CN106400133A - Device and method for producing eletrospinning fibers - Google Patents

Device and method for producing eletrospinning fibers Download PDF

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Publication number
CN106400133A
CN106400133A CN201610809663.7A CN201610809663A CN106400133A CN 106400133 A CN106400133 A CN 106400133A CN 201610809663 A CN201610809663 A CN 201610809663A CN 106400133 A CN106400133 A CN 106400133A
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CN
China
Prior art keywords
electrospun
spinning
syringe
coma
cabinet
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CN201610809663.7A
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Chinese (zh)
Inventor
靳林
王振领
李春阳
胡彬
黄敬斌
李贵军
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Zhoukou Normal University
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Zhoukou Normal University
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Priority to CN201610809663.7A priority Critical patent/CN106400133A/en
Publication of CN106400133A publication Critical patent/CN106400133A/en
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    • 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
    • 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
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • 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
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • 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
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields

Abstract

The invention provides a device for producing eletrospinning fibers. The device includes an eletrospinning cabinet, a high-voltage power supply, a boost pump, a circular receiving device and a rotation support. The invention provides a method for producing the eletrospinning fibers by using the device. The method includes mixing high polymer and a solvent to acquire a spinning solution; arranging the spinning solution in an injector, and starting the high-voltage power supply, the boost pump and the rotation support to perform spinning; separating a receiving liquid from fiber agglomerates in the circular receiving device to acquire the fiber agglomerates; and freezing the fiber agglomerates, and freeze-drying the fiber agglomerates to acquire the eletrospinning fibers. The device can produce the eletrospinning fibers, the produced eletrospinning fibers have three-dimensional directional fluffy structures, are large in specific surface area, have lots of connection holes inside, and can achieve three-dimensional cultivation of cells in vitro.

Description

A kind of apparatus and method preparing electrospinning fibre
Technical field
The present invention relates to electrospinning fibre technical field, more particularly, to prepare the apparatus and method of electrospinning fibre.
Background technology
Electrospinning fibre technology is that liquid pulls out the filament of nanometer or micro-meter scale using the electric charge on macromolecular liquid, its Detailed process is:Apply a high voltage in the syringe needle of injection pumping so that in syringe needle liquid carry electric charge, between electric charge Mutually exclusive and attract each other with earth terminal so that liquid can overcome surface tension to project surface and reach the receipts silk of ground connection Device.
Electrospinning fibre is one of of paramount importance material in Cell culture invitro support, in regeneration and the reparation of injury tissue Field has huge application prospect.The dominant mechanism that electrospinning fibre carries out cell culture is that the diameter Distribution of nanoscale can Simulate natural extra-cellular matrix structure well, and then promote adhesion, migration, growth and the induced cell proliferation of cell and turn Change.The fiber with ordered arrangement, due to its unique arrangement mode, can guide cell directional growth and promote nerve trunk thin Born of the same parents, to the formation of neutral net, therefore suffer from the extensive concern of researcher.
Traditional Electrospinning only can prepare the electrospun fiber membrane of the oriented and ordered structure with two dimension, this fiber Film is only cell and provides the growing space on surface, and narrow and small aperture makes cell be difficult to enter into internal stent growth, and then Greatly reduce the loading of support cell and the space of cell growth, be difficult to the real growing environment simulating cells in vivo.Cause This, existing two dimension directional fiber film can not meet the application requirement of its field of tissue engineering technology.
In recent years, the nanofiber exploitation with three-dimensional puffy structure is provided very with the In vitro culture studied as cell Good environment, can promote adhesion, migration, propagation and the growth of cell, and then form the organ or tissue with three dimensional structure. The purposes of such nanofiber can be expanded by coating somatomedin and other protein moleculars, be that the propagation of cell is carried with differentiation Supply environment advantageously.
But, with biomedical development, disorderly arranged three-dimensional electrospinning fibre can not meet the growth of specific cells Need.The growth of some cells (as neural stem cell) needs the arrangement architecture of three-dimensional order with differentiation, accordingly, it would be desirable to exploitation is new Technology prepare three-dimensional order arrangement puffy structure electrospinning fibre, so that cell is sticked on this three dimensional structure, to move Move and propagation, so that tissue is rebuild.
