CN116376465A - Environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape and preparation method thereof - Google Patents
Environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape and preparation method thereof Download PDFInfo
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- CN116376465A CN116376465A CN202310473464.3A CN202310473464A CN116376465A CN 116376465 A CN116376465 A CN 116376465A CN 202310473464 A CN202310473464 A CN 202310473464A CN 116376465 A CN116376465 A CN 116376465A
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- acrylate
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- adhesive layer
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000012790 adhesive layer Substances 0.000 claims abstract description 77
- 229920001577 copolymer Polymers 0.000 claims abstract description 55
- 239000000853 adhesive Substances 0.000 claims abstract description 33
- 230000001070 adhesive effect Effects 0.000 claims abstract description 33
- 239000000178 monomer Substances 0.000 claims abstract description 32
- 230000009477 glass transition Effects 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 27
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000003292 glue Substances 0.000 claims abstract description 19
- 239000010410 layer Substances 0.000 claims description 21
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 16
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- 239000002904 solvent Substances 0.000 claims description 13
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 9
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 claims description 8
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- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 claims description 8
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- KVILQFSLJDTWPU-UHFFFAOYSA-N heptadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCOC(=O)C=C KVILQFSLJDTWPU-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
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- NQSLZEHVGKWKAY-UHFFFAOYSA-N 6-methylheptyl 2-methylprop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C(C)=C NQSLZEHVGKWKAY-UHFFFAOYSA-N 0.000 claims description 4
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 4
- CUXGDKOCSSIRKK-UHFFFAOYSA-N 7-methyloctyl prop-2-enoate Chemical compound CC(C)CCCCCCOC(=O)C=C CUXGDKOCSSIRKK-UHFFFAOYSA-N 0.000 claims description 4
- LVGFPWDANALGOY-UHFFFAOYSA-N 8-methylnonyl prop-2-enoate Chemical compound CC(C)CCCCCCCOC(=O)C=C LVGFPWDANALGOY-UHFFFAOYSA-N 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- PZDUWXKXFAIFOR-UHFFFAOYSA-N hexadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C=C PZDUWXKXFAIFOR-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- HZLFQUWNZMMHQM-UHFFFAOYSA-N piperazin-1-ylmethanol Chemical compound OCN1CCNCC1 HZLFQUWNZMMHQM-UHFFFAOYSA-N 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- XOALFFJGWSCQEO-UHFFFAOYSA-N tridecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCOC(=O)C=C XOALFFJGWSCQEO-UHFFFAOYSA-N 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- RZFODFPMOHAYIR-UHFFFAOYSA-N oxepan-2-one;prop-2-enoic acid Chemical compound OC(=O)C=C.O=C1CCCCCO1 RZFODFPMOHAYIR-UHFFFAOYSA-N 0.000 claims description 3
- JRWNODXPDGNUPO-UHFFFAOYSA-N oxolane;prop-2-enoic acid Chemical compound C1CCOC1.OC(=O)C=C JRWNODXPDGNUPO-UHFFFAOYSA-N 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- FEUIEHHLVZUGPB-UHFFFAOYSA-N oxolan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC1CCCO1 FEUIEHHLVZUGPB-UHFFFAOYSA-N 0.000 claims 1
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- 238000012360 testing method Methods 0.000 description 12
- 239000002390 adhesive tape Substances 0.000 description 10
- 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 description 7
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 125000005396 acrylic acid ester group Chemical group 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 description 2
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- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000010837 adhesive waste Substances 0.000 description 1
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- 229940116229 borneol Drugs 0.000 description 1
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 description 1
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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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
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
-
- 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
- C09J133/064—Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
-
- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
-
- 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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
-
- 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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
-
- 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
- C09J2301/302—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 the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of high polymer materials, in particular to an environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape and a preparation method thereof. The invention designs the bio-based acrylate adhesive layer with extremely low glass transition temperature and high glass transition temperature through the low-temperature bending resistance and high-temperature adhesiveness and cohesion required by the flexible foldable mobile phone, and the adhesive layer meets certain modulus and adhesive force requirements through the regulation and control of the bio-based acrylate copolymer monomer, the molecular weight, the functional resin and the cross-linking agent, meets the requirements of the bio-based acrylate copolymer adhesive layer on low temperature flexibility, high temperature cohesive force, high temperature stripping without residual glue and cutting without glue overflow, and uses the bio-based raw material which is easy to biodegrade, thereby solving the problems of difficult degradation, high pollution and high toxicity of the petroleum-based adhesive layer.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to an environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape and a preparation method thereof.
