CN111002667A - Release film and preparation method thereof - Google Patents
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- CN111002667A CN111002667A CN201911317773.1A CN201911317773A CN111002667A CN 111002667 A CN111002667 A CN 111002667A CN 201911317773 A CN201911317773 A CN 201911317773A CN 111002667 A CN111002667 A CN 111002667A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
- B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/06—Interconnection of layers permitting easy separation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/08—PCBs, i.e. printed circuit boards
Abstract
The invention relates to a preparation method of a release film, which comprises the following steps: providing a first raw material, a second raw material and a third raw material, wherein the first raw material is at least one of polytetrafluoroethylene, ethylene-tetrafluoroethylene copolymer, polyvinylidene fluoride and polyvinyl fluoride, the second raw material is a bonding material, and the third raw material is a polyester material; respectively adding the first raw material, the second raw material and the third raw material into a first single-screw extruder, a second single-screw extruder and a third single-screw extruder, wherein the temperature of the first single-screw extruder is controlled to be 280-320 ℃, the temperature of the second single-screw extruder is controlled to be 80-150 ℃, and the temperature of the third single-screw extruder is controlled to be 250-280 ℃; and extruding through a T-shaped die head by adopting a three-layer co-extrusion method to obtain the release film with the ABC three-layer structure, wherein the layer A in the release film is a release layer, the layer B is an adhesive layer, and the layer C is a supporting layer. The invention also provides a release film.
Description
Technical Field
The invention relates to the field of film materials, in particular to a release film and a preparation method thereof.
Background
The release film refers to a film having a surface with separability, and the release film has no or only slight stickiness with a specific material after being contacted with a limited condition. The release film is widely applied to the industry fields of electronics, packaging, silk screen printing, transfer printing, nameplate, switches, flexible circuits, insulating products, laser anti-counterfeiting, laminating, medicine, toilet paper, adhesive products, die cutting and punching processing and the like.
In the high temperature of more than 180 ℃ in the Flexible Printed Circuit (FPC) lamination, the silicon-containing release film can leave silica gel on the Polyimide (PI) film at such high temperature, which can lead to the FPC not to be used, so that the silicon-free high-temperature-resistant release film is needed. Therefore, a fluorine-containing release film or a polymethylpentene (PMP) release film is often used, isovaleric acid is easily separated out from the PMP release film in a high-temperature pressing process, small molecules of the type are adsorbed on the PI film and need to be heated and then volatilized, and the working efficiency is influenced. In addition, with the rapid development of the 5G technology, a Modified Polyimide (MPI) film or a Liquid Crystal Polymer (LCP) film is required to be used in an antenna wiring board, and the antenna wiring board needs to be pressed at a high temperature of 220 ℃ to 250 ℃, so that a PMP release film cannot be used, and thus, a release film resistant to high temperature needs to be developed.
Disclosure of Invention
In view of the above, the present invention provides a high temperature resistant release film.
A preparation method of a release film comprises the following steps:
providing a first raw material, a second raw material and a third raw material, wherein the first raw material is at least one of polytetrafluoroethylene, ethylene-tetrafluoroethylene copolymer, polyvinylidene fluoride and polyvinyl fluoride, the second raw material is a bonding material, and the third raw material is a polyester material;
respectively adding the first raw material, the second raw material and the third raw material into a first single-screw extruder, a second single-screw extruder and a third single-screw extruder, wherein the temperature of the first single-screw extruder is controlled to be 280-320 ℃, the temperature of the second single-screw extruder is controlled to be 80-150 ℃, and the temperature of the third single-screw extruder is controlled to be 250-280 ℃; and
and extruding through a T-shaped die head by adopting a three-layer co-extrusion method to obtain the release film with an ABC three-layer structure, wherein the layer A in the release film is a release layer, the layer B is an adhesive layer, and the layer C is a supporting layer.
Compared with the prior art, the release film provided by the invention adopts a three-layer co-extrusion method to obtain the release layer comprising the release layer, the adhesive layer and the support layer, wherein the support layer is made of polyester material, and the release layer adopts non-PMP fluorine material, such as: polytetrafluoroethylene, ethylene-tetrafluoroethylene copolymer or polyvinylidene fluoride and polyvinyl fluoride, and finally obtaining the ABC three-layer integrally-formed structure. The three-layer co-extrusion method can realize one-step in-place, and also avoids the defects of complicated steps caused by attaching a release layer or coating a release coating on the substrate in the prior art.
