CN109466124B - Release film - Google Patents

Release film Download PDF

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CN109466124B
CN109466124B CN201711444161.XA CN201711444161A CN109466124B CN 109466124 B CN109466124 B CN 109466124B CN 201711444161 A CN201711444161 A CN 201711444161A CN 109466124 B CN109466124 B CN 109466124B
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release layer
release
release film
layer
carbon black
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CN109466124A (en
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金亚东
赵爽
杨承翰
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Ningbo Solartron Technology Co Ltd
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Ningbo Solartron Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00Layered 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
    • B32B7/04Interconnection of layers
    • B32B7/06Interconnection of layers permitting easy separation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/06Layered 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/18Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/32Layered products comprising a layer of synthetic resin comprising polyolefins
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/306Resistant to heat
    • B32B2307/3065Flame resistant or retardant, fire resistant or retardant
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/70Other properties
    • B32B2307/71Resistive to light or to UV
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00Electrical equipment
    • B32B2457/08PCBs, i.e. printed circuit boards

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  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

The invention relates to a protective film, in particular to a release film. The invention provides a release film, aiming at solving the problem of single release force of the existing 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.

Description

Release film
Technical Field
The invention relates to a protective film, in particular to a release film.
Background
The release film is widely applied to the manufacturing process of circuit boards in the electronic industry as a protective film, and the use of the release film can effectively reduce the product defects caused by the overflow of adhesives during the manufacturing of the circuit boards. The common release film mostly adopts a surface coating treatment method to improve the release force, so that the release film has good easy-to-peel property for meeting different viscosity requirements in the production process; however, the PET release film prepared by the surface coating method has the risk of silicon transfer in the using process, and is often accompanied with residual glue during stripping, which causes pollution to products and increases the cost of cleaning procedures. In addition, the traditional pressing mode of the circuit board can not meet the production requirements, most manufacturers begin to select Roll-to-Roll technology, and the requirements on the flame retardance, the ultraviolet resistance, the release property and the like of the release film are further improved. And the release force of the existing release film is single, so that the requirement of different downstream manufacturers on the release force cannot be met.
TPX has good heat resistance, incompatibility and mechanical property as a resin with high crystallinity and excellent performance. The release film prepared by taking TPX as a raw material has excellent release property and high temperature resistance without surface coating, but has poor weather resistance and flame retardance, the flame retardance grade is UL94HB, the long-term storage and repeated use are not facilitated, the product yield is influenced, and the cost is increased.
Disclosure of Invention
The invention provides a release film, aiming at solving the problem of single release force of the existing release film. 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.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a release film which sequentially comprises an upper release layer, a functional layer and a lower release layer.
The release film is also called TPX release film, and TPX is poly-4-methylpentene.
Further, the outer surface of the upper release layer or the lower release layer is embossed.
After the outer surface of the upper release layer or the lower release layer of the release film is embossed, the upper release layer and the lower release layer have different roughness.
Further, the roughness difference between the outer surfaces of the upper release layer and the lower release layer is 12.5-15, or the roughness difference between the outer surfaces of the lower release layer and the upper release layer is 12.5-15.
Further, the difference between the roughness of the outer surfaces of the upper release layer and the lower release layer is preferably 13.6-14.9.
Further, the difference between the surface roughness of the upper release layer and the lower release layer is most preferably 13.6.
Further, the roughness difference between the outer surfaces of the lower release layer and the upper release layer is 13.6-14.9.
Further, the difference between the roughness of the outer surfaces of the lower release layer and the upper release layer is most preferably 13.6.
Further, the upper release layer comprises inorganic particles, and the lower release layer comprises inorganic particles.
Further, the inorganic particles in the upper release layer and the lower release layer are ultraviolet screening agents.
Further, the ultraviolet shielding agent in the upper release layer and the lower release layer is carbon black.
Further, the particle size of the inorganic particles in the upper release layer and the lower release layer is 5-20 nm.
The particle size of the inorganic particles is an average particle size.
Further, the specific surface area of the inorganic particles in the upper release layer and the lower release layer is 200-500 m2/g。
Further, the particle size of the inorganic particles in the upper release layer and the lower release layer is preferably 5-10 nm.
Further, the specific surface area of the inorganic particles in the upper release layer and the lower release layer is preferably 200-300m2/g。
Further, the particle size of the inorganic particles in the upper release layer and the lower release layer is most preferably 10 nm.
