CN114507486A - 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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- CN114507486A CN114507486A CN202011277267.7A CN202011277267A CN114507486A CN 114507486 A CN114507486 A CN 114507486A CN 202011277267 A CN202011277267 A CN 202011277267A CN 114507486 A CN114507486 A CN 114507486A
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- protective film
- polypropylene
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- 230000001681 protective effect Effects 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000004743 Polypropylene Substances 0.000 claims abstract description 66
- 229920001155 polypropylene Polymers 0.000 claims abstract description 66
- -1 polypropylene Polymers 0.000 claims abstract description 65
- 239000012790 adhesive layer Substances 0.000 claims abstract description 36
- 239000002344 surface layer Substances 0.000 claims abstract description 21
- 239000012792 core layer Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229920006038 crystalline resin Polymers 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 7
- 229920005989 resin Polymers 0.000 claims abstract description 7
- JMMZCWZIJXAGKW-UHFFFAOYSA-N 2-methylpent-2-ene Chemical group CCC=C(C)C JMMZCWZIJXAGKW-UHFFFAOYSA-N 0.000 claims description 29
- 229920000642 polymer Polymers 0.000 claims description 27
- 229920001971 elastomer Polymers 0.000 claims description 24
- 239000000806 elastomer Substances 0.000 claims description 24
- 229920005629 polypropylene homopolymer Polymers 0.000 claims description 15
- 239000010410 layer Substances 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 abstract description 17
- 230000008018 melting Effects 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 7
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 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
- 238000012360 testing method Methods 0.000 description 6
- 238000009472 formulation Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 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
- 230000008859 change Effects 0.000 description 1
- 238000010073 coating (rubber) Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007334 copolymerization reaction 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
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000011179 visual inspection Methods 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 is warped, foggy and edge-melting in a high-temperature process environment, and the protective film is difficult to peel off due to adhesive residue 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 and high-crystalline resin, the core layer is made of polypropylene resin, and the adhesive layer is made of a 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 demand of protective films, the requirements for the functions of the protective films are increasing, and particularly, high temperature resistant protection is required in the process of manufacturing electronic elements such as ITO, TP and the like, which requires that the protective films have good high temperature resistant characteristics to better protect the surfaces of the products.
Common high temperature resistant protection film in the existing market is the rubber coating film, and general self-adhesive film does not have the high temperature resistant characteristic, and after the high temperature baking of 150 ℃, the protection film can all appear warpage, white fog and even melt a great deal of problems such as limit, seriously influence the performance of final product.
Disclosure of Invention
The invention provides a high-temperature-resistant protective film and a preparation method thereof, aiming at solving the problems of warping, white fog and even edge melting of the existing protective film in a high-temperature process. The protective film has good high-temperature resistance, and does not generate warping, white fog and edge melting in a high-temperature process environment.
Furthermore, in order to solve the problems that the existing protective film has warping, 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, does not have warping, white fog and edge melting in the high-temperature process environment, does not have the problems of adhesive residue and the like after being baked and torn at high temperature, and is suitable for various process technologies with high-temperature resistance 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 homopolymerized polypropylene and high-crystalline resin, the core layer is selected from polypropylene resin, and the adhesive layer is a polypropylene mixture.
Generally, the existing protective film cannot resist high temperature, particularly, the adhesive layer resin material has a low melting point, is melted after high temperature, remains on the surface of an attached object after cooling, and is not easy to peel. Aiming at the existing problems, the invention mainly solves the problems by selecting a high-temperature resistant material with higher crystallinity or higher melting point as the adhesive layer.
Further, the surface layer is composed of homopolymerized polypropylene and high-crystalline resin.
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 homopolymerized polypropylene (PP) has higher crystallinity and better rigidity, and has higher melting point and better heat resistance compared with random copolymerization polypropylene.
Further, the highly crystalline resin in the surface layer is selected from methylpentene polymers having a density of 0.85-0.87g/cm3The melt index is between 21 and 27g/10 min.
Furthermore, the methyl pentene polymer is a transparent crystalline resin, has high modulus and high crystallinity, has a melting point of 240 ℃ or higher, and has good heat resistance.
Further, the surface layer is composed of 80% -90% of homopolymerized polypropylene and 10% -20% of methyl pentene polymer. The percentage is weight percentage.
Furthermore, the core layer of the high-temperature resistant 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 protective film is characterized in that the adhesive layer is a polypropylene mixture.
