CN116023739A - Composite packaging bag for oral liquid medicine and preparation method thereof - Google Patents
Composite packaging bag for oral liquid medicine and preparation method thereof Download PDFInfo
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- CN116023739A CN116023739A CN202211572326.2A CN202211572326A CN116023739A CN 116023739 A CN116023739 A CN 116023739A CN 202211572326 A CN202211572326 A CN 202211572326A CN 116023739 A CN116023739 A CN 116023739A
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- silicon dioxide
- zif
- oral liquid
- packaging bag
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- 239000007788 liquid Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 239000003814 drug Substances 0.000 title claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 144
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 67
- 239000004743 Polypropylene Substances 0.000 claims abstract description 58
- -1 polypropylene Polymers 0.000 claims abstract description 58
- 229920001155 polypropylene Polymers 0.000 claims abstract description 58
- 150000001875 compounds Chemical class 0.000 claims abstract description 29
- 229920001690 polydopamine Polymers 0.000 claims abstract description 23
- 229920002472 Starch Polymers 0.000 claims abstract description 15
- 239000008107 starch Substances 0.000 claims abstract description 15
- 235000019698 starch Nutrition 0.000 claims abstract description 15
- 239000004952 Polyamide Substances 0.000 claims abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 8
- 239000011888 foil Substances 0.000 claims abstract description 8
- 229920002647 polyamide Polymers 0.000 claims abstract description 8
- 229920006267 polyester film Polymers 0.000 claims abstract description 8
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 4
- 238000001125 extrusion Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 239000008367 deionised water Substances 0.000 claims description 43
- 229910021641 deionized water Inorganic materials 0.000 claims description 43
- 235000012239 silicon dioxide Nutrition 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 29
- 239000007864 aqueous solution Substances 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 28
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 26
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 22
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 22
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 229920000587 hyperbranched polymer Polymers 0.000 claims description 19
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 239000004593 Epoxy Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 12
- 229920002545 silicone oil Polymers 0.000 claims description 12
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 229940126062 Compound A Drugs 0.000 claims description 10
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000004005 microsphere Substances 0.000 claims description 9
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 7
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- YJKHMSPWWGBKTN-UHFFFAOYSA-N 2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoroheptyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)F YJKHMSPWWGBKTN-UHFFFAOYSA-N 0.000 claims description 6
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 6
- 230000004224 protection Effects 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 239000013530 defoamer Substances 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000010096 film blowing Methods 0.000 abstract description 6
- 230000004888 barrier function Effects 0.000 abstract description 5
- 230000002209 hydrophobic effect Effects 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 2
- 235000011187 glycerol Nutrition 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000747 poly(lactic acid) Polymers 0.000 description 2
- 239000004626 polylactic acid Substances 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- 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
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
Abstract
The invention relates to the technical field of packaging bags, in particular to a composite packaging bag for oral liquid medicine and a preparation method thereof. The polyester film, the aluminum foil, the polyamide film and the modified polypropylene film are arranged from top to bottom. Wherein the modified polypropylene film is prepared from polypropylene, starch, a defoaming agent, a ZIF-L-silicon dioxide compound and a plasticizer through melt extrusion and film blowing. The ZIF-L-silica composite is prepared by compounding a ZIF-L compound and modified silica with hydrophobic performance through polydopamine. The prepared composite packaging bag for the oral liquid medicine has good mechanical property and barrier property, and meets the packaging requirement of the oral liquid medicine.
Description
Technical Field
The invention relates to the technical field of packaging bags, in particular to a composite packaging bag for oral liquid medicine and a preparation method thereof.
Background
The oral liquid medicine has small dosage, quick absorption and quick effect, and the taste of the liquid medicine is improved by adding the corrective, so that the liquid medicine is easy to take, and has wide use group and large sales. Oral solutions are typically packaged using bottles or plastic bags. Nowadays, bagged oral liquid medicine is used by more and more manufacturers due to the advantages of portability, light weight and the like. The packaging bag for oral liquid medicine is usually made of polyolefin, polylactic acid and other materials, and the packaging bag for oral liquid medicine needs to have the advantages of excellent mechanical property, high barrier property, good air tightness, no toxicity and no easy pollution by external environment substances. However, the mechanical properties and air tightness of the single polyolefin and polylactic acid packaging bag are still to be improved.
