CN112251171A - High-temperature-resistant pressure-sensitive coating material, preparation method and protective film - Google Patents

High-temperature-resistant pressure-sensitive coating material, preparation method and protective film Download PDF

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Publication number
CN112251171A
CN112251171A CN202011146598.7A CN202011146598A CN112251171A CN 112251171 A CN112251171 A CN 112251171A CN 202011146598 A CN202011146598 A CN 202011146598A CN 112251171 A CN112251171 A CN 112251171A
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pressure
sensitive adhesive
coating material
protective film
sensitive
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CN112251171B (en
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许显成
张建军
王中正
邬艺
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Sichuan Yuxi Electronic Technology Co ltd
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Sichuan Yuxi Electronic Technology Co ltd
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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
    • 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
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • 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

Abstract

The invention discloses a high-temperature-resistant pressure-sensitive coating material, a preparation method and a protective film, wherein the pressure-sensitive coating material comprises the following raw materials in percentage by mass: polyacrylate pressure-sensitive adhesive: 50% -65%; a crosslinking agent: 0.5 to 6 percent; solvent: 10% -30%; auxiliary agent: 5% -20%; the cross-linking agent adopts a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate and diphenylmethane diisocyanate hollow particles; the outer diameter of the hollow particles is 1 mm-80 mm; the auxiliary agent adopts ethanol. According to the invention, by improving the types, the proportion and the adding state of the added composition of the isocyanate crosslinking agent, adding the auxiliary agent and adjusting the overall proportion relation of the raw materials of the pressure-sensitive coating material, the polyacrylate pressure-sensitive adhesive and the isocyanate crosslinking agent are fully contacted and fully subjected to crosslinking reaction, and the protective film with good high temperature resistance, humidity resistance, heat resistance and acid and alkali resistance is obtained.

Description

High-temperature-resistant pressure-sensitive coating material, preparation method and protective film
Technical Field
The invention relates to the technical field of display screen protective films, in particular to a high-temperature-resistant pressure-sensitive coating material, a preparation method and a protective film.
Background
In order to prevent the screen surface of the electronic product from being scratched or worn and affecting the use effect, a screen protection film is generally attached to the screen surface of the electronic product. The protective film is generally composed of a base material layer and an adhesive layer coated on the base material layer. The requirements on the adhesive are high, and the adhesive can resist high temperature, strong acid and strong alkali and the like, so that the local position of the smart phone can be well protected in the manufacturing process.
In the prior art, in the preparation process of the pressure-sensitive coating liquid, an isocyanate crosslinking agent (having isocyanate groups (-NCO) with high reactivity) is added into the acrylate pressure-sensitive adhesive, and the reactive functional groups of the isocyanate crosslinking agent can react with carboxylic acid and hydroxyl groups in the acrylate pressure-sensitive adhesive for crosslinking. But the acrylic ester pressure-sensitive coating liquid is often not fully crosslinked and still contains incompletely reacted carboxylic acid and hydroxyl groups, so that the stability of the protective film prepared from the acrylic ester pressure-sensitive coating liquid is poor, such as high temperature resistance, damp and heat resistance and acid and alkali resistance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the conventional polyacrylate pressure-sensitive adhesive protective film has poor stability, such as poor high temperature resistance, poor heat and humidity resistance, poor acid and alkali resistance and the like, and the invention provides a high temperature resistant pressure-sensitive coating material and a protective film for solving the problems.
The invention is realized by the following technical scheme:
a high-temperature-resistant pressure-sensitive coating material comprises the following raw materials in percentage by mass: polyacrylate pressure-sensitive adhesive: 50% -65%; a crosslinking agent: 0.5 to 6 percent; solvent: 10% -30%; auxiliary agent: 5% -20%; the cross-linking agent adopts a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate and diphenylmethane diisocyanate hollow particles; the outer diameter of the hollow particles is 1 mm-80 mm; the auxiliary agent adopts ethanol.