Background
With the continuous development of the full screen technology, the mobile phone screen accounts for more than 90%, the limit is approached, the screen size is difficult to be increased under the condition that the mobile phone size is not increased, and the screen size is too large, so that the problems of inconvenient operation, inconvenient carrying and the like are caused. Following the full screen, future consumer electronics innovations continue and the appearance of the cell phone may also evolve toward diversity. With the development of scientific technology and market demands, flexible foldable mobile phones were first used in 2019 in the world of mobile communication. The mobile phone and the tablet computer have the advantages of portability and functional diversity, so that the mobile phone and the tablet computer are combined together, market hotspots are formed once the mobile phone and the tablet computer are seen, and market attention and demands are increased year by year. In order to meet the demands of current consumers, various head manufacturers invest a large amount of resources in recent years to promote the development of folding screen technology.
The flexible foldable mobile phone is folded outwards or inwards, and a series of new requirements are provided for screen flexibility. For common screen bonding or under-screen bonding, the same need to be upgraded to meet the requirement that the screen can still maintain reliable bonding, appearance and other performances after being subjected to horizontal stress of hundreds of thousands of repeated folding and aging in high and low temperature environments. In order to meet the folding function, the adhesive tape for bonding the internal parts of the mobile phone is required to provide good adhesion and bending resistance because the adhesive tape can be folded for a long time and at high frequency in the practical use process.
The prior art folding screen adhesive tape generally comprises a 50 mu m release layer, a 25 mu m adhesive layer, a 25-50 mu mTTU/foam core material, a 25 mu m adhesive layer and a 50 mu m release layer, wherein the TPU core material has high low-temperature breaking strength and elastic modulus, has relatively poor bending resistance and is difficult to meet the requirement of connecting internal parts of the folding screen. Crease is easy to appear after the foam core material is bent at low temperature, and the appearance effect of the folding screen is affected. The adhesive layer has extremely low elastic modulus and high Wen Yican adhesive, and is easy to overflow after being cut. In addition, the adhesive tape prepared by the prior art is thicker, and the process needs multiple coating steps, so that the appearance is affected, and the cost is increased.
At present, the acrylic acid ester pressure-sensitive adhesive industry mainly depends on acrylic acid ester monomers produced by petrochemical industry, the pressure-sensitive adhesive is used as a disposable product for daily use, the demand of the pressure-sensitive adhesive is relatively large, the consumption of petroleum resources is inevitably accelerated, the petroleum resources belong to non-renewable or difficult-renewable resources, and the depletion of the earth resources is inevitably caused by excessive exploitation. In addition, the acrylic pressure-sensitive adhesive from petrochemical sources is slow in biodegradation, is difficult to degrade by direct discarding or landfilling, and is difficult to degrade, so that the environmental problem caused by waste adhesive products which cannot be degraded is increasingly serious, and therefore, the development of the environment-friendly degradable acrylic pressure-sensitive adhesive is an urgent need. However, for acrylic pressure-sensitive adhesive products, the variety of raw materials from natural materials that can be used is limited. Because it is desirable to have excellent properties of petroleum-based tape articles even better in addition to ensuring that the source of the raw materials is highly natural. The production of bio-based acrylate monomers is generally based on the catalytic esterification reaction of alcohols extracted from plants with acrylic acid, wherein the sources of bio-based alcohols are generally natural products such as vegetable oil, borneol and the like, and the sources of the raw materials are abundant, have strong reproducibility and accord with the strategy of sustainable development. The bio-derived acrylate monomers have different structural units in their side chain groups than petroleum-based products, but are also reactive, so similar synthetic processes can be used to prepare bio-based acrylate adhesives.
The adhesive layer for the current flexible foldable mobile phone has extremely low-temperature flexibility, easy glue overflow during slitting, high Wen Yican glue and obviously reduced viscosity under high temperature and high humidity.
