CN114311915B - A multi-layer high temperature resistant fluorine-containing release film and preparation method thereof - Google Patents
A multi-layer high temperature resistant fluorine-containing release film and preparation method thereof Download PDFInfo
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 34
- 239000011737 fluorine Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005266 casting Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000001125 extrusion Methods 0.000 claims abstract description 12
- 239000000155 melt Substances 0.000 claims description 23
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 claims description 19
- 229920000515 polycarbonate Polymers 0.000 claims description 12
- 239000004417 polycarbonate Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229920000178 Acrylic resin Polymers 0.000 claims description 9
- 239000004925 Acrylic resin Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 5
- 239000004642 Polyimide Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000000691 measurement method Methods 0.000 claims description 4
- 229920001721 polyimide Polymers 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 17
- 229920000728 polyester Polymers 0.000 abstract description 15
- 239000011347 resin Substances 0.000 abstract description 15
- 229920005989 resin Polymers 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 13
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 2
- 238000011109 contamination Methods 0.000 abstract 1
- 239000013538 functional additive Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 138
- 229920000139 polyethylene terephthalate Polymers 0.000 description 10
- 239000005020 polyethylene terephthalate Substances 0.000 description 10
- 238000012545 processing Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 8
- -1 polytetrafluoroethylene, ethylene-tetrafluoroethylene copolymer Polymers 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000003475 lamination Methods 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- QHSJIZLJUFMIFP-UHFFFAOYSA-N ethene;1,1,2,2-tetrafluoroethene Chemical compound C=C.FC(F)=C(F)F QHSJIZLJUFMIFP-UHFFFAOYSA-N 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- PEVRKKOYEFPFMN-UHFFFAOYSA-N 1,1,2,3,3,3-hexafluoroprop-1-ene;1,1,2,2-tetrafluoroethene Chemical compound FC(F)=C(F)F.FC(F)=C(F)C(F)(F)F PEVRKKOYEFPFMN-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- Extrusion Moulding Of Plastics Or The Like (AREA)
- Laminated Bodies (AREA)
Abstract
本发明属于离型膜技术领域，特别是指一种多层耐高温含氟离型膜及制备方法。本发明的含氟离型膜包括第一离型层、结构层和第二离型层，离型膜通过多层共挤流延方式制成，结构层材料包括聚酯类聚合物、氟树脂和功能助剂，两层离型层包括含氟类树脂，本发明的离型层具有良好的耐高温性和抗拉伸强度，结构层与离型层间不含粘结剂，制备工艺简单，并避免了现有技术中粘结剂对离型层的污染的问题，实现了离型膜的耐高温、抗拉、成型工艺简单的技术效果。The present invention belongs to the technical field of release films, and in particular refers to a multi-layer high-temperature resistant fluorine-containing release film and a preparation method thereof. The fluorine-containing release film of the present invention comprises a first release layer, a structural layer and a second release layer, and the release film is made by a multi-layer co-extrusion casting method, and the structural layer material comprises a polyester polymer, a fluorine resin and a functional additive, and the two release layers comprise a fluorine-containing resin. The release layer of the present invention has good high temperature resistance and tensile strength, and there is no adhesive between the structural layer and the release layer. The preparation process is simple, and the problem of contamination of the release layer by the adhesive in the prior art is avoided, so as to achieve the technical effects of high temperature resistance, tensile resistance and simple molding process of the release film.
Description
Technical Field
The invention belongs to the technical field of films, and particularly relates to a multilayer high-temperature-resistant fluorine-containing release film and a preparation method thereof.
Background
With the development of the information age, electronic devices tend to be functionalized and diversified, and requirements on release films are also higher and higher, so that release films with excellent performance are indispensable in the manufacturing process of electronic accessories.
