CN116139321A - PLA nanocomposite and preparation method thereof - Google Patents
PLA nanocomposite and preparation method thereof Download PDFInfo
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- CN116139321A CN116139321A CN202310307064.5A CN202310307064A CN116139321A CN 116139321 A CN116139321 A CN 116139321A CN 202310307064 A CN202310307064 A CN 202310307064A CN 116139321 A CN116139321 A CN 116139321A
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- polylactic acid
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 145
- 239000004626 polylactic acid Substances 0.000 claims abstract description 136
- 238000009987 spinning Methods 0.000 claims abstract description 64
- 239000002131 composite material Substances 0.000 claims abstract description 54
- -1 rare earth compound Chemical class 0.000 claims abstract description 38
- 239000002086 nanomaterial Substances 0.000 claims abstract description 37
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002070 nanowire Substances 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000000839 emulsion Substances 0.000 claims abstract description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 239000010703 silicon Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 150000007524 organic acids Chemical class 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 37
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 18
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000005096 rolling process Methods 0.000 claims description 9
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 8
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 8
- 239000001630 malic acid Substances 0.000 claims description 8
- 235000011090 malic acid Nutrition 0.000 claims description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 4
- WFJXYIUAMJAURQ-UHFFFAOYSA-N 2-propan-2-ylsulfinylpropane Chemical compound CC(C)S(=O)C(C)C WFJXYIUAMJAURQ-UHFFFAOYSA-N 0.000 claims description 3
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 3
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000004334 sorbic acid Substances 0.000 claims description 2
- 235000010199 sorbic acid Nutrition 0.000 claims description 2
- 229940075582 sorbic acid Drugs 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 9
- 229940079593 drug Drugs 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 206010052428 Wound Diseases 0.000 description 9
- 208000027418 Wounds and injury Diseases 0.000 description 9
- 239000004745 nonwoven fabric Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 230000006750 UV protection Effects 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 229910052684 Cerium Inorganic materials 0.000 description 4
- 239000010410 layer Substances 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000011241 protective layer Substances 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 235000016068 Berberis vulgaris Nutrition 0.000 description 1
- 241000335053 Beta vulgaris Species 0.000 description 1
- 208000005422 Foreign-Body reaction Diseases 0.000 description 1
- 206010039509 Scab Diseases 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 210000000416 exudates and transudate Anatomy 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/26—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/425—Porous materials, e.g. foams or sponges
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/62—Compostable, hydrosoluble or hydrodegradable materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
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- 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 application provides a PLA nanocomposite and a preparation method thereof, and relates to the technical field of nanomaterials. The preparation method comprises the following steps: dissolving polylactic acid in a solvent to prepare polylactic acid solution; dissolving rare earth compound in organic acid, and then adding ethanol solution to prepare rare earth ion precursor solution; adding the rare earth ion precursor solution into the polylactic acid solution under the condition of constant temperature stirring, and uniformly mixing to obtain spinning solution; spinning the spinning solution by adopting an electrostatic spinning process, and drying to obtain polylactic acid composite nano-filaments; and padding the polylactic acid composite nano wire in the organic silicon emulsion, and drying to obtain the polylactic acid composite nano material. The polylactic acid polymer is adopted as the main raw material of the composite nano material, and rare earth ions are doped, so that the polylactic acid polymer has excellent biodegradability, regenerability, safety and high specific surface area, has a high drug carrying function, and can be used for various products in the field of biological medicine.
Description
Technical Field
The application relates to the technical field of nano materials, in particular to a PLA nano composite material and a preparation method thereof.
Background
In daily activities, skin is used as a first defense line of a human body, and when the skin is damaged by external stimuli such as burns, wounds, operations and the like, wounds formed on the surface of the skin can cause other complications if not treated in time; medical dressing refers to a cover for wrapping a wound, which mainly serves to protect the wound skin and provide a good environment for wound healing.
The traditional medical dressing is mainly made of natural fiber materials such as sterile cotton, gauze strips, cotton films and the like, and can only be used for drying and physically isolating wounds. Although the traditional dressing has the characteristics of simple acquisition, easy manufacture, low price and the like, the traditional dressing also has a plurality of disadvantages, such as: traditional dressing is easy to cause wound bonding after wound exudate crusts, new wounds can be caused when dressing changes are carried out, pain is also accompanied, traditional dressing also has no ability of rapid healing, pathogens can easily enter the wounds to cause bacterial growth, and more medical resources are occupied when dressing changes are carried out.