Further, the specific surface area of the inorganic particles in the upper release layer and the lower release layer is most preferably 300m2/g。
Further, the functional layer includes an inorganic flame retardant.
Further, the inorganic flame retardant is antimony trioxide.
Further, the content of the inorganic flame retardant in the functional layer is 1.5-2%, and the percentage is weight percentage.
Further, the content of the inorganic flame retardant in the functional layer is preferably 1.5%.
Further, the functional layer further comprises an organic flame retardant, the inorganic flame retardant and the organic flame retardant form a composite flame retardant, and the weight ratio of the inorganic flame retardant to the organic flame retardant is 1: 0.8-1.5.
Further, the weight ratio of the inorganic flame retardant to the organic flame retardant is preferably 1: 0.8.
Further, the organic flame retardant is m-phenylene tetraphenyl diphosphate.
Further, the composite flame retardant is antimony trioxide and m-phenylene tetraphenyl diphosphate, and the composite ratio is 1: 0.8-1.5. The compounding ratio refers to the weight ratio of the inorganic flame retardant and the organic flame retardant in the composite flame retardant.
Furthermore, the addition amount of antimony trioxide in the functional layer is 1.5-2%, and the addition amount of m-phenylene tetraphenyl diphosphate is 1-2%.
Furthermore, the addition amount of antimony trioxide in the functional layer is preferably 1.5%, and the addition amount of m-phenylene tetraphenyl diphosphate is preferably 1.2%.
Further, the total thickness of the release film is 115 micrometers, and the sum of the thicknesses of the upper release layer and the lower release layer is 40-60% of the total thickness of the release film.
Further, the sum of the thicknesses of the upper release layer and the lower release layer is preferably 52% of the total thickness of the release film.
Further, the thickness of the upper release layer is 20-30% of the total thickness, and the thickness of the lower release layer is 20-30% of the total thickness.
Further, the thickness of the upper release layer is preferably 26% of the total thickness, and the thickness of the lower release layer is preferably 26% of the total thickness.
Further, the thickness of the functional layer is 40-60% of the total thickness of the release film.
Further, the thickness of the functional layer is 48% of the total thickness of the release film.
Further, the upper release layer and the lower release layer both comprise a polymer. The polymer in the upper release layer and the lower release layer comprises TPX and one or a combination of at least two selected from PMMA (polymethyl methacrylate), EVA (ethylene-vinyl acetate copolymer) and HDPE (high density polyethylene).
Further, the upper release layer comprises 81-85% of TPX, 3-7% of PMMA, 3-7% of HDPE, 0.3-0.7% of carbon black, 2% of antioxidant, 1-1.5% of heat stabilizer, 1.5-2% of modified montmorillonite, 0.5-0.8% of defoaming agent and 0.7-1% of thickening agent. The percentages are weight percentages.
Further, the lower release layer comprises 81-85% of TPX, 3-7% of EVA, 3-7% of HDPE, 0.3-0.7% of carbon black, 2% of antioxidant, 1-1.5% of heat stabilizer, 1.5-2% of modified montmorillonite, 0.5-0.8% of defoaming agent and 0.7-1% of thickening agent. The percentages are weight percentages.
Further, the functional layer comprises 30-31% of TPX, 5% of PMMA, 50-53% of PE (polyethylene), 5-5.5% of PBT (polybutylene terephthalate), 2.5-4% of a composite flame retardant, 1.2-2% of modified montmorillonite, 0.5% of a defoaming agent, 0.8-1% of a thickening agent and 1.5% of an antioxidant. The percentages are weight percentages.
Further, the antioxidant in the release film is bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide, the heat stabilizer in the upper release layer and the lower release layer is mercaptan organotin, the defoaming agent in the release film is a GPES type defoaming agent (polyether defoaming agent), and the thickening agent in the release film is methyl cellulose.
The invention also provides a method for preparing the release film, which is a multilayer co-extrusion casting process and comprises the following steps:
(1) melting the raw materials of the upper release layer, the functional layer and the lower release layer through different extruder charging barrels, extruding the raw materials through an extruder, and casting the cast sheet through a die head in a tape casting way;
(2) adjusting the thickness by longitudinal drawing;
(3) embossing on the outer surface of the upper release layer or the lower release layer through an embossing roller;
(4) and (6) cooling and shaping.
