CN119471867B - OCA optical film and preparation method thereof - Google Patents
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- CN119471867B CN119471867B CN202411931509.8A CN202411931509A CN119471867B CN 119471867 B CN119471867 B CN 119471867B CN 202411931509 A CN202411931509 A CN 202411931509A CN 119471867 B CN119471867 B CN 119471867B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
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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
- C09J1/00—Adhesives based on inorganic constituents
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
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Abstract
本发明涉及光学膜技术领域，特别涉及一种OCA光学薄膜及其制备方法，包括五层结构，依次为含氟异形膜层、含硅粘合剂层、改性PET基体、含硅粘合剂层和含氟异形膜层，制备所述含硅粘合剂层的原料为含硅粘合剂。本发明的OCA光学薄膜耐老化黄变性能、耐高温性能、柔韧性优异，此外具有更好的透光率、透过率、阻燃性能和低折射率。The present invention relates to the field of optical film technology, and in particular to an OCA optical film and a preparation method thereof, comprising a five-layer structure, which is a fluorine-containing profiled film layer, a silicon-containing adhesive layer, a modified PET substrate, a silicon-containing adhesive layer and a fluorine-containing profiled film layer in sequence, and the raw material for preparing the silicon-containing adhesive layer is a silicon-containing adhesive. The OCA optical film of the present invention has excellent aging and yellowing resistance, high temperature resistance, and flexibility, and also has better light transmittance, transmittance, flame retardancy and low refractive index.
Description
Technical Field
The invention relates to the technical field of optical films, in particular to an OCA optical film and a preparation method thereof.
Background
Along with the continuous development of technology, large-scale electronic equipment such as smart phones, tablet computers and intelligent televisions are more and more, screens in such electronic products are one of the most important parts, most of screens are made of various layer structures such as display components, touch films, polaroids and cover plates, and the components are required to be bonded together, so that some adhesives are required, OCA adhesives are one of the more common adhesives used in the field of flexible screens, and meanwhile, the electronic products have wide application prospects in the fields of aerospace, transportation and the like.
The conventional OCA is widely used mainly in the form of acrylic acid system and polyurethane system, especially acrylic acid and urea system, which has the advantages of better transparency, easy involvement, low price and the like, but the conventional OCA adhesive has poor adhesion, so that the improvement is needed.
For example, CN116200140a discloses "an OCA adhesive, OCA layer, OCA film and application" which is prepared by using acrylate monomer a, acrylate monomer B, hydrophilic acrylate monomer, curing agent, tackifier, elastic resin, organic solvent and the like as main raw materials, and the OCA layer has better cohesiveness and creep recovery performance, and is not easy to crack, deform and the like.
And as CN107353854B discloses an OCA optical adhesive and an OCA optical adhesive film, which are prepared from saturated polyacrylate containing a crosslinkable group, an oligomer containing an unsaturated bond, a diluent, a photoinitiator and a crosslinking agent, wherein the optical film has higher viscosity and better stripping property.
However, in addition to the above problems, conventional OCAs have poor heat resistance, and the problem of yellowing of the film material is further caused by the poor heat resistance, which limits the application of OCAs, and the above-mentioned publication does not mention and solve the problem.
Therefore, development of an OCA optical film with excellent aging and yellowing resistance, high temperature resistance and flexibility, better light transmittance, better flame retardant property and lower refractive index is urgent.
Disclosure of Invention
The invention mainly aims to provide an OCA optical film and a preparation method thereof, wherein the OCA optical film has excellent ageing and yellowing resistance, high temperature resistance and flexibility, and further has better light transmittance, flame retardant property and low refractive index.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides an OCA optical film which comprises five layers of structures, wherein the five layers of structures sequentially comprise a fluorine-containing special-shaped film layer, a silicon-containing adhesive layer, a modified PET matrix, a silicon-containing adhesive layer and a fluorine-containing special-shaped film layer, and the silicon-containing adhesive layer is prepared from silicon-containing adhesives.
The traditional OCA binder mainly adopts an acrylic acid system and a polyurethane system, but the poor heat resistance of the binder of the system can further cause the yellowing problem of the film material, thereby limiting the application of the OCA.
According to the OCA optical film disclosed by the application, each layer is bonded by adopting the modified silicon-containing adhesive layer, and meanwhile, the modified PET matrix is compounded, so that the light transmittance of the OCA adhesive can be further improved, probably because the silicon-containing adhesive layer is higher in light transmittance, when the traditional PET is adopted, the light transmittance of the whole OCA film is reduced due to low PET light transmittance, and the modified PET matrix is higher in light transmittance, and can keep the excellent light transmittance of the OCA film after being compounded. In addition, the OCA film disclosed by the application has the advantages of ageing and yellowing resistance, high temperature resistance and excellent flexibility.