Polylactic acid (PLA) fiber is a synthetic fiber obtained by fermenting starch such as wheat, corn, beet, potato, etc. into lactic acid and polymerizing and spinning, and can be decomposed into CO under certain conditions 2 And water, has excellent biodegradability and regenerability, and does not cause foreign body reaction to organisms, has been widely used in the field of modern biological medicine, but the current polylactic acid (PLA) dressing has obvious disadvantages of poor antibacterial property, and the surface of the polylactic acid nonwoven fabric is easy to adhere bacteria, thus bringing a plurality of hazards to human bodies.
Disclosure of Invention
The aim of the application is to provide a preparation method of PLA nanocomposite, which is to dope rare earth ions into polylactic acid nanomaterial to improve the antibacterial property of the polylactic acid nanocomposite.
Another object of the present application is to provide a PLA nanocomposite with the advantages of good antimicrobial properties, uv-resistance stability.
In order to solve the technical problems, the application adopts the technical scheme that:
in one aspect, the present application provides a method of preparing a PLA nanocomposite, comprising the steps of:
dissolving polylactic acid in a solvent to prepare polylactic acid solution;
dissolving rare earth compound in organic acid, and then adding ethanol solution to prepare rare earth ion precursor solution;
adding the rare earth ion precursor solution into the polylactic acid solution under the condition of constant temperature stirring, and uniformly mixing to obtain spinning solution;
spinning the spinning solution by adopting an electrostatic spinning process, and drying to obtain polylactic acid composite nano-filaments;
and padding the polylactic acid composite nano wire in the organic silicon emulsion, and drying to obtain the polylactic acid composite nano material.
On the other hand, the application provides the PLA nanocomposite prepared by the preparation method.
Compared with the prior art, the embodiment of the application has at least the following advantages or beneficial effects:
the polylactic acid polymer is adopted as the main raw material of the composite nano material, and the biodegradability, the regenerability and the safety of the polylactic acid polymer, the porosity, the pore connectivity and the high specific surface area of the nano material are utilized, so that the polylactic acid polymer has a high drug carrying function and can be used for various products in the field of biological medicine. The rare earth elements are doped in the polylactic acid, and the polylactic acid nano material can be used as a carrier of rare earth ions, so that the rare earth ions are attached to the pores of the polylactic acid nano material, and the antibacterial property of the polylactic acid nano material is improved.
In addition, the polylactic acid composite nano wire is immersed in the organic silicon emulsion, a layer of protective film can be formed on the surface of the polylactic acid composite nano wire by the organic silicon emulsion, the rare earth ions doped in the polylactic acid nano material are prevented from falling off, the ultraviolet resistance of the whole composite material can be improved by the protective layer, and the service life of the composite material is prolonged.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail with reference to specific examples.
A method for preparing a PLA nanocomposite, comprising the steps of:
dissolving polylactic acid in a solvent to prepare polylactic acid solution;
dissolving rare earth compound in organic acid, and then adding ethanol solution to prepare rare earth ion precursor solution;
adding the rare earth ion precursor solution into the polylactic acid solution under the condition of constant temperature stirring, and uniformly mixing to obtain spinning solution;
spinning the spinning solution by adopting an electrostatic spinning process, and drying to obtain polylactic acid composite nano-filaments;
and padding the polylactic acid composite nano wire in the organic silicon emulsion, and drying to obtain the polylactic acid composite nano material.
The polylactic acid polymer is adopted as the main raw material of the composite nano material, and the biodegradability, the regenerability and the safety of the polylactic acid polymer, the porosity, the pore connectivity and the high specific surface area of the nano material are utilized, so that the polylactic acid polymer has a high drug carrying function and can be used for various products in the field of biological medicine. The rare earth elements are doped in the polylactic acid, and the polylactic acid nano material can be used as a carrier of rare earth ions, so that the rare earth ions are attached to the pores of the polylactic acid nano material, and the antibacterial property of the polylactic acid nano material is improved.
In addition, the polylactic acid composite nano wire is immersed in the organic silicon emulsion, a layer of protective film can be formed on the surface of the polylactic acid composite nano wire by the organic silicon emulsion, the rare earth ions doped in the polylactic acid nano material are prevented from falling off, the ultraviolet resistance of the whole composite material can be improved by the protective layer, and the service life of the composite material is prolonged.
