CN110734711A - Pressure-sensitive adhesive for polarizer protective film and preparation method thereof - Google Patents

Pressure-sensitive adhesive for polarizer protective film and preparation method thereof Download PDF

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Publication number
CN110734711A
CN110734711A CN201910881930.5A CN201910881930A CN110734711A CN 110734711 A CN110734711 A CN 110734711A CN 201910881930 A CN201910881930 A CN 201910881930A CN 110734711 A CN110734711 A CN 110734711A
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pressure
sensitive adhesive
protective film
solvent
parts
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CN110734711B (en
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唐承明
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Guangdong Dongli New Materials Polytron Technologies Inc
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Guangdong Dongli New Materials Polytron Technologies Inc
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38—Pressure-sensitive adhesives [PSA]
    • C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/385—Acrylic polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04—Homopolymers or copolymers of esters
    • C09J133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/255—Polyesters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2433/00—Presence of (meth)acrylic polymer
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2467/00—Presence of polyester
    • C09J2467/006—Presence of polyester in the substrate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Polarising Elements (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses pressure-sensitive adhesives for polarizer protective films, which belong to the technical field of pressure-sensitive adhesives and are prepared from the following raw materials, by weight, 31-35 parts of soft monomers, 6-8 parts of functional monomers, 0.15-0.35 part of initiators, 57-63 parts of solvents and 2-4 parts of curing agents.

Description

Pressure-sensitive adhesive for polarizer protective film and preparation method thereof
Technical Field
The invention belongs to the technical field of pressure-sensitive adhesives, and particularly relates to pressure-sensitive adhesives for polarizer protective films and a preparation method thereof.
Background
The polaroid is widely applied to consumer and industrial electronic display screen panels, such as mobile phones, computers, liquid crystal televisions, automotive electronics, medical instruments, instruments and meters and the like, and other application scenes also comprise sunglasses, anti-dazzle goggles, filter lenses of photographic equipment, light quantity controllers and the like, under the double drive of continuous increase of market demand and continuous expansion of screen area of consumer electronic terminals (televisions, tablet computers, smart phones and the like), the global display panel industry continuously and stably develops, and is expected to reach 5 hundred million square meters in 2019, wherein the large-size TFT-LCD contributes more than 80 percent of demand, the polaroid is an indispensable component for TFT-LCD imaging, and according to prediction, the global productivity of the polaroid is expected to reach 7.28 hundred million square meters in 2019, so the special shipment protective film for the polaroid is not less than 7.3 hundred million square meters per year, and the economic value is 30-40 yuan per year.
The polaroid is subjected to surface treatment, so that the liquid crystal panel is endowed with higher definition, and the functions of reflection resistance, pollution resistance, scratch resistance and the like are achieved. Before the surface treatment process, the surface of the polaroid cannot be polluted by any chemical pollution, the change of the surface energy of the polaroid can seriously influence the treatment effect, and great material waste is caused.
As a protective film for a polarizer, it is necessary to have excellent chemical stability and to ensure that its influence on the surface energy of the polarizer is within 2 dynes. In addition, the protective film has good fitting performance, and automatic bubble discharge can be realized during operation; the protective film is also highly transparent, which facilitates optical inspection of the quality of the polarizer, and the protective film needs to have antistatic properties to prevent dust contamination.
The invention aims to develop pressure-sensitive adhesives for the shipment protective film of the polaroid, which have extremely low surface energy influence on the surface of the polaroid, and have broad market prospect and high economic value.
Disclosure of Invention
The invention mainly aims to overcome the defects that the existing acrylate pressure-sensitive adhesive is easy to remain adhesive, is easy to precipitate, cannot resist high temperature and the like, and pressure-sensitive adhesives for the shipment protective film of the polaroid are developed.
In order to solve the problems, the adopted technical scheme is as follows:
pressure-sensitive adhesive for polarizer protective film is prepared from (by weight parts) soft monomer 31-35, functional monomer 6-8, initiator 0.15-0.35, solvent 57-63, and curing agent 2-4.