Chinese patent CN211106113 (application No. 201921296084.2) provides an environment-friendly PET release film, which comprises a PET base layer, two stretch-resistant layers, two wear-resistant layers, and a PET release layer, but the temperature resistance and stretch-resistant properties are insufficient. The common release film base material is PP, PE, PET, and the release film is prepared by plasma treatment, fluorine coating treatment or a mode of coating a silicon release agent on the surface of the base material, and has the defects of insufficient extensibility, insufficient temperature resistance, easiness in pollution to electronic devices and the like. Chinese patent CN106042553a (application No. 201610408694.1) provides a high temperature resistant release film, in which the release layer is polymethylpentene and the support layer is polyolefin, but the film has too high elastic modulus, and wrinkles are easily generated in thermoforming of electronic devices. The fluorine-containing resin is good in temperature resistance and excellent in tensile property, and is increasingly researched when being applied to a release film, chinese patent CN111002667A (application number is 201911317773.1) provides a release film constructed by fluorine-containing resin and polyester materials, the release film comprises a first raw material, a second raw material and a third raw material, 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, the third raw material is a polyester material, and the three-layer ABC release film with a structure of a release layer-bonding layer-supporting layer is obtained through coextrusion by three extruders, and has good high temperature resistance and low thermal shrinkage rate, but the bonding material is used between the first layer and the third layer, and the lamination step is needed, so that the prepared release film is insufficient in tensile property and the application of the release film in the field of film materials is limited.
In summary, the conventional release film substrate has the defects of insufficient extensibility, insufficient temperature resistance, poor practicality and the like, and the adhesive layer is often required to be used as a transition layer due to poor compatibility between the fluorine-containing resin layer and the polyester layer in the release film, and is easy to remain on the release layer, so that pollution to the electronic device is possibly caused when the release film substrate is used for manufacturing and processing the electronic device, and therefore, in order to meet the practical application, the release film which does not need the adhesive layer and has good tensile property, high temperature resistance and environmental protection performance needs to be developed.
Disclosure of Invention
Aiming at the problems, the invention provides a high-temperature resistant fluorine-containing release film and a preparation method thereof, wherein the release film comprises a first release layer, a structural layer and a second release layer from bottom to top, the release film is prepared by a multilayer coextrusion casting mode, the structural layer comprises polyester polymers, fluororesin and functional auxiliary agents, the two release layers are the same or different and are fluorine-containing resins, the release layer has good high-temperature resistance and tensile strength, the structural layer and the release layer do not contain adhesive, the preparation process is simple, the problem of pollution of the adhesive to the release layer in the prior art is avoided, and the technical effects of high-temperature resistance, tensile resistance and simple forming process of the release film are realized.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The invention provides a multilayer high-temperature-resistant fluorine-containing release film which is characterized by comprising a first release layer, a structural layer and a second release layer, wherein the structural layer is arranged between the first release layer and the second release layer in a clamping manner, and the first release layer, the structural layer and the second release layer are manufactured into a three-layer release film by a multilayer coextrusion casting mode; the total thickness of the release film is 60-100 mu m, the thickness ratio of the structural layer is 60-75%, the thickness ratio of the first release layer is 10-25%, and the thickness ratio of the second release layer is 10-25%; the structural layer comprises the following components in percentage by mass: 76-87wt% of polyester polymer, 12-19wt% of fluororesin and 1-5wt% of compatilizer, wherein the first release layer and the second release layer comprise the same or different fluororesin.
The content of the fluororesin in the structural layer can be selected according to the viscosity of the mixed resin formed by mixing and granulating the fluororesin and the polyester polymer in a molten state, the content of the fluororesin in the structural layer is in a range of 12-19%, and an excessive ratio can lead to the reduction of the tensile strength and the reduction of the extensibility of the structural layer after the mixed resin is molten and extruded; too low a fluororesin content will result in poor adhesion between the structural layer and the first release layer, and between the structural layer and the second release layer.
Preferably, the polyester polymer comprises one or a mixture of a plurality of Polycarbonate (PC), polybutylene terephthalate (PBT), polyethylene naphthalate (PEN) and polyethylene terephthalate (PET), and preferably, the polyester polymer is PC or PET.
Preferably, the melt index of the polyester polymer is 5-20g/10min, the tensile strength is 40-70MPa, and the tensile modulus is 400-800MPa.
Preferably, the fluororesin is perfluoroethylene propylene copolymer (FEP) or ethylene-tetrafluoroethylene copolymer (ETFE)
Preferably, the melt index of the fluororesin is 5-20g/10min, the tensile strength is 20-50MPa, and the tensile modulus is 400-800MPa. Research shows that the molecular weight of the polymer is an important factor affecting the melt index, and the higher the molecular weight of the polymer, the higher the melt index. For ethylene-tetrafluoroethylene polymers, the larger the ratio of tetrafluoroethylene units in ETFE, the greater the melt index of the ETFE polymer. The melt index of the fluororesin is controlled in the range of 5-20g/10min, the excessive melt index causes more difficult processing, the smoothness and the flatness of the formed film are reduced, and the processing cost is increased.
