CN105887335A - Biomedical electrostatic spinning membrane based on medical high-polymer materials - Google Patents

Biomedical electrostatic spinning membrane based on medical high-polymer materials Download PDF

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Publication number
CN105887335A
CN105887335A CN201610336210.7A CN201610336210A CN105887335A CN 105887335 A CN105887335 A CN 105887335A CN 201610336210 A CN201610336210 A CN 201610336210A CN 105887335 A CN105887335 A CN 105887335A
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parts
electrostatic spinning
spinning membrane
biomedical
membrane
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不公告发明人
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Cai Liufeng
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Cai Liufeng
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING 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
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-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
    • D04H1/42—Non-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
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING 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
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005—Synthetic yarns or filaments
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING 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
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-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
    • D04H1/72—Non-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
    • D04H1/728—Non-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
    • 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
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/04—Macromolecular materials
    • A61L31/042—Polysaccharides
    • 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
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/04—Macromolecular materials
    • A61L31/06—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • 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
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING 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
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • D04H3/03—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2509/00—Medical; Hygiene
    • D10B2509/02—Bandages, dressings or absorbent pads
    • D10B2509/022—Wound dressings

Abstract

The invention provides a biomedical electrostatic spinning membrane based on medical high-polymer materials. The biomedical electrostatic spinning membrane comprises polylactic acid-glycolic acid copolymers, poly butylene succinate, polyurethane, chitosan, p-chloro-o-nitroaniline, diethyl phosphite, glutaraldehyde, vinyl trimethoxy silane, propyl methacrylate, dibutyltin dilaurate and N, N-dimethyl formamide. A method for preparing the biomedical electrostatic spinning membrane includes adding various components into a mixing stirrer and uniformly stirring and mixing the components with one another to obtain mixed materials; adding the obtained mixed materials into a reaction kettle and carrying out heating stirring reaction on the mixed materials in nitrogen atmosphere to obtain spinning liquid; delivering the obtained spinning liquid into an electrostatic spinning device and preparing an electrostatic spinning membrane from the spinning liquid; drying the electrostatic spinning membrane at the constant temperature under the vacuum condition and then carrying out radiation sterilization on the electrostatic spinning membrane by the aid of Co<60> to obtain the biomedical electrostatic spinning membrane. The biomedical electrostatic spinning membrane has the advantages that the electrostatic spinning membrane in a dry state and a wet state is high in mechanical strength and is good in flexibility, and accordingly requirements on the mechanical performance of the biomedical electrostatic spinning membrane can be completely met during surgery operation and after the biomedical electrostatic spinning membrane is implanted in a patient.

Description

Bio-medical static spinning membranes based on medical macromolecular materials
Technical field
The invention belongs to medical macromolecular materials technical field, be specifically related to a kind of bio-medical static spinning membrane and system thereof Preparation Method.
Background technology
Fiber typically refers to any plant, animal, regeneration, synthesis or the chopped fiber of mineral and long filament.Typically The draw ratio continuous print silk more than 1000 is become fiber.Fiber typically has flexibility, and the material of composition fiber all has necessarily Elastic recovery.Conventional fibre can be divided into natural fiber and staple fibre.The diameter of conventional fibrous materials mostly is 5～50 μm Scope, in the fiber being usually used in weaving, silkworm silk is the thinnest, a diameter of 4～5 μm, the superfine Denier fibre diameter of recent development Up to 0.4～4 μm.
Nanofiber refers to the fiber that diameter is in nanometer range (1～100nm), it is also possible to by the nanometer of different dimensions The fiber of fiber composite conventional method molding is also considered as nanofiber.When diameter narrows down to from micron (such as 10～100 μm) When submicron or nanometer, polymer fiber, compared with corresponding material, shows multiple surprising characteristic, such as the biggest ratio table (its specific surface area is the 10 of micrometer fibers to area3Times), flexible and superpower mechanical behavior (such as: hardness and tensile strength), The characteristic of these excellences makes nanofiber have many important purposes.
