CN115612291A - Extinction polyamide film and preparation method thereof - Google Patents
Extinction polyamide film and preparation method thereof Download PDFInfo
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- CN115612291A CN115612291A CN202211393731.8A CN202211393731A CN115612291A CN 115612291 A CN115612291 A CN 115612291A CN 202211393731 A CN202211393731 A CN 202211393731A CN 115612291 A CN115612291 A CN 115612291A
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- polyamide
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- 230000008033 biological extinction Effects 0.000 title claims abstract description 84
- 239000004952 Polyamide Substances 0.000 title claims abstract description 60
- 229920002647 polyamide Polymers 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 46
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 45
- 239000010410 layer Substances 0.000 claims abstract description 40
- 239000012792 core layer Substances 0.000 claims abstract description 36
- 239000012793 heat-sealing layer Substances 0.000 claims abstract description 35
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 14
- 229920000728 polyester Polymers 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- -1 polypropylene carbonate Polymers 0.000 claims description 27
- 229920001903 high density polyethylene Polymers 0.000 claims description 22
- 239000004700 high-density polyethylene Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 14
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 13
- 239000004698 Polyethylene Substances 0.000 claims description 13
- 229920000573 polyethylene Polymers 0.000 claims description 13
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 12
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 11
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 11
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 11
- 229920000379 polypropylene carbonate Polymers 0.000 claims description 11
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- 239000003431 cross linking reagent Substances 0.000 claims description 9
- 239000003999 initiator Substances 0.000 claims description 9
- 239000004677 Nylon Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229920001778 nylon Polymers 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000009998 heat setting Methods 0.000 claims description 3
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- IMSODMZESSGVBE-UHFFFAOYSA-N 2-Oxazoline Chemical compound C1CN=CO1 IMSODMZESSGVBE-UHFFFAOYSA-N 0.000 claims description 2
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 2
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000299 Nylon 12 Polymers 0.000 claims description 2
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 229920002961 polybutylene succinate Polymers 0.000 claims description 2
- 239000004631 polybutylene succinate Substances 0.000 claims description 2
- 229920001610 polycaprolactone Polymers 0.000 claims description 2
- 239000004632 polycaprolactone Substances 0.000 claims description 2
- 229920006233 biaxially oriented polyamide Polymers 0.000 abstract description 9
- 238000007789 sealing Methods 0.000 abstract description 7
- 230000004888 barrier function Effects 0.000 abstract description 5
- 239000005021 flexible packaging material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 15
- 238000012360 testing method Methods 0.000 description 13
- 239000002985 plastic film Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
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- 238000012538 light obscuration Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229920003020 cross-linked polyethylene Polymers 0.000 description 2
- 239000004703 cross-linked polyethylene Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
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- 229920005989 resin Polymers 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OPZZWWFHZYZBRU-UHFFFAOYSA-N butanedioic acid;butane-1,1-diol Chemical compound CCCC(O)O.OC(=O)CCC(O)=O OPZZWWFHZYZBRU-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
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- 239000000843 powder Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
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- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the technical field of flexible packaging materials, and particularly relates to an extinction polyamide film and a preparation method thereof. The extinction polyamide film comprises an extinction layer, a core layer and a heat sealing layer; the raw materials of the extinction layer comprise 87.9-93.99% of extinction base master batch, 3-6% of crystalline polyester, 0.01-0.1% of dibutyltin dilaurate and 3-6% of compatilizer in percentage by mass; the raw material of the core layer comprises 100% of polyamide 6; the heat-sealing raw materials comprise 95-97% of copolyamide and 3-5% of polyamide anti-sticking master batch. The extinction polyamide film provided by the invention has good barrier property and heat sealing property on the premise of excellent extinction property, and simultaneously ensures that the extinction polyamide film has excellent mechanical property of the conventional BOPA film, thereby expanding the application range of the extinction polyamide film and having higher application value.
Description
Technical Field
The invention belongs to the technical field of flexible packaging materials, and particularly relates to an extinction polyamide film and a preparation method thereof.
