CN110527453B - Acrylic copolymer-based adhesive sheet for 5G antenna process - Google Patents
Acrylic copolymer-based adhesive sheet for 5G antenna process Download PDFInfo
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- CN110527453B CN110527453B CN201910853891.8A CN201910853891A CN110527453B CN 110527453 B CN110527453 B CN 110527453B CN 201910853891 A CN201910853891 A CN 201910853891A CN 110527453 B CN110527453 B CN 110527453B
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/08—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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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
- C09J2451/00—Presence of graft polymer
-
- 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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- Chemical & Material Sciences (AREA)
- 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 adhesive sheet for a 5G antenna process, which comprises an acrylic copolymer, wherein the acrylic copolymer comprises the following components in parts by weight: 50-70 parts of isooctyl acrylate, 10-20 parts of ethyl acrylate, 1-5 parts of hydroxyethyl acrylate, 2-6 parts of acryloyl morpholine, 3-6 parts of methyl acrylate, 10-20 parts of methoxy polyethylene glycol methacrylate, 0.1-0.5 part of azobisisobutyronitrile and 150-200 parts of solvent. The acrylic copolymer can effectively improve the adhesive property and the temperature resistance of the adhesive sheet to the 5G antenna composition, well control the high-speed peeling force before and after high temperature and high humidity, and has no pollution to an attached object.
Description
Technical Field
The invention relates to the technical field of adhesive sheets, in particular to an acrylic copolymer-based adhesive sheet for a 5G antenna process.
Background
Since the implementation of 5G signals of mobile phones requires high frequency and low dielectric loss for antennas and substrates, many of the existing LCPs (Liquid Crystal Polymer) materials are used, but the LCP antennas have complicated processes and high requirements. The preparation of the soft substrate needs to be carried out by processes of acid washing, plasma sputtering, high-temperature pressing and the like, and a protective material needs to be attached to avoid pollution and damage.
Because LCP material surface energy is low, and the adhesion is very poor, to the requirement of protection film: low viscosity (peeling force less than 20gf/25mm), easy bonding and peeling, no transfer and contamination after high temperature and high humidity. The LCP is difficult to be stuck by adopting the existing polyacrylate and polyurethane protective materials; if silica gel is adopted, the price is high, and the transfer ghost is easy to cause pollution to the attached object.
Disclosure of Invention
The invention aims to provide an acrylic copolymer-based adhesive sheet for a 5G antenna process, which solves the problems that the existing adhesive sheet cannot adhere to LCP and pollute an attached object.
In order to solve the technical problem, the invention provides an adhesive sheet for a 5G antenna process, which comprises an acrylic copolymer, wherein the acrylic copolymer is obtained by polymerizing the following components in parts by weight: 50-70 parts of isooctyl acrylate, 10-20 parts of butyl acrylate, 1-5 parts of hydroxyethyl acrylate, 2-6 parts of acryloyl morpholine, 3-6 parts of methyl acrylate, 10-20 parts of methoxy polyethylene glycol methacrylate, 0.1-0.5 part of azobisisobutyronitrile and 150-200 parts of solvent.
Further, the preparation method of the acrylic copolymer comprises the following steps: putting part of monomers and a solvent into a reaction kettle, adding an initiator azobisisobutyronitrile at the temperature of 60-65 ℃ on the premise of introducing sufficient nitrogen, and reacting for 1-3 hours; then adding the residual monomers, and continuing to react for 1-2 h; then heating to 70-75 ℃, and continuing to react for 2-5 h; and then adding the rest solvent, diluting and cooling to obtain the acrylic copolymer.
Further, the solvent is benzene-free solvent, including ethyl acetate, acetone, butanone, isopropanol and mixtures thereof.
Further, the weight average molecular weight Mw of the acrylic copolymer is 30 to 80 ten thousand.
The invention provides an adhesive sheet for a 5G antenna process, which comprises a substrate, an adhesive layer coated on the substrate and a release film attached to the adhesive layer, wherein the adhesive comprises the following components in parts by weight: 100 parts of acrylic copolymer, 2-10 parts of curing agent, 0.001-0.002 part of catalyst and 20-60 parts of solvent; wherein the acrylic copolymer is the acrylic copolymer.
Further, the catalyst is an organic metal compound, and comprises an organic tin catalyst, an organic bismuth catalyst, an organic zirconium catalyst, an organic zinc catalyst, an organic aluminum catalyst and a mixture thereof.
Further, the curing agent is a polyisocyanate curing agent, and preferably, the curing agent is a hexamethylene diisocyanate adduct curing agent.
Further, the solvent is a benzene-free solvent comprising ethyl acetate, acetone, butanone, isopropanol, and mixtures thereof.
Further, the substrate may be a substrate commonly used in the art, including but not limited to paper, plastic film, foam, non-woven fabric, aluminum foil, and the like. Preferably, the substrate is a PET substrate.
