CN115197656A - High and low temperature resistant acrylate pressure-sensitive adhesive, and preparation method and application thereof - Google Patents

High and low temperature resistant acrylate pressure-sensitive adhesive, and preparation method and application thereof Download PDF

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Publication number
CN115197656A
CN115197656A CN202210824204.1A CN202210824204A CN115197656A CN 115197656 A CN115197656 A CN 115197656A CN 202210824204 A CN202210824204 A CN 202210824204A CN 115197656 A CN115197656 A CN 115197656A
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China
Prior art keywords
sensitive adhesive
pressure
roller
coating
low temperature
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Chinese (zh)
Inventor
孙靖先
侯莹莹
郭忠成
周仕禄
刘仕民
赵龙
赵夕
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China Tobacco Shandong Industrial Co Ltd
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China Tobacco Shandong Industrial Co Ltd
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Priority to CN202210824204.1A priority Critical patent/CN115197656A/en
Publication of CN115197656A publication Critical patent/CN115197656A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38Pressure-sensitive adhesives [PSA]
    • C09J7/381Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/385Acrylic polymers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05CAPPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C1/00Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating
    • B05C1/04Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length
    • B05C1/08Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line
    • B05C1/0808Details thereof, e.g. surface characteristics
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05CAPPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C1/00Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating
    • B05C1/04Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length
    • B05C1/08Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line
    • B05C1/0826Apparatus in which liquid or other fluent material is applied to the surface of the work by contact with a member carrying the liquid or other fluent material, e.g. a porous member loaded with a liquid to be applied as a coating for applying liquid or other fluent material to work of indefinite length using a roller or other rotating member which contacts the work along a generating line the work being a web or sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05CAPPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C11/00Component parts, details or accessories not specifically provided for in groups B05C1/00 - B05C9/00
    • B05C11/02Apparatus for spreading or distributing liquids or other fluent materials already applied to a surface ; Controlling means therefor; Control of the thickness of a coating by spreading or distributing liquids or other fluent materials already applied to the coated surface
    • B05C11/04Apparatus for spreading or distributing liquids or other fluent materials already applied to a surface ; Controlling means therefor; Control of the thickness of a coating by spreading or distributing liquids or other fluent materials already applied to the coated surface with blades
    • B05C11/048Scrapers, i.e. metering blades having their edge oriented in the upstream direction in order to provide a reverse angle of attack
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05CAPPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C13/00Means for manipulating or holding work, e.g. for separate articles
    • B05C13/02Means for manipulating or holding work, e.g. for separate articles for particular articles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05CAPPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C9/00Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important
    • B05C9/08Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying liquid or other fluent material and performing an auxiliary operation
    • B05C9/14Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying liquid or other fluent material and performing an auxiliary operation the auxiliary operation involving heating or cooling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/02Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
    • B05D3/0254After-treatment
    • B05D3/0263After-treatment with IR heaters
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00Adhesives 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
    • C09J133/02Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00Adhesives 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
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/062Copolymers with monomers not covered by C09J133/06
    • C09J133/064Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
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    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00Adhesives 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
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/08Homopolymers or copolymers of acrylic acid esters
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    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/20Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22Plastics; Metallised plastics
    • C09J7/24Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/241Polyolefin, e.g.rubber
    • C09J7/243Ethylene or propylene polymers
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09J7/00Adhesives in the form of films or foils
    • C09J7/20Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22Plastics; Metallised plastics
    • C09J7/25Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/255Polyesters
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00Investigating materials by mechanical methods
    • G01N19/04Measuring adhesive force between materials, e.g. of sealing tape, of coating
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
    • G01N3/18Performing tests at high or low temperatures
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    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/30Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/302Additional 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
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    • C09J2423/00Presence of polyolefin
    • C09J2423/10Presence of homo or copolymers of propene
    • C09J2423/106Presence of homo or copolymers of propene in the substrate
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    • C09J2433/00Presence of (meth)acrylic polymer
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    • C09J2467/00Presence of polyester
    • C09J2467/006Presence of polyester in the substrate

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  • Chemical & Material Sciences (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention provides a high and low temperature resistant acrylate pressure-sensitive adhesive, a preparation method and application thereof, and belongs to the technical field of adhesives, wherein the preparation method comprises the steps of S1, preparing a pressure-sensitive adhesive solution, mixing solvent raw materials according to a certain mass proportion, then adding an additive, and uniformly stirring; s2, forming the pressure-sensitive adhesive, namely initiating acrylate polymerization, coating a product on a base material by using a preparation device, and attaching a protective film to obtain the pressure-sensitive adhesive; or coating the pressure-sensitive adhesive solution on a base material by using a preparation device, irradiating and reacting for 2 minutes under an LED light source, and then attaching a protective film to obtain the pressure-sensitive adhesive; and S3, testing the pressure-sensitive adhesive, namely cutting off and sampling the obtained pressure-sensitive adhesive tape and testing the use performance of the pressure-sensitive adhesive tape in high and low temperature environments by using a testing system.