The extruder charging barrel comprises four temperature zone heating sections, and the set temperatures of the different temperature zone heating sections are 260-300 ℃.
Wherein the heat setting temperature is 30-70 ℃.
Wherein the cooling temperature is-5 to 20 ℃.
Further, the upper release layer comprises 83-85% of TPX, 3-7% of PMMA, 3-5% of HDPE, and 0.5-0.7% of carbon black, wherein the average particle diameter of the carbon black is 5-10nm, and the specific surface area is 200-300 m-22 percent of antioxidant and 1 to 1.2 percent of heat stabilizer1.5-2% of modified montmorillonite, 0.6-0.8% of defoaming agent and 0.7-1% of thickening agent; the functional layer comprises 31% of TPX, 5% of PMMA, 52% of PE, 5% of PBT, 2.7% of composite flame retardant, 1.5% of modified montmorillonite, 0.5% of defoaming agent, 0.8% of thickening agent and 1.5% of antioxidant; the lower release layer comprises 83-85% of TPX, 3-7% of EVA, 3-5% of HDPE, 0.5-0.7% of ultraviolet shielding agent, 2% of antioxidant, 1-1.2% of heat stabilizer, 1.5-2% of modified montmorillonite, 0.6-0.8% of defoaming agent and 0.7-1% of thickening agent. The technical scheme comprises an embodiment 5, an embodiment 8, an embodiment 10 and embodiments 14-15.
Further, the mixture ratio of the upper release layer is 85% of TPX, 3% of PMMA, 5% of HDPE and 0.7% of carbon black, the average particle diameter of the carbon black is 10nm, and the specific surface area is 300m2The anti-oxidant is 2 percent, the heat stabilizer is 1 percent, the modified montmorillonite is 1.5 percent, the defoaming agent is 0.8 percent, and the thickening agent is 1 percent; the functional layer comprises 31% of TPX, 5% of PMMA, 52% of PE, 5% of PBT, 2.7% of composite flame retardant, 1.5% of modified montmorillonite, 0.5% of defoaming agent, 0.8% of thickening agent and 1.5% of antioxidant; the lower release layer comprises 85% of TPX, 3% of EVA, 5% of HDPE, 0.7% of ultraviolet screening agent, 2% of antioxidant, 1% of heat stabilizer, 1.5% of modified montmorillonite, 0.8% of defoaming agent and 0.7-1% of thickening agent. The above technical solutions include embodiment 8 and embodiment 15.
Compared with the prior art, the invention has the beneficial effects that: the upper release layer and the lower release layer in the release film provided by the invention comprise inorganic particles, the inorganic particles in the upper release layer and the lower release layer have good ultraviolet shielding property and oxidation resistance, and the weather resistance of the TPX release film material can be improved by adding a small amount of the inorganic particles; the middle functional layer is a flame retardant layer, and an inorganic and organic composite flame retardant is adopted, so that the flame retardance of the release film can be greatly improved; the difference of the surface roughness of the upper release layer and the lower release layer can enlarge the change range of the release force of the release film so as to meet the requirements of different downstream manufacturers on the release force; the release film provided by the invention is a double-sided release film with different release forces, a surface coating treatment method is not needed to improve the release force, the risk of silicon transfer does not exist, residual glue is left during stripping, and the pollution and the production cost are reduced. Therefore, the release film provided by the invention has excellent release property and weather resistance, is easy to store and not easy to yellow, has good mechanical strength when used at high temperature, and has excellent flame-retardant and ultraviolet-resistant properties; the method can be used for Roll-to-Roll manufacturing process of circuit boards with higher requirements on release films.
Drawings
Fig. 1 is a schematic structural view of a release film provided in the present invention;
fig. 2 is a schematic view of the pressing of the release film according to the present invention.
Detailed Description
The technical solution of the present invention will be described in detail with reference to fig. 1 and the specific embodiment.
Fig. 1 is a schematic structural diagram of a release film provided by the present invention, wherein a represents an upper release layer, B represents a functional layer, and C represents a lower release layer.
Fig. 2 is a schematic view of the pressing of the release film provided by the present invention, wherein 1 represents the release film provided by the present invention, 2 represents the cover film, and 3 represents the flexible circuit board.
