CN116836655A - Optical pressure-sensitive adhesive for high-light-transmittance foldable screen and preparation method thereof - Google Patents
Optical pressure-sensitive adhesive for high-light-transmittance foldable screen and preparation method thereof Download PDFInfo
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- CN116836655A CN116836655A CN202311005342.8A CN202311005342A CN116836655A CN 116836655 A CN116836655 A CN 116836655A CN 202311005342 A CN202311005342 A CN 202311005342A CN 116836655 A CN116836655 A CN 116836655A
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 51
- 230000003287 optical effect Effects 0.000 title claims abstract description 49
- 238000002834 transmittance Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title description 12
- 239000000178 monomer Substances 0.000 claims abstract description 79
- 239000003999 initiator Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 11
- -1 acrylic ester Chemical class 0.000 claims abstract description 10
- 239000012948 isocyanate Substances 0.000 claims abstract description 8
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 150000001412 amines Chemical class 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 69
- 239000000463 material Substances 0.000 claims description 50
- 239000007788 liquid Substances 0.000 claims description 39
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 37
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 29
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 23
- 238000005303 weighing Methods 0.000 claims description 23
- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical compound OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical compound CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 claims description 12
- 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 12
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 9
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 claims description 8
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 5
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 5
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 125000005396 acrylic acid ester group Chemical group 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229920001897 terpolymer Polymers 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 238000004383 yellowing Methods 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
- 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
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
-
- 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
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses an optical pressure-sensitive adhesive for a high-light-transmission foldable screen, which comprises the following components: the component A comprises the following components in parts by weight: 94-100 parts of acrylic ester soft monomer, 2-6 parts of functional monomer, 0.3-0.5 part of initiator, 100 parts of solvent, and 1-3 parts of isocyanate monomer and mixture thereof; component B: 1-2 parts of amine-containing reducer. The optical pressure-sensitive adhesive for the high-light-transmittance foldable screen has obviously improved light transmittance, is more excellent than the optical performance of the common OCA pressure-sensitive adhesive, has higher mechanical property due to the improvement of molecular weight, and has the bending times completely reaching the use standard of the foldable screen. The comprehensive performance meets the performance requirement of the foldable screen on the optical pressure-sensitive adhesive, and has wide market application prospect in the field of flexible electronics.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to an optical pressure-sensitive adhesive for a high-light-transmittance foldable screen and a preparation method thereof.
Background
Smartphones are composed of many thin layers with complex structures in which OCA optical pressure sensitive adhesives play an important role, particularly in foldable phones, which are required under external deformation to help dissipate the stress generated to prevent delamination or warpage of the film. Meanwhile, the light transmittance is directly determined to be interactive and used as a display screen. Therefore, the OCA optical pressure-sensitive adhesive is required to have sufficient adhesion, flexibility and elasticity, and high light transmittance. With the advent of the 5G flexible foldable screen cell phone age, the market for optical pressure sensitive adhesives applied to flexible foldable screens will grow in size.
However, the conventional OCA optical pressure-sensitive adhesive has various defects of low light transmittance, high haze, easy yellowing and the like, and meanwhile, the toughness and the mechanical properties under high and low temperature conditions cannot reach the folding standard.
Disclosure of Invention
In order to achieve the technical objective, the first aspect of the present invention provides an optical pressure-sensitive adhesive for a high-transmittance foldable screen, which has the following specific technical scheme:
an optical pressure sensitive adhesive for a high light transmission foldable screen, comprising:
the component A comprises the following components in parts by weight:
94-100 parts of acrylic ester soft monomer,
2-6 parts of functional monomer,
0.3 to 0.5 part of initiator,
100 parts of a solvent, namely a solvent,
1-3 parts of isocyanate monomer and mixture thereof;
component B:
1-2 parts of amine-containing reducer.
In some embodiments, the acrylate soft monomer is one or more of ethyl acrylate, isooctyl acrylate, and n-butyl acrylate.
In some embodiments, the functional monomer is one or more of acrylic acid, hydroxyethyl acrylate, and hydroxybutyl acrylate.
In some embodiments, the initiator is azobisisobutyronitrile.
In some embodiments, the solvent is ethyl acetate.
In some embodiments, the isocyanate monomer and mixtures thereof are toluene diisocyanate and one or both of its trimers, diphenylmethane diisocyanate.
