CN114672258A - Protective film for manufacturing process or shipment of ultrathin flexible glass and preparation method thereof - Google Patents
Protective film for manufacturing process or shipment of ultrathin flexible glass and preparation method thereof Download PDFInfo
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- CN114672258A CN114672258A CN202210240577.4A CN202210240577A CN114672258A CN 114672258 A CN114672258 A CN 114672258A CN 202210240577 A CN202210240577 A CN 202210240577A CN 114672258 A CN114672258 A CN 114672258A
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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
- C09J7/20—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
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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
- 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
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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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
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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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
- 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
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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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
- C09J2433/00—Presence of (meth)acrylic polymer
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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
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
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Abstract
The invention relates to a protective film for manufacturing or shipping ultrathin flexible glass and a preparation method thereof, wherein the protective film comprises a base material and a pressure-sensitive adhesive layer, and the pressure-sensitive adhesive layer is coated on one side surface of the base material. The pressure-sensitive adhesive solution for forming the pressure-sensitive adhesive layer comprises the following raw materials in parts by weight: 25-70 parts of main resin, 10-80 parts of solvent, 5-25 parts of temperature-resistant auxiliary agent, 2-8 parts of cross-linking agent, 1-5 parts of curing retarder and 0.1-3 parts of antistatic agent. The temperature-resistant auxiliary agent can effectively improve the TG value of the pressure-sensitive adhesive layer, so that the hardness of the pressure-sensitive adhesive layer is higher, and the viscosity rising degree is lower when the pressure-sensitive adhesive layer is subjected to high temperature. Meanwhile, the temperature-resistant auxiliary agent can effectively improve the temperature resistance of the pressure-sensitive adhesive layer. On the whole, the climbing degree of the peeling force of the pressure-sensitive adhesive layer under high temperature is lower. In addition, the temperature-resistant auxiliary agent and the main resin react to further increase the molecular weight, so that the crosslinking network is tighter, and therefore, small molecules (such as a plasticizer and the like) in the pressure-sensitive adhesive layer and the base material are difficult to migrate at high temperature.
Description
Technical Field
The invention relates to the technical field of protective films for ultrathin flexible glass, in particular to a protective film for ultrathin flexible glass manufacturing procedures or shipment and a preparation method thereof.
Background
AMOLED (Active Matrix/Organic Light Emitting Diode) has advantages of low power consumption, high color gamut, high brightness, high resolution, wide viewing angle, and high response speed, and has gradually become a mainstream display. UTG (Ultra Thin Glass) is arranged on one side face of the AMOLED foldable screen, the thickness of UTG is 20-80 mu m, and the minimum bending radius is 1-2.5 mm. UTG A protective film is attached to one side of the container during manufacture or shipment. However, the UTG is subjected to high temperature during the manufacturing process, so that the peeling force of the protective film is increased seriously, and the protective film is not easy to peel off from UTG.
Therefore, how to reduce the climbing of the peeling force after the conventional ultra-thin flexible glass process or the protective film for shipment is subjected to high temperature is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the problem that the peeling force is seriously increased after the traditional ultrathin flexible glass manufacturing procedure or the traditional protective film for shipment is subjected to high temperature, the invention provides the ultrathin flexible glass manufacturing procedure or the protective film for shipment and the preparation method thereof.
The protective film for the ultrathin flexible glass manufacturing process or shipment comprises a base material and a pressure-sensitive adhesive layer, wherein the pressure-sensitive adhesive layer is coated on one side surface of the base material;
the pressure-sensitive adhesive liquid for forming the pressure-sensitive adhesive layer comprises the following raw materials in parts by weight:
25-70 parts of main resin, 10-80 parts of solvent, 5-25 parts of temperature-resistant assistant, 2-8 parts of cross-linking agent, 1-5 parts of curing retarder and 0.1-3 parts of antistatic agent.
