CN113861479A - Water oxygen barrier film - Google Patents

Water oxygen barrier film Download PDF

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CN113861479A
CN113861479A CN202111119555.4A CN202111119555A CN113861479A CN 113861479 A CN113861479 A CN 113861479A CN 202111119555 A CN202111119555 A CN 202111119555A CN 113861479 A CN113861479 A CN 113861479A
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acrylate
microspheres
fluorine
water
coating
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张爱迪
谢彬彬
齐永高
舒欣
刘勇
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Nanjing Beidi New Material Technology Co ltd
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Nanjing Beidi New Material Technology Co ltd
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    • C08J2433/06—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract

The invention discloses a water oxygen barrier film, which takes PET as a substrate, a back coating is introduced at the back, and a bottom coating, a vapor deposition layer and a top coating are distributed and introduced on the PET, wherein the bottom coating mainly comprises fluorine-containing acrylate polymer and modified organic silicon microspheres, the vapor deposition layer mainly comprises silicon oxide or aluminum oxide, the top coating is acrylate polymer, and in the vapor deposition layer, the silicon oxide or the aluminum oxide layer is a first barrier and can have the barrier effect on water oxygen firstly; secondly, the organic silicon microspheres in the bottom coating have the function of absorbing and intercepting water vapor; meanwhile, the fluorine-containing acrylate polymer has a barrier effect on water and oxygen, and even if less water and oxygen pass through the evaporation layer, the fluorine-containing acrylate polymer can be blocked by the bottom coating; thirdly, the coordination compound formed by the fluorine-containing acrylate polymer and the organic matter on the surface of the organic silicon has a more compact structure, can have a secondary blocking effect on water and oxygen, and further blocks and isolates the water and oxygen passing through the first barrier.

