CN111285961A - Optical acrylic adhesive, preparation method thereof and optical film - Google Patents
Optical acrylic adhesive, preparation method thereof and optical film Download PDFInfo
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- CN111285961A CN111285961A CN202010214839.0A CN202010214839A CN111285961A CN 111285961 A CN111285961 A CN 111285961A CN 202010214839 A CN202010214839 A CN 202010214839A CN 111285961 A CN111285961 A CN 111285961A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/24—Homopolymers or copolymers of amides or imides
- C09J133/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2433/00—Presence of (meth)acrylic polymer
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- 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
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention discloses an optical acrylic adhesive, which belongs to the technical field of adhesives and at least comprises the following raw materials: acrylic monomers, initiators and solvents; wherein the acrylic monomers include: acrylic acid soft monomer, acrylic acid hard monomer and acrylic acid functional monomer; based on 100 parts by weight of the acrylic acid monomer, 30-60 parts by weight of the acrylic acid soft monomer, 30-50 parts by weight of the acrylic acid hard monomer and 10-30 parts by weight of the acrylic acid functional monomer are added; at least one of the acrylic soft monomer and the acrylic functional monomer should contain a hydrophilic group. The adhesive provided by the invention has the advantages of no acid, high viscosity and antistatic performance; when the adhesive is applied to an optical film, the peeling force can reach more than 1500 gf/inch.
Description
Technical Field
The invention belongs to the technical field of adhesives, and relates to an optical acrylic adhesive, a preparation method thereof and an optical film.
Background
In recent years, with the development of applications of electronic products, optical OCAs, optical rupture films, and optical double-sided tapes have been increasingly used for adhesion protection of materials such as electronic components. The sticky tape produces and stores static easily in the transportation use, and static not only can adsorb a large amount of dust, still can damage electronic components, causes the short circuit, and static accumulation can produce a series of harm to a certain extent moreover, causes bigger loss. The metal parts of the electronic components are easily corroded by acid, so the adhesive tape cannot contain acid.
The glue is a high molecular polymer, generally an insulator, and the antistatic property of the glue is mainly increased by the following methods: firstly, inorganic fillers with conductive capability, such as conductive carbon black, metal fillers and the like are added into the glue, and the fillers have influence on the light transmittance of products and are difficult to disperse; secondly, small molecular substances with certain antistatic ability, such as surfactants with strong water absorption capacity, certain ionic liquids, lithium salts and the like are added into the glue, but the substances all face the problem of compatibility with the glue and are greatly influenced by humidity.
In addition, most of the prior antistatic optical films mainly comprise a medium-low viscosity protective film with the viscosity of 1-300gf/inch, and the viscosity is difficult to reach more than 1000gf/inch by the prior art; therefore, the market is not available for highly viscous optical films.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide an optical acrylic adhesive which has the characteristics of no acid, static resistance and high viscosity, and when the optical acrylic adhesive is applied to an optical film, the stripping force can reach more than 1500gf/inch, so that the market vacancy is filled.
In addition, the inventor finds out in experiments that the OCA optical glue can be made to have antistatic property by adding the hydrophilic monomer, and the antistatic effect and the proportion of the hydrophilic monomer are in a direct proportion relation in a certain range.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in a first aspect, the invention discloses an optical acrylic adhesive, which at least comprises the following raw materials in parts by weight: acrylic monomers, initiators and solvents; the acrylic monomers include: acrylic acid soft monomer, acrylic acid hard monomer and acrylic acid functional monomer; based on 100 parts by weight of the acrylic acid monomer, 30-60 parts by weight of the acrylic acid soft monomer, 30-50 parts by weight of the acrylic acid hard monomer and 10-30 parts by weight of the acrylic acid functional monomer. Wherein at least one of the acrylic soft monomer and the acrylic functional monomer should contain a hydrophilic monomer.
Further, the optical acrylic adhesive provided by the invention is characterized in that the acrylic soft monomer is one or two of alkyl acrylate and alkyl methacrylate with the glass transition temperature of less than-30 ℃.
Further, the optical acrylic adhesive of the present invention, the acrylic soft monomer comprises: one or more of butyl acrylate, butyl methacrylate and isooctyl acrylate.
Further, according to the optical acrylic adhesive, the acrylic soft monomer further comprises alkoxy acrylate, and the alkoxy acrylate accounts for 5% -10% of the total amount of the acrylic monomers in percentage by weight.
