CN113524843A - High-barrier composite film and preparation method thereof - Google Patents
High-barrier composite film and preparation method thereof Download PDFInfo
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- CN113524843A CN113524843A CN202110885312.5A CN202110885312A CN113524843A CN 113524843 A CN113524843 A CN 113524843A CN 202110885312 A CN202110885312 A CN 202110885312A CN 113524843 A CN113524843 A CN 113524843A
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- layer
- barrier composite
- monomer
- composite film
- adhesive
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- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title abstract description 22
- 239000000178 monomer Substances 0.000 claims abstract description 67
- 239000003999 initiator Substances 0.000 claims abstract description 37
- 239000010410 layer Substances 0.000 claims abstract description 34
- 238000000576 coating method Methods 0.000 claims abstract description 33
- 239000011248 coating agent Substances 0.000 claims abstract description 31
- 239000000853 adhesive Substances 0.000 claims abstract description 28
- 230000001070 adhesive effect Effects 0.000 claims abstract description 28
- 239000008234 soft water Substances 0.000 claims abstract description 24
- 239000000839 emulsion Substances 0.000 claims abstract description 23
- 229920001684 low density polyethylene Polymers 0.000 claims abstract description 22
- 239000004702 low-density polyethylene Substances 0.000 claims abstract description 22
- 239000012790 adhesive layer Substances 0.000 claims abstract description 18
- 239000003607 modifier Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 238000004132 cross linking Methods 0.000 claims abstract description 15
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 15
- 230000004888 barrier function Effects 0.000 claims abstract description 14
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 12
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract 6
- 239000000243 solution Substances 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 238000007731 hot pressing Methods 0.000 claims description 13
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000003851 corona treatment Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 5
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 3
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 3
- 125000005442 diisocyanate group Chemical group 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims 1
- 239000012205 single-component adhesive Substances 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 description 17
- 239000004698 Polyethylene Substances 0.000 description 8
- 238000004806 packaging method and process Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 238000013329 compounding Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- -1 polyethylene terephthalate Polymers 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000007756 gravure coating Methods 0.000 description 4
- 238000007602 hot air drying Methods 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000010816 packaging waste Substances 0.000 description 3
- 239000005033 polyvinylidene chloride Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- 235000006226 Areca catechu Nutrition 0.000 description 1
- 244000080767 Areca catechu Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000011127 biaxially oriented polypropylene Substances 0.000 description 1
- 229920006378 biaxially oriented polypropylene Polymers 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
- B29C65/4865—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding containing additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/01—General aspects dealing with the joint area or with the area to be joined
- B29C66/02—Preparation of the material, in the area to be joined, prior to joining or welding
- B29C66/028—Non-mechanical surface pre-treatments, i.e. by flame treatment, electric discharge treatment, plasma treatment, wave energy or particle radiation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/40—General aspects of joining substantially flat articles, e.g. plates, sheets or web-like materials; Making flat seams in tubular or hollow articles; Joining single elements to substantially flat surfaces
- B29C66/41—Joining substantially flat articles ; Making flat seams in tubular or hollow articles
- B29C66/45—Joining of substantially the whole surface of the articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered 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
- B32B27/08—Layered 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 of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/40—Applications of laminates for particular packaging purposes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/20—Esters of polyhydric alcohols or phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/24—Homopolymers or copolymers of amides or imides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2009/00—Layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/726—Permeability to liquids, absorption
- B32B2307/7265—Non-permeable
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2439/00—Containers; Receptacles
- B32B2439/70—Food packaging
Abstract
The invention provides a high-barrier composite film, which comprises: a BOPE layer; a layer of LDPE; an adhesive layer disposed between the BOPE layer and the LDPE layer; the adhesive layer includes: 55-70 wt% of soft water; 10-18 wt% of a hydrophilic monomer; 8-15 wt% of functional monomer; 2-8 wt% of a crosslinking monomer; 0.5-4 wt% of an emulsifier; 0.3-2 wt% of an initiator; 0.5-3 wt% of a neutralizing agent; 0.8 to 4 wt% of a modifier. The adhesive provided by the invention is a single-component adhesive, the bonding force is strong, and the performance of the manufactured high-barrier composite film is excellent; because the modifier is added in the preparation of the emulsion, the emulsion is separated out on the surface of the coating in a micro flaky structure after being coated and dried, and the better barrier property is promoted. The invention also provides a preparation method of the high-barrier composite layer.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a high-barrier composite film and a preparation method thereof.
