CN112810273A - Release film containing 4-methyl-1-pentene polymer and preparation method thereof - Google Patents
Release film containing 4-methyl-1-pentene polymer and preparation method thereof Download PDFInfo
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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
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/06—Embossing
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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
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/18—Handling of layers or the laminate
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- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/18—Handling of layers or the laminate
- B32B38/1808—Handling of layers or the laminate characterised by the laying up of the layers
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- 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
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- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
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- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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Abstract
The invention discloses a release film containing 4-methyl-1-pentene polymer, which is characterized by comprising an outer film layer, a core film layer and an inner film layer from top to bottom in sequence; the outer membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of (3-5) to 1; the core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100 (5-10); the inner membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 1 (2-4). The invention also discloses a preparation method of the release film containing the 4-methyl-1-pentene polymer. The release film containing the 4-methyl-1-pentene polymer disclosed by the invention is good in release property, high temperature resistance, weather resistance and flame retardance, good in comprehensive performance and performance stability and excellent in mechanical property.
Description
Technical Field
The invention relates to the technical field of film materials, in particular to a release film containing 4-methyl-1-pentene polymer and a preparation method thereof.
Background
With the progress of electronic technology, electronic products are gradually developed to high density, miniaturization and high reliability, and in the preparation process, flexible circuit boards with high precision, good stability and high reliability are often required. Research and development of the flexible circuit board drives rapid development of the release film, and the release film also provides good performance support for manufacturing the flexible circuit board. Release the type membrane and be indispensable in the current process of soft flexible circuit board production, can effectively reduce the excessive influence of gluing to the finished product yield of flexible circuit board of protection film laminating process from the use of type membrane. The development and utilization of the release film with excellent comprehensive performance have very important significance for promoting the development of the flexible circuit board technology and even the whole electronic technology.
The release film is a film with a distinguishable surface, and the release film has no viscosity or slight viscosity after being contacted with a specific material under a limited condition, and in general, in order to increase the release force of the plastic film, the plastic film is subjected to plasma treatment, fluorine coating or silicon coating release agent on the surface layer of the film material, so that the release film can show extremely light and stable release force for various organic pressure-sensitive adhesives. The traditional release film has poor performance, and particularly has the phenomenon of glue leakage in the pressing process at high temperature. In the course of working at flexible circuit board, when the phenomenon of leaking glue takes place, the cull can glue on the circuit board, is difficult to clear away, and at this moment, clear away the cull and can increase manufacturing cost. More seriously, the residual glue can cause poor contact of the golden fingers, which can bring serious adverse effects to the performance of the circuit board. In addition, release films on the market are more or less prone to deformation after being stretched; cannot withstand higher temperatures; the wound release film is easy to adhere together and difficult to separate out; the release property, the high temperature resistance, the weather resistance and the flame retardance need to be further improved.
The Chinese invention patent with the application number of 201711444161.X discloses a release film. The release film sequentially comprises an upper release layer, a functional layer and a lower release layer. The release film provided by the invention has small release force and excellent easy-to-peel property and bonding property; meanwhile, the release film provided by the invention is a double-sided release film with different release forces; in addition, the release film disclosed by the invention has good flame retardance and ultraviolet resistance, is easy to transport and store, does not need coating, is simple in process and is suitable for production of high-requirement printed circuit boards. However, each layer of the release film contains organic and inorganic components with poor compatibility, and the types and the amounts of the inorganic additive components are large, so that the release film is easy to have the phenomena of poor performance stability and inorganic component extravasation in the storage and use processes, and the quality of printed circuit board products is influenced.
Therefore, it is an urgent problem to be solved by researchers in the industry how to provide a release film containing 4-methyl-1-pentene polymer, which has good release property, high temperature resistance, weather resistance and flame retardance, good comprehensive performance and performance stability, and excellent mechanical property.