In recent years, research worker adopts various method preparation orientation electro spinning nano fibers, such as by improving reception device etc., But the fibre compact obtaining is piled up, and aperture is little and does not connect, it is difficult to meet external Three-dimensional cell culture it is impossible to meet higher Organizational project requires.
Content of the invention
Present invention solves the technical problem that being to provide a kind of preparation method of electrospinning fibre, the electrospinning of the application preparation is fine Dimension has three-dimensional orientation structure, achievable cells in vitro dimensional culture.
In view of this, this application provides a kind of device preparing electrospinning fibre, including:Electrospun cabinet, high voltage power supply, push away Enter pump, Electrospun reception device and runing rest, described Electrospun reception device includes circumferential receptacle device and runing rest;
The top of described Electrospun cabinet is provided with perforate, and propulsion pump lower end is fixed with syringe, and described syringe passes through institute State perforate to be arranged inside described Electrospun cabinet;
It is provided with spinning vessel immediately below the internal and described syringe of described Electrospun cabinet;
The circumferential receptacle device being loaded with reception liquid in described spinning vessel and not being totally submerged in described reception liquid;
The runing rest of described Electrospun reception device is arranged at described spinning vessel upper end, and described circumferential receptacle device is same Axle sleeve is in the outside of described runing rest;
Described spinning vessel outer bottom is provided with conductive layer;
Described conductive layer is connected with the negative pole of described high voltage power supply, the positive pole phase of described syringe and described high voltage power supply Even, described high voltage power supply is arranged at the outside of described Electrospun cabinet.
Preferably, the metal needle of described syringe and the distance of described reception liquid liquid level are 5~25cm.
Preferably, described spinning vessel is square container, and the length of described square container is more than 30cm, highly for 10~ 30cm.
Preferably, the conductive material of described conductive layer is stannum film.
Preferably, described reception liquid is selected from ethanol, methanol, acetone, water, dimethylformamide, chloroform, dichloromethane With one of oxolane or two kinds.
Preferably, the metal needle of described syringe is provided with heat insulating lamella, described heat insulating lamella is away from described metal needle At the bottom 3~10cm of head.
Present invention also provides the method preparing electrospinning fibre using the device described in such scheme, comprise the following steps:
High polymer is mixed with solvent, obtains spinning solution;
Described spinning solution is placed in syringe, opens high voltage power supply, propulsion pump and runing rest, start spinning;
Reception liquid in coma on circumferential receptacle device is separated, obtains coma;
Lyophilizing after described coma is freezed, obtains electrospinning fibre.
Preferably, described high polymer is selected from shitosan, sodium alginate, polyvinyl alcohol, collagen, protein, polylactic acid, gathers oneself One of lactone, polyaniline, polrvinyl chloride, polyethylene, polyethylene terephthalate and Poly(D,L-lactide-co-glycolide Or it is multiple;The concentration of described spinning solution is 6wt%~15wt%.
Preferably, described supply voltage is 5~25 kilovolts, and the fltting speed of described propulsion pump is 0.1~2.5ml/h.
Preferably, the step obtaining coma is specially:
Coma on circumferential receptacle device is transferred to equipped with the reception in the beaker of ultra-pure water, displacing in coma Liquid, repeated several times, obtain the coma containing ultra-pure water.
This application provides a kind of device preparing electrospinning fibre and the method preparing electrospinning fibre using described device.This Application is specially using the method that the device of electrospinning fibre prepares electrospinning fibre:First high polymer is mixed with solvent, spun Silk solution, recycles described device that above-mentioned spinning solution is placed in syringe, and opens high voltage power supply and propulsion pump, starts to spin Silk;Then the solvent in the coma on circumferential receptacle device is carried out separating, obtain coma, finally carry out the cold of coma Freeze and lyophilizing, obtain electrospinning fibre.In above process, the work of mutually exclusive power between electric charge for the spinning solution and electric field force With under, project from the syringe needle of syringe, form filament, due to the rotation of circumferential receptacle device, fiber is oriented, fiber is falling During be subject to the effects such as gravity, electric field force, repulsion between the twisting resistance of circumferential receptacle device and fiber and fiber, Fiber contacts are released to after reception liquid, and fiber can be dispersed in the presence of above-mentioned active force, finally carry out cold Freeze and lyophilizing, the form after making fiber disperse is preserved, thus preparing the electrospinning fibre of three-dimensional orientation puffy structure, its Specific surface area is big, and there is substantial amounts of internal connecting hole inside, is capable of cells in vitro dimensional culture.