In order to solve the problems, prolong the storage time of oral liquid medicine and strengthen the mechanical property of the packaging bag, the invention provides a composite packaging bag for oral liquid medicine and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a composite packaging bag for oral liquid medicine and a preparation method thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a composite packaging bag for oral liquid medicine comprises the following steps:
step one: taking ZIF-L compound and deionized water, and performing ultrasonic dispersion for 30-40min to obtain a dispersion liquid; taking Tris-HCl solution, regulating the pH to 8.5-9, adding dispersion liquid, uniformly stirring, adding dopamine hydrochloride, stirring for 22-24 hours, filtering, washing and drying to obtain the polydopamine-coated ZIF-L; taking ZIF-L coated with polydopamine and deionized water, performing ultrasonic dispersion for 30-40min, adding modified silicon dioxide, stirring for 3-5h, filtering, washing and drying to obtain a ZIF-L-silicon dioxide compound;
step two: taking polypropylene, starch, a defoaming agent, a ZIF-L-silicon dioxide compound and a plasticizer, uniformly mixing, carrying out melt extrusion, blowing a film, cutting and rolling to obtain a modified polypropylene film;
step three: the polyester film, the aluminum foil, the polyamide film and the modified polypropylene film are stacked from top to bottom, compounded, split and bagged to obtain the composite packaging bag for oral liquid medicine.
More preferably, the modified polypropylene film comprises the following components: 50-70 parts of polypropylene, 25-30 parts of starch, 0.5-1 part of defoamer, 3-5 parts of ZIF-L-silicon dioxide compound and 7-10 parts of plasticizer.
More optimally, in the first step, the preparation method of the ZIF-L compound comprises the following steps: taking 2-methylimidazole and deionized water, and uniformly stirring to prepare a 2-methylimidazole aqueous solution; uniformly stirring zinc nitrate hexahydrate and deionized water to prepare a zinc nitrate hexahydrate aqueous solution; and (3) dropwise adding the zinc nitrate hexahydrate aqueous solution into the 2-methylimidazole aqueous solution, stirring for 5-6 hours, centrifuging, washing and drying to obtain the ZIF-L compound.
More optimally, in the first step, the preparation method of the modified silicon dioxide comprises the following steps: and (3) taking epoxy silicon dioxide, hyperbranched polymer, N-dimethylformamide and triethylamine, heating to 125-130 ℃ under the protection of nitrogen, reacting for 5.5-6.5 hours, cooling, filtering, washing and drying to obtain the modified silicon dioxide.
More optimally, the preparation method of the epoxy silicon dioxide comprises the following steps:
step A: taking ethanol, ammonia water and deionized water, uniformly stirring, adding tetraethoxysilane, reacting for 4.5-5.5 hours at 25-30 ℃, centrifuging, and washing to obtain silicon dioxide microspheres;
and (B) step (B): taking silicon dioxide microspheres, ethanol and deionized water, and uniformly stirring to obtain a silicon dioxide solution; uniformly stirring KH560, ethanol and deionized water to obtain KH560 solution; heating the silicon dioxide solution to 68-72 ℃, dropwise adding KH560 solution, reacting for 10-14h at 68-72 ℃, cooling, filtering, and drying to obtain epoxy silicon dioxide.
More optimally, the preparation method of the hyperbranched polymer comprises the following steps: heating and stirring aminoethylpiperazine and chloroform in a nitrogen environment at 35-45 ℃, dropwise adding ethylene glycol dimethacrylate, and reacting for 45-55h to obtain a compound A; heating and stirring compound A and chloroform at 35-45 ℃, adding dodecafluoroheptyl methacrylate, and reacting for 4.5-5.5 hours at 25-35 ℃ to obtain the hyperbranched polymer.
More preferably, the defoamer is silicone oil.
More preferably, the plasticizer is glycerol.
