CN111440555A - High-temperature-resistant and easy-to-peel CPP protective film and preparation method thereof - Google Patents
High-temperature-resistant and easy-to-peel CPP protective film and preparation method thereof Download PDFInfo
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- CN111440555A CN111440555A CN201910734129.8A CN201910734129A CN111440555A CN 111440555 A CN111440555 A CN 111440555A CN 201910734129 A CN201910734129 A CN 201910734129A CN 111440555 A CN111440555 A CN 111440555A
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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
- C09J7/29—Laminated material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08J2423/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
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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
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- C09J2423/00—Presence of polyolefin
- C09J2423/04—Presence of homo or copolymers of ethene
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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
- C09J2423/00—Presence of polyolefin
- C09J2423/10—Presence of homo or copolymers of propene
- C09J2423/106—Presence of homo or copolymers of propene in the substrate
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Abstract
The invention relates to the field of protective film materials, in particular to a high-temperature-resistant and easily-stripped CPP protective film and a preparation method thereof. The invention provides a high-temperature-resistant and easily-stripped CPP protective film and a preparation method thereof, aiming at solving the problems that the protective film cannot bulge or wrinkle in a high-temperature process environment, and the protective film cannot have the problems of white fog, adhesive residue, difficult stripping and the like after being torn. The protective film sequentially comprises a surface layer, a core layer and an adhesive layer; the surface layer is composed of homopolymerized polypropylene, polyolefin resin and heat-resistant inorganic filler, the core layer is made of polypropylene resin, and the adhesive layer is made of metallocene polyolefin elastomer. The protective film not only has high temperature resistance, but also has no problems of white fog, adhesive residue, difficult peeling and the like after being baked and torn at high temperature, and is suitable for various high temperature resistant protection processes.
Description
Technical Field
The invention relates to the field of protective film materials, in particular to a high-temperature-resistant and easily-stripped CPP protective film and a preparation method thereof.
Background
In recent years, with the rapid development of flexible screen O L ED technology, the demand for ultra-thin displays such as liquid crystal displays is increasing, so that ITO thin films are widely used.
The common high-temperature resistant protective film in the market at present is a glue coating film, glue is generally coated on a polyester film, and residual glue can be left on the surface of an ITO film after the protective film is baked at high temperature to influence the product performance. After the conventional self-adhesive protective film is baked at a high temperature of 150 ℃, the problems of warping, white fog, adhesive residue, difficult peeling and the like can occur, and the performance of a final product is seriously influenced.
Disclosure of Invention
The invention provides a high-temperature-resistant and easily-stripped CPP protective film and a preparation method thereof, aiming at solving the problem that the existing protective film is not easy to strip in a high-temperature process environment.
Furthermore, the invention provides a high-temperature-resistant and easily-stripped CPP protective film, which aims to solve the problems that the existing protective film can bulge and wrinkle in a high-temperature process environment, and white fog, adhesive residue, difficult stripping and the like can also occur after tearing. The protective film has high temperature resistance, does not bulge or wrinkle in a high-temperature process environment, does not have the problems of white fog, adhesive residue, difficult peeling and the like after being baked and torn at high temperature, and is suitable for various high-temperature resistant protection processes.
In order to solve the technical problems, the invention adopts the following technical scheme.
The invention provides a high-temperature-resistant and easily-stripped CPP protective film which sequentially comprises a surface layer, a core layer and an adhesive layer, wherein the surface layer comprises homopolymerized polypropylene, polyolefin resin and heat-resistant inorganic filler, the core layer is selected from polypropylene resin, and the adhesive layer is selected from metallocene polyolefin elastomer.
In general, the surface layer and the adhesive layer of the existing protective film are not high-temperature resistant, and the problems of easy wrinkling, adhesive residue, serious viscosity increase, difficult peeling and the like occur after high temperature, and the invention mainly solves the problems by selecting high-temperature resistant materials with higher crystallinity or higher melting point.
The CPP protective film is a casting polypropylene protective film.
Further, the surface layer is composed of homo-polypropylene, polyolefin resin and heat-resistant inorganic filler.
Further, the density of the homopolymerized polypropylene in the surface layer is 0.90-0.91g/cm3And the melt index is between 3.0 and 8.0g/10 min.
The homo-polypropylene (PP) and the common copolymerized PP have no great difference in density and melt index indexes, mainly in structure, and the homo-PP has higher crystallinity, higher melting point and higher rigidity.
Further, the polyolefin resin in the skin layer is selected from 4-methylpentene polymers, the density of the 4-methylpentene polymers being 0.83-0.85g/cm3The melt index is between 21 and 27g/10 min.
