CN113462302A - Low-climbing high-dyne-value polyurethane protective film and preparation method thereof - Google Patents

Low-climbing high-dyne-value polyurethane protective film and preparation method thereof Download PDF

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Publication number
CN113462302A
CN113462302A CN202110667561.7A CN202110667561A CN113462302A CN 113462302 A CN113462302 A CN 113462302A CN 202110667561 A CN202110667561 A CN 202110667561A CN 113462302 A CN113462302 A CN 113462302A
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pet film
temperature
layer
polyurethane
coating
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CN113462302B (en
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张峰
师强
李杰霞
余莉
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Sichuan Dongcai Technology Group Co Ltd
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Sichuan Dongcai Technology Group 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
    • 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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • 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
    • 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
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
    • C09J7/403—Adhesives in the form of films or foils characterised by release liners characterised by the structure of the release 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
    • 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
    • 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
    • C09J2467/005—Presence of polyester in the release coating
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/70—Wind energy
    • Y02E10/72—Wind turbines with rotation axis in wind direction

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Laminated Bodies (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a low-climbing high-dyne value polyurethane protective film and a preparation method thereof, which are characterized in that: the low-climbing high-dyne-value polyurethane protective film is formed by compounding a PET film layer, a bottom coating layer, a polyurethane adhesive layer, a release layer and the PET film layer in sequence. The preparation method comprises the following steps: mixing a polyurethane prepolymer, an isocyanate curing agent, a temperature-resistant hardening agent, a retarder and an organic solvent to prepare a polyurethane adhesive; coating a primer solution on one side of the PET film layer, and drying to form a primer layer; coating a polyurethane adhesive on the bottom coating, drying the polyurethane adhesive through a drying tunnel with the temperature of 65-130 ℃ and the total length of 24-45 m at the linear speed of 10-35 m/min, compounding the polyurethane adhesive with the single-sided release PET film, and curing to obtain the single-sided release PET film. The low-climbing high-dyne-value polyurethane protective film is suitable for protecting the surface of the copper foil adhesive tape in the processes of transportation, storage and manufacture, and has good performance and strong practicability.

Description

Low-climbing high-dyne-value polyurethane protective film and preparation method thereof
Technical Field
The invention belongs to a layered product and preparation thereof, and relates to a low-climbing high-dyne-value polyurethane protective film and a preparation method thereof. The low-climbing high-dyne-value polyurethane protective film (prepared) is mainly used on a copper foil adhesive tape, has a protective effect on the surface of the copper foil adhesive tape, prevents the surface of the copper foil from being oxidized, scratched, deliquesced and the like, and does not influence the use of the copper foil adhesive tape in the subsequent processing procedures of mobile phones, notebook computers and other digital products.
Background
With the rapid development of electronic products, the copper foil tape is widely applied to the transportation, storage and manufacturing processes of touch display panels of mobile phones, computers and other digital products, on one hand, the copper foil tape is easily oxidized and scratched in the transportation and storage processes and needs to be protected by a protective film on the surface of the copper foil, on the other hand, when the copper foil tape is subjected to pretreatment, a temperature resistance test needs to be carried out after being placed for 7 days at a temperature of 80 ℃, when the protective film is peeled off after the temperature resistance test, the change of the bonding force of the protective film is required to be not more than 300% of the initial bonding force, the surface tension of the copper foil is not influenced, and the dyne value of the surface of the copper foil is kept at 36 and above.
At present, the protective film for the surface of the copper foil mainly comprises a silica gel protective film and an acrylic protective film, and in the prior art, CN106752754A discloses a back adhesive polyurethane protective film and a preparation method thereof, which are mainly used in the automobile industry for enhancing the friction resistance and the weather resistance of the surface of an automobile; CN109111868A discloses 'an ultra-low tear film voltage polyurethane protective film and a preparation method thereof', which is used as an antistatic protective film for processing a touch screen; a protective film for a copper foil adhesive tape is not available in the prior art, and meanwhile, the protective film has temperature resistance, the climbing of the bonding force after temperature resistance is not more than 300% of the initial bonding force, and the protective film also has a literature report of a polyurethane protective film with a high dyne value on the surface of a copper foil.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a low-climbing high-dyne value polyurethane protective film and a preparation method thereof. The polyurethane protective film has the advantages that no residual glue, glue and silicon are left on the copper foil tape, after a temperature resistance test for 7 days at the temperature of 80 ℃, the protective film has low bonding force and high climbing rate, the climbing value is not more than 300% of the initial bonding force, and after the temperature resistance test, the dyne value of the surface of the copper foil is 36 or more, so that the polyurethane protective film is suitable for the low climbing high dyne value polyurethane protective film used in the transportation and manufacturing processes of the copper foil tape and the preparation method thereof.
The content of the invention is as follows: a low-climbing high-dyne value polyurethane protective film is characterized in that: the polyurethane protective film with the low climbing and the high dyne value is formed by compounding a (transparent) PET film layer (1), a primer layer (2) coated on one side (namely one side) of the (transparent) PET film layer (1), a polyurethane adhesive layer (3) coated on the primer layer (2), a release layer (4) coated on one side of the (transparent) PET film layer (5) and the (transparent) PET film layer (5) in sequence;
the PET film layer (namely the PET film) is a polyethylene terephthalate film layer for short, and the thickness of the PET film can be 10-125 micrometers;
the base coat (2) is prepared by coating (or coating) a base coat liquid on one side (namely one side) of the PET film layer (1) and then drying, wherein the base coat liquid can be any one of waterborne polyurethane (such as waterborne polyurethane with the brand number of 6274 (Dow Corning) sun-Tack U-120 (Su Xunzhou Xun Shang Ji Co., Ltd.), waterborne acrylic resin (such as waterborne acrylic resin with the brand number of 7499 (Dow Corning), Nnocryl A-1127 (Su Xun Co., Ltd.), and the like) and waterborne polyester (such as waterborne polyester with the brand number of P5200 ADHES PROMO (Dow Corning); the like); the production and provision enterprises of the base coating liquid comprise: dow Corning, Shenzhen, Shenli, Shenshu, Guangzhou Zhi research New materials, Guangzhou, Xunzhou, Xun Shang Mao, etc., the same as the above;
the polyurethane adhesive layer (3) is prepared by coating (or called coating) a polyurethane adhesive (or called polyurethane adhesive resin composition) on the bottom coating (2) and then drying, and the polyurethane adhesive comprises the following raw material components in percentage by mass:
40-70 parts by mass of polyurethane prepolymer (or polyurethane prepolymer resin), and product production providing enterprises comprise: nanjing bock new materials Co., Ltd, Shanghai trades Co., Ltd (i.e., Nippon lion), Changxing Chemicals, Taiwan New Industrial Co., Ltd, and the like, the same applies later;
3-15 parts by mass of an isocyanate curing agent, wherein the isocyanate curing agent is one or a mixture of more than two of methyl diisocyanate (TDI for short), isophorone diisocyanate (IPDI for short), diphenylmethane diisocyanate (MDI for short) and hexamethylene diisocyanate (HDI for short); the product production providing enterprises comprise: changxing chemistry, taiwan new synthesis industries ltd, kossi, basf, japan npu, winning, vencorex, wancor, etc., the same last;
2 ~ 8 parts by mass temperature resistant hardener, product production provides the enterprise and has: nanjing bock new material Co., Ltd, Shanghai trades Co., Ltd (i.e., King of Japan), Zhongshan city Co., Ltd and the like;
1-5 parts by mass of retarder, and product production providing enterprises have: nanjing Bokesi New Material Co., Ltd, Zhengzhou Yuyu chemical products Co., Ltd, Shanghai Yuji chemical industry Co., Ltd, and the like, the same applies later;
and 50-100 parts by mass of an organic solvent, wherein the organic solvent is one or a mixture of more than two of ethyl acetate, butanone, cyclohexanone, toluene, methyl isobutyl ketone, butyl acetate and methyl ethyl ketone;
the release layer (4) is prepared by coating (or called coating) a silicon-containing release agent on one side (namely one side) of the PET film layer (5) and then drying, wherein the release layer (4) and the PET film layer (5) form a single-side release PET film, and the single-side release PET film can be made by Sichuan Dong material science and technology group Limited company or can be a commercially available product.