The preparation method of the TPX release film provided by the invention is a multilayer coextrusion casting process, and comprises the following steps:
(1) melting the raw materials of the upper release layer, the functional layer and the lower release layer through different extruder charging barrels, extruding the raw materials through an extruder, and casting the cast sheet through a die head in a tape casting way;
(2) adjusting the thickness by longitudinal drawing;
(3) embossing on the outer surface of the upper release layer or the lower release layer through an embossing roller;
(4) and (6) cooling and shaping.
The extruder charging barrel comprises four temperature zone heating sections, and the set temperatures of the different temperature zone heating sections are 260-300 ℃.
Wherein the heat setting temperature is 30-70 ℃.
Wherein the cooling temperature is-5 to 20 ℃.
The method for testing the main performance of the TPX release film provided by the invention is briefly described as follows:
release property: 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 release property of the release film.
Flame retardancy: and (3) carrying out a 10-second combustion test on the product, and judging the flame retardant grade according to the self-extinguishing time and the dripping condition, wherein the flame retardant grade is gradually increased from HB, V-2 and V-1 to V-0, and HB is the lowest flame retardant grade.
Ultraviolet resistance: and testing by adopting an ultraviolet aging resistance tester to observe whether the material has obvious color change.
Roughness: and (4) testing by using a roughness tester, contacting the surface of the material by using a probe, and displaying a reading, namely the surface roughness of the material.
Yellowing: placing the material in a yellowing resistance tester, setting the temperature at 50 ℃, setting the distance between the material and a lamp at 25cm, irradiating the material and observing whether the material has a yellowing trend.
Example 1
The invention provides a release film which sequentially comprises an upper release layer, a functional layer and a lower release layer.
The upper release layer A comprises the following components in percentage by weight:
TPX: 81%, PMMA: 5%, HDPE: 7%, carbon black: 0.3% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.5 percent, modified montmorillonite: 2%, GPES: 0.5%, methylcellulose: 0.7 percent.
The functional layer B comprises the following components in percentage by weight:
TPX: 31%, PMMA: 5%, PE: 50%, PBT: 5%, antimony trioxide: 2%, m-phenylene tetraphenyl diphosphate: 2 percent, modified montmorillonite: 2%, GPES: 0.5%, methylcellulose: 1%, bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide: 1.5 percent.
The lower release layer C comprises the following components in percentage by weight:
TPX: 81%, EVA: 5%, HDPE: 7%, carbon black: 0.3% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.5 percent, modified montmorillonite: 2%, GPES: 0.5%, methylcellulose: 0.7 percent.
The preparation method of the release film comprises the following steps:
(1) melting the raw materials of the upper release layer, the functional layer and the lower release layer through different extruder charging barrels, extruding the raw materials through an extruder, and casting the cast sheet through a die head in a tape casting way;
(2) adjusting the thickness by longitudinal drawing;
(3) embossing on the outer surface of the upper release layer through an embossing roller;
(4) and (6) cooling and shaping.
In the preparation process of the release film, the temperatures of four temperature zones of a charging barrel of an extruder are respectively 260 ℃, 270 ℃ and 270 ℃, the heat setting temperature is 50 ℃, and the cooling temperature is 10 ℃.
The total thickness of the prepared release film was 115 μm, the thicknesses of the upper release layer a and the lower release layer C were 20% of the total thickness, respectively, and the thickness of the functional layer B was 60% of the total thickness, and the performance test results are shown in table 1.
Example 2
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX: 81%, PMMA: 5%, HDPE: 7%, carbon black: 0.3% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.5 percent, modified montmorillonite: 2%, GPES: 0.5%, methylcellulose: 0.7 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 31%, PMMA: 5%, PE: 52%, PBT: 5%, antimony trioxide: 1.5%, m-phenylene tetraphenyl diphosphate: 1.2 percent, modified montmorillonite: 1.5%, GPES: 0.5%, methylcellulose: 0.8%, bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 81%, EVA: 5%, HDPE: 7%, carbon black: 0.3% by weight, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.5 percent, modified montmorillonite: 2%, GPES: 0.5%, methylcellulose: 0.7 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 270 ℃, 280 ℃ and 280 ℃, the heat setting temperature is 30 ℃, and the cooling temperature is-5 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed, the total thickness was 115 μm, the thicknesses of the upper release layer a and the lower release layer C were 26% and 48% respectively, and the performance test results are shown in table 1. The results of the performance test of the obtained release film are shown in table 1.