In one specific embodiment, the temperature-resistant additive is one of polyacrylate, cellulose ester, hydrogenated rosin and phenolic resin, the molecular weight is 2-100 ten thousand, and the TG value is-15-150 ℃.
In one embodiment, the substrate is a pre-heat treated PET.
In one embodiment, the host resin is one of polyacrylic acid, polyacrylate and urethane acrylate, the molecular weight is 5-100 ten thousand, and the TG value is-40 ℃ to-10 ℃.
In one embodiment, the solvent is one of an ester solvent, an ether solvent, an aromatic hydrocarbon solvent, an aliphatic hydrocarbon solvent and a ketone solvent;
the cross-linking agent is one of isocyanate cross-linking agent and epoxy cross-linking agent;
the solidification retarder is one of acetylacetone, p-hydroxyanisole, modified triethylene diamine and modified dimethylamino diethyl ether;
The antistatic agent is one of metal ion salt, ionic liquid and carbon nano tube.
In one specific embodiment, the adhesive further comprises a release film;
the release film is attached to one side of the pressure-sensitive adhesive layer far away from the base material.
The method for preparing the protective film for manufacturing or shipping the ultrathin flexible glass provided by any embodiment based on the same concept comprises the following steps:
adding the main resin, the temperature-resistant auxiliary agent, the cross-linking agent, the curing retarder and the antistatic agent into the solvent in the amount, and uniformly stirring to obtain a pressure-sensitive adhesive solution;
coating the pressure-sensitive adhesive liquid on one side surface of the base material, and drying in an oven at the drying temperature of 40-130 ℃ to obtain a semi-finished product A;
sticking a release film on one side surface of the pressure-sensitive adhesive layer of the semi-finished product A, which is far away from the base material, to prepare a semi-finished product B;
and (3) placing the semi-finished product B into a curing chamber for curing at the temperature of 20-70 ℃ for 24-240 hours to obtain the ultrathin flexible glass protective film for manufacturing or shipment.
In one embodiment, before applying the pressure-sensitive adhesive solution to one side of the substrate, the method further comprises the following steps:
the substrate is subjected to a pre-heat treatment.
The invention has the beneficial effects that: according to the protective film for the ultrathin flexible glass manufacturing process or shipment, the temperature-resistant auxiliary agent is added into the pressure-sensitive adhesive liquid for forming the pressure-sensitive adhesive layer, and the temperature-resistant auxiliary agent can effectively improve the TG value of the pressure-sensitive adhesive layer, so that the hardness of the pressure-sensitive adhesive layer is higher, and further, the viscosity rising degree is lower when the pressure-sensitive adhesive layer is subjected to high temperature. Meanwhile, the temperature-resistant auxiliary agent can effectively improve the temperature resistance of the pressure-sensitive adhesive layer. On the whole, the climbing degree of the peeling force of the pressure-sensitive adhesive layer under high temperature is lower. In addition, the temperature-resistant auxiliary agent and the main resin react to further increase the molecular weight, so that the crosslinking network is tighter, and therefore, small molecules (such as a plasticizer and the like) in the pressure-sensitive adhesive layer and the base material are difficult to migrate at high temperature. Therefore, when the protective film is subjected to high temperature, bubbles and white fog are generated very little, the optical performance is effectively improved, and the optical inspection failure rate of the product is reduced. Moreover, even if the protective film is adhered to UTG for a long time, the substance is not easy to precipitate, the surface performance of UTG is improved, and the yield of UTG is improved.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of a protective film for ultra-thin flexible glass manufacturing or shipping according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
Referring to fig. 1, as an embodiment of the present invention, the present invention provides a protective film for ultrathin flexible glass manufacturing or shipping, which includes a substrate 110 and a pressure sensitive adhesive layer 120, wherein the pressure sensitive adhesive layer 120 is coated on one side of the substrate 110. The pressure-sensitive adhesive solution for forming the pressure-sensitive adhesive layer 120 comprises the following raw materials in parts by weight: 25-70 parts of main resin, 10-80 parts of solvent, 5-25 parts of temperature-resistant auxiliary agent, 2-8 parts of cross-linking agent, 1-5 parts of curing retarder and 0.1-3 parts of antistatic agent, wherein the total is 100 parts.
