CN116023864A - Optical adhesive, adhesive sheet and preparation method thereof - Google Patents
Optical adhesive, adhesive sheet and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of adhesives, and in particular relates to an optical adhesive, an adhesive sheet and a preparation method thereof, comprising the following steps: acrylate copolymer a and acrylate oligomer B; wherein the acrylic ester copolymer A comprises the following copolymer in parts by weight: 50-80 parts of soft monomer; 10-25 parts of polar crosslinkable monomer; 10-25 parts of hard monomer; the weight average molecular weight of the acrylic ester copolymer A is 300000-1000000g/mol; the acrylate oligomer B comprises the following oligomers in parts by weight: 30-60 parts of a cyclic acrylate monomer in a molecule; 40-70 parts of alkyl acrylate monomer containing branched chain or straight chain; the weight average molecular weight of the acrylate oligomer B is 5000-100000g/mol. The invention improves the level difference filling property and the adhesive force in normal temperature and high temperature environment on the basis of higher normal temperature storage modulus, and has good foam inhibition capability in high temperature application.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to an optical adhesive, an adhesive sheet and a preparation method thereof.
Background
With the development of modern society, more and more optical cement is applied to products such as electronic paper, smart phones, tablet computers, vehicle-mounted screens and the like. In these display devices, a protective panel is usually disposed on the surface of the display module. An air layer is arranged between the protection panel and the display module to prevent the protection panel from colliding with the display module when the protection panel is extruded and deformed by external force. However, the display quality is degraded due to the refractive index difference between the display panel, the air layer, and the protective panel.
The prior art thus solves the above-mentioned problems by introducing a layer of optical cement to fill the air layer. Optical adhesives are a special type of adhesives used for cementing transparent optical elements. The adhesive is required to be colorless and transparent, has light transmittance of more than 90%, good cementing strength, can be cured at room temperature or medium temperature, and has the characteristics of small curing shrinkage and the like. The current optical adhesive sheet is a substrate-free double-sided adhesive tape which is prepared by coating an optical adhesive on one release film and covering the upper layer with another release film by heating or illumination. The double-sided adhesive tape can bond the touch control layer and the display layer, thereby eliminating an air layer, improving the display effect and isolating dust and water vapor.
However, the border printed ink layer may create a level difference on the back side of the protective panel. If the optical adhesive layer level difference is poor in filling property, bubbles and light reflection loss are likely to occur between the adhesive layer and the panel due to the floating of the adhesive layer near the ink level difference. In addition, most of the existing protection panels are made of PC/PMMA materials, and water vapor is easy to generate at high temperature, so that the optical adhesive layer has a foaming phenomenon in a high-temperature high-humidity application scene. Therefore, the optical adhesive layer is required to have not only good level difference filling performance, but also good foam inhibition capability in a high-temperature high-humidity scene.
The prior art scheme is to improve the level difference filling property by reducing the glass transition temperature of the optical cement and the storage modulus at normal temperature. The reduction of the glass transition temperature and the storage modulus at normal temperature can improve the level difference filling property of the optical adhesive, but the poor effect is caused by the fact that adhesive overflows easily to pollute the edge of the panel when the protective panel is attached to the display panel; on the other hand, the protective panels are mostly made of PC, PMMA and the like, and are easy to generate water vapor at high temperature and high humidity. The existing optical adhesive is used for improving the level difference filling property, and has lower storage modulus at high temperature, so that bubbles are easy to generate near the level difference under the high-temperature and high-humidity conditions, and water vapor generated by PC or PMMA is less easy to inhibit, so that the adhesive film is foamed.
Disclosure of Invention
The invention provides an optical adhesive, an adhesive sheet and a preparation method thereof, which are used for solving the problem that the storage modulus of the existing optical adhesive is too low.
