CN114507486B - High-temperature-resistant protective film and preparation method thereof - Google Patents
High-temperature-resistant protective film and preparation method thereof Download PDFInfo
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- CN114507486B CN114507486B CN202011277267.7A CN202011277267A CN114507486B CN 114507486 B CN114507486 B CN 114507486B CN 202011277267 A CN202011277267 A CN 202011277267A CN 114507486 B CN114507486 B CN 114507486B
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- 230000001681 protective effect Effects 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000004743 Polypropylene Substances 0.000 claims abstract description 56
- -1 polypropylene Polymers 0.000 claims abstract description 55
- 229920001155 polypropylene Polymers 0.000 claims abstract description 55
- 239000012790 adhesive layer Substances 0.000 claims abstract description 40
- 229920005629 polypropylene homopolymer Polymers 0.000 claims abstract description 24
- 239000002344 surface layer Substances 0.000 claims abstract description 18
- 239000012792 core layer Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- JMMZCWZIJXAGKW-UHFFFAOYSA-N 2-methylpent-2-ene Chemical compound CCC=C(C)C JMMZCWZIJXAGKW-UHFFFAOYSA-N 0.000 claims description 29
- 239000000155 melt Substances 0.000 claims description 28
- 229920000642 polymer Polymers 0.000 claims description 28
- 229920001971 elastomer Polymers 0.000 claims description 25
- 239000000806 elastomer Substances 0.000 claims description 25
- 239000010410 layer Substances 0.000 claims description 10
- 229920001577 copolymer Polymers 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims 2
- 238000002844 melting Methods 0.000 abstract description 15
- 230000008018 melting Effects 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- 229920006038 crystalline resin Polymers 0.000 abstract description 5
- 239000003292 glue Substances 0.000 abstract description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 8
- 239000004926 polymethyl methacrylate Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000009472 formulation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002313 adhesive film Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920006124 polyolefin elastomer Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
Classifications
-
- 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
-
- 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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/10—Homopolymers or copolymers of propene
- C09J123/12—Polypropene
-
- 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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
-
- 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
- C09J2423/00—Presence of polyolefin
- C09J2423/006—Presence of polyolefin in the substrate
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention relates to the field of protective film materials, in particular to a high-temperature-resistant protective film and a preparation method thereof. The invention provides a high-temperature-resistant protective film and a preparation method thereof, aiming at solving the problems that the protective film can warp, white fog and melt edges in a high-temperature process environment, and the problems that residual glue can occur after tearing and stripping is difficult. The protective film sequentially comprises a surface layer, a core layer and an adhesive layer; the surface layer is composed of homo-polypropylene and high-crystalline resin, the core layer is polypropylene resin, and the adhesive layer is polypropylene mixture. The protective film not only has high temperature resistance, but also has no problems of warping, edge melting 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 protective film and a preparation method thereof.
Background
In recent years, with the increasing market demands of protective films, the requirements on the functions of the protective films are higher and higher, and particularly, the protective films are required to have better high-temperature resistance characteristics in the process of manufacturing electronic elements such as ITO, TP and the like, so that the surfaces of products can be better protected.
The common high temperature resistant protective film in the market at present is a coated film, but the common self-adhesive film does not have high temperature resistant property, and after the protective film is baked at a high temperature of 150 ℃, the protective film can have various problems such as warping, white fog, edge melting and the like, so that the performance of a final product is seriously influenced.
Disclosure of Invention
The invention provides a high-temperature-resistant protective film and a preparation method thereof, aiming at solving the problems that the existing protective film is warped, white fog and even molten edges in a high-temperature process. The protective film has good high temperature resistance, and no warpage, white fog and edge melting occur in a high temperature process environment.
Furthermore, in order to solve the problems that the existing protective film can generate warpage, white fog, edge melting and the like in a high-temperature process environment, the invention provides the high-temperature resistant protective film, which has good high-temperature resistance, can not generate warpage, white fog and edge melting in the high-temperature process environment, can not generate residual glue after being baked and torn at high temperature and the like, and is suitable for various process technologies with high-temperature resistant requirements.
In order to solve the technical problems, the invention adopts the following technical scheme.
