CN109868080B - Novel high-viscosity protective film and preparation method thereof - Google Patents
Novel high-viscosity protective film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of protective film materials, in particular to a novel high-viscosity protective film and a preparation method thereof. In order to solve the problems that the surface layer and the adhesive layer are easy to adhere and not easy to peel off in the unwinding process of the high-viscosity protective film, the invention provides a novel high-viscosity protective film and a preparation method thereof. The high-viscosity protective film sequentially comprises a surface layer, a core layer and a sticky layer, wherein the surface layer comprises 55-80% of an ethylene-propylene block copolymer, 0-30% of high-density polyethylene and 0-20% of release resin, and the total amount of the high-density polyethylene and the release resin is 20-45%. The protective film has the advantages of high adhesion, good attaching effect, small change of the adhesion with temperature and time, easy stripping, no adhesive residue and easy uncoiling, and is suitable for being used as an optical material surface protective film with high viscosity requirement.
Description
Technical Field
The invention relates to the field of protective film materials, in particular to a novel high-viscosity protective film and a preparation method thereof.
Background
In recent years, with the rapid development of the electronics industry, there has been an increasing demand for ultra-thin displays such as liquid crystal displays. The liquid crystal display is mainly formed by combining various optical films. To protect the optical film from dirt or scratches during handling and assembly, the surface needs to be protected. The protective film is formed by integrating the surface layer, the core layer and the adhesive layer, and can be usually wound into a roll shape, particularly for a high-viscosity protective film, under a larger winding pressure, the surface layer and the adhesive layer are closely attached, and tackifying components in the adhesive layer are easy to migrate to the surface layer, so that the problems of difficult unwinding, insufficient adhesive force of the adhesive layer and the like are caused. Particularly, after the optical film product is subjected to a high-temperature storage test, the peeling force is increased remarkably, and offset printing is left on the surface of the object to be pasted after peeling, which affects the final use.
Disclosure of Invention
In order to solve the problems that the surface layer and the adhesive layer are easy to adhere and not easy to peel off in the unwinding process of the high-viscosity protective film, the invention provides a novel high-viscosity protective film and a preparation method thereof. The high-viscosity protective film has low uncoiling force, namely the force required by uncoiling the protective film is low, and the surface layer can not pollute the adhesive layer and influence the adhesive force. Moreover, the high-viscosity protective film has high adhesion, good attaching effect, small influence of the adhesion along with the change of temperature and time, no adhesive residue, easy stripping and easy uncoiling, and is suitable for being used as the surface protective film of the optical material with high viscosity requirement.
In order to solve the technical problems, the invention adopts the following technical scheme.
The invention provides a novel high-viscosity protective film which sequentially comprises a surface layer, a core layer and a viscous layer, wherein the surface layer comprises 55-80% of an ethylene-propylene block copolymer, 0-30% of high-density polyethylene and 0-20% of release resin, and the percentage is weight percentage (also called weight percentage). The total amount of the high-density polyethylene and the release resin is 20-45%.
Further, the ethylene-propylene block copolymer of the skin layer has a density of 0.90 to 0.91g/cm3And the melt index is between 4.0 and 9.0g/10 min.
Further, the surface layer comprises 55-72% of ethylene-propylene block copolymer, 25-30% of high-density polyethylene and 3-15% of release resin, wherein the percentage is weight percentage. The total amount of the high-density polyethylene and the release resin is 28-45%. The ethylene-propylene block copolymer of the skin layer had a density of 0.90g/cm3The melt index was 4.0g/10 min. The foregoing technical solutions include examples 4 to 5, and example 9.
Further, the density of the high-density polyethylene resin in the surface layer is 0.945 to 0.963g/cm3And the melt index is between 4.0 and 9.0g/10 min.
Further, the release resin in the surface layer is a vinyl polymer chemically modified by styrene.
In the novel high-viscosity protective film, the core layer is selected from polypropylene resin, and the polypropylene resin is an ethylene-propylene block copolymer.
Further, the core layer is an ethylene-propylene block copolymer having a density of 0.91g/cm3The melt index was 4.0g/10 min.
Furthermore, in the novel high-viscosity protective film, the adhesive layer is an acrylic block copolymer, and the density of the adhesive layer is 1.08-1.13g/cm3And the melt index is between 1.2 and 3.5g/10 min.
The acrylic block copolymer of the adhesive layer is methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer. Polymethyl methacrylate is used as a hardness section, and polybutyl acrylate is used as a soft section.
Furthermore, in the novel high-viscosity protective film, the thickness of the surface layer is 8-10 μm, the thickness of the core layer is 28-32 μm, and the thickness of the adhesive layer is 8-10 μm.
The preparation method of the novel high-viscosity protective film comprises the following steps: the material is prepared in a three-layer coextrusion casting mode.