Description

Water oxygen barrier film
Technical Field
The invention relates to the technical field of barrier films, in particular to a water-oxygen barrier film.
Background
The barrier film has moisture barrier properties, typically against the penetration of air and moisture. Barrier films are generally used as encapsulating materials and have important applications in the fields of food, medicine, agriculture, Liquid Crystal Display (LCD), electronic paper, organic light emitting diodes, solar cells, and the like.
Currently, a commonly used barrier film is commercially available in a roll-to-roll process. The main process is to bond a thicker PET base film and a thinner barrier film (also referred to as a thin barrier film, mainly using PET as a substrate, and introducing a barrier layer, such as a water-oxygen barrier layer of inorganic silicon dioxide, silicon nitride, aluminum oxide, etc.) by a roll-to-roll process. There are many limitations to the above process. On one hand, the preparation technology of the barrier layer film is intensively mastered in the countries such as Han and the like, the resource source is limited, and the barrier layer film is easily influenced by related policies; on the other hand, the process for preparing the barrier film by adopting the roll-to-roll laminating process has higher requirements on equipment, the barrier film is thin (less than 20 microns), the transverse and longitudinal tension is difficult to control, MD (longitudinal lines or folds) and TD (transverse lines or folds) of the PET base film and the barrier film can be easily caused in the laminating process, the laminating yield is reduced, the water and oxygen barrier performance of the barrier film is finally influenced, and the performance of a terminal product is finally influenced.
Disclosure of Invention
In view of the above, embodiments of the present invention are expected to provide a water oxygen barrier film, so as to solve the problems of less preparation technology, higher manufacturing cost, complex process, low yield, and the like in the existing barrier film preparation process.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the invention provides a water oxygen barrier film, which comprises a back coating, a PET substrate layer, a bottom coating, a vapor deposition layer and a top coating from bottom to top;
the back coating is an acrylate solution containing microspheres, and the preparation method of the acrylate solution containing microspheres comprises the following steps: adding 0.1-0.5 wt% of microspheres and 0.01-0.1 wt% of photoinitiator into acrylate compound glue, and stirring for 2-10 hours;
the thickness of the PET substrate layer is 50-125 μm;
the bottom coating is modified organic silicon microspheres introduced into a fluorine-containing acrylate polymer, and the structural formula of the modified organic silicon microspheres is shown in the specification
Figure BDA0003276534320000021
Wherein R is1Is a nitrogen or oxygen or sulfur atom, R2Is an alkyl function, is-C (CH)3)3-or-CH (CH)3)2-or-CH2(CH3) -or CH3，R2Is an electron-deficient structure;
the evaporation layer is silicon oxide or aluminum oxide and has a thickness of 2-10 nm;
the top coat is an acrylate polymer.
Preferably, the acrylate compound is butyl acrylate or hydroxypropyl acrylate or polyethylene glycol diacrylate or isobornyl acrylate or methyl methacrylate or methoxy polyethylene glycol acrylate; the photoinitiator is p-N, N-dimethylamino benzoic acid isooctyl ester or methyl benzoylformate or 2,4,6 (trimethylbenzoyl) diphenylphosphine oxide or 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-acetone or triaryl sulfonium salts or benzophenone; the microspheres are 1-20 μm organic microspheres or 200nm-10 μm inorganic microspheres.
Further, the fluorine-containing acrylate polymer is prepared by dissolving a fluorine-containing acrylate monomer in a fluorine-containing organic solvent, wherein the fluorine-containing organic solvent is poly (N-perfluorocycloalkyl) amide methacrylate or poly (perfluorooctyl methyl acrylate).
Furthermore, the structural formula of the fluorine-containing acrylate monomer is shown in the specification
Figure BDA0003276534320000031
Wherein R is3is-CH3or-CH2(CH2)nCH3Wherein n is not less than 1, R4For buffer linking, R4is-CH2CH2-or-SO2NH-。
Preferably, the acrylate polymer is butyl acrylate or hydroxypropyl acrylate or polyethylene glycol diacrylate or isobornyl acrylate or methyl methacrylate or methoxy polyethylene glycol acrylate.
The invention has the following beneficial effects: in the evaporation coating, the siloxane compound or the alumina layer is a first barrier which has the function of blocking water and oxygen; secondly, the organic silicon microspheres in the bottom coating have the function of absorbing and intercepting water vapor; meanwhile, the fluorine-containing acrylate compound has a barrier effect on water and oxygen, and even if less water and oxygen pass through the evaporation layer, the fluorine-containing acrylate compound can be blocked by the bottom coating; and thirdly, a coordination compound formed by the fluorine-containing acrylate compound and organic matters on the surface of the organic silicon has a more compact structure, can have a secondary blocking effect on water and oxygen, and further blocks and isolates the water and oxygen passing through the first barrier.
Drawings
FIG. 1 is a schematic view of a water oxygen barrier film according to the present invention;
FIG. 2 is a schematic diagram of a coordination structure formed by a fluoroacrylate polymer and silicone microspheres of the present invention;
FIG. 3 is a graph showing the variation of the water vapor transmission rate of the water oxygen barrier film according to the thickness of the silicon dioxide evaporation layer;
FIG. 4 is a graph of the moisture vapor transmission rate of the water oxygen barrier film of the present invention as a function of primer thickness;
