CN119039648B - A degradable transparent high-barrier film and preparation method thereof - Google Patents
A degradable transparent high-barrier film and preparation method thereof Download PDFInfo
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- CN119039648B CN119039648B CN202411547434.3A CN202411547434A CN119039648B CN 119039648 B CN119039648 B CN 119039648B CN 202411547434 A CN202411547434 A CN 202411547434A CN 119039648 B CN119039648 B CN 119039648B
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Classifications
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
本发明公开了一种可降解透明高阻隔膜及其制备，包括六层膜，依次包括面涂层、无机镀层、前处理层、底涂层、基材层，热封层；所述前处理层包括NiCr镀层、SUS镀层、Si镀层中的一种或多种。本发明的可降解透明高阻隔膜应用在环保包装袋上，具有透明可视，高阻隔功能，可降解，全生命周期无污染可分解，无危害，能够在废弃后被降解并回归自然。
The present invention discloses a degradable transparent high-barrier film and its preparation, comprising a six-layer film, which sequentially comprises a top coating, an inorganic coating, a pre-treatment layer, a primer layer, a substrate layer, and a heat-sealing layer; the pre-treatment layer comprises one or more of a NiCr coating, a SUS coating, and a Si coating. The degradable transparent high-barrier film of the present invention is applied to environmentally friendly packaging bags, has transparent visibility, high barrier function, is degradable, pollution-free and decomposable throughout its life cycle, is harmless, and can be degraded and returned to nature after being discarded.
Description
Technical Field
The invention relates to the field of film processing, in particular to a degradable transparent high-barrier film and a preparation method thereof.
Background
The traditional packaging barrier film base materials are generally PET, nylon or BOPP and PE, and the barrier film is manufactured by vacuum coating and coating, so that the PET material and the PE or PP base materials have large performance difference and cannot be directly recycled, and the environment is not protected, white pollution and micro plastic pollution can be formed if the PET material is discarded in the environment and cannot be completely degraded within 200-300 years, the environment can be deeply polluted, and the packaging industry increasingly pays attention to the environmental protection problem along with the export of European Union plastics convention and 3060 carbon emission policy. The existing environment-friendly base material is of a single material type, generally a PP or PE base material, has poor barrier property, needs coating and coating processing, is really environment-friendly and harmless, and can not be degraded in the environment if the material does not enter the recovery system, and can still cause pollution. The other environment-friendly material is of a degradable type, and a degradable substrate such as PLA or PBAT is used, but the degradable pure substrate has no barrier property, and needs special coating and coating processing before having high barrier property, so that how to better carry out coating and coating processing on the degradable type substrate becomes the key point and the difficulty of research.
Disclosure of Invention
The present invention aims to overcome the above-mentioned drawbacks of the prior art and to provide a degradable transparent high barrier film. The degradable transparent high-barrier film is applied to environment-friendly packaging bags, has transparent and visible properties, has a high-barrier function, is degradable, has no pollution to the whole life cycle, can be decomposed, has no harm, and can be degraded and return to nature after being abandoned.
In order to solve the technical problems, the invention provides the following technical scheme:
A degradable transparent high-barrier film comprises six layers of films, and sequentially comprises a surface coating, an inorganic plating layer, a pretreatment layer, a bottom coating, a substrate layer and a heat sealing layer, wherein the pretreatment layer comprises one or more of a NiCr plating layer, a SUS plating layer and a Si plating layer.
The transparent high-barrier film with stacked multilayer film layers is manufactured after precise coating and vacuum coating, the product has high transparency, can visually and clearly see the state of the content, has high barrier property, can protect the content from being influenced by water vapor or oxygen, and prolongs the shelf life of the product. Compared with the traditional plastic barrier film, the biodegradable plastic barrier film has higher environmental protection property and sustainability.
The film has barrier property, water vapor transmittance WVTR (Vapor Transmission Rate) is less than or equal to 1g/m < 2 >/day, oxygen transmittance OTR (Oxygen Transmission Rate) is less than or equal to 1.0cc/m < 2 >/day, light transmittance is more than or equal to 88%, and peel force between layers is more than or equal to 2N/15mm.