Further, the optical acrylic adhesive provided by the invention is characterized in that the acrylic hard monomer is one or two of acrylic alkyl ester and methacrylic alkyl ester with the glass transition temperature of more than-30 ℃.
Further, the optical acrylic adhesive of the present invention comprises the following acrylic hard monomers: one or more of methyl acrylate, methyl methacrylate, isobornyl acrylate, isobornyl methacrylate, acrylamide and acryloyl morpholine.
Further, according to the optical acrylic adhesive, the acrylic functional monomer is an acrylic functional monomer containing hydroxyl or amino groups; the method comprises the following steps: one or more of hydroxyethyl acrylate, hydroxybutyl acrylate, hydroxypropyl acrylate and acrylamide.
Further, according to the optical acrylic adhesive, the initiator is one or more of azobisisobutyronitrile, azo-bis-valeronitrile, azodiisobutyronitrile and dimethyl azodiisobutyrate.
Further, the solvent of the optical acrylic adhesive is one or more of ethyl acetate, toluene and butanone.
Furthermore, the optical acrylic adhesive also contains an antistatic agent; the antistatic agent is polythiophene or lithium salt antistatic agent.
In a second aspect, the invention also discloses a preparation method of the optical acrylic adhesive, which is used for preparing the optical acrylic adhesive in the first aspect, wherein each raw material component is prepared according to the components in the first aspect; the preparation method comprises the following preparation steps:
the method comprises the following steps: putting an acrylic acid soft monomer, an acrylic acid hard monomer, an acrylic acid functional monomer and all solvents into a reaction container, introducing nitrogen and continuously stirring, stirring for 20 minutes at the temperature of 66 ℃, then adding a first-stage initiator, and keeping the reaction temperature for 3 hours;
step two: adding a second-stage initiator, and continuously stirring at the temperature of 75 ℃ to keep the reaction temperature for 1.5 hours;
step three: adding a third section of initiator, continuously stirring and keeping the reaction temperature for 3 hours at the temperature of 78 ℃, and then cooling; and obtaining the optical acrylic adhesive.
Further, in the preparation method of the optical acrylic adhesive, the first-stage initiator accounts for 15% -25% of the total amount of the initiator; the second stage initiator accounts for 35 to 45 percent of the total amount of the initiator; the third stage initiator accounts for 35-45% of the total amount of the initiator.
In a third aspect, the present disclosure discloses an optical film comprising: the optical acrylic adhesive comprises a PET (polyethylene terephthalate) base film, an optical acrylic adhesive layer coated on the PET base film and a release film; the optical acrylic adhesive layer is prepared by coating the optical acrylic adhesive of the first aspect; the optical acrylic adhesive is prepared by the preparation method of the second aspect.
With the optical film disclosed by the invention, when the thickness of the PET base film is 50 μm and the thickness of the optical acrylic adhesive layer is 25 μm, the stripping force of the optical film reaches more than 1500 gf/inch.
Compared with the prior art, the invention has the advantages that:
1. no acid; in the adhesive provided by the invention, acrylic monomers, initiators, solvents and antistatic liquid do not contain acid groups, so that the requirement of market application of electronic components can be met;
2. both antistatic property and high viscosity are taken into consideration; under the condition that an antistatic agent is not added into the adhesive provided by the invention, the adhesive has good antistatic performance, and the antistatic effect is better when matched with an antistatic liquid; the invention selects and uses soft monomer, hard monomer and functional monomer, the stripping force of the optical film can reach more than 1500 gf/inch;
3. the stability is strong, and the weather resistance is good; the invention does not adopt tackifying resin, has no compatibility problem, no yellowing problem, good weather resistance and excellent optical performance.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the prior art, because the antistatic adhesive tape mainly comprises an adhesive tape with medium and low viscosity, high viscosity is difficult to achieve, and along with the continuous updating and upgrading of electronic products, an optical film is required to have antistatic and perennial properties in some application occasions; in response to the market demand, the present inventors have conducted long-term research, and in continuous experimental research, it was found that the antistatic performance of the glue can be improved by adding a hydrophilic monomer to the glue, and the antistatic effect is proportional to the content of the hydrophilic monomer within a certain range.
Based on the above findings, the inventors have proposed the present invention for filling the gap of the market.
