CN115384153B - Composite film capable of being repeatedly heat-sealed and preparation method thereof - Google Patents
Composite film capable of being repeatedly heat-sealed and preparation method thereof Download PDFInfo
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- CN115384153B CN115384153B CN202210871538.4A CN202210871538A CN115384153B CN 115384153 B CN115384153 B CN 115384153B CN 202210871538 A CN202210871538 A CN 202210871538A CN 115384153 B CN115384153 B CN 115384153B
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000004698 Polyethylene Substances 0.000 claims abstract description 49
- -1 polyethylene Polymers 0.000 claims abstract description 49
- 229920000573 polyethylene Polymers 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000853 adhesive Substances 0.000 claims abstract description 16
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- 229920002799 BoPET Polymers 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 239000011888 foil Substances 0.000 claims abstract description 14
- 238000007731 hot pressing Methods 0.000 claims abstract description 13
- 238000013329 compounding Methods 0.000 claims abstract description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 66
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 63
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 34
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 33
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 31
- 239000000758 substrate Substances 0.000 claims description 31
- 239000002245 particle Substances 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 25
- 238000010992 reflux Methods 0.000 claims description 25
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 17
- 238000000576 coating method Methods 0.000 claims description 17
- 239000011246 composite particle Substances 0.000 claims description 17
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 15
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 229910021389 graphene Inorganic materials 0.000 claims description 14
- 238000006243 chemical reaction Methods 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
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 11
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 11
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 11
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 11
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 11
- 229940078494 nickel acetate Drugs 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- 238000000071 blow moulding Methods 0.000 claims description 10
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 10
- KJJPLEZQSCZCKE-UHFFFAOYSA-N 2-aminopropane-1,3-diol Chemical compound OCC(N)CO KJJPLEZQSCZCKE-UHFFFAOYSA-N 0.000 claims description 7
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 238000010030 laminating Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 9
- 230000004888 barrier function Effects 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000012793 heat-sealing layer Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 230000008033 biological extinction Effects 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000001263 acyl chlorides Chemical group 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- 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
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal 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
- B32B15/09—Layered products comprising a layer of metal comprising metal 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 comprising polyesters
-
- 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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- 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
-
- 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
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
-
- 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
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
-
- 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
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
-
- 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
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- 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
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
-
- 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
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/31—Heat sealable
-
- 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
- B32B2553/00—Packaging equipment or accessories not otherwise provided for
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/80—Packaging reuse or recycling, e.g. of multilayer packaging
Abstract
The invention discloses a composite film capable of repeatedly heat-sealing and a preparation method thereof, wherein the composite film is prepared by compounding a modified polyethylene film, a PET film and an aluminum foil, the PET film and the aluminum foil are firstly subjected to hot pressing, and then are bonded and hot pressed with the modified polyethylene film, a heat sealing layer of the composite film is the modified polyethylene film, so that the heat sealing film can be repeatedly heat-sealed, meanwhile, the heat sealing film can effectively isolate water vapor, has a good barrier effect by isolating oxygen, and meanwhile, the modified polyethylene film contains polar groups, so that the polyethylene film can be well bonded with an adhesive, and the phenomenon of opening the composite film can not occur in long-time use or special environment, thereby improving the heat sealing effect.
Description
Technical Field
The invention relates to the technical field of composite film preparation, in particular to a composite film capable of being repeatedly heat-sealed and a preparation method thereof.
Background
In recent years, with the rapid development of the packaging industry, the requirements of consumers on the packaging of various products are higher and higher, and the extinction PE film is one of the faster development. The extinction PE film not only has good visual presentation effect, can improve the packaging grade of products, but also has the characteristic of low price compared with the common PP, PET, NY and other extinction film materials, is favored by more and more packagers, and has the characteristics of rich raw material resources, moderate price, stable and reliable production process, superior comprehensive performance of products and the like, so that the application range of the PE film is gradually expanded, and particularly in the packaging field and the protection film field, the cost performance of the PE film is superior to that of other materials, and the consumption of the PE film always occupies the first of the common packaging materials. After the traditional PE film is manufactured into the PE film composite bag, after the product is filled, the PE film is sealed by heat sealing, so that the product quality can be well preserved and maintained, the PE film has good dampproof effect, but has high air permeability, so that the blocking effect is lower, and meanwhile, the molecular chain does not contain polar groups, so that the self-adhesive effect is poor.