Further, the polypropylene mixture of the adhesive layer is a mixture consisting of 0% -15% of polypropylene elastomer and 85% -100% of polypropylene and methyl pentene copolymer. The above percentages are weight percentages.
Further, the weight percent of polypropylene in the polypropylene and methylpentene copolymer (also referred to as propylene and methylpentene copolymer) is less than 10%.
Further, the polypropylene mixture of the adhesive layer is a mixture consisting of 0% -5% of polypropylene elastomer and 95% -100% of polypropylene and methyl pentene copolymer. The foregoing technical solutions include examples 1, 2 and example 6.
Further, the density of the polypropylene elastomer is 0.86-0.88g/cm3And the melt index is between 6.0 and 8.0g/10 min. The density of the polypropylene and the methylpentene copolymer is 0.83-0.85g/cm3And the melt index is between 4.0 and 6.0g/10 min.
Further, the polypropylene elastomer in the adhesive layer is metallocene polypropylene elastomer, and the density of the polypropylene elastomer is 0.86-0.88g/cm3The melt index is 6.0-8.0g/10 min.
The innovation point of the invention is mainly the formula of the protective film adhesive layer, and the addition of polypropylene in the polymer of the adhesive layer polypropylene and the methylpentene reduces the crystallinity and the glass transition temperature of the methylpentene polymer, so that the polymer formed by the polypropylene and the methylpentene becomes relatively soft, has good adhesion at normal temperature, and simultaneously maintains better heat resistance. Compared with the common polyolefin elastomer, the metallocene polypropylene elastomer has higher melting point and better adhesiveness, and the adhesiveness can be adjusted by adding a proper proportion.
Furthermore, the thickness of the surface layer of the high-temperature resistant protective film is 4-8 μm, the thickness of the core layer is 20-24 μm, and the thickness of the adhesive layer is 4-8 μm.
Furthermore, in the surface layer of the high-temperature resistant protective film, the content of the homopolymerized polypropylene is 80-90%, and the content of the methylpentene polymer is 10-20%.
Furthermore, the thickness of the surface layer of the high-temperature resistant protective film is 6 microns, the thickness of the core layer is 20 microns, and the thickness of the adhesive layer is 4 microns.
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 co-extrusion casting mode.
Compared with the prior art, the high-temperature-resistant protective film has the beneficial effects that the adhesive layer of the high-temperature-resistant protective film is selected from a mixture consisting of the polypropylene elastomer and the polymer of polypropylene and methylpentene, and compared with the conventional polyolefin resin adhesive layer, the heat resistance of the adhesive layer material is improved, and meanwhile, the adhesive layer material can be better attached to the surface of a product. The polypropylene and methylpentene polymer has high melting point, less temperature influence on viscosity, high crystallinity, less warpage, edge melting and other problems, and may be used in various kinds of high temperature protecting process.
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 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 initial peel force.
(2) High temperature peel force
And (3) placing the PMMA board adhered with the protective film in an oven at 150 ℃ for 1h, and then testing the stripping force of the protective film and the PMMA board.
(3) Protective film warping, white fog and edge melting
The PMMA plate stuck with the protective film is placed in an oven at 150 ℃ for 1h, and is confirmed by visual inspection after being cooled.
The high temperature resistance of the protective film adhesive layer is mainly to see whether the poor appearances such as warping, white fog, edge melting and the like appear after a high temperature test.
(4) Residual glue
And (3) placing the PMMA board adhered with the protective film in an oven at 150 ℃ for 1h, peeling the protective film, and then visually observing whether the surface of the PMMA board has residual glue left by the protective film.
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% homopolypropylene and 20% methylpentene polymer. The density of the homo-polypropylene is 0.90g/cm3The melt index was 8.0g/10 min. The density of the methylpentene polymer was 0.85g/cm3The melt index was 21.0g/10 min.
The core layer adopts 100 weight percent of homopolymerized polypropylene and has the density of 0.91g/cm3The melt index was 4.5g/10 min.
The adhesive layer adopts 100 percent of polymer of polypropylene and methylpentene, and the density of the adhesive layer is 0.83g/cm3The melt index was 6.0g/10 min.
The surface layer has a thickness of 6 μm, the core layer has a thickness of 20 μm, and the adhesive layer has a thickness of 4 μm.
Example 2
The high temperature resistant protective film as provided in example 1, except that:
the skin layer comprised 85% homopolypropylene 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/cm3The melt index was 6.0g/10 min.
Example 3
The high temperature resistant protective film as provided in example 1, except that:
the skin layer comprised 90% homopolypropylene 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/cm3The melt index was 8.0g/10 min.
