CN116200148A - Polyacrylate pressure-sensitive adhesive with high stripping force - Google Patents
Polyacrylate pressure-sensitive adhesive with high stripping force Download PDFInfo
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- CN116200148A CN116200148A CN202310381944.7A CN202310381944A CN116200148A CN 116200148 A CN116200148 A CN 116200148A CN 202310381944 A CN202310381944 A CN 202310381944A CN 116200148 A CN116200148 A CN 116200148A
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 72
- 229920000058 polyacrylate Polymers 0.000 title claims abstract description 60
- 239000000178 monomer Substances 0.000 claims abstract description 136
- 239000003999 initiator Substances 0.000 claims abstract description 58
- 239000002904 solvent Substances 0.000 claims abstract description 50
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 39
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 38
- 238000004132 cross linking Methods 0.000 claims abstract description 27
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 147
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 140
- 238000006243 chemical reaction Methods 0.000 claims description 79
- 239000000203 mixture Substances 0.000 claims description 54
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 49
- 238000003756 stirring Methods 0.000 claims description 40
- 238000004321 preservation Methods 0.000 claims description 39
- -1 acrylic ester Chemical class 0.000 claims description 28
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 27
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 23
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 14
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 13
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 13
- 229920002799 BoPET Polymers 0.000 claims description 13
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 13
- 238000004090 dissolution Methods 0.000 claims description 12
- 150000003505 terpenes Chemical class 0.000 claims description 11
- 235000007586 terpenes Nutrition 0.000 claims description 11
- 239000003292 glue Substances 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 2
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 2
- WCOATMADISNSBV-UHFFFAOYSA-K diacetyloxyalumanyl acetate Chemical compound [Al+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WCOATMADISNSBV-UHFFFAOYSA-K 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 239000005007 epoxy-phenolic resin Substances 0.000 claims description 2
- 239000012948 isocyanate Substances 0.000 claims description 2
- 150000002513 isocyanates Chemical class 0.000 claims description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 description 22
- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 5
- 238000012806 monitoring device Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000004831 Hot glue Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006332 epoxy adhesive Polymers 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Classifications
-
- 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
- Adhesives Or Adhesive Processes (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a polyacrylate pressure-sensitive adhesive with high stripping force, which consists of hard monomers, soft monomers, functional monomers, internal crosslinking monomers, solvents, initiators, curing agents and tackifying resins.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a polyacrylate pressure-sensitive adhesive with high stripping force and a preparation method thereof.
Background
The polyacrylate pressure-sensitive adhesive has the advantages of good pressure sensitivity, sensitivity when being subjected to pressure, outstanding good bonding performance and good solution to the problems of the surface and the interface of the material. With the continuous progress and development of technology, the application requirements of pressure-sensitive adhesive products are also becoming more and more extensive.
The polyacrylate pressure-sensitive adhesive is mainly applied to various high-end fields such as aerospace, communication electronics, automobile manufacturing, advertisement packaging, transportation, printing and coating, labels, protective films, medical and health and the like in the adhesive industry; the current adhesive industry mostly adopts hot melt adhesives, epoxy adhesives, solvent adhesives and the like, and has the advantages that high VOCs are commonly discharged, the harm to the environment is large, the environment is not easy to use, the current low-carbon environment-friendly requirement is not facilitated, the important strategic development direction proposed by China is not facilitated, namely, the great targets of carbon peak and carbon neutralization are realized, and therefore, the environment-friendly adhesive, the high-performance special adhesive and the production method are greatly developed.
The polyacrylate pressure-sensitive adhesive is divided into a water-based pressure-sensitive adhesive and an oil-based pressure-sensitive adhesive, wherein the water-based pressure-sensitive adhesive has poorer performance in a humid environment, a narrower application range and less application in high-end industries, so that the oil-based polyacrylate pressure-sensitive adhesive better solves the technical defects and shortcomings, has better optical performance, better weather resistance, better stability and better cohesive strength, and the polyacrylate pressure-sensitive adhesive in the current state has lower productivity and less supply of products, and particularly has a smaller number of polyacrylate pressure-sensitive adhesive technologies with high performance and high peel strength.
Disclosure of Invention
The first object of the invention is to provide a solvent polyacrylate pressure-sensitive adhesive with high peeling force, high cohesive strength, good chemical stability and good weather resistance, aiming at the special purpose requirement existing in the current adhesive industry.
The invention provides a polyacrylate pressure-sensitive adhesive with high stripping force, which aims at the defects and shortcomings commonly existing in the current polyacrylate pressure-sensitive adhesives.
The third object of the invention is to provide a preparation method of the polyacrylate pressure-sensitive adhesive.