The melt index measurement method of the polyester polymer is described in GB/T3682-2000, and the test conditions are as follows: the test temperature is 300 ℃ and the nominal load is 1.2kg; the melt index measurement method of the fluororesin is the same as GB/T3682-2000, and the test conditions are as follows: the test temperature was 297℃and the nominal load was 5kg.
The fluorine resin and most thermoplastic polymers lack of adhesiveness, the first release layer and the second release layer which take the fluorine resin as components have poor solid force with the structural layer which takes the polyester polymer as the main component, and the addition of the compatilizer in the structural layer can effectively improve the solid force between the structural layer and the release layer, so that the problem that the structural layer and the first release layer and the structural layer and the second release layer are peeled off in the shaping, cooling and traction processes after the forming is avoided.
The compatilizer comprises one or a mixture of a plurality of cyclic anhydride type, epoxy type and imide modified acrylic resin, and is preferably imide modified acrylic resin.
In the presence of the imide-modified acrylic resin, thermoplastic polyester polymer and fluororesin are mechanically kneaded and pelletized at high temperature to obtain a structural layer pellet. The tensile strength of the structural layer of the multilayer high-temperature-resistant fluorine-containing release film prepared by using the structural layer granules is obviously improved. The compatibilizers are intended to improve the properties of the structural layer by reducing the interfacial tension and by improving the phase interface between the polyester-based polymer and the fluororesin and the adhesion of both.
The invention also provides a preparation method of the multilayer high-temperature-resistant fluorine-containing release film, which is characterized by comprising the following steps of:
(1) The components of the structural layer are weighed according to the mass ratio and then mixed in a high-speed mixer, and then the structural layer granules are obtained after melt blending, extrusion, traction granulation and drying are carried out by a double-screw extruder.
(2) Preparing three extruders A, B, C, respectively adding fluororesin into the extruder A, C for extruding a first release layer and a second release layer of the release film, adding granules in the step (1) into the extruder B for extruding a structural layer of the release film, enabling melt extruded by the three extruders to enter and be compounded in a casting die head, preparing a multilayer high-temperature-resistant release film by shaping, cooling, traction and annealing the compounded multilayer melt, detecting and adjusting the thickness by an online thickness gauge, and winding a cut edge of the film to obtain a multilayer high-temperature-resistant release film product.
Preferably, the blending time in the step (1) is 2-10min, the extrusion temperature is 270-340 ℃, the screw speed is 15-80r/min, and the drying is carried out for 8h at 100 ℃ after traction granulation.
Preferably, in the step (2), the length-diameter ratio of the screw of the extruder A is 20-30, and the extruder A comprises four heating zone barrels, and the temperatures of the barrels are respectively set as follows: zone 1 220-340 ℃, zone 2 230-350 ℃, zone 3 230-360 ℃, zone 4 230-370 ℃.
Preferably, in the step (2), the length-diameter ratio of the screw of the extruder B is 25-30, and the extruder comprises four heating zone barrels, and the temperatures of the barrels are respectively set as follows: zone 1 210-340 ℃, zone 2 220-340 ℃, zone 3 220-350 ℃, zone 4 220-350 ℃.
Preferably, the process parameters of the extruder C in the step (2) are set to be the same as those of the extruder A.
Preferably, the casting die in the step (2) is a multi-runner in-mold composite casting die, and the temperature is set to be 250-370 ℃.
The one or more technical schemes provided by the invention have at least the following technical effects:
1. the release film prepared by the invention has good temperature resistance, excellent tensile property and no pollution.
2. The release film prepared by the invention has a three-layer structure as a whole, does not need an extra bonding layer and lamination step, has a simple molding process, has no solvent residue, and can not pollute an electronic device in the use process.
Detailed Description
The following specific examples are provided to further illustrate the invention. The raw materials used in the examples are all commercially available products. The tensile property test method of the multilayer high-temperature-resistant fluorine-containing release film refers to ISO 527-3 2018; heat shrinkage test method referring to GB/T12027-2004, the heat shrinkage of the etfe release layer was measured after 1 hour of constant temperature treatment in a 160 ℃ oven, and the heat shrinkage of the FEP release layer was measured after 1 hour of constant temperature treatment in a 210 ℃ oven.