Bio-medical field, modal membrane material is trauma dressing, filters barrier material and drug release material.Skin It is the natural cover for defense of human body, stablizes maintaining organismic internal environment and stop the invasion of microorganism to play an important role.Lose skin The barrier action of skin, body can produce the pathophysiological change of series of complex, loses including water and rock-soil coupling and soda acid Weighing apparatus, infection and septicemia etc., in some instances it may even be possible to threat to life.Exposed wound surface needs to cover with dressing to be protected by, to provide Be conducive to wound healing, promote the environment of tissue repair, and wound healing is the important prerequisite of body function rehabilitation after wound, Therefore, wound dressing becomes the study hotspot of biomedical materials field.
Nano biological medical films can show and differ markedly from some characteristics of traditional dressing " by materials processing to nanometer chi Very little, occur as soon as such as small-size effect, quantum effect, skin effect etc. and be different from the specific performance of conventional material.Such as: pass Silver-colored and the some other oxide material of system has certain sterilizing ability, and after being prepared as the granule of nanometer scale, sterilization is lived Property will significantly improve.Clinical application indicate that, nano-silver biological medical films is to staphylococcus aureus, escherichia coli, green pus bar Bacterium, bud robe bacillus etc. are respectively provided with antibacterial or bactericidal action, and also have the strongest bactericidal action to fungus, and have no office in applying Portion stimulates and allergic symptom, toxic reaction not yet occurs.The aperture of electrospun fibers film is generally between 500nm to 1 μm, sufficient To stop the intrusion of antibacterial, specific surface area is 5～100m2/ g, the absorption for wound exudate is highly effective, can control simultaneously Water volatilizees, and has oxygen permeability, improves liquid flow capacity, the feature grown of control microorganism.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art to provide a kind of bio-medical static spinning membrane and preparation thereof Method, this electrospinning film is respectively provided with higher mechanical strength under dry state and hygrometric state, and has preferable pliability, the most permissible To the requirement in terms of its mechanical property after meeting operative process and implanting.
A kind of bio-medical static spinning membrane, raw material includes in parts by weight: Poly(D,L-lactide-co-glycolide 2～9 Part, poly butylene succinate 1～7 parts, polyurethane 2～10 parts, chitosan 3～12 parts, p-chloro-o-nitroaniline 1～9 parts, sub- Diethyl phosphate 3～9 parts, glutaraldehyde 4～10 parts, vinyltrimethoxy silane 2～7 parts, propyl methacrylate 1～6 parts, Dibutyl tin dilaurate 3～10 parts, DMF 2～9 parts.
As the further improvement of foregoing invention, described bio-medical static spinning membrane, raw material includes in parts by weight: poly- Poly lactic coglycolic acid 3～7 parts, poly butylene succinate 2～6 parts, polyurethane 4～9 parts, chitosan 5～10 parts, P-chloro-o-nitroaniline 4～8 parts, diethyl phosphite 5～8 parts, glutaraldehyde 6～9 parts, vinyltrimethoxy silane 3～6 Part, propyl methacrylate 2～5 parts, dibutyl tin dilaurate 5～9 parts, DMF 4～7 parts.
As the further improvement of foregoing invention, described bio-medical static spinning membrane, raw material includes in parts by weight: poly- Poly lactic coglycolic acid 5 parts, poly butylene succinate 3 parts, polyurethane 7 parts, chitosan 8 parts, p-chloro-o-nitroaniline 6 parts, diethyl phosphite 6 parts, glutaraldehyde 7 parts, vinyltrimethoxy silane 5 parts, propyl methacrylate 3 parts, dibutyl 8 parts of tin dilaurate stannum, DMF 5 parts.
The preparation method of above-mentioned bio-medical static spinning membrane, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65～80 DEG C in nitrogen atmosphere, and stirring is anti- Answer 30～40min, obtain spinning liquid；
Step 3, sends step 2 gained spinning liquid into electrostatic spinning apparatus, and prepared thickness is the electrospinning film of 100 μm～2mm；
Step 4, by dried, through Co for step 3 gained electrospinning film constant-temperature vacuum under the conditions of 20～45 DEG C60Radiation sterilization, i.e. ?.
As the further improvement of foregoing invention, the mixing speed being uniformly mixed in step 1 is 300～400rpm, Mixing time is 20～40min.