Disclosure of Invention
The invention aims to provide an environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape and a preparation method thereof, which are used for solving the problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme: an environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape and a preparation method thereof.
An environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape, which is characterized in that: the pressure-sensitive adhesive tape comprises a first release layer, an adhesive layer and a second release layer; one side of the adhesive layer is provided with a first release layer, and the other side of the adhesive layer is provided with a second release layer;
the adhesive layer at least contains two glass transition temperatures, wherein the first glass transition temperature is between-70 ℃ and-30 ℃, and the second glass transition temperature is between 0 ℃ and 65 ℃; if the first glass transition temperature of the adhesive layer is < -70 ℃, the cohesive force of the adhesive layer is influenced by being too soft, the adhesive is Wen Yican, and the adhesive is easy to overflow after being cut; if the first glass transition temperature of the adhesive layer is > -30 ℃, the adhesive layer is not hard enough and has insufficient low-temperature flexibility, so that the adhesive layer is poor in low-temperature bending; if the second glass transition temperature of the adhesive layer is less than 0 ℃, the high-temperature cohesive force of the adhesive layer can be influenced, and the adhesive is Wen Yican; if the second glass transition temperature of the adhesive layer is > 65 ℃, the low temperature flexibility is affected by too hard to cause poor low temperature bending.
Further, the adhesive layer comprises the following components: a bio-based acrylate copolymer, a functional resin, and a curing agent;
adding functional resin into the bio-based acrylate copolymer, generating two-phase separation by utilizing the difference between polarities of the bio-based acrylate copolymer, and ensuring the simultaneous existence of high/low glass transition temperature parts so as to realize low-temperature flexibility and high-temperature resistance of the bio-based acrylate copolymer;
the adhesive layer provides good low-temperature flexibility and high-temperature cohesion through bonding the object to be bonded, and has no residual adhesive after high-temperature stripping and no adhesive overflow during slitting.
The glass transition temperature of the bio-based acrylate copolymer is between-80 ℃ and-40 ℃; if the glass transition temperature of the bio-based acrylic ester copolymer is < -80 ℃, the cohesion of the adhesive layer is influenced by being too soft, the adhesive is Wen Yican, and the adhesive is easy to overflow after being cut; if the glass transition temperature of the bio-based acrylate copolymer is > -40 ℃, the low temperature bending failure is caused by insufficient low temperature flexibility due to too hard.
The glass transition temperature of the functional resin is between 0 and 55 ℃;
the mass ratio of the bio-based acrylate copolymer to the functional resin is (50:50) - (95:5);
the usage amount of the curing agent is 0.5-2.5 wt% of the bio-based acrylate copolymer.
Further, the bio-based acrylate copolymer is polymerized by a main monomer and an auxiliary monomer, wherein the main monomer is one or more of n-butyl acrylate, 2-ethylhexyl acrylate, 2-octyl acrylate, n-octyl acrylate, isooctyl acrylate, isononyl acrylate, isodecyl acrylate, 2-propylheptyl acrylate, alkoxylated tetrahydrofuran acrylate, methoxyethyl acrylate, caprolactone, ethoxyethoxyethyl acrylate, methoxypolyethylene glycol acrylate, tridecyl acrylate, cetyl acrylate, heptadecyl acrylate, isooctyl methacrylate, lauryl methacrylate and dodecyl methacrylate which are sourced from bio-based; the auxiliary monomer is one or more of methyl acrylate, acrylic acid, acrylamide, acrylic acid-2-hydroxyethyl ester, acrylic acid-4-hydroxybutyl ester, methacrylic acid and methacrylamide
Further, in the bio-based acrylate copolymer, the mass ratio of the main monomer to the auxiliary monomer is (90:10) to (99.9:0.1).
Further, the functional resin is any one or more of polyester resin, polyacrylic resin and epoxy resin; the carboxyl or hydroxyl on the molecular chain segment of the bio-based acrylic ester copolymer and the cross-linking agent are chemically cross-linked to form an interpenetrating network structure, and the adhesive layer is provided for supporting and ensuring the high-temperature cohesion of the adhesive layer.