The invention provides a high-temperature-resistant protective film which sequentially comprises a surface layer, a core layer and an adhesive layer, wherein the surface layer comprises homo-polypropylene and high-crystalline resin, the core layer is selected from polypropylene resin, and the adhesive layer is a polypropylene mixture.
In general, the existing protective film is not resistant to high temperature, particularly the melting point of the adhesive layer resin material is low, the adhesive layer resin material can be melted after high temperature, and the adhesive layer resin material is left on the surface of a stuck object after cooling and is not easy to peel. The invention solves the problems by mainly selecting a high-temperature resistant material with higher crystallinity or higher melting point as an adhesive layer.
Further, the surface layer is composed of homo-polypropylene and high crystalline resin.
Further, the density of the homo-polypropylene in the surface layer is 0.90-0.91g/cm 3 The melt index is between 3.0 and 8.0g/10min.
The crystallinity of the homo-polypropylene (PP) is higher, the rigidity is better, and compared with the random copolymer polypropylene, the melting point is higher, and the heat resistance is better.
Further, the high crystalline resin in the skin layer is selected from methylpentene polymers having a density of 0.85-0.87g/cm 3 The melt index is between 21 and 27g/10 min.
Furthermore, the methylpentene polymer is transparent crystalline resin, has higher modulus and higher crystallinity, and has better heat resistance when the melting point is above 240 ℃.
Further, the surface layer is composed of 80% -90% of homopolypropylene and 10% -20% of methylpentene polymer. The percentage content is weight percentage content.
Furthermore, the high temperature resistant protective film is characterized in that the core layer is made of polypropylene resin.
Further, the polypropylene resin of the core layer is selected from homo-polypropylene having a density of 0.90-0.91g/cm 3 Between them, the melt index is between 3.0 and 8.0g/10min.
Furthermore, the high temperature resistant protective film and the adhesive layer are polypropylene mixture.
Further, the polypropylene mixture of the adhesive layer is a mixture composed of 0% -15% of polypropylene elastomer and 85% -100% of polypropylene and methylpentene copolymer. The percentages are weight percentages.
Further, the weight percent of polypropylene in the polypropylene-methylpentene copolymer (also referred to as propylene-methylpentene copolymer) is less than 10%.
Further, the polypropylene mixture of the adhesive layer is a mixture composed of 0% -5% of polypropylene elastomer and 95% -100% of polypropylene and methylpentene copolymer. The foregoing technical solutions include embodiments 1,2 and embodiment 6.
Further, the polypropylene elastomer has a density of 0.86 to 0.88g/cm 3 The melt index is between 6.0 and 8.0g/10min. The density of the polypropylene and methyl pentene copolymer is 0.83-0.85g/cm 3 The melt index is between 4.0 and 6.0g/10min.
Further toThe polypropylene elastomer in the adhesive layer is metallocene polypropylene elastomer, and the density is 0.86-0.88g/cm 3 The melt index is 6.0-8.0g/10min.
The innovation point of the invention is mainly that the formulation of the adhesive layer of the protective film is that the crystallinity and the glass transition temperature of the methylpentene polymer are reduced due to the addition of polypropylene in the polymer of the adhesive layer polypropylene and the methylpentene, so that the polymer composed of the polypropylene and the methylpentene becomes relatively soft, has good adhesion at normal temperature, and simultaneously maintains good heat resistance. Whereas metallocene polypropylene elastomers have a higher melting point and better adhesion than general polyolefin elastomers, the adhesion can be adjusted by adding a suitable proportion.
Further, the thickness of the surface layer of the high-temperature-resistant protective film is 4-8 mu m, the thickness of the core layer is 20-24 mu m, and the thickness of the adhesive layer is 4-8 mu m.
Further, in the high temperature resistant protective film, the content of the homo-polypropylene in the surface layer is 80% -90%, and the content of the methylpentene polymer is 10% -20%.
Further, in the high temperature resistant protective film, the thickness of the surface layer is 6 mu m, the thickness of the core layer is 20 mu m, and the thickness of the adhesive layer is 4 mu m.