In order to achieve the above purpose, the present invention is specifically implemented by the following technical scheme:
the polyacrylate pressure-sensitive adhesive with high peeling force comprises the following components in parts by weight:
acrylic ester soft monomer 38-42 parts
2-7 parts of hard monomer
1-2 parts of functional monomer
0.04 to 0.08 part of crosslinking monomer
45-60 parts of solvent
Initiator 0.2-0.6 parts
The polyacrylate pressure sensitive adhesive also comprises a curing agent and a resin;
the curing agent accounts for 0.1-0.9 part of the total weight of the acrylic ester soft monomer, the hard monomer, the functional monomer and the crosslinking monomer;
the weight of the resin accounts for 12-28 parts of the total weight of the acrylic ester soft monomer, the hard monomer, the functional monomer and the crosslinking monomer;
preferably, the curing agent comprises one or more of epoxy curing agent, aluminum triacetylacetonate curing agent and isocyanate curing agent;
preferably, the resin comprises one or more of terpene resin, epoxy resin, phenolic resin and rosin resin;
preferably, the acrylic ester soft monomer comprises butyl acrylate and isooctyl acrylate;
preferably, the hard monomer comprises one or two of vinyl acetate and methyl methacrylate;
preferably, the functional monomer comprises one or more of methacrylic acid, acrylic acid and itaconic acid;
preferably, the crosslinking monomer comprises one or more of hydroxyethyl acrylate, hydroxypropyl acrylate and N-methylolacrylamide;
preferably, the solvent comprises one or more of ethyl acetate, toluene, xylene, benzene, butanone and n-hexane;
preferably, the initiator comprises one or two of Azobisisobutyronitrile (AIBN) and dibenzoyl peroxide (BPO);
further preferably, the polyacrylate pressure-sensitive adhesive is prepared from the following raw materials in parts by weight:
24-26 parts of butyl acrylate, 15-18 parts of isooctyl acrylate, 2-7 parts of vinyl acetate, 0.04-0.08 part of hydroxyethyl acrylate, 1-2 parts of acrylic acid, 0.2-0.6 part of azobisisobutyronitrile, 25-30 parts of ethyl acetate, 20-30 parts of toluene and 1-5 parts of n-hexane, and 0.1-0.9 part of aluminum triacetate curing agent accounting for the total weight of butyl acrylate, isooctyl acrylate, vinyl acetate, hydroxyethyl acrylate, acrylic acid and Azobisisobutyronitrile (AIBN), wherein the terpene phenolic resin accounting for 12-28 parts of the total weight of butyl acrylate, isooctyl acrylate, vinyl acetate, hydroxyethyl acrylate, acrylic acid and Azobisisobutyronitrile (AIBN).
The preparation method of the polyacrylate pressure-sensitive adhesive with high stripping force comprises the following steps:
(1) Mixing the acrylic ester soft monomers except hard monomer vinyl acetate, the crosslinking monomers and the functional monomers into a monomer mixture, taking 58-62% of the monomer mixture, taking all n-hexane solvents and 80-85% of ethyl acetate solvents, uniformly mixing, adding into a reaction container provided with a condensing device and a dripping device, taking 7-8% of the total weight of the initiator azodiisobutyronitrile, dissolving with 2% of the total weight of the ethyl acetate solvents, and when the temperature in the reaction container reaches 70 ℃, putting into the reaction container for heat preservation reaction and controlling the stirring speed to be 90r/min;
(2) The mixture obtained in the step (1) is subjected to heat preservation, the heat preservation time is 5min after reflux occurs at the lower opening of a condenser, 7-8% of the total weight of an initiator AIBN is taken and dissolved by 2% of the total weight of the ethyl acetate solvent, and the mixture is put into a reactor for heat preservation reaction, and the temperature is controlled at 78-82 ℃;
(3) The acrylic ester prepolymer obtained in the step (2) is subjected to heat preservation reaction for 30min, and 1.5 percent of the total weight of the ethyl acetate solvent is added into 9 percent of the total weight of AIBN for dissolution;
(4) Adding the dissolved initiator obtained in the step (3) into the monomer mixture of the residual acrylic ester soft monomer, hard monomer, functional monomer and crosslinking monomer in the step (1), uniformly mixing the mixture, then dripping the mixture into the reaction container of the acrylic ester prepolymer in the step (1), carrying out heat preservation reflux reaction for 60-70 min, controlling the reaction temperature in the reaction container at 85-88 ℃ and gradually controlling the stirring speed at 125r/min;
(5) Keeping the temperature of the acrylate prepolymer obtained in the step (4) for 30min, mixing and dissolving 37-38.5% of the total mass of the initiator AIBN and hard monomer vinyl acetate, dripping for 20min, and controlling the temperature in the reactor at 85-88 ℃;
(6) Preserving the heat of the acrylate prepolymer obtained after the dripping in the step (5) for 1h, taking an initiator AIBN, wherein 37-38.5% of the total mass of the initiator AIBN is dissolved in 1.5% of the total mass of an ethyl acetate solvent, and dripping the initiator AIBN into a reaction container;
(7) The mixture obtained in the step (6) is subjected to heat preservation reaction for 2 hours;
(8) Cooling the mixture obtained in the step (7) to below 40 ℃, adding a toluene solvent, stirring for 30min at a stirring speed of 170r/min, and discharging;