Further, the weight average molecular weight of the bio-based acrylate copolymer is between 18 ten thousand and 100 ten thousand; if the weight average molecular weight of the bio-based acrylate copolymer is less than 18 ten thousand, the cohesion is too low to affect the high temperature cohesion, and the problem of adhesive residue overflow occurs, and if the weight average molecular weight of the bio-based acrylate copolymer is more than 100 ten thousand, the cohesion is too high to affect the low temperature flexibility.
Further, the adhesive layer has a storage modulus of between 0 and 200Kpa at-20 ℃; if the adhesive layer has a storage modulus of > 200Kpa at-20 ℃, the adhesive layer is too hard and has insufficient low-temperature flexibility, resulting in poor low-temperature bending.
Further, the adhesive layer has a storage modulus of between 8 and 25Kpa at 65 ℃; if the storage modulus of the adhesive layer is less than 8Kpa at 65 ℃, the adhesive layer is easy to have high Wen Canjiao peeling force reduction due to low high-temperature cohesion and easy to cut and overflow glue; if the adhesive layer has a storage modulus > 25Kpa at 65 c, the adhesive layer is too hard and thus has insufficient flexibility.
Further, the adhesive layer has a loss modulus to storage modulus ratio tan θ of 0.3 to 0.8 at 65 ℃.
Further, the adhesion layer has a peel force from the mirror surface steel plate of 5.0 to 8.0N/inch at 65 ℃.
The preparation method of the environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape comprises the following steps:
s1: taking functional monomers and auxiliary monomers of the bio-based acrylate copolymer, uniformly mixing to obtain a bio-based acrylate mixed monomer, adding a solvent and an initiator, heating and stirring under the protection of nitrogen, and preserving heat for 3-5 hours to obtain a bio-based acrylate copolymer solution;
s2: taking functional resin, adding toluene to obtain a functional resin solution, adding a bio-based acrylate copolymer solution, uniformly mixing, adding a diluting solvent, uniformly mixing, adding a curing agent, mixing for 20-50min, standing and defoaming to obtain a bio-based acrylate adhesive solution;
s3: coating a bio-based acrylate adhesive glue solution on the release surface of the first release layer, drying, compounding the dried adhesive layer with the release surface of the second release layer, and curing to obtain an environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape;
the first glass transition temperature of the adhesive layer is between-80 ℃ and-30 ℃, and the second glass transition temperature is between 0 ℃ and 65 ℃.
Further, the main monomer of the bio-based acrylate copolymer is one or more of n-butyl acrylate, 2-ethylhexyl acrylate, 2-octyl acrylate, n-octyl acrylate, isooctyl acrylate, isononyl acrylate, isodecyl acrylate, 2-propyl heptyl acrylate, alkoxylated tetrahydrofuran acrylate, methoxyethyl acrylate, caprolactone acrylate, ethoxyethoxyethyl acrylate, methoxypolyethylene glycol acrylate, tridecyl acrylate, cetyl acrylate, heptadecyl acrylate, isooctyl methacrylate, lauryl methacrylate and dodecyl methacrylate which are derived from bio-based sources; the auxiliary monomer is one or more of methyl acrylate, acrylic acid, acrylamide, acrylic acid-2-hydroxyethyl ester, acrylic acid-4-hydroxybutyl ester, methacrylic acid and methacrylamide.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides an environment-friendly double faced adhesive tape for a folding screen, which has low-temperature flexibility elastic modulus and good bending resistance, is not easy to be adhesive residue at high temperature, is free of adhesive overflow when being cut, and is applied to bonding a mobile phone screen with conductive graphite or a metal sheet. According to the low-temperature bending resistance, high-temperature adhesiveness and cohesion required by the flexible foldable mobile phone, the bio-based acrylate adhesive layer with extremely low glass transition temperature and high glass transition temperature is designed, so that the adhesive layer meets certain modulus and adhesive force requirements, meets the requirements of low-temperature flexibility, high-temperature cohesion, high-temperature stripping, no residual glue and no glue overflow during cutting of the bio-based acrylate copolymer adhesive layer, and uses bio-based raw materials which are easy to biodegrade, thereby solving the problems of difficult degradation, high pollution and high toxicity of the petroleum-based adhesive layer.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a schematic view of a bio-based double-sided tape structure of the present invention;
FIG. 2 is a graph showing the change in properties of the adhesive layer at various temperatures according to example 4 of the present invention;
in the figure: 1-a first release layer; a 2-adhesive layer; and 3-a second release layer.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only 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.