More optimally, the mass ratio of the ZIF-L coated with polydopamine to the modified silicon dioxide is 1: (2-3).
Compared with the prior art, the invention has the following beneficial effects:
(1) Preparing silicon dioxide microspheres, modifying the silicon dioxide microspheres by KH560, introducing epoxy groups on the surface of the silicon dioxide, and grafting the hyperbranched polymer with hydrophobic property on the epoxy silicon dioxide by utilizing ring-opening reaction of amino groups in the hyperbranched polymer and the epoxy groups on the epoxy silicon dioxide to obtain the silicon dioxide with hydrophobic property. The hydrophobic property and mechanical property of the polypropylene film are improved by adding the modified polypropylene into polypropylene.
(2) ZIF-L has excellent ultraviolet absorption performance, and the addition of the ZIF-L compound can enhance the ultraviolet resistance and ageing resistance of the polypropylene film and enhance the tensile strength of the film. However, ZIF-L is a surface porous substance, which can allow oxygen molecules to pass through, so that the oxygen permeation quantity of the polypropylene film is increased. In order to improve the barrier property of ZIF-L, it is compounded with modified silica. The polydopamine is used for compounding the two, and N atoms which are not coordinated in the imidazole ligand on the ZIF-L and zinc ion coordination sites can have hydrogen bonding action or coordination action with hydroxyl groups on the modified silicon dioxide, so that the mechanical property of the polypropylene film is improved. Meanwhile, the composite of the modified silicon dioxide blocks micropores on ZIF-L and improves the barrier property of the polypropylene film.
Meanwhile, the mass ratio of ZIF-L coated with polydopamine to modified silicon dioxide is controlled to be 1: (2-3) at which the performance of the polypropylene film is optimal.
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.
The raw materials and manufacturers used in the examples of the present invention are as follows:
2-methylimidazole was purchased from Shanghai Seiyaka Biotechnology Co., ltd;
zinc nitrate hexahydrate was purchased from Shanghai Ala Biochemical technologies Co., ltd;
aminoethylpiperazine was purchased from Shanghai Ala Biochemical technologies Co., ltd;
chloroform was purchased from the metallocene chemical reagent plant in Tianjin;
ethylene glycol dimethacrylate was purchased from Shanghai Seiyaka Biotech Co., ltd;
dodecafluoroheptyl methacrylate is available from marrong and lautus biotechnology limited;
KH560 is purchased from shanghai source leaf biotechnology limited;
ethyl orthosilicate was purchased from Jin Jinle, hunan chemical Co., ltd;
triethylamine was obtained from Shanghai Ala Biochemical technologies Co., ltd;
Tris-HCl was purchased from Beijing, happy Biotechnology Co., ltd;
dopamine hydrochloride was purchased from Beijing, happy Biotechnology Inc.
Example 1
Step one: preparation of ZIF-L Compounds:
taking 16.4g of 2-methylimidazole and deionized water, and uniformly stirring to prepare 500mL of 2-methylimidazole aqueous solution; taking 7.4g of zinc nitrate hexahydrate and deionized water, and uniformly stirring to prepare 500mL of zinc nitrate hexahydrate aqueous solution; and (3) dropwise adding the zinc nitrate hexahydrate aqueous solution into the 2-methylimidazole aqueous solution, stirring for 5.5 hours, centrifuging, washing and drying to obtain the ZIF-L compound.
Step two: preparation of hyperbranched polymers:
13g of amino ethyl piperazine and 40mL of chloroform are taken, heated and stirred under the nitrogen environment of 40 ℃, 20g of ethylene glycol dimethacrylate is dripped for reaction for 50 hours, the compound A is obtained, 3g of the compound A and 20mL of chloroform are taken, heated and stirred under the temperature of 40 ℃, 0.85g of dodecafluoroheptyl methacrylate is added, and the reaction is carried out for 5 hours under the temperature of 30 ℃ to obtain the hyperbranched polymer.
Step three: preparation of epoxy silica:
taking 80mL of ethanol, 8mL of ammonia water and 30mL of deionized water, uniformly stirring, adding 6mL of tetraethoxysilane, reacting for 5h at 27 ℃, centrifuging and washing to obtain the silica microspheres.