In the prior art, an isocyanate crosslinking agent with isocyanate group (-NCO) with high reactivity is added into acrylate pressure-sensitive adhesive, and can react with carboxylic acid and hydroxyl group in the acrylate pressure-sensitive adhesive for crosslinking, but the crosslinking is often insufficient, and the carboxylic acid and the hydroxyl group which are not completely reacted are still contained, so that the protective film prepared from the acrylate pressure-sensitive adhesive has poor high temperature resistance and acid-base resistance.
In the prior art, in order to overcome the above technical problems, insufficient crosslinking is usually overcome by modifying the crosslinking agent, such as adding other crosslinking agents on the basis of isocyanate crosslinking agents, or selecting other types of crosslinking agents; or the stability of the final protective film is improved by improving the raw materials and the synthesis method of the polyacrylate pressure-sensitive adhesive. The invention provides a high-temperature-resistant pressure-sensitive coating material, which is different from the prior art, and is characterized in that by improving the types and adding states of compositions added with isocyanate cross-linking agents, adding auxiliary agents and adjusting the overall proportion of raw materials of the pressure-sensitive coating material, polyacrylate pressure-sensitive adhesive and the isocyanate cross-linking agents are fully contacted and fully subjected to cross-linking reaction, so that a protective film with good high-temperature resistance, humidity resistance, acid resistance and alkali resistance is obtained.
More preferably, the hollow particles have an outer diameter of 5mm to 20 mm.
Further preferably, the mass ratio of the hexamethylene diisocyanate to the dicyclohexylmethane diisocyanate to the diphenylmethane diisocyanate is: 1:1:5.
Further preferably, the addition mass of the auxiliary agent is 20-30% of the mass of the polyacrylate pressure-sensitive adhesive.
Further preferably, the solvent is ethyl acetate or butanone.
A preparation method of a high-temperature-resistant pressure-sensitive coating material is used for preparing the high-temperature-resistant pressure-sensitive coating material, and is characterized by comprising the following steps:
step A, adding polyacrylate pressure-sensitive adhesive into a solvent, and stirring and mixing to obtain a mixed solution A;
step B, adding a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate into the mixed solution A, and stirring and mixing to obtain a mixed solution B;
and step C, adding the diphenylmethane diisocyanate hollow particles and the auxiliary agent into the mixed solution B, and stirring and mixing to obtain the pressure-sensitive adhesive coating liquid.
Further preferably, in the step A, the stirring time is 3min to 5 min; in the step B, the stirring time is 5min to 10 min; in the step C, the stirring time is 1 min-2 min.
The preparation method comprises the steps of dissolving polyacrylate pressure-sensitive adhesive in a solvent, adding hexamethylene diisocyanate and dicyclohexylmethane diisocyanate to be uniformly mixed, adding hollow diphenylmethane diisocyanate particles and an auxiliary agent to be further uniformly mixed, wherein the operations are carried out at normal temperature, and the stirring time and the stirring speed are optimal conditions for uniformly stirring all materials.
A high-temperature-resistant pressure-sensitive coating protective film is prepared from the high-temperature-resistant pressure-sensitive coating material or a pressure-sensitive adhesive coating liquid prepared by the preparation method of the high-temperature-resistant pressure-sensitive coating material by the following steps:
step 1, coating a pressure-sensitive adhesive coating liquid prepared from a high-temperature-resistant pressure-sensitive coating material on the surface of a base material, and heating to 45-50 ℃ for heat treatment;
step 2, heating to 100-120 ℃ and drying;
and 3, covering the release film on the surface of the pressure-sensitive adhesive for curing treatment to obtain the pressure-sensitive adhesive protective film.