Description

High and low temperature resistant acrylate pressure-sensitive adhesive, and preparation method and application thereof
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a high and low temperature resistant acrylate pressure-sensitive adhesive, a preparation method and an application thereof.
Background
The adhesive is widely applied to daily life of people, and provides various conveniences for the life of people. Pressure Sensitive Adhesive (PSA) is an important Adhesive that is very Pressure Sensitive and can be firmly bonded to an adherend by applying only a slight Pressure without the aid of solvents, heat or other means. Since the last century, the research and application of pressure-sensitive adhesives have been rapidly developed and now widely used in various industries. The acrylate pressure-sensitive adhesive is the most widely applied pressure-sensitive adhesive in the current market, is a copolymer of an acrylate monomer and other vinyl monomers, and has the excellent performances of good bonding strength, aging resistance, weather resistance, good transparency, medium resistance, no phase separation, no migration and the like.
The bonding mechanism of the pressure-sensitive adhesive is mainly as follows: the adhesive flows viscously after being applied with external pressure, and can be fully contacted with the surface of the base material, when the pressure-sensitive adhesive has enough wettability to the surface of the base material, molecules between interfaces can be in close contact to generate intermolecular acting force, so that adsorption balance is achieved, and strong adhesion is generated. Therefore, pressure sensitive adhesives must have good viscoelasticity and good wetting to the substrate to produce adequate adhesion. However, at low temperatures, when the temperature is near or below the glass transition temperature (Tg) of the pressure sensitive adhesive, the molecular segment movement of the polymer in the pressure sensitive adhesive is limited and the pressure sensitive adhesive does not contact the substrate sufficiently to cause adhesive failure. At high temperatures, solvents in the pressure sensitive adhesive may volatilize, causing the pressure sensitive adhesive to fail; meanwhile, at high temperature, the molecular chain of the pressure-sensitive adhesive becomes soft and fails to provide sufficient cohesive force, resulting in a decrease in adhesive property.
In recent years, the research on high-temperature resistant or low-temperature resistant pressure-sensitive adhesives has been advanced to some extent, but these preparation methods are generally complicated and cannot simultaneously achieve high and low temperature resistance. Therefore, it is of great importance to develop a novel pressure-sensitive adhesive which can be applied in high and low temperature environments.
Disclosure of Invention
The embodiment of the invention provides a high and low temperature resistant acrylate pressure-sensitive adhesive, a preparation method and application thereof.
In view of the above problems, the technical solution proposed by the present invention is:
the invention provides a preparation method of high and low temperature resistant acrylate pressure-sensitive adhesive, which comprises the following steps:
s1, preparing a pressure-sensitive adhesive solution, mixing solvent raw materials according to a certain mass ratio, adding an additive, and uniformly stirring;
s2, forming the pressure-sensitive adhesive, namely initiating acrylate polymerization, coating a product on a base material by using a preparation device, and attaching a protective film to obtain the pressure-sensitive adhesive; or coating the pressure-sensitive adhesive solution on a base material by using a preparation device, irradiating and reacting for 2 minutes under an LED light source, and then attaching a protective film to obtain the pressure-sensitive adhesive;
and S3, testing the pressure-sensitive adhesive, namely cutting off and sampling the obtained pressure-sensitive adhesive tape and testing the service performance of the pressure-sensitive adhesive tape in high and low temperature environments by using a testing system.
As a preferred embodiment of the present invention, in the step S1, the solvent raw material includes at least one of an ionic liquid, a viscous monomer, a cohesive monomer, and a functional monomer, the additive includes at least one of a cross-linking agent, an emulsifier, and an initiator, the ionic liquid may be added as a solvent to the acrylate, or may be copolymerized with the acrylate as a comonomer, and the ionic liquid may be added before, during, and after the acrylate is polymerized.
In a preferred embodiment of the present invention, in step S1, the mixed solution is added into a four-neck flask, and is mechanically stirred, and the stirring speed, the mixing time and the mixing temperature are controlled, and the initiator is added dropwise, and the reaction temperature and the reaction time are controlled.
As a preferred technical scheme of the invention, nitrogen can be introduced after the mixed solution is added into the four-neck flask.
As a preferable embodiment of the present invention, in the step S1, the substrate includes one of a BOPP film and a PET film.