In order to solve the technical problems, the invention provides an optical adhesive, which comprises the following components: acrylate copolymer a and acrylate oligomer B; wherein the acrylic ester copolymer A comprises the following copolymer in parts by weight: 50-80 parts of soft monomer; 10-25 parts of polar crosslinkable monomer; 10-25 parts of hard monomer; the weight average molecular weight of the acrylic ester copolymer A is 300000-1000000g/mol; the acrylate oligomer B comprises the following oligomers in parts by weight: 30-60 parts of a cyclic acrylate monomer in a molecule; 40-70 parts of alkyl acrylate monomer containing branched chain or straight chain; the weight average molecular weight of the acrylate oligomer B is 5000-100000g/mol; and the mass part ratio of the acrylic ester copolymer A to the acrylic ester oligomer B is 100 parts: 0-10 parts.
In yet another aspect, the present invention also provides a method for preparing the optical adhesive as described above, comprising the steps of: step S1, preparing an acrylate copolymer a, comprising: adding soft monomer, hard monomer and polar crosslinkable monomer into a reaction kettle provided with a reflux device, a thermometer and a stirring device, adding all solvents, heating to 60-70 ℃, introducing nitrogen for 60-80 minutes, adding 0.15-0.4 part of initiator and 0.01-0.2 part of chain transfer agent accounting for the total monomer, reacting for 10-12 hours, and cooling to room temperature to obtain an acrylic ester copolymer A with the solid content of 40-50 wt%; step S2, preparing an acrylate oligomer B, comprising: adding all acrylate monomers into a reaction kettle provided with a reflux device, a thermometer and a stirring device, adding all solvents, heating to 60-70 ℃, introducing nitrogen for 60-80 minutes, adding 0.2-0.8 part of initiator and 0.05-0.5 part of chain transfer agent which account for the total monomer amount, reacting for 4-6 hours, heating to reflux for 2-3 hours, and cooling to room temperature to obtain an acrylate copolymer B with the solid content of 25-35 wt%; and S3, mixing the obtained acrylic ester copolymer A, acrylic ester oligomer B, a cross-linking agent, a silane coupling agent and other auxiliary agents, standing and defoaming to obtain the optical adhesive.
In a third aspect, the present invention also provides an adhesive sheet comprising: an adhesive layer formed of an optical adhesive as described above; and the normal temperature storage modulus of the adhesive sheet is 30-200 KPa.
In a fourth aspect, the present invention also provides a method for producing an adhesive sheet as described above, comprising: and (3) coating the optical adhesive on a release film by using a coating shaft, baking for 5-10 min at 40-120 ℃, then attaching the release film with the thickness of 75um, and standing for 1-5 days at 40-120 ℃ to obtain the adhesive sheet.
The optical adhesive, the adhesive sheet and the preparation method thereof have the beneficial effects that the specific molecular weight range is selected and limited through proper monomer proportion, and the optical adhesive after cross-linking is enabled to have higher normal-temperature storage modulus by being matched with the addition of the oligomer, so that the level difference filling property and the adhesive force of normal-temperature and high-temperature environments are greatly improved, and the optical adhesive has better adhesive effect and good foam inhibition capability in high-temperature application.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
In order to make the above objects, features and advantages of the present invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the preparation of the optical adhesive of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but 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.
The invention provides an optical adhesive, comprising: acrylate copolymer a and acrylate oligomer B; wherein the acrylic ester copolymer A comprises the following copolymer in parts by weight: 50-80 parts of soft monomer; 10-25 parts of polar crosslinkable monomer; 10-25 parts of hard monomer; the weight average molecular weight of the acrylic ester copolymer A is 300000-1000000g/mol; the acrylate oligomer B comprises the following oligomers in parts by weight: 30-60 parts of a cyclic acrylate monomer in a molecule; 40-70 parts of alkyl acrylate monomer containing branched chain or straight chain; the weight average molecular weight of the acrylate oligomer B is 5000-100000g/mol; and the mass part ratio of the acrylic ester copolymer A to the acrylic ester oligomer B is 100 parts: 0-10 parts.