Preferably, the inorganic plating layer includes one or more of SiOx plating layer and AlOx plating layer.
The transparent high-barrier film is applied to high-end packaging bags, has higher requirements on coating adhesion and interlayer peeling force, and generally requires that the adhesion is more than or equal to 5B and the interlayer peeling force is more than 2N/15mm. Therefore, the invention uses the pretreatment plating layers such as NiCr, SUS or Si and the like, and has the main function of increasing the adhesive force between the SiOx or AlOx inorganic plating layers and the base material, and obviously improving the interlayer stripping force after the composite bag making.
Preferably, the top coating comprises one or more of a polyurethane coating and a PVA coating, the bottom coating comprises one or more of a polyurethane coating and an acrylic coating, the substrate layer comprises one or more of a PLA substrate and a PBAT substrate, and the heat sealing layer comprises modified PLA or modified PBAT.
The product is prepared from PLA or PBAT and the like which can be degraded as a substrate layer, and is required to be matched with a bottom coating due to poor barrier property of the degradable substrate, a pretreatment layer, an SiOx or AlOx coating layer and a top coating layer, and finally a functional film with high barrier property to water vapor, oxygen and the like is formed.
Preferably, the thickness of the top coating layer is 0.1-2 um, the thickness of the inorganic coating layer is 10-50 nm, the thickness of the pretreatment layer is 2-15 nm, the thickness of the bottom coating layer is 0.1-2 um, the thickness of the base material layer is 15-100 um, and the thickness of the heat sealing layer is 1-10 um, and is generally 8% -15% of the total thickness.
The invention adopts a double-layer coating process, but the thickness of the coating is nano-scale, and is very thin, for example, the thickness of the pretreatment thickness layer is about 10 nanometers, the thickness of an inorganic coating such as SiOx or AlOx is about 10-50 nanometers, the coating can reach transparency under the condition of extremely thin coating, in addition, the refractive index of the coating is matched with that of the surface coating, the refractive index of the coating is high, the refractive index of the coating is low, a certain anti-reflection effect is realized when the coating is matched, and the good transparency effect of the film is ensured.
The preparation method of the degradable transparent high-barrier film comprises the following steps:
A. Bonding the heat sealing layer on one side of the substrate layer, and co-extruding and stretching to obtain a substrate layer material with one side bonded with the heat sealing layer;
B. Coating a primer coating material on the other side of the substrate layer material of the single-sided bonding heat sealing layer, and forming the primer coating after curing;
C. vacuum coating is carried out on the bottom coating layer to form the pretreatment layer;
D. vapor deposition is carried out on the pretreatment layer to form the inorganic coating;
E. Coating a surface coating material on the inorganic coating, curing, and then curing to form the surface coating, thereby obtaining the degradable transparent high-barrier film.
The substrate layer is made of biodegradable materials such as PLA or PBAT and has a thickness of 15-100 um, and the PLA coiled material is made of starch raw materials proposed by renewable plant resources (such as corn, cassava and the like). The starch material is saccharified to obtain glucose, glucose and certain strain are fermented to prepare high-purity lactic acid, polylactic acid particles with certain molecular weight are synthesized by a chemical synthesis method, the polylactic acid PLA particles are prepared into a coiled film by melting and tabletting and bidirectional (axial and transverse) stretching, after the biaxial stretching, the mechanical properties and the processing properties of the base material such as the tensile strength are improved, and the material is degraded into carbon dioxide and water at a temperature higher than 55 ℃ or under the action of oxygen enrichment and microorganisms for about 180 days under the composting condition, so that the material is circulated in the nature without influencing the environment, and is an ideal green high-molecular material.
Preferably, in the step C, the vacuum coating operation comprises the steps of exciting plasma in a vacuum chamber by high corona, and then exciting target surface molecules by the plasma to combine with the bottom coating, so as to generate an anchoring effect of an organic and inorganic interface, thereby forming the pretreatment layer.