As a preferable technical scheme of the invention, the preparation device comprises a substrate roller, a coating tank, a drying box and a material collecting roller, the coating groove is filled with the prepared pressure-sensitive adhesive solution, the top of one side of the coating groove, which is close to the substrate roller, is provided with a material guide roller, a coating roller is arranged in the coating groove, two ends of a central shaft of the coating roller are rotationally connected with the inner wall of the coating groove, hairbrushes are locally and uniformly distributed on the outer surface of the coating roller, a scraping component is arranged on one side of the coating groove far away from the material guide roller, the drying box is arranged on one side of the coating groove, the bottom of the drying box is provided with a base, at least five LED lamp tubes are arranged inside the drying box, a protective film roller is arranged below the drying box, a fixed roller is arranged on one side of the drying box close to the outlet, fixed brackets are arranged at two ends of a central shaft of the fixed roller, one end of the fixed bracket is fixedly connected with the outer wall of the drying box, an adjusting roller is arranged below the fixed roller, the adjusting roller and the fixed roller are arranged in parallel, the material receiving roller is arranged on one side of the drying box close to the adjusting roller, a material receiving motor is arranged at one end of the central shaft of the material receiving roller, the output end of the material receiving motor is fixedly connected with the central shaft of the material receiving roller, the outer surface of the base material roller is provided with a base material belt, the end parts of the base material belt are sequentially wound on the outer surfaces of the guide roller, the coating roller and the fixing roller, the surface of protection membrane roller is provided with the protection film material area, the protection film material area around locating behind the surface of adjusting roller with the laminating of base material area forms the pressure-sensitive adhesive material area, the pressure-sensitive adhesive material area is final around locating receive the surface of material roller.
As a preferred technical solution of the present invention, the brush is in contact with a lower surface of the base material strip, and is configured to brush the pressure-sensitive adhesive solution in the coating groove onto the base material strip, the scraping assembly is disposed below the base material strip, the scraping assembly includes a scraper, an adjusting rod, and a fastening bolt, the scraper is in a "T" shape, a top of one end of the scraper, which is close to the coating roller, is obliquely disposed, a tip end of the scraper is in contact with the lower surface of the base material strip, a bottom of the adjusting rod is fixedly connected to a top of the coating groove, one end of the scraper is sleeved on the adjusting rod, the fastening bolt is in threaded fit with an end of the scraper, one end of the fastening bolt penetrates through the scraper and abuts against an outer surface of the adjusting rod, the LED tube is disposed on one side of the base material strip coated with the pressure-sensitive adhesive solution, the fixing bracket is provided with an adjusting groove, two ends of a central shaft of the adjusting roller are disposed inside the adjusting grooves on two sides, the adjusting roller is rotatably connected to a central shaft of the adjusting roller, the adjusting bolt is disposed below the fixing bracket, and an end of the adjusting bolt extends to the adjusting groove and abuts against a central shaft of the adjusting roller.
As a preferred technical scheme of the invention, the test system comprises a high-temperature test module and a low-temperature test module which are respectively used for placing the obtained pressure-sensitive adhesive in high-temperature and low-temperature environments for performance test, each of the high-temperature test module and the low-temperature test module is internally provided with a bonding tool, a temperature control unit, a stretching unit, an identification unit and a calculation unit, the temperature control unit, the stretching unit and the identification unit are electrically connected with the calculation unit, the bonding tool is used for fixing the pressure-sensitive adhesive and a test medium, the temperature control unit comprises a temperature sensor and a temperature regulator and is used for controlling the environment temperature in the test system, the stretching unit comprises a stretching motor and a tension sensor and is used for simulating the stretching use limit of the pressure-sensitive adhesive, the identification unit judges the bonding area of the pressure-sensitive adhesive and the start-stop time of the pressure-sensitive adhesive and an adherend damage, and the calculation unit is used for calculating the bonding strength of the pressure-sensitive adhesive by combining the bonding area, the bonding time and the tension value.
On the other hand, the invention provides the acrylate pressure-sensitive adhesive obtained by the preparation method and application of the acrylate pressure-sensitive adhesive in high and low temperature environments.
Compared with the prior art, the invention has the beneficial effects that: the acrylate pressure-sensitive adhesive with low glass transition temperature and high heat resistance is prepared by using the ionic liquid as a raw material, the pressure-sensitive adhesive has excellent high and low temperature resistance, the preparation method is convenient to apply, the device is simple in structure, the production cost is easy to control, and the obtained acrylate pressure-sensitive adhesive is good in service performance.