In some embodiments, the thickness of the silicon-containing adhesive layer is 100-3000 μm, and the thickness of the fluorine-containing special-shaped film layer is 1000-3000 μm.
In some embodiments, the thickness ratio of the silicon-containing adhesive layer to the modified PET substrate is 1 (0.1-10).
According to the application, the thickness ratio of the silicon-containing adhesive layer to the modified PET substrate is regulated, so that on one hand, the deterioration of the bonding effect caused by low bonding force can be prevented, and on the other hand, the reduction of the light transmittance of the OCA film caused by more reflection and scattering when light passes through the OCA film can be prevented.
In some embodiments, the silicon-containing adhesive comprises a modified inorganic silicon adhesive and an organic silicon adhesive in a mass ratio of 1 (0.8-1.5), wherein the modified inorganic silicon adhesive consists of a hollow core layer and a shell layer, and the outer layer of the shell layer is grafted with a structure shown in a formula I:
wherein R 1 is independently hydrogen, methyl, halogen, amino, epoxy, cyclohexene oxide, methylpropenyl, propenyl, hydroxy, siloxy, isocyanate, nitrile, nitro, phenyl, C1-C40 alkyl, C2-C40 vinyl, C1-C40 alkoxy, C3-C40 cycloalkyl, C3-C40 heterocycloalkyl, C6-C40 aryl or C3-C40 heteroaryl;
R 2 is independently hydrogen, methyl, halogen, amino, epoxy, cyclohexene oxide, methylpropenyl, propenyl, hydroxy, siloxy, isocyanate, nitrile, nitro, phenyl, C1-C40 alkyl, C2-C40 vinyl, C1-C40 alkoxy, C3-C40 cycloalkyl, C3-C40 heterocycloalkyl, C6-C40 aryl or C3-C40 heteroaryl, wherein any one of methyl, vinylmethyl, styrene or perfluorovinylmethyl is necessary;
R 3 is independently hydrogen, methyl, halogen, amino, epoxy, cyclohexene oxide, methylpropenyl, propenyl, hydroxy, siloxy, isocyanate, nitrile, nitro, phenyl, C1-C40 alkyl, C2-C40 vinyl, C1-C40 alkoxy, C3-C40 cycloalkyl, C3-C40 heterocycloalkyl, C6-C40 aryl or C3-C40 heteroaryl, wherein one propenyl or methylpropenyl is necessary;
x, y and z are each independently integers of 1-100, and p is an integer of 1-200; is a grafting site with a shell layer;
the structure of the structural unit A is as follows
Wherein the method comprises the steps ofIs a chemical bond connection site, and the structural unit B is a cross-linking agent residue.
In some embodiments, the method for preparing the silicon-containing adhesive comprises the following steps in parts by weight:
S1, preparing a suspension of a product A and a product B obtained by hydrolyzing and polycondensing any two of tin tetrachloride, zirconium tetrachloride, tetraethoxysilane and tetrabutyl titanate with water, heating to a reflux state, continuously stirring for 2-3 hours, centrifuging after the reaction is finished, washing with ethanol, drying, and calcining at 500-600 ℃ to obtain an inorganic silicon adhesive;
S2, mixing 80-90 parts of organosiloxane containing R 1 groups, 80-90 parts of organosiloxane containing R 2 groups and 80-90 parts of organosiloxane containing R 3 groups, adding 170-180 parts of toluene, 45-50 parts of deionized water and 2-4 parts of concentrated sulfuric acid, heating to 70-80 ℃ and stirring at constant temperature for 1-2 hours, filtering, concentrating and drying under reduced pressure after the reaction is finished, adding 35-45 parts of compound containing structural unit A and 160-180 parts of heptane, heating to 40-50 ℃ and continuously reacting for 12-14 hours, and cooling to room temperature after the reaction is finished to obtain a polysiloxane copolymer precursor;
S3, under the inert protective gas atmosphere, mixing 60-70 parts of tetraethyl orthosilicate, 180-220 parts of the inorganic silicon adhesive in the step S1, 80-90 parts of the polysiloxane copolymer precursor in the step S2 and the cross-linking agent, adding triethylamine, heating to 70-80 ℃, stirring at constant temperature for 1-3 hours, and obtaining the modified inorganic silicon adhesive after the reaction is finished;
And S4, mixing and uniformly stirring the organic silicon adhesive and the inorganic silicon adhesive in the step S3 to obtain the silicon-containing adhesive.