In some embodiments, the amine-containing reducing agent is one or both of dimethylaminoethyl acrylate and 2, 2-dimethylol butanoic acid, wherein the dimethylaminoethyl acrylate has the molecular structural formula:
the molecular structural formula of the 2, 2-dihydroxymethyl butyric acid is as follows:
the invention provides a preparation method of an optical pressure-sensitive adhesive for a high-light-transmission foldable screen, which comprises the following steps of:
a preparation method of an optical pressure-sensitive adhesive for a high-light-transmittance foldable screen comprises the following steps:
step one: weighing part of acrylic ester soft monomers, part of functional monomers, part of initiator and part of solvent in the component A, and uniformly mixing with the component B to form a monomer mixed solution bottom material;
step two: uniformly mixing the rest acrylic ester soft monomer, the functional monomer, part of initiator and solvent to form monomer mixed liquid drop for feeding;
step three: heating and stirring a reaction container, adding a monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding monomer mixed liquid drops into a constant-pressure dropping funnel, and dropwise adding after the bottom material starts to react and is cooled and refluxed for 2-4 hours;
step four: after all the monomer mixed solution is dripped, preserving heat and reacting for 1-2h;
step five: adding the rest initiator, keeping the temperature for 2-4 hours, and cooling and discharging;
step six: mixing the discharged material from the fifth step with isocyanate monomer and the mixture thereof according to the mass ratio of 1: mixing uniformly in a proportion of 0.01-0.06, coating, and curing for 5min at 120 ℃ to form the optical pressure-sensitive adhesive for the high-light-transmittance foldable screen.
In some embodiments, in step three, the stirring rate is 130-150r/min and the reaction temperature is 78-85 ℃.
The invention has the following technical effects:
firstly, amine-containing reducing agent is introduced, so that the use of an initiator and an external cross-linking agent is reduced to the greatest extent, the light transmittance is improved, and the curing speed is accelerated.
The amine groups being converted into amine radical cations (R 3 The alpha-amino radical generated by losing one proton (H+) after N+ can be used as an initiator for monomer radical polymerization, so that the use of a thermal initiator is reduced, and simultaneously, the alpha-amino radical can also be subjected to crosslinking reaction with an isocyanate curing agent to increase crosslinking sites.
The second, toughness and mechanical properties are closely related to the molecular weight of the acrylic ester copolymer, and in the free radical polymerization of acrylic ester monomers, oxygen free radicals generated by the reaction of oxygen molecules and free radicals are easy to be further combined with a polymerization intermediate, so that the consumption of the polymerization intermediate is reduced, and the molecular weight is reduced.
The tertiary amine can react with the inactive peroxy free radical generated by the growth free radical and the oxygen reaction to be converted into active alpha-amino free radical, thereby reducing the oxygen inhibition effect, avoiding the consumption of a polymerization intermediate in the synthesis process, and finally improving the molecular weight, so that the final product of the invention has strong toughness and mechanical property.
Detailed Description
The following describes the technical scheme of the present invention in detail with reference to examples, but the present invention is not limited to these examples.
Embodiment one:
the optical pressure-sensitive adhesive for the high-light-transmission foldable screen in the embodiment comprises the following components in parts by weight: 36g of isooctyl acrylate, 60g of butyl acrylate, 4g of hydroxybutyl acrylate, 0.2g of azobisisobutyronitrile, 100g of ethyl acetate, and 2g of toluene diisocyanate and its triple polymer. The component B consists of the following components in parts by weight: dimethylaminoethyl acrylate 1g.
The preparation process of the optical pressure-sensitive adhesive for the high-transmittance foldable screen in the embodiment is as follows:
step one, accurately weighing 18g of isooctyl acrylate, 30g of butyl acrylate, 2g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile, 50g of ethyl acetate and 1g of dimethylaminoethyl acrylate, and uniformly mixing to form a monomer mixed solution base material.
Step two, accurately weighing 18g of isooctyl acrylate, 30g of butyl acrylate, 2g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile and 50g of ethyl acetate, and uniformly mixing to form monomer mixed liquid drop for feeding.
Heating and stirring the reaction container, adding the monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding the monomer mixed liquid bottom material into a constant-pressure dropping funnel, and dropwise adding the monomer mixed liquid bottom material after the bottom material starts to react and is cooled and refluxed for 2 hours; wherein the stirring rate is 150r/min, and the reaction temperature is 80 ℃.
