosslinkable groups are included in amino, hydroxyl and carboxyl
It is one or more；
The oligomer containing unsaturated bond includes urethane acrylate, polyisoprene, polyethylene, acroleic acid esterification
One or more in polyacrylic acid, epoxy acrylate and polybutadiene acrylic acid ester；
The diluent includes butyl acrylate, hydroxyethyl methacrylate, isobornyl acrylate, isooctyl acrylate
Ester, tetrahydrofurfuryl acrylic acid, hexylene glycol double methyl methacrylate, double contracting propane diols double methacrylates, ethoxylated bisphenol A double third
Olefin(e) acid ester, polyethyleneglycol diacrylate, neopentyl glycol ethoxy-c epoxide double methacrylate, trimethylolpropane tris (methyl)
Acrylate, the amylalcohol triacrylate of season four, three (2- ethoxys) isocyanurate triacrylates, the amylalcohol tetrapropylene acid of season four
One or more in ester, the acrylate of dipentaerythrite five, triethyleneglycol divinylether and butyl vinyl ether.
OCA optical cements provided by the invention include the saturation polyacrylate containing crosslinkable groups, containing the low of unsaturated bond
Polymers, diluent, light trigger and crosslinking agent.Wherein, it is cross-linking in the saturation polyacrylate containing crosslinkable groups
Group includes the one or more in amino, hydroxyl and carboxyl.In the present invention, the content of amino is excellent in the polyacrylate
Elect 0~4.5wt% as, concretely 0,0.5wt%, 1wt%, 1.5wt%, 2wt%, 2.5wt%, 3wt%, 3.5wt%,
4wt% or 4.5wt%；The content of hydroxyl is preferably 0~7wt%, concretely 0,1wt%, 1.5wt%, 2wt%,
2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 5.5wt%, 6wt%, 6.5wt% or 7wt%；Carboxyl
Content is preferably 0~10wt%, concretely 0,1wt%, 2wt%, 3wt%, 3.8wt%, 4wt%, 5wt%, 6wt%,
7wt%, 8wt%, 9wt% or 10wt%.In one embodiment provided by the invention, the saturation containing crosslinkable groups is gathered
Acrylate is methacrylic acid, hydroxy-ethyl acrylate, Isooctyl acrylate monomer, vinylacetate, butyl acrylate and methyl-prop
The homopolymer or copolymer that one or more in acrylamide are polymerized.In the present invention, it is described full containing crosslinkable groups
Number-average molecular weight with polyacrylate is preferably 8000~12000, and more preferably 5000~15000, concretely 5000,
8000 or 12000.In one embodiment provided by the invention, the saturation polyacrylate containing crosslinkable groups includes number
The polyacrylate that the polyacrylate and number-average molecular weight that average molecular weight is 5000 are 8000, the number-average molecular weight are 5000
Polyacrylate and number-average molecular weight be 8000 polyacrylate mass ratio be preferably (5~10)：(20~30).At this
Invent in the one embodiment provided, the saturation polyacrylate containing crosslinkable groups can be made in accordance with the following methods
It is standby：First, by melamine, toluene and triethylamine hybrid reaction.Wherein, the quality of the melamine, toluene and triethylamine
Than being preferably 10：(60~90)：(0.5~1)；The temperature of the hybrid reaction is preferably 80~90 DEG C, concretely 85 DEG C；Institute
The time for stating hybrid reaction is preferably 3~7h, concretely 5h.After reaction terminates, obtained reaction product is purified.It
Afterwards by the reaction product of purifying and hydroxy-ethyl acrylate and toluenesulfonic acid hybrid reaction.Wherein, the reaction product of the purifying, third
The mass ratio of olefin(e) acid hydroxyl ethyl ester and toluenesulfonic acid is preferably 10：(140~150)：(0.5~1)；The temperature of the hybrid reaction is excellent
Elect 90~110 DEG C as, concretely 100 DEG C；The time of the hybrid reaction is preferably 3~5h, concretely 4h.Reaction terminates
Afterwards, obtained reaction product is blended in nitrogen atmosphere with toluene and azodiisobutyronitrile and reacted.Wherein, the reaction
The mass ratio of product, toluene and azodiisobutyronitrile is preferably 10：(5~6)：(0.1~0.2)；The temperature of the reaction is preferred
For 50~60 DEG C, concretely 55 DEG C；The temperature of the reaction is preferably 3~5h.After reaction terminates, add chain reaction and terminate
Agent, obtain the saturation polyacrylate containing crosslinkable groups.It is described containing cross-linking in another embodiment provided by the invention
The saturation polyacrylate of group can be prepared in accordance with the following methods：By methacrylic acid, vinyl acetate, acrylic acid fourth
Ester, 2-EHA, toluene and azodiisobutyronitrile, which are blended in nitrogen atmosphere, to be reacted.Wherein, the methyl
Acrylic acid, vinyl acetate, butyl acrylate, 2-EHA, the mass ratio of toluene and azodiisobutyronitrile are 10：(5
~6)：(10~12)：(20~25)：(5~5)：(0.1~0.2)；The temperature of the reaction is preferably 50~60 DEG C, specifically may be used
For 55 DEG C；The temperature of the reaction is preferably 3~5h, concretely 4h.After reaction terminates, chain cessationer is added, is obtained
Saturation polyacrylate containing crosslinkable groups.In the present invention, the saturation polyacrylic acid containing crosslinkable groups in OCA optical cements
The content of ester is 10~40 parts by weight, concretely 10 parts by weight, 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight,
35 parts by weight or 40 parts by weight.