Taking 2g of silicon dioxide microspheres, 70mL of ethanol and 40mL of deionized water, and uniformly stirring to obtain a silicon dioxide solution; taking 2.2mL KH560, 20mL ethanol and 30mL deionized water, and uniformly stirring to obtain KH560 solution; and heating the silicon dioxide solution to 70 ℃, dropwise adding KH560 solution, reacting for 12 hours at 70 ℃, cooling, filtering and drying to obtain the epoxy silicon dioxide.
Step four: preparation of modified silica:
taking 1.8g of epoxy silicon dioxide, 3g of hyperbranched polymer, 150mLN, N-dimethylformamide and 1.5mL of triethylamine, heating to 127 ℃ under the protection of nitrogen, reacting for 6 hours, cooling, filtering, washing and drying to obtain the modified silicon dioxide.
Step five: preparation of ZIF-L-silica composite:
taking 1g of ZIF-L compound and 10mL of deionized water, and performing ultrasonic dispersion for 35min to obtain a dispersion liquid; taking 200ml of Tris-HCl solution, regulating the pH to 8.7, adding the dispersion liquid, uniformly stirring, adding 1g of dopamine hydrochloride, stirring for 23h, filtering, washing and drying to obtain the polydopamine-coated ZIF-L; taking 1g of ZIF-L coated with polydopamine and 100mL of deionized water, performing ultrasonic dispersion for 35min, adding 2.5g of modified silica, stirring for 4h, filtering, washing and drying to obtain a ZIF-L-silica compound.
The mass ratio of the ZIF-L coated with polydopamine to the modified silicon dioxide is 1:2.5.
step six: preparation of modified polypropylene film:
and taking polypropylene, starch, silicone oil, ZIF-L-silicon dioxide compound and glycerin, uniformly mixing, melt extruding, film blowing, slitting and winding to obtain the modified polypropylene film.
The modified polypropylene film comprises the following components: 60 parts of polypropylene, 27 parts of starch, 0.7 part of silicone oil, 4 parts of ZIF-L-silicon dioxide compound and 8 parts of glycerin.
Step seven: a polyester film with the thickness of 12 mu m, an aluminum foil with the thickness of 8 mu m, a polyamide film with the thickness of 20 mu m and a modified polypropylene film with the thickness of 100 mu m are stacked from top to bottom, compounded, split into strips and made into bags to obtain the compound packaging bag for oral liquid medicine.
Example 2
Step one: preparation of ZIF-L Compounds:
taking 16.4g of 2-methylimidazole and deionized water, and uniformly stirring to prepare 500mL of 2-methylimidazole aqueous solution; taking 7.4g of zinc nitrate hexahydrate and deionized water, and uniformly stirring to prepare 500mL of zinc nitrate hexahydrate aqueous solution; and (3) dropwise adding the zinc nitrate hexahydrate aqueous solution into the 2-methylimidazole aqueous solution, stirring for 5 hours, centrifuging, washing and drying to obtain the ZIF-L compound.
Step two: preparation of hyperbranched polymers:
13g of aminoethylpiperazine and 40mL of chloroform are taken, heated and stirred under the nitrogen environment of 35 ℃, 20g of ethylene glycol dimethacrylate is dropwise added for reaction for 45 hours, the compound A is obtained, 3g of the compound A and 20mL of chloroform are taken, heated and stirred under the temperature of 35 ℃, 0.85g of dodecafluoroheptyl methacrylate is added, and the reaction is carried out for 4.5 hours under the temperature of 25 ℃ to obtain the hyperbranched polymer.
Step three: preparation of epoxy silica:
taking 80mL of ethanol, 8mL of ammonia water and 30mL of deionized water, uniformly stirring, adding 6mL of tetraethoxysilane, reacting for 4.5h at 25 ℃, centrifuging and washing to obtain the silica microspheres.