Example 3
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX: 81%, PMMA: 5%, HDPE: 7%, carbon black: 0.3% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.5 percent, modified montmorillonite: 2%, GPES: 0.5%, methylcellulose: 0.7 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 30%, PMMA: 5%, PE: 53%, PBT: 5.5%, antimony trioxide: 1.5%, m-phenylene tetraphenyl diphosphate: 1% of modified montmorillonite: 1.2%, GPES: 0.5%, methylcellulose: 0.8%, bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 81%, EVA: 5%, HDPE: 7%, carbon black: 0.3% by weight, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.5 percent, modified montmorillonite: 2%, GPES: 0.5%, ABase cellulose: 0.7 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 280 ℃, 300 ℃ and 300 ℃, the heat setting temperature is 70 ℃ and the cooling temperature is 20 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed, the total thickness was 115 μm, the thicknesses of the upper release layer a and the lower release layer C were respectively 30% and 40% of the total thickness, and the performance test results are shown in table 1.
Example 4
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX: 83%, PMMA: 7%, HDPE: 3%, carbon black: 0.5% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.2 percent, modified montmorillonite: 2%, GPES: 0.6%, methylcellulose: 0.7 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 31%, PMMA: 5%, PE: 50%, PBT: 5%, antimony trioxide: 2%, m-phenylene tetraphenyl diphosphate: 2 percent, modified montmorillonite: 2%, GPES: 0.5%, methylcellulose: 1% bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide (antioxidant): 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 83%, EVA: 7%, HDPE: 3%, carbon black: 0.5% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.2 percent, modified montmorillonite: 2%, GPES: 0.6%, methylcellulose: 0.7 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 260 ℃, 270 ℃ and 270 ℃, the heat setting temperature is 50 ℃ and the cooling temperature is 10 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed to a thickness of 115 μm, the thicknesses of the upper release layer a and the lower release layer C were 20% of the total thickness, respectively, and the thickness of the functional layer B was 60% of the total thickness, and the performance test results are shown in table 1.
Example 5
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX: 83%, PMMA: 7%, HDPE: 3%, carbon black: 0.5% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.2 percent, modified montmorillonite: 2%, GPES: 0.6%, methylcellulose: 0.7 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 31%, PMMA: 5%, PE: 52%, PBT: 5%, antimony trioxide: 1.5%, m-phenylene tetraphenyl diphosphate: 1.2 percent, modified montmorillonite: 1.5%, GPES: 0.5%, methylcellulose: 0.8%, bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 83%, EVA: 7%, HDPE: 3%, carbon black: 0.5% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.2 percent, modified montmorillonite: 2%, GPES: 0.6%, methylcellulose: 0.7 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 270 ℃, 280 ℃ and 280 ℃, the heat setting temperature is 30 ℃, and the cooling temperature is-5 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed to a thickness of 115 μm, the thicknesses of the upper release layer a and the lower release layer C were respectively 26% and 48% of the total thickness, and the performance test results are shown in table 1.
Example 6
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX: 83%, PMMA: 7%, HDPE: 3%, carbon black: 0.5% of carbon black, the average particle diameter of the carbon black being 10nm and the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.2 percent, modified montmorillonite: 2%, GPES: 0.6%, methylcellulose: 0.7 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 30%, PMMA: 5%, PE: 53%, PBT: 5.5%, antimony trioxide: 1.5%, m-phenylene tetraphenyl diphosphate: 1% of modified montmorillonite: 1.2%, GPES: 0.5%, methylcellulose: 0.8%, bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 83%, EVA: 7%, HDPE: 3%, carbon black: 0.5% of carbon black, the average particle diameter of the carbon black being 10nm, the specific surface area being 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1.2 percent, modified montmorillonite: 2%, GPES: 0.6%, methylcellulose: 0.7 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 280 ℃, 300 ℃ and 300 ℃, the heat setting temperature is 70 ℃ and the cooling temperature is 20 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed to a thickness of 115 μm, the thicknesses of the upper release layer a and the lower release layer C were respectively 30% and 40% of the total thickness, and the performance test results are shown in table 1.