In the present invention, the oligomer containing unsaturated bond includes urethane acrylate, polyisoprene, poly- second
One or more in alkene, acroleic acid esterification polyacrylic acid, epoxy acrylate and polybutadiene acrylic acid ester.Carried in the present invention
In one embodiment of confession, the oligomer includes urethane acrylate, polybutadiene acrylic acid ester and epoxy acrylate
In two or three.In one embodiment provided by the invention, the oligomer includes urethane acrylate and epoxy
Acrylate, the mass ratio of the urethane acrylate and epoxy acrylate is preferably (30~40)：(2~5).In this hair
In one embodiment of bright offer, the oligomer includes urethane acrylate and polybutadiene acrylic acid ester, the poly- ammonia
The mass ratio of ester acrylate and polybutadiene acrylic acid ester is preferably (15~20)：(25~30).Provided by the invention one
In individual embodiment, the oligomer includes polybutadiene acrylic acid ester and epoxy acrylate, the polybutadiene acrylic acid ester
Mass ratio with epoxy acrylate is preferably (25~30)：(15~20).In the present invention, it is described containing the oligomeric of unsaturated bond
The number-average molecular weight of thing is preferably 1000~5000.In the present invention, the trade mark of the Polyurethane acrylate is preferably Hua Kai
B-26980；The trade mark of the polybutadiene acrylic acid ester is preferably the UV-3026 of chemical industry on well；The board of the epoxy acrylate
Number be preferably Guangdong add one chemistry HS9104.In the present invention, the content of the oligomer containing unsaturated bond is in OCA optical cements
20~40 parts by weight, concretely 20 parts by weight, 25 parts by weight, 30 parts by weight, 32 parts by weight, 35 parts by weight or 40 parts by weight.
In the present invention, the diluent include butyl acrylate, hydroxyethyl methacrylate, isobornyl acrylate,
Isooctyl acrylate, tetrahydrofurfuryl acrylic acid, hexylene glycol double methyl methacrylate, double contracting propane diols double methacrylates, second
Aoxidize bisphenol-A double methacrylate, polyethyleneglycol diacrylate, neopentyl glycol ethoxy-c epoxide double methacrylate, three hydroxyl first
Base propane three (methyl) acrylate, the amylalcohol triacrylate of season four, three (2- ethoxys) isocyanurate triacrylates, Ji Si
One in amylalcohol tetraacrylate, the acrylate of dipentaerythrite five, triethyleneglycol divinylether and butyl vinyl ether
Kind is a variety of.In the present invention, the trade mark of the neopentyl glycol ethoxy-c epoxide double methacrylate is preferably permanent positive chemical industry
PO2-NPGDA.In the present invention, the content of diluent is 20~40 parts by weight in OCA optical cements, concretely 20 parts by weight,
25 parts by weight, 30 parts by weight, 35 parts by weight, 38 parts by weight or 40 parts by weight.