In this embodiment, the pressure sensitive adhesive layer 120 of the ultra-thin flexible glass process or shipping protective film can be attached on one side of the UTG. The pressure-sensitive adhesive solution for forming the pressure-sensitive adhesive layer 120 comprises the following raw materials: the curing agent comprises main resin, a solvent, a temperature-resistant auxiliary agent, a cross-linking agent and a curing retarder. Wherein, the solvent can dissolve the main resin, the temperature-resistant auxiliary agent, the cross-linking agent and the curing retarder. The crosslinking agent is capable of curing the host resin. The cure retarder is capable of extending the length of cure. Here, it should be noted that the curing retarder is volatilized by heat during the process of drying the pressure-sensitive adhesive liquid to form the pressure-sensitive adhesive layer 120. By adding the temperature-resistant auxiliary agent into the pressure-sensitive adhesive liquid, the temperature-resistant auxiliary agent can effectively improve the TG value of the pressure-sensitive adhesive layer 120, so that the hardness of the pressure-sensitive adhesive layer 120 is higher, and the viscosity rise degree is lower after the pressure-sensitive adhesive layer 120 is subjected to high temperature. Meanwhile, the temperature-resistant auxiliary agent can effectively improve the temperature resistance of the pressure-sensitive adhesive layer 120. The antistatic agent can greatly reduce the possibility of static electricity generation when the release film 130 is peeled off from the pressure-sensitive adhesive layer 120. Overall, the peel force of the pressure-sensitive adhesive layer 120 increases to a lower degree after exposure to high temperatures. In addition, the temperature-resistant auxiliary reacts with the main resin to further increase the molecular weight, so that the crosslinked network is more compact, and thus the small molecules (such as plasticizer and the like) in the pressure-sensitive adhesive layer 120 and the base material 110 are difficult to migrate at high temperature. Therefore, when the protective film is subjected to high temperature, bubbles and white fog are generated very little, the optical performance is effectively improved, and the optical inspection failure rate of the product is reduced. Moreover, even if the protective film is adhered to UTG for a long time, the substance is not easy to precipitate, the surface performance of UTG is improved, and the yield of UTG is improved.
In one embodiment of the invention, the main body resin is one of polyacrylic acid, polyacrylate and polyurethane acrylate, the molecular weight is 5-100 ten thousand, and the TG value is-40 ℃ to-10 ℃. Compared with the traditional main body resin, the TG value is higher, the hardness deflection and the molecular weight are relatively larger, so that the rising degree of the peeling force is lower when the pressure-sensitive adhesive layer 120 is subjected to high temperature. The temperature-resistant additive is one of polyacrylate, cellulose ester, hydrogenated rosin and phenolic resin, the molecular weight is 2-100 ten thousand, and the TG value is-15-150 ℃. The temperature-resistant auxiliary agent has good compatibility with the main resin, and does not affect the optical performance of the pressure-sensitive adhesive layer 120. The TG value of the temperature-resistant auxiliary agent is higher than that of the main resin, so that the TG value of the pressure-sensitive adhesive layer 120 is higher and the hardness is higher. As such, the pressure-sensitive adhesive layer 120 has a lower degree of peel force build-up after being subjected to high temperature, so that the protective film is easily peeled off from UTG.
In one embodiment of the present invention, the substrate 110 is a pre-heat treated PET. Here, the preheating temperature is 120 ℃ to 240 ℃. The thermal shrinkage of PET after the preset treatment is lower than 0.8%. Therefore, in the UTG process, when the protective film is subjected to high temperature, the bidirectional thermal shrinkage rate is low, and the UTG is not driven to shrink and deform, so that the product yield is improved.