The invention comprises the following steps: the (transparent) PET film layer (1) and/or the (transparent) PET film layer (5) are preferably the (transparent) PET film layer (1) and/or the (transparent) PET film layer (5) subjected to corona treatment.
The invention comprises the following steps: the specific preparation method of the single-sided release PET film comprises the following steps: coating a silicon-containing release agent layer on one side (namely one side) of the PET film on a coating machine, wherein the coating thickness is 0.3-1 mu m, and obtaining the coated single-side release PET film; the coated single-sided release PET film is operated at a linear speed of 35m/min, passes through a drying tunnel with the total length of 42m, and sequentially passes through the drying tunnel, wherein the temperature of the first section is 75 ℃, the temperature of the second section is 90 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 110 ℃ and the temperature of the sixth section is 100 ℃ to prepare the single-sided release PET film.
The silicon-containing release agent is a commercially available common silicon-containing release agent, and product providing enterprises comprise: dow kangning, Shenzhen, Chu hawk new materials Limited, Fushan Yiyousai new materials Limited.
The invention comprises the following steps: characterized in that: the thickness of the bottom coating (2) is preferably 0.1-0.5 μm, and the thickness of the polyurethane adhesive layer (3) is preferably 0.5-15 μm.
The invention comprises the following steps: the temperature-resistant hardening AGENT can be one of a temperature-resistant hardening AGENT of traded trades of Shanghai, namely Nippon lion, with the trade name of CROSSLINKING AGENT N and a temperature-resistant hardening AGENT of combined chemical industry of Zhongshan city, with the trade name of 3053;
the retarder may be any one of BPU retarder, BT-180 retarder of New Material Ltd of Bakko, Nanjing, and acetylacetone of Chengzhou Yuhe chemical products Ltd or Shanghai Yujiyi chemical industries Ltd.
Another aspect of the invention is: a preparation method of a low-climbing high-dyne-value polyurethane protective film is characterized by comprising the following steps:
a. preparing a polyurethane adhesive (or called polyurethane adhesive resin composition):
taking raw materials of 40-70 parts by mass of polyurethane prepolymer (or called polyurethane prepolymer resin), 3-15 parts by mass of isocyanate curing agent, 2-8 parts by mass of temperature-resistant hardening agent, 1-5 parts by mass of retarder and 50-100 parts by mass of organic solvent according to the raw material components and mass ratio, and uniformly mixing (forming a uniform solution of a body system) to obtain the polyurethane adhesive;
the isocyanate curing agent is one or a mixture of more than two of methyl diisocyanate (TDI for short), isophorone diisocyanate (IPDI for short), diphenylmethane diisocyanate (MDI for short) and hexamethylene diisocyanate (HDI for short);
the organic solvent is one or a mixture of more than two of ethyl acetate, butanone, cyclohexanone, toluene, methyl isobutyl ketone, butyl acetate and methyl ethyl ketone.
The viscosity of the prepared polyurethane adhesive is 50-500 cps (at 25 ℃);
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating (or called coating) a layer of primer on one side (surface) of a PET film layer (1) by taking the PET film layer (1) (namely the PET film), and drying at the temperature of 80-120 ℃ for 1-10 minutes to form a primer layer (2);
uniformly coating (or called coating) the polyurethane adhesive prepared in the step a on a bottom coating (2) by using a comma scraper or a slit at the temperature of 20-25 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 0.5-15 mu m, and thus obtaining the PET film after coating; the glued PET film passes through a drying tunnel with the total length of 24-45 m at a linear speed (operation) of 10-35 m/min, sequentially passes through the drying tunnel with the first section temperature of 65-85 ℃, the second section temperature of 95-110 ℃, the third section temperature of 100-130 ℃, the fourth section temperature of 110-130 ℃, the fifth section temperature of 110-130 ℃ and the VI section temperature of 100-110 ℃, is further polymerized and is subjected to solvent removal in the polyurethane adhesive, and the PET film with the polyurethane adhesive layer is prepared;
then compounding one surface of a release layer (4) of the single-sided release PET film with one surface of a polyurethane adhesive layer of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.4-0.5 MPa and the temperature is room temperature (25 ℃), finally putting the PET film into a drying room at 40-60 ℃ for curing for 24-72 hours to obtain the low-climbing high-dyne value polyurethane protective film, and further rolling, slitting, packaging, warehousing and the like the prepared low-climbing high-dyne value polyurethane protective film;
the PET film layer (namely the PET film) is a polyethylene glycol terephthalate film layer for short, and the thickness of the PET film layer (namely the PET film) can be 10-125 micrometers;
the primer solution is any one of waterborne polyurethane, waterborne acrylic resin and waterborne polyester;
the release layer (4) is prepared by coating (or called coating) a silicon-containing release agent on one side (namely one side) of the PET film layer (5) and then drying, wherein the release layer (4) and the PET film layer (5) form a single-side release PET film, and the single-side release PET film can be made by Sichuan Dong material science and technology group Limited company or can be a commercially available product.
In another aspect of the invention: the PET film layer (1) and/or the (transparent) PET film layer (5) are/is preferably the PET film layer (1) and/or the (transparent) PET film layer (5) subjected to corona treatment;
in another aspect of the invention: the specific preparation method of the single-sided release PET film comprises the following steps: coating a silicon-containing release agent layer on one side (namely one side) of the PET film on a coating machine, wherein the coating thickness is 0.3-1 mu m, and obtaining the coated single-side release PET film; the coated single-sided release PET film is operated at a linear speed of 35m/min, passes through a drying tunnel with the total length of 42m, and sequentially passes through the drying tunnel, wherein the temperature of the first section is 75 ℃, the temperature of the second section is 90 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 110 ℃ and the temperature of the sixth section is 100 ℃ to prepare the single-sided release PET film.
The silicon-containing release agent is a commercially available common silicon-containing release agent, and product providing enterprises comprise: dow kangning, Shenzhen, Chu hawk new materials Limited, Fushan Yiyousai new materials Limited.
In another aspect of the invention: the thickness of the bottom coating (2) is preferably 0.1-0.5 μm, and the thickness of the polyurethane adhesive layer (3) is preferably 0.5-15 μm.