The pressure-sensitive adhesive coating material provided by the invention comprises polyacrylate pressure-sensitive adhesive, hexamethylene diisocyanate, dicyclohexylmethane diisocyanate, diphenylmethane diisocyanate hollow particles, a solvent and an auxiliary agent ethanol; after the temperature is quickly raised to 45-50 ℃, the diphenylmethane diisocyanate hollow particles can be dissolved, the internal air is discharged, the air temperature is higher than the ambient temperature, and part of the air can be lifted to separate from the colloid to play a certain stirring role; after most of the diphenylmethane diisocyanate hollow particles are dissolved, the temperature is continuously raised to the cross-linking reaction temperature, at the moment, the ethanol can be quickly volatilized, the air released by the hollow particles can be quickly floated while stirring, so that the polyacrylate pressure-sensitive adhesive and the cross-linking agent can be well stirred to perform uniform and sufficient reaction, and the protective film with good high temperature resistance, humidity resistance, heat resistance and acid and alkali resistance is obtained.
Further preferably, in the step 1, the heating rate is 5 ℃/min to 10 ℃/min, and the heat treatment time is 5min to 20 min; in the step 2, the heating rate is 5-10 ℃/min, and the drying treatment time is as follows: 20min-40 min.
Preferably, the thickness of the base material is 30-100 μm, the coating thickness of the pressure-sensitive adhesive coating liquid is 10-40 μm, and the thickness of the release film is 20-50 μm.
The invention has the following advantages and beneficial effects:
1. the invention provides a high-temperature-resistant pressure-sensitive coating material, which is different from the prior art, and is characterized in that by improving the types, the proportion and the adding state of an added composition of an isocyanate crosslinking agent, adding an auxiliary agent and adjusting the overall proportion relation of raw materials of the pressure-sensitive coating material, polyacrylate pressure-sensitive adhesive is fully contacted with the isocyanate crosslinking agent and fully performs crosslinking reaction, so that a protective film with good high-temperature resistance, humidity resistance, heat resistance and acid and alkali resistance is obtained.
2. The pressure-sensitive adhesive coating material provided by the invention comprises polyacrylate pressure-sensitive adhesive, hexamethylene diisocyanate, dicyclohexylmethane diisocyanate, diphenylmethane diisocyanate hollow particles, a solvent and auxiliary agent ethanol, wherein the diphenylmethane diisocyanate hollow particles and the auxiliary agent ethanol play a role of a 'latent catalyst'; after the temperature is quickly raised to 45-50 ℃, the diphenylmethane diisocyanate hollow particles can be dissolved, the internal air is discharged, the air temperature is higher than the ambient temperature, and part of the air can be lifted to separate from the colloid to play a certain stirring role; after most of the diphenylmethane diisocyanate hollow particles are dissolved, the temperature is continuously raised to the cross-linking reaction temperature, at the moment, the ethanol can be quickly volatilized, the air released by the hollow particles can be quickly floated while stirring, so that the polyacrylate pressure-sensitive adhesive and the cross-linking agent can be well stirred to perform uniform and sufficient reaction, and the protective film with good high temperature resistance, humidity resistance, heat resistance and acid and alkali resistance is obtained.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1
The embodiment provides a high-temperature-resistant pressure-sensitive coating protective film, which is prepared by the following steps:
step 1, the pressure-sensitive coating material comprises the following raw materials:
the pressure-sensitive coating material comprises the following raw materials in percentage by mass:
polyacrylate pressure-sensitive adhesive: 50 percent; a crosslinking agent: 1 percent; solvent: 30 percent; auxiliary agent: 19 percent;
the cross-linking agent adopts a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate and diphenylmethane diisocyanate hollow particles; the mass ratio of hexamethylene diisocyanate to dicyclohexylmethane diisocyanate to diphenylmethane diisocyanate is as follows: 1:1:5.
The auxiliary agent adopts ethanol, and the mass of the auxiliary agent is 38% of that of the polyacrylate pressure-sensitive adhesive.
The outer diameter of the hollow particles is 10 mm.
The solvent adopts ethyl acetate.
