CN107496992A - A kind of three dimensional patterned Fe3O4/ medical macromolecular materials composite nano fiber and preparation method thereof - Google Patents
A kind of three dimensional patterned Fe3O4/ medical macromolecular materials composite nano fiber and preparation method thereof Download PDFInfo
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- CN107496992A CN107496992A CN201710766396.4A CN201710766396A CN107496992A CN 107496992 A CN107496992 A CN 107496992A CN 201710766396 A CN201710766396 A CN 201710766396A CN 107496992 A CN107496992 A CN 107496992A
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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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified 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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
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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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/18—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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
-
- 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
-
- 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
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
Abstract
The invention discloses a kind of three dimensional patterned Fe3O4/ medical macromolecular materials composite nano fiber and preparation method thereof.This method is by Fe3O4Nano particle mixes with solvent supersonic, adds medical macromolecular materials, obtains electrospinning liquid；Start electrospinning using electrospinning liquid, obtain composite nano fiber；Separate, dry with reception device again, be sub-partitioned into small pieces, then tweezer small pieces and soak, put to bottom and be prefixed in the culture dish of rubidium Fe-B permanent magnet；Panel stack obtains three dimensional patterned Fe in culture dish obtained by continuous tweezer3O4/ medical macromolecular materials composite nano fiber.The three dimensional patterned composite nano fiber of the present invention will not only destroy the original microcosmic biomimetic features of Electrospun nano-fibers, the two dimensional surface for breaking electrostatic spinning technique applied to tissue engineering bracket limits, a kind of contactless efficient bionic three-dimensional construction method is provided, and the cavernous structure after patterning is advantageous to cell adhesion, propagation etc..
Description
Technical field
The present invention relates to the three-dimensional manometer fiber art of multistage composite insertion pore structure, and in particular to a kind of three-D pattern
Change Fe3O4/ medical macromolecular materials composite nano fiber and preparation method thereof.
Background technology
In recent years, the continuous development of organizational project provides sound assurance for the health of the mankind, wherein, timbering material is made
To condense the road that the most ring of the wisdom of humanity experienced many decades and move towards bionical structure in organizational project.A variety of
In the technology for preparing timbering material, electrostatic spinning technique can prepare the nanofiber of microstructure bionic extracellular matrix because of it
And it is widely used in field of tissue engineering technology.But because electrostatic spinning technique is difficult to construct three-dimensional manometer undulation degree
Expect and its application is restricted again.
Three-dimensional manometer fibrous material can not be obtained by simply increasing the sample preparation time, can only cause the hole of sample
Gap rate declines, and over time, receiver is caused electric conductivity to decline and then receiving efficiency is declined most by fiber covering
Spinning is caused to fail eventually.Following four can be substantially divided into by preparing the method for three-dimensional structure by electrostatic spinning technique at present.（1）
Continuous electro-spinning or multilayer electrospinning.Thin layer fiber is prepared by the way of similar two dimensional surface electrospinning, is then entered by parameter regulation
Row continuous electro-spinning.Make that the three-dimensional porous structure that thickness is hundreds of microns can be prepared in this way.（2）By to preparation
Fibrous material is post-processed, such as is folded, crimps or be layering, and constructs three-dimensional structure.（3）There is three-dimensional by design
The receiver of structure replaces the planar receiver of two dimension to prepare nanofiber to obtain three-dimensional structure as template.（4）It is logical
Cross the parameter for changing electrostatic spinning（Such as electric-field intensity, solution concentration and relative humidity）Come realize the rapid accumulation of silk fiber or
Assemble to obtain three-dimensional structure.
But under may be because operation difficulty greatly using these methods one side and then causing efficiency relatively low；The opposing party
Face, processing procedure can destroy the bionical characteristic of the original microstructure of Electrospun nano-fibers to a certain extent, and can not shape
Into macroscopic view-microcosmic multistage composite insertion pore structure, so as to which required three-dimensional microenvironment can not be provided for cell.Therefore, how
The three-dimensional manometer fiber that multistage composite insertion pore structure is effectively prepared using electrospinning is current urgent problem to be solved.
The content of the invention
It is an object of the invention to overcome the shortcomings of that fast and effective three-dimensional manometer fiber can not be built by electrospinning now, carry
For a kind of three dimensional patterned Fe3O4/ medical macromolecular materials composite nano fiber and preparation method thereof, this method are based on Static Spinning
Silk technology, it is efficiently quick in the case where not introducing other complex technologys and post processing to prepare tool multistage composite insertion pore structure
Three-dimensional rack, i.e. electrospinning composite magnetic nanofiber, under magnetic fields, fast pattern and three-dimensional structure.