In the present invention, the light trigger include but is not limited to 2,2- diethoxy acetophenones, acetophenone, propiophenone,
Benzophenone, fluorenes, benzaldehyde, anthraquinone, carbazole, 3- methyl acetophenones, 4- methyl acetophenones, 4- methoxyacetophenones, to two
Acetylbenzene, 3- methoxy benzophenones, 2,4,6- tri-methyl benzophenones, polymerization (2- hydroxy-2-methyls -1-
(4- (1- methyl ethylenes) phenyl) acetone), 4- allyl benzenes ethyl ketone, camphorquinone, 2,4,6- trimethyl benzoyl diphenyls
The chloro- 4 '-benzyl benzophenone of base phosphine oxide, 4- methyl benzophenones, 4-, 2- hydroxy-2-methyl -1- phenyl -
1- acetone, benzoyl, benzoyl methyl ether, benzoin butyl ether, double (4- dimethylaminophenyls) ketone, the contracting of benzyl methoxyl group
Ketone, o-toluic acid ester, benzil dimethyl ketal, methyl benzoylformate, double (trichloromethyl) -6- styryls s- tri-
Double (the trichloromethyl)-s- triazines of piperazine, 2- (naphthalene -1- bases) -4,6-, 2- (4- methoxynaphthalene -1- bases) -4,6- double (trichloromethyls) -
In s- triazines, 2-4- trichloromethyls (piperonyl) -6- triazines and 2-4- trichloromethyls (4 '-methoxyl-styrene) -6- triazines
One or more.In one embodiment provided by the invention, the light trigger includes acetophenone and benzil dimethyl
Ketal, the mass ratio of the acetophenone and benzil dimethyl ketal is preferably (0.5~1)：(1.5~2).In the present invention,
The content of light trigger is 0.5~5 parts by weight in OCA optical cements, concretely 0.5 parts by weight, 1 parts by weight, 1.5 parts by weight, 2
Parts by weight, 2.5 parts by weight, 3 parts by weight, 3.5 parts by weight, 4 parts by weight, 4.5 parts by weight or 5 parts by weight.
In the present invention, the crosslinking agent includes polynary amine crosslinker, isocyanate crosslinking and aziridines crosslinking agent
In one or more.Wherein, the polynary amine crosslinker concretely triethylene tetramine；The isocyanate crosslinking is specific
It can be toluene di-isocyanate(TDI) (abbreviation TDI)；The aziridines crosslinking agent concretely aziridine.Provided by the invention one
In individual embodiment, the crosslinking agent includes polynary amine crosslinker and aziridines crosslinking agent, the polynary amine crosslinker and nitrogen third
The mass ratio of pyridine class crosslinking agent is preferably (0.1~0.2)：(0.25~0.3).In the present invention, crosslinking agent in OCA optical cements
Content is 0.1~2 parts by weight, concretely 0.3 parts by weight, 0.35 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 1 parts by weight,
1.5 parts by weight, 1.6 parts by weight, 1.8 parts by weight or 2 parts by weight.
In the present invention, light stabilizer and antioxidant are preferably also included in the OCA optical cements.Wherein, the light is steady
Determine agent include but is not limited to 4,4 '-butylidene double (the 6- tert-butyl group -3- methylphenols), poly- (DPG) phenyl phosphites,
Double (octylsulfo the methyl)-O- cresols of 2- ethylhexyls diphenylphosphite, 4,6-, 1,3,5- trimethyls -2,4,6- three (3,
5- di-tert-butyl-4-hydroxyl benzyls) benzene, octadecyl -3- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester, triethylene glycol-bis-
(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester, 2,2- di-2-ethylhexylphosphine oxides (4- methyl -6- (1- methylcyclohexyls)-benzene
Phenol), diphenylisodecyl base ester, the isodecyl base ester of phosphorous acid three, diphenylethyllene pentaerythritol diphosphites, it is double (2,
4- di-tert-butyl-phenyls) pentaerythritol diphosphites, double (4,6- DI-tert-butylphenol compounds), the hexamethylene bis [3- (uncles of 3,5- bis-
Butyl -4- hydroxy phenyls) propionic ester], three (2,4- di-tert-butyl-phenyls) phosphite esters, double (1,2,2,6,6- pentamethyl -4- piperazines
Piperidinyl) sebacate, (2,2,6,6- tetramethyl -4- piperidyls) sebacate and double-(1- octyloxy -2,2,6,6- tetramethyls -
4- piperidyls) one or more in sebacate.In one embodiment provided by the invention, the light stabilizer includes 2-
Two kinds or three in ethylhexyl diphenylphosphite, diphenylisodecyl base ester and double (4,6- DI-tert-butylphenol compounds)
Kind.In one embodiment provided by the invention, the light stabilizer includes diphenylisodecyl base ester and double (4,6- bis-
Tert-butyl phenol), the mass ratio of the diphenylisodecyl base ester and double (4,6- DI-tert-butylphenol compounds) is preferably (0.2
~0.5)：(1~2).In one embodiment provided by the invention, the light stabilizer includes 2- ethylhexyl diphenyl phosphorous
Acid esters and double (4,6- DI-tert-butylphenol compounds), the 2- ethylhexyls diphenylphosphite and pair (4,6- DI-tert-butylphenol compounds)
Mass ratio be preferably (3~5)：(0.5~1).In the present invention, in OCA optical cements the content of light stabilizer be preferably 0.1~
5 parts by weight, concretely 1 parts by weight, 1.2 parts by weight, 1.5 parts by weight, 2 parts by weight, 2.5 parts by weight, 3 parts by weight, 3.5 weight
Part or 4 parts by weight.