FIG. 5 is a graph showing the variation of the water vapor transmission rate of the water oxygen barrier film according to the thickness of the silicon dioxide evaporation layer;
wherein: reference numeral 1 denotes a back coat layer, 2 denotes a PET base layer, 3 denotes a primer layer, 4 denotes a vapor deposition layer, and 5 denotes a top coat layer.
Detailed Description
So that the manner in which the features and aspects of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings.
A water oxygen barrier film comprises a back coating 1, a PET substrate layer 2, a bottom coating 3, an evaporation coating 4 and a top coating 5 from bottom to top;
the back coating 1 is an acrylate solution containing microspheres, and the preparation method of the acrylate solution containing microspheres comprises the following steps: adding 0.1-0.5 wt% of microspheres and 0.01-0.1 wt% of photoinitiator into acrylate compound glue, and stirring for 2-10 hours;
coating the acrylic ester solution containing the microspheres on the back surface of the PET substrate layer 2 by adopting a laminating and coating all-in-one machine to form a back coating layer 1;
the microspheres introduced into the back coating 1 mainly increase the scratch resistance of the PET film;
here, the acrylate compound is butyl acrylate or hydroxypropyl acrylate or polyethylene glycol diacrylate or isobornyl acrylate or methyl methacrylate or methoxy polyethylene glycol acrylate;
here, the photoinitiator is isooctyl p-N, N-dimethylaminobenzoate or methyl benzoylformate or 2,4,6 (trimethylbenzoyl) diphenylphosphine oxide or 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-propanone or triarylsulfonium salts or benzophenone;
here, the microspheres are organic microspheres with the particle size of 1-20 μm or inorganic microspheres with the particle size of 200nm-10 μm; the organic microspheres can be polymethyl methacrylate microspheres or polystyrene microspheres or polyvinyl chloride microspheres; the inorganic microspheres can be titanium dioxide microspheres, zinc oxide microspheres or montmorillonite microspheres;
the thickness of the PET substrate layer 2 is 50-125 μm;
the bottom coating 3 is modified organic silicon microspheres introduced into a fluorine-containing acrylate polymer, and the structural formula of the modified organic silicon microspheres is shown in the specification
Figure BDA0003276534320000051
Wherein R is1Is a nitrogen or oxygen or sulfur atom, R2Is an alkyl function, is-C (CH)3)3-or-CH (CH)3)2-or-CH2(CH3) -or CH3，R2Is an electron-deficient structure;
here, the fluorine-containing acrylate polymer is prepared by dissolving a fluorine-containing acrylate monomer in a fluorine-containing organic solvent, wherein the fluorine-containing organic solvent is poly (N-perfluorocycloalkyl) amide methacrylate or poly (perfluorooctyl methyl acrylate);
here, the fluorine-containing acrylate monomer has the structural formula
Figure BDA0003276534320000052
Wherein R is3is-CH3or-CH2(CH2)nCH3Wherein n is not less than 1, R4For buffer chaining, it can be-CH2CH2-or-SO2NH-；
Here, the fluoroacrylate polymer may form a coordinate bond with an electron-deficient structure (functional group) on the surface of the silicone microsphere, as shown in fig. 2, in this structure of fig. 2, a coordination structure is formed between fluorine atoms in the fluoroacrylate polymer and organic matter on the surface of the silicone microsphere, and this coordination structure acts as a barrier to water and oxygen.
Here, the main role of the fluoroacrylate polymer is: the introduced fluorine-containing polymer has high weather resistance, high heat resistance, high stability and the like, and simultaneously has the characteristics of hydrophobicity, hydrophobicity and the like.
The evaporation layer 4 is silicon oxide or aluminum oxide, and the thickness is 2-10 nm;
here, a vacuum coating evaporation process is adopted, a layer of evaporation compound, which can be silicon oxide or aluminum oxide, is introduced into the surface of the undercoat layer 3, and the thickness of the evaporation layer 4 is 2-10 nm.
The top coat 5 is an acrylate polymer.
Here, the acrylate polymer is butyl acrylate or hydroxypropyl acrylate or polyethylene glycol diacrylate or isobornyl acrylate or methyl methacrylate or methoxy polyethylene glycol acrylate.
The silicon dioxide evaporation layers with different thicknesses are introduced on the PET substrate layer with the thickness of 75 μm, and as shown in figure 3, the water oxygen barrier film has lower water oxygen transmission rate and better water oxygen barrier performance along with the larger thickness of the silicon dioxide evaporation layer.
The primer layers with different thicknesses are introduced on the PET substrate layer with the thickness of 75 microns, wherein the addition content of modified organic silicon microspheres (2 microns) is respectively 0.2%, 0.5% and 0.8%, as shown in figure 4, the water-oxygen transmission rate of the water-oxygen barrier film is lower and the water-oxygen barrier performance is better along with the larger thickness of the primer layer, and the water-oxygen barrier performance is better along with the more addition content of the organic silicon microspheres.
The primer layer thickness was chosen to be 5 μm with 0.5% addition of modified silicone microspheres (2 microns), as shown in fig. 5, the lower the water oxygen transmission rate of the water oxygen barrier film, the better the water oxygen barrier performance, with the larger the silica evaporated layer thickness.
The specific type of the above-mentioned devices is not limited and detailed, and the deep connection mode of the above-mentioned devices is not detailed, and can be understood by those skilled in the art as the common general knowledge.
The embodiments of the present invention are only described in the detailed description, and the scope of the present invention is not limited thereto. Since the present invention can be modified by a person skilled in the art, the present invention is not limited to the embodiments described above.