The pretreatment layer is a plating layer of NiCr, SUS or Si and the like, the thickness of the pretreatment layer is 2-15 nm, the adhesion force between the SiOx or AlOx plating layer and the bottom coating is increased, the pretreatment layer is in a vacuum chamber, plasma is excited at first by high corona, and then molecules on the surface layer of a target material of NiCr, SUS or Si are combined with the surface of the coating by plasma excitation, so that the anchoring effect of an organic interface and an inorganic interface is formed.
Preferably, in step D, the vapor deposition includes one or more of physical vapor deposition and chemical vapor deposition.
The inorganic coating is SiOx or AlOx with the thickness of 10-50 nm, the physical microcosmic compactness of SiOx and AlOx and the adsorption of molecular unsaturated bonds to gas molecules are utilized to form a functional layer with excellent vapor and oxygen barrier performance and high transparency, the coating is a non-metal layer and can be detected through metal detection by microwave heating, the coating is prepared through a PVD (physical vapor deposition) or CVD (chemical vapor deposition) process, the PVD processing mode is that the gas pressure is less than or equal to 4.0x10 < -4 > mbar in a high-vacuum chamber, a nano SiOx or AlOx coating is formed by adopting a high-energy electron beam thermal evaporation or crucible heating evaporation mode, or plasma is formed under the high voltage, an Si target or an Al target material is bombarded under the controlled action, the SiOx or AlOx target material reacts with the introduced process gas O2 to form a compact nano coating on the surface of the base coat, the SiOx layer can also be deposited by adopting a CVD (chemical vapor deposition) mode, the plasma is discharged by utilizing gas ionization to generate the thin gas under the high-frequency electric field, the SiOx gas is generated in the high-frequency electric field, the raw material gas is reacted with the silicon oxide (silicon oxide) in the oxygen-containing silicon (silicon oxide) to form compact surface on the silicon oxide substrate. The reaction deposition temperature is generally 200-400 ℃.
Preferably, in the step B, the coating comprises one or more of gravure coating and narrow slit coating, and the curing comprises one or more of heat drying curing and UV curing.
The thickness of the bottom coating is 0.1-2 um, the adhesive force between the coating and the PLA or PBAT degradable base materials is increased, the bottom coating is polyurethane or acrylic paint, the polyurethane or acrylic paint is uniformly coated on the PLA or PBAT surface in a gravure or narrow slit coating mode, and the coating is treated through a hot baking or UV curing process, so that the internal polymer reaction crosslinking of the paint is finally cured on the base material surface.
Preferably, in the step E, the coating comprises one or more of gravure coating and narrow slit coating, and the curing comprises one or more of heat drying curing and UV curing.
Preferably, in the step E, the temperature of the curing process is 40-60 ℃, and the time of the curing process is 48-120 hours.
The surface coating also has the function of blocking water vapor and oxygen, simultaneously protects SiOx or AlOx plating layers with the thickness of 0.1-2 um, uses polyurethane or PVA (polyvinyl alcohol) and other coatings, uniformly coats polyurethane or acrylic coatings on the surface of PLA or PBAT and other biodegradable substrates in a gravure or narrow slit coating mode, treats the coatings through a thermal baking or UV curing process, finally cures the interiors of the coatings on the surface of the substrate through a crosslinking reaction, and adopts a curing process of 40-60 degrees Cx 48H-120H after the coating process is finished, so that reactive crosslinking of polymers of the coatings is more sufficient and stable.
And the heat sealing layer is used for heat sealing in the packaging process. The heat sealing layer adopts modified PLA or modified PBAT, the melting point of the modified PLA or PBAT is lower than that of common PLA or PBAT, the thickness is about 8% -15% of the total thickness, the heat sealing layer is formed by heat sealing under the conditions of 85 ℃ and 0.1mpa and 0.5-3S, and the heat sealing strength can reach more than 2.5N/15 mm.