Background
In the current food packaging in the market, most of high-barrier coating films are compounded with PE or CPP (polyethylene terephthalate) through adhesives to form bags for packaging, so that the performances of sealing, blocking oxygen and water vapor and the like are provided, and the food retention period is prolonged. Therefore, high barrier composite films occupy a large portion of the food packaging market.
Chinese patent publication No. CN203077750U discloses a coating composite film suitable for sauce packaging, which is prepared by coating a high-barrier PVDC coating on a PET substrate, coating an adhesive on the coating, and compounding the coating with a PE film to form a bag, so as to meet the requirements of food packaging performance. However, the PVDC coating film cannot be recycled, and the PE film compounded therewith cannot be recycled; in addition, the waste can generate substances such as hydrogen chloride, dioxin and the like which are toxic and harmful to human bodies and the surrounding environment when being incinerated. At present, countries such as Europe and America and the like replace PVDC coatings by other environment-friendly materials.
With the rising demand of the public for green health and the stricter national environmental regulations, the environmental protection, non-toxicity and performance diversification of the packaging material will be the inevitable trend. For example, chinese patent publication No. CN103264559A discloses an areca-nut packaging composite film and a method for preparing the same, which comprises coating an environment-friendly high-barrier polyvinyl alcohol coating on a BOPP film, and then compounding with a PE film by using an adhesive to make a bag. Although the packaging material with the structure can be completely combusted after use or recycled for re-granulation; however, the production process is complicated, a coater and a compound machine are required to be equipped, and a large amount of organic solvent is required to be used as primer in the process of coating the high-barrier coating. Therefore, if the coating process can be saved, the production efficiency can be greatly improved and the production cost can be reduced.
In conclusion, the development of a novel high-barrier composite film for food packaging has become a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In view of this, the present invention provides a high-barrier composite film and a method for preparing the same, and the high-barrier composite film provided by the present invention has a good barrier property.
The invention provides a high-barrier composite film, which comprises:
a BOPE layer;
a layer of LDPE;
an adhesive layer disposed between the BOPE layer and the LDPE layer;
the adhesive layer includes:
55-70 wt% of soft water;
10-18 wt% of a hydrophilic monomer;
8-15 wt% of functional monomer;
2-8 wt% of a crosslinking monomer;
0.5-4 wt% of an emulsifier;
0.3-2 wt% of an initiator;
0.5-3 wt% of a neutralizing agent;
0.8-4 wt% of a modifier; the modifier is selected from one or more of montmorillonite and kaolin.
Preferably, the thickness of the BOPE layer is 30-50 micrometers;
the thickness of the LDPE layer is 40-60 microns.
Preferably, the hydrophilic monomer is selected from one or more of hydroxyethyl acrylate, hydroxypropyl acrylate and N-methylol acrylamide.
Preferably, the functional monomer is selected from one or more of methacrylic acid and lauryl acrylate.
Preferably, the crosslinking monomer is selected from one or more of aziridine and diisocyanate.
Preferably, the emulsifier is selected from one or more of secondary alkyl sodium sulfonate, sodium dodecyl sulfonate and sodium dodecyl benzene sulfonate.
Preferably, the initiator is selected from one or more of tert-butyl hydroperoxide and potassium persulfate.
Preferably, the neutralizing agent is one or more selected from triethylamine and ammonia water.
The invention provides a preparation method of a high-barrier composite film, which comprises the following steps:
carrying out corona treatment on one surface of the BOPE base material to obtain a corona surface;
coating an adhesive on the corona surface and then drying to obtain an adhesive layer;
and carrying out hot pressing on the adhesive layer and the LDPE film to obtain the high-barrier composite layer.