In another aspect of the invention: the temperature-resistant hardening AGENT in the step a can be one of a temperature-resistant hardening AGENT of traded company of Shanghai, namely Nippon Shiwang, with the trade name of CROSSLINKING AGENT N and a temperature-resistant hardening AGENT of combined chemical company of Zhongshan city with the trade name of 3053;
the retarder in the step a may be any one of BPU retarder, BT-180 retarder of Nanjing Baker New Material Co., Ltd, and acetylacetone of Zhengzhou Yuhe chemical products Co., Ltd or Shanghai Yuji chemical industries Co., Ltd.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
(1) according to the invention, the polyurethane adhesive is prepared by the polyurethane prepolymer, the isocyanate curing agent, the temperature-resistant hardening agent, the retarder and the organic solvent, the polyurethane adhesive is uniformly coated on the surface of the PET film by a coating process, and a compact polyurethane adhesive layer is formed by drying, wherein the adhesive layer has good stability and air release performance, and does not drop adhesive, silicon and residual adhesive, so that the low-climbing high-dyne value polyurethane protective film with good performance is obtained;
(2) the low-climbing high-dyne-value polyurethane protective film (prepared) plays a role of a protective film in the processes of transportation, storage and manufacture procedure of a copper foil adhesive tape, prevents the copper foil adhesive tape from being oxidized, scratched and the like, and meanwhile, after the surface of the copper foil adhesive tape is attached, the protective film is peeled off after a temperature resistance test (placed at the temperature of 80 ℃ for 7 days), the bonding force of the protective film does not exceed 300% of the initial bonding force of the protective film, and after the protective film is peeled off, the surface tension of the copper foil is not influenced, namely the dyne value of the surface of the copper foil is kept at 36 or above;
(3) according to the low-climbing high-dyne-value polyurethane protective film, an automatic contact angle measuring device (model: HD-U805-2) manufactured by Haada instruments Limited of Dongguan city of China is adopted, the contact angle of the protective film and water is measured, the contact angle of the protective film and the water is 85.0-90.0 degrees, and the surface of copper foil can keep good surface tension;
(4) the low-climbing high-dyne-value polyurethane protective film is a protective film with low film tearing voltage, low viscosity and no adhesive residue, has temperature resistance, has the advantages that the climbing of the bonding force does not exceed 300 percent of the initial bonding force after temperature resistance, has the dyne value on the surface of a copper foil, keeps the dyne value at 36 or above, and is suitable for the use of a copper foil adhesive tape in the processes of transportation, storage and manufacture procedure; the preparation process is simple, easy to operate and high in practicability.
Drawings
FIG. 1 is a schematic cross-sectional structural view of a low-climb high-dyne polyurethane protective film (prepared) using the present invention and examples;
in the figure: 1. 5-polyethylene terephthalate film layer (PET film layer), 2-bottom coating layer, 3-polyurethane adhesive layer and 4-release layer.
Detailed Description
The following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims appended hereto.
Example 1: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive (or called polyurethane adhesive resin composition):
at room temperature, 50 parts by mass of polyurethane prepolymer, 5 parts by mass of isocyanate curing AGENT [ methyl diisocyanate (TDI) ], 3 parts by mass of temperature-resistant hardening AGENT (the temperature-resistant hardening AGENT with the brand number of CROSSLINKING AGENT N of Shanghai trades company Limited (namely Japan lion), 1 part by mass of retarder (BPU retarder of Nanjing bock new material Co., Ltd.), and 70 parts by mass of organic solvent (ethyl acetate) are put into a container and uniformly mixed (a uniform solution of a formation system) to prepare the polyurethane adhesive; the viscosity of the prepared polyurethane adhesive is 230cps (25 ℃);
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating (or called coating) a layer of primer solution (selected from waterborne polyurethane) on one surface of a PET film, and drying at 90 ℃ for 2 minutes to form a primer layer 2, wherein the thickness of the primer layer is 0.2 mu m;
uniformly coating (or called coating) the polyurethane adhesive prepared in the step a on the base coat 2 (by using a comma scraper or a slit) at the temperature of 22 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 5 mu m, and obtaining a coated PET film; the PET film after gluing is passed through a drying tunnel with the total length of 42m at the linear speed (operation) of 25m/min, and sequentially passed through the drying tunnel, wherein the temperature of the first section is 70 ℃, the temperature of the second section is 95 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 120 ℃ and the temperature of the sixth section is 100 ℃, and further polymerization is carried out and the solvent in the polyurethane adhesive is removed, so as to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.4MPa and the temperature is room temperature (25 ℃), finally placing the PET film into a drying room at 45 ℃ for curing for 48 hours to obtain the low-climbing high-dyne value polyurethane protective film, and further rolling, slitting, packaging, warehousing and the like the obtained low-climbing high-dyne value polyurethane protective film.
Through detection: the initial adhesion of the low-climb high-dyne polyurethane protective film prepared in this example was 6.3gf/25mm, the dyne value of the protective film surface was 34, and the dyne value of the copper foil tape was 40; the adhesion force is 15.8gf/25mm after 7 days at the temperature of 80 ℃, and the dyne value of the copper foil at the position where the protective film is attached is 38; the contact angle between the copper foil surface of the copper foil tape and water is 88.4 degrees, and the contact angle between the copper foil attached to the protective film and water is 86.7 degrees.
Example 2: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive (or called polyurethane adhesive resin composition):
putting 55 parts by mass of polyurethane prepolymer, 7 parts by mass of isocyanate curing AGENT [ isophorone diisocyanate (IPDI) ], 2 parts by mass of temperature-resistant hardening AGENT (the temperature-resistant hardening AGENT with the trade name of CROSSLINKING AGENT N of Shanghai Changjiang trade company Limited (namely Japan lion king)), 1 part by mass of retarder (BT-180 retarder of Nanjing Pockesi New Material Co., Ltd.), and 80 parts by mass of organic solvent (ethyl acetate) into a container at room temperature, and uniformly mixing (forming a uniform solution), thereby preparing the polyurethane adhesive; the viscosity of the prepared polyurethane adhesive is 245cps (25 ℃);
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating a layer of primer solution (selected from waterborne polyurethane) on one surface (surface) of a PET film, and drying at 90 ℃ for 2 minutes to form a primer layer 2 with the thickness of 0.2 mu m;
uniformly coating (or called coating) the polyurethane adhesive prepared in the step a on the bottom coating layer 2 (by using a comma scraper or a slit) at the temperature of 20 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 5 mu m, and obtaining a coated PET film; the PET film after gluing is passed through a drying tunnel with the total length of 42m at the linear speed (operation) of 25m/min, and sequentially passed through the drying tunnel, wherein the temperature of the first section is 70 ℃, the temperature of the second section is 95 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 120 ℃ and the temperature of the sixth section is 100 ℃, and further polymerization is carried out and the solvent in the polyurethane adhesive is removed, so as to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.4MPa and the temperature is room temperature (25 ℃), finally placing the PET film into a drying room at 45 ℃ for curing for 48 hours to obtain the low-climbing high-dyne value polyurethane protective film, and further rolling, slitting, packaging, warehousing and the like the obtained low-climbing high-dyne value polyurethane protective film.
Through detection: the initial adhesion of the low-climb high-dyne polyurethane protective film prepared in this example was 5.4gf/25mm, the dyne value of the protective film surface was 34, and the dyne value of the copper foil tape was 40; the adhesion force after 7 days at 80 ℃ is 14.3gf/25mm, and the dyne value of the copper foil at the position where the protective film is attached is 38; the contact angle between the copper foil surface of the copper foil tape and water is 88.4 degrees, and the contact angle between the copper foil attached to the protective film and water is 87.1 degrees.