In this embodiment, specifically, the soft monomer in the acrylate copolymer a is one or two of 2-ethylhexyl acrylate, isooctyl methacrylate, butyl acrylate, and dodecyl methacrylate; the polar crosslinkable monomer is one or two of (methyl) acrylic acid, hydroxyethyl (methyl) acrylate, hydroxypropyl (methyl) acrylate and hydroxybutyl acrylate; the hard monomer is one or two of isobornyl (methyl) acrylate, methyl (methyl) acrylate, acrylamide, acryloylmorpholine, N-vinyl pyrrolidone and vinyl acetate.
In this embodiment, specifically, the acrylate monomer containing a cyclic acrylate in the molecule of the acrylate oligomer B is one or two of isobornyl acrylate, isobornyl methacrylate, and tetrahydrofuranyl acrylate, so as to improve interfacial adhesion and foam inhibition capability at high temperature; the alkyl acrylate monomer containing branched chain or straight chain is one or two of methyl methacrylate, ethyl methacrylate and propyl methacrylate.
In this embodiment, specifically, the acrylate copolymer a and the acrylate oligomer B are prepared by solution polymerization; wherein the solvent for solution polymerization is one or more of ethyl acetate, toluene, butanone, butyl acetate and n-hexane; the initiator for the solution polymerization is one or more of azodiisobutyronitrile, dibenzoyl peroxide and azodiisoheptonitrile.
In this embodiment, specifically, the solution polymerization is further added with a chain transfer agent, which is any one of 2-mercaptoethanol, α -thioglycerol, octylmercaptan, dodecylmercaptan, and t-dodecylmercaptan, to adjust the molecular weight of the acrylate copolymer a and the acrylate oligomer B.
In this embodiment, specifically, the solution polymerization is further added with a crosslinking agent, which is any one of an epoxy crosslinking agent, an isocyanate crosslinking agent, an aziridine crosslinking agent, and a metal chelate crosslinking agent, so that the polymer forms a crosslinked structure, and the crosslinked adhesive layer improves the foaming resistance; the mass part ratio of the acrylic ester copolymer A to the cross-linking agent is 100 parts: 0-3 parts; in order to form a crosslinked structure, a crosslinking agent having thermal crosslinking is preferable, the crosslinking temperature is preferably 40 to 120 ℃, and the crosslinking time is controlled to 5 minutes to 5 days.
In the embodiment, specifically, the solution polymerization is further added with a silane coupling agent and an auxiliary agent, and the adhesive force of the adhesive is improved by adding the silane coupling agent; the auxiliary agent comprises an antioxidant and an ultraviolet stabilizer; wherein the mass part ratio of the acrylic copolymer A to the silane coupling agent is 100 parts: 0-2 parts; the mass part ratio of the acrylic ester copolymer A to the auxiliary agent is 100 parts: 0-1 part.
As shown in fig. 1, the invention also provides a preparation method of the optical adhesive, which comprises the following steps: step S1, preparing an acrylate copolymer a, comprising: adding soft monomer, hard monomer and polar crosslinkable monomer into a reaction kettle provided with a reflux device, a thermometer and a stirring device, adding all solvents, heating to 60-70 ℃, introducing nitrogen for 60-80 minutes, adding 0.15-0.4 part of initiator and 0.01-0.2 part of chain transfer agent accounting for the total monomer, reacting for 10-12 hours, and cooling to room temperature to obtain an acrylic ester copolymer A with the solid content of 40-50 wt%; step S2, preparing an acrylate oligomer B, comprising: adding all acrylate monomers into a reaction kettle provided with a reflux device, a thermometer and a stirring device, adding all solvents, heating to 60-70 ℃, introducing nitrogen for 60-80 minutes, adding 0.2-0.8 part of initiator and 0.05-0.5 part of chain transfer agent which account for the total monomer amount, reacting for 4-6 hours, heating to reflux for 2-3 hours, and cooling to room temperature to obtain an acrylate copolymer B with the solid content of 25-35 wt%; and S3, mixing the obtained acrylic ester copolymer A, acrylic ester oligomer B, a cross-linking agent, a silane coupling agent and other auxiliary agents, standing and defoaming to obtain the optical adhesive.
The present invention also provides an adhesive sheet comprising: an adhesive layer formed of an optical adhesive as described above; and the normal temperature storage modulus of the adhesive sheet is 30-200 KPa.