In the present invention, the antioxidant includes but is not limited to Hexaethyl Asia phosphoric triamide, dialkyl phosphite, three
One or more in iso-octyl phosphite ester, thiophosphoryl disulfide, 1,2- diphenylisobenzofurans and triphenyl phosphorus.
In one embodiment provided by the invention, the antioxidant includes dialkyl phosphite, thiophosphoryl disulfide and three
Two or three in phenyl phosphorus.In one embodiment provided by the invention, the antioxidant includes dialkyl phosphite
With thiophosphoryl disulfide, the mass ratio of dialkyl phosphite and the thiophosphoryl disulfide be preferably (0.6~
1)：(0.5~1).In one embodiment provided by the invention, the antioxidant includes dialkyl phosphite, thio phosphorus
Acyl group disulfide and triphenyl phosphorus, the mass ratio of the dialkyl phosphite, thiophosphoryl disulfide and triphenyl phosphorus are excellent
Elect as (0.5~1)：(0.1~0.5)：(0.8~1).In the present invention, the content of antioxidant is preferably in OCA optical cements
0.1~2 parts by weight, concretely 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.8 parts by weight, 1 weight
Part, 1.1 parts by weight, 1.2 parts by weight, 1.3 parts by weight, 1.4 parts by weight, 1.5 parts by weight or 2 parts by weight.
In the present invention, directly each component is mixed in proportion and can obtain OCA optical cements provided by the invention.
The present invention is in optimized selection by the content of the constituent to optical cement and each composition, obtains excellent performance
OCA optical cements, the OCA optical cements coating wetability it is excellent, it is not in shrinkage cavity to be coated on base material；Prepared by the optical cement
Obtained OCA optical adhesive films have higher viscosity, and are bonded on display material and are not easy cull, and glued membrane, which has, preferably to be peeled off
Property.Do not shunk, without shrinkage cavity test result indicates that OCA optical cements provided by the invention are coated on mould release membrance, by the optical cement system
Into OCA optical adhesive films peeling force ＞ 900gf, not cull after stripping.
A kind of OCA optical adhesive films provided by the invention, are prepared in accordance with the following methods：Light described in above-mentioned technical proposal
Learn glue to be coated and solidify successively, obtain OCA optical adhesive films.
OCA optical adhesive films provided by the invention are formed after being coated and solidified successively by the OCA optical cements, specific mistake
Journey includes：First the OCA optical cements are coated on base material, it solidified afterwards, OCA optical cements are formed on base material
Film.Wherein, the base material is preferably mould release membrance；The device that the coating uses is preferably scraper coating machine or slit coating
Machine.In the present invention, the step of solidification specifically includes：Ultra-violet curing is first carried out, then carries out heat cure.Wherein, the purple
The UV energy of outer solidification is preferably 1500~3000mJ/cm2, concretely 1500mJ/cm2、1800mJ/cm2、2000mJ/
cm2、2200mJ/cm2、2500mJ/cm2、2700mJ/cm2Or 3000mJ/cm2；The device of the ultra-violet curing preferably uses metal
Halogen lamp or mercury lamp；The temperature of the heat cure is preferably 90~200 DEG C, concretely 90 DEG C, 100 DEG C, 120 DEG C, 150 DEG C, 170
DEG C, 180 DEG C, 190 DEG C or 200 DEG C；The time of the heat cure is preferably 1~10min, concretely 1min, 3min, 5min,
7min, 8min or 10min；The device for carrying out the heat cure preferably uses baking box.