Preferably, the soft monomer is butyl acrylate and/or isooctyl acrylate.
preferably, the soft monomer is composed of 80-90 wt% butyl acrylate and 10-20 wt% isooctyl acrylate.
Preferably, the functional monomer is or more of acrylic acid, hydroxyethyl acrylate and methacryloyloxyethyl trimethyl ammonium chloride.
preferably, the functional monomer is composed of acrylic acid, hydroxyethyl acrylate and methacryloyloxyethyl trimethyl ammonium chloride according to the mass ratio of 1 (5.8-6.2) to (5-5.5).
Preferably, the solvent is or more of ethyl acetate, methyl acetate, acetone and toluene.
Preferably, the curing agent is an isocyanate curing agent or an epoxy curing agent.
, the isocyanate curing agent is preferably or more of hexamethylene polyisocyanate, isophorone diisocyanate, toluene diisocyanate and triglycidyl isocyanurate.
, the epoxy curing agent is preferably an m-xylylene diamine type epoxy resin.
Preferably, the initiator is at least selected from a peroxy initiator and an azo initiator.
preferably, the peroxy initiator is at least selected from the group consisting of ammonium persulfate, potassium persulfate, dicumyl peroxide, cumene hydroperoxide, t-butyl hydroperoxide, di-t-butyl peroxide, dibenzoyl peroxide, lauroyl peroxide, t-butyl peroxybenzoate, t-butyl peroxypivalate, diisopropyl peroxydicarbonate, and dicyclohexyl peroxydicarbonate.
, it is preferable that the azo initiator is at least kinds selected from Azobisisoheptonitrile (ABVN), Azobisisobutyronitrile (AIBN), and 2, 2' -azo-bis- (2-methylbutyronitrile).
The invention also provides a preparation method of the pressure-sensitive adhesive for the polarizer protective film, which comprises the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with a feeding amount of 40-60%, and putting the solvent into a reaction kettle to be heated to a reflux state;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1-1.5 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the mixture to be completely dripped within 3-3.5h, and carrying out reflux and heat preservation for 0.5-1.5h after the dripping is completed;
E. adding initiator and 5-15% solvent mixed solution, refluxing and maintaining for 0.5-1.5 h;
F. adding initiator and 5-15% solvent mixed solution, refluxing and maintaining for 1.5-2.5 h;
G. cooling the temperature of the reaction kettle to below 50 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
The invention also provides protective films, which are prepared by uniformly coating the pressure-sensitive adhesive for the polarizer protective film on a base material, preserving heat for 1-3min at the temperature of 110-50 ℃, and curing for 45-50h at the temperature of 45-50 ℃.
The substrate includes, but is not limited to, a PET substrate having a thickness of 40-60 μm.
The thickness of the dry glue on the protective film is 8-12 mu m.
The invention also provides application of the protective film to polarizer surface protection.
Compared with the prior art, the invention has the beneficial effects that:
the pressure-sensitive adhesive for the polarizer protective film has excellent antistatic property, can not generate a large amount of static charges during peeling to cause dust adsorption and potential safety hazard, has strong heat resistance and small peeling force, has no residual adhesive after being subjected to cold tearing after being baked at a high temperature of 180 ℃, has no precipitation, no yellowing, easy peeling and good humidity and heat resistance, and the prepared polarizer protective film is highly transparent, has extremely low surface energy influence on the surface of a polarizer, has excellent chemical stability and good fitting performance, can realize automatic bubble discharge during operation, and has wide market prospect and high economic value.
Detailed Description
The technical features of the technical solution provided by the present invention are further clearly and completely described in the following description with reference to the specific embodiments, and the protection scope of the present invention is not limited thereto.
Further, the recitation of preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When numerical ranges are disclosed herein, the above ranges are considered to be continuous and include the minimum and maximum values for the range and every values between such minimum and maximum values, further includes when a range is referred to an integer every integers between the minimum and maximum values of the range.