Disclosure of Invention
The invention mainly aims to provide a release film containing 4-methyl-1-pentene polymer, which has good release property, high temperature resistance, weather resistance and flame retardance, good comprehensive performance and performance stability and excellent mechanical property; meanwhile, the invention also provides a preparation method of the release film containing the 4-methyl-1-pentene polymer, and the preparation method is simple and feasible, has small dependence on equipment, high preparation efficiency and finished product qualification rate, and is suitable for industrial production.
In order to achieve the above object, the present invention provides a release film containing 4-methyl-1-pentene polymer, which is characterized by comprising, from top to bottom, an outer film layer, a core film layer and an inner film layer; the outer membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of (3-5) to 1; the core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100 (5-10); the inner membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 1 (2-4).
Preferably, the thickness ratio of the outer membrane layer, the core membrane layer and the inner membrane layer is 1 (4-6) to 1.
Preferably, the preparation method of the 4-methyl-1-pentene polymer grafted and modified by the probenazole comprises the following steps: uniformly mixing the probenazole, the 4-methyl-1-pentene polymer and the peroxide initiator to obtain a mixture, and adding the mixture into a double-screw extruder for melt extrusion to obtain the probenazole grafted and modified 4-methyl-1-pentene polymer.
Preferably, the mass ratio of the probenazole to the 4-methyl-1-pentene polymer to the peroxide initiator is (0.1-0.2) to (2-3) to (0.001-0.002).
Preferably, the peroxide initiator is one or a mixture of several of tert-butyl peroxybenzoate, dicyclohexyl peroxydicarbonate and lauroyl peroxide which are mixed according to any proportion.
Preferably, the temperature of the melt extrusion is 260-280 ℃.
Preferably, the 4-methyl-1-pentene polymer comprises a homopolymer of 4-methyl-1-pentene and/or a copolymer of 4-methyl-1-pentene and an olefin having 2 to 20 carbon atoms other than 4-methyl-1-pentene.
Preferably, the olefin having 2 to 20 carbon atoms other than 4-methyl-1-pentene is at least one of 1-octene, 1-decene, 1-tetradecene, and 1-octadecene.
Preferably, the preparation method of the probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer comprises the following steps: adding probenazole, allylpentafluorobenzene, 2, 4-diphenyl-4-methyl-1-pentene and an initiator into a high-boiling-point solvent, stirring and reacting for 4-6 hours at 65-75 ℃ under an inert gas atmosphere, precipitating in water, washing the precipitated polymer for 3-6 times by using ethanol, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the probenazole/allylpentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer.
Preferably, the mass ratio of the allylbenzothiazole to the allylpentafluorobenzene to the 2, 4-diphenyl-4-methyl-1-pentene to the initiator to the high boiling point solvent is 1 (1-2) to 3-5 (0.06-0.08) to 30-40.
Preferably, the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide; the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the hyperbranched polyethylene fiber is prepared by the method of patent example 1 of Chinese invention with application number of 201410250304.3, and has a diameter of 1-3 μm and a length of 3-6 mm.
Another object of the present invention is to provide a method for preparing a release film containing 4-methyl-1-pentene polymer, comprising the steps of:
step S1, respectively granulating, melting and extruding the raw materials of the outer film layer, the core film layer and the inner film layer, and then carrying out tape casting and sheet casting treatment;
step S2, adjusting thickness by longitudinal drawing, superposing, and embossing the outer surface of the outer film layer or the inner film layer through an embossing roller;
and step S3, heat setting to obtain the release film containing the 4-methyl-1-pentene polymer.
Preferably, the heat setting temperature is 60-80 ℃.
Due to the application of the technical scheme, the invention has the following beneficial effects:
(1) the preparation method of the release film containing the 4-methyl-1-pentene polymer, disclosed by the invention, is simple and feasible, has small dependence on equipment and high preparation efficiency and finished product qualification rate, and is suitable for industrial production.