Brief description
Fig. 1 prepares the schematic device of electrospinning fibre for the present invention;
Fig. 2 is the SEM photograph of the three-dimensional orientation polyacrylonitrile fibre of the embodiment of the present invention 1 preparation;
Fig. 3 is the fluorogram of the three-dimensional orientation polyacrylonitrile fibre of the embodiment of the present invention 1 preparation;
Fig. 4 is the SEM photograph of the three-dimensional orientation Poly-L-lactic acid fiber of the embodiment of the present invention 2 preparation.
Specific embodiment
For a further understanding of the present invention, with reference to embodiment, the preferred embodiment of the invention is described, but It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention Limit.
The embodiment of the invention discloses a kind of device preparing electrospinning fibre, including:Including:Electrospun cabinet, high voltage power supply, Propulsion pump, Electrospun reception device and runing rest, described Electrospun reception device includes circumferential receptacle device and runing rest;
The top of described Electrospun cabinet is provided with perforate, and propulsion pump lower end is fixed with syringe, and described syringe passes through institute State perforate to be arranged inside described Electrospun cabinet;
It is provided with spinning vessel immediately below the internal and described syringe of described Electrospun cabinet;
The circumferential receptacle device being loaded with reception liquid in described spinning vessel and not being totally submerged in described reception liquid;
The runing rest of described Electrospun reception device is arranged at described spinning vessel upper end, and described circumferential receptacle device is same Axle sleeve is in the outside of described runing rest;
Described spinning vessel outer bottom is provided with conductive layer;
Described conductive layer is connected with the negative pole of described high voltage power supply, the positive pole phase of described syringe and described high voltage power supply Even, described high voltage power supply is arranged at the outside of described Electrospun cabinet.
As shown in figure 1, Fig. 1 prepares the device of electrospinning fibre for the present invention, wherein 1 is propulsion pump, and 2 is syringe, and 3 is electricity Spinning cabinet, 4 is circumferential receptacle device, and 5 is runing rest, and 6 is spinning vessel, and 7 is conductive layer, and 8 is high voltage power supply.
According to the present invention, described Electrospun cabinet 3 is the cabinet of closing well known to those skilled in the art, and it can be closing Cuboid cabinet or closing square cabinet, to its shape, the application has no particular limits, described Electrospun The cabinet that cabinet 3 is preferably closing is to prevent the impact to electrospinning fibre for the air-flow during preparing electrospinning fibre.Described The top of Electrospun cabinet 3 is provided with through hole, with Electrospun cabinet 3 as square or as a example cuboid, the top of described Electrospun cabinet Can be the top of four sides of the upper surface of Electrospun cabinet or Electrospun cabinet, but electrospinning fibre for convenience Preparation, the application preferably Electrospun cabinet upper surface arrange perforate.Syringe 2 is arranged in Electrospun cabinet for convenience Portion, described perforate is preferably rectangle perforate.The lower end of described propulsion pump 1 is fixed with syringe 2, and described syringe 2 passes through institute State perforate and be arranged inside described Electrospun cabinet 3, described propulsion pump 1 is those skilled in the art with described syringe 2 and knows Part, this application is had no particular limits.Preferably, the metal needle of herein described syringe 2 is the bottom of from It is provided with heat insulating lamella, it contributes to stable and concentrates electric field, prevents fiber from flying away at the supreme 3~10cm in portion.
Herein described spinning vessel 6 is arranged at the inside of described Electrospun cabinet;Because Electrospun liquid is in the process declining Middle meeting is affected by gravity, and therefore, in order that Electrospun liquid is smoothed out spinning, herein described spinning vessel 6 is arranged at The underface of described syringe 2.The application has no particular limits to the shape of described spinning vessel, can be square, also may be used Think circle, preferably, described spinning vessel 6 is preferably square container, and its length is preferably greater than 30cm, to prevent electricity Spin fiber to be attached to around spinning vessel mouth;The highly preferred of described spinning vessel 6 is 10~30cm.Herein described spinning is held The concrete size of device 6 also needs to be selected further according to the amount of fiber prepared and the size of Electrospun cabinet, so that electric Spin the three-dimensional orientation fibrous framework that fiber is more likely formed high porosity.