Disclosure of Invention
The invention aims to provide a composite film capable of being repeatedly heat-sealed and a preparation method thereof, which solves the problems that the PE heat-sealed film in the prior art is poor in gas barrier property, common in barrier effect and difficult to adhere.
The aim of the invention can be achieved by the following technical scheme:
a composite film capable of being repeatedly heat-sealed is prepared by compounding a modified polyethylene film, a PET film and an aluminum foil pressed film.
Further, the modified polyethylene film is prepared by the following steps:
step A1: dissolving maleic anhydride in acetone, stirring at a rotating speed of 150-200r/min and a temperature of 5-10 ℃, adding 2-amino-1, 3-propanediol acetone solution, stirring for 10-15min, heating to a temperature of 60-70 ℃, carrying out reflux treatment for 30-40min, adding triethylamine, acetic anhydride and nickel acetate, continuously refluxing for 2-3h, adding reactants into ice water, filtering to remove filtrate, drying a filter cake to obtain an intermediate 1, adding linear low-density polyethylene particles, the intermediate 1 and benzoyl peroxide into a double-screw extruder, extruding and granulating at a screw rotating speed of 60-120r/min and a temperature of 160-170 ℃ to obtain modified particles;
the reaction process is as follows:
step A2: dispersing graphene oxide in deionized water, adding thionyl chloride, stirring and refluxing for 7-9 hours at the rotation speed of 200-300r/min and the temperature of 110-120 ℃, removing thionyl chloride and deionized water by reduced pressure distillation, dispersing a substrate in the deionized water again, adding diethanolamine and triethylamine, stirring for 5-8 hours at the rotation speed of 500-800r/min and the temperature of 70-80 ℃, centrifuging to remove a supernatant, and drying the substrate to obtain modified graphene;
step A3: uniformly mixing aluminum nitrate, magnesium nitrate, methanol and ethylene glycol to obtain a dripping solution, uniformly mixing sodium dodecyl sulfate, methanol and ethylene glycol, stirring at a rotating speed of 200-300r/min and a temperature of 20-25 ℃, adding the dripping solution, maintaining the pH value of the reaction solution to be 9, heating to a temperature of 155-165 ℃, carrying out reflux treatment for 15-20h, filtering to remove filtrate, washing a substrate to be neutral and drying, dispersing in n-butanol, carrying out reflux treatment for 20-30h at a temperature of 120-130 ℃, adding modified graphene, carrying out ultrasonic treatment for 5-7 kHz at a frequency of 40-50kHz, filtering to remove the filtrate, and drying the substrate to obtain composite particles;
step A4: dissolving modified particles in paraxylene, adding PTMG-1000 and composite particles, stirring and dripping toluene-2, 3-diisocyanate at the rotation speed of 120-150r/min and the temperature of 60-70 ℃, reacting for 20-30min, heating to the temperature of 80-90 ℃, reacting for 2-3h, cooling to the temperature of 40-50 ℃, adding triethylamine, continuously stirring for 20-30min, uniformly mixing the reaction solution with deionized water, filtering to remove filtrate, drying a substrate, adding the substrate into a blow molding machine, and blow molding to form a film, thus obtaining the modified polyethylene film.
Further, the dosage ratio of the maleic anhydride, the 2-amino-1, 3-propanediol, the triethylamine, the acetic anhydride and the nickel acetate in the step A1 is 0.05mol:0.05mol:5g:12g:3.5g, and the dosage mass ratio of the linear low density polyethylene particles, the intermediate 1 and the benzoyl peroxide is 40:5:1.2.
Further, the dosage ratio of graphene oxide, thionyl chloride and diethanolamine in the step A2 is 1g to 2mL to 1mL.
Further, the dosage ratio of aluminum nitrate, magnesium nitrate, methanol and ethylene glycol in the step A3 is 0.03mol:0.01mol:10mL:10mL, the dosage ratio of sodium dodecyl sulfate, methanol, ethylene glycol and dropwise adding liquid is 7g:40mL:40mL:20mL, and the dosage mass ratio of the substrate to the modified graphene is 5:3.
Further, the dosage mass ratio of the modified particles, PTMG-1000, composite particles and toluene-2, 3-diisocyanate in the step A4 is 5.8:10.5:0.1:12.6.