Firstly, the invention provides an optical acrylic adhesive, which at least comprises the following raw materials: acrylic monomers, initiators and solvents; the component contents of the raw materials can be properly adjusted according to different application requirements, and the invention is not elaborated in detail. But it should be noted that: the acrylic monomers in the present invention should include: acrylic acid soft monomer, acrylic acid hard monomer and acrylic acid functional monomer; wherein, the content of each monomer is calculated by 100 parts by weight of acrylic acid monomer, the acrylic acid soft monomer accounts for 30-60 parts by weight, the acrylic acid hard monomer accounts for 30-50 parts by weight, and the acrylic acid functional monomer accounts for 10-30 parts by weight. At least one of the soft monomer and the functional group-containing monomer should contain a hydrophilic group.
The acrylic acid soft monomer is one or two of acrylic acid alkyl ester and methacrylic acid alkyl ester with the glass transition temperature of less than-30 ℃; the method specifically comprises the following steps: one or more of butyl acrylate, butyl methacrylate and isooctyl acrylate.
More preferably, the acrylic soft monomer provided by the invention further comprises alkoxy acrylate, wherein the alkoxy acrylate accounts for 3-15% of the total amount of the acrylic monomers by weight percentage, and preferably 5-10%; the alkoxy acrylates of the present invention include, but are not limited to, the following: 2 (2-ethoxyethoxy) ethyl acrylate, methoxyethyl acrylate, methoxypolyethylene glycol monoacrylate, methoxypolyethylene glycol monomethacrylate; preferably: 2- (2-ethoxyethoxy) ethyl acrylate.
The acrylic hard monomer is one or more of acrylic acid alkyl ester and methacrylic acid alkyl ester with the glass transition temperature of more than-30 ℃; the method specifically comprises the following steps: one or more of methyl acrylate, methyl methacrylate, isobornyl acrylate, isobornyl methacrylate, acrylamide and acryloyl morpholine. Preferably: methyl acrylate, isoborneol acrylate and acrylamide.
The acrylic functional monomer is an acrylic functional monomer containing a hydroxyl group or an amino group; the method specifically comprises the following steps: one or more of hydroxyethyl acrylate, hydroxybutyl acrylate, hydroxypropyl acrylate and acrylamide; preferably: hydroxyethyl acrylate and acrylamide.
As the above initiator, it is one or more of azobisisobutyronitrile, azobisisovaleronitrile and dimethyl azobisisobutyrate. Preferably: azobisisobutyronitrile.
The solvent is one or more of ethyl acetate, toluene and butanone; preferably ethyl acetate is used in combination with butanone.
In addition, the inventor also finds that the optical acrylic adhesive can be matched with an antistatic agent to ensure that the antistatic effect is better; therefore, the adhesive can also contain an antistatic agent; wherein the antistatic agent is polythiophene or lithium salt antistatic agent; preferably a polythiophene-based antistatic agent; the invention specifically selects the following components: chemical Deordor chemical HN-TAC-16.
The invention further provides a preparation method of the optical acrylic adhesive, which is used for preparing the optical acrylic adhesive, wherein the raw material components are prepared according to the method; the preparation method specifically comprises the following preparation steps:
the method comprises the following steps: putting an acrylic acid soft monomer, an acrylic acid hard monomer, an acrylic acid functional monomer and all solvents into a reaction container, introducing nitrogen and continuously stirring, stirring for 20 minutes at the temperature of 66 ℃, then adding a first-stage initiator, and keeping the reaction temperature for 3 hours;
step two: adding a second-stage initiator, and continuously stirring at the temperature of 75 ℃ to keep the reaction temperature for 1.5 hours;
step three: adding a third section of initiator, continuously stirring and keeping the reaction temperature for 3 hours at the temperature of 78 ℃, and then cooling; and obtaining the optical acrylic adhesive.
Wherein, the initiator can be used singly, or can be added in stages, but it is worth noting that: the first stage initiator accounts for 15-25% of the total amount of the initiator; the second stage initiator accounts for 35 to 45 percent of the total amount of the initiator; the third stage initiator accounts for 35 to 45 percent of the total amount of the initiator; preferably: the first stage initiator accounts for 20% of the total amount of the initiator; the second stage initiator accounts for 40% of the total amount of the initiator; the third stage initiator accounts for 40 percent of the total amount of the initiator.
The adhesive provided by the invention can be widely applied to: the present invention will be described in detail below with reference to an optical protective film as an example in order to emphasize the practical effects of the present invention while considering high adhesion and antistatic performance in the fields of optical tapes, OCA optical protective films, OCA optical adhesive films, and the like, but the present invention is not limited to the field of the optical protective films.