In some embodiments of the present application, the solvent is one or more mixed solvents of dichloromethane, chloroform, diisopropyl sulfoxide and N, N-dimethylformamide, and the mass fraction of the polylactic acid solution is 5-15%.
In some embodiments of the present application, the rare earth compound is cerium oxide, cerium nitrate, cerium chloride, lanthanum oxide, lanthanum nitrate, or lanthanum chloride.
In some embodiments of the present application, the organic acid is formic acid, acetic acid, malic acid or sorbic acid, the concentration of the ethanol is 50-60%, and the rare earth ion content in the rare earth ion precursor solution is 40-60%.
In some embodiments of the present application, the mass of the rare earth compound is 1-8% of the mass of the polylactic acid.
In some embodiments of the present application, the spinning step is specifically: adding the spinning solution into an electrostatic spinning machine, adjusting the spinning voltage to 5-20kv, the propelling speed of a liquid propeller to 0.1-0.2mm/s, the rotating speed of a receiving roller to 50-100r/min, and the receiving distance to 10-15cm.
In some embodiments of the present application, the drying temperature is 60-80 ℃ and the drying time is 24-48 hours.
In some embodiments of the present application, the padding is performed at a temperature of 30-40 ℃ for 20-40min, and the rolling allowance is 70-80%.
In some embodiments of the present application, the drying temperature is 50-60 ℃ and the drying time is 10-30min.
A PLA nanocomposite is prepared by the preparation method.
The features and capabilities of the present application are described in further detail below in connection with the examples.
Example 1
A PLA nanocomposite is prepared by the following steps:
1) Placing 50g of polylactic acid into a dichloromethane solvent, stirring and completely dissolving to prepare 10% by mass of polylactic acid liquid for later use;
2) Weighing 3g of cerium oxide, adding malic acid, heating and stirring for 10min at 50 ℃ to fully dissolve, and then adding an ethanol solution with the concentration of 60% to prepare a precursor solution with the cerium ion of 55%;
3) Stirring the polylactic acid liquid at a constant temperature of 35 ℃, adding the precursor liquid, and uniformly mixing to obtain spinning liquid;
4) Adding the spinning solution into a meter of an electrostatic spinning machine, adjusting the spinning voltage to 10kv, the propelling speed of a liquid propeller to 0.15mm/s, the rotating speed of a receiving roller to 80r/min, and the receiving distance to 12cm, spinning the spinning solution, then drying the spinning solution in a constant-temperature oven at 70 ℃ for 24 hours, and removing the solvent to obtain the polylactic acid composite nano-wire;
5) Padding the polylactic acid composite nano-wire in organic silicon emulsion at the temperature of 35 ℃ for 30min and the rolling allowance of 70%, and drying in a 55 ℃ oven for 20min to obtain the polylactic acid composite nano-material of the embodiment.
Example 2
A PLA nanocomposite is prepared by the following steps:
1) Placing 50g of polylactic acid into a chloroform solvent, stirring and completely dissolving to prepare 8% of polylactic acid liquid for later use;
2) Weighing 3.5g of lanthanum oxide, adding malic acid, heating and stirring at 55 ℃ for 10min to fully dissolve, and then adding 50% ethanol solution to prepare a precursor solution with lanthanum ions of 45%;
3) Stirring the polylactic acid liquid at a constant temperature of 35 ℃, slowly adding the precursor liquid, and continuously stirring and uniformly mixing to obtain spinning liquid;
4) Adding the spinning solution into a meter of an electrostatic spinning machine, adjusting the spinning voltage to 15kv, adjusting the propelling speed of a liquid propeller to 0.1mm/s, adjusting the rotating speed of a receiving roller to 100r/min and the receiving distance to 15cm, spinning the spinning solution, drying the spinning solution in a constant-temperature oven at 75 ℃ for 36 hours, and removing the solvent to obtain the polylactic acid composite nano-wire;
5) Padding the polylactic acid composite nano-wires in organic silicon emulsion at the temperature of 35 ℃ for 30min and the rolling allowance of 75%, and drying in a 60 ℃ oven for 20min to obtain the polylactic acid composite nano-material of the embodiment.