Further, the polyolefin resin is a highly crystalline polyolefin resin. The highly crystalline polyolefin resin is a transparent crystalline resin, and has a high modulus and a high crystallinity.
Further, the heat-resistant inorganic filler in the surface layer is selected from hydrophilic fumed silica having an average particle diameter of 7 to 12 nm.
Furthermore, the surface layer consists of 80-90% of homopolymerized polypropylene, 8-19% of 4-methylpentene polymer and 1-3% of hydrophilic fumed silica. The percentages are weight percentages (also referred to as weight percentages).
Furthermore, the core layer of the high-temperature-resistant and easily-stripped CPP protective film is polypropylene resin.
Further, the polypropylene resin of the core layer is selected from homo-polypropylene, and the density of the polypropylene resin is 0.90-0.91g/cm3In between, the melt index is between 3.0 and 8.0g/10 min.
Furthermore, the high-temperature-resistant and easily-stripped CPP protective film is characterized in that the adhesive layer is a metallocene polyolefin elastomer.
Further, the metallocene polyolefin elastomer is selected from ethylene-octene copolymers. Further, the density of the ethylene-octene copolymer is 0.86-0.88g/cm3And the melt index is between 4.0 and 6.0g/10 min.
The innovation point of the invention is mainly the formula of the surface layer and the adhesive layer of the protective film, the surface layer improves the heat resistance of the material by adding high-crystalline polymer and heat-resistant inorganic filler, and the adhesive layer improves the heat resistance of the material by selecting high-melting-point metallocene polyolefin elastomer.
Furthermore, the high-temperature-resistant and easily-stripped CPP protective film has the surface layer thickness of 5-8 microns, the core layer thickness of 20-28 microns and the adhesive layer thickness of 5-8 microns.
Furthermore, in the surface layer of the high-temperature-resistant and easily-stripped CPP protective film, the content of homo-polypropylene is 80-85%, the content of 4-methylpentene polymer is 13-17%, and the content of hydrophilic fumed silica is 2-3%. The foregoing technical solutions include examples 4 to 6.
Furthermore, the high-temperature-resistant and easily-stripped CPP protective film has the surface layer thickness of 6 microns, the core layer thickness of 24 microns and the adhesive layer thickness of 5 microns.
The invention also provides a preparation method of the high-temperature-resistant and easy-to-peel CPP protective film, and the high-temperature-resistant and easy-to-peel CPP protective film is prepared in a three-layer co-extrusion casting mode.
Compared with the prior art, the high-temperature-resistant and easily-stripped CPP protective film has the beneficial effects that the combination method of adding the high-crystalline polyolefin and the heat-resistant inorganic filler into the surface layer of the high-temperature-resistant and easily-stripped CPP protective film improves the heat resistance of the surface layer of the material, and simultaneously can effectively reduce the uncoiling force required by the protective film after high temperature, the viscosity of the metallocene elastomer in the adhesive layer is slightly changed along with the temperature, the problems of white fog, adhesive residue, difficult stripping and the like can not occur after the surface of an adherend is torn, and the high-temperature-resistant and easily-stripped CP.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to these examples.
The performance test method for the protective film is as follows:
(1) unwind force test
The Kejian tensile tester is adopted, and the reference standard is GB/T2792.
The unwinding force refers to the force when the surface layer of the protective film is separated from the adhesive layer. Two 25mm wide samples of protective film were laminated together and attached to a standard steel plate, and the attached film was then rolled at 300mm/min using a 2kg FINAT standard roller. The upper film was peeled off a section from the lower film and then tested according to the 180 ° peel strength test method, and the maximum value was recorded as the unwinding force. The unwinding force is not particularly limited, and generally, the lower the unwinding force, the more preferable the unwinding force is, the more easily the peeling is performed, and the less likely the unwinding force remains.
(2) Initial peel force test
A25 mm wide sample of protective film was applied to the ITO film, and the applied film was then rolled at 300mm/min using a 2kg FINAT standard roller. The film was peeled off a section from the ITO film and then tested according to the 180 ° peel strength test method, and the average value was recorded as the initial peel force. The results of measurement are shown in column 3 of Table 2 (ITO film peeling force (initial peeling force), gf/25 mm).
(3) High temperature peel force
And (3) placing the ITO film adhered with the protective film in a 90 ℃ oven for 1h, and then testing the stripping force of the protective film and the ITO film. See column 4 in Table 2 (last column: ITO film peeling force, 90 ℃, 1h, unit gf/25mm), mainly embodying the heat resistance stability of the protective film adhesive layer material. The smaller the difference between the high-temperature peel force and the initial peel force, the smaller the influence of the temperature on the peel force, and the better the heat resistance stability of the adhesive layer material. If the adhesive layer material has poor heat resistance, small molecules are likely to be precipitated and adhere to the surface of the adherend. Poor heat resistance of the adhesive layer material causes the peel force to climb significantly.