As the further improvement of foregoing invention, in step 3, electrospinning conditions is: just spinning voltage is 10～15kV, continuous Spinning voltage increases by 0.5～2.0kV accordingly and is adjusted by often consuming 1 milliliter of electrospinning liquid consumption, and receiving range is 5～50cm, goes out Liquid speed is 5～25mL/h, and receptor is the surface rotating metallic disk with tinfoil of diameter 10～300cm, disc rotation speed It is 10～1000rpm.
As the further improvement of foregoing invention, the time that is vacuum dried in step 4 is 24～72h.
The bio-medical static spinning membrane of the present invention, on the one hand, be respectively provided with higher mechanical strength under dry state and hygrometric state, And there is preferable pliability, to the requirement in terms of its mechanical property after operative process can being met completely and implanting； On the other hand, the fibre diameter that the electrostatic spinning process used prepares is in nanometer to submicron order and smooth surface, greatly Little homogeneous electrospinning fibre, obtained electrospinning film any surface finish is smooth and thickness is homogeneous.
Detailed description of the invention
Embodiment 1
A kind of bio-medical static spinning membrane, raw material includes in parts by weight: Poly(D,L-lactide-co-glycolide 2 parts, polybutadiene Acid butanediol ester 1 part, polyurethane 2 parts, chitosan 3 parts, p-chloro-o-nitroaniline 1 part, diethyl phosphite 3 parts, glutaraldehyde 4 Part, vinyltrimethoxy silane 2 parts, propyl methacrylate 1 part, dibutyl tin dilaurate 3 parts, N, N-dimethyl formyl Amine 2 parts.
The preparation method of above-mentioned bio-medical static spinning membrane, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 300rpm, and mixing time is 40min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65 DEG C in nitrogen atmosphere, stirring reaction 40min, obtains spinning liquid；
Step 3, sends step 2 gained spinning liquid into electrostatic spinning apparatus, and electrospinning conditions is: just spinning voltage is 10kV, continuous Spinning voltage increases 0.5kV accordingly and is adjusted by often consuming 1 milliliter of electrospinning liquid consumption, and receiving range is 5cm, goes out liquid speed and is 5mL/h, receptor is the surface rotating metallic disk with tinfoil of diameter 10cm, and disc rotation speed is 10rpm, and prepared thickness is The electrospinning film of 100 μm；
Step 4, by step 3 gained electrospinning film after under the conditions of 20 DEG C, constant-temperature vacuum is dried 72h, through Co60Radiation sterilization, to obtain final product.
Embodiment 2
A kind of bio-medical static spinning membrane, raw material includes in parts by weight: Poly(D,L-lactide-co-glycolide 3 parts, polybutadiene Acid butanediol ester 2 parts, polyurethane 4 parts, chitosan 5 parts, p-chloro-o-nitroaniline 4 parts, diethyl phosphite 5 parts, glutaraldehyde 6 Part, vinyltrimethoxy silane 3 parts, propyl methacrylate 2 parts, dibutyl tin dilaurate 5 parts, N, N-dimethyl formyl Amine 4 parts.
The preparation method of above-mentioned bio-medical static spinning membrane, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 350rpm, and mixing time is 30min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 70 DEG C in nitrogen atmosphere, stirring reaction 35min, obtains spinning liquid；
Step 3, sends step 2 gained spinning liquid into electrostatic spinning apparatus, and electrospinning conditions is: just spinning voltage is 12kV, continuous Spinning voltage increases 1.2kV accordingly and is adjusted by often consuming 1 milliliter of electrospinning liquid consumption, and receiving range is 30cm, goes out liquid speed and is 15mL/h, receptor is the surface rotating metallic disk with tinfoil of diameter 80cm, and disc rotation speed is 200rpm, prepares thickness Electrospinning film for 1.2mm；
Step 4, by step 3 gained electrospinning film after under the conditions of 45 DEG C, constant-temperature vacuum is dried 24h, through Co60Radiation sterilization, to obtain final product.
Embodiment 3
A kind of bio-medical static spinning membrane, raw material includes in parts by weight: Poly(D,L-lactide-co-glycolide 5 parts, polybutadiene Acid butanediol ester 3 parts, polyurethane 7 parts, chitosan 8 parts, p-chloro-o-nitroaniline 6 parts, diethyl phosphite 6 parts, glutaraldehyde 7 Part, vinyltrimethoxy silane 5 parts, propyl methacrylate 3 parts, dibutyl tin dilaurate 8 parts, N, N-dimethyl formyl Amine 5 parts.