(2) The release film containing the 4-methyl-1-pentene polymer disclosed by the invention overcomes the defects that the traditional release film is poor in performance, and particularly the phenomenon of glue leakage occurs in the pressing process at a higher temperature. In the processing process of the flexible circuit board, when glue leakage occurs, residual glue can be adhered to the circuit board and is difficult to remove, at the moment, the removal of the residual glue can increase the manufacturing cost, and more seriously, the residual glue can cause poor contact of golden fingers, so that the defect of serious adverse effect can be brought to the performance of the circuit board; the problem that release films on the market are easy to deform after being stretched more or less is also solved; cannot withstand higher temperatures; the wound release film is easy to adhere together and difficult to separate out; the release film containing the 4-methyl-1-pentene polymer has the defects that the release property, the high temperature resistance, the weather resistance and the flame retardance need to be further improved, and the release film containing the 4-methyl-1-pentene polymer has good release property, high temperature resistance, weather resistance and flame retardance, good comprehensive performance and performance stability and excellent mechanical property through the synergistic effect of all the components and the film layer.
(3) The release film containing the 4-methyl-1-pentene polymer disclosed by the invention sequentially comprises an outer film layer, a core film layer and an inner film layer from top to bottom, and 4-methyl-1-pentene polymer components are contained among the layers, so that the layers are tightly bonded and are not easy to delaminate; the outer mold layer is prepared by blending 4-methyl-1-pentene polymer and probenazole graft modified 4-methyl-1-pentene polymer according to the mass ratio of (3-5) to 1; through the addition of the 4-methyl-1-pentene polymer modified by the allyl benzothiazole graft, the release performance is better, and the high-temperature resistance, the weather resistance and the flame retardance are better. The 4-methyl-1-pentene polymer and the 4-methyl-1-pentene polymer grafted and modified by the probenazole both contain 4-methyl-1-pentene polymer structural units, so that the 4-methyl-1-pentene polymer and the probenazole have good compatibility and good performance stability.
(4) The invention discloses a release film containing 4-methyl-1-pentene polymer, wherein a core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100 (5-10); due to the addition of the hyperbranched polyethylene fibers, the mechanical and mechanical properties of the film are improved; the hyperbranched structure can improve the compatibility between the hyperbranched structure and the copolymer; the structural unit of the copolymer contains 2, 4-diphenyl-4-methyl-1-pentene and probenazole, so that the adhesive force between the copolymer and the outer membrane layer and between the copolymer and the inner membrane layer is enhanced; under the multiple actions of electronic effect, steric effect and conjugation effect, the copolymer prepared by copolymerization of all comonomers has good comprehensive performance, excellent release property and weather resistance, easy storage, difficult yellowing, good mechanical strength in high-temperature use and excellent flame-retardant and ultraviolet-resistant performance.
(5) According to the release film containing the 4-methyl-1-pentene polymer, the whole film layer structure is free of inorganic components, the compatibility problem is avoided, and further the phase separation phenomenon is avoided, so that the performance stability is good; the double-sided release film is adopted, the release force is improved without adopting a surface coating treatment method, the risk of silicon transfer does not exist, residual glue is left during stripping, and the pollution and the production cost are reduced.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
In the embodiment of the invention, the raw materials are all purchased commercially; the hyperbranched polyethylene fiber is prepared by the method in the embodiment 1 of the Chinese patent with the application number of 201410250304.3.
Example 1
A release film containing 4-methyl-1-pentene polymer is characterized by comprising an outer film layer, a core film layer and an inner film layer from top to bottom in sequence; the outer membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 3: 1; the core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100: 5; the inner membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 1: 2; the thickness ratio of the outer film layer to the core film layer to the inner film layer is 1:4: 1.
The preparation method of the 4-methyl-1-pentene polymer grafted and modified by probenazole comprises the following steps: uniformly mixing the probenazole, the 4-methyl-1-pentene polymer and the peroxide initiator to obtain a mixture, and adding the mixture into a double-screw extruder for melt extrusion to obtain the probenazole grafted and modified 4-methyl-1-pentene polymer.