The invention also provides a preparation method of the adhesive sheet, which comprises the following steps: and (3) coating the optical adhesive on a release film by using a coating shaft, baking for 5-10 min at 40-120 ℃, then attaching the release film with the thickness of 75um, and standing for 1-5 days at 40-120 ℃ to obtain the adhesive sheet.
The monomer, initiator, solvent, curing agent, silane coupling agent and other auxiliary agent used in the patent are abbreviated as follows, see table 1:
table 1 raw materials and abbreviations
The raw material formulation of the acrylate oligomer B is shown in Table 2, and the following is a synthetic process by taking example C-1 as an example:
c-1: isobornyl acrylate (IBOA) 40 parts by weight, methyl Methacrylate (MMA) 60 parts by weight, n-dodecyl mercaptan 0.3 parts by weight as a chain transfer agent, and ethyl acetate 200 parts by weight as a polymerization solvent were put into a four-necked flask, and stirred under nitrogen at 65 ℃ for 1 hour. Then, 0.4 parts by weight of azobisisobutyronitrile as a polymerization initiator was charged into a four-necked flask, reacted at 65℃for 4 hours, and then heated to reflux for 2 hours. Thus, acrylic acid acrylate oligomer B was obtained.
The raw material formulation of the polymer A is shown in Table 2, and the following synthesis process is illustrated by taking example D-1 and comparative example E-1 as examples:
d-1: 60 parts of 2-EHA, 20 parts of HEA, 13 parts of NVP, 7 parts of IBOA, 0.1 part by weight of N-dodecyl mercaptan of a chain transfer agent and 150 parts of EtAc are added into a four-neck flask with mechanical stirring, an N2 port, a thermometer and condensed water, the mixture is fully stirred, the temperature is raised to 65 ℃, the nitrogen flow is 0.5/min, 0.2 part of AIBN is added after 60 minutes of nitrogen is introduced, and the mixture is kept at 65 ℃ and is reacted in a nitrogen environment for 10 hours and cooled to room temperature, so that the polymer A is obtained.
E-1: in a four-necked flask equipped with mechanical stirring, an N2 port, a thermometer and condensed water, 75 parts of LMA, 15 parts of HEA, 15 parts of MMA, 0.1 part by weight of N-dodecyl mercaptan of a chain transfer agent and 150 parts of EtAc were added, stirring was sufficient, heating was carried out to 65℃with a nitrogen flow of 0.5/min, and after 60 minutes of nitrogen was introduced, 0.2 part of AIBN was added, and the reaction was maintained at 65℃for 12 hours under a nitrogen atmosphere and cooled to room temperature.
TABLE 2 raw material proportions
| Examples | 2-EHA | BA | LMA | HEA | HPA | NVP | IBOMA | IBOA | MMA | AIBN | NDM | EtAc | MEK | NV |
| C-1 | / | / | / | / | / | / | / | 40 | 60 | 0.4 | 0.3 | 200 | / | 0.33 |
| C-2 | / | / | / | / | / | / | 20 | 20 | 60 | 0.4 | 0.3 | 200 | / | 0.33 |
| C-3 | / | / | / | / | / | / | 20 | 40 | 40 | 0.4 | 0.2 | 100 | 100 | 0.33 |
| D-1 | 60 | / | / | 20 | / | 13 | / | 7 | / | 0.2 | 0.1 | 150 | / | 0.4 |
| D-2 | 70 | / | / | 15 | / | 15 | / | / | / | 0.2 | 0.1 | 150 | / | 0.4 |
| D-3 | 70 | / | / | 15 | / | / | / | 15 | / | 0.2 | 0.1 | 150 | / | 0.4 |
| D-4 | / | 60 | / | 20 | / | 13 | / | 7 | / | 0.2 | 0.1 | 100 | 50 | 0.4 |
| D-5 | / | 60 | / | / | 20 | / | / | 20 | / | 0.2 | 0.1 | 150 | / | 0.4 |
| D-6 | / | / | 60 | / | 20 | / | 20 | / | / | 0.2 | 0.1 | 150 | / | 0.4 |
| E-1 | / | 75 | 15 | / | / | / | / | 15 | 0.2 | 0.1 | 150 | / | 0.4 | |
| E-2 | / | 75 | / | 15 | / | / | / | / | 15 | 0.2 | 0.1 | 100 | 50 | 0.4 |
Preparation of an adhesive sheet:
the adhesive sheet was prepared by mixing, coating and curing the formulations given in table 3, using example 1, and the procedure was as follows:
100 parts of copolymer A, 3 parts of oligomer B, 0.5 part of L-75, 0.5 part of KH550 and 0.2 part of antioxidant 1010 are weighed, fully mixed, and then static defoaming is carried out, the mixture is coated on a release film by using a coating shaft, then the mixture is heated for 5 minutes at 90 ℃, then the mixture is attached to another release film, the thickness of the adhesive film is 150um, and the adhesive film is prepared after being placed for 5 days at 50 ℃.