The adhesive layer formula of the invention adopts acrylic block copolymer, polymethyl methacrylate is used as a hardness segment, and polybutyl acrylate is used as a soft segment, compared with the prior general polystyrene block copolymer elastomer, the soft segment has lower Tg, is softer, and can provide better adhesion effect and permanent adhesion. When the polystyrene blend elastomer is used as an adhesive layer, tackifying components such as petroleum resin, terpene resin and the like are often required to be added to improve the adhesive force, and when the addition ratio is too high, the adhesive force is greatly changed along with the temperature and the time, and residual glue is easily left on the surface of an adherend to cause pollution. The acrylic block copolymer adhesive layer scheme provided by the invention can meet the requirement of the surface structure of the optical film on high viscosity by directly using the acrylic block copolymer adhesive layer scheme without compounding with other tackifying components. And the problems of adhesive layer precipitation and difficult uncoiling do not exist.
Compared with the prior art, the novel high-viscosity protective film provided by the invention has low uncoiling force, and the surface layer cannot pollute the adhesive layer and influence the adhesive force. Moreover, the high-viscosity protective film has high adhesion, good attaching effect, no adhesive residue, easy stripping and small influence of the adhesive force along with the change of temperature and time.
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) tensile Strength and elongation at Break test
An American Instron universal tester is used, the reference standard being GB/T1040.3.
(2) Unwind force, peel force test
The Kejian tensile tester is adopted, and the reference standard is GB/T2792.
And (3) unwinding force test: two 25mm wide film samples 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.
And (3) testing the peeling force: a25 mm wide sample of the film was applied to a PMMA plate and the applied film was then rolled at 300mm/min using a 2kg FINAT standard roller. The film was peeled off the PMMA plate for a period and then tested according to the 180 ° peel strength test method, and the average value was recorded as the peel force.
(3) Residual gum test
Attaching a protective film on the optical film, then pressing the optical film by using a film laminating machine, placing the optical film in a 50 ℃ oven for 3d, taking out the protective film, tearing the protective film, observing the residual glue on the optical film under light, wherein no residual glue is marked as 'O', slight residual glue is marked as 'Delta', and serious residual glue is marked as 'X'. The test indicates whether the surface of the adherend is contaminated with the protective film. No residual glue is excellent, slight residual glue is good, and serious residual glue is unqualified.
Example 1
The novel high-viscosity protective film provided by the invention sequentially comprises a surface layer, a core layer and a viscous layer.
The surface layer adopts an ethylene-propylene block copolymer and a release resin, wherein the weight ratio of the ethylene-propylene block copolymer to the release resin is 80%: 20 percent of the components are compounded. The density of the ethylene-propylene block copolymer was 0.90g/cm3The melt index was 9.0g/10 min. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The core layer adopts 100 weight percent of ethylene-propylene block copolymer and has the density of 0.90g/cm3The melt index was 5.0g/10 min.
The adhesive layer adopts a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer with the density of 1.13g/cm3The melt index was 1.2g/10 min.
The surface layer has a thickness of 10 μm, the core layer has a thickness of 30 μm, and the adhesive layer has a thickness of 10 μm.
Example 2
The novel high-viscosity protective film as provided in example 1, except that:
the surface layer adopts an ethylene-propylene block copolymer and high-density polyethylene, and the weight ratio of the ethylene-propylene block copolymer to the high-density polyethylene is 80%: 20 percent of the components are compounded. The density of the ethylene-propylene block copolymer was 0.90g/cm3The melt index was 9.0g/10 min. The high density polyethylene has a density of 0.945g/cm3。
Example 3
The novel high-viscosity protective film as provided in example 1, except that:
the surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed by 80 percent: 10%: 10 percent of the components are compounded. The density of the ethylene-propylene block copolymer was 0.91g/cm3The melt index was 4.0g/10 min. The density of the high density polyethylene is 0.963g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The adhesive layer adopts methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer. The density of the powder was 1.11g/cm3The melt index was 1.5g/10 min.
Example 4
The novel high-viscosity protective film as provided in example 1, except that:
the surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed by 72 percent: 25%: 3 percent of the components are compounded. The density of the ethylene-propylene block copolymer was 0.91g/cm3The melt index was 4.0g/10 min. The density of the high density polyethylene is 0.963g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The adhesive layer adopts a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer with the density of 1.08g/cm3The melt index was 3.5g/10 min.
Example 5
The novel high-viscosity protective film as provided in example 1, except that:
the surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed in a ratio of 67%: 28 percent to 5 percent. The density of the ethylene-propylene block copolymer was 0.91g/cm3The melt index was 4.0g/10 min. The high density polyethylene has a density of 0.945g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The adhesive layer adopts a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer with the density of 1.08g/cm3The melt index was 3.5g/10 min.
Example 6
The novel high-viscosity protective film as provided in example 1, except that:
the surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed in a proportion of 65%: 27 percent to 8 percent. The density of the ethylene-propylene block copolymer was 0.90g/cm3The melt index was 9.0g/10 min. Density of high density polyethyleneIs 0.963g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The adhesive layer adopts a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer with the density of 1.11g/cm3The melt index was 1.5g/10 min.