The purpose of the present invention is achieved through the following technical solutions.
A kind of three dimensional patterned Fe3O4The preparation method of/medical macromolecular materials composite nano fiber, comprises the following steps：
（1）By Fe3O4Nano particle and solvent supersonic mixing, obtain finely dispersed Fe3O4Suspension；
（2）To step（1）Gained Fe3O4Medical macromolecular materials are added in suspension, is well mixed, obtains electrospinning liquid；
（3）Using Stainless steel mesh as reception device, step is used（2）In electrospinning liquid start electrospinning, patterned
Fe3O4/ medical macromolecular materials composite nano fiber；
（4）By step（3）The Fe of middle gained patterning3O4/ medical macromolecular materials composite nano fiber separates with reception device,
Dry, be sub-partitioned into composite nano fiber small pieces, then tweezer composite nano fiber small pieces and soak, put to bottom and be prefixed rubidium
In the culture dish of Fe-B permanent magnet；
（5）Composite nano fiber panel stack is in step obtained by continuous tweezer（4）In culture dish in, obtain with multistage composite
Penetrate the three dimensional patterned Fe of pore structure3O4/ medical macromolecular materials composite nano fiber.
Preferably, step（1）The solvent is dichloromethane and N,N-dimethylformamide.
Preferably, step（1）The ultrasonic number is each 30min twice, and is replaced and surpassed with cold water in ultrasonic procedure
The water being heated in sound pond.
Preferably, step（2）The high polymer material is polycaprolactone（PCT）Deng medical macromolecular materials.
Preferably, step（3）The condition of the electrospinning is：Delivery rate is 1 ml/h, and rotating shaft rotating speed is 120 ± 10
R/min, it is 13 ± 2 cm to receive height, and working bin temperature is 43 ± 2 DEG C, and relative humidity is 40 ± 5%.
Preferably, step（5）Middle stacking composite nano fiber small pieces need to adjust upper and lower two layers of relative position to ensure net
Lattice are corresponding.
It is a kind of with the three dimensional patterned of multistage composite insertion pore structure as made from above-described preparation method
Fe3O4/ medical macromolecular materials composite nano fiber.
The present invention is based on electrostatic spinning technique, first, using Stainless steel mesh as template reception device, prepares doping rapidly
Be magnetic the composite nano fiber grid material of ferric oxide nanometer particle.Cell is inoculated in after material surface in external magnetic field afterwards
In the presence of add up layer by layer rapid structure three-dimensional structure, remove magnetic field again after in vitro culture certain time and formed with extracellular base
Matter is bonded as overall three-dimensional cell-composite body.
Compared with the prior art, the invention has the advantages that：
The present invention first uses Stainless steel mesh to carry out patterned process to magnetic composite nano fiber as reception device, can be rapid
Obtain the composite nano fiber with center through hole structure；Stacking processing is carried out to the composite nano fiber after patterning afterwards, can
Rapid build goes out to have the three-dimensional Fe of macroscopic view-microcosmic compound insertion pore structure3O4/ medical macromolecular materials composite Nano is fine
Dimension.It is easy to operate the present invention is to provide efficiently contactless three-dimensional structure, and Electrospun nano-fibers original will not be destroyed
Some bionical characteristics of microstructure.In addition, the multistage composite insertion pore structure of this composite nano fiber is more beneficial for tissue
Various seed cells the cell behavior such as sticks, breeds in engineering.
Brief description of the drawings
Fig. 1 a, Fig. 1 b are the Fe of the gained patterning of embodiment 13O4/ medical macromolecular materials composite nano fiber microscopic appearance
Electron microscope；
Fig. 2 a, Fig. 2 b are the Fe of the gained patterning of embodiment 23O4/ medical macromolecular materials composite nano fiber microscopic appearance
Electron microscope；
Fig. 3 is the three dimensional patterned Fe of the gained of embodiment 23O4The macrograph of/medical macromolecular materials composite nano fiber；
Fig. 4 a, Fig. 4 b are the three dimensional patterned Fe of the gained of embodiment 23O4The electron microscope of/medical macromolecular materials composite nano fiber.