Example 3
A PLA nanocomposite is prepared by the following steps:
1) Placing 50g of polylactic acid into a chloroform solvent, stirring and completely dissolving to prepare a polylactic acid solution with the mass fraction of 6% for later use;
2) Weighing 1g of lanthanum nitrate, adding malic acid, heating and stirring for 10min at 55 ℃ to fully dissolve, and then adding an ethanol solution with the concentration of 50% to prepare a precursor solution with lanthanum ions of 40%;
3) Stirring the polylactic acid liquid at a constant temperature of 35 ℃, slowly adding the precursor liquid, and continuously stirring and uniformly mixing to obtain spinning liquid;
4) Adding the spinning solution into a meter of an electrostatic spinning machine, adjusting the spinning voltage to 5kv, the propelling speed of a liquid propeller to 0.1mm/s, the rotating speed of a receiving roller to 50r/min, the receiving distance to 10cm, spinning the spinning solution, and then drying the spinning solution in a constant-temperature oven at 75 ℃ for 48 hours, and removing the solvent to obtain the polylactic acid composite nano-wire;
5) Padding the polylactic acid composite nano-wire in organic silicon emulsion at the temperature of 35 ℃ for 30min and the rolling allowance of 70%, and drying in a 60 ℃ oven for 10min to obtain the polylactic acid composite nano-material of the embodiment.
Example 4
A PLA nanocomposite is prepared by the following steps:
1) Placing 50g of polylactic acid into a diisopropyl sulfoxide solvent, stirring and completely dissolving to prepare 7% by mass of polylactic acid liquid for later use;
2) Weighing 3g of lanthanum chloride, adding acetic acid, heating and stirring for 15min at 60 ℃ to fully dissolve, and then adding an ethanol solution with the concentration of 50% to prepare a precursor solution with the lanthanum ion of 55%;
3) Stirring the polylactic acid liquid at a constant temperature of 30 ℃, slowly adding the precursor liquid, and continuously stirring and uniformly mixing to obtain spinning liquid;
4) Adding the spinning solution into a meter of an electrostatic spinning machine, adjusting the spinning voltage to 12kv, adjusting the propelling speed of a liquid propeller to 0.2mm/s, adjusting the rotating speed of a receiving roller to 100r/min and the receiving distance to 12cm, spinning the spinning solution, drying the spinning solution in a constant-temperature oven at 80 ℃ for 36 hours, and removing the solvent to obtain the polylactic acid composite nano-wire;
5) Padding the polylactic acid composite nano-wires in organic silicon emulsion at 38 ℃ for 30min with the rolling allowance of 80%, and drying in a 60 ℃ oven for 10min to obtain the polylactic acid composite nano-material of the embodiment.
Example 5
A PLA nanocomposite is prepared by the following steps:
1) 50g of polylactic acid was put in a mixed solvent of methylene chloride and N, N-dimethylformamide (volume ratio 1: 1) After stirring and completely dissolving, preparing the polylactic acid liquid with the mass fraction of 6 percent for standby;
2) Weighing 2g of cerium chloride, adding malic acid, heating and stirring for 10min at 60 ℃ to fully dissolve, and then adding an ethanol solution with the concentration of 50% to prepare a precursor solution with the cerium ion of 50%;
3) Stirring the polylactic acid liquid at a constant temperature of 35 ℃, slowly adding the precursor liquid, and continuously stirring and uniformly mixing to obtain spinning liquid;
4) Adding the spinning solution into a meter of an electrostatic spinning machine, adjusting the spinning voltage to 8kv, adjusting the propelling speed of a liquid propeller to 0.2mm/s, adjusting the rotating speed of a receiving roller to 100r/min and the receiving distance to 12cm, spinning the spinning solution, drying the spinning solution in a constant-temperature oven at 75 ℃ for 48 hours, and removing the solvent to obtain the polylactic acid composite nano-wire;
5) Padding the polylactic acid composite nano-wire in organic silicon emulsion at 38 ℃ for 30min with the rolling allowance of 80%, and drying in a 55 ℃ oven for 10min to obtain the polylactic acid composite nano-material of the embodiment.