In a specific embodiment of the present invention, the solvent is one of an ester solvent, an ether solvent, an aromatic hydrocarbon solvent, an aliphatic hydrocarbon solvent, and a ketone solvent. Here, the lipid solvent may be ethyl acetate, methyl formate, or the like. The ether solvent can be diethyl ether or hexyl ether. The aromatic hydrocarbon solvent may be benzene or xylene, etc. The ketone solvent may be acetone or methyl ethyl ketone. The cross-linking agent is one of isocyanate cross-linking agent and epoxy cross-linking agent. The curing retarder is one of acetylacetone, p-hydroxyanisole, modified triethylene diamine and modified dimethylamino diethyl ether. The antistatic agent is one of metal ion salt, ionic liquid and carbon nano tube. Here, it is to be noted that the metal ion salt may be a lithium salt.
In an embodiment of the invention, the protective film for the ultra-thin flexible glass manufacturing process or shipment further includes a release film 130, and the release film 130 is attached to a side of the pressure sensitive adhesive layer 120 away from the substrate 110, so as to protect the pressure sensitive adhesive layer 120 of the protective film when the protective film is not in use. Specifically, the release film 130 is made of PET or PE. Before the release film 130 is attached to the pressure sensitive adhesive layer 120, the release film 130 may be subjected to an antistatic treatment to achieve different impedances. The thickness of the substrate 110 is 16 to 250 μm, and is selected according to actual needs.
The invention also provides a preparation method of the protective film for the ultrathin flexible glass manufacturing process or shipment, which comprises the following steps:
and adding the main resin, the temperature-resistant auxiliary agent, the crosslinking agent, the curing retarder and the antistatic agent into the solvent in the amount, and uniformly stirring to obtain the pressure-sensitive adhesive solution.
In the step, ethyl acetate is selected as a solvent, and 25-70 parts by weight of main resin, 5-25 parts by weight of temperature-resistant auxiliary agent, 2-8 parts by weight of cross-linking agent, 1-5 parts by weight of curing retarder and 0.1-3 parts by weight of antistatic agent are added into 10-80 parts by weight of ethyl acetate. Stirring uniformly to obtain pressure-sensitive adhesive liquid for later use.
And coating the pressure-sensitive adhesive liquid on one side surface of the base material 110, and drying in an oven at the drying temperature of 40-130 ℃ to obtain a semi-finished product A.
In this step, one side of the substrate 110 is subjected to corona, and then, a pressure-sensitive adhesive solution is applied to the corona side of the substrate 110. And then, placing the base material 110 coated with the pressure-sensitive adhesive solution in an oven, and drying at 40-130 ℃ to obtain a semi-finished product A. Here, it should be noted that the preferable drying temperature is 100-.
And attaching the release film 130 to one side surface of the pressure-sensitive adhesive layer 120 of the semi-finished product A far away from the substrate 110 to obtain a semi-finished product B.
In this step, before the release film 130 is attached to the semi-finished product a, the release film 130 is subjected to an antistatic treatment in advance. Then, the release film 130 is attached to one side of the pressure-sensitive adhesive layer 120 of the semi-finished product a away from the substrate 110 to protect the pressure-sensitive adhesive layer 120. When the pressure-sensitive adhesive layer 120 is required to be used, the release film 130 is peeled off from the pressure-sensitive adhesive layer 120.
And (3) placing the semi-finished product B into a curing chamber for curing at the temperature of 20-70 ℃ for 24-240 hours to obtain the ultrathin flexible glass protective film for manufacturing or shipment.
In this step, the semi-finished product B is placed in a curing chamber for curing. The preferred curing temperature is 40-50 ℃, and the preferred curing time is 96-144 h. Therefore, the pressure-sensitive adhesive layer 120 has high chemical property stability and high weather resistance, and is favorable for storage and long-distance transportation.