Example 1
A multilayer high-temperature-resistant fluorine-containing release film comprises a first release layer, a structural layer and a second release layer from top to bottom. The structural layer comprises the following components in percentage by mass: ETFE:12%; PC:87%; fluoropolyimide modified acrylic resin: 1%. The thickness of the structural layer was 36. Mu.m. The first release layer and the second release layer are ETFE layers, and the thickness is 12 μm. The ETFE has a melt index of 5g/10min, a tensile strength of 20.0MPa and a tensile modulus of 400MPa. The melt index of PC was 5g/10min, the tensile strength was 40.0MPa, and the tensile modulus was 400MPa.
The preparation method of the release film comprises the following steps:
(1) The components of the structural layer are weighed according to the mass ratio and then mixed in a high-speed mixer for 4min, then are subjected to melt blending by a double-screw extruder, the extrusion temperature is controlled at 280 ℃, the screw rotation speed is 30r/min, and the structural layer is dried for 8h at 100 ℃ after traction granulation and sealing for standby.
(2) The extrusion casting film machine set comprises three extruders, wherein the extruders A and C are used for extruding two layers of outer release films, the extruder B is used for extruding a structural layer film, the melt extruded by the three-layer extruder passes through a multi-runner in-mold compound casting die head, the multi-layer melt after compounding is subjected to shaping, cooling, traction, annealing and other steps to prepare a multi-layer high-temperature-resistant release film, the thickness is detected and adjusted by an online thickness gauge, and the film is wound by cutting edges to obtain a multi-layer high-temperature-resistant release film product.
The preparation process parameters of the release film are as follows:
A extruder: the extruder for processing ETFE resin was a screw with an aspect ratio of 30 and a barrel with four heating zones, with a temperature set at 260 c for zone 1, 270 c for zone 2, 280 c for zone 3, and 290 c for zone 4. The thickness of the first release layer was adjusted to 12 μm.
B extruder: the extruder for processing the structural layer mixture material selects a screw with the length-diameter ratio of 25 and a charging barrel with four heating areas, wherein the temperature is set to 240 ℃ in a zone 1, 250 ℃ in a zone 2, 260 ℃ in a zone 3 and 270 ℃ in a zone 4. The extrusion thickness was adjusted to 36. Mu.m.
And the technological parameter setting of the extruder C is the same as that of the extruder A.
Multi-channel die head: the temperature was set to 295 ℃. And after each section of the equipment reaches a set temperature value and is kept for 0.5h, starting feeding production. The mechanical properties of each layer of the obtained release film are shown in Table 1.
Example 2
A multilayer high temperature resistant fluorine-containing release film as in example 1 except that the structural layer comprises the following components in mass fraction: ETFE:19%; PC:76%; fluoropolyimide modified acrylic resin: 5%. Wherein the melt index of ETFE is 20g/10min, the tensile strength is 50.0MPa, and the tensile modulus is 800MPa. The melt index of PC was 20g/10min, the tensile strength was 70.0MPa, and the tensile modulus was 800MPa. The preparation procedure of the release film of this example is the same as that of example 1, and the mechanical properties of each layer of the release film obtained are shown in table 1.
Example 3
A multilayer high-temperature-resistant fluorine-containing release film comprises a first release layer, a structural layer and a second release layer from top to bottom. The structural layer comprises the following components in percentage by mass: fluororesin ETFE:5%; polyethylene terephthalate (PET): 80%; 5% of fluorine polyimide modified acrylic resin. The thickness of the structural layer was 70. Mu.m. The first release layer and the second release layer are ETFE layers, and the thickness is 15 μm. The ETFE has a melt index of 10g/10min, a tensile strength of 35.0MPa and a tensile modulus of 430MPa. PET has a melt index of 10g/10min, a tensile strength of 40.0MPa and a tensile modulus of 450MPa.
The preparation steps of the release film are as follows:
(1) The components of the structural layer are weighed according to the mass ratio and then mixed in a high-speed mixer for 4min, then are subjected to melt blending by a double-screw extruder, the extrusion temperature is controlled at 270 ℃, the screw rotation speed is 30r/min, and the structural layer is dried for 8h at 100 ℃ after traction granulation and sealing for standby.
(2) The extrusion casting film machine set comprises three extruders, wherein the extruders A and C are used for extruding a first release film and a second release film, the extruder B is used for extruding a structural layer film, a melt extruded by the three-layer extruder passes through a multi-runner in-mold compound casting die head, the compound multi-layer melt is subjected to shaping, cooling, traction, annealing and other steps to prepare a multi-layer high-temperature-resistant release film, the thickness is detected and adjusted by an online thickness gauge, and the film is wound by cutting edges to obtain a multi-layer high-temperature-resistant release film product.