Background
The extinction film is a plastic film with low gloss and high haze, light irradiates the extinction layer to show diffuse reflection and scattering, so that the film has very low gloss similar to a paper surface, the reflected light is weak and soft, and the film has high haze and high light transmittance, and has the advantages of comfortable hand feeling, elegant appearance, vivid color reproduction in printing and the like. The delustered polyamide film can create the image of a natural product in food packaging and gift packaging, and the grade of the product is improved. Biaxially oriented polyamide film (BOPA film) has excellent mechanical property, oxygen barrier property and puncture resistance, and the BOPA film with the extinction effect is bound to be widely applied in a plurality of fields such as heavy objects, electronics, medicines and the like.
However, the conventional biaxially oriented polyamide has poor barrier properties against water vapor and does not have heat sealing properties, and is usually used in combination with a cast polyethylene film or a polypropylene film. The addition of complex processes can cause environmental problems such as waste liquid treatment, and also increase costs. The existing biaxial stretching extinction polyamide film added with inorganic powder can affect the transparency of the film. If the transparency of the polyamide film is reduced, the polyamide film may cause a whitening phenomenon after further ink-jetting or color-filling, especially for dark products, and the packaging grade is seriously affected.
Disclosure of Invention
In order to solve the problems of poor water resistance, insufficient transparency and incapability of heat sealing of the extinction BOPA film in the prior art, the invention provides an extinction polyamide film which comprises an extinction layer, a core layer and a heat sealing layer;
the extinction layer comprises the following components in percentage by mass: 87.9 to 93.99 percent of extinction base master batch, 3 to 6 percent of crystalline polyester, 0.01 to 0.1 percent of dibutyltin dilaurate and 3 to 6 percent of compatilizer;
the core layer comprises the following components in percentage by mass: 100% polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 95 to 97 percent of copolyamide and 3 to 5 percent of polyamide anti-sticking master batch;
in one embodiment, the extinction base master batch comprises the following components in percentage by mass: 46 to 59.48 percent of polyamide 6, 40 to 50 percent of high density polyethylene, 0.01 to 0.5 percent of initiator, 0.5 to 3 percent of cross-linking agent and 0.01 to 0.5 percent of antioxidant.
In one embodiment, the matte base masterbatch is prepared by:
mixing polyamide 6 and high-density polyethylene in a mixing container, and then putting an antioxidant, an initiator and a cross-linking agent into the mixing container for mixing;
and putting the mixed mixture into a co-rotating double-screw extruder, and carrying out melt extrusion, granulation and drying to obtain the composite material.
Preferably, the mixing vessel employs a low speed mixer. Specifically, the polyamide 6 and the high-density polyethylene are mixed in the low-speed mixer for 10-15 min, and the subsequent antioxidant, the initiator and the cross-linking agent are thrown into the low-speed mixer and then are continuously mixed for 5-8 min, wherein the rotating speed of the low-speed mixer is 100-200 r/min.
Preferably, the drying process is drying in a dehumidifier at 80 ℃ for 4-5 hours;
preferably, the processing temperature of the co-rotating twin-screw extruder is 180 to 230 ℃, and the screw rotating speed is 250 to 450 revolutions per minute.
In one embodiment, the crystalline polyester is at least one of polycaprolactone, polypropylene carbonate, and polybutylene succinate.
In one embodiment, the copolymerized polyamide is formed by copolymerizing at least two monomers of nylon 6, nylon 66, nylon 10, nylon 12, nylon 1010 and nylon 1212. Preferably, the copolymerized polyamide is a terpolymer nylon. Further, the melting point of the copolyamide ranges from 110 ℃ to 130 ℃, and can be adjusted by a person skilled in the art according to actual conditions.
In one embodiment, the compatibilizer is at least one of polyethylene grafted maleic anhydride, polyethylene grafted glycidyl methacrylate, polyethylene grafted epoxy, and polyethylene grafted oxazoline.
In one embodiment, the initiator is at least one of dicumyl peroxide, di-tert-butyl peroxide, cumene hydroperoxide and tert-butyl hydroperoxide.
In one embodiment, the cross-linking agent is at least one of vinyltriethoxysilane, vinyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane.
In one embodiment, the antioxidant is at least one of antioxidant 1010, antioxidant 1076, antioxidant 1098, antioxidant 168 and antioxidant DSTP.
In one embodiment, the thickness of the extinction layer is 1-3 μm; the thickness of the core layer is 9-19 mu m; the thickness of the heat sealing layer is 1-3 μm.