Table 3 coating formulation
The adhesive sheet thus obtained was subjected to physical properties test, and the test results are shown in Table 4.
1. Thickness of (L)
Placing the adhesive sheet at 25 ℃ and 50% RH standard temperature for 1h, testing the thickness of the adhesive sheet by adopting a Sanfeng film thickness meter, and recording data mu 1; then, the thickness mu 2 of the light film and the heavy film of the adhesive sheet is tested by a film thickness meter; the thickness μ=μ1- μ2 of the adhesive film.
2. Gel fraction
The adhesive sheets obtained in examples and comparative examples were weighed by a precision balance to obtain the film weight m1, and the filter screen weight m2 was weighed by a precision balance to wrap the film. Next, the film coated on the above filter was immersed in acetic acid ethyl acetate at room temperature (25 ℃ C.) for 24 hours. Thereafter, the film wrapping the filter screen was taken out and dried in an oven at 80℃for 4 hours. After drying, its mass m3 was weighed by a precision balance. At this time, the gel fraction was: gel fraction = (m 3-m 2)/m 1 x100%
3. Storage modulus at normal temperature
G' and tan delta in shear were measured using a TA mixer rheometer DHR-2. OCA samples were laminated to 50mm x 50m gauge, 0.1mm ± 0.05mm thickness, and no pucker bubbles, and fabricated into circular samples of diameter phi 8mm using a tooling. Tearing off one surface of the release film from the prepared sample, and attaching the release film to the lower port of the test column; tearing off the release film on the other side of the sample, adjusting a machine, and pressing the sample onto a test table; adjusting test parameters such as test temperature interval, frequency and the like; after clicking the "start" test, the storage modulus G' data was read.
4. 180 ° peel adhesion test:
the samples were cut into 2.5cm wide strips and the test procedure was performed as described in ASTM international standard D3330 method a, test panel being Polycarbonate (PC). After bonding, the test was performed after 20 minutes of standing under the humidity condition of the test thermometer, and the average adhesion force required for tearing the spline off the panel was expressed in gf/25 mm.
5. Level difference filling property
A glass plate with level differences (level difference height: 30 mu, 45 mu) was obtained. The adhesive sheets obtained in examples and comparative examples were peeled off to form light release films, and the exposed adhesive films were bonded to polyethylene terephthalate films (PET, thickness: 100 μm) which had been corona-treated in advance. Then, the heavy release film was peeled off, and the adhesive film was adhered to a glass plate with a step, and this was used as a sample for evaluation.