further, the polyacrylate pressure-sensitive adhesive obtained in the step (8) is added with a curing agent and resin, stirred, uniformly stirred to obtain the polyacrylate pressure-sensitive adhesive, coated on a PET film, placed in an electrothermal blowing drying oven at 80 ℃ for curing for 10min, and the cured pressure-sensitive adhesive is covered and isolated by release PET, and the thickness of a glue layer is controlled to be 20-25 mu m;
further, the amount of the added curing agent accounts for 1-9% of the total weight of the acrylic ester soft monomer, the hard monomer, the crosslinking monomer and the functional monomer; the weight of the added resin accounts for 12-28% of the total weight of the soft monomer, the hard monomer, the crosslinking monomer and the functional monomer;
furthermore, the temperature of the initiator AIBN added in the step (1) is 70 ℃ and the initiator AIBN is added at one time, the temperature of the initiator AIBN added in the step (2) is 78-82 ℃ and is required to be added dropwise, the temperature is kept for 30min, the temperature of the initiator AIBN added in the steps (4), (5) and (6) is 85-88 ℃, the temperature is required to be added dropwise, and the heat-preserving time is 30min, 1h and 2h respectively;
further, the added curing agent is aluminum triacetylacetonate curing agent, and the added resin is terpene resin;
the invention realizes the aim of high peeling strength by designing the technical proposal, including controlling the addition of curing agents and resins with different dosages.
In the technical scheme, the invention has the following beneficial effects:
1. compared with the prior art, the polyacrylate pressure-sensitive adhesive with high stripping force is provided, and the problems of high stripping force, good stability, good water resistance and low toxicity and pollution are realized;
2. compared with the prior art, the invention provides the polyacrylate pressure-sensitive adhesive with the stripping force of up to 20N/25mm, and simultaneously has better cohesive strength under the high-temperature aging condition of 80 ℃ and keeps no displacement for 72 hours; the displacement can be avoided for 360 hours at normal temperature, so that no residual glue is produced, and the transfer phenomenon is avoided;
3. the invention has the characteristics of convenient use and simple operation process, has lower cost, can be improved according to different requirements of users, and can be widely applied to industries of communication electronics, advertisement packaging, transportation, protective films and the like.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and explanation only and is not intended to limit the present invention.
Example 1
The polyacrylate pressure-sensitive adhesive with high stripping force is prepared from the following raw materials:
24g of butyl acrylate, 15g of isooctyl acrylate, 2.5g of vinyl acetate, 0.05g of hydroxyethyl acrylate, 1.5g of acrylic acid, 0.3g of azodiisobutyronitrile, 30g of ethyl acetate, 25g of toluene, 2g of n-hexane, 0.03g of aluminum triacetylacetonate curing agent and 12g of terpene resin are weighed.
The polyacrylate pressure-sensitive adhesive with high stripping force comprises the following steps:
mixing the acrylic ester soft monomers, the crosslinking monomers and the functional monomers except the hard monomer vinyl acetate into a monomer mixture, taking 58% of the monomer mixture, taking all normal hexane solvents and 86% ethyl acetate solvents, uniformly mixing, adding into a reaction container provided with a condensing device, a dripping device and a temperature monitoring device, taking 7% of the total weight of the initiator azodiisobutyronitrile, dissolving with 2% of the total weight of the ethyl acetate solvents, when the temperature in the reaction container reaches 70 ℃, putting into the reaction container for heat preservation reaction, controlling the stirring speed to 90r/min, taking the heat preservation time to be 5min after reflux occurs at the lower opening of the condenser, taking 7% of the total weight of the initiator AIBN, dissolving with 2% of the total weight of the ethyl acetate solvents, putting into the reactor for heat preservation reaction, and controlling the temperature to be 78-82 ℃, adding 2% of the total weight of an ethyl acetate solvent into 9% of the total weight of AIBN for dissolution, adding the dissolved initiator into the monomer mixture of the residual 42% of acrylic ester soft monomer, hard monomer, functional monomer and crosslinking monomer, uniformly mixing the mixture, dripping the mixture into a reaction container for heat preservation reflux reaction for 60-70 min, controlling the reaction temperature in the reaction container to 85-88 ℃, gradually controlling the stirring speed to 125r/min, keeping the temperature of the dripping acrylate prepolymer for 30min, adding the initiator AIBN 37.5% of the total weight of AIBN and the hard monomer vinyl acetate for mixed dissolution and dripping for 20min, controlling the temperature in the reactor to 85-88 ℃, keeping the temperature of the dripping acrylate prepolymer for 1h, and then taking an initiator AIBN, wherein 37.5 percent of the total mass of the initiator AIBN is dissolved in 8 percent of the total mass of an ethyl acetate solvent, dropwise adding the initiator AIBN into a reaction container, carrying out heat preservation reaction on the obtained mixture for 2 hours, cooling the obtained mixture to below 40 ℃, adding a toluene solvent, stirring for 30 minutes, controlling the stirring speed at 170r/min, and discharging.