The invention also provides a preparation method for preparing the extinction polyamide film, which comprises the following steps:
mixing the raw materials of the extinction layer, the core layer and the heat-sealing layer respectively according to a proportion, respectively melting and extruding, flowing out through a T-shaped die head, and cooling through a chilling roller to form an unstretched film casting sheet;
step-by-step stretching the cast sheet of the unstretched film to obtain a stretched film;
and (3) carrying out heat setting on the stretched film to obtain the extinction polyamide film.
Preferably, the surface temperature of the cold roll is 15 ℃ to 40 ℃.
Preferably, the temperature of the step-by-step stretching is 65-180 ℃, and the stretching ratio is 2.5 multiplied by 2.5-3.5 multiplied by 3.5.
Preferably, the setting temperature is 170-210 ℃, the setting time is 3-20 s, and the relaxation rate is 1-3%.
Based on the above, compared with the prior art, the invention has the following beneficial effects:
1. according to the extinction polyamide film provided by the invention, the high-density polyethylene material and the high-crystallinity polyester material are introduced, the initiator initiates the cross-linking agent to perform silane reaction to generate cross-linked polyethylene, and then the compatilizer performs compatibilization reaction, so that the water resistance of the extinction polyamide film is further improved, and the application range of the polyamide film is expanded.
2. The extinction polyamide film extinction layer provided by the invention can provide excellent water resistance and optical transmittance, the core layer provides excellent mechanical support and oxygen resistance, and the heat sealing layer provides good heat sealing performance, so that the extinction polyamide film provided by the invention can be used independently without being compounded with a cast polyolefin heat sealing layer, thereby reducing downstream compounding processes, preventing a plurality of environmental problems such as downstream waste liquid treatment and the like, and simultaneously reducing the processing cost.
3. The crystalline polyester capable of crystallizing at high speed is added in the extinction layer, and the crystallinity of the crystalline polyester can be utilized to improve the protrusion effect of the surface of the film, increase the diffuse reflection effect of the surface of the film and improve the extinction performance. Meanwhile, a small amount of crystalline polyester can be used as a heterogeneous nucleating agent to induce polyamide 6 and crosslinked polyethylene to crystallize, so that the extinction performance is improved. Furthermore, the introduction of the crystalline polyester can adjust the fluidity of the crosslinked high-density polyethylene resin and the polyamide resin after the compatibilization reaction.
4. The extinction layer adopts the polyethylene graft material as the reactive compatilizer of the polyamide 6 and the high-density polyethylene, so that the poor dispersion effect caused by phase separation caused by incompatibility of the nonpolar high-density polyethylene and the polar polyamide is prevented, and the extinction performance and the mechanical property are influenced. Meanwhile, functional groups such as maleic anhydride in the compatilizer react with amino functional groups in polyamide, and a small amount of water molecules separated after reaction are further crosslinked with silane-grafted high-density polyethylene resin in the dibutyltin dilaurate catalytic basic extinction master batch to form crosslinking protrusions, so that the optical diffuse reflection effect is improved, and the extinction performance is improved.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts; in the following description, the drawings are illustrated in a schematic view, and the drawings are not intended to limit the present invention.
Fig. 1 is a schematic structural diagram of an embodiment of a matte polyamide film provided by the present invention.
Reference numerals:
100. 200 light eliminating layers and 300 heat sealing layers of core layers
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments; the technical features designed in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other; all other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
In the description of the present invention, it should be noted that all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs, and should not be construed as limiting the present invention; it will be further understood that terms used herein should be interpreted as having a meaning that is consistent with their meaning in the context of this specification and the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The invention also provides examples and comparative examples as shown in the following table:
example 1
The film structure sequentially comprises an extinction layer, a core layer and a heat sealing layer from outside to inside;
the extinction layer comprises the following components in percentage by mass: 89.95% of extinction base master batch, 5% of polypropylene carbonate, 0.05% of dibutyltin dilaurate and 5% of polyethylene-grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% of polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1010 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 53.8% of polyamide 6, 45% of high-density polyethylene, 0.1% of dicumyl peroxide, 1 vinyl triethoxysilane and 0.1% of antioxidant 1010.