The invention provides an optical film, which mainly comprises: the optical acrylic adhesive comprises a PET (polyethylene terephthalate) base film, an optical acrylic adhesive layer coated on the PET base film and a release film; the optical acrylic adhesive layer is prepared by coating the optical acrylic adhesive; the optical acrylic adhesive is prepared by adopting the preparation method of the optical acrylic adhesive;
for the optical film disclosed by the invention, when the thickness of the PET base film is 50 μm and the thickness of the optical acrylic adhesive layer is 25 μm, the stripping force of the optical film reaches more than 1500gf/inch under the condition of ensuring good antistatic effect.
To illustrate the technical effects of the present invention in more detail, the following embodiments are described:
example 1:
50 parts by weight of butyl acrylate, 15 parts by weight of isobornyl acrylate, 10 parts by weight of hydroxyethyl acrylate, 13 parts by weight of methyl acrylate, 2 parts by weight of acrylamide, 10 parts by weight of 2- (2-ethoxyethoxy) ethyl acrylate, 80 parts by weight of ethyl acetate and 20 parts by weight of butanone are put into a reactor. Introducing nitrogen, stirring for 20 minutes, removing air in the reactor, ensuring the temperature to be 66 ℃, then adding 0.1 part by weight of azobisisobutyronitrile, and reacting for 3 hours; then adding 0.2 weight part of azodiisobutyronitrile, and ensuring the temperature to be 75 ℃ for reaction for 1.5 hours; and finally, adding 0.2 weight part of azodiisobutyronitrile, ensuring the temperature to be 78 ℃ for reaction for 3 hours, and then cooling to obtain the optical acrylic adhesive.
Example 2:
50 parts by weight of isooctyl acrylate, 20 parts by weight of isoborneol acrylate, 30 parts by weight of hydroxyethyl acrylate, 80 parts by weight of ethyl acetate and 20 parts by weight of butanone are added into a reactor. Introducing nitrogen, stirring for 20 minutes, removing air in the reactor, ensuring the temperature to be 66 ℃, then adding 0.1 part by weight of azobisisobutyronitrile, and reacting for 3 hours; then adding 0.2 weight part of azodiisobutyronitrile, and ensuring the temperature to be 75 ℃ for reaction for 1.5 hours; and finally, adding 0.2 weight part of azodiisobutyronitrile, ensuring the temperature to be 78 ℃ for reaction for 3 hours, and then cooling to obtain the optical acrylic adhesive.
Example 3:
45 parts by weight of butyl acrylate, 15 parts by weight of isobornyl acrylate, 30 parts by weight of hydroxyethyl acrylate, 10 parts by weight of 2 (2-ethoxyethoxy) ethyl acrylate, 80 parts by weight of ethyl acetate and 20 parts by weight of butanone are added into a reactor. Introducing nitrogen, stirring for 20 minutes, removing air in the reactor, ensuring the temperature to be 66 ℃, then adding 0.1 part by weight of azobisisobutyronitrile, and reacting for 3 hours; then adding 0.2 weight part of azodiisobutyronitrile, and ensuring the temperature to be 75 ℃ for reaction for 1.5 hours; and finally, adding 0.2 weight part of azodiisobutyronitrile, ensuring the temperature to be 78 ℃ for reaction for 3 hours, and then cooling to obtain the optical acrylic adhesive.
Inventive examples 1-3 and comparative examples are compared in the following comparative manner using conditions 1 and 2, wherein:
condition 1: the examples 1 to 3 were mixed with a desired isocyanate curing agent (AH 2400, Eat Korea), coated on 50um PET/50um antistatic PET substrates, respectively, with a thickness of 25um, baked at 120 ℃ for 2min, and then laminated with 50um release films.
After 72h at 45 ℃, standing in an environment with the temperature of 23 +/-1 ℃ and the humidity of 50 +/-5% for 1h, and testing the stripping force, the antistatic value, the light transmittance and the normal temperature retention.
Condition 2. the resin compositions of examples 1 to 3 were mixed with the required isocyanate curing agent (Korea AH2400) and antistatic agent HN-TAC-16 (Dride chemical), respectively coated on 50um PET/50um antistatic PET substrates, and then bonded with 50um release films after being baked at 120 ℃ for 2min, with a thickness of 25 um.
After 72h at 45 ℃, standing in an environment with the temperature of 23 +/-1 ℃ and the humidity of 50 +/-5% for 1h, and testing the stripping force, the antistatic value, the light transmittance and the normal temperature retention.