It is loaded with reception liquid and circumferential receptacle device 4, described circumferential receptacle device 4 is by electrospinning in described spinning vessel 6 The device that fiber is wound, prepared by the winding in order to realize electrospinning fibre, the application is by circumferential receptacle device 4 and runing rest 5 are referred to as Electrospun reception device, and described circumferential receptacle device 4 is coaxially placed on outside runing rest 5, described circumferential receptacle device 4 are not exclusively immersed in reception liquid.In order to beneficial to preparation, the metal needle of described syringe 2 and the reception carrying out electrospinning fibre The distance of liquid liquid level is preferably 5cm~15cm, more preferably 8~10cm.Described reception liquid be preferably ethanol, methanol, acetone, One or more of water, dimethylformamide, chloroform, dichloromethane and oxolane, in an embodiment, described reception Liquid is preferably ethanol.
During preparing electrospinning fibre, spinning solution is injected downwards, in the presence of electric field force with gravity, its formation Spinning fibre, spinning fibre drops down onto circumferential receptacle device 4 surface, and circumferential receptacle device 4 rotates in the presence of runing rest 5, Being continuously increased with spinning fibre, spinning fibre constantly disperses, and forms coma.Herein described runing rest 5 is to drive The device of circumferential receptacle device 4 rotation, it is arranged at the upper end of described spinning vessel 6.Axis in described circumferential receptacle device 4 On direction, described runing rest 5 is preferably provided with rotation motor, to realize the automatic rotation of circumferential receptacle device.In order to protect The stable rotation of card runing rest, the application is preferably provided with the runing rest four direction parallel with described spinning vessel Frame, described frame is fixed on the surrounding of runing rest by rotation motor.
In order that spinning fibre is wound on circumferential receptacle device, the application is provided with high voltage power supply 8 and conductive layer 7, institute State the outside that high voltage power supply 8 is arranged at described Electrospun cabinet 3, and its positive pole is connected with syringe 2, positive pole is connected with conductive layer 7; Described conductive layer 7 is arranged at spinning vessel 6 bottom and and described Electrospun cabinet 3 between.Preferably, herein described height The negative pole of voltage source 8 also can make grounding simultaneously, can avoid producing electrostatic in preparation process, improve the safety of fiber preparation Property.The material of described conductive layer is preferably stannum film.
Present invention also provides the method preparing electrospinning fibre using said apparatus, comprise the following steps:
High polymer is mixed with solvent, obtains spinning solution;
Described spinning solution is placed in syringe, opens high voltage power supply, propulsion pump and runing rest, start spinning;
Reception liquid in coma on circumferential receptacle device is separated, obtains coma;
Lyophilizing after described coma is freezed, obtains electrospinning fibre.
According to the present invention, carry out the preparation of spinning solution first, high polymer will mix with solvent, obtain spinning solution; During this, described high polymer is biomaterial well known to those skilled in the art, can be according to from different types of biology material Material, obtains the three-dimensional electrospinning fibre support of different mechanical strengths, biocompatibility and degradation property;Example, described high polymer Be preferably selected from shitosan, sodium alginate, polyvinyl alcohol, collagen, protein, polylactic acid, polycaprolactone, polyaniline, polrvinyl chloride, One or more of polyethylene, polyethylene terephthalate and Poly(D,L-lactide-co-glycolide;More preferably left-handed poly- Lactic acid (PLLA) or polyacrylonitrile (PAN);Described solvent is similarly solvent well known to those skilled in the art, be preferably selected from DMF, THF and CH2Cl2One of or two kinds.The concentration of described spinning solution preferably 6wt%~20wt%, more preferably 10~ 15wt%, in order to the preparation of spinning fibre.
Then the application proceeds by spinning, specially:Spinning solution is placed in syringe, opens high voltage power supply, push away Enter pump and runing rest, start spinning;During this, spinning solution forms spinning fibre in dropping process, its be subject to gravity, Repulsion between electric field force, the twisting resistance of circumferential receptacle device and fiber and fiber etc. acts on, in fiber contacts to reception liquid After be released, formed homodisperse coma.The voltage of described high voltage power supply is preferably 10~20 kilovolts, and more preferably 12 ~16 kilovolts;The fltting speed of described propulsion pump is preferably 0.5~1.5 milli l/h, more preferably 0.6~1.2 milli l/h.