Taking 2g of silicon dioxide microspheres, 70mL of ethanol and 40mL of deionized water, and uniformly stirring to obtain a silicon dioxide solution; taking 2.2mL KH560, 20mL ethanol and 30mL deionized water, and uniformly stirring to obtain KH560 solution; and heating the silicon dioxide solution to 68 ℃, dropwise adding KH560 solution, reacting for 10 hours at 68 ℃, cooling, filtering and drying to obtain the epoxy silicon dioxide.
Step four: preparation of modified silica:
taking 1.8g of epoxy silicon dioxide, 3g of hyperbranched polymer, 150mLN, N-dimethylformamide and 1.5mL of triethylamine, heating to 125 ℃ under the protection of nitrogen, reacting for 5.5h, cooling, filtering, washing and drying to obtain the modified silicon dioxide.
Step five: preparation of ZIF-L-silica composite:
taking 1g of ZIF-L compound and 10mL of deionized water, and performing ultrasonic dispersion for 30min to obtain a dispersion liquid; taking 200ml of Tris-HCl solution, regulating the pH to 8.5, adding the dispersion liquid, uniformly stirring, adding 1g of dopamine hydrochloride, stirring for 22 hours, filtering, washing and drying to obtain the polydopamine-coated ZIF-L; taking 1g of ZIF-L coated with polydopamine and 100mL of deionized water, performing ultrasonic dispersion for 30min, adding 2g of modified silica, stirring for 3h, filtering, washing and drying to obtain the ZIF-L-silica compound.
The mass ratio of the ZIF-L coated with polydopamine to the modified silicon dioxide is 1:2.
step six: preparation of modified polypropylene film:
and taking polypropylene, starch, silicone oil, ZIF-L-silicon dioxide compound and glycerin, uniformly mixing, melt extruding, film blowing, slitting and winding to obtain the modified polypropylene film.
The modified polypropylene film comprises the following components: 50 parts of polypropylene, 25 parts of starch, 0.5 part of silicone oil, 3 parts of ZIF-L-silicon dioxide compound and 7 parts of glycerin.
Step seven: a polyester film with the thickness of 12 mu m, an aluminum foil with the thickness of 8 mu m, a polyamide film with the thickness of 20 mu m and a modified polypropylene film with the thickness of 100 mu m are stacked from top to bottom, compounded, split into strips and made into bags to obtain the compound packaging bag for oral liquid medicine.
Example 3
Step one: preparation of ZIF-L Compounds:
taking 16.4g of 2-methylimidazole and deionized water, and uniformly stirring to prepare 500mL of 2-methylimidazole aqueous solution; taking 7.4g of zinc nitrate hexahydrate and deionized water, and uniformly stirring to prepare 500mL of zinc nitrate hexahydrate aqueous solution; and (3) dropwise adding the zinc nitrate hexahydrate aqueous solution into the 2-methylimidazole aqueous solution, stirring for 6 hours, centrifuging, washing and drying to obtain the ZIF-L compound.
Step two: preparation of hyperbranched polymers:
13g of aminoethylpiperazine and 40mL of chloroform are taken, heated and stirred under the nitrogen environment of 45 ℃, 20g of ethylene glycol dimethacrylate is dropwise added for reaction for 55 hours, the compound A is obtained, 3g of the compound A and 20mL of chloroform are taken, heated and stirred under the temperature of 45 ℃, 0.85g of dodecafluoroheptyl methacrylate is added for reaction for 5.5 hours at the temperature of 35 ℃, and the hyperbranched polymer is obtained.
Step three: preparation of epoxy silica:
taking 80mL of ethanol, 8mL of ammonia water and 30mL of deionized water, uniformly stirring, adding 6mL of tetraethoxysilane, reacting for 5.5h at 30 ℃, centrifuging and washing to obtain the silica microspheres.
Taking 2g of silicon dioxide microspheres, 70mL of ethanol and 40mL of deionized water, and uniformly stirring to obtain a silicon dioxide solution; taking 2.2mL KH560, 20mL ethanol and 30mL deionized water, and uniformly stirring to obtain KH560 solution; and heating the silicon dioxide solution to 72 ℃, dropwise adding KH560 solution, reacting for 14h at 72 ℃, cooling, filtering and drying to obtain the epoxy silicon dioxide.