On the other hand, the invention also provides a preparation method of the high-temperature-resistant protective film, and the high-temperature-resistant protective film is prepared in a three-layer coextrusion casting mode.
Compared with the prior art, the adhesive layer of the high-temperature-resistant protective film has the beneficial effects that the adhesive layer is a mixture composed of the polypropylene elastomer and the polymer of polypropylene and methylpentene, and compared with the conventional polyolefin resin adhesive layer, the adhesive layer has the advantages that the heat resistance of the adhesive layer material is improved, and meanwhile, the adhesive layer can be better attached to the surface of a product. The polymer of polypropylene and methylpentene has the advantages of low viscosity, low temperature influence, high crystallinity, difficult warping and edge melting after high temperature, no white fog and residual glue after tearing the surface of the object, and suitability for various processes with high temperature protection requirements.
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) Initial peel force test
A25 mm wide sample of the protective film was attached to a PMMA plate and the attached film was then rolled at 300mm/min using a 2kg FINAT standard roller. The film was peeled off from the PMMA plate for a period of time and then tested according to the 180 peel strength test method, and the average value was recorded as the initial peel force.
(2) High temperature peel force
After the PMMA plate with the protective film attached was placed in an oven at 150℃for 1 hour, the peel force of the protective film from the PMMA plate was measured.
(3) Protective film warpage, haze and edge melting
The PMMA plate with the protective film was placed in an oven at 150deg.C for 1h, cooled, and visually confirmed.
The high temperature resistance of the adhesive layer of the protective film mainly shows whether bad appearance such as warpage white fog, edge melting and the like occurs after a high temperature test.
(4) Residual glue
And (3) placing the PMMA plate adhered with the protective film in a baking oven at 150 ℃ for 1h, and visually observing whether residual glue remained on the protective film exists on the surface of the PMMA plate after the protective film is peeled off.
Example 1
The high-temperature-resistant protective film provided by the invention sequentially comprises a surface layer, a core layer and an adhesive layer.
The skin layer comprised 80% homo-polypropylene and 20% methylpentene polymer. The density of the homo-polypropylene was 0.90g/cm 3 The melt index was 8.0g/10min. The density of the methylpentene polymer was 0.85g/cm 3 The melt index was 21.0g/10min.
The core layer adopts 100 weight percent of homo-polypropylene with the density of 0.91g/cm 3 The melt index was 4.5g/10min.
The adhesive layer adopts 100% polypropylene and methylpentene polymer, and has a density of0.83g/cm 3 The melt index was 6.0g/10min.
The thickness of the skin layer was 6 μm, the thickness of the core layer was 20 μm, and the thickness of the adhesive layer was 4 μm.
Example 2
The high temperature resistant protective film provided in example 1 is different in that:
the skin layer comprised 85% homo-polypropylene and 15% methylpentene polymer.
The adhesive layer adopts 5% of polypropylene elastomer and 95% of polymer of polypropylene and methylpentene, and the density of the polypropylene elastomer is 0.86g/cm 3 The melt index was 6.0g/10min.
Example 3
The high temperature resistant protective film provided in example 1 is different in that:
the skin layer comprised 90% homo-polypropylene and 10% methylpentene polymer.
The adhesive layer adopts 10% of polypropylene elastomer and 90% of polymer of polypropylene and methylpentene, and the density of the polypropylene elastomer is 0.88g/cm 3 The melt index was 8.0g/10min.
Example 4
The high temperature resistant protective film provided in example 1 is different in that:
the skin layer comprised 80% homo-polypropylene and 20% methylpentene polymer. The density of the homo-polypropylene was 0.91g/cm 3 The melt index was 3.0g/10min. The density of the methylpentene polymer was 0.87g/cm 3 The melt index was 27.0g/10min.
The adhesive layer adopts 10% of polypropylene elastomer and 90% of polymer of polypropylene and methylpentene, and the density of the polypropylene elastomer is 0.88g/cm 3 The melt index was 8.0g/10min.