In an embodiment of the present invention, before applying the pressure-sensitive adhesive solution to one side of the substrate 110, the method further includes the following steps:
the substrate 110 is subjected to a preheating treatment.
In this step, the substrate 110 made of PET is preheated at 120-240 ℃, and the thermal shrinkage of the PET after the preheating is lower than 0.8%. When the protective film is subjected to high temperature, the thermal shrinkage rate is small, so that the protective film is not easy to deform.
Example 1
The base material 110 was PET and had a thickness of 100 μm. The thickness of the pressure sensitive adhesive layer 120 is 10 μm, and the pressure sensitive adhesive layer 120 comprises the following raw materials in parts by weight: 50 parts of polyacrylic acid (with the molecular weight of 50 ten thousand and the TG value of-23 ℃), 30 parts of ethyl acetate, 10 parts of polyacrylate (with the molecular weight of 60 ten thousand and the TG value of 30 ℃), 5 parts of isocyanate crosslinking agent, 4 parts of acetylacetone and 1 part of metal ion salt.
Preparing a protective film for ultrathin flexible glass manufacturing procedure or shipment: first, a pressure-sensitive adhesive solution was prepared. Then, coating the pressure-sensitive adhesive solution on one side surface of the substrate 110, and placing the substrate in an oven for drying at the drying temperature of 110 ℃ to obtain a semi-finished product A. And then, attaching a release film 130 to one side of the pressure-sensitive adhesive layer 120 of the semi-finished product A, which is far away from the substrate 110, to prepare a semi-finished product B. And finally, placing the semi-finished product B in a curing chamber for curing at the temperature of 50 ℃ for 120 hours to obtain the ultrathin flexible glass manufacturing procedure or the protective film for shipment.
Example 2
Compared with the example 1, the temperature-resistant auxiliary agent is changed into cellulose ester, and other experimental conditions are not changed.
Example 3
Compared with the example 1, the temperature-resistant additive is changed into hydrogenated rosin, and other experimental conditions are not changed.
Example 4
Compared with the example 1, the temperature-resistant auxiliary agent is changed into phenolic resin, and other experimental conditions are not changed.
Example 5
Compared with the example 1, the temperature-resistant auxiliary agent is not added, and other experimental conditions are not changed.
The peel force of the ultra-thin flexible glass manufactured in examples 1 to 5 was measured at room temperature, and the results are shown in table 1:
TABLE 1
The ultra-thin flexible glass manufactured in examples 1 to 5 was left to stand at 150 ℃ for 60 minutes, and then the peel strength of the ultra-thin flexible glass manufactured in examples 1 to 5 was measured, and the results are shown in table 2:
TABLE 2
The ultra-thin flexible glass manufactured in examples 1 to 5 was tested for light transmittance, haze and two-way heat shrinkage in the process or shipment of the protective film, and the test results are shown in table 3:
TABLE 3
As can be seen from tables 1 to 3, the peeling force increases to a greater extent after the ultra-thin flexible glass manufactured in example 5 is subjected to high temperature in the manufacturing process or the protective film for shipment. The peeling force rises to a small extent after the ultra-thin flexible glass manufacturing process or the protective film for shipment manufactured by examples 1 to 4 is subjected to high temperature. Namely, the temperature-resistant auxiliary agent is added to the pressure-sensitive adhesive solution, so that the pressure-sensitive adhesive layer 120 can resist the high temperature of 60-180 ℃ in the manufacturing process. After the manufacturing process, the protective film pair UTG still has low adhesive force, no substance is separated out, and the climbing degree of the peeling force of the pressure-sensitive adhesive layer 120 after being subjected to high temperature can be effectively reduced. After the temperature-resistant auxiliary agent is added, the transmittance of the protective film is kept above 88%, the haze is kept below 5%, the protective film is relatively flat, the problems of concave-convex points and point-shaped foreign matters are avoided, and damage such as abrasion to UTG is avoided. The bidirectional thermal shrinkage of the protective film after heat resistance is less than 0.8 percent, and UTG is not easy to deform. In addition, after the whole high-temperature process and circulation process, the protective film is peeled off from UTG, and the UTG surface is not polluted.