The preparation process parameters of the release film are as follows:
a extruder: the extruder for processing ETFE resin was a screw with an aspect ratio of 30 and a barrel with four heating zones, with a temperature set at 260 c for zone 1, 270 c for zone 2, 280 c for zone 3, and 290 c for zone 4. The film thickness was adjusted to 15 μm.
B extruder: the extruder for processing the structural layer mixture material selects a screw with the length-diameter ratio of 25 and a charging barrel with four heating areas, wherein the temperature is set to be 230 ℃ in a zone 1, 240 ℃ in a zone 2, 250 ℃ in a zone 3 and 260 ℃ in a zone 4. The film thickness was adjusted to 70 μm.
And the technological parameter setting of the extruder C is the same as that of the extruder A.
Multi-channel die head: the temperature was set in the range of 295 ℃. And after each section of the equipment reaches a set temperature value and is kept for 0.5h, starting feeding production. The mechanical properties of each layer of the obtained release film are shown in table 1.
Example 4
A multilayer high-temperature resistant fluorine-containing release film and a preparation method thereof are provided, wherein the release film comprises a first release layer, a structural layer and a second release layer from top to bottom in sequence. The structural layer is a mixed layer of 12% of fluorine resin FEP, 85% of Polycarbonate (PC) and 3% of fluorine polyimide modified acrylic resin, and the thickness is 70 mu m. The first release layer and the second release layer are FEP resin layers, and the thickness of the first release layer and the second release layer is 10 mu m and 15 mu m respectively. The FEP of the fluororesin has a melt index of 10g/10min, a tensile strength of 35.0MPa and a tensile modulus of 430MPa. The melt index of PC was 10g/10min, the tensile strength was 40.0MPa, and the tensile modulus was 450MPa.
The preparation method comprises the following steps:
(1) The components of the structural layer, namely, 12% of fluorine resin FEP, 85% of Polycarbonate (PC) and 3% of fluorine polyimide modified acrylic resin, are weighed according to mass ratio, mixed in a high-speed mixer for 4min, then melt-blended by a double-screw extruder, extruded at 340 ℃ and screw speed of 30r/min, dried at 100 ℃ for 8h after traction granulation, and sealed for later use.
(2) The extrusion casting film machine set comprises three extruders, wherein the extruders A and C are used for extruding a first release film and a second release film, the extruder B is used for extruding a structural layer film, a melt extruded by the three-layer extruder passes through a multi-runner in-mold compound casting die head, the compound multi-layer melt is subjected to shaping, cooling, traction, annealing and other steps to prepare a multi-layer high-temperature-resistant release film, the thickness is detected and adjusted by an online thickness gauge, and the film is wound by cutting edges to obtain a multi-layer high-temperature-resistant release film product.
The preparation process parameters of the release film are as follows:
A extruder: the extruder for processing FEP resin selects a screw with an aspect ratio of 30 and a barrel with four heating zones, the temperature is set to 330 c in zone 1, 340 c in zone 2, 350 c in zone 3, and 360 c in zone 4. The film thickness was adjusted to 10 μm.
B extruder: the extruder for processing the structural layer mixture material selects a screw with the length-diameter ratio of 25 and a charging barrel with four heating areas, wherein the temperature is set to 240 ℃ in a zone 1, 250 ℃ in a zone 2, 260 ℃ in a zone 3 and 270 ℃ in a zone 4. The film thickness was adjusted to 70 μm.
And the technological parameter setting of the extruder C is the same as that of the extruder A, and the thickness of the extruder C is 15 mu m.
Multi-channel die head: the temperature was set at 360 ℃. And after each section of the equipment reaches a set temperature value and is kept for 0.5h, starting feeding production.
The mechanical properties of each layer of the obtained release film are shown in table 1.