Step 2, preparing pressure-sensitive adhesive coating liquid:
step 2-1, adding polyacrylate pressure-sensitive adhesive into a solvent, and stirring and mixing for 3-5 min; as a mixed solution A;
step 2-2, adding a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate into the mixed solution A, and stirring and mixing for 5-10 min; as a mixed solution B;
step 2-3, adding the diphenylmethane diisocyanate hollow particles and the auxiliary agent into the mixed solution B, and stirring and mixing for 1-2 min;
in the steps A to C, the stirring speed is 60 r/min.
Step 3, preparing a pressure-sensitive coating protective film:
step 3-1, coating a pressure-sensitive adhesive coating liquid prepared from a high-temperature-resistant pressure-sensitive coating material on the surface of a base material, and heating to 45 ℃ at a heating rate of 10 ℃/min to perform heat treatment for 10 min;
step 3-2, heating to 120 ℃ at a heating rate of 5 ℃/min, and drying for 30 min;
and 3-3, covering the release film on the surface of the pressure-sensitive adhesive for curing treatment to obtain the pressure-sensitive adhesive protective film.
The base material is a PET film with the thickness of 50 μm; the coating thickness of the pressure-sensitive adhesive coating liquid was 10 μm; the release film is a polyester release film with the thickness of 40 mu m.
Example 2
The embodiment provides a high-temperature-resistant pressure-sensitive coating protective film, which is prepared by the following steps:
step 1, the pressure-sensitive coating material comprises the following raw materials:
the pressure-sensitive coating material comprises the following raw materials in percentage by mass:
polyacrylate pressure-sensitive adhesive: 65 percent; a crosslinking agent: 5 percent; solvent: 20 percent; auxiliary agent: 10 percent;
the cross-linking agent adopts a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate and diphenylmethane diisocyanate hollow particles; the mass ratio of hexamethylene diisocyanate to dicyclohexylmethane diisocyanate to diphenylmethane diisocyanate is as follows: 1:1:5.
The auxiliary agent adopts ethanol, and the mass of the auxiliary agent is 15% of that of the polyacrylate pressure-sensitive adhesive.
The outer diameter of the hollow particles is 10 mm.
The solvent adopts ethyl acetate.
Step 2, preparing pressure-sensitive adhesive coating liquid:
step 2-1, adding polyacrylate pressure-sensitive adhesive into a solvent, and stirring and mixing for 3-5 min; as a mixed solution A;
step 2-2, adding a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate into the mixed solution A, and stirring and mixing for 5-10 min; as a mixed solution B;
step 2-3, adding the diphenylmethane diisocyanate hollow particles and the auxiliary agent into the mixed solution B, and stirring and mixing for 1-2 min;
in the steps A to C, the stirring speed is 60 r/min.
Step 3, preparing a pressure-sensitive coating protective film:
step 3-1, coating a pressure-sensitive adhesive coating liquid prepared from a high-temperature-resistant pressure-sensitive coating material on the surface of a base material, and heating to 45 ℃ at a heating rate of 10 ℃/min to perform heat treatment for 10 min;
step 3-2, heating to 120 ℃ at a heating rate of 5 ℃/min, and drying for 30 min;
and 3-3, covering the release film on the surface of the pressure-sensitive adhesive for curing treatment to obtain the pressure-sensitive adhesive protective film.
The base material is a PET film with the thickness of 50 μm; the coating thickness of the pressure-sensitive adhesive coating liquid was 10 μm; the release film is a polyester release film with the thickness of 40 mu m.
Example 3
The embodiment provides a high-temperature-resistant pressure-sensitive coating protective film, which is prepared by the following steps:
step 1, the pressure-sensitive coating material comprises the following raw materials:
the pressure-sensitive coating material comprises the following raw materials in percentage by mass:
polyacrylate pressure-sensitive adhesive: 56 percent; a crosslinking agent: 2 percent; solvent: 29 percent; auxiliary agent: 13 percent;
the cross-linking agent adopts a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate and diphenylmethane diisocyanate hollow particles; the mass ratio of hexamethylene diisocyanate to dicyclohexylmethane diisocyanate to diphenylmethane diisocyanate is as follows: 1:1:5.