Fourthly, after all the monomer mixed solution is dripped, preserving heat and reacting for 2 hours;
and fifthly, adding 0.1g of azodiisobutyronitrile, continuously preserving heat for 3 hours, and cooling and discharging.
Step six, weighing the discharged material, toluene diisocyanate and the tri-polymer thereof according to the mass ratio of 1: mixing uniformly in a proportion of 0.01, coating, and curing for 5min at 120 ℃ to form the optical pressure-sensitive adhesive for the high-transmittance foldable screen.
Embodiment two:
the optical pressure-sensitive adhesive for the high-light-transmission foldable screen in the embodiment comprises the following components in parts by weight: 30g of ethyl acrylate, 65g of butyl acrylate, 5g of hydroxyethyl acrylate, 0.2g of azobisisobutyronitrile, 100g of ethyl acetate, and 2.5g of toluene diisocyanate and its triple polymer. The component B consists of the following components in parts by weight: dimethylaminoethyl acrylate 1g.
The preparation process of the optical pressure-sensitive adhesive for the high-transmittance foldable screen in the embodiment is as follows:
step one, accurately weighing 15g of ethyl acrylate, 33g of butyl acrylate, 2.5g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile, 50g of ethyl acetate and 1g of dimethylaminoethyl acrylate, and uniformly mixing to form a monomer mixed liquid base material.
Step two, accurately weighing 15g of ethyl acrylate, 32g of butyl acrylate, 2.5g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile and 50g of ethyl acetate, and uniformly mixing to form monomer mixed liquid drop for feeding.
Heating and stirring the reaction container, adding the monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding the monomer mixed liquid bottom material into a constant-pressure dropping funnel, and dropwise adding the monomer mixed liquid bottom material after the bottom material starts to react and is cooled and refluxed for 2 hours; wherein the stirring rate is 150r/min, and the reaction temperature is 80 ℃.
Fourthly, after all the monomer mixed solution is dripped, preserving heat and reacting for 2 hours;
and fifthly, adding 0.1g of azodiisobutyronitrile, continuously preserving heat for 3 hours, and cooling and discharging.
Step six, weighing the discharged material, toluene diisocyanate and the tri-polymer thereof according to the mass ratio of 1: mixing evenly in a proportion of 0.025, coating, and curing for 5min at 120 ℃ to form the optical pressure-sensitive adhesive for the high-transmittance foldable screen.
Embodiment III:
the optical pressure-sensitive adhesive for the high-light-transmission foldable screen in the embodiment comprises the following components in parts by weight: 96g of butyl acrylate, 4g of hydroxybutyl acrylate, 0.3g of azobisisobutyronitrile and 100g of ethyl acetate. Toluene diisocyanate and its triple polymer 2g. The component B consists of the following components in parts by weight: 1g of 2, 2-dimethylolbutyric acid.
The preparation process of the optical pressure-sensitive adhesive for the high-transmittance foldable screen in the embodiment is as follows:
firstly, accurately weighing 48g of butyl acrylate, 2g of hydroxybutyl acrylate, 0.1g of azodiisobutyronitrile, 50g of ethyl acetate and 1g of 2, 2-dihydroxymethyl butyric acid, and uniformly mixing to form a monomer mixed liquid base material.
Step two, accurately weighing 48g of butyl acrylate, 2g of hydroxybutyl acrylate, 0.1g of azodiisobutyronitrile and 50g of ethyl acetate, and uniformly mixing to form monomer mixed liquid drop for feeding.
Heating and stirring the reaction container, adding the monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding the monomer mixed liquid bottom material into a constant-pressure dropping funnel, and dropwise adding the monomer mixed liquid bottom material after the bottom material starts to react and is cooled and refluxed for 2 hours; wherein the stirring rate is 150r/min, and the reaction temperature is 78 ℃.
Fourthly, after all the monomer mixed solution is dripped, preserving heat and reacting for 2 hours;
and fifthly, adding 0.1g of azodiisobutyronitrile, continuously preserving heat for 3 hours, and cooling and discharging.
Step six, weighing the discharged material, toluene diisocyanate and the tri-polymer thereof according to the mass ratio of 1: and (3) uniformly mixing the components in a proportion of 0.02, coating, and curing for 5min at 120 ℃ to form the optical pressure-sensitive adhesive for the high-transmittance foldable screen.