1. The preparation method of the bio-based acrylate copolymer solution (A1-A5) comprises the following specific steps:
weighing raw materials according to parts by weight, adding a bio-based acrylate mixed monomer into a reactor with reflux condensation, heating and stirring 1/2 of the total mass of the mixed monomer, 1/2 of the total mass of a solvent and 1/4 of the total mass of an initiator under the protection of nitrogen, wherein the temperature is 85 ℃, after the reaction starts, uniformly dripping 1/2 of the total mass of the initiator, the rest bio-based acrylate mixed monomer and 1/2 of the total mass of the solvent within 60min, continuously reacting for 2 hours at the temperature of 80 ℃, and finally adding the rest initiator and preserving the heat for 4 hours to obtain the bio-based acrylate copolymer solution.
Specifically, the bio-based comonomer is selected from one or more of 2-ethylhexyl acrylate (2-EHA), heptadecyl acrylate (C17A), n-Octyl Acrylate (OA), methyl Acrylate (MA) and Acrylic Acid (AA); the initiator is Azobisisobutyronitrile (AIBN); the solvent is selected from any one of Ethyl Acetate (EAC) and toluene (Tol). The resulting acrylate copolymer solution was tested for weight average molecular weight (Mw) and glass transition temperature (Tg).
The specific bio-based acrylate copolymer solution formulation (feed mass ratio) is shown in table 1.
TABLE 1
2. The preparation method of the bio-based acrylate copolymer solution (A6-A7) comprises the following specific steps:
weighing raw materials according to parts by weight, adding a bio-based acrylate mixed monomer into a reactor with reflux condensation, heating and stirring 4/5 of the total mass of the mixed monomer, 2/5 of the total mass of a solvent and 1/3 of the total mass of an initiator under the protection of nitrogen, uniformly dropwise adding 1/6 of the total mass of the initiator and 1/5 of the total mass of the residual bio-based acrylate mixed monomer and the solvent within 120min after reacting for 120min at 70 ℃, continuously reacting for 3 hours at 70 ℃, finally adding the residual initiator, preserving heat for 3 hours, and finally adding the residual solvent to obtain the bio-based acrylate copolymer solution.
Specifically, the bio-based comonomer is selected from one or more of 2-ethylhexyl acrylate (2-EHA), n-Octyl Acrylate (OA), methyl Acrylate (MA) and Acrylic Acid (AA); the initiator is selected from Azodiisobutyronitrile (AIBN) and dibenzoyl peroxide (BPO); the solvent is selected from any one of Ethyl Acetate (EAC) and toluene (Tol). The resulting acrylate copolymer solution was tested for weight average molecular weight (Mw) and glass transition temperature (Tg).
The specific bio-based acrylate copolymer solution formulation (feed mass ratio) is shown in table 2.
TABLE 2
3. Preparation of bio-based acrylate adhesive glue solution
And taking the functional resin, and adding toluene to ensure that the concentration of the functional resin is 50%, thereby obtaining a functional resin solution. Mixing the bio-based acrylate copolymer solution prepared in the first step with a functional resin solution according to a certain proportion to obtain 100 parts by mass of bio-based acrylate master batch, adding a diluting solvent into the obtained master batch, stirring for 30min, uniformly mixing, finally adding a curing agent, stirring for 30min, uniformly mixing, standing and defoaming to obtain the bio-based acrylate adhesive glue solution.
The ratio of the amounts by mass of the above components in the specific examples to the comparative examples is shown in Table 3.
Table 3 the functional resin is selected from any one of polyester resin (B1), polyester resin (B2), polyester resin (B3), acrylic resin (B4) and epoxy resin (B5). The polyester resin (B1) is provided by Toyo-yo, and has a product number of 280 and a Tg of 68 ℃; the polyester resin (B2) is provided by Toyo-yo, and has a product number of GK-680 and a Tg of 10 ℃; the polyester resin (B3) is provided by Mitsubishi chemical, with the product number of TP249 and the Tg of 36 ℃; acrylic resin (B4) was supplied by mitsubishi chemical under the trade designation BR116, tg 48 ℃; epoxy resin (B5) was supplied by Nanya under the trade designation NPES-901 and had a Tg of 60 ℃.