The mass ratio of the probenazole to the 4-methyl-1-pentene polymer to the peroxide initiator is 0.1:2: 0.001; the peroxide initiator is tert-butyl peroxybenzoate; the temperature of the melt extrusion is 260 ℃; the 4-methyl-1-pentene polymer comprises a homopolymer of 4-methyl-1-pentene.
The preparation method of the probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer comprises the following steps: adding probenazole, allylpentafluorobenzene, 2, 4-diphenyl-4-methyl-1-pentene and an initiator into a high-boiling-point solvent, stirring and reacting for 4 hours at 65 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 3 times by using ethanol, and finally drying in a vacuum drying oven at 85 ℃ to constant weight to obtain the probenazole/allylpentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer.
The mass ratio of the probenazole to the allyl pentafluorobenzene to the 2, 4-diphenyl-4-methyl-1-pentene to the initiator to the high-boiling-point solvent is 1:1:3:0.06: 30; the initiator is azobisisobutyronitrile; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen.
The diameter of the hyperbranched polyethylene fiber is 1 mu m, and the length of the hyperbranched polyethylene fiber is 3 mm.
The preparation method of the release film containing the 4-methyl-1-pentene polymer is characterized by comprising the following steps:
step S1, respectively granulating, melting and extruding the raw materials of the outer film layer, the core film layer and the inner film layer, and then carrying out tape casting and sheet casting treatment;
step S2, adjusting thickness by longitudinal drawing, superposing, and embossing the outer surface of the outer film layer or the inner film layer through an embossing roller;
step S3, heat setting to obtain a release film containing the 4-methyl-1-pentene polymer; the heat-setting temperature was 60 ℃.
Example 2
A release film containing 4-methyl-1-pentene polymer is characterized by comprising an outer film layer, a core film layer and an inner film layer from top to bottom in sequence; the outer membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 3.5: 1; the core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100: 6; the inner membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 1: 2.5; the thickness ratio of the outer film layer to the core film layer to the inner film layer is 1:4.5: 1.
The preparation method of the 4-methyl-1-pentene polymer grafted and modified by probenazole comprises the following steps: uniformly mixing probenazole, 4-methyl-1-pentene polymer and peroxide initiator to obtain a mixture, and adding the mixture into a double-screw extruder for melt extrusion to obtain probenazole grafted and modified 4-methyl-1-pentene polymer; the mass ratio of the probenazole to the 4-methyl-1-pentene polymer to the peroxide initiator is 0.13:2.2: 0.0013; the peroxide initiator is dicyclohexyl peroxydicarbonate; the melt extrusion temperature was 265 ℃.
The 4-methyl-1-pentene polymer is a polymer prepared by copolymerizing 4-methyl-1-pentene and 1-octene according to a mass ratio of 3: 5.
The preparation method of the probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer comprises the following steps: adding probenazole, allylpentafluorobenzene, 2, 4-diphenyl-4-methyl-1-pentene and an initiator into a high-boiling-point solvent, stirring and reacting for 4.5 hours at 67 ℃ in an inert gas atmosphere, precipitating in water, washing the precipitated polymer for 4 times by using ethanol, and finally drying in a vacuum drying oven at 87 ℃ to constant weight to obtain a probenazole/allylpentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer; the mass ratio of the probenazole to the allyl pentafluorobenzene to the 2, 4-diphenyl-4-methyl-1-pentene to the initiator to the high-boiling-point solvent is 1:1.2:3.5:0.065: 33; the initiator is azobisisoheptonitrile; the high boiling point solvent is N, N-dimethylformamide; the inert gas is helium.
The diameter of the hyperbranched polyethylene fiber is 1.5 mu m, and the length of the hyperbranched polyethylene fiber is 4 mm.