Example 2
The film is composed of a light extinction layer, a core layer and a heat sealing layer from outside to inside in sequence;
the extinction layer comprises the following components in percentage by mass: 87.9% of a matte base master batch, 6% of polypropylene carbonate, 0.1% of dibutyltin dilaurate and 6% of polyethylene-grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 95% polyamide 6/66/1010 and 5% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 46 percent of polyamide 6, 50 percent of high-density polyethylene, 0.5 percent of dicumyl peroxide, 3 percent of vinyl triethoxysilane and 0.5 percent of antioxidant 1010.
Example 3
The film is composed of a light extinction layer, a core layer and a heat sealing layer from outside to inside in sequence;
the extinction layer comprises the following components in percentage by mass: 93.99% of a matte base master batch, 3% of polypropylene carbonate, 0.01% of dibutyltin dilaurate and 3% of polyethylene-grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 97% polyamide 6/66/1010 and 3% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 59.48 percent of polyamide 6, 40 percent of high-density polyethylene, 0.01 percent of dicumyl peroxide, 0.5 percent of vinyl triethoxysilane and 0.01 percent of antioxidant 1010.
Example 4
The film is sequentially provided with a delustering layer, a core layer and a heat sealing layer from outside to inside;
the extinction layer comprises the following components in percentage by mass: 89.95% of extinction base master batch, 5% of butanediol succinate, 0.05% of dibutyltin dilaurate and 5% of polyethylene grafted glycidyl methacrylate;
the core layer comprises the following components in percentage by mass: 100% polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1212 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 53.8% of polyamide 6, 45% of high-density polyethylene, 0.1% of di-tert-butyl peroxide, 1% of vinyltrimethoxysilane and 0.1% of antioxidant 1076.
Comparative example 1
The film is composed of a light extinction layer, a core layer and a heat sealing layer from outside to inside in sequence;
the extinction layer comprises the following components in percentage by mass: 94.95% of a matte base master batch, 0.05% of dibutyltin dilaurate and 5% of polyethylene grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1010 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 53.8 percent of polyamide 6, 45 percent of high-density polyethylene, 0.1 percent of dicumyl peroxide, 1 percent of vinyl triethoxysilane and 0.1 percent of antioxidant 1010.
Comparative example 2
The film is sequentially provided with a delustering layer, a core layer and a heat sealing layer from outside to inside;
the extinction layer comprises the following components in percentage by mass: 90% of extinction base master batch, 5% of polypropylene carbonate and 5% of polyethylene grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1010 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 53.8 percent of polyamide 6, 45 percent of high-density polyethylene, 0.1 percent of dicumyl peroxide, 1 percent of vinyl triethoxysilane and 0.1 percent of antioxidant 1010.
Comparative example 3
The film is sequentially provided with a delustering layer, a core layer and a heat sealing layer from outside to inside;
the extinction layer comprises the following components in percentage by mass: 94.95% of a matte base master batch, 5% of polypropylene carbonate and 0.05% of dibutyltin dilaurate;
the core layer comprises the following components in percentage by mass: 100% polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1010 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 53.8 percent of polyamide 6, 45 percent of high-density polyethylene, 0.1 percent of dicumyl peroxide, 1 percent of vinyl triethoxysilane and 0.1 percent of antioxidant 1010.
Comparative example 4
The film is composed of a light extinction layer, a core layer and a heat sealing layer from outside to inside in sequence;
the extinction layer comprises the following components in percentage by mass: 89.95% of a matte base master batch, 5% of polypropylene carbonate, 0.05% of dibutyltin dilaurate and 5% of polyethylene-grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% of polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1010 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 53.9% polyamide 6, 45% high density polyethylene, 1% vinyltriethoxysilane and 0.1% antioxidant 1010.
Comparative example 5
The film is sequentially provided with a delustering layer, a core layer and a heat sealing layer from outside to inside;
the extinction layer comprises the following components in percentage by mass: 89.95% of extinction base master batch, 5% of polypropylene carbonate, 0.05% of dibutyltin dilaurate and 5% of polyethylene-grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% of polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1010 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 54.8 percent of polyamide 6, 45 percent of high-density polyethylene, 0.1 percent of dicumyl peroxide and 0.1 percent of antioxidant 1010.