The preparation method of the repeatedly heat-sealable composite film specifically comprises the following steps:
step S1: laminating PET film and aluminum foil, and performing hot pressing treatment for 10-15min at 250-300 ℃ and 10-12MPa to obtain a modified film;
step S2: coating adhesive on PET surface of modified film and modified polyethylene film at coating speed of 20-33m/min, lifting box on adhesive coated surface of modified film and modified polyethylene film, hot pressing at 75-85deg.C and pressure of 0.5-0.8MPa to obtain composite film.
Further, the adhesive is DORUSMD3931 aqueous adhesive, and the coating thickness of the adhesive is 30-40 mu m.
The invention has the beneficial effects that: the invention relates to a composite film capable of repeatedly heat-sealing, which is prepared by compounding a modified polyethylene film, a PET film and an aluminum foil film, wherein the PET film and the aluminum foil film are firstly subjected to hot pressing, and then are subjected to bonding hot pressing with the modified polyethylene film, the modified polyethylene film is prepared by taking maleic anhydride as a raw material to react with 2-amino-1, 3-propanediol, so that maleic anhydride molecules are subjected to ring opening to form carboxyl groups, one carboxyl group reacts with amino groups on the 2-amino-1, 3-propanediol, then, under the action of triethylamine, acetic anhydride and nickel acetate, dehydration condensation is performed to prepare an intermediate 1, the intermediate 1 and linear low density polyethylene particles are subjected to melt grafting, under the action of benzoyl peroxide, a linear low density polyethylene molecular chain generates free radicals, the free radicals react with the intermediate 1 to form new free radicals, then the modified particle is prepared by combining the modified particle with a linear low density polyethylene molecular chain, capturing hydrogen atoms on the molecular chain, further grafting an intermediate 1 on the linear low density polyethylene molecular chain, treating graphene oxide with thionyl chloride to convert part of carboxyl groups on the surface of the graphene oxide into acyl chloride groups, further reacting with ethylene glycol amine under the action of triethylamine and primary amine to graft a large amount of alcohol hydroxyl groups on the surface of the graphene, preparing modified graphene, preparing hydrotalcite-like compound by using aluminum nitrate and magnesium nitrate through a hydrothermal method, dissolving the hydrotalcite-like compound in n-butyl alcohol, then carrying out ultrasonic treatment with the modified graphene to disperse the hydrotalcite-like compound on the surface of the graphene, preparing composite particles, modified particles and PTMG-1000 under the action of toluene-2, 3-diisocyanate to react the alcohol hydroxyl groups with isocyanate groups, the modified polyethylene film is prepared by polymerizing the modified particle molecular chains with the surfaces of the composite particles and then blowing the film, the heat sealing layer of the heat sealing composite film is the modified polyethylene film, so that the heat sealing film can be repeatedly heat-sealed, meanwhile, the heat sealing film can effectively isolate water vapor and oxygen, so that the heat sealing film has a good barrier effect, and meanwhile, the modified polyethylene film contains polar groups, so that the polyethylene film can be well adhered to an adhesive, and the phenomenon of opening the heat sealing composite film can not occur in long-time use or special environment, thereby improving the heat sealing effect.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A composite film capable of being repeatedly heat-sealed is prepared by compounding a modified polyethylene film, a PET film and an aluminum foil pressed film;
the composite film is prepared by the following steps:
step S1: laminating a PET film and an aluminum foil, and carrying out hot pressing treatment for 10min under the conditions of the temperature of 250 ℃ and the pressure of 10MPa to obtain a modified film;
step S2: coating the modified film PET surface and the modified polyethylene film with DORUSMD3931 aqueous binder under the condition of coating speed of 20m/min, coating the adhesive with thickness of 30 μm, bonding the modified film and the modified polyethylene film adhesive coating surface, and hot-pressing to form a film under the condition of temperature of 75 ℃ and pressure of 0.5MPa to obtain the composite film.