The above description is only an overview of the technical solutions of the present invention, and the present invention can be implemented in accordance with the content of the description so as to make the technical means of the present invention more clearly understood, and the above and other objects, features, and advantages of the present invention will be more clearly understood.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of high and low temperature resistant acrylate pressure-sensitive adhesive disclosed by the invention;
FIG. 2 is a schematic view of a manufacturing apparatus according to the present disclosure;
FIG. 3 is an enlarged view at A in FIG. 2;
FIG. 4 is an enlarged view at B in FIG. 2;
FIG. 5 is a block diagram of the test system disclosed herein;
description of reference numerals: 100. a substrate roll; 101. a strip of base material; 200. a coating tank; 201. a material guide roller; 202. a coating roller; 2021. a brush; 203. a scraping component; 2031. a scraper; 2032. adjusting a rod; 2033. fastening a bolt; 300. a drying box; 301. a base; 302. an LED lamp tube; 303. a protective film roll; 3031. protecting the film material belt; 304. a fixed roller; 3041. a fixed bracket; 3042. an adjustment groove; 3043. adjusting the bolt; 305. a regulating roller; 400. a material receiving roller; 401. a pressure-sensitive adhesive tape; 402. a material receiving motor; 10. a high temperature test module; 20. a low temperature test module; 30. bonding the tool; 40. a temperature control unit; 50. a stretching unit; 60. an identification unit; 70. and a computing unit.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without inventive efforts based on the embodiments of the present invention, are within the scope of protection of the present invention.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without inventive efforts based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example one
Referring to the attached figure 1, the invention provides a technical scheme: a process for preparing the high-and low-temp resistant acrylate pressure-sensitive adhesive features that the ionic liquid is 1-butyl-3-methylimidazolium bistrifluoromethyliminate ([ BMIM)]NTF 2 ) The adhesive monomer is Butyl Acrylate (BA) and isooctyl acrylate (EHA), the cross-linking agent is polyethylene glycol diacrylate (PEGDA), and the initiator is a photoinitiator 1173, and the method comprises the following steps:
s1, 1-butyl-3-methylimidazolium bistrifluoromethyliminium salt ([ BMIM ]]NTF 2 ) Mixing Butyl Acrylate (BA) and isooctyl acrylate (EHA) according to the mass ratio of 50;
s2, coating the obtained solution on a BOPP film by using a preparation device, irradiating and reacting for 2 minutes under a 365nm LED light source, and attaching a protective film to obtain the pressure-sensitive adhesive;
s3, using a test system to obtain the pressure-sensitive adhesive, wherein the glass transition temperature of the pressure-sensitive adhesive is-68 ℃, the thermal decomposition temperature of the pressure-sensitive adhesive is 350 ℃, the pressure-sensitive adhesive has good adhesion, the adhesion tensile shear strength on glass at-40 ℃ is 35kPa, and the adhesion tensile shear strength on glass at 80 ℃ is 31kPa.
In the embodiment of the invention, the ionic liquid can be used as a solvent to be added into the acrylate, and can also be used as a comonomer to be copolymerized with the acrylate, and the ionic liquid can be added before the polymerization of the acrylate and after the polymerization and the polymerization.
Example two
The invention provides a technical scheme that: a preparation method of high and low temperature resistant acrylate pressure-sensitive adhesive selects 1-butyl-3-methylimidazole chloride ([ BMIM ] Cl) as ionic liquid, ethyl Acrylate (EA) as viscous monomer, methyl Acrylate (MA) as hard monomer, acrylic Acid (AA) as functional monomer, 1, 6-hexanediol diacrylate (HDDA) as cross-linking agent and photo-initiator 1173 as initiator, and comprises the following steps:
s1, mixing 1-butyl-3-methylimidazolium chloride ([ BMIM ] Cl), ethyl Acrylate (EA), methyl Acrylate (MA) and Acrylic Acid (AA) in a mass ratio of 50;
s2, coating the obtained solution on a BOPP film by using a preparation device, irradiating and reacting for 2 minutes under a 365nm LED light source, and attaching a protective film to obtain a pressure-sensitive adhesive;
s3, the glass transition temperature of the pressure-sensitive adhesive is-70 ℃, the thermal decomposition temperature is 300 ℃, the pressure-sensitive adhesive has good adhesion, the adhesion tensile shear strength on glass at-40 ℃ is 29kPa, and the adhesion tensile shear strength on glass at 80 ℃ is 25kPa.
EXAMPLE III
The invention provides a technical scheme that: a preparation method of high and low temperature resistant acrylate pressure-sensitive adhesive selects 1-vinyl-3-butylimidazole tetrafluoroborate ([ VBIm) as ionic liquid]BF 4 ) And 1-methyl-3-ethylimidazole tetrafluoroborate ([ EMIM ]]BF 4 ) The preparation method comprises the following steps of (1) preparing a high-performance adhesive, wherein the adhesive monomer is Ethyl Acrylate (EA), the functional monomer is Acrylic Acid (AA), the crosslinking agent is 1, 6-hexanediol diacrylate (HDDA), and the initiator is a photoinitiator 1173:
s1, 1-vinyl-3-butylimidazolium tetrafluoroborate ([ VBIm)]BF 4 ) 1-methyl-3-ethylimidazole tetrafluoroborate ([ EMIM ]]BF 4 ) Mixing Ethyl Acrylate (EA) and Acrylic Acid (AA) according to the mass ratio of 30;
s2, coating the obtained solution on a PET film by using a preparation device, irradiating and reacting for 2 minutes under a 365nm LED light source, and attaching a protective film to obtain the pressure-sensitive adhesive;
s3, the glass transition temperature of the pressure-sensitive adhesive is-70 ℃, the thermal decomposition temperature of the pressure-sensitive adhesive is 300 ℃, the pressure-sensitive adhesive has good adhesion, the adhesion tensile shear strength on glass at-40 ℃ is 26kPa, and the adhesion tensile shear strength on glass at 80 ℃ is 24kPa.