Example 6
A PLA nanocomposite is prepared by the following steps:
1) Placing 50g of polylactic acid into a chloroform solvent, stirring and completely dissolving to prepare a polylactic acid solution with the mass fraction of 6% for later use;
2) Weighing 4g of cerium chloride, adding malic acid, heating and stirring for 10min at 60 ℃ to fully dissolve, and then adding an ethanol solution with the concentration of 50% to prepare a precursor solution with the cerium ion of 60%;
3) Stirring the polylactic acid liquid at a constant temperature of 35 ℃, slowly adding the precursor liquid, and continuously stirring and uniformly mixing to obtain spinning liquid;
4) Adding the spinning solution into a meter of an electrostatic spinning machine, adjusting the spinning voltage to 10kv, the propelling speed of a liquid propeller to 0.15mm/s, the rotating speed of a receiving roller to 90r/min, and the receiving distance to 12cm, spinning the spinning solution, drying in a constant-temperature oven at 70 ℃ for 48 hours, and removing the solvent to obtain the polylactic acid composite nano-wire;
5) Padding the polylactic acid composite nano-wires in organic silicon emulsion at 38 ℃ for 30min with the rolling allowance of 80%, and drying in a 50 ℃ oven for 30min to obtain the polylactic acid composite nano-material of the embodiment.
Comparative example 1
The difference between the comparative example and the example 1 is that the comparative example is not doped with rare earth element, namely the preparation method of the polylactic acid nanocomposite of the comparative example is as follows:
1) Placing 50g of polylactic acid into a dichloromethane solvent, stirring and completely dissolving to prepare 10% by mass of polylactic acid liquid for later use;
2) Adding the polylactic acid solution into a meter of an electrostatic spinning machine, adjusting the spinning voltage to 10kv, adjusting the propelling speed of a liquid propeller to 0.15mm/s, adjusting the rotating speed of a receiving roller to 80r/min and the receiving distance to 12cm, spinning the spinning solution, drying in a constant-temperature oven at 70 ℃ for 24 hours, and removing the solvent to obtain the polylactic acid composite nano-wire;
3) Padding the polylactic acid composite nano-wire in organic silicon emulsion at the temperature of 35 ℃ for 30min and the rolling allowance of 70%, and drying in a 55 ℃ oven for 20min to obtain the polylactic acid composite nano-material of the embodiment.
Comparative example 2
The present comparative example is different from example 1 in that the polylactic acid composite nanowire prepared in the present comparative example is not padded in the silicone emulsion. The method comprises the following specific steps:
1) Placing 50g of polylactic acid into a dichloromethane solvent, stirring and completely dissolving to prepare 10% by mass of polylactic acid liquid for later use;
2) Weighing 3g of cerium oxide, adding malic acid, heating and stirring for 10min at 50 ℃ to fully dissolve, and then adding an ethanol solution with the concentration of 60% to prepare a precursor solution with the cerium ion of 55%;
3) Stirring the polylactic acid liquid at a constant temperature of 35 ℃, adding the precursor liquid, and uniformly mixing to obtain spinning liquid;
4) Adding the spinning solution into a meter of an electrostatic spinning machine, adjusting the spinning voltage to 10kv, adjusting the propelling speed of a liquid propeller to 0.15mm/s, adjusting the rotating speed of a receiving roller to 80r/min and the receiving distance to 12cm, spinning the spinning solution, and then drying the spinning solution in a constant-temperature oven at 70 ℃ for 24 hours, and removing the solvent in the spinning solution to obtain the polylactic acid composite nanomaterial of the comparative example.
Experimental example
The polylactic acid composite nanomaterial prepared in examples 1-3 and comparative examples 1-2 was prepared into a polylactic acid composite nanomaterial nonwoven fabric by the same preparation process.
Firstly, the antibacterial performance of the polylactic acid composite nano material non-woven fabrics of each experimental group is tested by adopting an AATCC100-2004 antibacterial test standard, and a blank group (common polylactic acid non-woven fabrics) is additionally arranged. And calculating the bacteriostasis rate.
Wherein, the antibacterial ratio= (number of inoculated colonies-number of residual colonies after test)/number of inoculated colonies.
The results are shown in Table 1.
TABLE 1
| Experimental group | Staphylococcus aureus antibacterial rate/% | Coli antibacterial rate/% |
| Example 1 | 99.99 | 99.97 |
| Example 2 | 99.99 | 100 |
| Example 3 | 99.97 | 99.99 |
| Comparative example 1 | 96.28 | 95.59 |
| Comparative example 2 | 97.38 | 97.84 |
| Blank group | 32.86 | 41.14 |
As can be seen from Table 1, the polylactic acid nanocomposite nonwoven fabrics prepared in examples 1-3 of the present application have better and stable antibacterial properties.