Example 3: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive (or called polyurethane adhesive resin composition):
at room temperature, 70 parts by mass of polyurethane prepolymer, 8 parts by mass of isocyanate curing agent [ diphenylmethane diisocyanate (MDI) ], 6 parts by mass of temperature-resistant hardening agent (3053 brand of Zhongshan City. Co., Ltd.), 3 parts by mass of retarder (acetylacetone of Zhengzhou Yuhe chemical products Co., Ltd. or Shanghai Yuji chemical industries Co., Ltd.), and 80 parts by mass of organic solvent (ethyl acetate) are put into a container and uniformly mixed (a uniform solution of a formation system is formed), thus obtaining the polyurethane adhesive; the viscosity of the prepared polyurethane adhesive is 391cps at 25 ℃;
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating a layer of primer solution (selected from waterborne polyurethane) on one surface (surface) of a PET film, and drying at 90 ℃ for 2 minutes to form a primer layer 2 with the thickness of 0.2 mu m;
uniformly coating (or called coating) the polyurethane adhesive prepared in the step a on the bottom coating layer 2 (by using a comma scraper or a slit) at the temperature of 25 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 5 mu m, and obtaining a coated PET film; the PET film after gluing is passed through a drying tunnel with the total length of 42m at the linear speed (operation) of 25m/min, and sequentially passed through the drying tunnel, wherein the temperature of the first section is 70 ℃, the temperature of the second section is 95 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 120 ℃ and the temperature of the sixth section is 100 ℃, and further polymerization is carried out and the solvent in the polyurethane adhesive is removed, so as to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.4MPa and the temperature is room temperature (25 ℃), finally placing the PET film into a drying room at 45 ℃ for curing for 48 hours to obtain the low-climbing high-dyne value polyurethane protective film, and further rolling, slitting, packaging, warehousing and the like the obtained low-climbing high-dyne value polyurethane protective film.
Through detection: the initial adhesion of the low-climb high-dyne polyurethane protective film prepared in this example was 4.2gf/25mm, the dyne value of the protective film surface was 34, and the dyne value of the copper foil tape was 40; the adhesion force is 8.9gf/25mm after 7 days at the temperature of 80 ℃, and the dyne value of the copper foil at the position where the protective film is attached is 40; the contact angle between the copper foil surface of the copper foil tape and water is 89.6 degrees, and the contact angle between the copper foil attached to the protective film and the water is 89.2 degrees.
Example 4: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive (or called polyurethane adhesive resin composition):
adding 65 parts by mass of polyurethane prepolymer, 7 parts by mass of isocyanate curing agent [ Hexamethylene Diisocyanate (HDI) ], 5 parts by mass of temperature-resistant hardening agent (3053 brand of Zhongshan City Confucius chinensis Co., Ltd.), 3 parts by mass of retarder (acetylacetone of Zhengzhou Yuhe chemical products Co., Ltd. or Shanghai Yuji Co., Ltd.), and 85 parts by mass of organic solvent (ethyl acetate) into a container at room temperature, and uniformly mixing (forming a uniform solution of a body system), thereby preparing the polyurethane adhesive; the viscosity of the prepared polyurethane adhesive is 363cps (25 ℃);
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating a layer of primer solution (selected from waterborne polyurethane) on one surface (surface) of a PET film, and drying at the temperature of 95 ℃ for 2 minutes to form a primer layer 2 with the thickness of 0.2 mu m;
uniformly coating (or called coating) the polyurethane adhesive prepared in the step a on the base coat 2 (by using a comma scraper or a slit) at the temperature of 23 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 10 mu m, and obtaining a coated PET film; the glued PET film passes through a drying tunnel with the total length of 42m at the linear speed (operation) of 20m/min, and sequentially passes through the drying tunnel, wherein the temperature of the first section is 70 ℃, the temperature of the second section is 95 ℃, the temperature of the third section is 110 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 120 ℃ and the temperature of the sixth section is 100 ℃, and the PET film is further polymerized and the solvent in the polyurethane adhesive is removed to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.5MPa and the temperature is room temperature (25 ℃), finally placing the PET film into a drying room at 45 ℃ for curing for 48 hours to obtain the low-climbing high-dyne value polyurethane protective film, and further rolling, slitting, packaging, warehousing and the like the prepared low-climbing high-dyne value polyurethane protective film;
through detection: the initial adhesion of the low-climb high-dyne polyurethane protective film prepared in this example was 4.6gf/25mm, the dyne value of the protective film surface was 34, and the dyne value of the copper foil tape was 40; the adhesion force is 10.5gf/25mm after 7 days at the temperature of 80 ℃, and the dyne value of the copper foil at the position where the protective film is attached is 40; the contact angle between the copper foil surface of the copper foil tape and water is 89.6 degrees, and the contact angle between the copper foil attached to the protective film and the water is 89.0 degrees.
In examples 1-4 above:
the PET film layer (namely PET film) is a polyethylene terephthalate film layer for short, and the PET film is a polyethylene terephthalate film;
the thickness of the PET film can be any one of 10-125 micrometers;
the release layer 4 is prepared by coating (or called coating) a silicon-containing release agent on one side (namely one side) of the PET film layer 5 and then drying, the release layer 4 and the PET film layer 5 form a single-side release PET film, and the single-side release PET film can be made by Sichuan Dong material science and technology group, Inc. or can be a commercially available product.
In examples 1-4 above: the specific preparation method of the single-sided release PET film can be as follows: coating a silicon-containing release agent layer on one side (namely one side) of the PET film on a coating machine, wherein the coating thickness is one of 0.3-1 mu m, so as to obtain the coated single-side release PET film; running the coated single-sided release PET film at a linear speed of 35m/min, passing through a drying tunnel with the total length of 42m, and sequentially passing through the drying tunnel, wherein the temperature of the first section is 75 ℃, the temperature of the second section is 90 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 110 ℃ and the temperature of the sixth section is 100 ℃ to prepare the single-sided release PET film;
the silicon-containing release agent is a commercially available common silicon-containing release agent, and product providing enterprises comprise: dow kangning, Shenzhen, Chu hawk new materials Limited, Fushan Yiyousai new materials Limited.
Example 5: see the drawings.
A low-climbing high-dyne value polyurethane protective film is composed of a (transparent) PET film layer 1, a primer layer 2 coated on one side (namely one side) of the (transparent) PET film layer 1, a polyurethane adhesive layer 3 coated on the primer layer 2, a release layer 4 coated on one side of a (transparent) PET film layer 5 and the (transparent) PET film layer 5 in sequence;
the base coat 2 is prepared by coating (or called coating) base coat liquid on one side (namely one side) of the PET film layer 1 and then drying;
the polyurethane adhesive layer 3 is prepared by coating a polyurethane adhesive (or called polyurethane adhesive resin composition, and the same) on the bottom coating 2 and then drying, and the polyurethane adhesive comprises the following raw material components in percentage by mass: 40 parts by mass of polyurethane prepolymer, 3 parts by mass of isocyanate curing agent, 2 parts by mass of temperature-resistant hardening agent, 1 part by mass of retarder and 50 parts by mass of organic solvent.
Example 6: see the drawings.
A low-climbing high-dyne value polyurethane protective film is composed of a (transparent) PET film layer 1, a primer layer 2 coated on one side (namely one side) of the (transparent) PET film layer 1, a polyurethane adhesive layer 3 coated on the primer layer 2, a release layer 4 coated on one side of a (transparent) PET film layer 5 and the (transparent) PET film layer 5 in sequence;
the base coat 2 is prepared by coating (or called coating) base coat liquid on one side (namely one side) of the PET film layer 1 and then drying;
the polyurethane adhesive layer 3 is prepared by coating (or called coating) a polyurethane adhesive on the bottom coating 2 and then drying, and the polyurethane adhesive comprises the following raw material components in percentage by mass: 70 parts by mass of polyurethane prepolymer, 15 parts by mass of isocyanate curing agent, 8 parts by mass of temperature-resistant hardening agent, 5 parts by mass of retarder and 100 parts by mass of organic solvent.