The auxiliary agent adopts ethanol, and the mass of the auxiliary agent is 23% of that of the polyacrylate pressure-sensitive adhesive.
The outer diameter of the hollow particles is 10 mm.
The solvent adopts ethyl acetate.
Step 2, preparing pressure-sensitive adhesive coating liquid:
step 2-1, adding polyacrylate pressure-sensitive adhesive into a solvent, and stirring and mixing for 3-5 min; as a mixed solution A;
step 2-2, adding a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate into the mixed solution A, and stirring and mixing for 5-10 min; as a mixed solution B;
step 2-3, adding the diphenylmethane diisocyanate hollow particles and the auxiliary agent into the mixed solution B, and stirring and mixing for 1-2 min;
in the steps A to C, the stirring speed is 60 r/min.
Step 3, preparing a pressure-sensitive coating protective film:
step 3-1, coating a pressure-sensitive adhesive coating liquid prepared from a high-temperature-resistant pressure-sensitive coating material on the surface of a base material, and heating to 45 ℃ at a heating rate of 10 ℃/min to perform heat treatment for 10 min;
step 3-2, heating to 120 ℃ at a heating rate of 5 ℃/min, and drying for 30 min;
and 3-3, covering the release film on the surface of the pressure-sensitive adhesive for curing treatment to obtain the pressure-sensitive adhesive protective film.
The base material is a PET film with the thickness of 50 μm; the coating thickness of the pressure-sensitive adhesive coating liquid was 10 μm; the release film is a polyester release film with the thickness of 40 mu m.
Example 4
The embodiment provides a high-temperature-resistant pressure-sensitive coating protective film, which is prepared by the following steps:
step 1, the pressure-sensitive coating material comprises the following raw materials:
the pressure-sensitive coating material comprises the following raw materials in percentage by mass:
polyacrylate pressure-sensitive adhesive: 56 percent; a crosslinking agent: 2 percent; solvent: 29 percent; auxiliary agent: 13 percent;
the cross-linking agent adopts a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate and diphenylmethane diisocyanate hollow particles; the mass ratio of hexamethylene diisocyanate to dicyclohexylmethane diisocyanate to diphenylmethane diisocyanate is as follows: 1:1:5.
The auxiliary agent adopts ethanol, and the mass of the auxiliary agent is 23% of that of the polyacrylate pressure-sensitive adhesive.
The outer diameter of the hollow particles is 5 mm.
The solvent adopts ethyl acetate.
Step 2, preparing pressure-sensitive adhesive coating liquid:
step 2-1, adding polyacrylate pressure-sensitive adhesive into a solvent, and stirring and mixing for 3-5 min; as a mixed solution A;
step 2-2, adding a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate into the mixed solution A, and stirring and mixing for 5-10 min; as a mixed solution B;
step 2-3, adding the diphenylmethane diisocyanate hollow particles and the auxiliary agent into the mixed solution B, and stirring and mixing for 1-2 min;
in the steps A to C, the stirring speed is 60 r/min.
Step 3, preparing a pressure-sensitive coating protective film:
step 3-1, coating a pressure-sensitive adhesive coating liquid prepared from a high-temperature-resistant pressure-sensitive coating material on the surface of a base material, and heating to 45 ℃ at a heating rate of 10 ℃/min to perform heat treatment for 10 min;
step 3-2, heating to 120 ℃ at a heating rate of 5 ℃/min, and drying for 30 min;
and 3-3, covering the release film on the surface of the pressure-sensitive adhesive for curing treatment to obtain the pressure-sensitive adhesive protective film.
The base material is a PET film with the thickness of 50 μm; the coating thickness of the pressure-sensitive adhesive coating liquid was 10 μm; the release film is a polyester release film with the thickness of 40 mu m.