And (II) carrying out ultraviolet irradiation treatment on the polylactic acid nanocomposite nonwoven fabrics in the examples 1-3 and the comparative examples 1-2, wherein the parameters of each experimental group are the same during the treatment, and the treatment time is 12 hours. After treatment, each experimental group was subjected to bacteriostasis test, and the test method was the same as that of experimental example (one). The antibacterial effect is shown in Table 2.
TABLE 2
From the comparison between table 1 and table 2, it can be seen that the polylactic acid nanocomposite nonwoven fabrics prepared in examples 1-3 of the present application can still maintain high antibacterial performance after 12 hours of ultraviolet irradiation, which indicates that the polylactic acid nanocomposite nonwoven fabrics have good ultraviolet resistance stability. The antibacterial rate in comparative example 2 is greatly reduced, which indicates that the organosilicon emulsion has better effect on ultraviolet resistance.
In summary, the PLA nanocomposite and the preparation method thereof according to the embodiments of the present application have the following advantages:
the polylactic acid polymer is adopted as the main raw material of the composite nano material, and the biodegradability, the regenerability and the safety of the polylactic acid polymer, the porosity, the pore connectivity and the high specific surface area of the nano material are utilized, so that the polylactic acid polymer has a high drug carrying function and can be used for various products in the field of biological medicine. The rare earth elements are doped in the polylactic acid, and the polylactic acid nano material can be used as a carrier of rare earth ions, so that the rare earth ions are attached to the pores of the polylactic acid nano material, and the antibacterial property of the polylactic acid nano material is improved.
In addition, the polylactic acid composite nano wire is immersed in the organic silicon emulsion, a layer of protective film can be formed on the surface of the polylactic acid composite nano wire by the organic silicon emulsion, the rare earth ions doped in the polylactic acid nano material are prevented from falling off, the ultraviolet resistance of the whole composite material can be improved by the protective layer, and the service life of the composite material is prolonged.
The embodiments described above are some, but not all, of the embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
Claims (10)
1. A method for preparing a PLA nanocomposite, comprising the steps of:
dissolving polylactic acid in a solvent to prepare polylactic acid solution;
dissolving rare earth compound in organic acid, and then adding ethanol solution to prepare rare earth ion precursor solution;
adding the rare earth ion precursor solution into the polylactic acid solution under the condition of constant temperature stirring, and uniformly mixing to obtain spinning solution;
spinning the spinning solution by adopting an electrostatic spinning process, and drying to obtain polylactic acid composite nano-filaments;
and padding the polylactic acid composite nano wire in the organic silicon emulsion, and drying to obtain the polylactic acid composite nano material.
2. The preparation method of the PLA nanocomposite material according to claim 1, wherein the solvent is one or more mixed solvents of dichloromethane, chloroform, diisopropyl sulfoxide and N, N-dimethylformamide, and the mass fraction of the polylactic acid solution is 5-15%.
3. The method for preparing a PLA nanocomposite according to claim 1, wherein the rare earth compound is cerium oxide, cerium nitrate, cerium chloride, lanthanum oxide, lanthanum nitrate, or lanthanum chloride.
4. The method for preparing a PLA nanocomposite according to claim 3, wherein the organic acid is formic acid, acetic acid, malic acid or sorbic acid, the concentration of ethanol is 50-60%, and the content of rare earth ions in the rare earth ion precursor solution is 40-60%.
5. The method for preparing a PLA nanocomposite according to claim 1, wherein the mass of the rare earth compound is 1-8% of the mass of the polylactic acid.
6. The method for preparing a PLA nanocomposite according to claim 1, characterized in that said spinning step is in particular: adding the spinning solution into an electrostatic spinning machine, adjusting the spinning voltage to 5-20kv, the propelling speed of a liquid propeller to 0.1-0.2mm/s, the rotating speed of a receiving roller to 50-100r/min, and the receiving distance to 10-15cm.
7. The method for preparing a PLA nanocomposite according to claim 1, wherein the drying temperature is 60 to 80 ℃ and the drying time is 24 to 48 hours.
8. The method for preparing a PLA nanocomposite according to claim 1, wherein the padding temperature is 30-40 ℃, the impregnation time is 20-40min, and the rolling margin is 70-80%.
9. The method for preparing a PLA nanocomposite according to claim 8, wherein the drying temperature is 50-60 ℃ and the drying time is 10-30min.
10. A PLA nanocomposite material, characterized in that it is prepared by the preparation method according to any one of claims 1 to 9.
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