Example 7: see the drawings.
A low-climbing high-dyne value polyurethane protective film is composed of a (transparent) PET film layer 1, a primer layer 2 coated on one side (namely one side) of the (transparent) PET film layer 1, a polyurethane adhesive layer 3 coated on the primer layer 2, a release layer 4 coated on one side of a (transparent) PET film layer 5 and the (transparent) PET film layer 5 in sequence;
the base coat 2 is prepared by coating (or called coating) base coat liquid on one side (namely one side) of the PET film layer 1 and then drying;
the polyurethane adhesive layer 3 is prepared by coating (or called coating) a polyurethane adhesive on the bottom coating 2 and then drying, and the polyurethane adhesive comprises the following raw material components in percentage by mass: 55 parts by mass of a polyurethane prepolymer, 9 parts by mass of an isocyanate curing agent, 5 parts by mass of a temperature-resistant hardener, 3 parts by mass of a retarder, and 75 parts by mass of an organic solvent.
Example 8: see the drawings.
A low-climbing high-dyne value polyurethane protective film is composed of a (transparent) PET film layer 1, a primer layer 2 coated on one side (namely one side) of the (transparent) PET film layer 1, a polyurethane adhesive layer 3 coated on the primer layer 2, a release layer 4 coated on one side of a (transparent) PET film layer 5 and the (transparent) PET film layer 5 in sequence;
the base coat 2 is prepared by coating (or called coating) base coat liquid on one side (namely one side) of the PET film layer 1 and then drying;
the polyurethane adhesive layer 3 is prepared by coating (or called coating) a polyurethane adhesive on the bottom coating 2 and then drying, and the polyurethane adhesive comprises the following raw material components in percentage by mass: 45 parts by mass of a polyurethane prepolymer, 4 parts by mass of an isocyanate curing agent, 3 parts by mass of a temperature-resistant hardener, 1.5 parts by mass of a retarder, and 60 parts by mass of an organic solvent.
Example 9: see the drawings.
A low-climbing high-dyne value polyurethane protective film is composed of a (transparent) PET film layer 1, a primer layer 2 coated on one side (namely one side) of the (transparent) PET film layer 1, a polyurethane adhesive layer 3 coated on the primer layer 2, a release layer 4 coated on one side of a (transparent) PET film layer 5 and the (transparent) PET film layer 5 in sequence;
the base coat 2 is prepared by coating (or called coating) base coat liquid on one side (namely one side) of the PET film layer 1 and then drying;
the polyurethane adhesive layer 3 is prepared by coating (or called coating) a polyurethane adhesive on the bottom coating 2 and then drying, and the polyurethane adhesive comprises the following raw material components in percentage by mass: 50 parts by mass of a polyurethane prepolymer, 5 parts by mass of an isocyanate-based curing agent, 3.5 parts by mass of a temperature-resistant curing agent, 2.5 parts by mass of a retarder, and 66 parts by mass of an organic solvent.
Example 10: see the drawings.
A low-climbing high-dyne value polyurethane protective film is composed of a (transparent) PET film layer 1, a primer layer 2 coated on one side (namely one side) of the (transparent) PET film layer 1, a polyurethane adhesive layer 3 coated on the primer layer 2, a release layer 4 coated on one side of a (transparent) PET film layer 5 and the (transparent) PET film layer 5 in sequence;
the base coat 2 is prepared by coating (or called coating) base coat liquid on one side (namely one side) of the PET film layer 1 and then drying;
the polyurethane adhesive layer 3 is prepared by coating (or called coating) a polyurethane adhesive on the bottom coating 2 and then drying, and the polyurethane adhesive comprises the following raw material components in percentage by mass: 65 parts by mass of polyurethane prepolymer, 13 parts by mass of isocyanate curing agent, 7 parts by mass of temperature-resistant curing agent, 4.5 parts by mass of retarder and 90 parts by mass of organic solvent.
Example 11: see the drawings.
A low-climbing high-dyne value polyurethane protective film is composed of a (transparent) PET film layer 1, a primer layer 2 coated on one side (namely one side) of the (transparent) PET film layer 1, a polyurethane adhesive layer 3 coated on the primer layer 2, a release layer 4 coated on one side of a (transparent) PET film layer 5 and the (transparent) PET film layer 5 in sequence;
the base coat 2 is prepared by coating (or called coating) base coat liquid on one side (namely one side) of the PET film layer 1 and then drying;
the polyurethane adhesive layer 3 is prepared by coating (or called coating) a polyurethane adhesive on the bottom coating 2 and then drying, and the polyurethane adhesive comprises the following raw material components in percentage by mass: 55 parts by mass of polyurethane prepolymer, 11 parts by mass of isocyanate curing agent, 6.5 parts by mass of temperature-resistant hardening agent, 3.5 parts by mass of retarder and 75 parts by mass of organic solvent.
In examples 5 to 11 above:
the PET film layer (namely the PET film) is a polyethylene terephthalate film layer for short, and the thickness of the PET film can be any one of 10-125 micrometers;
the primer can be any one of waterborne polyurethane (such as the waterborne polyurethane with the brand number of 6274 (Dow Corning) sun-Tack U-120 (the product of Xunzhou dynasty Co., Ltd., the same below), waterborne acrylic resin (such as the waterborne acrylic resin with the brand number of 7499 (Dow Corning), Nnocryl A-1127 (the product of Guangzhou dynasty Co., Ltd.), the same below) and waterborne polyester (such as the waterborne polyester with the brand number of P5200 ADHES PROMO (Dow Corning Co., Ltd., the same below); the production and provision enterprises of the base coating liquid comprise: dow Corning, Shenzhen, Shenli, Shenshu, Guangzhou Zhi research New materials, Guangzhou, Xunzhou, Xun Shang Mao, etc., the same as the above;
the polyurethane prepolymer (or polyurethane prepolymer resin) and product production providing enterprises comprise: nanjing bock new materials Co., Ltd, Shanghai trades Co., Ltd (i.e., Nippon lion), Changxing Chemicals, Taiwan New Industrial Co., Ltd, and the like, the same applies later;
the isocyanate curing agent can be one or a mixture of more than two of methyl diisocyanate (TDI for short), isophorone diisocyanate (IPDI for short), diphenylmethane diisocyanate (MDI for short) and hexamethylene diisocyanate (HDI for short); the product production providing enterprises comprise: changxing chemistry, taiwan new synthesis industries ltd, kossi, basf, japan npu, winning, vencorex, wancor, etc., the same last;
the temperature-resistant hardening AGENT can be one of a temperature-resistant hardening AGENT of traded trades of Shanghai, namely Nippon lion, with the trade name of CROSSLINKING AGENT N and a temperature-resistant hardening AGENT of combined chemical industry of Zhongshan city, with the trade name of 3053;
the retarder can be any one of BPU retarder, BT-180 retarder and acetylacetone of Zhengzhou Yuhe chemical products company Limited or Shanghai Yugji chemical products company Limited of Nanjing Pocksi new material company Limited;
the organic solvent can be one or a mixture of more than two of ethyl acetate, butanone, cyclohexanone, toluene, methyl isobutyl ketone, butyl acetate and methyl ethyl ketone;
the release layer 4 is prepared by coating (or called coating) a silicon-containing release agent on one side (namely one side) of the PET film layer 5 and then drying, the release layer 4 and the PET film layer 5 form a single-side release PET film, and the single-side release PET film can be made by Sichuan Dong material science and technology group, Inc. or can be a commercially available product.