OCA optical adhesive films provided by the invention by the OCA optical cements are coated and solidification after formed, have higher viscous
Property and preferable fissility.In optimal technical scheme provided by the invention, successively by the way of ultra-violet curing and heat cure
The OCA optical cements after coating are solidified, further improve the viscosity and fissility of solidified glue film.Experimental result table
The peeling force ＞ 900gf of bright OCA optical adhesive films provided by the invention, not cull after stripping.
For the sake of becoming apparent from, it is described in detail below by following examples.
In the following embodiments and comparative example of the present invention, polyacrylate is the saturation polyacrylic acid containing crosslinkable groups
Ester, wherein, amino content 1.5%wt, hydroxy radical content 3%wt, carboxyl-content in the polyacrylate that number-average molecular weight is 5000
0%wt；Amino content 0%, hydroxy radical content 0%, carboxyl-content 3.8%wt in the polyacrylate that number-average molecular weight is 8000；
Amino content 0.5%wt, hydroxy radical content 1.5%wt, carboxyl-content 0%wt in the polyacrylate that number-average molecular weight is 12000.
The polyacrylate preparation method that number-average molecular weight is 5000 is as follows：10 parts by weight melamines, add 60 weight
Part formaldehyde, 1 parts by weight triethylamine, 85 DEG C of hybrid reactions 5 hours；After purification, every 10 parts by weight purification adds 140 parts by weight
Hydroxy-ethyl acrylate and 1 parts by weight p-methyl benzenesulfonic acid, 100 DEG C of hybrid reactions 4 hours；By 10 parts by weight previous step products, 5 are added
Parts by weight of toluene, 0.1 parts by weight azodiisobutyronitrile, 55 DEG C of inflated with nitrogen hybrid reaction 3 hours, it is eventually adding chain reaction termination
Agent, react 30 minutes.
The polyacrylate preparation method that number-average molecular weight is 8000 is as follows：By 10 weight parts of methacrylic acid, 5 parts by weight
Vinyl acetate, 10 parts by weight propylene acid butyl esters, 20 parts by weight of acrylic acid 2- ethylhexyls, 5 parts by weight of toluene, 0.1 parts by weight are even
Nitrogen bis-isobutyronitrile, 55 DEG C of inflated with nitrogen hybrid reaction 4 hours, chain cessationer is eventually adding, reacted 30 minutes.
The polyacrylate preparation method that number-average molecular weight is 12000 is as follows：10 parts by weight melamines, add 90 weight
Part formaldehyde, 1 parts by weight triethylamine, 85 DEG C of hybrid reactions 5 hours；After purification, every 10 parts by weight purification adds 140 parts by weight
Hydroxy-ethyl acrylate and 1 parts by weight p-methyl benzenesulfonic acid, 100 DEG C of hybrid reactions 4 hours；By 10 parts by weight previous step products, 5 are added
Parts by weight of toluene, 0.1 parts by weight azodiisobutyronitrile, 55 DEG C of inflated with nitrogen hybrid reaction 5 hours, it is eventually adding chain reaction termination
Agent, react 30 minutes.
In the following embodiments and comparative example of the present invention, Polyurethane acrylate is Hua Kai B-26980；Polybutadiene allyl
Chemical industry UV-3026 on olefin(e) acid ester well；Epoxy acrylate Guangdong adds a chemical HS9104；Neopentyl glycol ethoxy-c epoxide double third
The permanent positive chemical industry PO2-NPGDA of olefin(e) acid ester.
Embodiment 1~4
1) composition design
The constituent of OCA optical cements provided in an embodiment of the present invention refers to following table：
The constituent of the embodiment OCA optical cements of table 1
2) prepared by glued membrane
According to the ratio of table 1, each component is well mixed, the OCA optical cements that 4 embodiments provide is respectively obtained, orders successively
Entitled OCA optical cements 1, OCA optical cements 2, OCA optical cements 3, OCA optical cements 4.
The OCA optical cements are coated on mould release membrance respectively using slit type coater, first carried out with mercury lamp ultraviolet
Irradiation solidification, UV energy is in 2000mJ/cm2, then 180 DEG C of temperature baking 5min in an oven, thickness is obtained as 200 μm
OCA optical adhesive films, be named as OCA optical adhesive films 1, OCA optical adhesive films 2, OCA optical adhesive films 3, OCA optical adhesive films 4 successively.