The invention provides a pressure-sensitive adhesive for polarizer protective films in aspects, which is prepared from the following raw materials, by weight, 31-35 parts of soft monomers, 6-8 parts of functional monomers, 0.15-0.35 part of initiators, 57-63 parts of solvents and 2-4 parts of curing agents.
In embodiments, the pressure-sensitive adhesive for polarizer protective films is prepared from 33 parts by weight of soft monomers, 7 parts by weight of functional monomers, 0.25 part by weight of initiators, 60 parts by weight of solvents, and 3 parts by weight of curing agents.
In embodiments, the soft monomer is butyl acrylate and/or isooctyl acrylate.
In preferred embodiments, the soft monomer consists of 80-90 wt% butyl acrylate and 10-20 wt% isooctyl acrylate.
In more preferred embodiments, the soft monomer consists of 85 wt% butyl acrylate and 15 wt% isooctyl acrylate.
In embodiments, the functional monomer is or more of acrylic acid, hydroxyethyl acrylate, methacryloyloxyethyl trimethyl ammonium chloride.
In preferred embodiments, the functional monomer consists of acrylic acid, hydroxyethyl acrylate and methacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1 (5.8-6.2) to (5-5.5).
In more preferred embodiments, the functional monomer consists of acrylic acid, hydroxyethyl acrylate, methacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1: 6: 5.2.
In embodiments, the solvent is or more of ethyl acetate, methyl acetate, acetone, toluene.
In embodiments, the curing agent is an isocyanate-based curing agent or an epoxy curing agent.
In preferred embodiments, the isocyanate curing agent is or more of hexamethylene polyisocyanate, isophorone diisocyanate, toluene diisocyanate, and triglycidyl isocyanurate.
In preferred embodiments, the epoxy curing agent is an m-xylylene type epoxy resin.
In embodiments, the initiator is selected from at least peroxy initiators and azo initiators.
In preferred embodiments, the peroxy initiator is at least of ammonium persulfate, potassium persulfate, dicumyl peroxide, cumene hydroperoxide, t-butyl hydroperoxide, di-t-butyl peroxide, dibenzoyl peroxide, lauroyl peroxide, t-butyl peroxybenzoate, t-butyl peroxypivalate, diisopropyl peroxydicarbonate, and dicyclohexyl peroxydicarbonate.
In preferred embodiments, the azo-type initiator is at least of Azobisisoheptonitrile (ABVN), Azobisisobutyronitrile (AIBN), 2' -azo-bis- (2-methylbutyronitrile).
The second aspect of the present invention provides a preparation method of the pressure-sensitive adhesive for polarizer protective films, comprising the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with a feeding amount of 40-60%, and putting the solvent into a reaction kettle to be heated to a reflux state;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1-1.5 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the mixture to be completely dripped within 3-3.5h, and carrying out reflux and heat preservation for 0.5-1.5h after the dripping is completed;
E. adding initiator and 5-15% solvent mixed solution, refluxing and maintaining for 0.5-1.5 h;
F. adding initiator and 5-15% solvent mixed solution, refluxing and maintaining for 1.5-2.5 h;
G. cooling the temperature of the reaction kettle to below 50 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
The third aspect of the invention provides protective films, wherein the pressure-sensitive adhesive for the polarizer protective film is uniformly coated on a substrate, and is subjected to heat preservation at the temperature of 110-50 ℃ for 1-3min and then cured at the temperature of 45-50 ℃ for 45-50h to obtain the protective film.
In embodiments, the substrate includes, but is not limited to, a PET substrate having a thickness of 40-60 μm.
In embodiments, the dry glue on the protective film has a thickness of 8-12 μm.
The fourth aspect of the present invention provides the use of the above protective film for protecting a surface of a polarizer.
The present invention will now be described in detail by way of examples, and the starting materials used are commercially available unless otherwise specified.