Preferably, the preparation method of the adhesive comprises the following steps:
firstly mixing a functional monomer, a crosslinking monomer and an emulsifier to obtain a pre-emulsified monomer;
secondly, mixing the initiator and part of the soft water to obtain an initiator solution;
reacting the rest soft water, the hydrophilic monomer, part of the pre-emulsified monomer and part of the initiator solution to obtain emulsion;
carrying out third mixing on the emulsion, the residual pre-emulsified monomer and the residual initiator solution, and then carrying out heat preservation to obtain a mixed solution;
and fourthly, mixing the mixed solution, the neutralizing agent and the modifying agent to obtain the adhesive.
The high-barrier composite adhesive provided by the invention is a single-component adhesive, the bonding force is strong, and the manufactured high-barrier composite film has excellent performance; because the modifier is added in the preparation of the emulsion, the emulsion is separated out on the surface of the coating in a micro flaky structure after being coated and dried, and the better barrier property is promoted; the preparation method provided by the invention has the advantages of simple process, mild and easily-controlled conditions, and the effect of the traditional coating composite film can be achieved only by one compounding process after the emulsion preparation is finished; the inner layer and the outer layer of the high-barrier composite film provided by the invention are made of polyethylene, and the used packaging waste is favorable for recycling, so that the resource recycling is realized.
Drawings
Fig. 1 is a schematic structural diagram of a high-barrier composite film according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The structure schematic diagram of the high-barrier composite film provided by the embodiment of the invention is shown in fig. 1, and the invention provides the high-barrier composite film, which comprises the following components:
a BOPE layer 1;
an LDPE layer 3;
and the adhesive layer 2 is arranged between the BOPE layer and the LDPE layer.
In the invention, the thickness of the BOPE (biaxially oriented polyethylene film) layer is preferably 30-50 microns, more preferably 35-45 microns, and most preferably 40 microns.
In the invention, the thickness of the LDPE (low density polyethylene) layer is preferably 40-60 micrometers, more preferably 45-55 micrometers, and most preferably 50 micrometers.
In the invention, the thickness of the adhesive layer is preferably 3-5 micrometers, more preferably 3.5-4.5 micrometers, and most preferably 4 micrometers.
In the present invention, the adhesive layer includes:
55-70 wt% of soft water;
10-18 wt% of a hydrophilic monomer;
8-15 wt% of functional monomer;
2-8 wt% of a crosslinking monomer;
0.5-4 wt% of an emulsifier;
0.3-2 wt% of an initiator;
0.5-3 wt% of a neutralizing agent;
0.8 to 4 wt% of a modifier.
In the present invention, the mass content of the soft water is preferably 60 to 65%, and more preferably 62 to 63%. The soft water used in the present invention is not particularly limited, and those known to those skilled in the art can be used.
In the present invention, the mass content of the hydrophilic monomer is preferably 12 to 16%, and more preferably 14%.
In the present invention, the hydrophilic monomer is preferably one or more selected from the group consisting of hydroxyethyl acrylate, hydroxypropyl acrylate and N-methylol acrylamide.
In the invention, the mass content of the functional monomer is preferably 10-13%, and more preferably 11-12%.
In the present invention, the functional monomer is preferably selected from one or more of methacrylic acid and lauryl acrylate.
In the present invention, the mass content of the crosslinking monomer is preferably 4 to 6%, and more preferably 5%.
In the present invention, the crosslinking monomer is preferably selected from one or more of aziridine and diisocyanate.
In the present invention, the mass content of the emulsifier is preferably 1 to 3%, and more preferably 2%.
In the present invention, the emulsifier is preferably one or more selected from the group consisting of secondary alkyl sodium sulfonate, sodium dodecyl sulfonate and sodium dodecyl benzene sulfonate.
In the present invention, the mass content of the initiator is preferably 0.5 to 1.5%, more preferably 0.8 to 1.2%, and most preferably 1%.
In the present invention, the initiator is preferably one or more selected from the group consisting of t-butyl hydroperoxide and potassium persulfate.
In the present invention, the mass content of the neutralizing agent is preferably 1 to 2%, more preferably 1.5%.
In the present invention, the neutralizing agent is preferably one or more selected from triethylamine and ammonia water.
In the present invention, the mass content of the modifier is preferably 1 to 3%, more preferably 2%.