The modified polyethylene film is prepared by the following steps:
step A1: dissolving maleic anhydride in acetone, stirring at a rotation speed of 150r/min and a temperature of 5 ℃, adding 2-amino-1, 3-propanediol acetone solution, stirring for 10min, heating to a temperature of 60 ℃, carrying out reflux treatment for 30min, adding triethylamine, acetic anhydride and nickel acetate, continuously refluxing for 2h, adding reactants into ice water, filtering to remove filtrate, drying a filter cake to obtain an intermediate 1, adding linear low density polyethylene particles, the intermediate 1 and benzoyl peroxide into a double-screw extruder, extruding and granulating at a screw rotation speed of 60r/min and a temperature of 160 ℃, and obtaining modified particles;
step A2: dispersing graphene oxide in deionized water, adding thionyl chloride, stirring and refluxing for 7 hours at the rotation speed of 200r/min and the temperature of 110 ℃, then removing thionyl chloride and deionized water by reduced pressure distillation, dispersing a substrate in the deionized water again, adding diethanolamine and triethylamine, stirring for 5 hours at the rotation speed of 500r/min and the temperature of 70 ℃, centrifuging to remove a supernatant, and drying the substrate to obtain modified graphene;
step A3: uniformly mixing aluminum nitrate, magnesium nitrate, methanol and ethylene glycol to obtain a dripping solution, uniformly mixing sodium dodecyl sulfate, methanol and ethylene glycol, stirring at a rotation speed of 200r/min and a temperature of 20 ℃, adding the dripping solution, maintaining the pH value of the reaction solution to be 9, heating to 155 ℃, carrying out reflux treatment for 15 hours, filtering to remove filtrate, washing a substrate to be neutral, drying, dispersing in n-butyl alcohol, carrying out reflux treatment at a temperature of 120 ℃ for 20 hours, adding modified graphene, carrying out ultrasonic treatment at a frequency of 40kHz for 5 hours, filtering to remove filtrate, and drying the substrate to obtain composite particles;
step A4: dissolving modified particles in paraxylene, adding PTMG-1000 and composite particles, stirring and dropwise adding toluene-2, 3-diisocyanate at the rotation speed of 120r/min and the temperature of 60 ℃, reacting for 20min, heating to the temperature of 80 ℃, reacting for 2h, cooling to the temperature of 40 ℃, adding triethylamine, continuously stirring for 20min, uniformly mixing the reaction solution with deionized water, filtering to remove filtrate, drying a substrate, adding into a blow molding machine, and blow molding to form a film to obtain the modified polyethylene film.
The dosage ratio of the maleic anhydride, the 2-amino-1, 3-propanediol, the triethylamine, the acetic anhydride and the nickel acetate in the step A1 is 0.05mol:0.05mol:5g:12g:3.5g, and the dosage mass ratio of the linear low density polyethylene particles, the intermediate 1 and the benzoyl peroxide is 40:5:1.2.
The dosage ratio of graphene oxide, thionyl chloride and diethanolamine in the step A2 is 1g to 2mL to 1mL.
The dosage ratio of aluminum nitrate, magnesium nitrate, methanol and ethylene glycol in the step A3 is 0.03mol:0.01mol:10mL:10mL, the dosage ratio of sodium dodecyl sulfate, methanol and ethylene glycol and the dosage ratio of dropwise adding liquid are 7g:40mL:40mL:20mL, and the dosage mass ratio of substrate and modified graphene is 5:3.
The dosage and mass ratio of the modified particles, PTMG-1000, composite particles and toluene-2, 3-diisocyanate in the step A4 is 5.8:10.5:0.1:12.6.
Example 2
A composite film capable of being repeatedly heat-sealed is prepared by compounding a modified polyethylene film, a PET film and an aluminum foil pressed film;
the composite film is prepared by the following steps:
step S1: laminating a PET film and an aluminum foil, and carrying out hot pressing treatment for 10min under the conditions that the temperature is 280 ℃ and the pressure is 11MPa to obtain a modified film;
step S2: coating the modified film PET surface and the modified polyethylene film with DORUSMD3931 aqueous binder under the condition of coating speed of 33m/min, coating the adhesive with thickness of 35 μm, bonding the modified film and the modified polyethylene film adhesive coating surface, and hot-pressing to form a film under the condition of temperature of 80 ℃ and pressure of 0.7MPa to obtain the composite film.