Further, adding 0.03g of a curing agent and 12g of resin into the obtained polyacrylate pressure-sensitive adhesive polymer, stirring, wherein the resin and the curing agent are uniformly dissolved by ethyl acetate or toluene in advance, coating the polyacrylate pressure-sensitive adhesive obtained after uniform stirring on a PET film, placing the PET film in an electrothermal blowing drying oven at 80 ℃ for curing for 10min, covering and isolating the cured pressure-sensitive adhesive by using release PET, and controlling the thickness of a glue layer to be 20-25 mu m for testing.
The polyacrylate pressure-sensitive adhesive with high peeling strength prepared in the embodiment 1 of the invention adopts GB-2792-1998 (China) test standard, and the 180-degree peeling strength is 15.7N/25mm; the shear creep retention test method is in accordance with GB/T4851-1998 (China) test standard, the normal temperature holding viscosity is more than 168h, the high temperature creep resistance test at 80 ℃ is less than 24h, and the residual glue phenomenon exists.
Example 2
The polyacrylate pressure-sensitive adhesive with high stripping force is prepared from the following raw materials:
24g of butyl acrylate, 15g of isooctyl acrylate, 2.5g of vinyl acetate, 0.05g of hydroxyethyl acrylate, 1.5g of acrylic acid, 0.3g of azodiisobutyronitrile, 30g of ethyl acetate, 25g of toluene, 2g of n-hexane, 0.03g of aluminum triacetylacetonate curing agent and 16g of terpene resin are weighed.
The polyacrylate pressure-sensitive adhesive with high stripping force comprises the following steps:
mixing the acrylic ester soft monomers, the crosslinking monomers and the functional monomers except the hard monomer vinyl acetate into a monomer mixture, taking 58% of the monomer mixture, taking all normal hexane solvents and 86% ethyl acetate solvents, uniformly mixing, adding into a reaction container provided with a condensing device, a dripping device and a temperature monitoring device, taking 7% of the total weight of the initiator azodiisobutyronitrile, dissolving with 2% of the total weight of the ethyl acetate solvents, when the temperature in the reaction container reaches 70 ℃, putting into the reaction container for heat preservation reaction, controlling the stirring speed to 90r/min, taking the heat preservation time to be 5min after reflux occurs at the lower opening of the condenser, taking 7% of the total weight of the initiator AIBN, dissolving with 2% of the total weight of the ethyl acetate solvents, putting into the reactor for heat preservation reaction, and controlling the temperature to be 78-82 ℃, adding 2% of the total weight of an ethyl acetate solvent into 9% of the total weight of AIBN for dissolution, adding the dissolved initiator into the monomer mixture of the residual 42% of acrylic ester soft monomer, hard monomer, functional monomer and crosslinking monomer, uniformly mixing the mixture, dripping the mixture into a reaction container for heat preservation reflux reaction for 60-70 min, controlling the reaction temperature in the reaction container to 85-88 ℃, gradually controlling the stirring speed to 125r/min, keeping the temperature of the dripping acrylate prepolymer for 30min, adding the initiator AIBN 37.5% of the total weight of AIBN and the hard monomer vinyl acetate for mixed dissolution and dripping for 20min, controlling the temperature in the reactor to 85-88 ℃, and keeping the temperature of the dripping acrylate prepolymer for 1h, and then taking an initiator AIBN, wherein 37.5 percent of the total mass of the initiator AIBN is dissolved in 8 percent of the total mass of an ethyl acetate solvent and dropwise added into a reaction container, carrying out heat preservation reaction on the obtained mixture for 2 hours, cooling the obtained mixture to below 40 ℃, adding a toluene solvent, stirring for 30 minutes, stirring at a speed of 170r/min, and discharging.
Further, adding 0.03g of a curing agent and 16g of resin into the obtained polyacrylate pressure-sensitive adhesive polymer, stirring, wherein the resin and the curing agent are uniformly dissolved by ethyl acetate or toluene in advance, coating the polyacrylate pressure-sensitive adhesive obtained after uniform stirring on a PET film, placing the PET film in an electrothermal blowing drying oven at 80 ℃ for curing for 10min, covering and isolating the cured pressure-sensitive adhesive by using release PET, and controlling the thickness of a glue layer to be 20-25 mu m for preparation for testing;
the polyacrylate pressure-sensitive adhesive with high peeling strength prepared in the embodiment 2 of the invention adopts GB 2792-1998 (China) test standard, and the 180-degree peeling strength is 16.7N/25mm; the shear creep retention test method is in accordance with GB/T4851-1998 (China) test standard, the normal temperature sticking is more than 168h, and the high temperature creep resistance test at 80 ℃ is more than 72h.