The preparation method of the release film containing the 4-methyl-1-pentene polymer is characterized by comprising the following steps:
step S1, respectively granulating, melting and extruding the raw materials of the outer film layer, the core film layer and the inner film layer, and then carrying out tape casting and sheet casting treatment;
step S2, adjusting thickness by longitudinal drawing, superposing, and embossing the outer surface of the outer film layer or the inner film layer through an embossing roller;
step S3, heat setting to obtain a release film containing the 4-methyl-1-pentene polymer; the heat-setting temperature was 65 ℃.
Example 3
A release film containing 4-methyl-1-pentene polymer is characterized by comprising an outer film layer, a core film layer and an inner film layer from top to bottom in sequence; the outer membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 4: 1; the core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100: 7.5; the inner membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 1: 3; the thickness ratio of the outer film layer to the core film layer to the inner film layer is 1:5: 1.
The preparation method of the 4-methyl-1-pentene polymer grafted and modified by probenazole comprises the following steps: uniformly mixing probenazole, 4-methyl-1-pentene polymer and peroxide initiator to obtain a mixture, and adding the mixture into a double-screw extruder for melt extrusion to obtain probenazole grafted and modified 4-methyl-1-pentene polymer; the mass ratio of the probenazole to the 4-methyl-1-pentene polymer to the peroxide initiator is 0.15:2.5: 0.0015; the peroxide initiator is lauroyl peroxide; the melt extrusion temperature was 270 ℃.
The 4-methyl-1-pentene polymer is a copolymer formed by copolymerizing 4-methyl-1-pentene, 1-decene and 1-tetradecene according to the mass ratio of 1:3: 2.
The preparation method of the probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer comprises the following steps: adding probenazole, allylpentafluorobenzene, 2, 4-diphenyl-4-methyl-1-pentene and an initiator into a high-boiling-point solvent, stirring and reacting for 5 hours at 70 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 5 times by using ethanol, and finally drying in a vacuum drying oven at 90 ℃ to constant weight to obtain a probenazole/allylpentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer; the mass ratio of the probenazole to the allyl pentafluorobenzene to the 2, 4-diphenyl-4-methyl-1-pentene to the initiator to the high-boiling-point solvent is 1:1.5:4:0.07: 35; the initiator is azobisisobutyronitrile; the high boiling point solvent is N, N-dimethylacetamide; the inert gas is neon.
The diameter of the hyperbranched polyethylene fiber is 2 mu m, and the length of the hyperbranched polyethylene fiber is 4.5 mm.
The preparation method of the release film containing the 4-methyl-1-pentene polymer is characterized by comprising the following steps:
step S1, respectively granulating, melting and extruding the raw materials of the outer film layer, the core film layer and the inner film layer, and then carrying out tape casting and sheet casting treatment;
step S2, adjusting thickness by longitudinal drawing, superposing, and embossing the outer surface of the outer film layer or the inner film layer through an embossing roller;
step S3, heat setting to obtain a release film containing the 4-methyl-1-pentene polymer; the heat-setting temperature was 70 ℃.
Example 4
A release film containing 4-methyl-1-pentene polymer is characterized by comprising an outer film layer, a core film layer and an inner film layer from top to bottom in sequence; the outer membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 4.5: 1; the core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100: 9; the inner membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 1: 3.5; the thickness ratio of the outer film layer to the core film layer to the inner film layer is 1:5.5: 1.
The preparation method of the 4-methyl-1-pentene polymer grafted and modified by probenazole comprises the following steps: uniformly mixing probenazole, 4-methyl-1-pentene polymer and peroxide initiator to obtain a mixture, and adding the mixture into a double-screw extruder for melt extrusion to obtain probenazole grafted and modified 4-methyl-1-pentene polymer; the mass ratio of the probenazole to the 4-methyl-1-pentene polymer to the peroxide initiator is 0.18:2.8: 0.0019; the peroxide initiator is formed by mixing tert-butyl peroxybenzoate, dicyclohexyl peroxydicarbonate and lauroyl peroxide according to the mass ratio of 1:3: 5; the melt extrusion temperature was 275 ℃.