The modified polyethylene film is prepared by the following steps:
step A1: dissolving maleic anhydride in acetone, stirring at 180r/min and 8 ℃ and adding 2-amino-1, 3-propanediol acetone solution, stirring for 13min, heating to 65 ℃, carrying out reflux treatment for 35min, adding triethylamine, acetic anhydride and nickel acetate, continuously refluxing for 2.5h, adding reactants into ice water, filtering to remove filtrate, drying a filter cake to obtain an intermediate 1, adding linear low density polyethylene particles, the intermediate 1 and benzoyl peroxide into a double-screw extruder, and carrying out extrusion granulation at the screw speed of 60r/min and the temperature of 165 ℃ to obtain modified particles;
step A2: dispersing graphene oxide in deionized water, adding thionyl chloride, stirring and refluxing for 8 hours at the rotation speed of 300r/min and the temperature of 115 ℃, then removing thionyl chloride and deionized water by reduced pressure distillation, dispersing a substrate in the deionized water again, adding diethanolamine and triethylamine, stirring for 6 hours at the rotation speed of 500r/min and the temperature of 75 ℃, centrifuging to remove a supernatant, and drying the substrate to obtain modified graphene;
step A3: uniformly mixing aluminum nitrate, magnesium nitrate, methanol and ethylene glycol to obtain a dripping solution, uniformly mixing sodium dodecyl sulfate, methanol and ethylene glycol, stirring at a rotation speed of 300r/min and a temperature of 23 ℃, adding the dripping solution, maintaining the pH value of the reaction solution to be 9, heating to 160 ℃, carrying out reflux treatment for 18 hours, filtering to remove filtrate, washing a substrate to be neutral, drying, dispersing in n-butyl alcohol, carrying out reflux treatment at a temperature of 125 ℃ for 25 hours, adding modified graphene, carrying out ultrasonic treatment at a frequency of 45kHz for 6 hours, filtering to remove filtrate, and drying the substrate to obtain composite particles;
step A4: dissolving modified particles in paraxylene, adding PTMG-1000 and composite particles, stirring and dropwise adding toluene-2, 3-diisocyanate at the rotation speed of 150r/min and the temperature of 65 ℃, reacting for 25min, heating to the temperature of 85 ℃, reacting for 2.5h, cooling to the temperature of 45 ℃, adding triethylamine, continuously stirring for 25min, uniformly mixing the reaction solution with deionized water, filtering to remove filtrate, drying a substrate, adding into a blow molding machine, and blow molding to form a film to obtain the modified polyethylene film.
The dosage ratio of the maleic anhydride, the 2-amino-1, 3-propanediol, the triethylamine, the acetic anhydride and the nickel acetate in the step A1 is 0.05mol:0.05mol:5g:12g:3.5g, and the dosage mass ratio of the linear low density polyethylene particles, the intermediate 1 and the benzoyl peroxide is 40:5:1.2.
The dosage ratio of graphene oxide, thionyl chloride and diethanolamine in the step A2 is 1g to 2mL to 1mL.
The dosage ratio of aluminum nitrate, magnesium nitrate, methanol and ethylene glycol in the step A3 is 0.03mol:0.01mol:10mL:10mL, the dosage ratio of sodium dodecyl sulfate, methanol and ethylene glycol and the dosage ratio of dropwise adding liquid are 7g:40mL:40mL:20mL, and the dosage mass ratio of substrate and modified graphene is 5:3.
The dosage and mass ratio of the modified particles, PTMG-1000, composite particles and toluene-2, 3-diisocyanate in the step A4 is 5.8:10.5:0.1:12.6.
Example 3
A composite film capable of being repeatedly heat-sealed is prepared by compounding a modified polyethylene film, a PET film and an aluminum foil pressed film;
the composite film is prepared by the following steps:
step S1: laminating a PET film and an aluminum foil, and carrying out hot pressing treatment for 15min under the conditions of the temperature of 300 ℃ and the pressure of 12MPa to obtain a modified film;
step S2: coating the modified film PET surface and the modified polyethylene film with DORUSMD3931 aqueous binder under the condition of coating speed of 33m/min, coating the adhesive with thickness of 40 μm, bonding the modified film and the modified polyethylene film adhesive coating surface, and hot-pressing to form a film under the condition of temperature of 85 ℃ and pressure of 0.8MPa to obtain the composite film.