The invention also provides a release film obtained by the method. The release film has a longitudinal thermal shrinkage rate of 0.1-0.3% and a transverse thermal shrinkage rate of-0.10% at 180 ℃ for 30 minutes.
The release film has the following advantages that firstly, the release film is made of a self-release material, the surface of the release film is a silicon-free layer, and the silicon layer residue in the pressing process is avoided. Secondly, the release film is of a three-layer integrated structure, has high temperature resistance, can be pressed at 250 ℃, and has high release property. Thirdly, the bonding layer has good flexibility, so that the release film has low thermal shrinkage. The release film has wide application prospect.
Drawings
Fig. 1 is a schematic structural view of the release film of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a preparation method of a release film, which comprises the following steps:
s1, providing a first raw material, a second raw material and a third raw material, wherein the first raw material is at least one of Polytetrafluoroethylene (PTFE), ethylene-tetrafluoroethylene copolymer (ETFE), polyvinylidene fluoride (PVDF) and polyvinyl fluoride (PVF), the second raw material is a bonding material, and the third raw material is a polyester material;
s2, adding the first raw material, the second raw material and the third raw material into a first single-screw extruder, a second single-screw extruder and a third single-screw extruder respectively, wherein the temperature of the first single-screw extruder is controlled to be 280-320 ℃, the temperature of the second single-screw extruder is controlled to be 80-150 ℃, and the temperature of the third single-screw extruder is controlled to be 250-280 ℃; and
and S3, extruding through a T-shaped die by adopting a three-layer co-extrusion method to obtain the release film with an ABC three-layer structure, wherein the layer A in the release film is a release layer, the layer B is an adhesive layer, and the layer C is a supporting layer.
In step S1, the first raw material is non-PMP material, i.e. decomposition at high temperature to separate out isovaleric acid is avoided. Preferably, the first raw material is at least one of polytetrafluoroethylene and polyvinyl fluoride.
The bonding material includes styrene-butadiene-styrene copolymer (SEBS). The polyester material comprises at least one of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT). Preferably, the polyester material is PBT.
In step S2, the first single screw extruder, the second single screw extruder, and the third single screw extruder are used to melt, plasticize, filter, and pass through a distribution block, and then enter the T-die of step S3. The separation is caused by different materials and different melting temperatures of the raw materials, so that the raw materials are extruded by different screw extruders respectively to obtain molten raw materials.
Of course, the filter mesh pore sizes of the first single screw extruder, the second single screw extruder, and the third single screw extruder are all 10 μm to 15 μm. This is because the mesh facilitates the components being in a molten state.
In step S3, the T-die pack in the three-layer coextrusion method has a temperature of 280-320 ℃, a casting speed of 50-100 m/min, and a cold roll temperature of 60-100 ℃.
After being extruded through a T-shaped die head, the layer A of the release film is cooled by a cooling roller, and the layer C is cooled by a back cooling roller.
The thicknesses of the finally obtained layer A, layer B and layer C are not limited. The thickness of the A layer can be 2-10 μm, the thickness of the B layer can be 2-5 μm, and the thickness of the C layer can be 25-56 μm.
The invention also provides the release film prepared by the preparation method. Referring to fig. 1, the release film includes a layer a, a layer B, and a layer C, wherein the layer a is a release layer, the layer B is an adhesive layer, and the layer C is a supporting layer. The release film has a longitudinal thermal shrinkage rate of 0.1-0.3% and a transverse thermal shrinkage rate of-0.10% at 180 ℃ for 30 minutes. The release film has excellent release force, and particularly, the release force is 25g/in-50 g/in.
The release film has the following advantages that firstly, the release film is made of a self-release material, the surface of the release film is a silicon-free layer, and the silicon layer residue in the pressing process is avoided. Secondly, the release film is of a three-layer integrated structure, has high temperature resistance, can be pressed at 250 ℃, and has high release property. Thirdly, the bonding layer has good flexibility, so that the release film has low thermal shrinkage.
The release film and the method for producing the release film according to the present invention will be described below with reference to examples.
Of the materials for layer A, PTFE resin was purchased from Asahi glass, USA under the trademark CD 123E. ETFE resin was purchased from Asahi glass, USA under the trademark C55 AP. PVDF resin was purchased from arkema, france under the trade designation 460. PVF resin is purchased in Zhejiang blue sky for environmental protection.