In examples 5 to 11 above: the specific preparation method of the single-sided release PET film can be as follows: coating a silicon-containing release agent layer on one side (namely one side) of the PET film on a coating machine, wherein the coating thickness is one of 0.3-1 mu m, so as to obtain the coated single-side release PET film; running the coated single-sided release PET film at a linear speed of 35m/min, passing through a drying tunnel with the total length of 42m, and sequentially passing through the drying tunnel, wherein the temperature of the first section is 75 ℃, the temperature of the second section is 90 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 110 ℃ and the temperature of the sixth section is 100 ℃ to prepare the single-sided release PET film; the method is the same as the prior art;
the silicon-containing release agent is a commercially available common silicon-containing release agent, and product providing enterprises comprise: dow kangning, Shenzhen, Chu hawk new materials Limited, Fushan Yiyousai new materials Limited.
In examples 5 to 11 above: the thickness of the bottom coating layer 2 is any one of 0.1-0.5 mu m, and the thickness of the polyurethane adhesive layer 3 is any one of 0.5-15 mu m.
Example 12:
a low-climbing high-dyne value polyurethane protective film is characterized in that a (transparent) PET film layer 1 and a (transparent) PET film layer 5 are subjected to corona treatment to form the (transparent) PET film layer 1 and the (transparent) PET film layer 5; otherwise, the same as in any of examples 5 to 11 was omitted.
Example 13:
a low-climbing high-dyne value polyurethane protective film is characterized in that a (transparent) PET film layer 1 is subjected to corona treatment; otherwise, the same as in any of examples 5 to 11 was omitted.
Example 14:
the low-climbing high-dyne value polyurethane protective film is characterized in that the (transparent) PET film layer 5 is subjected to corona treatment; otherwise, the same as in any of examples 5 to 11 was omitted.
Example 15: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive (or called polyurethane adhesive resin composition, the same applies hereinafter):
taking raw materials of 55 parts by mass of polyurethane prepolymer (or called polyurethane prepolymer resin, the same applies later), 9 parts by mass of isocyanate curing agent, 5 parts by mass of temperature-resistant hardening agent, 3 parts by mass of retarder and 75 parts by mass of organic solvent, and mixing the raw materials uniformly (forming a uniform solution of a body system) at room temperature to obtain the polyurethane adhesive;
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating (or called coating, the same as the latter) a layer of primer on one side (surface) of a PET film layer 1 (namely the PET film) and drying at the temperature of 100 ℃ for 6 minutes to form a primer layer 2;
uniformly coating (or called coating) the polyurethane adhesive prepared in the step a on the base coat 2 (by using a comma scraper or a slit) at the temperature of 22 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 8 mu m, and obtaining a coated PET film; the PET film after gluing is passed through a drying tunnel with the total length of 33m at a linear speed (operation) of 23m/min, and sequentially passed through the drying tunnel, wherein the temperature of the first section is 75 ℃, the temperature of the second section is 102 ℃, the temperature of the third section is 115 ℃, the temperature of the fourth section is 120 ℃, the temperature of the fifth section is 120 ℃ and the temperature of the sixth section is 105 ℃, and further polymerization is carried out and the solvent in the polyurethane adhesive is removed, so as to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.45MPa and the temperature is room temperature (25 ℃), and finally placing the PET film into a drying room at 50 ℃ for curing for 48 hours to obtain the low-climbing high-dyne value polyurethane protective film; and further, the prepared low-climbing high-dyne value polyurethane protective film can be rolled, cut, packaged and put in storage and the like.
Example 16: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive:
taking raw materials of 40 parts by mass of polyurethane prepolymer, 3 parts by mass of isocyanate curing agent, 2 parts by mass of temperature-resistant hardening agent, 1 part by mass of retarder and 50 parts by mass of organic solvent according to the raw material composition and mass ratio, and uniformly mixing (forming a uniform solution of a body system) to obtain a polyurethane adhesive;
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating a layer of primer solution on one side (surface) of a PET film layer 1 by taking the PET film layer 1, and drying at the temperature of 80 ℃ for 10 minutes to form a primer layer 2;
uniformly coating the polyurethane adhesive prepared in the step a on the base coating layer 2 (by using a comma scraper or a slit) at the temperature of 20 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 0.5 mu m, and thus obtaining a coated PET film; the PET film after gluing is passed through a drying tunnel with the total length of 24m at the linear speed (operation) of 10m/min, and sequentially passed through the drying tunnel, wherein the temperature of the first section is 65 ℃, the temperature of the second section is 95 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 110 ℃ and the temperature of the sixth section is 100 ℃, and further polymerization is carried out and the solvent in the polyurethane adhesive is removed, so as to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.4MPa and the temperature is room temperature (25 ℃), and finally placing the PET film into a drying room at 40 ℃ for curing for 72 hours to obtain the low-climbing high-dyne value polyurethane protective film; and further, the prepared low-climbing high-dyne value polyurethane protective film can be rolled, cut, packaged and put in storage and the like.
Example 17: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive:
taking raw materials of 70 parts by mass of polyurethane prepolymer, 15 parts by mass of isocyanate curing agent, 8 parts by mass of temperature-resistant hardening agent, 5 parts by mass of retarder and 100 parts by mass of organic solvent according to the raw material composition and mass ratio, and uniformly mixing (forming a uniform solution of a body system) to obtain a polyurethane adhesive;
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating a layer of primer solution on one side (surface) of a PET film layer 1 by taking the PET film layer 1, and drying at the temperature of 120 ℃ for 1 minute to form a primer layer 2;
uniformly coating the polyurethane adhesive prepared in the step a (by using a comma scraper or a slit) on the bottom coating layer 2 at the temperature of 25 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 15 mu m, and obtaining a coated PET film; the glued PET film passes through a drying tunnel with the total length of 45m at a linear speed (operation) of 35m/min, and sequentially passes through the drying tunnel, wherein the temperature of the first section is 85 ℃, the temperature of the second section is 110 ℃, the temperature of the third section is 130 ℃, the temperature of the fourth section is 130 ℃, the temperature of the fifth section is 130 ℃ and the temperature of the sixth section is 110 ℃, and the PET film is further polymerized and the solvent in the polyurethane adhesive is removed to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.5MPa and the temperature is room temperature (25 ℃), and finally placing the PET film into a drying room at 60 ℃ for curing for 24 hours to obtain the low-climbing high-dyne value polyurethane protective film; and further, the prepared low-climbing high-dyne value polyurethane protective film can be rolled, cut, packaged and put in storage and the like.