Comparative example 6
The film is sequentially provided with a delustering layer, a core layer and a heat sealing layer from outside to inside;
the extinction layer comprises the following components in percentage by mass: 89.95% of extinction base master batch, 5% of polypropylene carbonate, 0.05% of dibutyltin dilaurate and 5% of polyethylene-grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% of polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1010 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 53.9% polyamide 6, 45% high density polyethylene, 0.1% dicumyl peroxide and 1% vinyltriethoxysilane.
Comparative example 7
The film is composed of a light extinction layer, a core layer and a heat sealing layer from outside to inside in sequence;
the extinction layer comprises the following components in percentage by mass: 79% of a matte base master batch, 10% of polypropylene carbonate, 1% of dibutyltin dilaurate and 10% of polyethylene-grafted maleic anhydride;
the core layer comprises the following components in percentage by mass: 100% polyamide 6;
the heat sealing layer comprises the following components in percentage by mass: 96% polyamide 6/66/1010 and 4% polyamide release masterbatch.
The extinction base master batch comprises the following components in percentage by mass: 33% of polyamide 6, 60% of high-density polyethylene, 1% of dicumyl peroxide, 5% of vinyltriethoxysilane and 1% of antioxidant 1010.
Comparative example 8
Commercial BOPA film, 15um thick.
The above examples 1 to 4 and comparative examples 1 to 7 were all prepared by the following procedure:
(1) Preparation of matt polyamide film:
mixing the raw materials of the extinction layer, the core layer and the heat sealing layer respectively according to a proportion, melting and extruding the raw materials respectively through respective extruders, flowing out through a T-shaped die head, and cooling the raw materials through a chilling roller with the surface temperature of 35 ℃ to form an unstretched film casting sheet;
longitudinally stretching the cast sheet of the unstretched film at the temperature of 67 ℃, and then transversely stretching the cast sheet of the unstretched film at the temperature of 165 ℃ to obtain a stretched film, wherein the stretching ratio is 3.0 multiplied by 3.3 times;
and (3) carrying out heat setting on the stretched film, wherein the setting temperature is 185 ℃, the setting time is 10s, and the relaxation rate is 1%, so as to obtain the extinction polyamide film.
(2) Preparation of matting base master batch:
putting polyamide 6 and high-density polyethylene into a low-speed mixer, mixing for 10min, putting an antioxidant, an initiator and a cross-linking agent into the low-speed mixer, and mixing for 5min, wherein the rotating speed of the low-speed mixer is 100 revolutions per minute;
putting the mixed mixture into a feeding hopper of a co-rotating double-screw extruder, performing melt extrusion and granulation, and drying in a dehumidifier at 80 ℃ for 4 hours to obtain the product; wherein the processing temperature of the co-rotating twin-screw extruder is 220 ℃, and the screw rotating speed is 300 r/min.
The examples and comparative examples were tested for various properties according to the following test criteria:
average thickness: testing according to GB/T20220-2006 average thickness of plastic film and sheet samples, average thickness of rolls and unit mass surface test standard;
haze and light transmittance: testing according to GB/T2410-2008 'determination standard of transparent plastic light transmittance and haze';
gloss: testing according to GB/T8807-1988 method for testing specular gloss of plastics;
water vapor transmission rate: testing according to GB/T26253-2010 determination of water vapor transmission rate of plastic films and sheets;
oxygen transmission rate: testing according to GB/T1038-2000 method for testing gas permeability of plastic films and sheets;
heat seal strength: testing according to QB/T2538-1998 method for testing heat seal strength of plastic film packaging bags;
tensile strength and elongation at break: according to GB/T1040.3-2006 "determination of tensile Properties of Plastic films" third part: film and sheet test conditions were tested.
The results of the performance tests of the examples and comparative examples are shown in table 1.
Table 1 results of performance testing
As can be seen from Table 1, the matte polyamide films obtained in examples 1 to 4 have better properties than those of comparative examples 1 to 8. As can be seen from the examples 1-4 and the comparative examples 1-7, the comprehensive performance of the extinction polyamide film provided by the invention is obtained by the mixture ratio and the components, and the performance requirements of the extinction polyamide film can not be met under the condition of missing any component or misadjustment of the ratio. As can be seen from examples 1 to 4 and comparative example 8, the extinction polyamide film provided by the invention has obvious advantages compared with the existing commercially available products, obtains barrier property, heat sealing property and extinction effect on the basis of BOPA film, and has good industrial application prospect.