Claims (5)

1. The water and oxygen barrier film is characterized by comprising a back coating, a PET substrate layer, a bottom coating, a vapor deposition layer and a top coating from bottom to top;
the back coating is an acrylate solution containing microspheres, and the preparation method of the acrylate solution containing microspheres comprises the following steps: adding 0.1-0.5 wt% of microspheres and 0.01-0.1 wt% of photoinitiator into acrylate compound glue, and stirring for 2-10 hours;
the thickness of the PET substrate layer is 50-125 μm;
the bottom coating is modified organic silicon microspheres introduced into a fluorine-containing acrylate polymer, and the structural formula of the modified organic silicon microspheres is shown in the specification
Figure FDA0003276534310000011
Wherein R is1Is a nitrogen or oxygen or sulfur atom, R2Is an alkyl function, is-C (CH)3)3-or-CH (CH)3)2-or-CH2(CH3) -or CH3，R2Is an electron-deficient structure;
the evaporation layer is silicon oxide or aluminum oxide and has a thickness of 2-10 nm;
the top coat is an acrylate polymer.
2. The water oxygen barrier film according to claim 1, wherein the acrylate compound is butyl acrylate or hydroxypropyl acrylate or polyethylene glycol diacrylate or isobornyl acrylate or methyl methacrylate or methoxy polyethylene glycol acrylate; the photoinitiator is p-N, N-dimethylamino benzoic acid isooctyl ester or methyl benzoylformate or 2,4,6 (trimethylbenzoyl) diphenylphosphine oxide or 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-acetone or triaryl sulfonium salts or benzophenone; the microspheres are 1-20 μm organic microspheres or 200nm-10 μm inorganic microspheres.
3. The water oxygen barrier membrane according to claim 1, wherein said fluorine-containing acrylate polymer is prepared by dissolving a fluorine-containing acrylate monomer in a fluorine-containing organic solvent, and said fluorine-containing organic solvent is poly (N-perfluorocycloalkyl) amide methacrylate or poly (perfluorooctyl methyl acrylate).
4. The water oxygen barrier film of claim 3 wherein the fluorine-containing acrylate monomer has the formula
Figure FDA0003276534310000021
Wherein R is3is-CH3or-CH2(CH2)nCH3Wherein n is not less than 1, R4For buffer linking, R4is-CH2CH2-or-SO2NH-。
5. A water oxygen barrier film according to claim 1 wherein said acrylate polymer is butyl acrylate or hydroxypropyl acrylate or polyethylene glycol diacrylate or isobornyl acrylate or methyl methacrylate or methoxy polyethylene glycol acrylate.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1539896A (en) * 2003-10-30 2004-10-27 复旦大学 Method for improving performance of macromoledule substrate in obstructing water
WO2014119662A1 (en) * 2013-01-31 2014-08-07 大日本印刷株式会社 Gas barrier film
CN108047852A (en) * 2017-12-14 2018-05-18 合肥乐凯科技产业有限公司 A kind of polyester film
CN109312201A (en) * 2016-06-16 2019-02-05 3M创新有限公司 Fill the barrier property adhesive composition of nanoparticle
CN109535459A (en) * 2018-10-22 2019-03-29 张家港康得新光电材料有限公司 A kind of barrier film and preparation method thereof and blue light transmitance adjusting method
CN111775518A (en) * 2020-07-01 2020-10-16 汕头万顺新材集团股份有限公司 Barrier film structure with high weather resistance

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1539896A (en) * 2003-10-30 2004-10-27 复旦大学 Method for improving performance of macromoledule substrate in obstructing water
WO2014119662A1 (en) * 2013-01-31 2014-08-07 大日本印刷株式会社 Gas barrier film
CN109312201A (en) * 2016-06-16 2019-02-05 3M创新有限公司 Fill the barrier property adhesive composition of nanoparticle
CN108047852A (en) * 2017-12-14 2018-05-18 合肥乐凯科技产业有限公司 A kind of polyester film
CN109535459A (en) * 2018-10-22 2019-03-29 张家港康得新光电材料有限公司 A kind of barrier film and preparation method thereof and blue light transmitance adjusting method
CN111775518A (en) * 2020-07-01 2020-10-16 汕头万顺新材集团股份有限公司 Barrier film structure with high weather resistance

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