The implementation of the invention has the following beneficial effects:
The barrier film and the heat-sealing bag manufactured after being coated and coated by PLA or PBAT base materials are degradable, reduce carbon footprint, accord with global environmental protection policy trend, have excellent barrier performance, protect contents from being influenced by water vapor or oxygen, have good transparency, can visually and clearly see the state of the contents, can be heated by microwaves because the barrier layer is SiOx or AlOx nonmetal and is oxide, and are also convenient for detecting whether metal residues exist in the packaging bag in a scanning mode. Biodegradable plastics are very environmentally friendly and once in contact with soil, the material will begin the biodegradation process. Can be naturally degraded in the landfill site. Biodegradable plastics do not have any impact on the solid waste collection and recovery system and also reduce the associated collection costs.
The invention particularly adopts biodegradable biaxially oriented PLA or PBAT and other base materials, and adopts vacuum coating and coating processing to manufacture transparent high-barrier film, which combines the package functionality and degradable environmental protection, and adopts coating (SiOx or AlOx) coating processing to ensure that the material has high barrier property and the protection content is not damaged by oxygen, water vapor and the like, and simultaneously, the coating (SiOx or AlOx) coating material is transparent, so that the transparency of the package can be realized, and the package content is clearly visible. The blocking layer is made of SiOx or AlOx nonmetal and is oxide, so that microwave heating can be performed, and whether metal residues exist in the packaging bag or not can be detected in a scanning mode conveniently.
Drawings
FIG. 1 is a schematic view of the degradable transparent high barrier film structure of the present invention.
Detailed Description
Example 1
As shown in figure 1, the degradable transparent high-barrier film comprises six layers of films, namely a top coating layer, an inorganic plating layer, a pretreatment layer, a bottom coating layer, a substrate layer and a heat sealing layer.
The preparation method comprises the following steps:
A. bonding a heat sealing layer on one side of a substrate layer, and co-extruding and stretching to obtain a substrate layer material with one side bonded with the heat sealing layer;
B. coating a primer coating material on the other side of the substrate layer material of the single-sided bonding heat seal layer, and forming a primer coating after curing;
C. vacuum coating is carried out on the bottom coating to form a pretreatment layer;
D. vapor deposition is carried out on the pretreatment layer to form an inorganic coating;
E. And (3) coating a surface coating material on the inorganic coating, curing, and curing at 45 ℃ for 72 hours to form the surface coating, thereby obtaining the degradable transparent high-barrier film.
In this example, the topcoat was 1um thick polyurethane, the inorganic coating was 30nm thick AlOx, the pretreatment layer was 10nm thick NiCr coating, the primer layer was 1um thick acrylic coating, the substrate layer was 40um thick PLA, and the heat seal layer was 4um thick modified PLA.
Example 2
As shown in figure 1, the degradable transparent high-barrier film comprises six layers of films, namely a top coating layer, an inorganic plating layer, a pretreatment layer, a bottom coating layer, a substrate layer and a heat sealing layer.
The preparation method comprises the following steps:
A. bonding a heat sealing layer on one side of a substrate layer, and co-extruding and stretching to obtain a substrate layer material with one side bonded with the heat sealing layer;
B. coating a primer coating material on the other side of the substrate layer material of the single-sided bonding heat seal layer, and forming a primer coating after curing;
C. vacuum coating is carried out on the bottom coating to form a pretreatment layer;
D. vapor deposition is carried out on the pretreatment layer to form an inorganic coating;
E. And (3) coating a top coating material on the inorganic coating, curing, and then curing at 40 ℃ for 120 hours to form the top coating, thereby obtaining the degradable transparent high-barrier film.
In this example, the topcoat was a 2um thick PVA, the inorganic coating was a 50nm thick SiOx, the pretreatment layer was a 15nm thick SUS coating, the primer was a 2um thick polyurethane-based coating, the substrate layer was a 100um thick PBAT, and the heat seal layer was a 10um thick modified PBAT.
Example 3
As shown in figure 1, the degradable transparent high-barrier film comprises six layers of films, namely a top coating layer, an inorganic plating layer, a pretreatment layer, a bottom coating layer, a substrate layer and a heat sealing layer.