Example 5
The embodiment provides a high-temperature-resistant pressure-sensitive coating protective film, which is prepared by the following steps:
step 1, the pressure-sensitive coating material comprises the following raw materials:
the pressure-sensitive coating material comprises the following raw materials in percentage by mass:
polyacrylate pressure-sensitive adhesive: 56 percent; a crosslinking agent: 2 percent; solvent: 29 percent; auxiliary agent: 13 percent;
the cross-linking agent adopts a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate and diphenylmethane diisocyanate hollow particles; the mass ratio of hexamethylene diisocyanate to dicyclohexylmethane diisocyanate to diphenylmethane diisocyanate is as follows: 1:1:5.
The auxiliary agent adopts ethanol, and the mass of the auxiliary agent is 23% of that of the polyacrylate pressure-sensitive adhesive.
The outer diameter of the hollow particles is 20 mm.
The solvent adopts ethyl acetate.
Step 2, preparing pressure-sensitive adhesive coating liquid:
step 2-1, adding polyacrylate pressure-sensitive adhesive into a solvent, and stirring and mixing for 3-5 min; as a mixed solution A;
step 2-2, adding a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate into the mixed solution A, and stirring and mixing for 5-10 min; as a mixed solution B;
step 2-3, adding the diphenylmethane diisocyanate hollow particles and the auxiliary agent into the mixed solution B, and stirring and mixing for 1-2 min;
in the steps A to C, the stirring speed is 60 r/min.
Step 3, preparing a pressure-sensitive coating protective film:
step 3-1, coating a pressure-sensitive adhesive coating liquid prepared from a high-temperature-resistant pressure-sensitive coating material on the surface of a base material, and heating to 45 ℃ at a heating rate of 10 ℃/min to perform heat treatment for 10 min;
step 3-2, heating to 120 ℃ at a heating rate of 5 ℃/min, and drying for 30 min;
and 3-3, covering the release film on the surface of the pressure-sensitive adhesive for curing treatment to obtain the pressure-sensitive adhesive protective film.
The base material is a PET film with the thickness of 50 μm; the coating thickness of the pressure-sensitive adhesive coating liquid was 10 μm; the release film is a polyester release film with the thickness of 40 mu m.
Comparative example 1
Based on the technical scheme of the embodiment 3, the difference is that: the pressure-sensitive coating material comprises the following raw materials in percentage by mass: polyacrylate pressure-sensitive adhesive: 75 percent; a crosslinking agent: 3 percent; solvent: 15 percent; auxiliary agent: 7 percent.
Comparative example 2
Based on the technical scheme of the embodiment 3, the difference is that: the pressure-sensitive coating material comprises the following raw materials in percentage by mass: polyacrylate pressure-sensitive adhesive: 40 percent; a crosslinking agent: 0.5 percent; solvent: 39 percent; auxiliary agent: 20.5 percent.
Comparative example 3
Based on the technical scheme of the embodiment 3, the difference is that: the cross-linking agent adopts hexamethylene diisocyanate liquid, dicyclohexyl methane diisocyanate liquid and diphenylmethane diisocyanate solid, namely, the diphenylmethane diisocyanate is solid particles.
Comparative example 4
Based on the technical scheme of the embodiment 3, the difference is that: the mass ratio of the hexamethylene diisocyanate to the dicyclohexylmethane diisocyanate to the diphenylmethane diisocyanate is 1:1: 0.8.
Comparative example 5
Based on the technical scheme of the embodiment 3, the difference is that: the pressure-sensitive coating material comprises the following raw materials in percentage by mass: polyacrylate pressure-sensitive adhesive: 63%; a crosslinking agent: 3 percent; solvent: 34 percent; no ethanol auxiliary agent.
Comparative example 6
Based on the technical scheme of the embodiment 3, the difference is that: the pressure-sensitive coating material comprises the following raw materials in percentage by mass: polyacrylate pressure-sensitive adhesive: 63%; a crosslinking agent: 3 percent; solvent: 34 percent; the cross-linking agent adopts hexamethylene diisocyanate liquid, dicyclohexyl methane diisocyanate liquid and diphenylmethane diisocyanate solid, namely no ethanol auxiliary agent, and the diphenylmethane diisocyanate is solid particles.