Embodiment four:
the optical pressure-sensitive adhesive for the high-light-transmission foldable screen in the embodiment comprises the following components in parts by weight: 40g of isooctyl acrylate, 55g of butyl acrylate, 5g of hydroxybutyl acrylate, 0.2g of azobisisobutyronitrile, 100g of ethyl acetate and 2.5g of diphenylmethane diisocyanate. The component B consists of the following components in parts by weight: dimethylaminoethyl acrylate 1g.
The preparation process of the optical pressure-sensitive adhesive for the high-transmittance foldable screen in the embodiment is as follows:
step one, accurately weighing 20g of isooctyl acrylate, 23g of butyl acrylate, 2.5g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile, 50g of ethyl acetate and 1g of dimethylaminoethyl acrylate, and uniformly mixing to form a monomer mixed liquid bottom material.
Step two, accurately weighing 20g of isooctyl acrylate, 22g of butyl acrylate, 2.5g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile and 50g of ethyl acetate, and uniformly mixing to form monomer mixed liquid drop for feeding.
Heating and stirring the reaction container, adding the monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding the monomer mixed liquid bottom material into a constant-pressure dropping funnel, and dropwise adding the monomer mixed liquid bottom material after the bottom material starts to react and is cooled and refluxed for 2 hours; wherein the stirring rate is 150r/min, and the reaction temperature is 80 ℃.
Fourthly, after all the monomer mixed solution is dripped, preserving heat and reacting for 2 hours;
and fifthly, adding 0.1g of azodiisobutyronitrile, continuously preserving heat for 3 hours, and cooling and discharging.
Step six, weighing the discharged materials and diphenylmethane diisocyanate according to the mass ratio of 1: mixing evenly in a proportion of 0.025, coating, and curing for 5min at 120 ℃ to form the optical pressure-sensitive adhesive for the high-transmittance foldable screen.
Fifth embodiment:
the optical pressure-sensitive adhesive for the high-light-transmission foldable screen in the embodiment comprises the following components in parts by weight: isooctyl acrylate 20g, butyl acrylate 76g, hydroxybutyl acrylate 4g, azobisisobutyronitrile 0.15g, ethyl acetate 100g, diphenylmethane diisocyanate 2g. The component B consists of the following components in parts by weight: 2g of 2, 2-dimethylolbutyric acid.
The preparation process of the optical pressure-sensitive adhesive for the high-transmittance foldable screen in the embodiment is as follows:
firstly, accurately weighing 10g of isooctyl acrylate, 38g of butyl acrylate, 2g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile, 50g of ethyl acetate and 0.2g of 2, 2-dihydroxymethylbutanoic acid, and uniformly mixing to form a monomer mixed solution base material.
Step two, accurately weighing 10g of isooctyl acrylate, 38g of butyl acrylate, 2g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile and 50g of ethyl acetate, and uniformly mixing to form monomer mixed liquid drop for feeding.
Heating and stirring the reaction container, adding the monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding the monomer mixed liquid bottom material into a constant-pressure dropping funnel, and dropwise adding the monomer mixed liquid bottom material after the bottom material starts to react and is cooled and refluxed for 2 hours; wherein the stirring rate is 130r/min, and the reaction temperature is 80 ℃.
Fourthly, after all the monomer mixed solution is dripped, preserving heat and reacting for 2 hours;
and fifthly, adding 0.05g of azodiisobutyronitrile, continuously preserving heat for 3 hours, and cooling and discharging.
Step six, weighing the discharged materials and diphenylmethane diisocyanate according to the mass ratio of 1: and (3) uniformly mixing the components in a proportion of 0.02, coating, and curing for 5min at 120 ℃ to form the optical pressure-sensitive adhesive for the high-transmittance foldable screen.
Example six:
the optical pressure-sensitive adhesive for the high-light-transmission foldable screen in the embodiment comprises the following components in parts by weight: 94g of butyl acrylate, 6g of hydroxybutyl acrylate, 0.15g of azodiisobutyronitrile, 100g of ethyl acetate, 3g of toluene diisocyanate and a terpolymer thereof. The component B consists of the following components in parts by weight: dimethylaminoethyl acrylate 2g.
The preparation process of the optical pressure-sensitive adhesive for the high-transmittance foldable screen in the embodiment is as follows:
step one, accurately weighing 47g of butyl acrylate, 3g of hydroxybutyl acrylate, 0.05g of azodiisobutyronitrile, 50g of ethyl acetate and 2g of dimethylaminoethyl acrylate, and uniformly mixing to form a monomer mixed liquid base material.