Example 3
The polyacrylate pressure-sensitive adhesive with high stripping force is prepared from the following raw materials:
24g of butyl acrylate, 15g of isooctyl acrylate, 2.5g of vinyl acetate, 0.05g of hydroxyethyl acrylate, 1.5g of acrylic acid, 0.3g of azodiisobutyronitrile, 30g of ethyl acetate, 25g of toluene, 2g of n-hexane, 0.03g of aluminum triacetylacetonate curing agent and 20g of terpene resin are weighed.
The polyacrylate pressure-sensitive adhesive with high stripping force comprises the following steps:
mixing the acrylic ester soft monomers, the crosslinking monomers and the functional monomers except the hard monomer vinyl acetate into a monomer mixture, taking 58% of the monomer mixture, taking all normal hexane solvents and 86% ethyl acetate solvents, uniformly mixing, adding into a reaction container provided with a condensing device, a dripping device and a temperature monitoring device, taking 7% of the total weight of the initiator azodiisobutyronitrile, dissolving with 2% of the total weight of the ethyl acetate solvents, when the temperature in the reaction container reaches 70 ℃, putting into the reaction container for heat preservation reaction, controlling the stirring speed to 90r/min, taking the heat preservation time to be 5min after reflux occurs at the lower opening of the condenser, taking 7% of the total weight of the initiator AIBN, dissolving with 2% of the total weight of the ethyl acetate solvents, putting into the reactor for heat preservation reaction, and controlling the temperature to be 78-82 ℃, adding 2% of the total weight of an ethyl acetate solvent into 9% of the total weight of AIBN for dissolution, adding the dissolved initiator into the monomer mixture of the residual 42% of acrylic ester soft monomer, hard monomer, functional monomer and crosslinking monomer, uniformly mixing the mixture, dripping the mixture into a reaction container for heat preservation reflux reaction for 60-70 min, controlling the reaction temperature in the reaction container to 85-88 ℃, gradually controlling the stirring speed to 125r/min, keeping the temperature of the dripping acrylate prepolymer for 30min, adding the initiator AIBN 37.5% of the total weight of AIBN and the hard monomer vinyl acetate for mixed dissolution and dripping for 20min, controlling the temperature in the reactor to 85-88 ℃, and keeping the temperature of the dripping acrylate prepolymer for 1h, and then taking an initiator AIBN, wherein 37.5 percent of the total mass of the initiator AIBN is dissolved in 8 percent of the total mass of an ethyl acetate solvent and dropwise added into a reaction container, carrying out heat preservation reaction on the obtained mixture for 2 hours, cooling the obtained mixture to below 40 ℃, adding a toluene solvent, stirring for 30 minutes, stirring at a speed of 170r/min, and discharging.
Further, adding 0.03g of a curing agent and 20g of resin into the obtained polyacrylate pressure-sensitive adhesive polymer, stirring, wherein the resin and the curing agent are uniformly dissolved by ethyl acetate or toluene in advance, coating the polyacrylate pressure-sensitive adhesive obtained after uniform stirring on a PET film, placing the PET film in an electrothermal blowing drying oven at 80 ℃ for curing for 10min, covering and isolating the cured pressure-sensitive adhesive by using release PET, and controlling the thickness of a glue layer to be 20-25 mu m for preparation for testing;
the polyacrylate pressure-sensitive adhesive with high peeling strength prepared in the embodiment 3 of the invention adopts GB 2792-1998 (China) test standard, and the 180-degree peeling strength is 19.4N/25mm; the shear creep retention test method is in accordance with GB/T4851-1998 (China) test standard, the normal temperature holding viscosity is more than 240h, the high temperature creep resistance test at 80 ℃ is more than 72h, and the displacement is 1mm.
Example 4
The polyacrylate pressure-sensitive adhesive with high stripping force is prepared from the following raw materials:
24g of butyl acrylate, 15g of isooctyl acrylate, 2.5g of vinyl acetate, 0.05g of hydroxyethyl acrylate, 1.5g of acrylic acid, 0.3g of azodiisobutyronitrile, 30g of ethyl acetate, 25g of toluene, 2g of n-hexane, 0.03g of aluminum triacetylacetonate curing agent and 24g of terpene resin are weighed.