TABLE 1 mechanical Properties of structural layer, first Release layer, second Release layer of the Release film of the examples
| Project | Example 1 | Example 2 | Example 3 | Example 4 |
| Tensile Strength of structural layer/MPa | 30.8 | 48.9 | 28.7 | 31.2 |
| Tensile strength of first release layer/MPa | 18.5 | 46.7 | 36.2 | 34.7 |
| Second release layer tensile Strength/MPa | 19.3 | 47.9 | 35.4 | 33.5 |
| Elongation at break/% | 267 | 236 | 247 | 146 |
| Elongation at break/% | 282 | 228 | 254 | 137 |
| First release layer heat shrinkage/% | 2.2 | 2.4 | 2.3 | 2.1 |
| Second release layer heat shrinkage/% | 2.3 | 2.3 | 2.1 | 2.0 |
As shown in the table above, the release layer raw material of the high-temperature-resistant fluorine-containing release film prepared by the invention is ETFE or FEP material, and has excellent heat shrinkage performance and tensile performance. The release film is integrally of a three-layer structure formed by co-extrusion, no extra bonding layer or lamination step is needed, the forming process is simple, no solvent residue exists on the surface of the release layer, and the electronic device cannot be polluted in the use process. Meanwhile, the structural layer adopts polyester polymers to replace fluorine resin polymers, so that the cost of the release film material is reduced.
Claims (5)
1. The multilayer high-temperature-resistant fluorine-containing release film is characterized by comprising a first release layer, a structural layer and a second release layer, wherein the structural layer is arranged between the first release layer and the second release layer in a clamping manner, and the first release layer, the structural layer and the second release layer are manufactured into a three-layer release film in a multilayer coextrusion casting mode; the total thickness of the release film is 60-100 mu m, the thickness ratio of the structural layer is 60-75%, the thickness ratio of the first release layer is 10-25%, and the thickness ratio of the second release layer is 10-25%;
The structural layer comprises the following components in percentage by mass: 76% of polycarbonate, 19% of ethylene-tetrafluoroethylene copolymer and 5% of fluorine polyimide modified acrylic resin,
The first release layer and the second release layer are ethylene-tetrafluoroethylene copolymer,
The melt index of the polycarbonate is 20g/10min, the tensile strength is 70.0MPa, and the tensile modulus is 800MPa;
The melt index of the ethylene-tetrafluoroethylene copolymer is 20g/10min, the tensile strength is 50.0MPa, and the tensile modulus is 800MPa;
the melt index measurement method of the polycarbonate is described in GB/T3682-2000, and the test conditions are as follows: the test temperature is 300 ℃ and the nominal load is 1.2kg;
the melt index measurement method of the ethylene-tetrafluoroethylene copolymer is referred to GB/T3682-2000, and the test conditions are as follows: the test temperature was 297℃and the nominal load was 5kg.
2. The method for preparing the multilayer high temperature resistant fluorine-containing release film according to claim 1, comprising the steps of:
(1) Weighing the components of the structural layer according to the mass ratio, mixing in a high-speed mixer, and carrying out melt blending, extrusion, traction granulation and drying by a double-screw extruder to obtain structural layer granules;
(2) Preparing three extruders A, B, C, respectively adding ethylene-tetrafluoroethylene copolymer into the extruder A, C for extruding a first release layer and a second release layer of the release film, adding granules in the step (1) into the extruder B for extruding a structural layer of the release film, enabling melt extruded by the three extruders to enter and be compounded in a casting die head, preparing a multilayer high-temperature-resistant release film by shaping, cooling, traction and annealing the compounded multilayer melt, detecting and adjusting the thickness by an online thickness meter, cutting edges of the film, and rolling the film to obtain a multilayer high-temperature-resistant fluorine-containing release film product.
3. The preparation method according to claim 2, wherein the blending time in the step (1) is 2-10min, the extrusion temperature is 270-340 ℃, the screw rotation speed is 15-80r/min, and the drying is carried out at 100 ℃ for 8h after the traction granulation.
4. The method according to claim 2, wherein the extruder a in step (2) has a screw aspect ratio of 20 to 30, and comprises four heating zone barrels having temperatures set to: zone 1 220-340 ℃, zone 2 230-350 ℃, zone 3 230-360 ℃, zone 4 230-370 ℃; the length-diameter ratio of the screw of the extruder B is 25-30, and the extruder B comprises four heating zone charging barrels, wherein the temperatures of the charging barrels are respectively set as follows: zone 1 210-340 ℃, zone 2 220-340 ℃, zone 3 220-350 ℃, zone 4 220-350 ℃; the process parameters of extruder C are set as in extruder A.
5. The production method according to claim 2, wherein the casting die in step (2) is a multi-pass in-mold composite casting die, and the temperature is set to 250 to 370 ℃.
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