Step four: preparation of modified silica:
taking 1.8g of epoxy silicon dioxide, 3g of hyperbranched polymer, 150mLN, N-dimethylformamide and 1.5mL of triethylamine, heating to 130 ℃ under the protection of nitrogen, reacting for 6.5h, cooling, filtering, washing and drying to obtain the modified silicon dioxide.
Step five: preparation of ZIF-L-silica composite:
taking 1g of ZIF-L compound and 10mL of deionized water, and performing ultrasonic dispersion for 40min to obtain a dispersion liquid; taking 200ml of Tris-HCl solution, regulating the pH to 9, adding the dispersion liquid, uniformly stirring, adding 1g of dopamine hydrochloride, stirring for 24 hours, filtering, washing and drying to obtain the polydopamine-coated ZIF-L; taking 1g of ZIF-L coated with polydopamine and 100mL of deionized water, performing ultrasonic dispersion for 40min, adding 3g of modified silica, stirring for 5h, filtering, washing and drying to obtain the ZIF-L-silica compound.
The mass ratio of the ZIF-L coated with polydopamine to the modified silicon dioxide is 1:3.
step six: preparation of modified polypropylene film:
and taking polypropylene, starch, silicone oil, ZIF-L-silicon dioxide compound and glycerin, uniformly mixing, melt extruding, film blowing, slitting and winding to obtain the modified polypropylene film.
The modified polypropylene film comprises the following components: 70 parts of polypropylene, 30 parts of starch, 1 part of silicone oil, 5 parts of ZIF-L-silicon dioxide compound and 10 parts of glycerin.
Step seven: a polyester film with the thickness of 12 mu m, an aluminum foil with the thickness of 8 mu m, a polyamide film with the thickness of 20 mu m and a modified polypropylene film with the thickness of 100 mu m are stacked from top to bottom, compounded, split into strips and made into bags to obtain the compound packaging bag for oral liquid medicine.
Example 4: the silica was modified without adding hyperbranched polymer, and the rest was the same as in example 1.
Step one: preparation of ZIF-L Compounds:
taking 16.4g of 2-methylimidazole and deionized water, and uniformly stirring to prepare 500mL of 2-methylimidazole aqueous solution; taking 7.4g of zinc nitrate hexahydrate and deionized water, and uniformly stirring to prepare 500mL of zinc nitrate hexahydrate aqueous solution; and (3) dropwise adding the zinc nitrate hexahydrate aqueous solution into the 2-methylimidazole aqueous solution, stirring for 5.5 hours, centrifuging, washing and drying to obtain the ZIF-L compound.
Step two: preparation of silica microspheres:
taking 80mL of ethanol, 8mL of ammonia water and 30mL of deionized water, uniformly stirring, adding 6mL of tetraethoxysilane, reacting for 5h at 27 ℃, centrifuging and washing to obtain the silica microspheres.
Step three: preparation of ZIF-L-silica composite:
taking 1g of ZIF-L compound and 10mL of deionized water, and performing ultrasonic dispersion for 35min to obtain a dispersion liquid; taking 200ml of Tris-HCl solution, regulating the pH to 8.7, adding the dispersion liquid, uniformly stirring, adding 1g of dopamine hydrochloride, stirring for 23h, filtering, washing and drying to obtain the polydopamine-coated ZIF-L; taking 1g of ZIF-L coated with polydopamine and 100mL of deionized water, performing ultrasonic dispersion for 35min, adding 2.5g of silica microspheres, stirring for 4h, filtering, washing and drying to obtain the ZIF-L-silica composite.
The mass ratio of the ZIF-L coated with polydopamine to the modified silicon dioxide is 1:2.5.
step four: preparation of modified polypropylene film:
and taking polypropylene, starch, silicone oil, ZIF-L-silicon dioxide compound and glycerin, uniformly mixing, melt extruding, film blowing, slitting and winding to obtain the modified polypropylene film.