Step two, accurately weighing 47g of butyl acrylate, 3g of hydroxybutyl acrylate, 0051g of azodiisobutyronitrile and 50g of ethyl acetate, and uniformly mixing to form monomer mixed liquid drop for feeding.
Heating and stirring the reaction container, adding the monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding the monomer mixed liquid bottom material into a constant-pressure dropping funnel, and dropwise adding the monomer mixed liquid bottom material after the bottom material starts to react and is cooled and refluxed for 2 hours; wherein the stirring rate is 130r/min, and the reaction temperature is 80 ℃.
Fourthly, after all the monomer mixed solution is dripped, preserving heat and reacting for 2 hours;
and fifthly, adding 0.05g of azodiisobutyronitrile, continuously preserving heat for 3 hours, and cooling and discharging.
Step six, weighing the discharged material, toluene diisocyanate and the tri-polymer thereof according to the mass ratio of 1: mixing uniformly in a proportion of 0.06, coating, and curing for 5min at 120 ℃ to form the high-light-transmittance foldable screen optical pressure-sensitive adhesive.
Comparative example:
the composite material consists of the following components in parts by weight: 30g of isooctyl acrylate, 70g of butyl acrylate, 2g of acrylic acid, 0.5g of azodiisobutyronitrile, 100g of ethyl acetate, 1g of toluene diisocyanate and a terpolymer thereof.
The preparation method comprises the following steps:
step one, accurately weighing 15g of isooctyl acrylate, 35g of butyl acrylate, 1g of acrylic acid, 0.2g of azodiisobutyronitrile and 50g of ethyl acetate, and uniformly mixing to form a monomer mixed liquid base material.
Step two, accurately weighing 15g of isooctyl acrylate, 35g of butyl acrylate, 1g of acrylic acid, 0.2g of azodiisobutyronitrile and 50g of ethyl acetate, and uniformly mixing to form monomer mixed liquid drop for feeding.
Heating and stirring the reaction container, adding the monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding the monomer mixed liquid bottom material into a constant-pressure dropping funnel, and dropwise adding the monomer mixed liquid bottom material after the bottom material starts to react and is cooled and refluxed for 2 hours; wherein the stirring rate is 130r/min and the reaction temperature is 85 ℃.
Fourthly, after all the monomer mixed solution is dripped, preserving heat and reacting for 2 hours;
and fifthly, adding 0.1g of azodiisobutyronitrile, continuously preserving heat for 3 hours, and cooling and discharging.
Step six, weighing the discharged material, toluene diisocyanate and the tri-polymer thereof according to the mass ratio of 1: mixing uniformly in a proportion of 0.005, coating, and curing for 5min at 120 ℃ to form the optical pressure-sensitive adhesive for the high-transmittance foldable screen.
Performance test:
light transmittance test: and (3) adopting a spectrophotometer, setting the wavelength to be 550nm, cutting the prepared OCA pressure-sensitive adhesive film into strips with the length of 40mm and the width of 10mm, and putting the strips into grooves of the spectrophotometer in groups for light transmittance measurement.
Folding endurance test: and (3) testing by using a YUASA bending-resistant machine, preparing a sample with the width of 2.5cm and the length of 6cm, fixing the sample at the speed of 30r/min, setting the frequency of 10w times, starting the test, and observing whether peeling, breaking, whitening and the like occur on the sample after the test is finished.
Peel strength test: and testing 180-degree peeling strength by adopting a tensile machine, cutting the prepared OCA pressure-sensitive adhesive film into strips with the length of 170mm and the width of 25mm, pasting the strips on a glass sheet to serve as a sample, pasting the sample on the middle position of a steel plate parallel to the longitudinal direction of the plate, rolling for 3 times by using a rolling device, standing for 20min, and testing.
