CN116769435A - Ultraviolet light curing OCA optical cement and manufacturing method thereof - Google Patents
Ultraviolet light curing OCA optical cement and manufacturing method thereof Download PDFInfo
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- CN116769435A CN116769435A CN202310794052.XA CN202310794052A CN116769435A CN 116769435 A CN116769435 A CN 116769435A CN 202310794052 A CN202310794052 A CN 202310794052A CN 116769435 A CN116769435 A CN 116769435A
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- 230000003287 optical effect Effects 0.000 title claims abstract description 34
- 201000007909 oculocutaneous albinism Diseases 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000004568 cement Substances 0.000 title claims description 5
- 239000000853 adhesive Substances 0.000 claims abstract description 44
- 230000001070 adhesive effect Effects 0.000 claims abstract description 44
- 239000007822 coupling agent Substances 0.000 claims abstract description 13
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 claims abstract description 8
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000000670 limiting effect Effects 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 15
- 239000002313 adhesive film Substances 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 11
- 238000006116 polymerization reaction Methods 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 9
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 8
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 claims description 6
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-UHFFFAOYSA-N 0.000 claims description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 6
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003112 inhibitor Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 150000004645 aluminates Chemical class 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- -1 beta-methoxyethoxy Chemical group 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000011049 filling Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000010354 integration Effects 0.000 abstract 1
- 238000001723 curing Methods 0.000 description 24
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 3
- 238000003848 UV Light-Curing Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009044 synergistic interaction Effects 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/003—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses ultraviolet light curing OCA optical adhesive and a preparation method thereof, wherein the OCA optical adhesive comprises the following components in parts by weight: 100 parts of mixed virgin rubber of the A component virgin rubber and the B component virgin rubber, 0.01-0.1 part of TDI (time delay and integration) thermosetting agent, 0.5-1 part of trimethylolpropane triacrylate, 0.2-1 part of photoinitiator 184 and 0.01-0.1 part of coupling agent; the limiting properties of the a-component virgin rubber are as follows: tg between-13 and-17 ℃, molecular weight Mw:500000 to 600000; the definition performance of the B component virgin rubber is mainly as follows: tg is between-19 and-25 ℃, molecular weight Mw:250000 to 350000. The OCA optical adhesive provided by the invention has the advantages of hardness and softness, capability of rapidly filling an air gap, full-filling effect of LOCA, no problem of concave-convex points, and further firm adhesion of a panel and a touch screen after ultraviolet light curing.
Description
Technical Field
The invention relates to the technical field of OCA optical adhesives, in particular to an ultraviolet light curing OCA optical adhesive and a manufacturing method thereof.
Background
OCA optical adhesive is a special double-sided pressure-sensitive adhesive without base material and optical transparent, and has the advantages of no color, transparency, light transmittance of more than 90 percent, small curing shrinkage, and being a main adhesive for bonding optical components. At present, the bonding of OCA optical cement is a full bonding process, and the panel and the touch screen are bonded together in a seamless mode, so that screen dust and water vapor can be completely eradicated.
When the traditional OCA optical adhesive is fully attached, a panel and a touch screen can be bonded, but an air gap between the panel and the touch screen cannot be filled due to poor creep performance; liquid Optically Clear Adhesive (LOCA) fills the air gap to better characterize the display assembly, but requires special adhesive supply equipment for production and is costly to use.
Disclosure of Invention
The invention aims to solve the technical problem of providing the ultraviolet light curing OCA optical adhesive, which is rigid and flexible, can quickly fill an air gap, has the full filling effect of LOCA, has no problem of concave-convex points, and further firmly bonds a panel and a touch screen after ultraviolet light curing. Meanwhile, a manufacturing method of ultraviolet light curing OCA optics is provided.
In order to achieve the above purpose, the invention adopts the following technical scheme: an ultraviolet light curing OCA optical adhesive comprises the following components in parts by weight:
100 parts of mixed virgin rubber of A component and B component,
0.01 to 0.1 part of TDI thermosetting agent,
0.5 to 1 part of trimethylolpropane triacrylate,
0.2-1 part of photoinitiator 184,
0.01-0.1 part of coupling agent;
the limiting performance of the A-component virgin rubber is as follows: tg between-13 and-17 ℃, molecular weight Mw:500000~600000, normal temperature modulus 75~85Kpa, viscosity: 8500 to 11000cps;
the limiting performance of the B-component virgin rubber is mainly as follows: tg is between-19 and-25 ℃, molecular weight Mw: 250000-350000, normal temperature modulus 50-70 Kpa, viscosity: 6000 to 8000cps.