Embodiment 5
With reference to the preparation method of embodiment 3, it is differed only in is adjusted to 2000mJ/cm by UV energy2, by baking box
Temperature is adjusted to 120 DEG C, and baking time is adjusted to 10min, and the OCA optical adhesive films that thickness is 200 μm are prepared, are named as
OCA optical adhesive films 5.
Embodiment 6
With reference to the preparation method of embodiment 3, it is differed only in is adjusted to 3000mJ/cm by UV energy2, by baking box
Temperature is adjusted to 90 DEG C, and baking time is adjusted to 10min, and the OCA optical adhesive films that thickness is 200 μm are prepared, are named as OCA
Optical adhesive film 6.
Comparative example 1~2
1) composition design
The constituent of OCA optical cements provided in an embodiment of the present invention refers to following table：
The constituent of the comparative example OCA optical cements of table 2
2) prepared by glued membrane
According to the ratio of table 2, each component is well mixed, the OCA optical cements that 2 comparative examples provide is respectively obtained, orders successively
Entitled OCA optical cements 7, OCA optical cements 8.
The OCA optical cements are coated on mould release membrance respectively using slit type coater, first carried out with mercury lamp ultraviolet
Irradiation solidification, UV energy is in 3000mJ/cm2, the OCA optical adhesive films that thickness is 200 μm are obtained, are named as OCA light successively
Learn glued membrane 7, OCA optical adhesive films 8.
Embodiment 7
Performance test
(1) glued membrane is transferred in PET film, carries out 180 ° of peel strength measure of pressure-sensitive tape, adhesive tape peeling force is surveyed
Test-object is accurate and method is according to GB/T 7122-1996
(2) glued membrane is transferred in PET film, fits in steel plate or glass, the naturally reciprocal pressing of 2kg rollers once, is stood
20 minutes, whether tearing up glued membrane gently, seeing also had glue to remain on jointing material；
(3) glued membrane that two sides is covered with to mould release membrance is placed under the conditions of 80 DEG C and toasted, and the time is 200 hours.By
(1) peeling force is tested, observes the viscosity of glued membrane after aging.
(4) tested according to the test method standard GB/T 30776-2014 of adhesive tape tensile strength and elongation at break.
(5) wetability of coating, by glue coating and the mould release membrance of 20-30gf off-type forces, 10min is stood, observation is uncured
Glued membrane area whether can shrink or produce circular shrinkage cavity.
Test result is as shown in Table 3 and Table 4：
The embodiment glue film performance test result of table 3
The comparative example glue film performance test result of table 4
| Test event | Comparative example 1 | Comparative example 2 |
| Peeling force (gf) | 570 | 630 |
| Aging peeling force (gf) | 150 | 180 |
| Whether cull | Cull | Cull |
| Elongation at break | 100% | 120% |
| Whether glue shrinks on mould release membrance | Shrinkage cavity, glue area reduce | Shrinkage cavity, glue area reduce |
By table 3 and table 4 as can be seen that glued membrane prepared by OCA of embodiment of the present invention optical cements has higher viscosity, and
It is not easy cull on fitting display material, glued membrane elongation height has preferable fissility.It is in addition, provided in an embodiment of the present invention
OCA optical cements also have preferable coating in mould release membrance.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of OCA optical cements, in terms of parts by weight, including following components：
Crosslinkable groups in the saturation polyacrylate containing crosslinkable groups include one kind in amino, hydroxyl and carboxyl
It is or a variety of；
The oligomer containing unsaturated bond includes urethane acrylate, polyisoprene, polyethylene, acroleic acid esterification poly- third
One or more in olefin(e) acid, epoxy acrylate and polybutadiene acrylic acid ester；
The diluent include butyl acrylate, hydroxyethyl methacrylate, isobornyl acrylate, isooctyl acrylate,
The double propylene of tetrahydrofurfuryl acrylic acid, hexylene glycol double methyl methacrylate, double contracting propane diols double methacrylates, ethoxylated bisphenol A
Acid esters, polyethyleneglycol diacrylate, neopentyl glycol ethoxy-c epoxide double methacrylate, trimethylolpropane tris (methyl) third
Olefin(e) acid ester, the amylalcohol triacrylate of season four, three (2- ethoxys) isocyanurate triacrylates, the amylalcohol tetraacrylate of season four,
One or more in the acrylate of dipentaerythrite five, triethyleneglycol divinylether and butyl vinyl ether.
