CN105664243B - A kind of three-dimensional rack and preparation method thereof of polylactic acid nano micron fibre structure - Google Patents

A kind of three-dimensional rack and preparation method thereof of polylactic acid nano micron fibre structure Download PDF

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Publication number
CN105664243B
CN105664243B CN201610106725.8A CN201610106725A CN105664243B CN 105664243 B CN105664243 B CN 105664243B CN 201610106725 A CN201610106725 A CN 201610106725A CN 105664243 B CN105664243 B CN 105664243B
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polylactic acid
micron
fibre structure
dimensional rack
acid nano
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CN105664243A (en
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汪学军
楼涛
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Qingdao University
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Qingdao University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14Macromolecular materials
    • A61L27/18Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326Condensation or reaction polymers
    • D04H1/435Polyesters
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Medicinal Chemistry (AREA)
  • Dermatology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials For Medical Uses (AREA)
  • Artificial Filaments (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

The present invention relates to a kind of three-dimensional racks and preparation method thereof of polylactic acid nano micron fibre structure, it is used distinguishes electrostatic spinning nano and micron chitin fiber film under certain condition, by nanometer and micron chitin fiber film, high speed shear divides the three-dimensional rack of available polylactic acid nano micron fibre structure after sample, freeze forming and freeze-drying at staple fiber in water according to a certain ratio.The preparation method simple process, the acid fiber by polylactic of different-diameter can be obtained using method of electrostatic spinning, the ratio and concentration of adjustable nanometer and micrometer fibers during freeze forming, the polylactic acid being prepared receive micron three-dimensional rack with good biocompatibility and mechanical property.

Description

A kind of three-dimensional rack and preparation method thereof of polylactic acid nano micron fibre structure
Technical field
The present invention relates to a kind of three-dimensional racks and preparation method thereof of polylactic acid nano micron fibre structure, belong to bio-medical Field of material technology.
Background technique
A kind of synthetic polymer timbering material that polylactic acid is ratified earliest as U.S. FDA, have it is nontoxic, with human body phase Capacitive is good, in vivo can degradable absorption the advantages that, be widely used in the tissues such as bone, cartilage, blood vessel and skin and device Official reparation (Lee EJ etc., Ann Biomed Eng, 2014;42 (2): 323).The microstructure of bracket has its comprehensive performance Large effect can enhance the absorption of protein research shows that nano fiber scaffold has biggish specific surface area and adsorption site, The adsorption site for increasing cell adherence, to can promote the reparation of tissue and organ.But simple nanofiber mechanical strength compared with It is low, it can not apply in the reparation of the more demanding tissue of mechanical strength and organ.In comparison, micrometer fibers bracket have compared with Good mechanical property, and degradation rate is slow, the structural stability being able to maintain that in stent implantation procedure.Therefore, in the bracket It there is nanometer and the microstructure of micrometer fibers then can overcome the contradiction between biocompatibility and mechanical property simultaneously.At present The method that polylactic acid mostly uses Thermal inactive during preparing three-dimensional rack, using tetrahydrofuran or dioxanes equal solvent Nanometer and micrometer fibers shape bracket can be respectively obtained, but the control of its fibre diameter is more difficult, while obtaining nanometer and micron Fiber is then more difficult (CN103159977A).It is thin that the method that researcher passes through electrostatic spinning at present also can get acid fiber by polylactic Film, but it is also very difficult for obtaining three-dimensional rack by method of electrostatic spinning.
Summary of the invention
Main imagination of the invention is to prepare nanometer and micron polylactic acid film respectively using the method for electrostatic spinning, by one Fixed proportion mixes nanometer and micron polylactic acid fiber membrane, and by polylactic acid film high speed shear at staple fiber, freeze-dried Obtain three-dimensional nano micron fibre polylactic acid bracket.
The preparation method of three wiener micron polylactic acid brackets is described in detail below in the present invention.
(1) electrostatic spinning nano polylactic acid fiber membrane, prepares the solution of polylactic acid 10.0%, and solvent is chloroform and dioxanes Mixture, volume ratio 70:30, spinning voltage is between 20~25kV.
(2) electrostatic spinning micron polylactic acid fiber membrane, prepares the solution of polylactic acid 20.0%, and solvent is chloroform and dioxanes Mixture, volume ratio 90:10, spinning voltage is between 12~15kV.
(3) quantitative nanometer and micron polylactic acid fiber membrane are weighed respectively, is added in quantitative water, in water high speed Cut into staple fiber.
(4) divide sample into weighing bottle, the freeze forming at -18 DEG C, available polylactic acid is received micro- after being lyophilized in freeze dryer The three-dimensional rack of rice fibre structure.
Polylactic acid molecule amount used above is between 5~100,000, the mass ratio of nanometer polylactic acid and micron polylactic acid Between 20:80 to 80:20, the total concentration of polylactic acid nano micrometer fibers in water is between 1~3%.
The three-dimensional rack of polylactic acid nano micron fibre structure produced by the present invention is white disk, and shape and height can be Divide in sample and uses different containers and sample volume is divided to adjust.The structure that nano micron fibre coexists assigns the good bio-compatible of bracket Property and mechanical strength.The preparation method simple process is also convenient to adjustment spinning condition in preparation and obtains receiving for different-diameter Rice and micron acid fiber by polylactic, compared to simple method of electrostatic spinning, which can easily prepare the bracket of three-dimensional structure.
Specific embodiment
Combined with specific embodiments below, the content of present invention is further described, but implementation of the invention is not It is confined to this.
Embodiment 1: taking the chloroform of 7ml and the dioxanes of 3ml respectively, is uniformly mixed, and weighs 1.0g polylactic acid, stirs molten Solution stands 12 hours.PLA solution is added in syringe, the voltage spinning of 20kV is passed to, collects the aluminium foil in ground connection On, it can get acid fiber by polylactic diameter in the film of 50-750nm.The chloroform of 9ml and the dioxanes of 1ml are taken respectively, and mixing is equal It is even, 2.0g polylactic acid is weighed, stirring and dissolving stands 12 hours.PLA solution is added in syringe, the electricity of 15kV is passed to Pressure spinning silk is collected on the aluminium foil of ground connection, can get film of the acid fiber by polylactic diameter at 1-10 μm.Weigh respectively 0.2g and 0.8g nanometers and micron polylactic acid fiber membrane, cut into staple fiber in 100ml water high speed, divide sample into weighing bottle, at -18 DEG C Lower freeze forming can get the three-dimensional rack of polylactic acid nano micron fibre structure after being lyophilized in freeze dryer.
Embodiment 2: taking the chloroform of 21ml and the dioxanes of 9ml respectively, is uniformly mixed, and weighs 3.0g polylactic acid, stirs molten Solution stands 12 hours.PLA solution is added in syringe, the voltage spinning of 25kV is passed to, collects the aluminium foil in ground connection On, it can get acid fiber by polylactic diameter in the film of 50-300nm.The chloroform of 9ml and the dioxanes of 1ml are taken respectively, and mixing is equal It is even, 2.0g polylactic acid is weighed, stirring and dissolving stands 12 hours.PLA solution is added in syringe, the electricity of 12kV is passed to Pressure spinning silk is collected on the aluminium foil of ground connection, can get film of the acid fiber by polylactic diameter at 1-10 μm.Weigh respectively 2.4g and 0.6g nanometers and micron polylactic acid fiber membrane, cut into staple fiber in 100ml water high speed, divide sample into weighing bottle, at -18 DEG C Lower freeze forming can get the three-dimensional rack of polylactic acid nano micron fibre structure after being lyophilized in freeze dryer.