The polyacrylate pressure-sensitive adhesive with high stripping force comprises the following steps:
mixing the acrylic ester soft monomers, the crosslinking monomers and the functional monomers except the hard monomer vinyl acetate into a monomer mixture, taking 58% of the monomer mixture, taking all normal hexane solvents and 86% ethyl acetate solvents, uniformly mixing, adding into a reaction container provided with a condensing device, a dripping device and a temperature monitoring device, taking 7% of the total weight of the initiator azodiisobutyronitrile, dissolving with 2% of the total weight of the ethyl acetate solvents, when the temperature in the reaction container reaches 70 ℃, putting into the reaction container for heat preservation reaction, controlling the stirring speed to 90r/min, taking the heat preservation time to be 5min after reflux occurs at the lower opening of the condenser, taking 7% of the total weight of the initiator AIBN, dissolving with 2% of the total weight of the ethyl acetate solvents, putting into the reactor for heat preservation reaction, and controlling the temperature to be 78-82 ℃, adding 2% of the total weight of an ethyl acetate solvent into 9% of the total weight of AIBN for dissolution, adding the dissolved initiator into the monomer mixture of the residual 42% of acrylic ester soft monomer, hard monomer, functional monomer and crosslinking monomer, uniformly mixing the mixture, dripping the mixture into a reaction container for heat preservation reflux reaction for 60-70 min, controlling the reaction temperature in the reaction container to 85-88 ℃, gradually controlling the stirring speed to 125r/min, keeping the temperature of the dripping acrylate prepolymer for 30min, adding the initiator AIBN 37.5% of the total weight of AIBN and the hard monomer vinyl acetate for mixed dissolution and dripping for 20min, controlling the temperature in the reactor to 85-88 ℃, and keeping the temperature of the dripping acrylate prepolymer for 1h, and then taking an initiator AIBN, wherein 37.5 percent of the total mass of the initiator AIBN is dissolved in 8 percent of the total mass of an ethyl acetate solvent, dropwise adding the initiator AIBN into a reaction container, carrying out heat preservation reaction on the obtained mixture for 2 hours, cooling the obtained mixture to below 40 ℃, adding a toluene solvent, stirring for 30 minutes, controlling the stirring speed to 170r/min, and discharging.
Further, adding 0.03g of a curing agent and 24g of resin into the obtained polyacrylate pressure-sensitive adhesive polymer, stirring, wherein the resin and the curing agent are uniformly dissolved by ethyl acetate or toluene in advance, coating the polyacrylate pressure-sensitive adhesive obtained after uniform stirring on a PET film, placing the PET film in an electrothermal blowing drying oven at 80 ℃ for curing for 10min, covering and isolating the cured pressure-sensitive adhesive by using release PET, and controlling the thickness of a glue layer to be 20-25 mu m for preparation for testing;
the polyacrylate pressure-sensitive adhesive with high peeling strength prepared in the embodiment 4 of the invention adopts GB 2792-1998 (China) test standard, and the 180-degree peeling strength is 21.5N/25mm; the shear creep retention test method is in accordance with GB/T4851-1998 (China) test standard, the normal temperature holding viscosity is more than 240h, the high temperature creep resistance test at 80 ℃ is more than 72h, and no displacement exists.
Example 5
The polyacrylate pressure-sensitive adhesive with high stripping force is prepared from the following raw materials:
24g of butyl acrylate, 15g of isooctyl acrylate, 2.5g of vinyl acetate, 0.05g of hydroxyethyl acrylate, 1.5g of acrylic acid, 0.3g of azodiisobutyronitrile, 30g of ethyl acetate, 25g of toluene, 2g of n-hexane, 0.03g of aluminum triacetylacetonate curing agent and 28g of terpene resin are weighed.
The polyacrylate pressure-sensitive adhesive with high stripping force comprises the following steps:
mixing the acrylic ester soft monomers, the crosslinking monomers and the functional monomers except the hard monomer vinyl acetate into a monomer mixture, taking 58% of the monomer mixture, taking all normal hexane solvents and 86% ethyl acetate solvents, uniformly mixing, adding into a reaction container provided with a condensing device, a dripping device and a temperature monitoring device, taking 7% of the total weight of the initiator azodiisobutyronitrile, dissolving with 2% of the total weight of the ethyl acetate solvents, when the temperature in the reaction container reaches 70 ℃, putting into the reaction container for heat preservation reaction, controlling the stirring speed to 90r/min, taking the heat preservation time to be 5min after reflux appears at the lower opening of the condenser, taking 7% of the total weight of the initiator AIBN, dissolving with 2% of the total weight of the ethyl acetate solvents, putting into the reactor for heat preservation reaction, controlling the temperature to be 78-82 ℃, adding 2% of the total weight of an ethyl acetate solvent into 9% of the total weight of AIBN for dissolution, adding the dissolved initiator into the monomer mixture of the residual 42% of acrylic ester soft monomer, hard monomer, functional monomer and crosslinking monomer, uniformly mixing the mixture, dripping the mixture into a reaction container for heat preservation reflux reaction for 60-70 min, controlling the reaction temperature in the reaction container to 85-88 ℃, gradually controlling the stirring speed to 125r/min, keeping the temperature of the dripping acrylate prepolymer for 30min, adding the initiator AIBN 37.5% of the total weight of AIBN and the hard monomer vinyl acetate for mixed dissolution and dripping for 20min, controlling the temperature in the reactor to 85-88 ℃, and keeping the temperature of the dripping acrylate prepolymer for 1h, and then taking 37.5% of the total mass of initiator AIBN, dissolving in 8% of the total mass of ethyl acetate solvent, dripping into a reaction container, carrying out heat preservation reaction on the obtained mixture for 2 hours, cooling the obtained mixture to below 40 ℃, adding toluene solvent, stirring for 30 minutes, controlling the stirring speed to 170r/min, and discharging.