Contain reception liquid in the coma obtaining in said process, be unpurified it is therefore desirable to obtain said process Coma enter line replacement in ultra-pure water, to obtain the coma containing ultra-pure water.Detailed process is:
By on circumferential receptacle device coma transfer as equipped with the beaker of ultra-pure water, displace coma reception liquid become Point, repeated several times, the solvent that accepts in coma eliminates.
Coma containing ultra-pure water is finally freezed and frozen dried by the application, so that the coma preparing Preserve the form after dispersion, and the form of freeze-dried rear fiber still can keep the form of fiber, finally prepares Three-dimensional orientation electrospinning fibre.Described freezing and described frozen dried are technology well known to those skilled in the art, to this application Have no particular limits;Specifically, described freezing is carried out preferably in refrigerator, and the temperature of described freezing is preferably -20~-80 ℃;Described frozen dried is carried out preferably in freeze dryer.
The application, during preparing electrospinning fibre, has carried out electrospinning fibre using the described device preparing electrospinning fibre Preparation, make fiber under the rotation of circumferential receptacle device, fiber is oriented;During falling, fiber is subject to gravity, electricity Repulsion between field force, the twisting resistance of circumferential receptacle device and fiber and fiber etc. acts on, after fiber contacts to reception liquid It is released, then make fiber in the presence of these power, dispersed;Then freezed after displacement, saved Form after fiber dispersion, the form of freeze-dried rear fiber still can keep the form of fiber, and then can prepare three Dimension orientation electrospinning fibre.
The electrospinning fibre of present invention preparation has three-dimensional orientation puffy structure, and very bigger than table, there is substantial amounts of inside inside Connecting hole, the preparation process is simple of the present invention, operating aspect is expected to large-scale production.It is high that the present invention also is adapted for substantial amounts of solubility Molecular material prepares three-dimensional orientation electrospinning fibre.Additionally, process is simple of the present invention, circumferential receptacle device can promote three-dimensional The electrospinning fibre support of directive construction is formed in electro-spinning process, and can lead to undergone mass production.
The three-dimensional orientation electrospinning fibre support of the application preparation can promote cell can smoothly enter the inside of support, real Now external dimensional culture, is conducive to the tactophily of cell and the excretion of nutrient substance conveying and metabolic waste, improves cell Survival rate and reproduction speed, promote seed cell propagation in the bracket, growth and differentiation;It is cell growth and propagation provides Good metabolism environment, has great application prospect in regeneration and the reparation field of injury tissue.
For a further understanding of the present invention, with reference to embodiment the present invention is provided prepare the device of electrospinning fibre with Method is described in detail, and protection scope of the present invention is not limited by the following examples.
The present invention adopts scanning electron microscope (SEM, Hitachi S-4800N) to observe the pattern of sample;Fluorescence imaging Carried out using the Leica TCS-SP2 Confocal Microscope laser confocal microscope that German Leica company produces Test.
Embodiment 1
As shown in figure 1, Fig. 1 prepares the device of electrospinning fibre for the present invention, it includes:Micro propulsion pump 1, syringe 2, electricity Spun glass cabinet 3, circumferential receptacle device 4, runing rest 5, cuboid spinning vessel 6, conductive layer 7, high voltage power supply 8;
The top of Electrospun glass cabinet 3 has a slot, and propulsion pump 1 lower end fixation is led to by syringe 2, syringe 2 Cross oblong shaped orifices to embed inside glass cabinet 3, glass cabinet 3 is internally provided with rectangle spinning vessel 6, and rectangular tank 6 is located at Immediately below syringe 2, in rectangle spinning vessel 6, it is loaded with reception liquid and circumferential receptacle device 4, circumferential receptacle device 4 axle is even Connect runing rest 5, runing rest 5 is arranged at rectangle spinning vessel 6 upper end, the outer bottom of rectangle spinning vessel 6 is provided with Conductive layer 7, conductive layer 7 is connected with the negative pole of high voltage power supply 8 by conductor wire;The tinsel of syringe 2 bottom setting and high pressure The positive pole of power supply 8 is connected, and the metal needle of syringe is 15cm with the distance of reception liquid liquid level;
The length of rectangle spinning vessel 6 is 45cm, highly for 20cm, the metal needle of syringe 2 from bottom supreme 3~ It is provided with heat insulating lamella at 10cm.