Example 4
The high temperature resistant protective film as provided in example 1, except that:
the skin layer comprised 80% homopolypropylene and 20% methylpentene polymer. The density of the homo-polypropylene is 0.91g/cm3The melt index was 3.0g/10 min. The density of the methylpentene polymer was 0.87g/cm3The melt index was 27.0g/10 min.
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/cm3The melt index was 8.0g/10 min.
Example 5
The high temperature resistant protective film as provided in example 1, except that:
the skin layer comprised 85% homopolypropylene and 15% methylpentene polymer. The density of the homo-polypropylene is 0.91g/cm3The melt index was 3.0g/10 min. The density of the methylpentene polymer was 0.87g/cm3The melt index was 27.0g/10 min.
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/cm3The melt index was 8.0g/10 min.
Example 6
The high temperature resistant C protective film provided in example 1, except that:
the skin layer comprised 90% homopolypropylene and 10% methylpentene polymer. The density of the homo-polypropylene is 0.91g/cm3The melt index was 3.0g/10 min. The density of the methylpentene polymer was 0.87g/cm3The melt index was 27.0g/10 min.
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/cm3The melt index was 6.0g/10 min.
Comparative example 1
The difference from example 1 is that: the surface layer adopts 100 percent of homopolymerized polypropylene and has the density of 0.9g/cm3The melt index was 8.0g/10 min. The adhesive layer is made of polypropylene elastomer and has a density of 0.86g/cm3The melt index was 6.0g/10 min.
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 high temperature peel force test results of the protective films are shown in table 2, and the warpage, white fog and edge melting phenomena after baking are shown in table 3.
Table 1 formulations of skin layers of protective films provided in examples 1 to 6 of the present invention and comparative example 1
Table 2 initial peel force and high temperature peel force test results of the protective films provided in inventive examples 1 to 6 and comparative example 1
TABLE 3 warpage, white fog, and edge melting after baking in inventive examples 1-6 and comparative example 1
By comparing the comparative examples and examples, it can be seen from the test results that inventive examples 1, 2, 6 exhibited relatively stable peel force on PMMA plates and the change in peel force at high temperature was small. Among them, the examples 3, 4 and 5, which have a high-temperature peel force exceeding 10gf/25mm, show that the rise of the peel force after the high-temperature baking is remarkable, and the content of the polypropylene elastomer in the adhesive layer needs to be controlled within 5% depending on the amount of the polypropylene elastomer added to the adhesive layer material. Therefore, the embodiments 1, 2 and 6 have better comprehensive performance and are more suitable for various manufacturing processes with high-temperature protection requirements.
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 protective film is characterized by sequentially comprising a surface layer, a core layer and an adhesive layer, wherein the surface layer comprises homopolymerized polypropylene and high-crystalline resin, the core layer is selected from polypropylene resin, and the adhesive layer is selected from a polypropylene mixture.
2. The high temperature resistant protective film according to claim 1, wherein the surface layer is composed of homo polypropylene and a high crystalline resin.
3. The high temperature resistant protective film according to claim 2, wherein the melt index of the homo-polypropylene in the surface layer is between 3.0 and 8.0g/10 min.
4. The high temperature resistant protective film of claim 2, wherein the high crystalline resin in the surface layer is selected from methylpentene polymers having a density of 0.85-0.87g/cm3The melt index is 21-27g/10 min.
5. The high temperature resistant protective film according to claim 4, wherein in the surface layer, the content of homo-polypropylene is 80% -90%, and the content of methylpentene polymer is 10% -20%.
6. The high temperature resistant protective film according to claim 1, wherein the core layer is selected from homo polypropylene having a melt index of 3.0-8.0g/10 min.
7. The high temperature resistant protective film according to claim 1, wherein the adhesive layer is composed of 0% -15% of polypropylene elastomer and 85% -100% of copolymer of polypropylene and methylpentene.
8. The high temperature resistant protective film according to claim 7, wherein the polypropylene elastomer in the adhesive layer is a metallocene polypropylene elastomer having a density of 0.86-0.88g/cm3The melt index is 6.0-8.0g/10 min.
9. The high temperature resistant protective film according to claim 7, wherein the density of the copolymer of polypropylene and methylpentene in the adhesive layer is 0.83-0.85g/cm3The melt index is 4.0-6.0g/10 min.
10. The method for preparing the high-temperature-resistant protective film according to claim 1, wherein the high-temperature-resistant protective film is prepared by a three-layer co-extrusion casting method.
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