Curing agent isocyanate was supplied by TONGYANG ink under the product number BHS8515 with a solids content of 5%.
The dilution solvent used was ethyl acetate, supplied by Jiangsu-rop.
TABLE 3 Table 3
6. Preparation of environment-friendly adhesive tape for folding screen
Coating bio-based acrylate adhesive glue solution on the release surface of the first release layer 1 by using a comma doctor blade coater, placing the coated bio-based acrylate adhesive glue solution in a baking oven at 100 ℃ for 2min to volatilize a solvent to form a bio-based adhesive layer, controlling the thickness of the adhesive layer to be 25 mu m, compositing the dried adhesive layer 2 with the release surface of the second release layer 3, and curing the coated environment-friendly adhesive tape for the folding screen at room temperature of 25 ℃ for 7 days to obtain the environment-friendly adhesive tape for the folding screen. After curing, the mixture was left at room temperature for 24 hours, and then physical properties were measured.
The first release layer 1 is a release film 1, and is provided by a new material with a thickness of sun-shining: 50 μm, and the release force is 15-20g/inch;
the second release layer 3 is a release film 2 provided by Jiangyin Huamei technology and has the thickness: 20 μm and the release force is 3-6g/inch.
Experiment
If the test conditions are not explicitly stated, the following tests are all tested under 23-50% RH.
The weight average molecular weight Mw of the acrylate copolymers was determined using a Waters E2695 gel permeation chromatograph. Test conditions: the mobile phase is tetrahydrofuran; column temperature, 40 ℃; mobile phase flow rate: 1.0mL/min.
Scraping a biobased acrylate adhesive glue solution coating on a 50 mu m release film by using a comma roller scraper, drying for 5min in a 100 ℃ oven to obtain an adhesive layer dry film, performing rheological test by using an American TA company HR-10 rotary rheometer, and testing the loss modulus G 'and the storage modulus G' of the adhesive layer under the condition that the temperature is-100-150 ℃, the heating rate is 5 ℃/min, the strain is 0.1% and the frequency is 1 Hz by using a temperature scanning.
Spreading a biobased acrylate adhesive glue solution coating on a 50 mu m release film by using a comma roller scraper, drying for 5min in a 100 ℃ oven to obtain an adhesive layer dry film, carrying out rheological test by using an American TA company HR-10 rotary rheometer, and recording the peaks of loss factor tan theta curve peaks of the adhesive layer measured under the condition that the temperature is-100-150 ℃ and the temperature rising rate is 5 ℃/min, the strain is 0.1 percent and the frequency is 1 hertz as glass transition temperatures Tg1 and Tg2 of the adhesive layer by using a temperature scanning.
The acrylate copolymer solution is scraped on a 50 μm release film by using a comma roller scraper, and is dried in a drying oven at 100 ℃ for 5min to obtain a copolymer dry film with a dry film thickness of 25 μm, and then the glass transition temperature Tg of the copolymer dry film is detected by a DSC measurement method. Measuring device: the test temperature range is-100-120 ℃ and the temperature rising rate is 5 ℃/min.
At 23 ℃, bonding a 50 μm thick standardized DONGLI D03 BOPET film on any one side of a 150mm by 25mm long tape sample, bonding the other side of the tape sample to a stainless steel mirror plate (150 mm by 50mm by 2mm thick and having a surface roughness of 10nm + -10 nm) meeting the material requirements of GB/T2792 peel test steel plates, rolling the sample back and forth on the stainless steel mirror plate bonded with the sample at a speed of 300mm/min for 1 time by using a 2kg roller, respectively standing for 20 minutes at-30 ℃/65 ℃, and then using a stretcher to perform 180 DEG peel strength test, wherein the peel speed is 300mm/min, the number of test samples is 3, and taking the arithmetic average of the 3 test results as the peel force result.