Example 7
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX: 85%, PMMA: 3%, HDPE: 5%, carbon black: 0.7% by weight of carbon black, having an average particle diameter of 10nm and a specific surface area of 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 31%, PMMA: 5%, PE: 50%, PBT: 5%, antimony trioxide: 2%, m-phenylene tetraphenyl diphosphate: 2 percent, modified montmorillonite: 2%, GPES: 0.5%, methylcellulose: 1%, bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 85%, EVA: 3%, HDPE: 5%, carbon black: 0.7% by weight of carbon black, having an average particle diameter of 10nm and a specific surface area of 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 260 ℃, 270 ℃ and 270 ℃, the heat setting temperature is 50 ℃ and the cooling temperature is 10 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed to a thickness of 115 μm, the thicknesses of the upper release layer a and the lower release layer C were 20% of the total thickness, respectively, and the thickness of the functional layer B was 60% of the total thickness, and the performance test results are shown in table 1.
Example 8
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX: 85%, PMMA: 3%, HDPE: 5%, carbon black: 0.7% by weight of carbon black, having an average particle diameter of 10nm and a specific surface area of 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 31%, PMMA: 5%, PE: 52%, PBT: 5%, antimony trioxide: 1.5%, m-phenylene tetraphenyl diphosphate: 1.2 percent, modified montmorillonite: 1.5%, GPES: 0.5%, methylcellulose: 0.8%, bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 85%, EVA: 3%, HDPE: 5%, carbon black: 0.7% by weight of carbon black having an average particle diameter of10nm, and a specific surface area of 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 270 ℃, 280 ℃ and 280 ℃, the heat setting temperature is 30 ℃, and the cooling temperature is-5 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed to a thickness of 115 μm, the thicknesses of the upper release layer a and the lower release layer C were respectively 26% and 48% of the total thickness, and the performance test results are shown in table 1.
Example 9
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX: 85%, PMMA: 3%, HDPE: 5%, carbon black: 0.7% by weight, and a specific surface area of carbon black of 10nm average particle diameter of 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 30%, PMMA: 5%, PE: 53%, PBT: 5.5%, antimony trioxide: 1.5%, m-phenylene tetraphenyl diphosphate: 1% of modified montmorillonite: 1.2%, GPES: 0.5%, methylcellulose: 0.8%, bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 85%, EVA: 3%, HDPE: 5%, carbon black: 0.7% by weight of carbon black, having an average particle diameter of 10nm and a specific surface area of 300m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 280 ℃, 300 ℃ and 300 ℃, the heat setting temperature is 70 ℃ and the cooling temperature is 20 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed to a thickness of 115 μm, the thicknesses of the upper release layer a and the lower release layer C were respectively 30% and 40% of the total thickness, and the performance test results are shown in table 1.
Release film as provided in example 1.
TPX: 85%, PMMA: 3%, HDPE: 5%, carbon black: 0.7% by weight of carbon black, and having an average particle diameter of 5nm and a specific surface area of 200m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 31%, PMMA: 5%, PE: 52%, PBT: 5%, antimony trioxide: 1.5%, m-phenylene tetraphenyl diphosphate: 1.2 percent, modified montmorillonite: 1.5%, GPES: 0.5%, methylcellulose: 0.8%, bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 85%, EVA: 3%, HDPE: 5%, carbon black: 0.7% by weight of carbon black, and having an average particle diameter of 5nm and a specific surface area of 200m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
in the preparation process of the release film, the four temperature zones of the charging barrel of the extruder are respectively 280 ℃, 300 ℃ and 300 ℃, the heat setting temperature is 70 ℃ and the cooling temperature is 20 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed to a thickness of 115 μm, the thicknesses of the upper release layer a and the lower release layer C were respectively 26% and 48% of the total thickness, and the performance test results are shown in table 1.
Example 11
Release film as provided in example 1.