Example four
The invention provides a technical scheme that: a method for preparing high and low temperature resistant acrylate pressure-sensitive adhesive selects 1-butyl-3-methylimidazolium hexafluorophosphate ([ BMIM ] as ionic liquid]PF 6 ) The adhesive monomer is dodecyl acrylate (LA) and Butyl Acrylate (BA), the hard monomer is octadecyl acrylate (SA), the functional monomer is Acrylic Acid (AA), the cross-linking agent is polyethylene glycol diacrylate (PEGDA), and the initiator is dibenzoyl peroxide (BPO), which comprises the following steps:
s1, dodecyl acrylate (LA), butyl Acrylate (BA), octadecyl acrylate (SA) and Acrylic Acid (AA) are mixed according to the mass ratio of 50]PF 6 ) Mixing according to the mass ratio of 50;
s2, coating the obtained solution on a PET film by using a preparation device, and attaching a protective film to obtain a pressure-sensitive adhesive;
s3, the glass transition temperature of the pressure-sensitive adhesive is-70 ℃, the thermal decomposition temperature of the pressure-sensitive adhesive is 300 ℃, the pressure-sensitive adhesive has good adhesion, the adhesion tensile shear strength on glass at-40 ℃ is 32kPa, and the adhesion tensile shear strength on glass at 80 ℃ is 28kPa.
EXAMPLE five
The invention provides a technical scheme that: a method for preparing high and low temperature resistant acrylate pressure sensitive adhesive selects 1-ethyl-3-methylimidazolium bistrifluoromethyliminate ([ EMIM ") as ionic liquid]NTF 2 ) The adhesive monomer is Butyl Acrylate (BA) and isooctyl acrylate (EHA), and the functional monomer isAcrylic Acid (AA) and Methyl Methacrylate (MMA), a crosslinking agent is polyethylene glycol diacrylate (PEGDA), an emulsifier is allyloxy fatty alcohol, an initiator is Azobisisobutyronitrile (AIBN), and the method comprises the following steps:
s1, 1-ethyl-3-methylimidazolium bistrifluoromethylimine salt ([ EMIM)]NTF 2 ) Butyl Acrylate (BA), isooctyl acrylate (EHA), acrylic Acid (AA) and Methyl Methacrylate (MMA) were mixed at a mass ratio of 30;
s2, coating the obtained solution on a PET film by using a preparation device, and attaching a protective film to obtain a pressure-sensitive adhesive;
and S3, using a test system to obtain the pressure-sensitive adhesive, wherein the glass transition temperature of the pressure-sensitive adhesive is-70 ℃, the thermal decomposition temperature of the pressure-sensitive adhesive is 350 ℃, the pressure-sensitive adhesive has good adhesion, the adhesive tensile shear strength on glass at-40 ℃ is 27kPa, and the adhesive tensile shear strength on glass at-80 ℃ is 25kPa.
EXAMPLE six
Referring to fig. 2-4, the present invention provides a technical solution: a preparation method of high and low temperature resistant acrylate pressure-sensitive adhesive is applied to a preparation device in first to fifth embodiments and comprises a substrate roller 100, a coating tank 200, a drying box 300 and a material receiving roller 400, wherein a prepared pressure-sensitive adhesive solution is filled in the coating tank 200 and is automatically filled according to the liquid level change in the coating tank 200 in the preparation process to ensure that the volume of the solution in the tank meets the production requirement, a material guide roller 201 is arranged at the top of one side, close to the substrate roller 100, of the coating tank 200, a coating roller 202 is arranged in the coating tank 200, two ends of a central shaft of the coating roller 202 are rotatably connected with the inner wall of the coating tank 200, brushes 2021 are uniformly distributed on the outer surface of the coating roller 202, the brushes 2021 on the surface continuously take up the solution in the coating tank 200 in the rotation process of the coating roller 202, and a material scraping assembly 203 is arranged at one side, far away from the material guide roller 201, of the coating tank 200, the scraping component 203 is arranged at the rear side of the movement direction of the coating roller 202, the drying box 300 is arranged at one side of the coating groove 200, the bottom of the drying box 300 is provided with a base 301, the drying box 300 is used for drying and forming after solution coating, the base 301 plays a supporting role, the inlet and outlet height of the drying box 300 is matched with the movement height of the material belt, the arrangement of a material belt steering shaft is reduced, the transmission error is reduced, at least five LED lamp tubes 302 are arranged inside the drying box 300, the input end of the LED lamp tubes 302 is connected with a controller, the wavelength and the operation time of the LED lamp tubes 302 can be adjusted through the controller, the protective film roller 303 is arranged below the drying box 300, the side of the drying box 300 close to the outlet is provided with a fixed roller 304, two ends of the central shaft of the fixed roller 304 are provided with fixed supports 3041, one end of the fixed supports 3041 is fixedly connected with the outer wall of the drying box 300, the fixed roller 304 is used for material pressing, and the material belt is prevented from jumping caused by tension influence in the movement process, an adjusting roller 305 is arranged below the fixed roller 304, the adjusting roller 305 is arranged in parallel with the fixed roller 304, the adjusting roller 305 is movably arranged and can control the distance between the adjusting roller 305 and a fixed pipe, the material receiving roller 400 is arranged on one side of the drying box 300 close to the adjusting roller 305, one end of the central shaft of the material receiving roller 400 is provided with a material receiving motor 402, the output end of the material receiving motor 402 is fixedly connected with the central shaft of the material receiving roller 400, the material receiving motor 402 provides power for the operation