Example 5
The high temperature resistant protective film provided in example 1 is different in that:
the skin layer comprised 85% homo-polypropylene and 15% methylpentene polymer. The density of the homo-polypropylene is0.91g/cm 3 The melt index was 3.0g/10min. The density of the methylpentene polymer was 0.87g/cm 3 The melt index was 27.0g/10min.
The adhesive layer adopts 15% of polypropylene elastomer and 85% of polymer of polypropylene and methylpentene, and the density of the polypropylene elastomer is 0.88g/cm 3 The melt index was 8.0g/10min.
Example 6
The high temperature resistant C protective film provided in example 1 is different in that:
the skin layer comprised 90% homo-polypropylene and 10% methylpentene polymer. The density of the homo-polypropylene was 0.91g/cm 3 The melt index was 3.0g/10min. The density of the methylpentene polymer was 0.87g/cm 3 The melt index was 27.0g/10min.
The adhesive layer adopts 5% of polypropylene elastomer and 95% of polymer of polypropylene and methylpentene, and the density of the polypropylene elastomer is 0.86g/cm 3 The melt index was 6.0g/10min.
Comparative example 1
The difference from example 1 is that: the surface layer adopts 100% homo-polypropylene with the density of 0.9g/cm 3 The melt index was 8.0g/10min. The adhesive layer adopts polypropylene elastomer with density of 0.86g/cm 3 The melt index was 6.0g/10min.
The formulations of the surface layers of the protective films obtained in examples 1 to 6 and comparative example 1 are shown in Table 1, the initial peel force and the high temperature peel force test results of the protective films are shown in Table 2, and the warpage, haze and edge melting phenomena after baking are shown in Table 3.
TABLE 1 formulations of the surface layers of the protective films provided in examples 1-6 and comparative example 1 of the present invention
TABLE 2 initial peel force and high temperature peel force test results for the protective films provided in examples 1-6 of the present invention and comparative example 1
TABLE 3 warpage, haze, edge melting phenomena after baking in examples 1-6 and comparative example 1 of the present invention
From comparison of the comparative examples and examples, it can be seen that examples 1,2, and 6 of the present invention exhibited relatively stable peeling force on PMMA plates and less variation in peeling force at high temperatures. Wherein, the high temperature peeling force of examples 3, 4 and 5 exceeds 10gf/25mm, which shows that the peeling force after high temperature baking rises more obviously, and the content of the polypropylene elastomer in the adhesive layer needs to be controlled within 5 percent relative to the addition amount of the polypropylene elastomer in the adhesive layer material. Therefore, the combination properties of examples 1,2 and 6 are better, and are more suitable for various manufacturing processes with high temperature protection requirements.
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention.
Claims (4)
1. The high temperature resistant protective film is characterized by sequentially comprising a surface layer, a core layer and an adhesive layer, wherein the adhesive layer is a polypropylene mixture;
the surface layer consists of homopolypropylene and high-crystallization resin, wherein the high-crystallization resin is methylpentene polymer, the content of the homopolypropylene in the surface layer is 80-90%, and the content of the methylpentene polymer is 10-20%; the melt index of the homo-polypropylene in the surface layer is 3.0-8.0g/10min, and the melt index of the methylpentene polymer is 21-27g/10min;
the core layer is made of homo-polypropylene, and the melt index of the core layer is 3.0-8.0g/10 min;
the polypropylene mixture of the adhesive layer is a mixture composed of 0% -5% of polypropylene elastomer and 95% -100% of polypropylene and methylpentene copolymer; the polypropylene elastomer in the adhesive layer is a metallocene polypropylene elastomer, and the melt index of the polypropylene elastomer is 6.0-8.0g/10min; the melt index of the polypropylene and methyl pentene copolymer is 4.0-6.0g/10min.
2. The high temperature resistant protective film according to claim 1, wherein the metallocene polypropylene elastomer in the adhesive layer has a density of 0.86 to 0.88g/cm 3 。
3. The high temperature resistant protective film according to claim 1, wherein the density of the copolymer of polypropylene and methylpentene in the adhesive layer is 0.83-0.85g/cm 3 。
4. A method for preparing a high temperature resistant protective film according to claim 1, wherein the high temperature resistant protective film is prepared by three-layer coextrusion casting.
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