The structure of the organosilicon adhesive is shown as a formula I:
in some embodiments, in step S3, the crosslinking agent has any one of the following structures:
(1)
(2) wherein n is an integer of 0 to 8, and R 4 is any one of-COOH, -OH, -SH or-NCO.
In some embodiments, the preparation method of the compound containing the structural unit A comprises the following steps of mixing 3-amino-1-propanol and 2, 6-di-tert-butyl-4-chlorophenol, adding the mixture into N, N-dimethylformamide, adding an acid binding agent, heating to 35-45 ℃, stirring at constant temperature for 12-14 h, and filtering after the reaction is finished to obtain the compound containing the structural unit A.
In some embodiments, the preparation method of the modified PET matrix comprises the following steps of melting and blending 1-3 parts of ionomers, 70-74 parts of PET and 1-2 parts of chain extender, extruding through a double-screw extruder, cooling, cutting and forming.
The OCA film is prepared by compounding a fluorine special-shaped film layer, a silicon-containing adhesive layer and a modified PET matrix, wherein the fluorine special-shaped film layer and the silicon-containing adhesive layer have higher light transmittance, and the traditional PET has certain light transmittance but still has a lifting space.
The modified PET matrix of the application can obtain the modified PET matrix with lower transparency and refractive index by adopting the melt blending of the ionomers, PET and the chain extender, improves the transmittance of the OCA film and reduces the refractive index, and simultaneously can enhance the flame retardant property of the OCA film, which is probably because the PET molecular chain has regular structure and stronger crystallization property, but the movement capability of the molecular chain is blocked due to the rigidity of the molecular chain, the self-made ionomer structure contains a small amount of ionizable groups, can generate hydrogen bond action with the PET matrix to form physical crosslinking, improves the transmittance of PET, can also act with the silicon-containing adhesive layer, increases the adhesive force between the modified PET matrix and the silicon-containing adhesive layer, and further contains a certain N element to improve the flame retardant property of the OCA film.
In some embodiments, the method of preparing the ionomer comprises the steps of:
a1, mixing N-methylallylamine, diglycolamine and cyanuric chloride, adding N, N-dimethylformamide, then adding an acid binding agent, heating to 40-45 ℃, stirring for 14-16 hours at a constant temperature, and concentrating and drying under reduced pressure after the reaction is finished to obtain a compound A;
A2, mixing the compound A, 3-methyl-1-butene and toluene, adding a catalyst, heating to 80-90 ℃, stirring for 2-3 hours at a constant temperature, and obtaining the ionomer after the reaction is finished.
In some embodiments, in the step A1, the molar ratio of the N-methylallylamine, the diglycolamine and the cyanuric chloride is (0.9-1.1): 2-2.2): 1.
In some embodiments, in step A2, the molar ratio of the compound A to 3-methyl-1-butene is 1 (2-2.4).
In some embodiments, in step A2, the catalyst is benzoyl peroxide and/or ammonium persulfate.
The invention further provides a preparation method of the OCA optical film, which comprises the following steps of respectively coating a layer of silicon-containing adhesive on the upper surface and the lower surface of a modified PET matrix to obtain a silicon-containing adhesive layer, scraping the silicon-containing adhesive layer, attaching a fluorine-containing special-shaped film layer on the silicon-containing adhesive layer, and curing the film at 200-300 ℃ for 1-2 hours to obtain the OCA optical film.
Compared with the prior art, the invention has the following beneficial effects:
(1) The OCA optical film is formed by bonding and compounding a fluorine-containing special-shaped film layer, a silicon-containing adhesive layer and a modified PET matrix, and has excellent ageing and yellowing resistance, high temperature resistance and flexibility, better light transmittance, flame retardance and low refractive index.
(2) According to the invention, the thickness ratio of the silicon-containing adhesive layer to the modified PET substrate is regulated, so that on one hand, the deterioration of the bonding effect caused by low bonding force can be prevented, and on the other hand, the reduction of the light transmittance of the OCA film caused by more reflection and scattering when light passes through the OCA film can be prevented.
(3) The self-made ionomer structure contains a small amount of ionizable groups, can generate hydrogen bond action with the PET matrix to form physical crosslinking, improves the transmittance of PET, can also act with the silicon-containing adhesive layer, increases the adhesive force between the modified PET matrix and the silicon-containing adhesive layer, and further contains a certain N element to improve the flame retardant property of the OCA film.