Examples
Example 1
The pressure-sensitive adhesive for the polarizer protective film is prepared from the following raw materials in parts by weight: 33 parts of soft monomer, 7 parts of functional monomer, 0.25 part of initiator, 60 parts of solvent and 3 parts of curing agent.
The soft monomer consists of 85 wt% of butyl acrylate and 15 wt% of isooctyl acrylate.
The functional monomer is prepared from acrylic acid, hydroxyethyl acrylate and methacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1: 6: 5.2.
The solvent is ethyl acetate.
The curing agent is hexamethylene polyisocyanate (Bayer N3390, Germany).
The initiator is dibenzoyl peroxide.
The preparation method of the pressure-sensitive adhesive for the polarizer protective film comprises the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with 50% of the material feeding amount, putting the solvent into a reaction kettle, and heating to 80 ℃ for reflux;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1.2 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dropping to be finished within 3.2 hours, and then carrying out reflux and heat preservation for 1 hour;
E. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with the feeding amount, refluxing and preserving heat for 1 h;
F. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with reflux and heat preservation for 2 h;
G. reducing the temperature of the reaction kettle to 40 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
kinds of protective film, uniformly coating the pressure sensitive adhesive for the polarizer protective film on a substrate, preserving heat at 120 ℃ for 2min, and curing at 48 ℃ for 48h to obtain the protective film.
The base material is a PET base material, and the thickness of the base material is 50 mu m.
The thickness of the pressure-sensitive adhesive dry glue on the protective film is 10 mu m.
The protective film is applied to protecting the surface of the polaroid.
Example 2
The pressure-sensitive adhesive for the polarizer protective film is prepared from the following raw materials in parts by weight: 31 parts of soft monomer, 6 parts of functional monomer, 0.15 part of initiator, 57 parts of solvent and 2 parts of curing agent.
31-35 parts of soft monomer, 6-8 parts of functional monomer, 0.15-0.35 part of initiator, 57-63 parts of solvent and 2-4 parts of curing agent
The soft monomer consists of 80 wt% of butyl acrylate and 20 wt% of isooctyl acrylate.
The functional monomer is prepared from acrylic acid, hydroxyethyl acrylate and methacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1: 5.8: 5.
The solvent is ethyl acetate.
The curing agent is hexamethylene polyisocyanate (Bayer N3390, Germany).
The initiator is dibenzoyl peroxide.
The preparation method of the pressure-sensitive adhesive for the polarizer protective film comprises the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with 50% of the material feeding amount, putting the solvent into a reaction kettle, and heating to 80 ℃ for reflux;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1.2 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dropping to be finished within 3.2 hours, and then carrying out reflux and heat preservation for 1 hour;
E. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with the feeding amount, refluxing and preserving heat for 1 h;
F. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with reflux and heat preservation for 2 h;
G. reducing the temperature of the reaction kettle to 40 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
kinds of protective film, uniformly coating the pressure sensitive adhesive for the polarizer protective film on a substrate, preserving heat at 120 ℃ for 2min, and curing at 48 ℃ for 48h to obtain the protective film.
The base material is a PET base material, and the thickness of the base material is 50 mu m.
The thickness of the pressure-sensitive adhesive dry glue on the protective film is 10 mu m.
The protective film is applied to protecting the surface of the polaroid.
Example 3
The pressure-sensitive adhesive for the polarizer protective film is prepared from the following raw materials in parts by weight: 35 parts of soft monomer, 8 parts of functional monomer, 0.35 part of initiator, 63 parts of solvent and 4 parts of curing agent.
The soft monomer consists of 90 wt% of butyl acrylate and 10 wt% of isooctyl acrylate.
The functional monomer is prepared from acrylic acid, hydroxyethyl acrylate and methacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1: 6.2: 5.5.
The solvent is ethyl acetate.
The curing agent is hexamethylene polyisocyanate (Bayer N3390, Germany).
The initiator is dibenzoyl peroxide.