The technical scheme further improved in the technical scheme is as follows:
1. in the scheme, the A-component virgin rubber consists of the following components in parts by weight:
30 parts of isooctyl acrylate,
5 parts of hydroxyethyl acrylate, which is used for preparing the adhesive,
4 parts of acryloylmorpholine,
11 parts of isobornyl acrylate,
60 parts of a solvent, and the solvent is mixed,
0.1 part of polymerization inhibitor BHT,
1 part of acrylic functional grafting monomer.
2. In the scheme, the solvent is a mixed solvent formed by 20 parts of toluene and 40 parts of ethyl acetate.
3. In the scheme, the B component virgin rubber consists of the following components in parts by weight:
40 parts of isooctyl acrylate,
4 parts of hydroxyethyl acrylate, namely a mixture of a plurality of components,
1 part of acryloylmorpholine,
5 parts of isobornyl acrylate,
50 parts of a solvent, namely a solvent,
0.2 part of AIBN initiator,
0.3 part of AIBN,
0.1 part of polymerization inhibitor BHT,
1 part of acrylic functional grafting monomer.
4. In the above scheme, the solvent is a mixed solvent formed by 40 parts of ethyl acetate and 10 parts of butanone.
5. The ultraviolet light curing OCA optical adhesive according to claim 1, wherein: the coupling agent is one of vinyl triethoxysilane, vinyl trimethoxysilane, vinyl tri (beta-methoxyethoxy) and aluminate coupling agent.
The technical scheme of the method adopted by the invention is as follows: the manufacturing method for the ultraviolet curing OCA optical adhesive comprises the following steps:
step one, uniformly mixing the component A and the component B, adding TDI (toluene diisocyanate) thermosetting agent, trimethylolpropane triacrylate, photoinitiator 184 and coupling agent into the mixture, uniformly stirring, and removing bubbles in vacuum;
and secondly, selecting a release film, coating by a slit or a scraper, directly coating the mixed ultraviolet light curing adhesive, putting the adhesive into an oven for baking to remove a solvent, compounding the release film, and then curing the prepared adhesive film at medium temperature to obtain the full-filled OCA optical adhesive.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the ultraviolet light curing OCA optical adhesive and the preparation method thereof, the A component adhesive with high Tg and the B component adhesive with low Tg are prepared by changing the monomer amount and the process, and the two monomers have the same types and different performances, but have small difference range, so that the two monomers are mutually cooperated and have no rejection; the component A adhesive with high Tg and the component B adhesive with low Tg can have mutual synergistic effect after being mixed in a certain proportion, so that the adhesive film is rigid and soft and is capable of quickly filling air gaps, has the full filling effect of LOCA, has no problem of concave-convex points, and further firmly adheres the panel and the touch screen after ultraviolet light curing.
Description of the embodiments
The present patent will be further understood by the specific examples given below, which are not intended to be limiting.
The invention is further described below with reference to examples:
examples 1 to 3: an ultraviolet light curing OCA optical adhesive comprises the following components in parts by weight as shown in Table 1:
TABLE 1
Component (A) | Example 1 | Example 2 | Example 3 | Example 4 |
Mixed virgin rubber | 100 parts of | 100 parts of | 100 parts of | 100 parts of |
TDI thermal curing agent | 0.04 part | 0.06 part | 0.04 part | 0.06 part |
Trimethylolpropane triacrylate | 0.6 part | 0.8 part | 0.6 part | 0.8 part |
Photoinitiator 184 | 0.6 part | 1.5 parts by weight | 0.4 part | 0.6 part |
Coupling agent | 0.07 part | 0.04 part | 0.05 part | 0.04 part |
;
The limiting performance of the A-component virgin rubber is as follows: tg between-13 and-17 ℃, molecular weight Mw:500000~600000, normal temperature modulus 75~85Kpa, viscosity: 8500 to 11000cps;
the limiting performance of the B-component virgin rubber is mainly as follows: tg is between-19 and-25 ℃, molecular weight Mw: 250000-350000, normal temperature modulus 50-70 Kpa, viscosity: 6000 to 8000cps.
The A component is synthesized by the following steps:
30 parts of isooctyl acrylate, 5 parts of hydroxyethyl acrylate, 4 parts of acryloylmorpholine and 11 parts of isobornyl acrylate are weighed and mixed in a reaction kettle, 20 parts of toluene and 40 parts of ethyl acetate are added as a mixed solvent for polymerization, nitrogen is introduced for 20min at 62 ℃ under 150r/min stirring, then 0.08 part of AIBN initiator is added, and after 12h of reaction, 0.1 part of AIBN is added for continuous reaction for 5h. And after the reaction is finished, cooling to below 60 ℃ and introducing air for half an hour, adding 0.1 part of polymerization inhibitor BHT, uniformly stirring and inhibiting polymerization for ten minutes, adding 1 part of acrylic functional grafting monomer, and heating to 74 ℃ for grafting at a high temperature for 6 hours to obtain the component A of the virgin rubber.