In the invention, the modifier is selected from one or more of montmorillonite and kaolin.
The invention provides a preparation method of a high-barrier composite film, which comprises the following steps:
carrying out corona treatment on one surface of the BOPE base material to obtain a corona surface;
coating an adhesive on the corona surface and then drying to obtain an adhesive layer;
and carrying out hot pressing on the adhesive layer and the LDPE film to obtain the high-barrier composite layer.
In the present invention, the BOPE substrate may be a BOPE film, which is the same as the BOPE layer in the above technical solution, and is not described herein again. In the present invention, the BOPE substrate is preferably a product prepared according to the method disclosed in the CN111452473A patent.
In the invention, the corona is preferably carried out so that the surface tension of the BOPE base material after corona is 40-45 dyne, more preferably 41-44 dyne, and most preferably 42-43 dyne; the corona treatment is preferably performed on a dry compound machine.
In the present invention, the coating is preferably performed using a gravure coating roll; the coating weight of the coating is preferably 3-5 g/m2More preferably 4g/m2。
In the present invention, the preparation method of the adhesive preferably includes:
firstly mixing a functional monomer, a crosslinking monomer and an emulsifier to obtain a pre-emulsified monomer;
secondly, mixing the initiator and part of the soft water to obtain an initiator solution;
reacting the rest soft water, the hydrophilic monomer, part of the pre-emulsified monomer and part of the initiator solution to obtain emulsion;
carrying out third mixing on the emulsion, the residual pre-emulsified monomer and the residual initiator solution, and then carrying out heat preservation to obtain a mixed solution;
and fourthly, mixing the mixed solution, the neutralizing agent and the modifying agent to obtain the adhesive.
In the present invention, the components and mass contents of the soft water, the hydrophilic monomer, the functional monomer, the crosslinking monomer, the emulsifier, the initiator, the neutralizer and the modifier are consistent with those described in the above technical solution, and are not described herein again.
In the present invention, the first mixing is preferably performed under stirring; the stirring speed is preferably 100-150 rpm, more preferably 110-140 rpm, and most preferably 120-130 rpm; the time for the first mixing is preferably 0.5 to 1 hour, more preferably 0.6 to 0.9 hour, and most preferably 0.7 to 0.8 hour.
In the present invention, the part of the soft water is preferably 25 to 35%, more preferably 28 to 32%, and most preferably 30% of the total mass of the soft water.
In the invention, the part of the pre-emulsified monomers is preferably 3-5% of the total mass of the pre-emulsified monomers, and more preferably 4%.
In the invention, the part of the initiator solution is preferably 1-3% of the total mass of the initiator solution, and more preferably 2%.
In the present invention, the reaction is preferably carried out in a reaction vessel; the reaction condition is preferably sealed vacuum negative pressure; the reaction is preferably carried out under the condition of stirring, and the stirring speed is preferably 150-200 rpm, more preferably 160-190 rpm, and most preferably 170-180 rpm; the reaction temperature is preferably 80-85 ℃, more preferably 81-84 ℃, and most preferably 82-83 ℃; the reaction time is preferably 0.5 to 1 hour, more preferably 0.6 to 0.9 hour, and most preferably 0.7 to 0.8 hour. In the present invention, the emulsion is a milky bluish emulsion.
In the present invention, the third mixing method preferably includes:
the remaining pre-emulsified monomer and the remaining initiator solution are added dropwise to the emulsion.
In the present invention, it is preferable that the remaining pre-emulsified monomer and the remaining initiator solution are respectively and continuously dropped by a metering pump; the dripping time is preferably 3 to 5 hours, and more preferably 4 hours.
In the invention, the temperature of the heat preservation is preferably 65-75 ℃, more preferably 68-72 ℃, and most preferably 70 ℃; the heat preservation time is preferably 0.5 to 1 hour, more preferably 0.6 to 0.9 hour, and most preferably 0.7 to 0.8 hour.
In the present invention, the fourth mixing is preferably performed under stirring, and the time of the fourth mixing is preferably 0.5 to 1 hour, more preferably 0.6 to 0.9 hour, and most preferably 0.7 to 0.8 hour.