The preparation method of above-mentioned bio-medical static spinning membrane, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 400rpm, and mixing time is 20min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 80 DEG C in nitrogen atmosphere, stirring reaction 30min, obtains spinning liquid；
Step 3, sends step 2 gained spinning liquid into electrostatic spinning apparatus, and electrospinning conditions is: just spinning voltage is 15kV, continuous Spinning voltage increases 2kV accordingly and is adjusted by often consuming 1 milliliter of electrospinning liquid consumption, and receiving range is 50cm, goes out liquid speed and is 25mL/h, receptor is the surface rotating metallic disk with tinfoil of diameter 300cm, and disc rotation speed is 1000rpm, prepares thickness Degree is the electrospinning film of 2mm；
Step 4, by step 3 gained electrospinning film after under the conditions of 35 DEG C, constant-temperature vacuum is dried 48h, through Co60Radiation sterilization, to obtain final product.
Embodiment 4
A kind of bio-medical static spinning membrane, raw material includes in parts by weight: Poly(D,L-lactide-co-glycolide 7 parts, polybutadiene Acid butanediol ester 6 parts, polyurethane 9 parts, chitosan 10 parts, p-chloro-o-nitroaniline 8 parts, diethyl phosphite 8 parts, glutaraldehyde 9 Part, vinyltrimethoxy silane 6 parts, propyl methacrylate 5 parts, dibutyl tin dilaurate 9 parts, N, N-dimethyl formyl Amine 7 parts.
The preparation method of above-mentioned bio-medical static spinning membrane, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 300rpm, and mixing time is 40min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65 DEG C in nitrogen atmosphere, stirring reaction 40min, obtains spinning liquid；
Step 3, sends step 2 gained spinning liquid into electrostatic spinning apparatus, and electrospinning conditions is: just spinning voltage is 10kV, continuous Spinning voltage increases 1.8kV accordingly and is adjusted by often consuming 1 milliliter of electrospinning liquid consumption, and receiving range is 35cm, goes out liquid speed and is 20mL/h, receptor is the surface rotating metallic disk with tinfoil of diameter 240cm, and disc rotation speed is 600rpm, prepares thickness Degree is the electrospinning film of 1.5mm；
Step 4, by step 3 gained electrospinning film after under the conditions of 35 DEG C, constant-temperature vacuum is dried 36h, through Co60Radiation sterilization, to obtain final product.
Embodiment 5
A kind of bio-medical static spinning membrane, raw material includes in parts by weight: Poly(D,L-lactide-co-glycolide 9 parts, polybutadiene Acid butanediol ester 7 parts, polyurethane 10 parts, chitosan 12 parts, p-chloro-o-nitroaniline 9 parts, diethyl phosphite 9 parts, glutaraldehyde 10 parts, vinyltrimethoxy silane 7 parts, propyl methacrylate 6 parts, dibutyl tin dilaurate 10 parts, N, N-dimethyl Methanamide 9 parts.
The preparation method of above-mentioned bio-medical static spinning membrane, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, and mixing speed is 300rpm, and mixing time is 40min, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65 DEG C in nitrogen atmosphere, stirring reaction 40min, obtains spinning liquid；
Step 3, sends step 2 gained spinning liquid into electrostatic spinning apparatus, and electrospinning conditions is: just spinning voltage is 10kV, continuous Spinning voltage increases 1.0kV accordingly and is adjusted by often consuming 1 milliliter of electrospinning liquid consumption, and receiving range is 40cm, goes out liquid speed and is 10mL/h, receptor is the surface rotating metallic disk with tinfoil of diameter 100cm, and disc rotation speed is 800rpm, prepares thickness Degree is the electrospinning film of 500 μm；
Step 4, by step 3 gained electrospinning film after under the conditions of 20 DEG C, constant-temperature vacuum is dried 72h, through Co60Radiation sterilization, i.e. ?.