The preparation method comprises the following steps:
A. bonding a heat sealing layer on one side of a substrate layer, and co-extruding and stretching to obtain a substrate layer material with one side bonded with the heat sealing layer;
B. coating a primer coating material on the other side of the substrate layer material of the single-sided bonding heat seal layer, and forming a primer coating after curing;
C. vacuum coating is carried out on the bottom coating to form a pretreatment layer;
D. vapor deposition is carried out on the pretreatment layer to form an inorganic coating;
E. And (3) coating a top coating material on the inorganic coating, curing, and then curing at 60 ℃ for 48 hours to form the top coating, thereby obtaining the degradable transparent high-barrier film.
In this example, the topcoat was 0.1um thick polyurethane, the inorganic coating was 10nm thick SiOx, the pretreatment layer was 2nm thick Si coating, the primer layer was 0.1um thick polyurethane-based coating, the substrate layer was 15um thick PLA, and the heat seal layer was 1um thick modified PLA.
Comparative example 1
The materials and the process as in example 1 are selected, and the difference is that step D is omitted, and other steps are unchanged, namely, the five-layer film barrier film without inorganic coating is prepared.
Comparative example 2
The materials and processes of example 1 were selected, except that step C was omitted and the other steps were unchanged, i.e., five-layer film barrier films without pretreatment layers were prepared.
Comparative example 3
The materials and processes of example 2 were selected, which were different in that step C was omitted and the other steps were unchanged, i.e. a five-layer film barrier film without a pretreatment layer was prepared.
Effect example 1
Performance tests were performed on the barrier films prepared in examples 1 to 3 and comparative examples 1 to 3, and the respective index test methods or instruments were as follows:
Light transmittance: ASTM D1003. The light transmittance of the barrier film material is tested under the room temperature condition (23+/-2 ℃) by adopting a spectrophotometer.
Visual appearance color. Specifically, under the condition of room temperature (23+/-2 ℃) and a fluorescent lamp, the film surface is 30cm to 40cm away from the film surface, visual observation is carried out, and whether the substrate is transparent or not is evaluated.
Initial Water penetration WVTR-ASTM F1249 MOCON. Cutting a sample piece of the barrier film by using a sampler, putting the sample piece into a professional water vapor transmittance tester, setting the relative humidity of 38 ℃ and 90% in the tester for measurement, and testing the water vapor amount transmitted per square meter of the barrier film every day. The unit is g/m2/day.
Initial oxygen permeation OTR ASTM D3985 MOCON. Cutting a barrier film sample by using a sampler, putting the sample into a professional oxygen transmittance tester, setting 23 ℃ and 0% relative humidity in the tester for measurement, and testing the amount of oxygen transmitted per square meter of barrier film every day. The unit is cc/m2/day.
Initial adhesion ASTM D3359-09. Drawing a hundred grid pattern on the barrier film by using a hundred grid knife, attaching the barrier film to the surface of the coating by using a 3M610 adhesive tape, pulling the adhesive tape open, and evaluating the shedding area of the coating and the plating layer. The adhesive force is 5B when no falling exists, the falling area is 4B when the falling area is less than 5%, the falling area is 3B when the falling area is 5% -15%, the falling area is 15% -35%, the falling area is 2B when the falling area is 35% -65%, the falling area is 2B, and the falling area is 0B when the falling area is more than 65%.
The interlayer stripping force after compounding is GB/T8808-88. The method comprises the steps of respectively clamping two layers of film materials of a composite sample by two ends of an electronic tension meter under the room temperature condition (23+/-2 ℃), wherein the two layers of film materials are 180 degrees, and the average value of the tension is automatically recorded by the electronic tension machine to be the stripping force according to the speed of 30 mm/min.
The test design is shown in table 1:
TABLE 1
Among them, the barrier film is a film having barrier properties against water vapor and oxygen, and the better the barrier properties, the lower the Water Vapor Transmission Rate (WVTR) and Oxygen Transmission Rate (OTR).