And (3) judging that the residual adhesive of the sample is excellent if the ratio of the area of the residual adhesive area on the surface of the stainless steel mirror surface steel plate after the peeling force test of the adhesive layer of the adhesive tape sample strip at 65 ℃ to the area of the area peeled off from the steel plate by the sample strip is less than or equal to 5%. And judging the residual adhesive difference of the sample if the ratio of the area of the residual adhesive area on the surface of the stainless steel mirror surface steel plate after the peeling force test of any adhesive layer of the adhesive tape sample strip at 65 ℃ to the area of the area peeled off from the steel plate by the sample strip is more than 5 percent. Here, the residual glue means a phenomenon in which the adhesive layer is broken by polymerization, and the surface of the substrate and the surface of the steel sheet are covered with the broken adhesive layer.
The performance of the biobased adhesive layers of each of the comparative examples and examples was tested and the results are shown in Table 4.
TABLE 4 Table 4
Conclusion: as can be seen from the comparison of Table 4, in example 1, the bio-based acrylate copolymer has a low Tg, resulting in poor cohesive force at high temperature of the adhesive layer, and the problem of adhesive residue occurs.
In example 2, the Tg of the biobased acrylate copolymer was too high, resulting in an adhesive layer with too high a low temperature storage modulus.
In example 3, the bio-based acrylate copolymer had a low molecular weight, and the adhesive layer had a low peel force due to poor cohesion at high temperature, and was prone to adhesive residue.
In examples 4 to 6, the functional resin polyester resin B3 was added to the bio-based acrylate copolymer A4 to A6, and the adhesive layer had a high and low temperature modulus and a peeling force satisfying the requirements, and was free from the problem of residual glue.
In example 7, the bio-based acrylate copolymer had a higher molecular weight, and the adhesive layer had a high temperature modulus, and the high temperature peel force was too high, which affected reworkability.
In example 8, the bio-based acrylate copolymer A4 was added with the functional resin polyester resin B1, and the adhesive layer had a high temperature modulus, and the adhesive surface was too hard and tack-free.
In example 9, the functional resin polyester resin B2 was added to the bio-based acrylate copolymer A4, and the adhesive layer had a low high temperature modulus and insufficient high temperature peel force.
In example 10, the functional resin B2 was added in too high an amount, the adhesive layer had too high a high/low temperature modulus, and the adhesive face was too hard and tack-free.
In example 11, the addition amount of the functional resin B2 was too low, and the adhesive layer had a low high temperature modulus and insufficient high temperature peel force.
In example 12, the functional resin acrylic resin B4 was added to the bio-based acrylate copolymer A4, and the adhesive layer had a high and low temperature modulus and a peeling force satisfying the requirements, and was free from the problem of residual glue.
In example 13, the bio-based acrylate copolymer A4 was added with the functional resin B5, and the adhesive layer had a high temperature modulus, and the adhesive surface was too hard and tack-free.
Functional resin is not added in the formulas of comparative examples 1-2, the adhesive layer has low high-temperature stripping force, poor cohesive force and easy residual glue, and the high-temperature stripping force is still lower through the increment of the cross-linking agent, but the low-temperature modulus is too high, and the low-temperature flexibility is poor.
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 (10)
1. An environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape, which is characterized in that: the pressure-sensitive adhesive tape comprises a first release layer (1), an adhesive layer (2) and a second release layer (3); one side of the adhesive layer (2) is provided with a first release layer (1), and the other side is provided with a second release layer (3);
the adhesive layer (2) has at least two glass transition temperatures, the first glass transition temperature is between-70 ℃ and-30 ℃, and the second glass transition temperature is between 0 ℃ and 65 ℃.
2. The environmentally friendly low-resistance Wen Wanshe pressure sensitive adhesive tape according to claim 1, wherein: the adhesive layer (2) comprises the following components: a bio-based acrylate copolymer, a functional resin, and a curing agent;
the glass transition temperature of the bio-based acrylate copolymer is between-80 ℃ and-40 ℃;
the glass transition temperature of the functional resin is between 0 and 55 ℃;
the mass ratio of the bio-based acrylate copolymer to the functional resin is (50:50) - (95:5);
the usage amount of the curing agent is 0.5-2.5 wt% of the bio-based acrylate copolymer.