The high light transmission foldable screens obtained in examples one to six were subjected to performance tests with an optical pressure sensitive adhesive and a comparative example, and the results are shown in the following table:
| transmittance of light | Molecular weight (Mn) | Folding endurance (secondary) | Peel strength/N/25 mm | |
| Example 1 | 98％ | 404216 | 12w | 14 |
| Example 2 | 98％ | 484536 | 14w | 15 |
| Example 3 | 97％ | 454628 | 14w | 12 |
| Example 4 | 98％ | 353759 | 11w | 16 |
| Example 5 | 99％ | 424056 | 12w | 15 |
| Example 6 | 99％ | 535206 | 15w | 11 |
| Comparative example | 88％ | 86038 | 5000 | 7 |
As can be seen from the results of the examples and the comparative examples, the optical pressure-sensitive adhesive for the high-light-transmittance foldable screen prepared by the invention has obviously improved light transmittance, is more excellent than the optical performance of the common OCA pressure-sensitive adhesive, has higher mechanical property due to the improvement of molecular weight, and completely reaches the use standard of the foldable screen in bending times. The comprehensive performance meets the performance requirement of the foldable screen on the optical pressure-sensitive adhesive, and has wide market application prospect in the field of flexible electronics.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. An optical pressure sensitive adhesive for a high light transmission foldable screen, comprising:
the component A comprises the following components in parts by weight:
94-100 parts of acrylic ester soft monomer,
2-6 parts of functional monomer,
0.3 to 0.5 part of initiator,
100 parts of a solvent, namely a solvent,
1-3 parts of isocyanate monomer and mixture thereof;
component B:
1-2 parts of amine-containing reducer.
2. The optical pressure-sensitive adhesive for a high-transmittance foldable screen according to claim 1, wherein the acrylic acid ester soft monomer is one or more of ethyl acrylate, isooctyl acrylate and n-butyl acrylate.
3. The optical pressure-sensitive adhesive for a high light transmittance foldable screen according to claim 1, wherein the functional monomer is one or more of acrylic acid, hydroxyethyl acrylate and hydroxybutyl acrylate.
4. The optical pressure-sensitive adhesive for a high light transmission foldable screen according to claim 1, wherein the initiator is azobisisobutyronitrile.
5. The optical pressure-sensitive adhesive for a high light transmission foldable screen according to claim 1, wherein the solvent is ethyl acetate.
6. The optical pressure-sensitive adhesive for high light transmittance foldable screen according to claim 1, wherein the isocyanate monomer and the mixture thereof are one or two of toluene diisocyanate and its tri-polymer, diphenylmethane diisocyanate.
7. The optical pressure-sensitive adhesive for high light transmittance foldable screen according to claim 1, wherein the amine-containing reducing agent is one or two of dimethylaminoethyl acrylate and 2, 2-dihydroxymethylbutanoic acid,
wherein, the molecular structural formula of the dimethylaminoethyl acrylate is as follows:
the molecular structural formula of the 2, 2-dihydroxymethyl butyric acid is as follows:
8. a method for preparing the optical pressure-sensitive adhesive for a high light transmittance foldable screen according to any one of claims 1 to 7, comprising the steps of:
step one: weighing part of acrylic ester soft monomers, part of functional monomers, part of initiator and part of solvent in the component A, and uniformly mixing with the component B to form a monomer mixed solution bottom material;
step two: uniformly mixing the rest acrylic ester soft monomer, the functional monomer, part of initiator and solvent to form monomer mixed liquid drop for feeding;
step three: heating and stirring a reaction container, adding a monomer mixed liquid bottom material into the reaction container after the system is heated to a set temperature, adding monomer mixed liquid drops into a constant-pressure dropping funnel, and dropwise adding after the bottom material starts to react and is cooled and refluxed for 2-4 hours;
step four: after all the monomer mixed solution is dripped, preserving heat and reacting for 1-2h;
step five: adding the rest initiator, keeping the temperature for 2-4 hours, and cooling and discharging;
step six: mixing the discharged material from the fifth step with isocyanate monomer and the mixture thereof according to the mass ratio of 1: mixing uniformly in a proportion of 0.01-0.06, coating, and curing for 5min at 120 ℃ to form the optical pressure-sensitive adhesive for the high-light-transmittance foldable screen.
9. The method for preparing an optical pressure-sensitive adhesive for a high light transmittance foldable screen as claimed in claim 8, wherein in the third step, the stirring rate is 130-150r/min and the reaction temperature is 78-85 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311005342.8A CN116836655A (en) | 2023-08-10 | 2023-08-10 | Optical pressure-sensitive adhesive for high-light-transmittance foldable screen and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311005342.8A CN116836655A (en) | 2023-08-10 | 2023-08-10 | Optical pressure-sensitive adhesive for high-light-transmittance foldable screen and preparation method thereof |
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| CN (1) | CN116836655A (en) |
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