of the device, the central shaft of the material receiving roller 400 is also provided with an angular velocity sensor (not shown in the figure) which is used for detecting the rotation speed of the material receiving roller 400, the output end of the angular velocity sensor is connected with a controller, the controller controls the operation frequency of the material receiving motor 402 through calculation to ensure the uniform coating of the solution and the drying irradiation time, the outer surface of the substrate roller 100 is provided with a base material belt 101, the end part of the base material belt 101 is sequentially wound on the outer surfaces of the guide roller 201, the coating roller 202 and the fixing roller 304, the base material belt 101 enters a coating operation area after being guided by the guide roller 201, the base material belt 101 is kept straight by the guide roller, the guide roller 201, the coating roller 202 and the fixing roller 304 rotate along with the operation of the base material belt 101, the process of coating the base material belt 101 with the pressure-sensitive adhesive is smooth, the outer surface of the protective film roller 303 is provided with a protective film material belt 3031, the protective film 3031 is wound on the outer surface of the adjusting roller 305 and then is attached to the base material belt 101 to form a pressure-sensitive adhesive material belt 401, the pressure-sensitive adhesive material belt 401 is finally wound on the outer surface of the receiving roller 400, the surface of the protective film 3031 attached to the base material belt 101 has high smoothness, and the pressure-sensitive adhesive material belt 401 can be conveniently torn off in use;
the brush 2021 is in contact with the lower surface of the base material belt 101, and is used for brushing the pressure-sensitive adhesive solution in the coating groove 200 onto the base material belt 101, the scraping component 203 is disposed below the base material belt 101, the scraping component 203 includes a scraper 2031, an adjusting rod 2032, and a fastening bolt 2033, the scraper 2031 is in a "T" type structure, the top of one end of the scraper 2031 close to the coating roller 202 is disposed in an inclined manner, the sharp corner end of the scraper 2031 is in contact with the lower surface of the base material belt 101, the scraper 2031 evenly smears the pressure-sensitive adhesive solution coated on the base material belt 101, and enables the redundant solution to automatically flow back into the coating groove 200, thereby improving the molding quality of the pressure-sensitive adhesive belt 401 and avoiding production waste, the bottom of the adjusting rod 2032 is fixedly connected to the top of the coating groove 200, one end of the scraper 2031 is sleeved on the adjusting rod 2032, the fastening bolt 2033 is in threaded fit with the end of the scraper 2031, one end of the fastening bolt 2033 is in contact with the outer surface of the adjusting rod 2032 after penetrating through the scraper 2031, the fastening bolt 2033 is abutted against the adjusting rod 2032 for adjusting the height, so that the gap between the scraper 2031 and the base material belt 101 is changed, the thickness of the solution coated on the base material belt 101 is different, the adjustability is strong, the operation is simple, and the preparation requirements of the pressure sensitive adhesive tapes 401 with different specifications are met, the LED lamp tube 302 is arranged at one side of the base material belt 101 coated with the pressure sensitive adhesive solution, so that the ultraviolet light emitted by the LED can play a role to the maximum extent, and the pressure sensitive adhesive can be more quickly formed, the fixing support 3041 is provided with the adjusting groove 3042, both ends of the central shaft of the adjusting roller 305 are respectively arranged inside the adjusting grooves 3042 at both sides, the adjusting roller 305 is rotatably connected with the central shaft, the adjusting bolt 3043 is arranged below the fixing support 3041, the end of the adjusting bolt 3043 is abutted against the central shaft of the adjusting roller 305 after extending to the inside of the adjusting groove 3042, and the adjusting roller 305 is extruded between the adjusting roller 305 and the fixing roller 304, the protective film tape 3031 is quickly adhered to the side of the base material tape 101 coated with the pressure-sensitive adhesive solution, so that the pressure-sensitive adhesive tape 401 is convenient to use and transport.
Specifically, the working principle of the preparation device is as follows: the base material belt 101 on the outer surface of the base material roller 100 is in contact with the brush 2021 on the outer surface of the coating roller 202 under the guiding action of the material guiding roller 201, the brush 2021 rubs against the base material belt 101, so that the coating roller 202 rotates, in the rotating process, the brush 2021 is immersed in the pressure sensitive adhesive solution to lift the solution and coat the solution on the lower surface of the base material belt 101, the base material belt 101 continues to advance, the coated solution is leveled by the scraper 2031 and enters the drying box 300, the LED lamp tube 302 emits ultraviolet light to initiate acrylate photopolymerization, so that the acrylate photopolymerization is integrated with the base material belt 101, at the outlet of the drying box 300, the protective film material belt 3031 wound on the outer surface of the adjusting roller 305 is adhered to the side of the base material belt 101 coated with the pressure sensitive adhesive by the extruding of the adjusting roller 305 and the fixing roller 304, and the pressure sensitive adhesive material belt 401 is formed and then is collected in a roll by the collecting roller 400.