The sample obtained was subjected to high-pressure defoaming treatment at 60℃and 0.5MPa for 30 minutes, and then left at normal pressure and 23℃and 50% RH for 6 hours. Next, the mixture was stored at 85℃under high temperature and high humidity conditions of 85% RH for 7 days, and then the step-difference filling property was evaluated. The level difference filling property is determined by whether or not the ink printing level difference is completely filled with the adhesive film, and when bubbles, floating, peeling, and the like are observed at the interface between the ink printing level difference and the adhesive film, it is determined that the ink printing level difference is not filled. The level difference filling property was evaluated as a level difference filling rate (%) represented by the following formula. Step filling ratio (%) = (ink step height (μ) at which no bubble, float, peel, etc. state at step after aging test/thickness of adhesive film: 150 μ) X100%
6. High-temperature high-humidity foam inhibition performance
A Polycarbonate (PC) plate with level difference (height of level difference: 30 μm) formed of printing ink was taken. The adhesive sheets obtained in examples and comparative examples were peeled off to form light release films, and the exposed adhesive films were bonded to polyethylene terephthalate films (PET, thickness: 100 μm) which had been corona-treated in advance. Then, the heavy release film was peeled off, and the adhesive film was adhered to a PC board with a step, and this was used as a sample for evaluation.
The sample obtained was subjected to high-pressure defoaming treatment at 60℃and 0.5MPa for 30 minutes, and then left at normal pressure and 25℃and 50% RH for 6 hours. Then, the mixture was stored at 85℃under high temperature and high humidity conditions of 85% RH for 500 hours. And then taking out the sample, standing at the normal temperature of 25 ℃ for 2 hours at 50% RH, cooling to the normal temperature, observing the surface condition of the attached sample, and recording the foaming condition: bubble-free is o; a small amount of foaming was delta; the number of blisters was x.
Table 4 physical properties of the adhesive sheet
As can be seen from table 4: the polymer A synthesized by proper monomer proportion is crosslinked by adding the oligomer B, so that the adhesive film has higher storage modulus at normal temperature, and the adhesive film has excellent section difference filling performance and better inhibition on foaming conditions of high temperature and high humidity.
In summary, the optical adhesive, the adhesive sheet and the preparation method thereof select and limit a specific molecular weight range through proper monomer mixture ratio, and the addition of the oligomer enables the crosslinked optical adhesive to have higher normal-temperature storage modulus, so that the level difference filling property and adhesive force of normal-temperature and high-temperature environments are greatly improved, better adhesive effect is obtained, and meanwhile, the adhesive has good foam inhibition capability in high-temperature application.
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (10)
1. An optical adhesive, comprising:
acrylate copolymer a and acrylate oligomer B; wherein the method comprises the steps of
The acrylic ester copolymer A comprises the following copolymers in parts by weight:
50-80 parts of soft monomer;
10-25 parts of polar crosslinkable monomer;
10-25 parts of hard monomer;
the weight average molecular weight of the acrylic ester copolymer A is 300000-1000000g/mol;
the acrylate oligomer B comprises the following oligomers in parts by weight:
30-60 parts of a cyclic acrylate monomer in a molecule;
40-70 parts of alkyl acrylate monomer containing branched chain or straight chain;
the weight average molecular weight of the acrylate oligomer B is 5000-100000g/mol; and
the mass part ratio of the acrylic ester copolymer A to the acrylic ester oligomer B is 100 parts: 0-10 parts.
2. The optical adhesive of claim 1, wherein the adhesive comprises a polymer,
in the acrylate copolymer A
The soft monomer is one or two of 2-ethylhexyl acrylate, isooctyl methacrylate, butyl acrylate and dodecyl methacrylate;
the polar crosslinkable monomer is one or two of (methyl) acrylic acid, hydroxyethyl (methyl) acrylate, hydroxypropyl (methyl) acrylate and hydroxybutyl acrylate;
the hard monomer is one or two of isobornyl (methyl) acrylate, methyl (methyl) acrylate, acrylamide, acryloylmorpholine, N-vinyl pyrrolidone and vinyl acetate.
3. The optical adhesive of claim 1, wherein the adhesive comprises a polymer,
in the acrylate oligomer B
The acrylic ester monomer containing the cyclic ring in the molecule is one or two of isobornyl acrylate, isobornyl methacrylate and tetrahydrofuranyl acrylate;
the alkyl acrylate monomer containing branched chain or straight chain is one or two of methyl methacrylate, ethyl methacrylate and propyl methacrylate.