The preparation method of the pressure-sensitive adhesive for the polarizer protective film comprises the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with 50% of the material feeding amount, putting the solvent into a reaction kettle, and heating to 80 ℃ for reflux;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1.2 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dropping to be finished within 3.2 hours, and then carrying out reflux and heat preservation for 1 hour;
E. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with the feeding amount, refluxing and preserving heat for 1 h;
F. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with reflux and heat preservation for 2 h;
G. reducing the temperature of the reaction kettle to 40 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
kinds of protective film, uniformly coating the pressure sensitive adhesive for the polarizer protective film on a substrate, preserving heat at 120 ℃ for 2min, and curing at 48 ℃ for 48h to obtain the protective film.
The base material is a PET base material, and the thickness of the base material is 50 mu m.
The thickness of the pressure-sensitive adhesive dry glue on the protective film is 10 mu m.
The protective film is applied to protecting the surface of the polaroid.
Example 4
The pressure-sensitive adhesive for the polarizer protective film is prepared from the following raw materials in parts by weight: 33 parts of soft monomer, 7 parts of functional monomer, 0.25 part of initiator, 60 parts of solvent and 3 parts of curing agent.
The soft monomer consists of 85 wt% of butyl acrylate and 15 wt% of isooctyl acrylate.
The functional monomer is prepared from acrylic acid and hydroxyethyl acrylate according to a mass ratio of 1: 6.
The solvent is ethyl acetate.
The curing agent is hexamethylene polyisocyanate (Bayer N3390, Germany).
The initiator is dibenzoyl peroxide.
The preparation method of the pressure-sensitive adhesive for the polarizer protective film comprises the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with 50% of the material feeding amount, putting the solvent into a reaction kettle, and heating to 80 ℃ for reflux;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1.2 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dropping to be finished within 3.2 hours, and then carrying out reflux and heat preservation for 1 hour;
E. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with the feeding amount, refluxing and preserving heat for 1 h;
F. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with reflux and heat preservation for 2 h;
G. reducing the temperature of the reaction kettle to 40 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
kinds of protective film, uniformly coating the pressure sensitive adhesive for the polarizer protective film on a substrate, preserving heat at 120 ℃ for 2min, and curing at 48 ℃ for 48h to obtain the protective film.
The base material is a PET base material, and the thickness of the base material is 50 mu m.
The thickness of the pressure-sensitive adhesive dry glue on the protective film is 10 mu m.
The protective film is applied to protecting the surface of the polaroid.
Example 5
The pressure-sensitive adhesive for the polarizer protective film is prepared from the following raw materials in parts by weight: 33 parts of soft monomer, 7 parts of functional monomer, 0.25 part of initiator, 60 parts of solvent and 3 parts of curing agent.
The soft monomer consists of 85 wt% of butyl acrylate and 15 wt% of isooctyl acrylate.
The functional monomer is prepared from acrylic acid, hydroxyethyl acrylate and methacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1: 6: 2.
The solvent is ethyl acetate.
The curing agent is hexamethylene polyisocyanate (Bayer N3390, Germany).
The initiator is dibenzoyl peroxide.
The preparation method of the pressure-sensitive adhesive for the polarizer protective film comprises the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with 50% of the material feeding amount, putting the solvent into a reaction kettle, and heating to 80 ℃ for reflux;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1.2 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dropping to be finished within 3.2 hours, and then carrying out reflux and heat preservation for 1 hour;
E. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with the feeding amount, refluxing and preserving heat for 1 h;
F. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with reflux and heat preservation for 2 h;
G. reducing the temperature of the reaction kettle to 40 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
kinds of protective film, uniformly coating the pressure sensitive adhesive for the polarizer protective film on a substrate, preserving heat at 120 ℃ for 2min, and curing at 48 ℃ for 48h to obtain the protective film.
The base material is a PET base material, and the thickness of the base material is 50 mu m.
The thickness of the pressure-sensitive adhesive dry glue on the protective film is 10 mu m.
The protective film is applied to protecting the surface of the polaroid.