Performance testing
1. Test method
(1) And (3) testing optical performance: and peeling off the release film from the protective film sample, and testing the full light transmittance and the haze of the protective film sample by using a haze meter/WGT-S.
(2) And (3) testing the peel strength: the 180 DEG peel force of the protective film samples was determined with reference to the standard GB/T2792-1998.
(3) And (3) testing high-temperature resistance: rolling the protective film sample back and forth by using a 2kg roller for 3 times to be attached to a clean glass plate, placing for 2 hours at 160 ℃, then taking out, naturally cooling to normal temperature, peeling the protective film sample from the glass plate, and observing the pollution condition of the surface of the glass plate after the protective film sample is peeled off under a darkroom strong light.
(4) Moisture and heat resistance test: and rolling the protective film sample back and forth for 3 times by using a 2kg roller to be attached to a clean glass plate, and putting the protective film sample into a damp-heat aging box, wherein the humidity condition is 90% RH, the temperature condition is 60 ℃, and the aging time is 6 d.
(5) And (3) testing acid and alkali resistance: rolling the protective film sample back and forth by using a 2kg roller for 3 times to be attached to a clean glass plate, placing the glass plate in strong acid (pH is 2) or strong base (pH is 13) to be soaked for 1h, taking out the glass plate, washing the glass plate by using clean water, drying the glass plate at normal temperature, stripping the protective film sample from the glass plate, and observing the pollution condition of the surface of the glass plate after the protective film sample is stripped under a darkroom floodlight.
2. Test results
Table 1 results of performance testing of protective film samples prepared in examples 1 to 5
Item Example 1 Example 2 Example 3 Example 4 Example 5
Light transmittance 90.8 91.2 91.0 91.2 91.1
Haze degree 1.0 0.9 0.9 0.9 0.9
Peel strength#1 15 16 21 19 18
Peel strength#2 13 15 20 19 16
High temperature resistance No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution
Moisture and heat resistance No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution
Acid and alkali resistance No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution No adhesive residue and pollution
Table 2 results of performance test of the protective films provided in comparative examples 1 to 6
Item Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5 Comparative example 6
Light transmittance 90.3 89.9 90.2 90.1 90.2 90.2
Fog city 0.9 0.8 0.9 0.9 0.9 0.9
Peel strength#1 19 15 18 20 17 20
Peel strength#2 11 5 10 10 9 8
High temperature resistance With pollution With pollution With pollution Is free of With pollution With pollution
Moisture and heat resistance With pollution With pollution With pollution With pollution With pollution With pollution
Acid and alkali resistance Is free of With pollution Is free of Is free of With pollution With pollution
Remarking: in tables 1 and 2, the peel strength#1Shows the peel strength before the wet heat treatment#2Both expressed in g/25mm after the wet heat treatment; in table 1, the term "contamination" refers to a phenomenon of contamination such as ghost, white fog, and the like.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The high-temperature-resistant pressure-sensitive coating material is characterized by comprising the following raw materials in percentage by mass:
polyacrylate pressure-sensitive adhesive: 50% -65%;
a crosslinking agent: 0.5 to 6 percent;
solvent: 10% -30%;
auxiliary agent: 5% -20%;
the cross-linking agent adopts a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate and diphenylmethane diisocyanate hollow particles; the outer diameter of the hollow particles is 1 mm-80 mm;
the auxiliary agent adopts ethanol.
2. The high temperature-resistant pressure-sensitive coating material according to claim 1, wherein the hollow particles have an outer diameter of 5mm to 20 mm.
3. The high temperature-resistant pressure-sensitive coating material as claimed in claim 3, wherein the mass ratio of hexamethylene diisocyanate to dicyclohexylmethane diisocyanate to diphenylmethane diisocyanate is: 1:1:5.