EXAMPLE seven
Referring to fig. 5, the present invention provides a technical solution: a preparation method of high and low temperature resistant acrylate pressure-sensitive adhesive is applied to a test system in first to fifth embodiments and comprises a high temperature test module 10 and a low temperature test module 20 which are respectively used for placing the obtained pressure-sensitive adhesive in high and low temperature environments for performance test, wherein a bonding tool 30, a temperature control unit 40, a stretching unit 50, an identification unit 60 and a calculation unit 70 are arranged in each of the high temperature test module 10 and the low temperature test module 20, the temperature control unit 40, the stretching unit 50 and the identification unit 60 are electrically connected with the calculation unit 70, the bonding tool 30 is used for fixing the pressure-sensitive adhesive and a test medium, in the above embodiments, the test medium is glass, the temperature control unit 40 comprises a temperature sensor and a temperature regulator and is used for controlling the environment temperature in the test system so as to meet test conditions, the stretching unit 50 comprises a stretching motor and a tension sensor and is used for simulating the stretching use limit of the pressure-sensitive adhesive, the identification unit 60 judges the bonding area of the pressure-sensitive adhesive and the breaking starting and stopping time of the pressure-sensitive adhesive and an adherend based on an image recognition technology, and a high-precision industrial camera is used for acquiring the change of the molecular chain bonding area of the pressure-sensitive adhesive in the stretching state, and calculating the bonding strength value of the bonding unit 70.
Example eight
The present example shows the acrylate pressure-sensitive adhesive obtained by the preparation method of any one of examples one to seven and its application in high and low temperature environments.
It should be understood that the specific order or hierarchy of steps in the processes disclosed is an example of exemplary approaches. Based upon design preferences, it is understood that the specific order or hierarchy of steps in the processes may be rearranged without departing from the scope of the present disclosure. The accompanying method claims present elements of the various steps in a sample order, and are not intended to be limited to the specific order or hierarchy presented.
In the foregoing detailed description, various features are grouped together in a single embodiment for the purpose of streamlining the disclosure. This method of disclosure is not to be interpreted as reflecting an intention that the claimed embodiments of the subject matter require more features than are expressly recited in each claim. Rather, as the following claims reflect, invention lies in less than all features of a single disclosed embodiment. Thus, the following claims are hereby expressly incorporated into the detailed description, with each claim standing on its own as a separate preferred embodiment of the invention.

Claims (9)

1. The preparation method of the high and low temperature resistant acrylate pressure-sensitive adhesive is characterized by comprising the following steps:
s1, preparing a pressure-sensitive adhesive solution, mixing solvent raw materials according to a certain mass ratio, adding an additive, and uniformly stirring;
s2, pressure-sensitive adhesive molding, namely initiating acrylate polymerization, coating a product on a base material by using a preparation device, and attaching a protective film to obtain the pressure-sensitive adhesive; or coating the pressure-sensitive adhesive solution on a base material by using a preparation device, irradiating and reacting for 2 minutes under an LED light source, and then attaching a protective film to obtain the pressure-sensitive adhesive;
s3, testing the pressure-sensitive adhesive, namely cutting off and sampling the obtained pressure-sensitive adhesive tape and testing the service performance of the pressure-sensitive adhesive tape in high and low temperature environments by using a testing system;
wherein, the preparation device comprises a substrate roller, a coating groove, a drying box and a material collecting roller, the coating groove is filled with a pressure-sensitive adhesive solution which is prepared, the top of one side of the coating groove close to the substrate roller is provided with a material guide roller, the coating groove is internally provided with the coating roller, the two ends of a central shaft of the coating roller are rotationally connected with the inner wall of the coating groove, the outer surface of the coating roller is locally and uniformly distributed with hairbrushes, one side of the coating groove far away from the material guide roller is provided with a material scraping component, the drying box is arranged at one side of the coating groove, the bottom of the drying box is provided with a base, the drying box is internally provided with at least five LED lamp tubes, a protective film roller is arranged below the drying box, one side of the drying box close to an outlet is provided with a fixed roller, and the two ends of the central shaft of the fixed roller are provided with fixed brackets, the one end of fixed bolster with the outer wall fixed connection of stoving case, the below of fixed roll is provided with the dancer roll, the dancer roll with fixed roll parallel arrangement, receive the material roller set up in the stoving case is close to one side of dancer roll, the center pin one end of receiving the material roller is provided with receives the material motor, receive the output of material motor with the center pin fixed connection of receiving the material roller, the surface of substrate roller is provided with the base material area, the tip of base material area is around locating in proper order the guide roller the coating roller with the surface of fixed roll, the surface of protective film roller is provided with the protection film material area, the protection film material area around locating behind the surface of dancer roll with the laminating of base material area forms the pressure-sensitive adhesive tape area, the pressure-sensitive adhesive tape is finally around locating the surface of receiving the material roller.