3. An environmentally friendly low-resistance Wen Wanshe pressure sensitive adhesive tape according to claim 2, wherein: the bio-based acrylic ester copolymer is polymerized by a main monomer and an auxiliary monomer, wherein the main monomer is one or more of n-butyl acrylate, 2-ethylhexyl acrylate, 2-octyl acrylate, n-octyl acrylate, isooctyl acrylate, isononyl acrylate, isodecyl acrylate, 2-propylheptyl acrylate, alkoxylated tetrahydrofuran acrylate, methoxyethyl acrylate, caprolactone acrylate, ethoxyethoxyethyl acrylate, methoxypolyethylene glycol acrylate, tridecyl acrylate, cetyl acrylate, heptadecyl acrylate, isooctyl methacrylate, lauryl methacrylate and lauryl methacrylate which are sourced from bio-based sources; the auxiliary monomer is one or more of methyl acrylate, acrylic acid, acrylamide, acrylic acid-2-hydroxyethyl ester, acrylic acid-4-hydroxybutyl ester, methacrylic acid and methacrylamide.
4. An environmentally friendly low-resistance Wen Wanshe pressure sensitive adhesive tape according to claim 3, wherein: in the bio-based acrylate copolymer, the mass ratio of the main monomer to the auxiliary monomer is (90:10) - (99.9:0.1).
5. An environmentally friendly low-resistance Wen Wanshe pressure sensitive adhesive tape according to claim 2, wherein: the functional resin is one or more of polyester resin, polyacrylic resin and epoxy resin.
6. An environmentally friendly low-resistance Wen Wanshe pressure sensitive adhesive tape according to claim 2, wherein: the weight average molecular weight of the bio-based acrylate copolymer is between 18 ten thousand and 100 ten thousand.
7. The environmentally friendly low-resistance Wen Wanshe pressure sensitive adhesive tape according to claim 1, wherein: the storage modulus of the adhesive layer (2) is between 0 and 200Kpa at the temperature of minus 20 ℃;
the storage modulus of the adhesive layer (2) is between 8 and 25Kpa at 65 ℃;
the adhesive layer (2) has a loss modulus to storage modulus ratio tan theta of 0.3-0.8 at 65 ℃.
8. The environmentally friendly low-resistance Wen Wanshe pressure sensitive adhesive tape according to claim 1, wherein: the peeling force between any surface of the adhesive layer (2) and the mirror surface steel plate is between 5.0 and 8.0N/inch under the condition of 65 ℃.
9. A preparation method of an environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape is characterized by comprising the following steps: the method comprises the following steps:
s1: taking functional monomers and auxiliary monomers of the bio-based acrylate copolymer, uniformly mixing to obtain a bio-based acrylate mixed monomer, adding a solvent and an initiator, heating and stirring under the protection of nitrogen, and preserving heat for 3-5 hours to obtain a bio-based acrylate copolymer solution;
s2: taking functional resin, adding toluene to obtain a functional resin solution, adding a bio-based acrylate copolymer solution, uniformly mixing, adding a diluting solvent, uniformly mixing, adding a curing agent, mixing for 20-50min, standing and defoaming to obtain a bio-based acrylate adhesive solution;
s3: coating a bio-based acrylate adhesive glue solution on a release surface of a first release layer (1), drying, compounding the dried adhesive layer (2) with a release surface of a second release layer (3), and curing to obtain an environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape;
the first glass transition temperature of the adhesive layer (2) is between-80 ℃ and-30 ℃, and the second glass transition temperature is between 0 ℃ and 65 ℃.
10. The method for preparing the environment-friendly low-resistance Wen Wanshe pressure-sensitive adhesive tape according to claim 9, which is characterized in that: the main monomer of the bio-based acrylic ester copolymer is one or more of n-butyl acrylate, 2-ethylhexyl acrylate, 2-octyl acrylate, n-octyl acrylate, isooctyl acrylate, isononyl acrylate, isodecyl acrylate, 2-propyl heptyl acrylate, alkoxylated tetrahydrofuranyl acrylate, methoxyethyl acrylate, caprolactone acrylate, ethoxyethoxyethyl acrylate, methoxypolyethylene glycol acrylate, tridecyl acrylate, cetyl acrylate, heptadecyl acrylate, isooctyl methacrylate, lauryl methacrylate and dodecyl methacrylate which are derived from bio-based sources; the auxiliary monomer is one or more of methyl acrylate, acrylic acid, acrylamide, acrylic acid-2-hydroxyethyl ester, acrylic acid-4-hydroxybutyl ester, methacrylic acid and methacrylamide.
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