Fig. 5 is the three dimensional patterned Fe of the gained of embodiment 1,23O4The Proliferation data of/medical macromolecular materials composite nano fiber
Figure.
Fig. 6 a are that medical macromolecular materials polycaprolactone nanofibers sticks electron microscope.
Fig. 6 b are the three dimensional patterned Fe of the gained of embodiment 13O4/ medical macromolecular materials composite nano fiber sticks Electronic Speculum
Figure.
Fig. 6 c are the three dimensional patterned Fe of the gained of embodiment 23O4/ medical macromolecular materials composite nano fiber sticks Electronic Speculum
Figure.
Embodiment
It is further described below in conjunction with example and specific implementation of the accompanying drawing to the present invention, but embodiments of the present invention
Not limited to this.
Embodiment 1
Weigh 0.42g Fe3O4Nano particle is placed in cillin bottle, is 1 according to volume ratio：1 ratio measures 3ml dichloros respectively
Methane and 3ml DMFs are transferred in supersonic wave cleaning machine after adding in cillin bottle and carry out ultrasonic disperse twice,
, the water being heated in supersonic cleaning machine is replaced with cold water in ultrasonic procedure 30 min/ time.0.84g polycaprolactones are then weighed to add
Enter in foregoing cillin bottle and be quickly transferred at a high speed（1500 rpms）Vibration is carried out on concussion blending instrument to mix 24 hours,
Obtain Fe3O4/ medical macromolecular materials electrospinning liquid.Will be stainless as the 304 of receiver using handheld small-sized electric cutting machine
Steel lattice cut into 25cm × 8cm grid and is cleaned by ultrasonic using supersonic cleaning machine, it is standby to dry；Start electricity in following condition
Spin：Delivery rate is 1 ml/h, and rotating shaft rotating speed is 120 r/min, and it is highly 13 cm to receive, 43 ± 2 DEG C of working bin temperature,
% ± 5 of relative humidity 40, the Fe patterned3O4/ medical macromolecular materials composite nano fiber, as shown in Figure 1 a, 1 b,
Fe3O4It is evenly dispersed in polycaprolactone fiber.
By the Fe of the patterning of preparation3O4/ medical macromolecular materials composite nano fiber separates with receiver to be dried, then
It is divided into 1cm × 1cm small pieces.The nanofiber small pieces soaked using tweezers tweezer are placed in bottom and are prefixed rubidium Fe-B permanent magnet
Culture dish in, continuous tweezer magnetic fibre small pieces simultaneously adjust up and down that two layers of relative position is to ensure that grid is corresponding, and then quickly
Construct the three dimensional patterned Fe with macroscopic view-microcosmic compound insertion pore structure3O4/ medical macromolecular materials composite Nano is fine
Dimension.The multistage composite insertion pore structure of this composite nano fiber is more beneficial for the glutinous of various seed cells in organizational project
The cell behaviors such as attached, propagation.
Embodiment 2
Weigh 0.63g Fe3O4Nano particle is placed in cillin bottle, is 1 according to volume ratio：1 ratio measures 3ml dichloros respectively
Methane and 3ml DMFs are transferred in supersonic wave cleaning machine after adding in cillin bottle and carry out ultrasonic disperse twice,
, the water being heated in supersonic cleaning machine is replaced with cold water in ultrasonic procedure 30 min/ time.0.84g polycaprolactones are then weighed to add
Enter in foregoing cillin bottle and be quickly transferred at a high speed（1500 rpms）Vibration is carried out on concussion blending instrument to mix 24 hours,
Obtain Fe3O4/ medical macromolecular materials electrospinning liquid.Will be stainless as the 304 of receiver using handheld small-sized electric cutting machine
Steel lattice cut into 25cm × 8cm grid and is cleaned by ultrasonic using supersonic cleaning machine, it is standby to dry；Start electricity in following condition
Spin：Delivery rate is 1 ml/h, and rotating shaft rotating speed is 130 r/min, and it is highly 15 cm to receive, 43 ± 2 DEG C of working bin temperature,
% ± 5 of relative humidity 40, the Fe patterned3O4/ medical macromolecular materials composite nano fiber, as shown in Fig. 2 a, Fig. 2 b,
Fe3O4Be evenly dispersed in polycaprolactone fiber, fiber surface is slightly coarse, from Fig. 4 a, Fig. 4 b it can be seen that material have it is bright
Aobvious fenestral fabric, and mesh-portion silk fiber is sparse, and this has directly to build 3 D stereo insertion hole after superposition
Effect.