Further, adding 0.03g of a curing agent and 28g of resin into the obtained polyacrylate pressure-sensitive adhesive polymer, stirring, wherein the resin and the curing agent are uniformly dissolved by ethyl acetate or toluene in advance, coating the polyacrylate pressure-sensitive adhesive obtained after uniform stirring on a PET film, placing the PET film in an electrothermal blowing drying oven at 80 ℃ for curing for 10min, covering and isolating the cured pressure-sensitive adhesive by using release PET, and controlling the thickness of a glue layer to be 20-25 mu m for preparation for testing;
the polyacrylate pressure-sensitive adhesive with high peeling strength prepared in the embodiment 5 of the invention adopts GB 2792-1998 (China) test standard, and the 180-degree peeling strength is 20.1N/25mm; the shear creep retention test method is in accordance with GB/T4851-1998 (China) test standard, the normal temperature holding viscosity is more than 240h, the high temperature creep resistance test at 80 ℃ is more than 72h, and no displacement exists.
In order to make the technical scheme of the invention better understood by those skilled in the art, the experimental test results of the invention are further described in detail, and comparison of the experimental results obtained by the measurement shows that the content of other components is kept unchanged, the resin dosage has an effect on the peeling strength and cohesive strength of the pressure-sensitive adhesive, and the peeling strength and cohesive strength are obviously improved along with the increase of the resin dosage, but the peeling strength is slightly reduced after the content exceeds 24% in the technical scheme of the invention; obviously, the invention can realize the peeling strength of more than 20N/25mm, the normal-temperature holding viscosity of more than 240h, and the high-temperature holding viscosity test of more than 72h at 80 ℃ without displacement.
While certain preferred embodiments of the present invention have been described above by way of illustration only, it will be understood by those skilled in the art that various modifications may be made to the described embodiments of the invention, or equivalents may be substituted for elements thereof, without departing from the spirit and scope of the invention. Accordingly, the foregoing description of the embodiments of the invention is illustrative in nature and is not to be construed as limiting the scope of the claims.
Claims (8)
1. The polyacrylate pressure-sensitive adhesive with high stripping force is characterized by comprising the following components in parts by weight:
acrylic ester soft monomer 38-42 parts
2-7 parts of hard monomer
1-2 parts of functional monomer
0.04 to 0.08 part of crosslinking monomer
45-60 parts of solvent
Initiator 0.2-0.6 parts
The acrylic ester soft monomer comprises butyl acrylate and isooctyl acrylate;
the hard monomer comprises one or two of vinyl acetate and methyl methacrylate;
the functional monomer comprises one or more of methacrylic acid, acrylic acid and itaconic acid;
the crosslinking monomer comprises one or more of hydroxyethyl acrylate, hydroxypropyl acrylate and N-methylolacrylamide;
the solvent comprises one or more of ethyl acetate, toluene, xylene, benzene, butanone and n-hexane;
the initiator comprises one or two of Azobisisobutyronitrile (AIBN) and dibenzoyl peroxide (BPO);
the polyacrylate pressure sensitive adhesive also comprises a curing agent and a resin;
the curing agent accounts for 0.1-0.9 part of the total weight of the acrylic ester soft monomer, the hard monomer, the functional monomer and the crosslinking monomer, and comprises one or more of epoxy curing agent, aluminum triacetylacetone curing agent and isocyanate curing agent;
the resin accounts for 12-28 parts of the total weight of the acrylic ester soft monomer, the hard monomer, the functional monomer and the crosslinking monomer, and comprises one or more of terpene resin, epoxy resin, phenolic resin and rosin resin.
2. The polyacrylate pressure sensitive adhesive with high stripping force as recited in claim 1, wherein the polyacrylate pressure sensitive adhesive is prepared from the following raw materials in parts by weight:
24-26 parts of butyl acrylate, 15-18 parts of isooctyl acrylate, 2-7 parts of vinyl acetate, 0.04-0.08 part of hydroxyethyl acrylate, 1-2 parts of acrylic acid, 0.2-0.6 part of azobisisobutyronitrile, 25-30 parts of ethyl acetate, 20-30 parts of toluene and 1-5 parts of n-hexane, and 0.1-0.9 part of aluminum triacetate curing agent accounting for the total weight of butyl acrylate, isooctyl acrylate, vinyl acetate, hydroxyethyl acrylate, acrylic acid and Azobisisobutyronitrile (AIBN);
the terpene resin accounts for 12-28 parts of the total weight of butyl acrylate, isooctyl acrylate, vinyl acetate, hydroxyethyl acrylate, acrylic acid and Azodiisobutyronitrile (AIBN).