The modified polyethylene film is prepared by the following steps:
step A1: dissolving maleic anhydride in acetone, stirring at a rotating speed of 200r/min and a temperature of 10 ℃, adding 2-amino-1, 3-propanediol acetone solution, stirring for 15min, heating to a temperature of 70 ℃, carrying out reflux treatment for 40min, adding triethylamine, acetic anhydride and nickel acetate, continuously refluxing for 3h, adding reactants into ice water, filtering to remove filtrate, drying a filter cake to obtain an intermediate 1, adding linear low density polyethylene particles, the intermediate 1 and benzoyl peroxide into a double-screw extruder, extruding and granulating at a screw rotating speed of 60-120r/min and a temperature of 170 ℃, and obtaining modified particles;
step A2: dispersing graphene oxide in deionized water, adding thionyl chloride, stirring and refluxing for 9 hours at the rotation speed of 300r/min and the temperature of 120 ℃, then removing thionyl chloride and deionized water by reduced pressure distillation, dispersing a substrate in the deionized water again, adding diethanolamine and triethylamine, stirring for 8 hours at the rotation speed of 800r/min and the temperature of 80 ℃, centrifuging to remove a supernatant, and drying the substrate to obtain modified graphene;
step A3: uniformly mixing aluminum nitrate, magnesium nitrate, methanol and ethylene glycol to obtain a dripping solution, uniformly mixing sodium dodecyl sulfate, methanol and ethylene glycol, stirring at a rotation speed of 300r/min and a temperature of 25 ℃, adding the dripping solution, maintaining the pH value of the reaction solution to be 9, heating to 165 ℃, carrying out reflux treatment for 20 hours, filtering to remove filtrate, washing a substrate to be neutral, drying, dispersing in n-butyl alcohol, carrying out reflux treatment for 30 hours at a temperature of 130 ℃, adding modified graphene, carrying out ultrasonic treatment for 7 hours at a frequency of 50kHz, filtering to remove filtrate, and drying the substrate to obtain composite particles;
step A4: dissolving modified particles in paraxylene, adding PTMG-1000 and composite particles, stirring and dropwise adding toluene-2, 3-diisocyanate at the rotation speed of 150r/min and the temperature of 70 ℃, reacting for 30min, heating to the temperature of 90 ℃, reacting for 3h, cooling to the temperature of 50 ℃, adding triethylamine, continuously stirring for 30min, uniformly mixing the reaction solution with deionized water, filtering to remove filtrate, drying a substrate, adding into a blow molding machine, and blow molding to form a film, thus obtaining the modified polyethylene film.
The dosage ratio of the maleic anhydride, the 2-amino-1, 3-propanediol, the triethylamine, the acetic anhydride and the nickel acetate in the step A1 is 0.05mol:0.05mol:5g:12g:3.5g, and the dosage mass ratio of the linear low density polyethylene particles, the intermediate 1 and the benzoyl peroxide is 40:5:1.2.
The dosage ratio of graphene oxide, thionyl chloride and diethanolamine in the step A2 is 1g to 2mL to 1mL.
The dosage ratio of aluminum nitrate, magnesium nitrate, methanol and ethylene glycol in the step A3 is 0.03mol:0.01mol:10mL:10mL, the dosage ratio of sodium dodecyl sulfate, methanol and ethylene glycol and the dosage ratio of dropwise adding liquid are 7g:40mL:40mL:20mL, and the dosage mass ratio of substrate and modified graphene is 5:3.
The dosage and mass ratio of the modified particles, PTMG-1000, composite particles and toluene-2, 3-diisocyanate in the step A4 is 5.8:10.5:0.1:12.6.
Comparative example 1
In this comparative example, a linear low density polyethylene film was used instead of the modified polyethylene film, and the rest of the procedure was the same.
Comparative example 2
This comparative example is a heat-sealable film repeatedly disclosed in chinese patent CN108189506 a.
Comparative example 3
This comparative example is a heat-sealable film repeatedly disclosed in chinese patent CN108504024 a.