The modified polypropylene film comprises the following components: 60 parts of polypropylene, 27 parts of starch, 0.7 part of silicone oil, 4 parts of ZIF-L-silicon dioxide compound and 8 parts of glycerin.
Step five: a polyester film with the thickness of 12 mu m, an aluminum foil with the thickness of 8 mu m, a polyamide film with the thickness of 20 mu m and a modified polypropylene film with the thickness of 100 mu m are stacked from top to bottom, compounded, split into strips and made into bags to obtain the compound packaging bag for oral liquid medicine.
Example 5: silica was not added, and the rest was the same as in example 1.
Step one: preparation of ZIF-L Compounds:
taking 16.4g of 2-methylimidazole and deionized water, and uniformly stirring to prepare 500mL of 2-methylimidazole aqueous solution; taking 7.4g of zinc nitrate hexahydrate and deionized water, and uniformly stirring to prepare 500mL of zinc nitrate hexahydrate aqueous solution; and (3) dropwise adding the zinc nitrate hexahydrate aqueous solution into the 2-methylimidazole aqueous solution, stirring for 5.5 hours, centrifuging, washing and drying to obtain the ZIF-L compound.
Step two: preparation of modified polypropylene film:
and taking polypropylene, starch, silicone oil, ZIF-L compound and glycerin, uniformly mixing, carrying out melt extrusion, film blowing, slitting and rolling to obtain the modified polypropylene film.
The modified polypropylene film comprises the following components: 60 parts of polypropylene, 27 parts of starch, 0.7 part of silicone oil, 4 parts of ZIF-L-silicon dioxide compound and 8 parts of glycerin.
Step three: a polyester film with the thickness of 12 mu m, an aluminum foil with the thickness of 8 mu m, a polyamide film with the thickness of 20 mu m and a modified polypropylene film with the thickness of 100 mu m are stacked from top to bottom, compounded, split into strips and made into bags to obtain the compound packaging bag for oral liquid medicine.
Example 6: the mass ratio of ZIF-L coated with polydopamine to modified silicon dioxide is controlled to be 1:1, the remainder being the same as in example 1.
Experiment
The modified polypropylene films prepared in examples 1 to 6 were subjected to performance test. The tensile strength of the modified polypropylene film was tested using an electronic tensile machine. The water vapor permeability of the modified polypropylene film was measured by a weight loss method using a water vapor permeability tester. The oxygen permeation amount of the modified polypropylene film was measured using a gas permeation tester by a differential pressure method. Contact angles were measured using a drop shape analyzer, with water being deionized water having a volume of 5 μl. The data obtained are shown below:
conclusion: as is clear from the data in the table, in example 4, the silica was modified without adding the hyperbranched polymer, the water vapor permeability was increased, the waterproof performance was deteriorated, and in example 5, the use performance of the polypropylene film was deteriorated without adding the silica. Example 6 the mass ratio of ZIF-L coated with polydopamine to modified silica was 1:1, the amount of the modified silica added becomes small, the water repellency becomes poor, the mechanical properties of the polypropylene film become poor, and at the same time, the oxygen permeation amount of the polypropylene film becomes large and the barrier property becomes poor due to the increased amount of the porous ZIF-L compound added.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a composite packaging bag for oral liquid medicine is characterized by comprising the following steps: the method comprises the following steps:
step one: taking ZIF-L compound and deionized water, and performing ultrasonic dispersion for 30-40min to obtain a dispersion liquid; taking Tris-HCl solution, regulating the pH to 8.5-9, adding dispersion liquid, uniformly stirring, adding dopamine hydrochloride, stirring for 22-24 hours, filtering, washing and drying to obtain the polydopamine-coated ZIF-L; taking ZIF-L coated with polydopamine and deionized water, performing ultrasonic dispersion for 30-40min, adding modified silicon dioxide, stirring for 3-5h, filtering, washing and drying to obtain a ZIF-L-silicon dioxide compound;
step two: taking polypropylene, starch, a defoaming agent, a ZIF-L-silicon dioxide compound and a plasticizer, uniformly mixing, carrying out melt extrusion, blowing a film, cutting and rolling to obtain a modified polypropylene film;
step three: the polyester film, the aluminum foil, the polyamide film and the modified polypropylene film are stacked from top to bottom, compounded, split and bagged to obtain the composite packaging bag for oral liquid medicine.