The 4-methyl-1-pentene polymer is a homopolymer of 4-methyl-1-pentene.
The preparation method of the probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer comprises the following steps: adding probenazole, allylpentafluorobenzene, 2, 4-diphenyl-4-methyl-1-pentene and an initiator into a high-boiling-point solvent, stirring and reacting for 5.5 hours at 73 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 5 times by using ethanol, and finally drying in a vacuum drying oven at 93 ℃ to constant weight to obtain a probenazole/allylpentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer; the mass ratio of the probenazole to the allyl pentafluorobenzene to the 2, 4-diphenyl-4-methyl-1-pentene to the initiator to the high-boiling-point solvent is 1:1.8:4.5:0.075: 38; the initiator is formed by mixing azodiisobutyronitrile and azodiisoheptonitrile according to the mass ratio of 3: 5; the high boiling point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide according to a mass ratio of 2:4: 5; the inert gas is argon.
The diameter of the hyperbranched polyethylene fiber is 2.5 mu m, and the length of the hyperbranched polyethylene fiber is 5.5 mm.
The preparation method of the release film containing the 4-methyl-1-pentene polymer is characterized by comprising the following steps:
step S1, respectively granulating, melting and extruding the raw materials of the outer film layer, the core film layer and the inner film layer, and then carrying out tape casting and sheet casting treatment;
step S2, adjusting thickness by longitudinal drawing, superposing, and embossing the outer surface of the outer film layer or the inner film layer through an embossing roller;
step S3, heat setting to obtain a release film containing the 4-methyl-1-pentene polymer; the heat-setting temperature was 77 ℃.
Example 5
A release film containing 4-methyl-1-pentene polymer is characterized by comprising an outer film layer, a core film layer and an inner film layer from top to bottom in sequence; the outer membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 5: 1; the core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100: 10; the inner membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 1: 4; the thickness ratio of the outer film layer to the core film layer to the inner film layer is 1:6: 1.
The preparation method of the 4-methyl-1-pentene polymer grafted and modified by probenazole comprises the following steps: uniformly mixing probenazole, 4-methyl-1-pentene polymer and peroxide initiator to obtain a mixture, and adding the mixture into a double-screw extruder for melt extrusion to obtain probenazole grafted and modified 4-methyl-1-pentene polymer; the mass ratio of the probenazole to the 4-methyl-1-pentene polymer to the peroxide initiator is 0.2:3: 0.002; the peroxide initiator is tert-butyl peroxybenzoate; the melt extrusion temperature was 280 ℃.
The 4-methyl-1-pentene polymer is a homopolymer of 4-methyl-1-pentene.
The preparation method of the probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer comprises the following steps: adding probenazole, allylpentafluorobenzene, 2, 4-diphenyl-4-methyl-1-pentene and an initiator into a high-boiling-point solvent, stirring and reacting for 6 hours at 75 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 6 times by using ethanol, and finally drying in a vacuum drying oven at 95 ℃ to constant weight to obtain a probenazole/allylpentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer; the mass ratio of the probenazole to the allyl pentafluorobenzene to the 2, 4-diphenyl-4-methyl-1-pentene to the initiator to the high-boiling-point solvent is 1:2:5:0.08: 40; the initiator is azobisisobutyronitrile; the high boiling point solvent is N, N-dimethylformamide; the inert gas is nitrogen.
The diameter of the hyperbranched polyethylene fiber is 3 mu m, and the length of the hyperbranched polyethylene fiber is 6 mm.
The preparation method of the release film containing the 4-methyl-1-pentene polymer is characterized by comprising the following steps:
step S1, respectively granulating, melting and extruding the raw materials of the outer film layer, the core film layer and the inner film layer, and then carrying out tape casting and sheet casting treatment;
step S2, adjusting thickness by longitudinal drawing, superposing, and embossing the outer surface of the outer film layer or the inner film layer through an embossing roller;
step S3, heat setting to obtain a release film containing the 4-methyl-1-pentene polymer; the heat-setting temperature was 80 ℃.