The repeated heat-sealing films obtained in examples 1 to 3 and comparative examples 1 to 3 were tested on the basis of a differential pressure method using a gas barrier tester, and the water vapor permeability unit g.mm/24 h.m 3 mPa, oxygen transmittance in cm 3 ·mm/24h·m 3 mPa, and immersing the composite film in water for 48h,96h and 144h, and observing whether the composite film has a film opening phenomenon or not, wherein the result is shown in the following table;
as is clear from the above table, the water vapor permeability of the composite heat-seal films obtained in examples 1 to 3 was 1.91 to 1.95 g.mm/24 h.m 3 mPa, oxygen transmission rate of 0.82-0.85cm 3 ·mm/24h·m 3 mPa, the film opening does not appear after the film is soaked in water for 144 hours, which shows that the film has good blocking effect and solves the problem of poor bonding effect of polyethylene materials.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (6)
1. A heat sealable composite film, comprising: is prepared by compounding a modified polyethylene film, a PET film and an aluminum foil film;
the modified polyethylene film is prepared by the following steps:
step A1: dissolving maleic anhydride in acetone, stirring, adding 2-amino-1, 3-propanediol acetone solution, stirring, heating for reflux treatment, adding triethylamine, acetic anhydride and nickel acetate, continuously refluxing, adding reactants into ice water, filtering to remove filtrate, drying a filter cake to obtain an intermediate 1, adding linear low-density polyethylene particles, the intermediate 1 and benzoyl peroxide into a double-screw extruder, extruding and granulating to obtain modified particles;
step A2: dispersing graphene oxide in deionized water, adding thionyl chloride, stirring and refluxing, removing thionyl chloride and deionized water by reduced pressure distillation, dispersing a substrate in deionized water again, adding diethanolamine and triethylamine, stirring, centrifuging to remove a supernatant, and drying the substrate to obtain modified graphene;
step A3: uniformly mixing aluminum nitrate, magnesium nitrate, methanol and ethylene glycol to obtain a dropwise adding solution, uniformly mixing sodium dodecyl sulfate, methanol and ethylene glycol, adding the dropwise adding solution, maintaining the pH value of the reaction solution, heating for reflux treatment, filtering to remove filtrate, washing a substrate to be neutral, drying, dispersing in n-butanol, carrying out reflux treatment, adding modified graphene, carrying out ultrasonic treatment, filtering to remove filtrate, and drying the substrate to obtain composite particles;
step A4: dissolving modified particles in paraxylene, adding PTMG-1000 and composite particles, stirring and dripping toluene-2, 3-diisocyanate for reaction, heating for continuous reaction, cooling, adding triethylamine, continuously stirring, uniformly mixing the reaction solution with deionized water, filtering to remove filtrate, drying a substrate, adding into a blow molding machine, and blow molding to form a film, thus obtaining the modified polyethylene film.
2. A heat-sealable composite film according to claim 1, wherein: the dosage ratio of the maleic anhydride, the 2-amino-1, 3-propanediol, the triethylamine, the acetic anhydride and the nickel acetate in the step A1 is 0.05mol:0.05mol:5g:12g:3.5g, and the dosage mass ratio of the linear low density polyethylene particles, the intermediate 1 and the benzoyl peroxide is 40:5:1.2.
3. A heat-sealable composite film according to claim 1, wherein: the dosage ratio of graphene oxide, thionyl chloride and diethanolamine in the step A2 is 1g to 2mL to 1mL.
4. A heat-sealable composite film according to claim 1, wherein: the dosage ratio of aluminum nitrate, magnesium nitrate, methanol and ethylene glycol in the step A3 is 0.03mol:0.01mol:10mL:10mL, the dosage ratio of sodium dodecyl sulfate, methanol and ethylene glycol and the dosage ratio of dropwise adding liquid are 7g:40mL:40mL:20mL, and the dosage mass ratio of substrate and modified graphene is 5:3.
5. A heat-sealable composite film according to claim 1, wherein: the dosage and mass ratio of the modified particles, PTMG-1000, composite particles and toluene-2, 3-diisocyanate in the step A4 is 5.8:10.5:0.1:12.6.
6. The method for producing a heat-sealable composite film repeatedly according to claim 1, wherein: the method specifically comprises the following steps:
step S1: laminating PET film and aluminum foil, and performing hot pressing treatment for 10-15min at 250-300 ℃ and 10-12MPa to obtain a modified film;
step S2: coating an adhesive on the PET surface of the modified film and the modified polyethylene film at the coating speed of 20-33m/min, bonding the adhesive-coated surfaces of the modified film and the modified polyethylene film, and hot-pressing to form a film at the temperature of 75-85 ℃ and the pressure of 0.5-0.8MPa to obtain the composite film.
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