The peeling force, antistatic value, light transmittance and room temperature holding power in the above conditions 1 and 2 were tested by the following test methods:
peel force test method: according to the standard of ASMTD3330, the adhesive tape is cut into strips with the width of 24.5mm, the strips are stood at the temperature of 23 +/-1 ℃ and the humidity of 50 +/-5 percent, a 340-degree steel plate is attached, a 2kg compression roller is used for rolling back and forth for 2 times at the speed of 300mm/min, and the 180-degree stripping force is tested after 20 min.
The antistatic value test method comprises the following steps: the antistatic value of the surface of the sample was measured by a TR-1000 antistatic meter in accordance with ASTM D-257.
The light transmittance test method comprises the following steps: the light transmittance haze of the adhesive tape was measured by a transmittance tester according to ASTM D1003.
The normal temperature retention test method comprises the following steps: according to the GB/T4851-2014 standard, the adhesive tape is cut into sample strips with the width of 24.5mm, the sample strips are stood at the temperature of 23 +/-1 ℃ and the humidity of 50 +/-5 percent, a 340-mm steel plate is attached, the attachment area is 24.5mm multiplied by 24.5mm, a 1kg weight is hung, and the normal-temperature retention force is tested.
Examples 1-3 were tested according to the test conditions of condition 1 and condition 2 and using the test method criteria described above, and the test results were as follows:
<1> condition 1 test data:
| name (R) | Example 1 | Example 2 | Example 3 |
| Peeling force gf/inch | 1600 | 1600 | 1700 |
| Retention at ambient temperature | Greater than 72 hours | Greater than 72 hours | Greater than 72 hours |
| Light transmittance/haze | 91.6/0.2 | 91.6/0.2 | 91.5/0.2 |
| Antistatic value omega/50 PET | 9.3*e11 | 1.1*e12 | 5.7*e11 |
| Antistatic PET with antistatic value omega/50 | 9*e10 | 9.7*e10 | 4.3*e10 |
<2> condition 2 test data:
in summary, the following steps: the comparison of examples 1 to 3 of the present invention shows that:
the glue prepared in the examples 1-3 has certain antistatic property, and the antistatic effect is in direct proportion to the proportion of hydrophilic monomers contained in the glue. And by matching with antistatic liquid and antistatic PET, the antistatic effect is better on the basis of ensuring the mechanical property of the adhesive tape.
The description and illustrations of the embodiments described herein are intended to provide a general understanding of the structure of various embodiments. The specification and illustrations are not intended to serve as an exhaustive and comprehensive description of all the elements and features of apparatus and systems that utilize the structures or methods described herein. Separate embodiments may also be provided in combination in a single embodiment, and conversely, various features that are, for brevity, described in the context of a single embodiment, may also be provided separately or in any sub-combination. Further, reference to values stated in ranges includes each and every value within that range. Many other embodiments will be apparent to those of skill in the art upon reading this specification only. Other embodiments may be used and derived from the disclosure, such that a structural substitution, logical substitution, or another change may be made without departing from the scope of the disclosure. The present invention is, therefore, to be considered as illustrative and not restrictive.
Claims (13)
1. An optical acrylic adhesive is characterized in that: at least comprises the following raw materials: acrylic monomers, initiators and solvents;
the acrylic monomers include: acrylic acid soft monomer, acrylic acid hard monomer and acrylic acid functional monomer; based on 100 parts by weight of the acrylic acid monomer, 30-60 parts by weight of the acrylic acid soft monomer, 30-50 parts by weight of the acrylic acid hard monomer and 10-30 parts by weight of the acrylic acid functional monomer are added;
wherein at least one of the acrylic soft monomer and the acrylic functional monomer should contain a hydrophilic monomer.
2. The optical acrylic adhesive according to claim 1, wherein: the acrylic acid soft monomer is one or two of acrylic acid alkyl ester and methacrylic acid alkyl ester with the glass transition temperature of less than minus 30 ℃.
3. The optical acrylic adhesive according to claim 2, wherein: the acrylic soft monomer comprises: one or more of butyl acrylate, butyl methacrylate and isooctyl acrylate.
4. The optical acrylic adhesive according to claim 3, wherein: the acrylic soft monomer also comprises alkoxy acrylate, and the alkoxy acrylate accounts for 5-10% of the total amount of the acrylic monomers in percentage by weight.
5. The optical acrylic adhesive according to claim 1, wherein: the acrylic hard monomer is one or two of acrylic acid alkyl ester and methacrylic acid alkyl ester with the glass transition temperature of more than-30 ℃.