Comparative example 1
The invention provides a release film containing 4-methyl-1-pentene polymer, the formula and the preparation method are similar to those of example 1, except that no probenazole is added to graft and modify the 4-methyl-1-pentene polymer.
Comparative example 2
The invention provides a release film containing 4-methyl-1-pentene polymer, the formula and the preparation method are similar to those of example 1, except that hyperbranched polyethylene fibers are not added.
Comparative example 3
The present invention provides a release film containing 4-methyl-1-pentene polymer, the formulation and preparation method thereof are similar to those of example 1, except that allyl pentafluorobenzene is not added in the preparation process of the allyl benzothiazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer.
In order to further illustrate the beneficial technical effects of the embodiments of the present invention, the release film containing 4-methyl-1-pentene polymer in each example was subjected to the relevant performance test, and the test results are shown in table 1; the test method is as follows:
1. testing the glue resistance: the release film is used for laminating the flexible circuit board, the laminating condition is 180 ℃, preheating is carried out for 10s, laminating is carried out for 120s, the glue overflow amount is not more than 1%, and the glue resistance is good if the glue is qualified; the glue overflow amount is more than 1 percent, and the glue resistance is poor if the glue is unqualified.
2. And (3) testing high-temperature resistance: the release film is used for laminating the flexible circuit board at 180 ℃, and no intermediate film layer substance flows out from the edge of the release film after lamination, so that the high-temperature resistance is good; after pressing, the material of the intermediate film layer flows out from the edge of the release film, so that the high temperature resistance is poor.
3. And (3) testing release performance: the release film is used for laminating the flexible circuit board at 180 ℃, after lamination, the release film can be easily peeled off, and the surface of the circuit board has no residual glue, so that the release performance is good; after lamination, the release is difficult to peel or residual glue is on the surface of the circuit board, so that the release performance is poor.
4. Mechanical properties: the test specimens were dumbbell-shaped, 0.5mm thick, 4.5mm wide, 20.0mm gauge length, and 5.0mm/min tensile rate, according to ASTM D638-2003.
5. Flame retardancy: tested according to GB/T2406.2-2009.
TABLE 1
| Item | Glue resistance | High temperature resistance | Release property | Modulus of elasticity/MPa | LIO/％ |
| Example 1 | Good taste | Good taste | Good taste | 248 | 30 |
| Example 2 | Good taste | Good taste | Good taste | 252 | 31 |
| Example 3 | Good taste | Good taste | Good taste | 257 | 33 |
| Example 4 | Good taste | Good taste | Good taste | 260 | 34 |
| Example 5 | Good taste | Good taste | Good taste | 262 | 34 |
| Comparative example 1 | Difference (D) | Difference (D) | Difference (D) | 206 | 26 |
| Comparative example 2 | Difference (D) | Difference (D) | Difference (D) | 190 | 29 |
| Comparative example 3 | Difference (D) | Difference (D) | Difference (D) | 212 | 28 |
As can be seen from Table 1, the release film containing 4-methyl-1-pentene polymer disclosed in the embodiment of the invention has excellent mechanical properties, high temperature resistance, release property and glue resistance, and better flame retardance, which is the result of the synergistic effect of the film layer structures of the raw materials.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A release film containing 4-methyl-1-pentene polymer is characterized by comprising an outer film layer, a core film layer and an inner film layer from top to bottom in sequence; the outer membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of (3-5) to 1; the core film layer is prepared by blending probenazole/allyl pentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer and hyperbranched polyethylene fibers according to the mass ratio of 100 (5-10); the inner membrane layer is prepared by blending 4-methyl-1-pentene polymer and probenazole grafted and modified 4-methyl-1-pentene polymer according to the mass ratio of 1 (2-4).