From the test results, it can be seen that if only the NiCr or SUS layer is plated, the adhesion and the interlayer peeling force after compounding are good, but the sample after plating has basically no barrier property, and if only the SiOx or AlOx layer is plated, the adhesion is poor. Only when the proposal of the invention is used for plating the NiCr/SUS+SiOx or plating the NiCr/SUS+AlOx layer simultaneously, the adhesive force, the interlayer stripping force and the barrier property are provided.
The above disclosure is only a preferred embodiment of the present invention, and it is needless to say that the scope of the invention is not limited thereto, and therefore, the equivalent changes according to the claims of the present invention still fall within the scope of the present invention.
Claims (9)
1. The degradable transparent high-barrier film is characterized by comprising six layers of films, wherein the films sequentially comprise a top coating, an inorganic coating, a pretreatment layer, a bottom coating, a substrate layer and a heat sealing layer, the pretreatment layer comprises one or more of an SUS coating and an Si coating, and the inorganic coating comprises one or more of an SiOx coating and an AlOx coating;
the preparation of the degradable transparent high-barrier film comprises the following steps:
A. Bonding the heat sealing layer on one side of the substrate layer, and co-extruding and stretching to obtain a substrate layer material with one side bonded with the heat sealing layer;
B. Coating a primer coating material on the other side of the substrate layer material of the single-sided bonding heat sealing layer, and forming the primer coating after curing;
C. vacuum coating is carried out on the bottom coating layer to form the pretreatment layer;
D. vapor deposition is carried out on the pretreatment layer to form the inorganic coating;
E. Coating a surface coating material on the inorganic coating, curing, and then curing to form the surface coating, thus obtaining the degradable transparent high-barrier film.
2. The degradable transparent high barrier film according to claim 1, wherein the topcoat comprises one or more of a polyurethane coating, a PVA coating, the basecoat comprises one or more of a polyurethane-based coating, an acrylic coating, the substrate layer comprises one or more of a PLA substrate, a PBAT substrate, and the heat seal layer comprises one or more of a modified PLA, a modified PBAT.
3. The degradable transparent high-barrier film according to claim 1, wherein the thickness of the top coating is 0.1-2 um, the thickness of the inorganic coating is 10-50 nm, the thickness of the pretreatment layer is 2-15 nm, the thickness of the bottom coating is 0.1-2 um, the thickness of the base material layer is 15-100 um, and the thickness of the heat sealing layer is 1-10 um.
4. A method of making the degradable transparent high barrier film of claim 1, comprising the steps of:
A. Bonding the heat sealing layer on one side of the substrate layer, and co-extruding and stretching to obtain a substrate layer material with one side bonded with the heat sealing layer;
B. Coating a primer coating material on the other side of the substrate layer material of the single-sided bonding heat sealing layer, and forming the primer coating after curing;
C. vacuum coating is carried out on the bottom coating layer to form the pretreatment layer;
D. vapor deposition is carried out on the pretreatment layer to form the inorganic coating;
E. Coating a surface coating material on the inorganic coating, curing, and then curing to form the surface coating, thus obtaining the degradable transparent high-barrier film.
5. The method of claim 4, wherein in step C, the vacuum coating comprises exciting a plasma in a vacuum chamber, and then exciting target surface molecules to combine with the primer layer by the plasma to generate an anchoring effect of an organic and inorganic interface, thereby forming the pretreatment layer.
6. The method of claim 4, wherein in step D, the vapor deposition comprises one or more of physical vapor deposition and chemical vapor deposition.
7. The method of producing a degradable transparent high barrier film according to claim 4, wherein in the step B, the coating comprises one or more of gravure coating and narrow slit coating, and the curing comprises one or more of baking curing and UV curing.
8. The method of producing a degradable transparent high barrier film according to claim 4, wherein in step E, the coating comprises one or more of gravure coating and narrow slit coating, and the curing comprises one or more of baking curing and UV curing.
9. The method for preparing a degradable transparent high-barrier film according to claim 4, wherein in the step E, the curing process is performed at a temperature of 40-60 ℃ and the curing process is performed for 48-120 hours.
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