In conclusion, compared with the prior art, the extinction polyamide film provided by the invention has good barrier property and heat sealing property on the premise of excellent extinction property, and simultaneously ensures that the extinction polyamide film has excellent mechanical property of the conventional BOPA film, thereby expanding the application range of the extinction polyamide film and having higher application value.
In addition, it will be appreciated by those skilled in the art that, notwithstanding the many problems inherent in the prior art, each embodiment or solution of the present invention may be improved in one or more respects, without necessarily simultaneously solving all the technical problems inherent in the prior art or in the background art. It will be understood by those skilled in the art that nothing in a claim should be taken as a limitation on that claim.
Although terms such as optical layers, core layers, heat seal layers, etc. are used more often herein, the possibility of using other terms is not excluded. These terms are used merely to more conveniently describe and explain the nature of the present invention; they are to be construed as being without limitation to any one or more of the appended limitations; the terms "first," "second," and the like in the description and in the claims, and in the foregoing description and in the drawings, if any, are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A matte polyamide film characterized by: comprises a extinction layer, a core layer and a heat sealing layer;
the extinction layer comprises, by mass, 87.9% -93.99% of extinction base master batch, 3% -6% of crystalline polyester, 0.01% -0.1% of dibutyltin dilaurate and 3% -6% of compatilizer;
the raw material of the core layer comprises 100% of polyamide 6;
the raw materials of the heat sealing layer comprise 95-97% of copolyamide and 3-5% of polyamide anti-sticking master batch.
2. A matted polyamide film according to claim 1, wherein: the extinction base master batch comprises the following components in percentage by mass: 46 to 59.48 percent of polyamide 6, 40 to 50 percent of high-density polyethylene, 0.01 to 0.5 percent of initiator, 0.5 to 3 percent of cross-linking agent and 0.01 to 0.5 percent of antioxidant.
3. A matted polyamide film according to claim 2, wherein: the preparation process of the extinction base master batch comprises the following steps:
putting polyamide 6 and high-density polyethylene into a mixing container, mixing, and then putting an antioxidant, an initiator and a cross-linking agent into the mixing container for mixing;
and putting the mixed mixture into a co-rotating double-screw extruder, and carrying out melt extrusion, granulation and drying to obtain the composite material.
4. A matted polyamide film according to claim 1, wherein: the crystalline polyester is at least one of polycaprolactone, polypropylene carbonate and polybutylene succinate.
5. A matted polyamide film according to claim 1, wherein: the copolymerized polyamide is copolymerized by at least two monomers of nylon 6, nylon 66, nylon 10, nylon 12, nylon 1010 and nylon 1212.
6. A matted polyamide film according to claim 1, wherein: the compatilizer is at least one of polyethylene grafted maleic anhydride, polyethylene grafted glycidyl methacrylate, polyethylene grafted epoxy and polyethylene grafted oxazoline.
7. A matted polyamide film according to claim 2, wherein: the initiator is at least one of dicumyl peroxide, di-tert-butyl peroxide, cumene hydroperoxide and tert-butyl hydroperoxide.
8. A matted polyamide film according to claim 2, wherein: the cross-linking agent is at least one of vinyl triethoxysilane, vinyl trimethoxysilane and gamma-methacryloxypropyl trimethoxysilane; the antioxidant is at least one of antioxidant 1010, antioxidant 1076, antioxidant 1098, antioxidant 168 and antioxidant DSTP.
9. A matted polyamide film according to claim 1, wherein: the thickness of the extinction layer is 1-3 mu m; the thickness of the core layer is 9-19 mu m; the thickness of the heat sealing layer is 1-3 μm.
10. A process for producing a matted polyamide film according to any one of claims 1 to 9, which comprises the steps of:
mixing the raw materials of the extinction layer, the core layer and the heat sealing layer respectively according to a proportion, respectively melting and extruding, flowing out through a T-shaped die head, and cooling through a chilling roller to form an unstretched film casting sheet;
step-by-step stretching the cast sheet of the unstretched film to obtain a stretched film;
and (3) performing heat setting on the stretched film to obtain the extinction polyamide film.
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