By the Fe of the patterning of preparation3O4/ medical macromolecular materials composite nano fiber separates with receiver to be dried, then
It is divided into 1cm × 1cm small pieces.The nanofiber small pieces soaked using tweezers tweezer are placed in bottom and are prefixed rubidium Fe-B permanent magnet
Culture dish in, continuous tweezer magnetic fibre small pieces simultaneously adjust up and down that two layers of relative position is to ensure that grid is corresponding, and then quickly
Construct the three dimensional patterned Fe with macroscopic view-microcosmic compound insertion pore structure3O4/ medical macromolecular materials composite Nano is fine
Dimension, as shown in figure 3, hole is uniformly mutually communicated.The multistage composite insertion pore structure of this composite nano fiber is more favourable
Various seed cells such as stick, bred at the cell behavior in organizational project, as Fig. 5, Fig. 6 a, Fig. 6 b, Fig. 6 c can be seen that magnetic
The addition of property ferric oxide nano particles enhances material surface biocompatibility, makes sprawling for its cell preferably.
Claims (7)
- A kind of 1. three dimensional patterned Fe3O4The preparation method of/medical macromolecular materials composite nano fiber, it is characterised in that including Following steps：（1）By Fe3O4Nano particle mixes with solvent supersonic, obtains finely dispersed Fe3O4Suspension；（2）To step（1）Gained Fe3O4Medical macromolecular materials are added in suspension, is well mixed, obtains electrospinning liquid；（3）Using Stainless steel mesh as reception device, step is used（2）In electrospinning liquid start electrospinning, patterned Fe3O4/ medical macromolecular materials composite nano fiber；（4）By step（3）The Fe of middle gained patterning3O4/ medical macromolecular materials composite nano fiber separates with reception device, Dry, be sub-partitioned into composite nano fiber small pieces, then tweezer composite nano fiber small pieces and soak, put to bottom and be prefixed rubidium In the culture dish of Fe-B permanent magnet；（5）Composite nano fiber panel stack is in step obtained by continuous tweezer（4）In culture dish in, obtain with multistage composite Penetrate the three dimensional patterned Fe of pore structure3O4/ medical macromolecular materials composite nano fiber.
- 2. preparation method according to claim 1, it is characterised in that：Step（1）The solvent is dichloromethane and N, N- Dimethylformamide.
- 3. preparation method according to claim 1, it is characterised in that：Step（1）The ultrasonic number is twice, every time 30min, and the water being heated in ultrasonic pond is replaced with cold water in ultrasonic procedure.
- 4. preparation method according to claim 1, it is characterised in that：Step（2）The high polymer material is polycaprolactone.
- 5. preparation method according to claim 1, it is characterised in that：Step（3）The condition of the electrospinning is：Delivery rate For 1 ml/h, rotating shaft rotating speed is 120 ± 10 r/min, and it is 13 ± 2 cm to receive height, and working bin temperature is 43 ± 2 DEG C, relative humidity is 40 ± 5%.
- 6. preparation method according to claim 1, it is characterised in that：Step（5）Middle stacking composite nano fiber small pieces need Upper and lower two layers of relative position is adjusted to ensure that grid is corresponding.
- A kind of 7. three dimensional patterned Fe as made from the preparation method described in claim any one of 1-63O4/ medical high polymer material Expect composite nano fiber.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110004504A (en) * | 2019-05-24 | 2019-07-12 | 北京化工大学 | A kind of patterning electrostatic spinning apparatus |
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| WO2017079328A1 (en) * | 2015-11-02 | 2017-05-11 | Nanofiber Solutions, Inc. | Electrospun fibers having contrast agents and methods of making the same |
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| EP1090928A1 (en) * | 1999-09-30 | 2001-04-11 | IsoTis N.V. | Polymers loaded with bioactive agents |
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| CN102978151A (en) * | 2012-11-06 | 2013-03-20 | 中国科学院大连化学物理研究所 | Method for flexibly producing cell module of different morphology and application |
| CN103405809A (en) * | 2013-07-23 | 2013-11-27 | 东华大学 | Method used for preparing microcarrier/polymer composite scaffold by electro-deposition |
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| CN110004504A (en) * | 2019-05-24 | 2019-07-12 | 北京化工大学 | A kind of patterning electrostatic spinning apparatus |
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