Of the materials for the layer B, SEBS was purchased from kraton, usa under the designation FG1901X, hardness 71D, specific gravity 0.9g/cm3, and PS/PB 30/70.
In the material of the layer C, PET resin is purchased from China petrochemical characterization chemical fiber company Limited and is of the brand FG 600. The PBT resin is purchased from China petrochemical characterization chemical fiber company Limited and has the brand number TX 722.
In the following examples, the materials of the layer a, the layer B and the layer C were added to different single screw extruders, respectively, subjected to melt plasticization and filtration, passed through distribution blocks, and then fed into a T-die capable of forming A, B, C three layers by extrusion, cooled to form a film, tempered, rolled, slit and packaged. Wherein the first single screw extruder corresponds to the layer A, the second single screw extruder corresponds to the layer B, and the third single screw extruder corresponds to the layer C. The cooling means corresponding to the material A is a cold attaching roller, and the cooling means corresponding to the material C is a back cold roller.
The temperatures of all the zones of the first single-screw extruder are 280 ℃, 290 ℃, 300 ℃, 310 ℃, 320 ℃, 300 ℃ and 290 ℃; the pore size of the filter screen was 15 μm. The temperature of each zone of the second single screw extruder is 80 ℃, 100 ℃, 120 ℃, 150 ℃, 135 ℃, 120 ℃ and 100 ℃; the pore size of the filter screen was 15 μm. The temperature of each area of the second single-screw extruder is 250-280 ℃; the pore size of the filter screen was 15 μm. The temperature of the T-die is 280 deg.C, 290 deg.C, 300 deg.C, 310 deg.C, 320 deg.C, 310 deg.C, 290 deg.C. The casting speed was 80 m/min. The temperature of the cold roll was 80 ℃.
Example 1
The layer A is PTFE, the layer B is SEBS, and the layer C is PET. The total thickness of the release film is 50 μm, the thickness of the A layer is 5 μm, the thickness of the B layer is 3 μm, and the thickness of the C layer is 42 μm.
Example 2
The layer A is ETFE, the layer B is SEBS, and the layer C is PET. The total thickness of the release film is 50 μm, the thickness of the A layer is 4 μm, the thickness of the B layer is 2 μm, and the thickness of the C layer is 46 μm.
Example 3
The layer A is PVDF, the layer B is SEBS, and the layer C is PBT. The total thickness of the release film is 55 μm, the thickness of the A layer is 8 μm, the thickness of the B layer is 2 μm, and the thickness of the C layer is 45 μm.
Example 4
The layer A is PVF, the layer B is SEBS, and the layer C is PBT. The total thickness of the release film is 60 μm, the thickness of the A layer is 10 μm, the thickness of the B layer is 3 μm, and the thickness of the C layer is 47 μm.
Example 5
The layer A is PTFE, the layer B is SEBS, and the layer C is PBT. The total thickness of the release film is 40 μm, the thickness of the A layer is 2 μm, the thickness of the B layer is 2 μm, and the thickness of the C layer is 36 μm.
Example 6
The layer A is PVDF, the layer B is SEBS, and the layer C is PET. The total thickness of the release film is 60 μm, the thickness of the A layer is 10 μm, the thickness of the B layer is 5 μm, and the thickness of the C layer is 45 μm.
Comparative example 1
TPX type release film of Japan Sanjingtong xylonite, with a mark of X-99BR and a thickness of 50 μm. This release film is different from the release film in example 1, and includes only PMP polyolefin resin.
Comparative example 2
The Japanese ponding electronic PBT release film is under the mark of RP50 and has the thickness of 50 mu m. This release film is different from the release film in example 1, and includes only PBT resin.
The release films of examples 1-6 and comparative examples 1-2 were tested as follows:
release force (release property) test: and (3) sticking the TESA7475 adhesive tape on the tested release surface, back-pressing the tape for three times by using a pressing roller to ensure that the adhesive tape is fully contacted with the release surface, peeling the tape at a peeling angle of 180 degrees after the tape is placed for 24 hours, and recording the test result of the release force. The smaller the release force, the easier the peeling, and the better the releasability of the release film.
Testing the thermal shrinkage rate: a200 mm X200 mm sample of release film was tested for its dimensions before heating in the Machine Direction (MD) and Transverse Direction (TD), then placed in an oven at 180 ℃ for 30min, and after cooling, it was taken out and tested for its heated dimensions. MD heat shrinkage ═ dimension before MD heating-dimension after MD heating x 100%/dimension before MD heating; TD heat shrinkage ratio (dimension before TD heating-dimension after MD heating) × 100%/dimension before TD heating. The test was performed three times and the average value was taken.