Example 6
The pressure-sensitive adhesive for the polarizer protective film is prepared from the following raw materials in parts by weight: 33 parts of soft monomer, 7 parts of functional monomer, 0.25 part of initiator, 60 parts of solvent and 3 parts of curing agent.
The soft monomer consists of 85 wt% of butyl acrylate and 15 wt% of isooctyl acrylate.
The functional monomer is prepared from acrylic acid, hydroxyethyl acrylate and methacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1: 6: 10.
The solvent is ethyl acetate.
The curing agent is hexamethylene polyisocyanate (Bayer N3390, Germany).
The initiator is dibenzoyl peroxide.
The preparation method of the pressure-sensitive adhesive for the polarizer protective film comprises the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with 50% of the material feeding amount, putting the solvent into a reaction kettle, and heating to 80 ℃ for reflux;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1.2 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dropping to be finished within 3.2 hours, and then carrying out reflux and heat preservation for 1 hour;
E. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with the feeding amount, refluxing and preserving heat for 1 h;
F. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with reflux and heat preservation for 2 h;
G. reducing the temperature of the reaction kettle to 40 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
kinds of protective film, uniformly coating the pressure sensitive adhesive for the polarizer protective film on a substrate, preserving heat at 120 ℃ for 2min, and curing at 48 ℃ for 48h to obtain the protective film.
The base material is a PET base material, and the thickness of the base material is 50 mu m.
The thickness of the pressure-sensitive adhesive dry glue on the protective film is 10 mu m.
The protective film is applied to protecting the surface of the polaroid.
Example 7
The pressure-sensitive adhesive for the polarizer protective film is prepared from the following raw materials in parts by weight: 33 parts of soft monomer, 7 parts of functional monomer, 0.25 part of initiator, 60 parts of solvent and 3 parts of curing agent.
The soft monomer consists of 85 wt% of butyl acrylate and 15 wt% of isooctyl acrylate.
The functional monomer is prepared from acrylic acid and methacryloyloxyethyl trimethyl ammonium chloride according to the mass ratio of 1: 5.2.
The solvent is ethyl acetate.
The curing agent is hexamethylene polyisocyanate (Bayer N3390, Germany).
The initiator is dibenzoyl peroxide.
The preparation method of the pressure-sensitive adhesive for the polarizer protective film comprises the following steps:
A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
B. weighing a solvent with 50% of the material feeding amount, putting the solvent into a reaction kettle, and heating to 80 ℃ for reflux;
C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1.2 h;
D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the dropping to be finished within 3.2 hours, and then carrying out reflux and heat preservation for 1 hour;
E. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with the feeding amount, refluxing and preserving heat for 1 h;
F. adding initiator with six parts of feeding amount and 10% of solvent mixed solution with reflux and heat preservation for 2 h;
G. reducing the temperature of the reaction kettle to 40 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
kinds of protective film, uniformly coating the pressure sensitive adhesive for the polarizer protective film on a substrate, preserving heat at 120 ℃ for 2min, and curing at 48 ℃ for 48h to obtain the protective film.
The base material is a PET base material, and the thickness of the base material is 50 mu m.
The thickness of the pressure-sensitive adhesive dry glue on the protective film is 10 mu m.
The protective film is applied to protecting the surface of the polaroid.
Evaluation of Performance
1. Glue line resistance test
The protective film was cut to 12 × 12mm size, the release film was peeled off, and the sheet resistance was measured on a high resistance meter (model: SME-8310).
2. 180 degree peel strength
The measurement was carried out by an electronic universal tester (the adherend was a standard test steel plate, and the peel rate was 300mm/min) in accordance with GB/T2792-1995 "180 ℃ peel strength test method for pressure-sensitive adhesive tapes".
3. High temperature resistance
And uniformly coating the pressure-sensitive adhesive for the polarizer protective film on glass, storing for 2h in an environment with the temperature of 180 ℃, and then peeling off to observe the condition of adhesive residue.