2. The method for preparing the high and low temperature resistant acrylate pressure sensitive adhesive according to claim 1, wherein in step S1, the solvent raw material comprises at least one of an ionic liquid, a viscous monomer, a cohesive monomer and a functional monomer, the additive comprises at least one of a cross-linking agent, an emulsifier and an initiator, the ionic liquid can be used as a solvent to be added to the acrylate or can be used as a comonomer to be copolymerized with the acrylate, and the ionic liquid can be added before, during and after the acrylate is polymerized.
3. The method for preparing the high and low temperature resistant acrylate pressure sensitive adhesive according to claim 1, wherein in the step S1, the mixed solution is added into a four-necked flask, mechanical stirring is adopted, the stirring speed, the mixing time and the mixing temperature are controlled, and the initiator is added dropwise, and the reaction temperature and the reaction time are controlled.
4. The method for preparing the high and low temperature resistant acrylate pressure sensitive adhesive according to claim 3, wherein nitrogen is introduced into the four-neck flask after the mixed solution is added.
5. The method of claim 1, wherein in step S1, the substrate comprises one of a BOPP film or a PET film.
6. The method according to claim 1, wherein the brush is in contact with a lower surface of the base material strip for brushing the pressure-sensitive adhesive solution in the coating groove onto the base material strip, the scraping assembly is disposed below the base material strip and includes a scraper having a T-shaped structure, an adjusting rod and a fastening bolt, the scraper is disposed at an inclined position near a top of the coating roller, a pointed end of the scraper is in contact with the lower surface of the base material strip, a bottom of the adjusting rod is fixedly connected to a top of the coating groove, an end of the scraper is sleeved on the adjusting rod, the fastening bolt is in threaded engagement with an end of the scraper, an end of the fastening bolt penetrates through the scraper and then abuts against an outer surface of the adjusting rod, the LED lamp tube is disposed on a side of the base material strip coated with the pressure-sensitive adhesive solution, the fixing bracket is provided with the adjusting groove, two ends of a central shaft of the adjusting roller are disposed on two sides of the adjusting groove, the adjusting roller is rotatably connected with the central shaft of the adjusting roller, the fixing bracket is provided with the adjusting bolt, and the adjusting bolt is disposed below the fixing bracket and extends to the adjusting groove.
7. The method for preparing the high and low temperature resistant acrylate pressure-sensitive adhesive according to claim 1, wherein the testing system comprises a high temperature testing module and a low temperature testing module, the high temperature testing module and the low temperature testing module are respectively used for placing the obtained pressure-sensitive adhesive in high and low temperature environments for performance testing, each of the high temperature testing module and the low temperature testing module is provided with a bonding tool, a temperature control unit, a stretching unit, an identification unit and a calculating unit, the temperature control unit, the stretching unit and the identification unit are electrically connected with the calculating unit, the bonding tool is used for fixing the pressure-sensitive adhesive and a testing medium, the temperature control unit comprises a temperature sensor and a temperature regulator and is used for controlling the environment temperature in the testing system, the stretching unit comprises a stretching motor and a tension sensor and is used for simulating the stretching use limit of the pressure-sensitive adhesive, the identification unit judges the bonding area of the pressure-sensitive adhesive and the start and stop time when the pressure-sensitive adhesive and an adherend are damaged based on an image recognition technology, and the calculating unit is used for calculating the bonding area, time and the tension value to obtain the bonding strength of the pressure-sensitive adhesive.
8. An acrylate pressure-sensitive adhesive obtained by the production method according to any one of claims 1 to 7.
9. Use of the acrylate pressure sensitive adhesive of claim 8 in high and low temperature environments.
CN202210824204.1A 2022-07-14 2022-07-14 High and low temperature resistant acrylate pressure-sensitive adhesive, and preparation method and application thereof Pending CN115197656A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101802830B1 (en) * 2017-06-29 2017-11-29 김운곤 Preparation Method of Protective Films for Display Devices
CN110643300A (en) * 2019-09-27 2020-01-03 南京五人光学薄膜有限公司 Optical temperature-resistant ultraviolet visbreaking film
CN114350270A (en) * 2022-02-23 2022-04-15 广东华丽宝实业有限公司 Preparation method and preparation equipment of pressure-sensitive adhesive PE protective film

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101802830B1 (en) * 2017-06-29 2017-11-29 김운곤 Preparation Method of Protective Films for Display Devices
CN110643300A (en) * 2019-09-27 2020-01-03 南京五人光学薄膜有限公司 Optical temperature-resistant ultraviolet visbreaking film
CN114350270A (en) * 2022-02-23 2022-04-15 广东华丽宝实业有限公司 Preparation method and preparation equipment of pressure-sensitive adhesive PE protective film

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