Test example 1
With reference to GB/T16886.5-2003, use the standard Hela cell line lixiviating solution to embodiment 1 to 5 gained static spinning membrane Carry out vitro cytotoxicity test experience.The preliminary experiment first passing through inoculum density gradient plate determines absorbance and cell proliferation The inoculum density that linear relationship is best, result shows when inoculum density is every hole 3000～4000Hela cell, cell proliferation Good and after inoculating 3 days cell have no obvious contact inhibition.
Prepare the lixiviating solution of 100%, 50%, 10% and 5% 4 kind of variable concentrations respectively, with detect cytotoxicity whether with Electrospinning film leachable is relevant.It is provided with negative control group (cell maintenance medium+groups of cells), positive controls (0.64% benzene simultaneously Phenol solution+groups of cells) and blank group (zeroing group), often organize and all have 6 multiple holes as parallel control.Each group of orifice plate is placed in Constant temperature 37 DEG C and 5%CO2Take out after cultivating 2 days in the incubator of concentration, add after MTT processes and observe under inverted microscope, knot The hole inner cell form of fruit display variable concentrations lixiviating solution group does not presents obvious difference.Each group is calculated by the OD value recorded Cell is relative to the rate of increase (RGR).Result shows, this experiment positive controls RGR value is 0, has obvious cytotoxicity, i.e. 0.64% phenol solution cytotoxicity is 5 grades；Embodiment 1 to 5 gained electrospinning film RGR value between 96～114%, cell toxicant Property is 0 grade or 1 grade, i.e. no cytotoxicity.
Test example 2
Surgical scissors after being sterilized by embodiment 1 gained electrospinning film is cut into the sample of a diameter of 7mm, by the soak with ethanol of 75% Flush three times with the PBS of pH7.4 again after 1h.Take the healthy SD rat 18 of body weight 180～200 grams, with 3% penta bar ratios Appropriate sodium carries out intraperitoneal anesthesia by 50mg/Kg concentration, and with iodophor disinfection after the shaving of back, then incision skin is to deep fascia, to two Side separation subcutaneous tissue, implants electrospinning film, is fixed in muscle layer with 3-0 stitching thread, then by skin closure, uses aseptic dressing Cover wrapping and periodically change dressings.The postoperative single cage of experimental mouse is raised, and optional 3 SD rats were cut in postoperative 1 week, 4 weeks and 13 weeks Skin takes out implants sample.
The sample taken out in rat body in different time points is first placed in the neutral formalin solution of 4% and fixes 24h, then Sucrose solution with 30% soaks 12h dehydration, then embeds with embedding medium and puts in liquid nitrogen cold under the conditions of-80 DEG C after quick-freezing Freeze 10h, use freezing microtome to prepare the frozen section that thickness is 7 μm afterwards, finally use Hematoxylin-eosin staining to cutting Sheet carries out dyeing and observing under an optical microscope.Result shows, embodiment 1 gained electrospinning film implant in SD rat body 1 week, 4 Week and 13 Zhou Houjun serve the effect that preferable shielding fiber tissue is grown into, and SD rat during whole in vivo test Obvious inflammatory reaction does not occur.

Claims (1)

1. a bio-medical static spinning membrane, it is characterised in that: raw material includes in parts by weight: poly lactic-co-glycolic acid is common Polymers 5 parts, poly butylene succinate 3 parts, polyurethane 7 parts, chitosan 8 parts, p-chloro-o-nitroaniline 6 parts, phosphorous acid diethyl Ester 6 parts, glutaraldehyde 7 parts, vinyltrimethoxy silane 5 parts, propyl methacrylate 3 parts, dibutyl tin dilaurate 8 parts, DMF 5 parts；
The preparation method of described bio-medical static spinning membrane, comprises the following steps:
Step 1, adds to, in mixing and blending machine, be uniformly mixed by each component, obtains mixed material；
Step 2, joins in reactor by step 1 gained mixed material, is heated to 65～80 DEG C in nitrogen atmosphere, and stirring is anti- Answer 30～40min, obtain spinning liquid；
Step 3, sends step 2 gained spinning liquid into electrostatic spinning apparatus, and prepared thickness is the electrospinning film of 100 μm～2mm；
Step 4, by dried, through Co for step 3 gained electrospinning film constant-temperature vacuum under the conditions of 20～45 DEG C60Radiation sterilization, to obtain final product.
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