Example 18: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive:
taking raw materials of 50 parts by mass of polyurethane prepolymer, 5 parts by mass of isocyanate curing agent, 3.5 parts by mass of temperature-resistant hardening agent, 2 parts by mass of retarder and 65 parts by mass of organic solvent according to the raw material component composition and mass ratio, and uniformly mixing (forming a uniform solution of a body system) to obtain a polyurethane adhesive;
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating a layer of primer solution on one side (surface) of a PET film layer 1 by taking the PET film layer 1, and drying at the temperature of 85 ℃ for 4 minutes to form a primer layer 2;
uniformly coating the polyurethane adhesive prepared in the step a (by using a comma scraper or a slit) on the bottom coating layer 2 at the temperature of 21 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 3 mu m, and thus obtaining a coated PET film; the PET film after gluing is passed through a drying tunnel with the total length of 30m at a linear speed (operation) of 15m/min, and sequentially passed through the drying tunnel, wherein the temperature of the first section is 72 ℃, the temperature of the second section is 100 ℃, the temperature of the third section is 105 ℃, the temperature of the fourth section is 118 ℃, the temperature of the fifth section is 118 ℃ and the temperature of the sixth section is 103 ℃, and further polymerization is carried out and the solvent in the polyurethane adhesive is removed, so as to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.4MPa and the temperature is room temperature (25 ℃), and finally placing the PET film into a drying room at 45 ℃ for curing for 60 hours to obtain the low-climbing high-dyne value polyurethane protective film; and further, the prepared low-climbing high-dyne value polyurethane protective film can be rolled, cut, packaged and put in storage and the like.
Example 19: see the drawings.
A preparation method of a low-climbing high-dyne-value polyurethane protective film comprises the following steps:
a. preparing a polyurethane adhesive:
taking raw materials of 66 parts by mass of polyurethane prepolymer, 13 parts by mass of isocyanate curing agent, 7 parts by mass of temperature-resistant hardening agent, 4 parts by mass of retarder and 90 parts by mass of organic solvent at room temperature, and uniformly mixing (forming a uniform solution of a body system) to obtain a polyurethane adhesive;
b. preparing a low-climbing high-dyne-value polyurethane protective film:
coating a layer of primer solution on one side (surface) of a PET film layer 1 by taking the PET film layer 1, and drying at the temperature of 110 ℃ for 2 minutes to form a primer layer 2;
uniformly coating the polyurethane adhesive prepared in the step a on the base coating layer 2 (by using a comma scraper or a slit) at the temperature of 24 ℃ on a coating machine, wherein the coating thickness (namely the thickness of the polyurethane adhesive) is 12 mu m, and obtaining a coated PET film; the PET film after gluing is passed through a drying tunnel with the total length of 40m at the linear speed (operation) of 28m/min, and sequentially passed through the drying tunnel, wherein the temperature of the first section is 80 ℃, the temperature of the second section is 105 ℃, the temperature of the third section is 120 ℃, the temperature of the fourth section is 125 ℃, the temperature of the fifth section is 125 ℃, and the temperature of the sixth section is 108 ℃, and further polymerization is carried out and the solvent in the polyurethane adhesive is removed, so as to prepare the PET film with the polyurethane adhesive layer;
then compounding the release layer 4 side of the single-sided release PET film with the polyurethane adhesive layer side of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a compression roller is 0.5MPa and the temperature is room temperature (25 ℃), and finally placing the PET film into a drying room at 55 ℃ for curing for 36 hours to obtain the low-climbing high-dyne value polyurethane protective film; and further, the prepared low-climbing high-dyne value polyurethane protective film can be rolled, cut, packaged and put in storage and the like.
Example 20:
a preparation method of a low-climbing high-dyne-value polyurethane protective film is characterized in that a PET film layer 1 and a (transparent) PET film layer 5 are subjected to corona treatment to form the PET film layer 1 and the (transparent) PET film layer 5; otherwise, the same as in any of examples 15 to 19, are omitted.
Example 21:
a preparation method of a low-climbing polyurethane protective film with a high dyne value is characterized in that a PET film layer 1 is subjected to corona treatment; otherwise, the same as in any of examples 15 to 19, are omitted.
Example 22:
a preparation method of a low-climbing high-dyne-value polyurethane protective film is characterized in that a (transparent) PET film layer 5 is subjected to corona treatment; otherwise, the same as in any of examples 15 to 19, are omitted.
In the above examples 15 to 22:
the isocyanate curing agent is one or a mixture of more than two of methyl diisocyanate (TDI for short), isophorone diisocyanate (IPDI for short), diphenylmethane diisocyanate (MDI for short) and hexamethylene diisocyanate (HDI for short);
the temperature-resistant hardening AGENT is one of a temperature-resistant hardening AGENT of Shanghai trades company Limited (namely Nippon lion king) with the trade name of CROSSLINKING AGENT N and a temperature-resistant hardening AGENT of Zhongshan city combined chemical industry company Limited with the trade name of 3053;
the retarder is BPU retarder, BT-180 retarder and any one of acetylacetone of Zhengzhou Yuhe chemical products company Limited or Shanghai Yugji chemical products company Limited of Nanjing Bocksi new materials company Limited;
the organic solvent is one or a mixture of more than two of ethyl acetate, butanone, cyclohexanone, toluene, methyl isobutyl ketone, butyl acetate and methyl ethyl ketone;
the primer solution is any one of waterborne polyurethane, waterborne acrylic resin and waterborne polyester.
In the above examples 15 to 22: the release layer 4 is prepared by coating (or called coating) a silicon-containing release agent on one side (namely one side) of the PET film layer 5 and then drying, the release layer 4 and the PET film layer 5 form a single-side release PET film, and the single-side release PET film can be made by Sichuan Dong material science and technology group, Inc. or can be a commercially available product.
In the above examples 15 to 22: the specific preparation method of the single-sided release PET film can be as follows: coating a silicon-containing release agent layer on one side (namely one side) of the PET film on a coating machine, wherein the coating thickness is one of 0.3-1 mu m, so as to obtain the coated single-side release PET film; running the coated single-sided release PET film at a linear speed of 35m/min, passing through a drying tunnel with the total length of 42m, and sequentially passing through the drying tunnel, wherein the temperature of the first section is 75 ℃, the temperature of the second section is 90 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 110 ℃ and the temperature of the sixth section is 100 ℃ to prepare the single-sided release PET film; the same as the prior art.
The silicon-containing release agent is a commercially available common silicon-containing release agent, and product providing enterprises comprise: dow kangning, Shenzhen, Chu hawk new materials Limited, Fushan Yiyousai new materials Limited.
In the above examples 15 to 22: the thickness of the bottom coating layer 2 is one of 0.1-0.5 μm, and the thickness of the polyurethane adhesive layer 3 is one of 0.5-15 μm.
In the above examples 15 to 22: the PET film layer (PET film) is a polyethylene terephthalate film layer for short, and the thickness of the PET film can be any one of the thicknesses of 10-125 micrometers.
The viscosity of the polyurethane adhesives prepared as described in examples 15-22 above was in the range of 50 to 500cps (25 ℃ C.).
In the above embodiment: the percentages used, not specifically indicated, are percentages by weight or known to those skilled in the art; the proportions used, not specifically noted, are mass (weight) proportions; the parts by mass (by weight) may all be grams or kilograms.
In the above embodiment: the process parameters (temperature, time, pressure, etc.) and the amounts of the components in each step are within the range, and any point can be applicable.
The present invention and the technical contents not specifically described in the above examples are the same as those of the prior art, and the raw materials are all commercially available products.
The present invention is not limited to the above-described embodiments, and both the embodiments described in the summary of the invention and the above-described embodiments can be implemented with the above-described advantageous effects.