4. The high-temperature-resistant pressure-sensitive coating material as claimed in claim 1, wherein the addition amount of the auxiliary agent is 20-30% of the weight of the polyacrylate pressure-sensitive adhesive.
5. The high temperature-resistant pressure-sensitive coating material as claimed in claim 1, wherein the solvent is ethyl acetate or butanone.
6. A method for preparing a high temperature resistant pressure sensitive coating material according to any one of claims 1 to 5, comprising the steps of:
step A, adding polyacrylate pressure-sensitive adhesive into a solvent, and stirring and mixing to obtain a mixed solution A;
step B, adding a liquid mixture of hexamethylene diisocyanate and dicyclohexylmethane diisocyanate into the mixed solution A, and stirring and mixing to obtain a mixed solution B;
and step C, adding the diphenylmethane diisocyanate hollow particles and the auxiliary agent into the mixed solution B, and stirring and mixing to obtain the pressure-sensitive adhesive coating liquid.
7. The method for preparing a high temperature resistant pressure sensitive coating material according to claim 6, wherein in the step A, the stirring time is 3min to 5 min; in the step B, the stirring time is 5min to 10 min; in the step C, the stirring time is 1 min-2 min.
8. A high temperature resistant pressure sensitive coating protective film, which is a pressure sensitive adhesive coating liquid prepared by using a high temperature resistant pressure sensitive coating material as claimed in any one of claims 1 to 5 or a preparation method of a high temperature resistant pressure sensitive coating material as claimed in any one of claims 6 to 7, characterized in that the protective film is prepared by the following method:
step 1, coating a pressure-sensitive adhesive coating liquid prepared from a high-temperature-resistant pressure-sensitive coating material on the surface of a base material, and heating to 45-50 ℃ for heat treatment;
step 2, heating to 100-120 ℃ and drying;
and 3, covering the release film on the surface of the pressure-sensitive adhesive for curing treatment to obtain the pressure-sensitive adhesive protective film.
9. The protective film according to claim 8, wherein the protective film comprises a high temperature resistant pressure sensitive coating,
in the step 1, the heating rate is 5-10 ℃/min, and the heat treatment time is 5-20 min;
in the step 2, the heating rate is 5-10 ℃/min, and the drying treatment time is as follows: 20min-40 min.
10. The high temperature resistant pressure sensitive coating protective film according to claim 8, wherein the thickness of the substrate is 30 to 100 μm, the coating thickness of the pressure sensitive adhesive coating liquid is 10 to 40 μm, and the thickness of the release film is 20 to 50 μm.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070155859A1 (en) * 2006-01-04 2007-07-05 Zhengzhe Song Reactive polyurethane hot melt adhesive
CN106433506A (en) * 2016-11-07 2017-02-22 苏州旭泽新材料科技有限公司 Protective film with heating-reducible adhesion and preparation method thereof
CN108441135A (en) * 2018-02-02 2018-08-24 苏州城邦达力材料科技有限公司 A kind of UV visbreakings composition, UV visbreaking films and preparation method thereof
CN109628027A (en) * 2018-10-18 2019-04-16 深圳市益达兴科技股份有限公司 A kind of high temperature-resistant acid-resistant alkacrylic ester pressure sensitive adhesive composition and protective film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070155859A1 (en) * 2006-01-04 2007-07-05 Zhengzhe Song Reactive polyurethane hot melt adhesive
CN106433506A (en) * 2016-11-07 2017-02-22 苏州旭泽新材料科技有限公司 Protective film with heating-reducible adhesion and preparation method thereof
CN108441135A (en) * 2018-02-02 2018-08-24 苏州城邦达力材料科技有限公司 A kind of UV visbreakings composition, UV visbreaking films and preparation method thereof
CN109628027A (en) * 2018-10-18 2019-04-16 深圳市益达兴科技股份有限公司 A kind of high temperature-resistant acid-resistant alkacrylic ester pressure sensitive adhesive composition and protective film

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