(4) The silicon-containing adhesive has a core-shell structure, the reflectivity of the adhesive can be improved and the refractive efficiency can be reduced through complementation and synergy of a plurality of different elements, and on the other hand, the outermost layer of the silicon-containing adhesive has a modified POSS structure, wherein double bonds in the modified POSS structure can improve the adhesive bonding capability of the adhesive, hindered phenol groups in the modified POSS structure improve the anti-aging yellowing performance of the adhesive, meanwhile, the chemical structure of the POSS groups endows the adhesive with certain toughness, and on the other hand, the crosslinking agent crosslinks the silicon-containing adhesive, so that pi-pi accumulation can be formed by phenyl groups in the modified POSS structure when the molecular weight of the modified POSS structure is increased and the temperature resistance of the adhesive is improved.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following preparation examples, examples and comparative examples, PET was purchased from Ningbo Co., ltd. For star plasticization, CESA-extend chain extender was purchased from Shenzhen Huixin plastics chemical Co., ltd., and acrylic adhesive was purchased from Dongguan New Material technology Co., ltd.
Preparation example 1
A process for preparing the compound containing structural unit A includes such steps as mixing 3-amino-1-propanol (0.3 mol) with 2, 6-di-tert-butyl-4-chlorophenol (0.36 mol), adding it to 300mLN, N-dimethylformamide, adding sodium hydrogen carbonate (0.42 mol), heating to 40 deg.C, constant-temp stirring for 13 hr, and filtering.
Preparation example 2
The silicon-containing adhesive comprises a modified inorganic silicon adhesive and an organic silicon adhesive in a mass ratio of 1:1.3, wherein the modified inorganic silicon adhesive consists of a hollow core layer and a shell layer, and the outer layer of the shell layer is grafted with a structure shown in a formula I:
Wherein R 1 is methyl, R 2 is methyl and hydrogen, R 3 is propenyl and hydroxy, x is 40, y is 40, z is 40, and p is 30; Is grafted to the shell layer, and the structure of the structural unit A is as follows
Wherein the method comprises the steps ofIs a chemical bond connection site, and the structural unit B is a cross-linking agent residue.
The preparation method of the silicon-containing adhesive comprises the following steps in parts by weight:
S1, mixing 100 parts of tetraethyl orthosilicate, 2L of deionized water and 70mL of 2mol/L sodium hydroxide solution, performing hydrolytic polycondensation for 3 hours at room temperature, centrifuging to obtain a product A, preparing 300 parts of tetrabutyl titanate and 900 parts of ethanol into a material A, preparing 900 parts of ethanol, 90 parts of deionized water and 72 parts of glacial acetic acid into a material B, adding the material B into the material A, stirring for 2 hours at room temperature, centrifuging to obtain a product B, mixing the product A and the product B with 2.5L of deionized water into a suspension, heating to a reflux state, continuously stirring for 2.5 hours, centrifuging after the reaction, washing with ethanol, drying, and calcining at 550 ℃ to obtain an inorganic silicon adhesive;
S2, mixing 85 parts of dimethyl dimethoxy silane, 85 parts of methyl diethoxy silane and 85 parts of allyl triethoxy silane, adding 175 parts of toluene, 47 parts of deionized water and 3 parts of 98wt% of concentrated sulfuric acid, heating to 75 ℃, stirring for 1.5 hours at constant temperature, filtering, decompressing, concentrating and drying after the reaction is finished, adding 40 parts of a compound containing a structural unit A and 170 parts of heptane, heating to 45 ℃ for continuous reaction for 13 hours, and cooling to room temperature after the reaction is finished to obtain a polysiloxane copolymer precursor;
S3, under the atmosphere of N 2, mixing 7 parts of tetraethyl orthosilicate, 200 parts of the inorganic silicon adhesive in the step S1, 85 parts of the polysiloxane copolymer precursor in the step S2 and 0.2 part of terephthalyl alcohol, adding 20 parts of triethylamine, heating to 75 ℃, stirring at constant temperature for 2 hours, and obtaining the modified inorganic silicon adhesive after the reaction is finished;
And S4, mixing and uniformly stirring the organic silicon adhesive and the inorganic silicon adhesive in the step S3 to obtain the silicon-containing adhesive.