In the present invention, it is preferable that the fourth mixing step further includes:
and standing the obtained mixture, and cooling to obtain the high-resistance waterproof composite adhesive.
In the invention, the drying temperature is preferably 60-80 ℃, more preferably 65-75 ℃, and most preferably 70 ℃; the drying is preferably carried out in an oven; the drying method is preferably far infrared or hot air drying.
In the present invention, the LDPE film is the same as the LDPE layer in the above technical solution, and is not described herein again. In the present invention, the LDPE film is preferably a product prepared according to the method disclosed in the CN111040363A patent.
In the invention, the hot pressing is preferably carried out by using a composite compression roller; the hot pressing temperature is preferably 50-60 ℃, more preferably 52-58 ℃ and most preferably 54-56 ℃; the pressure of the hot pressing is preferably 0.1-0.3 MPa, and more preferably 0.2 MPa.
In the invention, the high-barrier composite film is obtained by rolling preferably after hot pressing.
The high-barrier composite adhesive provided by the invention is a single-component adhesive, the bonding force is strong, and the manufactured high-barrier composite film has excellent performance; because the modifier is added in the preparation of the emulsion, the emulsion is separated out on the surface of the coating in a micro flaky structure after being coated and dried, and the better barrier property is promoted; the preparation method provided by the invention has the advantages of simple process, mild and easily-controlled conditions, and the effect of the traditional coating composite film can be achieved only by one compounding process after the emulsion preparation is finished; the inner layer and the outer layer of the high-barrier composite film provided by the invention are made of polyethylene, and the used packaging waste is favorable for recycling, so that the resource recycling is realized.
The BOPE base material adopted in the following embodiments of the invention is prepared according to the preparation method disclosed in embodiment 3 of Chinese patent CN 110450490A, and the puncture resistance strength is 6-8N/mm; the LDPE film is prepared according to the preparation method disclosed in embodiment 1 of Chinese patent CN111040363A, and the tensile strength is 20-25 MPa.
Comparative example 1
The product obtained was prepared according to the procedure of example 1 in patent CN 110861380A.
Example 1
1. The weight ratio and the specific type of the raw materials of the high-barrier composite adhesive are limited:
2. preparing high-barrier composite glue:
(1) mixing and stirring 14 wt% of functional monomer, 8 wt% of crosslinking monomer and 3 wt% of emulsifier for 0.5 hour, and controlling the stirring speed at 150 revolutions per minute to obtain pre-emulsified monomer;
(2) dissolving 0.5 wt% of initiator with part of soft water (accounting for 30 wt% of the total amount of the soft water) to prepare an initiator solution;
(3) adding the rest soft water, 18 wt% of hydrophilic monomer, 3 wt% of pre-emulsified monomer and 1 wt% of initiator solution into a reaction kettle, sealing, vacuumizing to-0.05 MPa, controlling the stirring speed at 150 rpm, and heating to 83 ℃ for reaction for about 0.8 hour to obtain milky bluish emulsion.
(4) The remaining pre-emulsified monomer and initiator solution were continuously added by a metering pump, and the dropping time was controlled to 3 hours.
(5) After the feeding is finished, keeping the temperature at 67 ℃ for 0.7 hour, then adding 0.5 wt% of neutralizing agent and 1 wt% of modifier, fully stirring for 0.5 hour, standing and cooling to obtain the high-resistance waterproof composite adhesive.
3. Manufacture of high barrier composite films
Performing corona treatment on the surface to be coated of the BOPE base material with 30 microns of puncture resistance strength of 6N/mm on a dry type composite machine to enable the surface tension to reach 45 dynes; coating the high-barrier adhesive on the corona surface of the BOPE film by using a gravure coating roller, wherein the coating amount is 5g/m25 microns thick; far infrared or hot air drying is carried out, the temperature of an oven is set to be 80 ℃, after drying of the oven, a composite compression roller is used for carrying out hot pressing on an adhesive layer on BOPE and a 60-micron LDPE film with the tensile strength of 25MPa, the hot pressing temperature is 50 ℃, and the pressure is 0.3 MPa; and rolling to obtain the novel high-barrier composite film.