Further, the adhesive sheet has a use layer thickness of not more than 35um, wherein the use layer means a substrate and an adhesive layer.
The invention has the beneficial effects that:
1. according to the acrylic copolymer, the methoxy polyethylene glycol methacrylate monomer is added into the acrylic copolymer, so that part of polyether chain segments are introduced to modify acrylate resin, and the wettability (initial adhesion) and the bonding property to LCP are effectively improved; in addition, an acryloyl morpholine monomer is added, so that the problem of poor temperature resistance of the adhesive film is effectively solved.
2. The adhesive sheet has good adhesive capacity and temperature resistance to LCP films made of low-polarity materials, well controls high-speed peeling force before and after high temperature and high humidity, and has no pollution to attached objects.
Drawings
FIG. 1 is a schematic structural view of one embodiment of an adhesive sheet of the invention;
wherein: 1. a PET substrate; 2. an adhesive layer; 3. and (4) a release film.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Examples 1 to 4, comparative examples 1 to 2: preparation of adhesive sheet for 5G antenna Process
1. Preparation of acrylic copolymer
According to the formula shown in Table 1, part of the monomers and ethyl acetate are put into the bottom of a reaction kettle, and an initiator azobisisobutyronitrile is added at 63 ℃ for reaction for 2 hours under the premise of ensuring sufficient nitrogen. Then, the residual monomer is added dropwise for 1 hour, and the reaction is continued for 1 hour after the dropwise addition is finished. Then the temperature is increased to 75 ℃, and the reaction is continued for 3 hours at the temperature of 75 ℃. And then adding the rest solvent, diluting and cooling to obtain the acrylic copolymer.
TABLE 1 Synthesis formulation of acrylic copolymer (parts by weight)
2. Preparation of adhesive sheet
The preparation method of the adhesive sheet comprises the following steps:
according to the application formula shown in Table 2, the composition is uniformly mixed, 8 μm dry glue is coated on 25 μm PET, the mixture is baked for 3min at 90 ℃, a 50 μm release film is attached, and the mixture is placed at 50 ℃ for 48h and then taken out for testing.
TABLE 2 formulation (parts by weight) of adhesive sheets of examples 1 to 4 and comparative examples 1 to 3
3. Performance testing
The adhesive sheets prepared in examples 1 to 4 and comparative examples 1 to 3 were subjected to the performance test according to the following method, and the test results are shown in table 3:
180 ° peel strength: the test is carried out according to the method specified in GB/T2792-2014.
180 ° high speed peel force: the test speed is 20m/min according to the method specified in GB/T2792-2014.
And (3) testing temperature resistance: and (3) attaching the adhesive sheet to a copper foil of 50um, aging in an oven at 180 ℃ for 30min, taking out, standing at room temperature for 30min, stripping the adhesive sheet, and observing whether the copper foil has residual glue or offset printing.
High-temperature high-humidity environment measurement: the adhesive sheet was attached to an LCP film, placed in a ring testing machine at 85 ℃ x 85% RH for 72h, then removed, placed at room temperature for 30min, tested for 180 ° peel strength and high speed peel force, and observed for the presence of adhesive residue or offset printing on the LCP film.
TABLE 3 test results of the adhesive sheets of examples 1 to 4 and comparative examples 1 to 3
As can be seen from Table 3, all of the conventional monomers used in comparative example 1 had a high peel force, but had very poor adhesion to LCP and poor temperature resistance; comparative example 2 is based on comparative example 1, partial methoxy polyethylene glycol methacrylate (M-90G) is added, and partial polyether chain segment is introduced to modify acrylate resin, so that the adhesive property on LCP is effectively improved.
Example 1 the problems of poor temperature resistance and poor ring test effect of the adhesive sheet are partially solved by adding part of acryloyl morpholine (ACMO) monomer on the basis of the comparative example 2; example 2 a part of acryloyl morpholine (ACMO) monomer is added to example 1, which improves the temperature resistance and ring test performance of the adhesive sheet.
Comparative example 3 the addition ratio of M-90G was increased on the basis of example 2, but no catalyst was added, the adhesion performance of the LCP film was significantly improved, but the high-speed peeling force was high, the loop-cut test climbing was severe, and the influence on the process tear was large.
Examples 3 and 4 the addition of different proportions of catalyst to comparative example 3 resulted in a partial reduction in the LCP film adhesion performance, but the high speed peel force before and after ring test was well controlled.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (8)
1. The adhesive sheet for the 5G antenna process is characterized by comprising an acrylic copolymer, wherein the acrylic copolymer is obtained by polymerization reaction of the following components in parts by weight: 50-70 parts of isooctyl acrylate, 10-20 parts of butyl acrylate, 1-5 parts of hydroxyethyl acrylate, 2-6 parts of acryloyl morpholine, 3-6 parts of methyl acrylate, 10-20 parts of methoxy polyethylene glycol methacrylate, 0.1-0.5 part of azobisisobutyronitrile and 150-200 parts of solvent;
wherein the weight average molecular weight Mw of the acrylic copolymer is 30-80 ten thousand, and the preparation method comprises the following steps:
putting half of the monomer and part of the solvent into a reaction kettle, adding an initiator azobisisobutyronitrile at the temperature of 60-65 ℃ on the premise of introducing sufficient nitrogen, and reacting for 1-3 hours; then adding the residual monomers, and continuing to react for 1-2 h; then heating to 70-75 ℃, and continuing to react for 2-5 h; and then adding the rest solvent, diluting and cooling to obtain the acrylic copolymer.