(4) High temperature peel surface dyne value test
The ITO film adhered with the protective film is placed in a 90 ℃ oven for 1h, changes of dyne values on the surface of the ITO film before and after baking are compared, an Arcotest dyne pen is used for testing (manufactured by Germany), in order to ensure accurate test data, at least 3 dyne pens of different models are ensured, and the dyne value on the surface of the film is determined by drawing a line on the surface of the film for 3 seconds by using the current numerical value dyne pen without shrinkage. The lower the dyne variation rate (difference between after baking and before baking/dyne before baking), the better the high temperature resistance of the protective film and the better the deposition (the less deposition, the less residue (residual gum) on the surface of the adherend, and the less the subsequent use will be affected).
(5) The protective film is raised and wrinkled,
the high temperature resistance of the surface layer of the protective film is mainly to see whether the poor appearance such as wrinkling appears after a high temperature test.
The protective film-attached ITO film was placed in an oven at 90 ℃ for 1h, and then confirmed by visual observation.
(6) White fog
And (3) placing the ITO film adhered with the protective film in a 90 ℃ oven for 1h, stripping the protective film, and then observing the surface of the ITO film by eyes.
(7) Residual glue
The lower the dyne change rate, the less the residual gum condition.
Example 1
The high-temperature-resistant and easy-to-peel CPP protective film provided by the invention sequentially comprises a surface layer, a core layer and an adhesive layer.
The surface layer comprises 90 percent of homopolymerized polypropylene, 9 percent of polyolefin resin and 1 percent of inorganic heat-resistant filler. The density of the homo-polypropylene is 0.90g/cm3The melt index was 8.0g/10 min. The polyolefin resin was a 4-methylpentene polymer having a density of 0.83g/cm3The melt index was 21.0g/10 min.
The core layer adopts 100 weight percent of homopolymerized polypropylene and has the density of 0.90g/cm3The melt index was 8.0g/10 min.
The adhesive layer adopts metallocene polyolefin elastomer, and the metallocene polyolefin elastomer isEthylene-octene copolymer having a density of 0.86g/cm3The melt index was 6.0g/10 min.
The surface layer has a thickness of 6 μm, the core layer has a thickness of 24 μm, and the adhesive layer has a thickness of 5 μm.
Example 2
The high temperature resistant easy-to-peel CPP protective film as provided in example 1, except that:
the surface layer comprises 90% of homo-polypropylene, 8% of polyolefin resin and 2% of heat-resistant inorganic filler.
Example 3
The high temperature resistant easy-to-peel CPP protective film as provided in example 1, except that:
the surface layer comprises 87 percent of homopolymerized polypropylene, 10 percent of polyolefin resin and 3 percent of heat-resistant inorganic filler. The density of the homo-polypropylene is 0.91g/cm3The melt index was 3.0g/10 min. The polyolefin resin was a 4-methylpentene polymer having a density of 0.85g/cm3The melt index was 27.0g/10 min.
Example 4
The high temperature resistant easy-to-peel CPP protective film as provided in example 1, except that:
the surface layer comprises 85% of homopolymerized polypropylene, 13% of polyolefin resin and 2% of heat-resistant inorganic filler. The density of the homo-polypropylene is 0.91g/cm3The melt index was 3.0g/10 min. The polyolefin resin was a 4-methylpentene polymer having a density of 0.85g/cm3The melt index was 27.0g/10 min.
The adhesive layer adopts metallocene polyolefin elastomer, the metallocene polyolefin elastomer is ethylene-octene copolymer, and the density of the metallocene polyolefin elastomer is 0.88g/cm3The melt index was 4.0g/10 min.
Example 5
The high temperature resistant easy-to-peel CPP protective film as provided in example 1, except that:
the surface layer comprises 83 percent of homopolymerized polypropylene, 15 percent of polyolefin resin and 2 percent of heat-resistant inorganic filler. The density of the homo-polypropylene is 0.91g/cm3The melt index was 3.0g/10 min. The polyolefin resin was a 4-methylpentene polymer having a density of 0.85g/cm3The melt index was 27.0g/10 min.
The adhesive layer adopts metallocene polyolefin elastomer, the metallocene polyolefin elastomer is ethylene-octene copolymer, and the density of the metallocene polyolefin elastomer is 0.88g/cm3The melt index was 4.0g/10 min.