Claims (10)

1. A low-climbing high-dyne value polyurethane protective film is characterized in that: the low-climbing high-dyne-value polyurethane protective film is formed by compounding a PET (polyethylene terephthalate) film layer (1), a primer layer (2) coated on one side of the PET film layer (1), a polyurethane adhesive layer (3) coated on the primer layer (2), a release layer (4) coated on one side of the PET film layer (5) and the PET film layer (5) in sequence;
the PET film layer is a polyethylene terephthalate film layer for short;
the base coat (2) is prepared by coating a base coat liquid on one side of the PET film layer (1) and drying, wherein the base coat liquid is any one of waterborne polyurethane, waterborne acrylic resin and waterborne polyester;
the polyurethane adhesive layer (3) is prepared by coating a polyurethane adhesive on the bottom coating (2) and then drying, and the polyurethane adhesive comprises the following raw material components in parts by mass:
40 to 70 parts by mass of a polyurethane prepolymer,
3-15 parts by mass of an isocyanate curing agent, wherein the isocyanate curing agent is one or a mixture of more than two of methyl diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate,
2-8 parts by mass of a temperature-resistant hardening agent,
1 to 5 parts by mass of a retarder,
and 50-100 parts by mass of an organic solvent, wherein the organic solvent is one or a mixture of more than two of ethyl acetate, butanone, cyclohexanone, toluene, methyl isobutyl ketone, butyl acetate and methyl ethyl ketone;
the release layer (4) is prepared by coating a silicon-containing release agent on one side of the PET film layer (5) and drying, and the release layer (4) and the PET film layer (5) form a single-side release PET film.
2. The low climb high dyne polyurethane protective film of claim 1, further comprising: the PET film layer (1) and/or the PET film layer (5) are/is the PET film layer (1) and/or the PET film layer (5) subjected to corona treatment.
3. The low-climb high-dyne polyurethane protective film of claim 1 or 2, characterized in that: the specific preparation method of the single-sided release PET film comprises the following steps: coating a layer of silicon-containing release agent on one side of the PET film on a coating machine, wherein the coating thickness is 0.3-1 mu m, and obtaining the coated single-side release PET film; the coated single-sided release PET film is operated at a linear speed of 35m/min, passes through a drying tunnel with the total length of 42m, and sequentially passes through the drying tunnel, wherein the temperature of the first section is 75 ℃, the temperature of the second section is 90 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 110 ℃ and the temperature of the sixth section is 100 ℃ to prepare the single-sided release PET film.
4. The low-climb high-dyne polyurethane protective film of claim 1 or 2, characterized in that: the thickness of the bottom coating (2) is 0.1-0.5 mu m, and the thickness of the polyurethane adhesive layer (3) is 0.5-15 mu m.
5. The low-climb high-dyne polyurethane protective film of claim 1 or 2, characterized in that: the temperature-resistant hardening AGENT is one of a temperature-resistant hardening AGENT of Shanghai trades Limited with the trademark of CROSSLINKING AGENT N and a temperature-resistant hardening AGENT of Zhongshan City Combined chemical industry Limited with the trademark of 3053;
the retarder is BPU retarder, BT-180 retarder and any one of acetylacetone of Zhengzhou Yuhe chemical products company Limited or Shanghai Yugji chemical products company Limited of Nanjing Pocksi new material company Limited.
6. A preparation method of a low-climbing high-dyne-value polyurethane protective film is characterized by comprising the following steps:
a. preparing a polyurethane adhesive:
taking raw materials of 40-70 parts by mass of polyurethane prepolymer, 3-15 parts by mass of isocyanate curing agent, 2-8 parts by mass of temperature-resistant hardening agent, 1-5 parts by mass of retarder and 50-100 parts by mass of organic solvent at room temperature, and mixing uniformly to obtain the polyurethane adhesive;
the isocyanate curing agent is one or a mixture of more than two of methyl diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate;
the organic solvent is one or a mixture of more than two of ethyl acetate, butanone, cyclohexanone, toluene, methyl isobutyl ketone, butyl acetate and methyl ethyl ketone;
b. preparing a low-climbing high-dyne-value polyurethane protective film:
taking a PET film layer (1), coating a layer of primer solution on one side of the PET film layer (1), and drying at the temperature of 80-120 ℃ for 1-10 minutes to form a primer layer (2);
uniformly coating the polyurethane adhesive prepared in the step a on the bottom coating (2) at the temperature of 20-25 ℃ on a coating machine, wherein the coating thickness is 0.5-15 mu m, and thus obtaining a coated PET film; passing the glued PET film through a drying tunnel with the total length of 24-45 m at a linear speed of 10-35 m/min, wherein the temperature of the first section, the temperature of the second section, the temperature of the third section, the temperature of the fourth section, the temperature of the fifth section and the temperature of the sixth section are respectively 65-85 ℃, 95-110 ℃, 100-130 ℃, 110-130 ℃ and 100-110 ℃ sequentially through the drying tunnel, and thus obtaining the PET film with the polyurethane adhesive layer;
then compounding one surface of a release layer (4) of the single-sided release PET film with one surface of a polyurethane adhesive layer of the PET film with the polyurethane adhesive layer under the conditions that the pressure of a press roller is 0.4-0.5 MPa and the temperature is room temperature (25 ℃), and finally putting the PET film into a drying room at 40-60 ℃ for curing for 24-72 hours to obtain the low-climbing high-dyne value polyurethane protective film;
the PET film layer is a polyethylene terephthalate film layer for short;
the primer solution is any one of waterborne polyurethane, waterborne acrylic resin and waterborne polyester;
the release layer (4) is prepared by coating a silicon-containing release agent on one side of the PET film layer (5) and drying, and the release layer (4) and the PET film layer (5) form a single-side release PET film.
7. The method of making a low-climb high-dyne polyurethane protective film according to claim 6, wherein: the PET film layer (1) and/or the PET film layer (5) are/is the PET film layer (1) and/or the PET film layer (5) subjected to corona treatment.
8. A process for the preparation of a low-climb high-dyne polyurethane protective film according to claim 6 or 7, characterized in that: the specific preparation method of the single-sided release PET film comprises the following steps: coating a layer of silicon-containing release agent on one side of the PET film on a coating machine, wherein the coating thickness is 0.3-1 mu m, and obtaining the coated single-side release PET film; the coated single-sided release PET film is operated at a linear speed of 35m/min, passes through a drying tunnel with the total length of 42m, and sequentially passes through the drying tunnel, wherein the temperature of the first section is 75 ℃, the temperature of the second section is 90 ℃, the temperature of the third section is 100 ℃, the temperature of the fourth section is 110 ℃, the temperature of the fifth section is 110 ℃ and the temperature of the sixth section is 100 ℃ to prepare the single-sided release PET film.
9. A process for the preparation of a low-climb high-dyne polyurethane protective film according to claim 6 or 7, characterized in that: the thickness of the bottom coating (2) is 0.1-0.5 mu m, and the thickness of the polyurethane adhesive layer (3) is 0.5-15 mu m.
10. A process for the preparation of a low-climb high-dyne polyurethane protective film according to claim 6 or 7, characterized in that: the temperature-resistant hardening AGENT in the step a is one of a temperature-resistant hardening AGENT of traded trades, Shanghai, having a trade name of CROSSLINKING AGENT N and a temperature-resistant hardening AGENT of combined chemical industry, Inc., of Zhongshan city, having a trade name of 3053;
the retarder in the step a is BPU retarder, BT-180 retarder and any one of acetylacetone of Zhengzhou Yuhe chemical products company Limited or Shanghai Yuji chemical products company Limited of New Material company of Nanjing Bockss.
CN202110667561.7A 2021-06-16 2021-06-16 Polyurethane protective film with low climbing up factor value and preparation method thereof Active CN113462302B (en)

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