2. optical cement according to claim 1, it is characterised in that the saturation polyacrylate containing crosslinkable groups
Number-average molecular weight is 8000~12000.
3. optical cement according to claim 1, it is characterised in that the number-average molecular weight of the oligomer containing unsaturated bond
For 1000~5000.
4. optical cement according to claim 1, it is characterised in that the light trigger includes 2,2- diethoxybenzene second
Ketone, acetophenone, propiophenone, benzophenone, fluorenes, benzaldehyde, anthraquinone, carbazole, 3- methyl acetophenones, 4- methyl acetophenones, 4-
Methoxyacetophenone, to diacetyl benzene, 3- methoxy benzophenones, 2,4,6- tri-methyl benzophenones, polymerization (2- hydroxyls
Base -2- methyl isophthalic acids-(4- (1- methyl ethylenes) phenyl) acetone), 4- allyl benzenes ethyl ketone, camphorquinone, 2,4,6- tri-
The chloro- 4 '-benzyl benzophenone of methyl benzoyl diphenyl phosphine oxide, 4- methyl benzophenones, 4-, 2- hydroxyls -2-
Methyl isophthalic acid-phenyl -1- acetone, benzoyl, benzoyl methyl ether, benzoin butyl ether, double (4- dimethylaminophenyls)
Ketone, benzyl methoxyl group ketal, o-toluic acid ester, benzil dimethyl ketal, methyl benzoylformate, double (three chloromethanes
Base) -6- styryl s- triazines, double (the trichloromethyl)-s- triazines of 2- (naphthalene -1- bases) -4,6-, 2- (4- methoxynaphthalene -1- bases) -
4,6- double (trichloromethyl)-s- triazines, 2-4- trichloromethyls (piperonyl) -6- triazines and 2-4- trichloromethyl (4 '-methoxybenzenes
Vinyl) one or more in -6- triazines.
5. optical cement according to claim 1, it is characterised in that the crosslinking agent includes polynary amine crosslinker, isocyanic acid
One or more in ester crosslinking agent and aziridines crosslinking agent.
6. optical cement according to claim 1, it is characterised in that also including light stabilizer and antioxidant.
7. optical cement according to claim 6, it is characterised in that the light stabilizer includes 4, double (uncles 6- of 4 '-butylidene
Butyl -3- methylphenols), poly- (DPG) phenyl phosphites, 2- ethylhexyls diphenylphosphite, 4,6- it is double (pungent
Base sulphomethyl)-O- cresols, 1,3,5- trimethyls -2,4,6- three (3,5- di-tert-butyl-4-hydroxyl benzyls) benzene, octadecyl -
3- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester, triethylene glycol-bis- (3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic acid
Ester, 2,2- di-2-ethylhexylphosphine oxides (4- methyl -6- (1- methylcyclohexyls)-phenol), diphenylisodecyl base ester, phosphorous acid three are different
It is decyl ester, diphenylethyllene pentaerythritol diphosphites, double (2,4- di-tert-butyl-phenyls) pentaerythritol diphosphites, double
(4,6- DI-tert-butylphenol compounds), hexamethylene bis [3- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester], the three (uncles of 2,4- bis-
Butyl phenyl) phosphite ester, double (1,2,2,6,6- pentamethyl -4- piperidyls) sebacates, (2,2,6,6- tetramethyl -4- piperazines
Piperidinyl) one or more in sebacate and double-(1- octyloxy -2,2,6,6- tetramethyl -4- piperidyls) sebacate；
The antioxidant includes Hexaethyl Asia phosphoric triamide, dialkyl phosphite, tri iso octyl phosphorite, thiophosphoryl
One or more in base disulfide, 1,2- diphenylisobenzofurans and triphenyl phosphorus.
8. a kind of OCA optical adhesive films, are prepared in accordance with the following methods：
Optical cement described in any one of claim 1~7 is coated and solidified successively, obtains OCA optical adhesive films.
9. OCA optical adhesive films according to claim 8, it is characterised in that specifically include the step of the solidification：First carry out
Ultra-violet curing, then carry out heat cure.
10. OCA optical adhesive films according to claim 9, it is characterised in that the UV energy of the ultra-violet curing is
1500~3000mJ/cm2；The temperature of the heat cure is 90~200 DEG C, and the time of the heat cure is 1~10min.
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