Example 6
The high temperature resistant easy-to-peel CPP protective film as provided in example 1, except that:
the surface layer comprises 80% of homo-polypropylene, 17% of polyolefin resin and 3% of heat-resistant inorganic filler. The density of the homo-polypropylene is 0.91g/cm3The melt index was 3.0g/10 min. The polyolefin resin was a 4-methylpentene polymer having a density of 0.84g/cm3The melt index was 24.0g/10 min.
The adhesive layer adopts metallocene polyolefin elastomer, the metallocene polyolefin elastomer is ethylene-octene copolymer, and the density of the metallocene polyolefin elastomer is 0.88g/cm3The melt index was 4.0g/10 min.
Example 7
The high temperature resistant easy-to-peel CPP protective film as provided in example 1, except that:
the surface layer comprises 80% of homopolymerized polypropylene, 19% of polyolefin resin and 1% of heat-resistant inorganic filler. The polyolefin resin was a 4-methylpentene polymer having a density of 0.84g/cm3The melt index was 24.0g/10 min. .
Comparative example 1
The difference from example 1 is that: the surface layer adopts homopolymerized polypropylene with the density of 0.9g/cm3The melt index was 8.0g/10 min.
The formulations of the surface layers of the protective films obtained in examples 1 to 7 and comparative example 1 are shown in table 1, and the unwinding force and peeling force test results are shown in table 2.
Table 1 formulations of skin layers of protective films provided in examples 1 to 7 of the present invention and comparative example 1
Table 2 unwind force, peel force test results for protective films provided in inventive examples 1-7 and comparative example 1
TABLE 3 dyne values before and after baking, swelling and white fogging phenomena of inventive examples 1-7 and comparative example 1
By comparing the comparative examples with the examples, it can be seen from the test results that the skin ply solutions provided by examples 4, 5, 6 of the present invention exhibit better unwind force and peel force levels and less variation in peel force at high temperatures. Among them, examples 4, 5 and 6 had a high-temperature peel force of not more than 12gf/25mm, and the surface dyne values before and after baking were also slightly changed. After optimization is performed on the aspects of comprehensive properties of materials and the like, the comprehensive properties of the embodiments 4, 5 and 6 are optimal, and the method is more suitable for various high-temperature-resistant protection processes.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. The high-temperature-resistant and easy-to-peel CPP protective film is characterized by sequentially comprising a surface layer, a core layer and an adhesive layer, wherein the surface layer comprises homopolymerized polypropylene, polyolefin resin and heat-resistant inorganic filler, the core layer is selected from polypropylene resin, and the adhesive layer is selected from polyolefin elastomers.
2. The high temperature resistant easy-peel CPP protective film according to claim 1, wherein the surface layer is composed of homo polypropylene, polyolefin resin, and heat-resistant inorganic filler.
3. The high temperature resistant easy-peeling CPP protective film according to claim 2, wherein the melt index of the homo-polypropylene in the surface layer is between 3.0g/10min and 8.0g/10 min.
4. The protective film according to claim 2, wherein the polyolefin resin in the surface layer is selected from 4-methylpentene polymer, and the density of the 4-methylpentene polymer is 0.83-0.85g/cm3The melt index is 21-27g/10 min.
5. The high temperature resistant, easy-to-peel CPP protective film according to claim 2, wherein the heat resistant inorganic filler in the surface layer is selected from hydrophilic fumed silica.
6. The high temperature resistant and easy-to-peel CPP protective film according to claim 5, wherein in the surface layer, the content of homo-polypropylene is 80% -90%, the content of 4-methylpentene polymer is 8% -19%, and the content of hydrophilic fumed silica is 1-3%.
7. The high temperature resistant easy-peeling CPP protective film according to claim 1, wherein the core layer is selected from homo polypropylene, and the melt index is 3.0-8.0g/10 min.
8. The protective film according to claim 1, wherein the adhesive layer is selected from metallocene polyolefin elastomers with a melt index of 4.0-6.0g/10 min.
9. The high temperature resistant and easy-to-peel CPP protective film according to claim 5, wherein in the surface layer, the content of homo-polypropylene is 80% -85%, the content of 4-methylpentene polymer is 13% -17%, and the content of hydrophilic fumed silica is 2-3%.
10. The preparation method of the high-temperature-resistant and easy-to-peel CPP protective film according to claim 1, characterized in that the high-temperature-resistant and easy-to-peel CPP protective film is prepared in a three-layer co-extrusion casting manner.
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| CN112760053A (en) * | 2020-12-16 | 2021-05-07 | 苏州绍荣光学科技有限公司 | Preparation process of CPP (chlorinated Polypropylene) protective film for conductive film |
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