Wherein the compound containing the structural unit A is prepared from preparation example 1, and the structure of the organosilicon adhesive is shown as a formula II:
Preparation example 3
The preparation method of the ionomer comprises the following steps:
a1, mixing 0.5mol of N-methylallylamine, 1.05mol of diglycolamine and 0.5mol of cyanuric chloride, adding 1L of N, N-dimethylformamide, then adding 0.7mol of sodium carbonate, heating to 42 ℃, stirring for 15 hours at constant temperature, concentrating under reduced pressure after the reaction is finished, and drying to obtain a compound A;
A2, mixing 0.5mol of compound A, 1.1mol of 3-methyl-1-butene and 1.8L of toluene, adding 0.5g of benzoyl peroxide, heating to 85 ℃, stirring for 2.5 hours at constant temperature, and obtaining the ionomer after the reaction is finished.
Preparation example 4
The preparation of the ionomers was carried out in the same manner as in preparation example 3, except that equimolar (3-aminocyclobutane-1, 1-diyl) dimethanol was used instead of 3-methyl-1-butene.
Preparation example 5
The preparation method of the ionomer, the specific embodiment is the same as in preparation example 3, except that 3-methyl-1-butene is 0.5mol.
Preparation example 6
The preparation method of the ionomer is the same as in preparation example 3, except that 1, 3-dichloro-2- (chloromethyl) propane is used instead of cyanuric chloride.
Preparation example 7
The preparation method of the ionomer, the specific embodiment is the same as that of preparation example 3, except that diglycolamine is 0.5mol.
Preparation example 8
The preparation method of the modified PET matrix comprises the following steps of melting and blending 2 parts of ionomers, 72 parts of PET and 1.5 parts of CESA-extend chain extender, extruding by a double-screw extruder, cooling, cutting and forming.
Wherein the ionomer was prepared in preparation example 3.
Preparation example 9
The preparation method of the modified PET substrate is the same as that of preparation example 8, except that the ionomer is prepared in preparation example 4.
Preparation example 10
The preparation method of the modified PET substrate is the same as that of preparation example 8, except that the ionomer is prepared in preparation example 5.
PREPARATION EXAMPLE 11
The preparation method of the modified PET substrate is the same as that of preparation example 8, except that the ionomer is prepared in preparation example 6.
Preparation example 12
The preparation method of the modified PET substrate is the same as that of preparation example 8, except that the ionomer is prepared in preparation example 7.
Example 1
An OCA optical film comprises five layers of structures, namely an FEP film layer, a silicon-containing adhesive layer, a modified PET matrix, a silicon-containing adhesive layer and an FEP film layer from top to bottom, wherein the silicon-containing adhesive layer is prepared from silicon-containing adhesive.
The preparation method of the OCA optical film comprises the following steps of respectively coating a layer of silicon-containing adhesive with the thickness of 1500 mu m on the upper surface and the lower surface of a modified PET matrix with the thickness of 7500 mu m to obtain a silicon-containing adhesive layer, pasting a 2000 mu mFEP film layer on the silicon-containing adhesive layer after scraping, and curing for 1.5 hours at the temperature of 250 ℃ to obtain the OCA optical film.
Wherein the modified PET substrate was prepared in preparation example 8, and the silicon-containing adhesive was prepared in preparation example 2.
Example 2
An OCA optical film comprises five layers of structures, namely an FEP film layer, a silicon-containing adhesive layer, a modified PET matrix, a silicon-containing adhesive layer and an FEP film layer from top to bottom, wherein the silicon-containing adhesive layer is prepared from silicon-containing adhesive.
The preparation method of the OCA optical film comprises the following steps of respectively coating a layer of silicon-containing adhesive with the thickness of 100 mu m on the upper surface and the lower surface of a modified PET matrix with the thickness of 1000 mu m to obtain a silicon-containing adhesive layer, scraping the silicon-containing adhesive layer, attaching a 1000 mu mFEP film layer on the silicon-containing adhesive layer, and curing for 2 hours at 200 ℃ to obtain the OCA optical film.
Wherein the modified PET substrate was prepared in preparation example 8, and the silicon-containing adhesive was prepared in preparation example 2.
Example 3
An OCA optical film comprises five layers of structures, namely an FEP film layer, a silicon-containing adhesive layer, a modified PET matrix, a silicon-containing adhesive layer and an FEP film layer from top to bottom, wherein the silicon-containing adhesive layer is prepared from silicon-containing adhesive.
The preparation method of the OCA optical film comprises the following steps of respectively coating a layer of silicon-containing adhesive with the thickness of 3000 mu m on the upper surface and the lower surface of a modified PET matrix with the thickness of 300 mu m to obtain a silicon-containing adhesive layer, scraping, attaching a 3000 mu mFEP film layer on the silicon-containing adhesive layer, and curing for 1h at 300 ℃ to obtain the OCA optical film.