Example 7
The novel high-viscosity protective film as provided in example 1, except that:
the surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed by 60 percent: 28 percent to 12 percent. The density of the ethylene-propylene block copolymer was 0.90g/cm3The melt index was 9.0g/10 min. The high density polyethylene has a density of 0.945g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The adhesive layer adopts a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer with the density of 1.13g/cm3The melt index was 1.2g/10 min.
Example 8
The novel high-viscosity protective film as provided in example 1, except that:
the surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed by 60 percent: 22%: 18 percent of the components are compounded. The density of the ethylene-propylene block copolymer was 0.90g/cm3The melt index was 9.0g/10 min. The density of the high density polyethylene is 0.963g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The adhesive layer adopts a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer with the density of 1.11g/cm3The melt index was 1.5g/10 min.
Example 9
The novel high-viscosity protective film as provided in example 1, except that:
the surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed by 55 percent: 30%: 15 percent of the components are compounded. The density of the ethylene-propylene block copolymer was 0.91g/cm3The melt index was 4.0g/10 min. The high density polyethylene has a density of 0.945g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The adhesive layer adopts a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer with the density of 1.08g/cm3The melt index was 3.5g/10 min.
Comparative example 1
The surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed in a ratio of 75%: 15%: 10 percent of the components are compounded. The density of the ethylene-propylene block copolymer was 0.91g/cm3The melt index was 4.0g/10 min. The high density polyethylene has a density of 0.945g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The core layer adopts 100 weight percent of ethylene-propylene block copolymer and has the density of 0.90g/cm3The melt index was 5.0g/10 min.
The adhesive layer adopts high-viscosity SEBS thermoplastic elastomer with the density of 0.95g/cm3The melt index was 14.5g/10 min.
Comparative example 2
The surface layer adopts ethylene-propylene block copolymer, and the high-density polyethylene and the release resin are mixed in a ratio of 75%: 15%: 10 percent of the components are compounded. The density of the ethylene-propylene block copolymer was 0.90g/cm3The melt index was 9.0g/10 min. The density of the high density polyethylene is 0.963g/cm3. The release resin is vinyl polymer chemically modified by styrene (produced by Mitsubishi chemical, brand number W200P).
The core layer adopts 100 weight percent of ethylene-propylene block copolymer and has the density of 0.90g/cm3The melt index was 5.0g/10 min.
The adhesive layer adopts highA viscous SEBS thermoplastic elastomer with the density of 0.94g/cm3The melt index was 4.8g/10 min.
Comparative example 3
The surface layer adopts 100 weight percent of ethylene-propylene block copolymer with the density of 0.90g/cm3The melt index was 9.0g/10 min.
The core layer adopts 100 weight percent of ethylene-propylene block copolymer and has the density of 0.90g/cm3The melt index was 5.0g/10 min.
The adhesive layer adopts a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer with the density of 1.08g/cm3The melt index was 3.5g/10 min.
The formula of the surface layer of the prepared protective film is shown in table 1, the main performance test results are shown in table 2, and the residual adhesive test results are shown in table 3.
Table 1 formulations of skin layers of protective films provided in examples 1 to 9 of the present invention and comparative examples 1 to 3
Table 2 main performance test results of the protective films provided in examples 1 to 9 of the present invention and comparative examples 1 to 3
Table 3 residual adhesive test results of protective films provided in examples 1 to 9 of the present invention and comparative examples 1 to 3
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| ○ | ○ | △ | ○ | ○ | △ |
| Example 7 | Example 8 | Example 9 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| ○ | △ | ○ | × | × | ○ |
By comparing the comparative examples with the examples, it can be seen from the test results that the adhesive layer scheme of the acrylic block copolymer provided by the invention has better adhesive force stability on PMMA plates and has smaller change with temperature and time. The protective films provided in examples 4, 5 and 9 have better comprehensive performance: the adhesive force is higher, close to or even higher than that of the high-viscosity SEBS, the unwinding force is lower, and the problems of adhesive residue and the like do not exist. As can be seen from comparative example 3, the invention also provides a scheme for high viscosity and low unwinding, and the lower unwinding force can be realized by optimizing each component of the surface layer.
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 (3)
1. The novel high-viscosity protective film is characterized by comprising a surface layer, a core layer and a viscous layer in sequence, wherein the surface layer comprises the following components: 55-72% of ethylene-propylene block copolymer, 25-30% of high-density polyethylene and 3-15% of release resin, wherein the percentages are weight percentages; the ethylene-propylene block copolymer of the skin layer had a density of 0.91g/cm3The melt index is 4.0g/10 min; the core layer is an ethylene-propylene block copolymer; the adhesive layer is a methyl methacrylate-butyl acrylate-methyl methacrylate block copolymer.
2. The novel high-viscosity protective film according to claim 1, wherein the density of the high-density polyethylene resin in the surface layer is 0.945 to 0.963g/cm3And the melt index is between 4.0 and 9.0g/10 min.
3. The method for preparing the novel high-viscosity protective film according to claim 1 or 2, wherein the high-viscosity protective film is prepared by three-layer co-extrusion casting.
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