The upper release layer A comprises the following components in percentage by weight:
TPX:85%,PMMA:3%HDPE: 5%, carbon black: 0.7% by weight, and a specific surface area of the carbon black of 20nm average particle diameter of 500m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
the functional layer B comprises the following components in percentage by weight:
TPX: 31%, PMMA: 5%, PE: 52%, PBT: 5%, antimony trioxide: 1.5%, m-phenylene tetraphenyl diphosphate: 1.2 percent, modified montmorillonite: 1.5%, GPES: 0.5%, methylcellulose: 0.8%, bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 1.5 percent;
the lower release layer C comprises the following components in percentage by weight:
TPX: 85%, EVA: 3%, HDPE: 5%, carbon black: 0.7% by weight of carbon black, and having an average particle diameter of 20nm and a specific surface area of 500m2Bis (3, 5-tert-butyl-4-hydroxyphenyl) sulfide: 2%, organotin mercaptides: 1% of modified montmorillonite: 1.5%, GPES: 0.8%, methylcellulose: 1 percent;
in the preparation process of the release film, the four temperatures of the barrel temperature of the extruder are respectively 280 ℃, 300 ℃ and 300 ℃, the heat setting temperature is 70 ℃ and the cooling temperature is 20 ℃.
The outer surface of the upper release layer a of the prepared release film was embossed to a thickness of 115 μm, the thicknesses of the upper release layer a and the lower release layer C were respectively 26% and 48% of the total thickness, and the performance test results are shown in table 1.
Example 12
The release film provided in example 1 was different in that the outer surface of the lower release layer C of the prepared release film was embossed.
Example 13
The release film provided in example 2 was different in that the outer surface of the lower release layer C of the prepared release film was embossed.
Example 14
The release film provided in example 5 was different in that the outer surface of the lower release layer C of the prepared release film was embossed.
Example 15
The release film provided in example 8, except that the outer surface of the lower release layer C of the prepared release film was embossed.
Table 1 results of performance test of release films prepared in examples 1 to 15
Figure BDA0001527102270000201
Figure BDA0001527102270000211
As can be seen from Table 1, the release film provided by the invention has good release property, flame retardance, ultraviolet resistance and yellowing resistance. The release films provided in the embodiments 5, 8 and 10 and 14 to 15 have good comprehensive performance, the release force of the upper release layer is 5 to 6g/in, the release force of the lower release layer is 17 to 20g/in, or the release force of the upper release layer is 17g/in, the release force of the lower release layer is 5 to 6g/in, the flame retardant rating is V-1, and the release film has at most slight color change and no yellowing phenomenon in an ultraviolet aging resistant tester. In particular, the release films provided in examples 8 and 15 have the best overall performance, the release force of the upper release layer is 6g/in, the release force of the lower release layer is 17g/in, or the release force of the upper release layer is 17g/in, the release force of the lower release layer is 6g/in, the flame retardant rating is V-1, and no color change or yellowing phenomenon occurs in an ultraviolet aging resistance tester.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. All equivalent changes and modifications made according to the disclosure of the present invention are covered by the scope of the claims of the present invention.

Claims (4)

1. The release film is characterized by sequentially comprising an upper release layer, a functional layer and a lower release layer; embossing the outer surface of the upper release layer or the lower release layer; the upper release layer comprises 83-85% of TPX, 3-7% of PMMA, 3-5% of HDPE, 0.5-0.7% of carbon black and 2%The antioxidant, the heat stabilizer, the modified montmorillonite, the defoaming agent and the thickening agent are respectively 1-1.2%, 1.5-2%, 0.6-0.8% and 0.7-1%; the average particle diameter of the carbon black is 5-10nm, and the specific surface area is 200-300m2(ii)/g; the functional layer comprises 31% of TPX, 5% of PMMA, 52% of PE, 5% of PBT, 2.7% of composite flame retardant, 1.5% of modified montmorillonite, 0.5% of defoaming agent, 0.8% of thickening agent and 1.5% of antioxidant; the lower release layer comprises 83-85% of TPX, 3-7% of EVA, 3-5% of HDPE, 0.5-0.7% of ultraviolet shielding agent, 2% of antioxidant, 1-1.2% of heat stabilizer, 1.5-2% of modified montmorillonite, 0.6-0.8% of defoaming agent and 0.7-1% of thickening agent.
2. The release film according to claim 1, wherein the difference between the roughness of the outer surfaces of the upper and lower release layers is 12.5-15, or the difference between the roughness of the outer surfaces of the lower and upper release layers is 12.5-15.
3. The release film according to claim 1, wherein the total thickness of the release film is 115 μm, and the sum of the thicknesses of the upper release layer and the lower release layer is 40-60% of the total thickness of the release film.
4. The release film according to claim 1, wherein the thickness of the functional layer is 40 to 60% of the total thickness of the release film.
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