2. The adhesive sheet for 5G antenna process according to claim 1, wherein the solvent is a benzene-free solvent comprising ethyl acetate, acetone, butanone, isopropanol and mixtures thereof.
3. The adhesive sheet for the 5G antenna process comprises a substrate, an adhesive layer coated on the substrate and a release film attached to the adhesive layer, and is characterized in that the adhesive comprises the following components in parts by weight: 100 parts of acrylic copolymer, 2-10 parts of curing agent, 0.001-0.01 part of catalyst and 20-60 parts of solvent.
4. The adhesive sheet for a 5G antenna process according to claim 3, wherein the catalyst is an organic metal compound comprising an organotin catalyst, an organobismuth catalyst, an organozirconium catalyst, an organozinc catalyst, an organoaluminum catalyst, and a mixture thereof.
5. The adhesive sheet for a 5G antenna process according to claim 3, wherein the curing agent is a polyisocyanate-based curing agent.
6. The adhesive sheet for 5G antenna process according to claim 3, wherein the curing agent is hexamethylene diisocyanate adduct curing agent.
7. The adhesive sheet for 5G antenna process according to claim 3, wherein the solvent is a benzene-free solvent comprising ethyl acetate, acetone, butanone, isopropanol and mixtures thereof.
8. The adhesive sheet for 5G antenna process according to claim 3, wherein the adhesive sheet has a use layer thickness of not more than 35 um.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910853891.8A CN110527453B (en) | 2019-09-10 | 2019-09-10 | Acrylic copolymer-based adhesive sheet for 5G antenna process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910853891.8A CN110527453B (en) | 2019-09-10 | 2019-09-10 | Acrylic copolymer-based adhesive sheet for 5G antenna process |
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| CN110527453B true CN110527453B (en) | 2021-11-19 |
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| JP2022172615A (en) * | 2021-05-06 | 2022-11-17 | 日東電工株式会社 | Pressure sensitive adhesive sheet having release films and usage thereof |
| CN115637116A (en) * | 2022-09-29 | 2023-01-24 | 太仓斯迪克新材料科技有限公司 | High-temperature-resistant low-climbing protective film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775258A (en) * | 2009-01-13 | 2010-07-14 | 日东电工株式会社 | Pressure-sensitive adhesive sheet |
| CN104650758A (en) * | 2013-11-22 | 2015-05-27 | 日东电工株式会社 | Double-sided adhesive piece |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005314476A (en) * | 2004-04-27 | 2005-11-10 | Nitto Denko Corp | Adhesive composition, adhesive sheet and surface-protective film |
| JP4994895B2 (en) * | 2007-03-09 | 2012-08-08 | リンテック株式会社 | Adhesive sheet |
| JP5537015B2 (en) * | 2008-10-24 | 2014-07-02 | リンテック株式会社 | Hard coat layer adhesive and adhesive sheet |
| JP2011168751A (en) * | 2010-02-22 | 2011-09-01 | Nitto Denko Corp | Surface protective film |
| CN104592913B (en) * | 2015-01-30 | 2016-11-02 | 日东电工（上海松江）有限公司 | The preparation method of acrylic adhesives, binding agent and application thereof |
| CN106832102B (en) * | 2017-01-05 | 2019-08-27 | 无锡海特新材料研究院有限公司 | A kind of high-performance acrylic acid ester pressure-sensitive and preparation method thereof |
| CN107523242A (en) * | 2017-08-31 | 2017-12-29 | 东莞市联洲知识产权运营管理有限公司 | A kind of heat-conducting type polyacrylate pressure-sensitive and preparation method thereof |
| JP7241465B2 (en) * | 2018-01-30 | 2023-03-17 | 日東電工株式会社 | Adhesive, curable adhesive composition, adhesive sheet and method for producing same |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775258A (en) * | 2009-01-13 | 2010-07-14 | 日东电工株式会社 | Pressure-sensitive adhesive sheet |
| CN104650758A (en) * | 2013-11-22 | 2015-05-27 | 日东电工株式会社 | Double-sided adhesive piece |
Non-Patent Citations (1)
| Title |
|---|
| Formulation/Property Relationships in Radiation-Cured;C. W. G. ANSELL等;《Journal of applied polymer sceince》;20000930;第3321-3326页 * |
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