4. The optical adhesive of claim 1, wherein the adhesive comprises a polymer,
the acrylic ester copolymer A and the acrylic ester oligomer B are prepared by solution polymerization; wherein the method comprises the steps of
The solvent for the solution polymerization is one or more of ethyl acetate, toluene, butanone, butyl acetate and n-hexane;
the initiator for the solution polymerization is one or more of azodiisobutyronitrile, dibenzoyl peroxide and azodiisoheptonitrile.
5. The optical adhesive of claim 4, wherein the adhesive comprises a polymer,
the solution polymerization is further added with a chain transfer agent which is any one of 2-mercaptoethanol, alpha-thioglycerol, octyl mercaptan, dodecyl mercaptan and tertiary dodecyl mercaptan.
6. The optical adhesive of claim 4, wherein the adhesive comprises a polymer,
the solution polymerization is also added with a cross-linking agent which is any one of an epoxy cross-linking agent, an isocyanate cross-linking agent, an aziridine cross-linking agent and a metal chelate cross-linking agent;
the mass part ratio of the acrylic ester copolymer A to the cross-linking agent is 100 parts: 0-3 parts.
7. The optical adhesive of claim 4, wherein the adhesive comprises a polymer,
the solution polymerization is also added with a silane coupling agent and an auxiliary agent;
the auxiliary agent comprises an antioxidant and an ultraviolet stabilizer; wherein the method comprises the steps of
The mass part ratio of the acrylic ester copolymer A to the silane coupling agent is 100 parts: 0-2 parts;
the mass part ratio of the acrylic ester copolymer A to the auxiliary agent is 100 parts: 0-1 part.
8. A method of preparing the optical adhesive of claim 1, comprising the steps of:
step S1, preparing an acrylate copolymer a, comprising: adding soft monomer, hard monomer and polar crosslinkable monomer into a reaction kettle provided with a reflux device, a thermometer and a stirring device, adding all solvents, heating to 60-70 ℃, introducing nitrogen for 60-80 minutes, adding 0.15-0.4 part of initiator and 0.01-0.2 part of chain transfer agent accounting for the total monomer, reacting for 10-12 hours, and cooling to room temperature to obtain an acrylic ester copolymer A with the solid content of 40-50 wt%;
step S2, preparing an acrylate oligomer B, comprising: adding all acrylate monomers into a reaction kettle provided with a reflux device, a thermometer and a stirring device, adding all solvents, heating to 60-70 ℃, introducing nitrogen for 60-80 minutes, adding 0.2-0.8 part of initiator and 0.05-0.5 part of chain transfer agent which account for the total monomer amount, reacting for 4-6 hours, heating to reflux for 2-3 hours, and cooling to room temperature to obtain an acrylate copolymer B with the solid content of 25-35 wt%;
and S3, mixing the obtained acrylic ester copolymer A, acrylic ester oligomer B, a cross-linking agent, a silane coupling agent and other auxiliary agents, standing and defoaming to obtain the optical adhesive.
9. An adhesive sheet, comprising:
an adhesive layer formed from the optical adhesive of claim 1; and
the normal temperature storage modulus of the adhesive sheet is 30-200 KPa.
10. A method of producing the adhesive sheet according to claim 9, comprising:
the optical adhesive according to claim 1 is coated on a release film by using a coating shaft, baked for 5-10 min at 40-120 ℃, then attached to a 75um thick release film, and placed for 1-5 days at 40-120 ℃ to obtain the adhesive sheet.
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| CN118006261A (en) * | 2024-04-09 | 2024-05-10 | 江苏皇冠新材料科技有限公司 | Acrylic pressure-sensitive adhesive for foldable display screen and adhesive sheet thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118006261A (en) * | 2024-04-09 | 2024-05-10 | 江苏皇冠新材料科技有限公司 | Acrylic pressure-sensitive adhesive for foldable display screen and adhesive sheet thereof |
| CN118006261B (en) * | 2024-04-09 | 2024-06-04 | 江苏皇冠新材料科技有限公司 | Acrylic pressure-sensitive adhesive for foldable display screen and adhesive sheet thereof |
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