The results of the above tests are shown in the following table.
TABLE 1
| Heat shrinkage/% (MD) | Heat shrinkage/% (TD) | Release force g/in | |
| Example 1 | 0.12 | -0.10 | 32 |
| Example 2 | 0.18 | 0.05 | 50 |
| Example 3 | 0.26 | -0.08 | 35 |
| Example 4 | 0.15 | -0.09 | 25 |
| Example 5 | 0.24 | 0.10 | 45 |
| Example 6 | 0.91 | -0.04 | 38 |
| Comparative example 1 | 1.0 | -0.3 | 56 |
| Comparative example 2 | 0.9 | 0.3 | 86 |
As can be seen from table 1, in example 4, the layer a is PVF, the layer B is SEBS, and the layer C is PBT. The total thickness of the release film was 60 μm. The release film has the most excellent release force.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the release film is characterized by comprising the following steps:
providing a first raw material, a second raw material and a third raw material, wherein the first raw material is at least one of polytetrafluoroethylene, ethylene-tetrafluoroethylene copolymer, polyvinylidene fluoride and polyvinyl fluoride, the second raw material is a bonding material, and the third raw material is a polyester material;
respectively adding the first raw material, the second raw material and the third raw material into a first single-screw extruder, a second single-screw extruder and a third single-screw extruder, wherein the temperature of the first single-screw extruder is controlled to be 280-320 ℃, the temperature of the second single-screw extruder is controlled to be 80-150 ℃, and the temperature of the third single-screw extruder is controlled to be 250-280 ℃; and
and extruding through a T-shaped die head by adopting a three-layer co-extrusion method to obtain the release film with an ABC three-layer structure, wherein the layer A in the release film is a release layer, the layer B is an adhesive layer, and the layer C is a supporting layer.
2. The method for preparing the release film according to claim 1, wherein the first raw material is at least one of polytetrafluoroethylene and polyvinyl fluoride.
3. The method of preparing the release film according to claim 1, wherein the adhesive material comprises styrene-butadiene-styrene copolymer.
4. The method for preparing the release film according to claim 1, wherein the polyester material comprises at least one of polyethylene terephthalate and polybutylene terephthalate.
5. The method for preparing a release film according to claim 1, wherein the temperature of the T-shaped die pack in the three-layer co-extrusion method is 280 ℃ to 320 ℃, the casting speed is 50m/min to 100m/min, and the temperature of the cold roll is 60 ℃ to 100 ℃.
6. The method for preparing the release film according to claim 1, wherein the first single-screw extruder, the second single-screw extruder and the third single-screw extruder each have a filter mesh pore size of 10 μm to 15 μm.
7. The method for preparing the release film according to claim 1, wherein after the extrusion through the T-die, the layer A of the release film is cooled by a chill roll and the layer C is cooled by a back chill roll.
8. The method for preparing the release film according to claim 1, wherein the thickness of the layer a is 2 μm to 10 μm, the thickness of the layer B is 2 μm to 5 μm, and the thickness of the layer C is 25 μm to 56 μm.
9. The release film prepared by the preparation method of any one of claims 1 to 8, wherein the release film has a longitudinal thermal shrinkage rate of 0.1 to 0.3 percent and a transverse thermal shrinkage rate of-0.10 to 0.10 percent under the test conditions of 180 ℃ and 30 minutes.
10. The release film according to claim 8, wherein the release film has a release force of 25g/in to 50 g/in.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112874080A (en) * | 2021-01-15 | 2021-06-01 | 芜湖夏鑫新型材料科技有限公司 | Silicon-free PE protective film for attaching release paper |
| CN113263816A (en) * | 2021-05-22 | 2021-08-17 | 江苏双星彩塑新材料股份有限公司 | Impact-resistant and explosion-proof polyester release film and preparation method thereof |
| CN113388138A (en) * | 2021-06-24 | 2021-09-14 | 扬州万润光电科技有限公司 | High-temperature stable release film and preparation method thereof |
| CN113896927A (en) * | 2021-12-10 | 2022-01-07 | 国家电投集团氢能科技发展有限公司 | Release film and preparation method and application thereof |
| CN115746725A (en) * | 2022-11-25 | 2023-03-07 | 浙江道明新材料有限公司 | High-dimensional-stability polyolefin release film and manufacturing method thereof |
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