Example 2
1. The weight ratio and the specific type of the raw materials of the high-barrier composite adhesive are limited:
2. preparation of high-barrier composite adhesive
(1) Mixing and stirring 10 wt% of functional monomer, 4 wt% of crosslinking monomer and 1.7 wt% of emulsifier for 1 hour, and controlling the stirring speed to be 100 r/min to obtain pre-emulsified monomer;
(2) dissolving 0.3 wt% of initiator with part of soft water (accounting for 30% of the total amount of the soft water) to prepare an initiator solution;
(3) adding the rest soft water, 12 wt% of hydrophilic monomer, 4 wt% of pre-emulsified monomer and 2 wt% of initiator solution into a reaction kettle, sealing, vacuumizing to-0.06 MPa, controlling the stirring speed at 200 r/min, and heating to 80 ℃ for reaction for about 1 hour to obtain milky bluish emulsion.
(4) Continuously adding the rest pre-emulsified monomers and the rest initiator solution through a metering pump; the dropping time was controlled to 5 hours.
(5) After the charging is finished, keeping the temperature at 65 ℃ for 1 hour, and then adding 3 wt% of neutralizer and 4 wt% of modifier; and after fully stirring for 0.8 hour, standing and cooling to obtain the high-resistance waterproof composite adhesive.
3. Manufacture of high barrier composite films
Performing corona treatment on the surface to be coated of the BOPE base material with the puncture strength of 7N/mm of 40 microns on a dry type compound machine to enable the surface tension to reach 43 dynes; coating the high-barrier adhesive on the corona surface of the BOPE film by using a gravure coating roller, wherein the coating amount is 4g/m2Thickness of 4 microns; far infrared or hot air drying is carried out, the temperature of an oven is set to be 70 ℃, after drying of the oven, a composite compression roller is used for carrying out hot pressing on an adhesive layer on BOPE and a LDPE film with the tensile strength of 23MPa of 50 microns, the hot pressing temperature is 55 ℃, and the pressure is 0.2 MPa; and rolling to obtain the novel high-barrier composite film.
Example 3
1. The weight ratio and the specific type of the raw materials of the high-barrier composite adhesive are limited:
2. preparation of high-barrier composite adhesive
(1) Mixing and stirring 9 wt% of functional monomer, 6 wt% of crosslinking monomer and 0.5 wt% of emulsifier for 0.6 hour, and controlling the stirring speed at 120 r/min to obtain pre-emulsified monomer;
(2) dissolving 2 wt% of initiator with part of soft water (accounting for 30% of the total amount of the soft water) to prepare an initiator solution;
(3) adding the rest soft water, 11 wt% of hydrophilic monomer, 5 wt% of pre-emulsified monomer and 3 wt% of initiator solution into a reaction kettle, sealing, vacuumizing to-0.04 MPa, controlling the stirring speed at 150 rpm, and heating to 85 ℃ for reaction for about 0.5 hour to obtain milky bluish emulsion.
(4) Continuously adding the rest pre-emulsified monomers and the rest initiator solution through a metering pump; the dropping time was controlled to 4 hours.
(5) After the charging is finished, continuously keeping the temperature at 75 ℃ for 0.5 hour, and then adding 0.7 wt% of neutralizer and 0.8 wt% of modifier; and fully stirring for 1 hour, standing and cooling to obtain the high-resistance waterproof composite adhesive.
3. Manufacture of high barrier composite films
Performing corona treatment on the surface to be coated of the BOPE base material with the puncture strength of 50 microns being 8N/mm on a dry type composite machine to enable the surface tension to reach 40 dynes; coating the high-barrier adhesive on the corona surface of the BOPE film by using a gravure coating roller, wherein the coating amount is 3g/m23 microns thick; far infrared or hot air drying is carried out, the temperature of an oven is set to be 60 ℃, after drying of the oven, a composite compression roller is used for carrying out hot pressing on an adhesive layer on BOPE and a LDPE film with the tensile strength of 20MPa of 40 micrometers, the hot pressing temperature is 60 ℃, and the pressure is 0.1 MPa; and rolling to obtain the novel high-barrier composite film.