The component B is synthesized by the following implementation scheme:
40 parts of isooctyl acrylate, 4 parts of hydroxyethyl acrylate, 1 part of acryloylmorpholine and 5 parts of isobornyl acrylate are weighed and mixed in a reaction kettle, 40 parts of ethyl acetate and 10 parts of butanone are added as solvents for polymerization, nitrogen is introduced for 20min under the condition of heating to 68 ℃ under the stirring of 150r/min, then 0.2 part of AIBN initiator is added, and after the reaction is carried out for 8h, 0.3 part of AIBN is added for continuous reaction for 3h. And after the reaction is finished, cooling to below 60 ℃ and introducing air for half an hour, adding 0.1 part of polymerization inhibitor BHT, uniformly stirring and inhibiting polymerization for ten minutes, adding 1 part of acrylic functional grafting monomer, and heating to 74 ℃ for grafting at a high temperature for 6 hours to obtain the component B of the virgin rubber.
The A-component and B-component virgin rubber in example 1 was used in an amount of 2:1, and the A component and the B component of the virgin rubber in the example 2 are mixed according to the proportion of 1:1, and the A component and the B component virgin rubber in the example 3 are mixed according to the proportion of 1: 2.
A manufacturing method for ultraviolet light curing OCA optical cement comprises the following steps:
uniformly mixing the component A and the component B according to a certain proportion, adding a thermosetting agent, a photo-curing monomer (reactive diluent monomer), a photoinitiator, a coupling agent and a little solvent into the mixture, uniformly stirring, and removing bubbles in vacuum;
step two, selecting a 50-100 mu m release film with release force (1 g-100 g), coating by a slit or a scraper, directly coating an ultraviolet curing adhesive with 200 mu m mixed, putting the ultraviolet curing adhesive into an oven to bake and remove a solvent, compounding the 50-100 mu m release film with proper release force (3-50 g), and then curing the prepared adhesive film for 2 days at medium temperature to obtain the full-filled OCA optical adhesive.
Comparative example 1: the ultraviolet light curing OCA optical adhesive consists of the following components in parts by weight, 100 parts of A-component virgin rubber, 0.02 part of TDI,0.7 part of TMPTA,0.3 part of photoinitiator 184 and 0.01 part of aluminate coupling agent are mixed and stirred uniformly, a 200 mu m adhesive film is coated after defoaming, and then the ultraviolet light curing OCA optical adhesive is obtained after curing for 2 days at medium temperature.
Comparative example 2: an ultraviolet light curing OCA optical adhesive is prepared by uniformly mixing 100 parts of B component virgin rubber with 0.02 part of TDI,0.7 part of TMPTA,0.3 part of photoinitiator 184 and 0.01 part of aluminate coupling agent, stirring, coating a 200 mu m adhesive film after defoaming, and curing for 2d at medium temperature.
The ultraviolet curing OCA optical adhesives obtained in examples 1 to 3 and comparative examples 1 to 2 were subjected to a peel force test, a rheology test, and an ink filling test:
(1) Peel force: the adhesive film is uncovered, a light release film is stuck on a 0.05MM transparent PET film, a sample with the width of 25.4MM and the length of 300MM is cut, the other heavy release film is uncovered, a roller with the speed of 2KG is used for rolling and sticking on a glass plate at the speed of 600MM/MIN, standing is carried out for 20MIN, then a 360nm LED lamp is used for irradiating 4000mj for UV curing, a tensile testing machine is used for testing the 180 DEG stripping adhesive force, and a specific testing method is referred to ASMTD3330 international standard.
(2) Storage modulus: samples for measurement were obtained by laminating each pressure-sensitive adhesive film layer to a thickness of about 1.5 mm. UV curing was performed by irradiating 4000mj with a 360nm LED lamp, and dynamic viscoelasticity was measured using ARES manufactured by TA Instruments under the following conditions. The storage modulus G' at 25℃was read from the measurement results.
(3) Creep: samples for measurement were obtained by laminating each pressure-sensitive adhesive film layer to a thickness of about 1.5 mm. UV curing was performed by irradiating 4000mj with a 360nm LED lamp, and creep was measured at 60 ℃ using ARES manufactured by TA Instruments. The deformation amount is read from the measurement result.
(4) And (3) observing concave-convex points: and (5) visually observing whether the concave-convex points exist or not by horizontally inclining the adhesive film by 30 degrees against lamplight.