Wherein the modified PET substrate was prepared in preparation example 8, and the silicon-containing adhesive was prepared in preparation example 2.
Example 4
An OCA optical film and a preparation method thereof are provided, and specific embodiments are the same as in example 1, except that a modified PET substrate is prepared in preparation example 9.
Example 5
An OCA optical film and a method for producing the same are described in example 1, except that a modified PET substrate was produced in production example 10.
Example 6
An OCA optical film and a method for producing the same are described in example 1, except that a modified PET substrate was produced in production example 11.
Example 7
An OCA optical film and a method for producing the same are described in example 1, except that a modified PET substrate was produced in production example 12.
Comparative example 1
An OCA optical film and a preparation method thereof are provided, and specific embodiments are the same as in example 1, except that a PET substrate is used instead of a modified PET substrate.
The preparation method of the PET matrix comprises the following steps of melting and blending 72 parts of PET through double screws and 1.5 parts of dicyandiamide, extruding by a rod extruder, cooling, cutting and forming.
Comparative example 2
An OCA optical film and a method for preparing the same, the specific embodiment is the same as example 1, except that acrylic adhesive is used instead of silicon-containing adhesive.
Performance test:
(1) The anti-ultraviolet performance is that an OCA optical film is placed in an ultraviolet aging box, a 1kW lamp tube is adopted, the distance is 50cm, the continuous irradiation aging is carried out for 100 hours, and the yellowing index of a glue layer is measured and calculated according to the GB/T7975-2005 standard;
(2) Peel force test, namely, the peel force of a silicon-containing adhesive layer in an optical film is tested according to GB/T7122-1996 'high-strength adhesive peel strength determination floating roller method';
(3) Testing elongation, namely cutting the OCA optical film into a dumbbell shape, and testing at a speed of 50mm/min by adopting a tensile testing machine, wherein the higher the elongation is, the better the toughness is;
(4) Temperature resistance performance the OCA optical film in method (3) was placed in 300 ℃ environment for 3 days, and elongation was again tested;
(5) Light transmittance test, namely measuring by adopting a photoelectric haze meter with the model of NDH 2000;
(6) The transmittance test, namely measuring by using a spectrophotometer UV3100, wherein the wavelength range is 400-700 nm;
(7) Flame retardant Property test according to UL-94 test.
The binders of each example and comparative example were tested according to the test methods described above, and the results are shown in table 1.
TABLE 1
According to the results, the OCA optical films of examples 1-3 have better anti-aging yellowing performance, flexibility and high-temperature resistance, and good transmittance, the bonding strength between the layers is high, the flame retardant performance is good, the OCA optical film is reduced in flexibility due to the fact that equimolar (3-aminocyclobutane-1, 1-diyl) dimethanol is adopted to replace 3-methyl-1-butene in example 4, but the peeling strength and transmittance of the OCA optical film are increased due to the fact that ionic bonds in the OCA optical film are increased, the transmittance and transmittance of the OCA optical film are slightly reduced due to the fact that the molar ratio of the compound A to 3-methyl-1-butene is changed, the transmittance and transmittance of the OCA optical film are reduced due to the fact that 1, 3-dichloro-2- (chloromethyl) propane is adopted to replace cyanuric chloride in example 6, the flame retardant performance of the OCA optical film is reduced due to the fact that the molar ratio of N-methallylamine, diglycolamine and cyanuric chloride is changed, the transmittance and transmittance of the OCA optical film is reduced due to the fact that the contrast ratio of the OCA optical film is reduced due to the fact that the modified substrate is changed, and the contrast ratio of the substrate is reduced due to the fact that the contrast ratio of the modified adhesive layer and the contrast ratio between the substrate and PET is reduced due to the fact that the contrast ratio is reduced due to the contrast ratio is reduced, and the contrast performance is reduced due to the contrast performance is obtained.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications and equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, and all such modifications and equivalents are intended to be encompassed in the scope of the claims of the present invention.
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| CN109642128A (en) * | 2016-11-24 | 2019-04-16 | 琳得科株式会社 | Double-sided silicone adhesive sheet and manufacturing method of double-sided silicone adhesive sheet |
| CN112574401A (en) * | 2020-10-01 | 2021-03-30 | 银金达(上海)新材料有限公司 | High-transmittance modified PET resin and application thereof |
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