Performance detection
The composite films prepared in the examples and the comparative examples of the invention are detected in peel strength, oxygen transmission rate and water vapor transmission rate, and the detection method and the detection result are as follows:
| example 1 | Example 2 | Example 3 | Comparative example 1 | Detection standard | |
| Peel strength (N/15mm) | 4 | 3 | 5 | 2.0 | GB/T8808-1988 |
| Oxygen transmission rate (cc/m)2·day) | 1 | 3 | 2 | 114 | GB/T 1038-2000 |
| Water vapor transmission rate (g/m)2·day) | 4 | 5 | 6 | 15 | GB/T 1037-1998 |
The high-barrier composite adhesive provided by the invention is a single-component adhesive, the bonding force is strong, and the manufactured high-barrier composite film has excellent performance; because the modifier is added in the preparation of the emulsion, the emulsion is separated out on the surface of the coating in a micro flaky structure after being coated and dried, and the better barrier property is promoted; the preparation method provided by the invention has the advantages of simple process, mild and easily-controlled conditions, and the effect of the traditional coating composite film can be achieved only by one compounding process after the emulsion preparation is finished; the inner layer and the outer layer of the high-barrier composite film provided by the invention are made of polyethylene, and the used packaging waste is favorable for recycling, so that the resource recycling is realized.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A high barrier composite membrane comprising:
a BOPE layer;
a layer of LDPE;
an adhesive layer disposed between the BOPE layer and the LDPE layer;
the adhesive layer includes:
55-70 wt% of soft water;
10-18 wt% of a hydrophilic monomer;
8-15 wt% of functional monomer;
2-8 wt% of a crosslinking monomer;
0.5-4 wt% of an emulsifier;
0.3-2 wt% of an initiator;
0.5-3 wt% of a neutralizing agent;
0.8-4 wt% of a modifier; the modifier is selected from one or more of montmorillonite and kaolin.
2. The high-barrier composite film according to claim 1, wherein the thickness of the BOPE layer is 30-50 microns;
the thickness of the LDPE layer is 40-60 microns.
3. The high barrier composite film according to claim 1, wherein the hydrophilic monomer is one or more selected from hydroxyethyl acrylate, hydroxypropyl acrylate and N-methylol acrylamide.
4. The high barrier composite film according to claim 1, wherein the functional monomer is selected from one or more of methacrylic acid and lauryl acrylate.
5. The high barrier composite film according to claim 1, wherein the crosslinking monomer is selected from one or more of aziridine and diisocyanate.
6. The high-barrier composite film according to claim 1, wherein the emulsifier is one or more selected from the group consisting of secondary alkyl sodium sulfonate, sodium dodecyl sulfonate and sodium dodecyl benzene sulfonate.
7. The high-barrier composite film according to claim 1, wherein the initiator is selected from one or more of tert-butyl hydroperoxide and potassium persulfate.
8. The high barrier composite film according to claim 1, wherein the neutralizing agent is one or more selected from triethylamine and ammonia water.
9. A method for preparing the high-barrier composite film according to claim 1, comprising the following steps:
carrying out corona treatment on one surface of the BOPE base material to obtain a corona surface;
coating an adhesive on the corona surface and then drying to obtain an adhesive layer;
and carrying out hot pressing on the adhesive layer and the LDPE film to obtain the high-barrier composite layer.
10. The method of claim 9, wherein the adhesive is prepared by a method comprising:
firstly mixing a functional monomer, a crosslinking monomer and an emulsifier to obtain a pre-emulsified monomer;
secondly, mixing the initiator and part of the soft water to obtain an initiator solution;
reacting the rest soft water, the hydrophilic monomer, part of the pre-emulsified monomer and part of the initiator solution to obtain emulsion;
carrying out third mixing on the emulsion, the residual pre-emulsified monomer and the residual initiator solution, and then carrying out heat preservation to obtain a mixed solution;
and fourthly, mixing the mixed solution, the neutralizing agent and the modifying agent to obtain the adhesive.
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| PCT/CN2021/112042 WO2023010602A1 (en) | 2021-08-03 | 2021-08-11 | High-barrier composite film and preparation method therefor |
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Application publication date: 20211022 |
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