4. High humidity and high temperature resistance
The pressure-sensitive adhesive for the polarizer protective film is uniformly coated on glass, stored for 48 hours in an environment with the temperature of 85 ℃ and the relative humidity of 85 percent, and then stripped to observe the condition of residual adhesive.
5. Light transmittance test
With reference to the standard GB/T2410-2008, the release film was peeled off using a haze meter (model: U3000), and the light transmittance was measured.
The pressure-sensitive adhesives for polarizer protective films prepared in examples 1 to 7 were tested, and the specific test results are shown in table 1.
Table 1: test result table
Figure BDA0002206167530000131
The foregoing examples are illustrative only and serve to explain features of the method of the invention the appended claims are intended to claim as much as possible, and the examples presented herein are illustrative of selected embodiments based on a combination of all possible examples.

Claims (10)

  1. pressure-sensitive adhesive for polarizer protective film, which is characterized by being prepared from the following raw materials, by weight, 31-35 parts of soft monomer, 6-8 parts of functional monomer, 0.15-0.35 part of initiator, 57-63 parts of solvent and 2-4 parts of curing agent.
  2. 2. The pressure-sensitive adhesive for polarizer protective films according to claim 1, wherein the soft monomer is butyl acrylate and/or isooctyl acrylate.
  3. 3. The pressure-sensitive adhesive for polarizer protective films according to claim 2, wherein the soft monomer is composed of 80 to 90 wt% of butyl acrylate and 10 to 20 wt% of isooctyl acrylate.
  4. 4. The pressure-sensitive adhesive for polarizer protective films according to claim 1, wherein the functional monomer is or more of acrylic acid, hydroxyethyl acrylate, and methacryloyloxyethyl trimethyl ammonium chloride.
  5. 5. The pressure-sensitive adhesive for polarizer protective films according to claim 1, wherein the solvent is or more of ethyl acetate, methyl acetate, acetone, and toluene.
  6. 6. The pressure-sensitive adhesive for polarizer protective films according to claim 1, wherein the curing agent is an isocyanate-based curing agent or an epoxy curing agent.
  7. 7. The pressure-sensitive adhesive for a polarizer protective film according to any of of claims 1 to 6, wherein the initiator is at least selected from peroxy initiators and azo initiators.
  8. 8, A method for preparing the pressure-sensitive adhesive for polarizer protective films according to any of claims 1-7, comprising the steps of:
    A. weighing soft monomers, functional monomers and initiator with two thirds of the material amount according to the weight parts, adding the soft monomers, the functional monomers and the initiator into a head tank, and uniformly stirring to obtain a mixed material;
    B. weighing a solvent with a feeding amount of 40-60%, and putting the solvent into a reaction kettle to be heated to a reflux state;
    C. rapidly adding thirds of the mixed material into the reaction kettle, and keeping reflux reaction for 1-1.5 h;
    D. dropwise adding the rest mixed materials into the reaction kettle at a constant speed, controlling the mixture to be completely dripped within 3-3.5h, and carrying out reflux and heat preservation for 0.5-1.5h after the dripping is completed;
    E. adding initiator and 5-15% solvent mixed solution, refluxing and maintaining for 0.5-1.5 h;
    F. adding initiator and 5-15% solvent mixed solution, refluxing and maintaining for 1.5-2.5 h;
    G. cooling the temperature of the reaction kettle to below 50 ℃, adding the rest solvent, uniformly stirring, and discharging to obtain a polymer;
    H. and uniformly stirring the polymer and the curing agent to obtain the pressure-sensitive adhesive for the polarizer protective film.
  9. 9, protective films, characterized in that, the pressure-sensitive adhesive for polarizer protective films according to any of claims 1-7 is uniformly coated on a substrate, and the protective film is prepared by heat preservation at 110-130 ℃ for 1-3min and curing at 45-50 ℃ for 45-50 h.
  10. 10, use of the protective film according to claim 9 for protecting the surface of a polarizer.
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