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," "one specific embodiment," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the equivalent alternatives or modifications within the scope of the present invention, the technical solution of the present invention and the inventive concept thereof.
Claims (8)
1. The protective film for the ultrathin flexible glass manufacturing process or shipment is characterized by comprising a base material and a pressure-sensitive adhesive layer, wherein the pressure-sensitive adhesive layer is coated on one side surface of the base material;
The pressure-sensitive adhesive solution for forming the pressure-sensitive adhesive layer comprises the following raw materials in parts by weight:
25-70 parts of main resin, 10-80 parts of solvent, 5-25 parts of temperature-resistant assistant, 2-8 parts of cross-linking agent, 1-5 parts of curing retarder and 0.1-3 parts of antistatic agent.
2. The protective film for ultrathin flexible glass manufacturing or shipment according to claim 1, wherein the temperature resistant auxiliary is one of polyacrylate, cellulose ester, hydrogenated rosin and phenolic resin, the molecular weight is 2-100 ten thousand, and the TG value is-15 ℃ to 150 ℃.
3. The ultra-thin flexible glass processing or shipping protective film of claim 1, wherein the substrate is pre-heat treated PET.
4. The ultra-thin flexible glass manufacturing or shipping protective film according to any of claims 1 to 3, wherein the host resin is one of polyacrylic acid, polyacrylate and urethane acrylate, the molecular weight is 5-100 ten thousand, and the TG value is-40 ℃ to-10 ℃.
5. The protective film for ultra-thin flexible glass manufacturing or shipment according to claim 4, wherein the solvent is one of an ester solvent, an ether solvent, an aromatic hydrocarbon solvent, an aliphatic hydrocarbon solvent, and a ketone solvent;
The cross-linking agent is one of isocyanate cross-linking agent and epoxy cross-linking agent;
the solidification retarder is one of acetylacetone, p-hydroxyanisole, modified triethylene diamine and modified dimethylamino diethyl ether;
the antistatic agent is one of metal ion salt, ionic liquid and carbon nano tube.
6. The ultra-thin flexible glass manufacturing or shipping protective film of any of claims 1-3, further comprising a release film;
the release film is attached to one side face, far away from the base material, of the pressure-sensitive adhesive layer.
7. The method for preparing the protective film for ultra-thin flexible glass manufacturing or shipment according to any of claims 1 to 6, comprising the steps of:
adding the main body resin, the temperature-resistant auxiliary agent, the crosslinking agent, the curing retarder and the antistatic agent in the above amount into the solvent in the above amount, and uniformly stirring to obtain the pressure-sensitive adhesive solution;
coating the pressure-sensitive adhesive liquid on one side surface of the base material, and drying in an oven at the drying temperature of 40-130 ℃ to obtain a semi-finished product A;
attaching the release film to one side surface, far away from the base material, of the pressure-sensitive adhesive layer of the semi-finished product A to prepare a semi-finished product B;
And (3) curing the semi-finished product B in a curing chamber at the temperature of 20-70 ℃ for 24-240 hours to obtain the protective film for manufacturing or shipping the ultrathin flexible glass.
8. The method for preparing the protective film for ultrathin flexible glass manufacturing process or shipment according to claim 7, further comprising the following steps before the step of applying the pressure-sensitive adhesive solution to one side of the substrate:
and carrying out preheating treatment on the substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210240577.4A CN114672258A (en) | 2022-03-10 | 2022-03-10 | Protective film for manufacturing process or shipment of ultrathin flexible glass and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115491145A (en) * | 2022-11-17 | 2022-12-20 | 昆山博益鑫成高分子材料有限公司 | OLED (organic light emitting diode) process protective film and preparation method thereof |
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