2. The release film containing the 4-methyl-1-pentene polymer as claimed in claim 1, wherein the thickness ratio of the outer film layer, the core film layer and the inner film layer is 1 (4-6): 1.
3. The release film containing 4-methyl-1-pentene polymer according to claim 1, wherein the preparation method of the 4-methyl-1-pentene polymer by the allyl benzothiazole graft modification comprises the following steps: uniformly mixing the probenazole, the 4-methyl-1-pentene polymer and the peroxide initiator to obtain a mixture, and adding the mixture into a double-screw extruder for melt extrusion to obtain the probenazole grafted and modified 4-methyl-1-pentene polymer.
4. The release film comprising 4-methyl-1-pentene polymer as claimed in claim 3, wherein the mass ratio of the probenazole to the 4-methyl-1-pentene polymer to the peroxide initiator is (0.1-0.2): (2-3): (0.001-0.002).
5. The release film containing 4-methyl-1-pentene polymer according to claim 3, wherein the peroxide initiator is one or more of tert-butyl peroxybenzoate, dicyclohexyl peroxydicarbonate and lauroyl peroxide, which are mixed in any proportion; the temperature of the melt extrusion is 260-280 ℃.
6. The release film according to claim 1, wherein the 4-methyl-1-pentene polymer comprises a homopolymer of 4-methyl-1-pentene and/or a copolymer of 4-methyl-1-pentene and an olefin having 2 to 20 carbon atoms other than 4-methyl-1-pentene; the olefin having 2-20 carbon atoms other than 4-methyl-1-pentene is at least one of 1-octene, 1-decene, 1-tetradecene and 1-octadecene.
7. The release film according to claim 1, wherein the process for preparing the copolymer of allylbenzothiazole/allylpentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene comprises the following steps: adding probenazole, allylpentafluorobenzene, 2, 4-diphenyl-4-methyl-1-pentene and an initiator into a high-boiling-point solvent, stirring and reacting for 4-6 hours at 65-75 ℃ under an inert gas atmosphere, precipitating in water, washing the precipitated polymer for 3-6 times by using ethanol, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the probenazole/allylpentafluorobenzene/2, 4-diphenyl-4-methyl-1-pentene copolymer.
8. The release film containing 4-methyl-1-pentene polymer according to claim 7, wherein the mass ratio of the allylbenzothiazole, the allylpentafluorobenzene, the 2, 4-diphenyl-4-methyl-1-pentene, the initiator and the high boiling point solvent is 1 (1-2): 3-5): 0.06-0.08): 30-40; the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N, N-dimethylacetamide; the inert gas is any one of nitrogen, helium, neon and argon.
9. The release film according to claim 7, wherein the hyperbranched polyethylene fibers have a diameter of 1-3 μm and a length of 3-6 mm.
10. A method for preparing a release film containing 4-methyl-1-pentene polymer according to any one of claims 1 to 9, comprising the steps of:
step S1, respectively granulating, melting and extruding the raw materials of the outer film layer, the core film layer and the inner film layer, and then carrying out tape casting and sheet casting treatment;
step S2, adjusting thickness by longitudinal drawing, superposing, and embossing the outer surface of the outer film layer or the inner film layer through an embossing roller;
step S3, heat setting to obtain a release film containing the 4-methyl-1-pentene polymer; the temperature of the heat setting is 60-80 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114603955A (en) * | 2022-05-11 | 2022-06-10 | 宁波长阳科技股份有限公司 | Three-layer composite release film for 3D printing process and preparation method thereof |
| CN115534461A (en) * | 2022-11-29 | 2022-12-30 | 苏州博理新材料科技有限公司 | Five-layer release film and preparation method and application thereof |
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| CN115534461A (en) * | 2022-11-29 | 2022-12-30 | 苏州博理新材料科技有限公司 | Five-layer release film and preparation method and application thereof |
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