3. The polyacrylate pressure sensitive adhesive with high peel force according to claims 1-2, wherein the polyacrylate pressure sensitive adhesive has the following preparation steps:
mixing the acrylic ester soft monomers except hard monomer vinyl acetate, the crosslinking monomers and the functional monomers into a monomer mixture, taking 58-62% of the monomer mixture, taking all n-hexane solvents and 80-85% of ethyl acetate solvents, uniformly mixing, adding into a reaction container provided with a condensing device, a stirring device and a dripping device, taking 7-8% of the total weight of the initiator azodiisobutyronitrile, dissolving with 2% of the total weight of the ethyl acetate solvents, and when the temperature in the reaction container reaches 70 ℃, putting into the reaction container for heat preservation reaction and controlling the stirring speed to be 90r/min;
the mixture obtained in the step (1) is subjected to heat preservation, the heat preservation time is 5min after reflux occurs at the lower opening of a condenser, 7-8% of the total weight of an initiator AIBN is taken and dissolved by 2% of the total weight of the ethyl acetate solvent, and the mixture is put into a reactor for heat preservation reaction, and the temperature is controlled at 78-82 ℃;
the acrylic ester prepolymer obtained in the step (2) is subjected to heat preservation reaction for 30min, and 1.5 percent of the total weight of the ethyl acetate solvent is added into 9 percent of the total weight of AIBN for dissolution;
adding the dissolved initiator obtained in the step (3) into the monomer mixture of the residual acrylic ester soft monomer, hard monomer, functional monomer and crosslinking monomer in the step (1), uniformly mixing the mixture, then dripping the mixture into the reaction container of the acrylic ester prepolymer in the step (1), carrying out heat preservation reflux reaction for 60-70 min, controlling the reaction temperature in the reaction container at 85-88 ℃ and gradually controlling the stirring speed at 125r/min;
keeping the temperature of the acrylate prepolymer obtained in the step (4) for 30min, mixing and dissolving 37-38.5% of the total mass of the initiator AIBN and hard monomer vinyl acetate, dripping for 20min, and controlling the temperature in the reactor at 85-88 ℃;
preserving the heat of the acrylate prepolymer obtained after the dripping in the step (5) for 1h, taking an initiator AIBN, wherein 37-38.5% of the total mass of the initiator AIBN is dissolved in 1.5% of the total mass of an ethyl acetate solvent, and dripping the initiator AIBN into a reaction container;
the mixture obtained in the step (6) is subjected to heat preservation reaction for 2 hours;
cooling the mixture obtained in the step (7) to below 40 ℃, adding a toluene solvent, stirring for 30min at a stirring speed of 170r/min, and discharging.
4. The method for preparing the polyacrylate pressure-sensitive adhesive with high stripping force according to claim 3, wherein the polyacrylate pressure-sensitive adhesive obtained in the step (8) is added with a curing agent and resin, the mixture is stirred, the polyacrylate pressure-sensitive adhesive obtained after uniform stirring is coated on a PET film, the PET film is placed in an electrothermal blowing drying oven at 80 ℃ for curing for 10min, the cured pressure-sensitive adhesive is covered and isolated by release PET, and the thickness of a glue layer is controlled to be 20-25 mu m.
5. The method for preparing a polyacrylate pressure sensitive adhesive with high release force according to claim 4, wherein the amount of the curing agent added is 1-9% of the total weight of the acrylate soft monomer, the hard monomer, the crosslinking monomer and the functional monomer.
6. The method for preparing a polyacrylate pressure sensitive adhesive with high release force according to claim 4, wherein the weight of the added resin is 12-28% of the total weight of the soft monomer, the hard monomer, the crosslinking monomer and the functional monomer.
7. The polyacrylate pressure-sensitive adhesive with high stripping force according to claim 3, wherein the temperature of the initiator azodiisobutyronitrile added in the step (1) is 70 ℃ and the initiator AIBN added in the step (2) is added at one time, the initiator AIBN is required to be added dropwise at 78-82 ℃ and is kept for 30min, the initiator AIBN added in the steps (4), (5) and (6) is required to be added dropwise at 85-88 ℃ and the heat-preserving time is 30min, 1h and 2h respectively.
8. The method for preparing a polyacrylate pressure sensitive adhesive with high peel force according to claim 4, wherein the added curing agent is aluminum triacetylacetonate curing agent, the added resin is terpene resin, and the curing agent and the resin are both solvents.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117165228A (en) * | 2023-09-07 | 2023-12-05 | 嘉兴金门量子材料科技有限公司 | High-viscosity aging-resistant non-yellowing pressure-sensitive adhesive and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117165228A (en) * | 2023-09-07 | 2023-12-05 | 嘉兴金门量子材料科技有限公司 | High-viscosity aging-resistant non-yellowing pressure-sensitive adhesive and preparation method and application thereof |
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