6. The optical acrylic adhesive according to claim 5, wherein: the acrylic hard monomer comprises: one or more of methyl acrylate, methyl methacrylate, isobornyl acrylate, isobornyl methacrylate, acrylamide and acryloyl morpholine.
7. The optical acrylic adhesive according to claim 1, wherein: the acrylic acid functional monomer is an acrylic acid functional monomer containing hydroxyl or amino; the method comprises the following steps: one or more of hydroxyethyl acrylate, hydroxybutyl acrylate, hydroxypropyl acrylate and acrylamide.
8. The optical acrylic adhesive according to claim 1, wherein: the initiator is one or more of azobisisobutyronitrile, azobisisovaleronitrile and dimethyl azobisisobutyrate.
9. The optical acrylic adhesive according to claim 1, wherein: the solvent is one or more of ethyl acetate, toluene and butanone.
10. The optical acrylic adhesive according to any one of claims 1 to 9, wherein: the adhesive also contains an antistatic agent; the antistatic agent is polythiophene or lithium salt antistatic agent.
11. A preparation method of an optical acrylic adhesive is characterized by comprising the following steps: the optical acrylic adhesive is used for preparing the optical acrylic adhesive as claimed in claim 1, wherein each raw material component is prepared according to the component as claimed in claim 1; the preparation method comprises the following preparation steps:
the method comprises the following steps: putting an acrylic acid soft monomer, an acrylic acid hard monomer, an acrylic acid functional monomer and all solvents into a reaction container, introducing nitrogen and continuously stirring, stirring for 20 minutes at the temperature of 66 ℃, then adding a first-stage initiator, and keeping the reaction temperature for 3 hours;
step two: adding a second-stage initiator, and continuously stirring at the temperature of 75 ℃ to keep the reaction temperature for 1.5 hours;
step three: adding a third section of initiator, continuously stirring and keeping the reaction temperature for 3 hours at the temperature of 78 ℃, and then cooling; and obtaining the optical acrylic adhesive.
12. The method for preparing an optical acrylic adhesive according to claim 11, wherein: the first-stage initiator accounts for 15% -25% of the total amount of the initiator; the second-stage initiator accounts for 35-45% of the total amount of the initiator; the third-stage initiator accounts for 35-45% of the total amount of the initiator.
13. An optical film, characterized in that: the method comprises the following steps: the optical acrylic adhesive comprises a PET (polyethylene terephthalate) base film, an optical acrylic adhesive layer coated on the PET base film and a release film; the optical acrylic adhesive layer is prepared by coating the optical acrylic adhesive according to claim 1; the optical acrylic adhesive is prepared by the preparation method of claim 11 or 12;
when the thickness of the PET base film is 50 μm and the thickness of the optical acrylic adhesive layer is 25 μm, the peeling force of the optical film reaches 1500gf/inch or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010214839.0A CN111285961A (en) | 2020-03-24 | 2020-03-24 | Optical acrylic adhesive, preparation method thereof and optical film |
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| CN112745786A (en) * | 2021-01-12 | 2021-05-04 | 江苏斯迪克新材料科技股份有限公司 | Optical adhesive with high refractive index and preparation method thereof |
| CN113930175A (en) * | 2021-10-27 | 2022-01-14 | 苏州赛伍应用技术股份有限公司 | Optical AB glue and preparation method and application thereof |
| CN114015389A (en) * | 2021-11-11 | 2022-02-08 | 青岛卓英社科技股份有限公司 | Composite optical membrane and preparation method thereof |
| CN114133898A (en) * | 2021-12-23 | 2022-03-04 | 佛山市领固胶粘科技有限公司 | High-permeability low-sensitization medical pressure-sensitive adhesive and preparation method thereof |
| CN114752323A (en) * | 2022-03-31 | 2022-07-15 | 江苏皇冠新材料科技有限公司 | Acrylate adhesive, adhesive tape and preparation method thereof |
| CN116333653A (en) * | 2023-03-27 | 2023-06-27 | 太仓斯迪克新材料科技有限公司 | OCA optical cement for bonding vehicle-mounted display screen and preparation method thereof |
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| CN114752323A (en) * | 2022-03-31 | 2022-07-15 | 江苏皇冠新材料科技有限公司 | Acrylate adhesive, adhesive tape and preparation method thereof |
| CN116333653A (en) * | 2023-03-27 | 2023-06-27 | 太仓斯迪克新材料科技有限公司 | OCA optical cement for bonding vehicle-mounted display screen and preparation method thereof |
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