(5) Ink level difference filling property: and transferring the adhesive film onto PET, attaching the adhesive film onto glass with cross ink level difference, standing for 1 day after UV is carried out after defoaming, and observing the filling condition of the ink level difference. Bubble-free, marked o; the presence of bubbles is denoted gamma.
Examples the test results are shown in table 3:
TABLE 3 Table 3
Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
Storage modulus at 25℃before UV (Kpa) | 70 | 75 | 69 | 86 | 60 |
Storage modulus at 25 ℃ after UV (Kpa) | 101 | 90 | 81 | 130 | 75 |
Creep at 60℃before UV (%) | 1032 | 1350 | 1644 | 901 | 1946 |
UV rear glass peel force (gf/inch) | 2145 | 2450 | 2737 | 1936 | 2932 |
Ink filling (percent) | ○ | ○ | ○ | ╳ | ○ |
Concave-convex point | Without any means for | Without any means for | Without any means for | Without any means for | Has the following components |
;
As shown in the evaluation results of table 3, the above data results were obtained: the single-component A adhesive has higher normal temperature modulus, harder adhesive film and smaller creep at 60 ℃ and can not completely fill the gap generated by the ink; the single-component B-component adhesive has lower normal temperature modulus, softer adhesive film and larger creep at 60 ℃, and can completely fill the gap generated by ink, but can cause the problem of concave-convex points due to the soft adhesive film; the adhesive films of examples 1-3 have moderate hardness due to the synergistic interaction of AB components, can completely fill the gaps generated by the ink, have no problem of concave-convex points, and have remarkable performance.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (7)
1. An ultraviolet curing OCA optical adhesive is characterized in that: the OCA optical adhesive comprises the following components in parts by weight:
100 parts of mixed virgin rubber of A component and B component,
0.01 to 0.1 part of TDI thermosetting agent,
0.5 to 1 part of trimethylolpropane triacrylate,
0.2-1 part of photoinitiator 184,
0.01-0.1 part of coupling agent;
the limiting performance of the A-component virgin rubber is as follows: tg between-13 and-17 ℃, molecular weight Mw:500000~600000, normal temperature modulus 75~85Kpa, viscosity: 8500 to 11000cps;
the limiting performance of the B-component virgin rubber is mainly as follows: tg is between-19 and-25 ℃, molecular weight Mw: 250000-350000, normal temperature modulus 50-70 Kpa, viscosity: 6000 to 8000cps.
2. The ultraviolet light curing OCA optical adhesive according to claim 1, wherein: the A component virgin rubber consists of the following components in parts by weight:
30 parts of isooctyl acrylate,
4-6 parts of hydroxyethyl acrylate,
3-5 parts of acryloylmorpholine,
9-13 parts of isobornyl acrylate,
50-70 parts of a solvent,
0.05 to 0.15 part of polymerization inhibitor BHT,
0.8-1.2 parts of acrylic functional grafting monomer.
3. The ultraviolet light curing OCA optical adhesive according to claim 2, wherein: the solvent is a mixed solvent formed by 20 parts of toluene and 40 parts of ethyl acetate.
4. The ultraviolet light curing OCA optical adhesive according to claim 1, wherein: the component B of the virgin rubber consists of the following components in parts by weight:
40 parts of isooctyl acrylate,
3-5 parts of hydroxyethyl acrylate,
0.8 to 1.2 parts of acryloylmorpholine,
3-7 parts of isobornyl acrylate,
40-60 parts of a solvent,
0.15 to 0.3 part of AIBN initiator,
0.2 to 0.4 part of AIBN,
0.05 to 0.15 part of polymerization inhibitor BHT,
0.8-1.2 parts of acrylic functional grafting monomer.
5. The ultraviolet light curable OCA optical adhesive of claim 4, wherein: the solvent is a mixed solvent formed by 40 parts of ethyl acetate and 10 parts of butanone.
6. The ultraviolet light curing OCA optical adhesive according to claim 1, wherein: the coupling agent is one of vinyl triethoxysilane, vinyl trimethoxysilane, vinyl tri (beta-methoxyethoxy) and aluminate coupling agent.
7. A method for manufacturing the ultraviolet curing OCA optical cement according to claim 1, which is characterized in that: the method comprises the following steps:
step one, uniformly mixing the component A and the component B, adding TDI (toluene diisocyanate) thermosetting agent, trimethylolpropane triacrylate, photoinitiator 184 and coupling agent into the mixture, uniformly stirring, and removing bubbles in vacuum;
and secondly, selecting a release film, coating by a slit or a scraper, directly coating the mixed ultraviolet light curing adhesive, putting the adhesive into an oven for baking to remove a solvent, compounding the release film, and then curing the prepared adhesive film at medium temperature to obtain the full-filled OCA optical adhesive.
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