Claims (5)

1. a kind of three-dimensional rack of polylactic acid nano micron fibre structure, it is characterised in that electrostatic spinning is received respectively under certain condition Rice and micron polylactic acid fiber membrane, according to a certain ratio by nanometer and micron polylactic acid fiber membrane in water high speed shear at short fibre Dimension, divides sample and the freeze forming at -18 DEG C, can get the three-dimensional branch of polylactic acid nano micron fibre structure after being lyophilized in freeze dryer Frame.
2. the three-dimensional rack of polylactic acid nano micron fibre structure according to claim 1, it is characterised in that used poly- Lactic acid molecules amount is between 5~100,000.
3. the three-dimensional rack of polylactic acid nano micron fibre structure according to claim 1, it is characterised in that electrostatic spinning is received When rice tunica fibrosa, PLA concentration 10.0%, solvent is the mixture of chloroform and dioxanes, volume ratio 70:30, spinning electricity It is pressed between 20~25kV.
4. the three-dimensional rack of polylactic acid nano micron fibre structure according to claim 1, it is characterised in that electrostatic spinning is micro- When rice polylactic acid fiber membrane, PLA concentration 20.0%, mixture of the solvent for chloroform and dioxanes, volume ratio 90:10, Spinning voltage is between 12~15kV.
5. the three-dimensional rack of polylactic acid nano micron fibre structure according to claim 1, it is characterised in that nanometer polylactic acid And the mass ratio of micron polylactic acid is between 20:80 to 80:20, the total concentration of polylactic acid nano micrometer fibers in water 1~ Between 3%.
CN201610106725.8A 2016-02-27 2016-02-27 A kind of three-dimensional rack and preparation method thereof of polylactic acid nano micron fibre structure Expired - Fee Related CN105664243B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103285424A (en) * 2013-05-27 2013-09-11 东华大学 Three-dimensional fiber-based aerogel tissue engineering scaffold and preparation method thereof
CN104888278A (en) * 2015-05-20 2015-09-09 东华大学 Nanometer/micrometer fiber three-dimensional porous structure support material and preparation and application of support material
CN105107022A (en) * 2015-09-21 2015-12-02 东华大学 Preparation method for nanofiber porous scaffold having compression elasticity in wet state

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2967833A4 (en) * 2013-03-14 2016-11-09 Lifenet Health Aligned fiber and method of use thereof
CN103691005B (en) * 2013-12-24 2015-10-28 华东交通大学 A kind of micro--Na fibrous tissue engineering rack and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103285424A (en) * 2013-05-27 2013-09-11 东华大学 Three-dimensional fiber-based aerogel tissue engineering scaffold and preparation method thereof
CN104888278A (en) * 2015-05-20 2015-09-09 东华大学 Nanometer/micrometer fiber three-dimensional porous structure support material and preparation and application of support material
CN105107022A (en) * 2015-09-21 2015-12-02 东华大学 Preparation method for nanofiber porous scaffold having compression elasticity in wet state

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