2. The method for preparing a composite packaging bag for oral liquid according to claim 1, wherein: the modified polypropylene film comprises the following components: 50-70 parts of polypropylene, 25-30 parts of starch, 0.5-1 part of defoamer, 3-5 parts of ZIF-L-silicon dioxide compound and 7-10 parts of plasticizer.
3. The method for preparing a composite packaging bag for oral liquid according to claim 1, wherein: in the first step, the ZIF-L compound is prepared by the following steps: taking 2-methylimidazole and deionized water, and uniformly stirring to prepare a 2-methylimidazole aqueous solution; uniformly stirring zinc nitrate hexahydrate and deionized water to prepare a zinc nitrate hexahydrate aqueous solution; and (3) dropwise adding the zinc nitrate hexahydrate aqueous solution into the 2-methylimidazole aqueous solution, stirring for 5-6 hours, centrifuging, washing and drying to obtain the ZIF-L compound.
4. The method for preparing a composite packaging bag for oral liquid according to claim 1, wherein: in the first step, the preparation method of the modified silicon dioxide comprises the following steps: and (3) taking epoxy silicon dioxide, hyperbranched polymer, N-dimethylformamide and triethylamine, heating to 125-130 ℃ under the protection of nitrogen, reacting for 5.5-6.5 hours, cooling, filtering, washing and drying to obtain the modified silicon dioxide.
5. The method for preparing a composite packaging bag for oral liquid according to claim 4, wherein: the preparation method of the epoxy silicon dioxide comprises the following steps:
step A: taking ethanol, ammonia water and deionized water, uniformly stirring, adding tetraethoxysilane, reacting for 4.5-5.5 hours at 25-30 ℃, centrifuging, and washing to obtain silicon dioxide microspheres;
and (B) step (B): taking silicon dioxide microspheres, ethanol and deionized water, and uniformly stirring to obtain a silicon dioxide solution; uniformly stirring KH560, ethanol and deionized water to obtain KH560 solution; heating the silicon dioxide solution to 68-72 ℃, dropwise adding KH560 solution, reacting for 10-14h at 68-72 ℃, cooling, filtering, and drying to obtain epoxy silicon dioxide.
6. The method for preparing a composite packaging bag for oral liquid according to claim 4, wherein: the preparation method of the hyperbranched polymer comprises the following steps: heating and stirring aminoethylpiperazine and chloroform in a nitrogen environment at 35-45 ℃, dropwise adding ethylene glycol dimethacrylate, and reacting for 45-55h to obtain a compound A; heating and stirring compound A and chloroform at 35-45 ℃, adding dodecafluoroheptyl methacrylate, and reacting for 4.5-5.5 hours at 25-35 ℃ to obtain the hyperbranched polymer.
7. The method for preparing a composite packaging bag for oral liquid according to claim 1, wherein: the defoaming agent is silicone oil.
8. The method for preparing a composite packaging bag for oral liquid according to claim 1, wherein: the plasticizer is glycerol.
9. The method for preparing a composite packaging bag for oral liquid according to claim 1, wherein: the mass ratio of the ZIF-L coated with polydopamine to the modified silicon dioxide is 1: (2-3).
10. A composite packaging bag for oral liquid according to any one of claims 1 to 9.
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| CN106279033A (en) * | 2016-08-05 | 2017-01-04 | 安徽建筑大学 | Lamellar intersection ZIF L and preparation method thereof |
| CN112225985A (en) * | 2020-09-04 | 2021-01-15 | 万华化学（宁波）有限公司 | Flame-retardant PP composite material and preparation method thereof |
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Denomination of invention: A composite packaging bag for oral medication and its preparation method Granted publication date: 20230912 Pledgee: Jiangyin branch of Bank of China Ltd. Pledgor: Jiangyin Shenmei packaging material Co.,Ltd. Registration number: Y2024980002440 |