The preparation of embodiment 2 three-dimensional orientation polyacrylonitrile electrospinning fibre, comprises the following steps:
1) preparation of spinning solution:Weigh 100 milligrams of PAN (molecular weight -10 ten thousand dalton), be dissolved in 1 milliliter of DMF solvent In, prepared 10wt%PAN solution, with ParafilmTM Solution bottle cap magnetic agitation 48 hours about, stand-by;
2) spinning process:Adjust micro propulsion pump parameter:3 milliliters of capacity, 1.0 mls/hour of fltting speed, open annular Reception device and runing rest, adjusting runing rest rotating speed makes slow-roll stabilization, contains into 3000ml ethanol, adjust liquid in square container Identity distance, from syringe needle 15cm, is opened high voltage power supply, 16 kilovolts of regulation voltage level, is started spinning, makes coma enter reception liquid ethanol In;
3) separate spinning fibre:PAN fiber group in ethanol is transferred to equipped with the beaker of ultra-pure water, solution will be received Each component permutation goes out three-dimensional orientation electrospinning fibre, and repeated several times eliminate the impurity such as the ethanol in three-dimensional fiber;
4) the three-dimensional electrospinning fibre group containing ultra-pure water is put into -80 DEG C of refrigerator freezings to freezing completely;
5) frozen samples that above-mentioned steps obtain are put into freeze dryer and carry out frozen dried, finally give PAN three-dimensional fiber Timbering material.As shown in Fig. 2 Fig. 2 is the SEM photograph of three-dimensional orientation polyacrylonitrile manufactured in the present embodiment, Fig. 3 is the present embodiment The fluorogram of the three-dimensional orientation polyacrylonitrile of preparation, from Fig. 2 and Fig. 3, three-dimensional electrospinning fibre support manufactured in the present embodiment Material is merrily and lightheartedly fluffy, and outward appearance is in spongy homogeneous clusters, and pore diameter is 10 μm~100 μm, and fibre diameter is 0.3~3 μm.
The preparation of embodiment 3 three-dimensional orientation Poly-L-lactic acid electrospinning fibre, comprises the following steps:
1) preparation of spinning solution:Weigh 65 milligrams of PLLA (molecular weight=200,000 dalton), be dissolved in lmL 9:1, CH2Cl2In/DMF (v/v) solvent, prepared 6.5wt%PLLA solution, magnetic agitation 6 hours, stand-by;
2) spinning process:Adjust micro propulsion pump parameter:1.0 milliliters of capacity, 0.6 ml/hour of fltting speed, run, Contain into 3000ml ethanol in square container, regulating liquid surface, apart from syringe needle 15cm, opens high voltage power supply, regulation voltage level is 12,000 Volt, starts spinning, so that coma is entered in reception liquid ethanol;
3) separate spinning fibre:PLLA coma in ethanol is transferred to equipped with the beaker of ultra-pure water, will receive molten The each component permutation of liquid goes out three-dimensional electrospinning fibre, and repeated several times eliminate the impurity such as the ethanol in three-dimensional fiber;
4) the three-dimensional electrospinning fibre group containing ultra-pure water that above-mentioned steps obtain is put into -80 DEG C of refrigerator freezings until tying completely Ice;
5) frozen samples that above-mentioned steps obtain are put into freeze dryer and carry out frozen dried, finally give PLLA three-dimensional orientation Fiber scaffold material.As shown in figure 3, Fig. 3 is the SEM photograph of three-dimensional orientation Poly-L-lactic acid fiber manufactured in the present embodiment, this The three-dimensional electrospinning fibre support material of embodiment preparation is merrily and lightheartedly fluffy, and outward appearance is in spongy homogeneous clusters, and pore diameter is 20 μm ~200 μm, fibre diameter is 0.5~3 μm.
The preparation of embodiment 4 three-dimensional orientation polyethylene electrospinning fibre, comprises the following steps:
1) preparation of spinning solution:Weigh 160 milligrams of PVC (molecular weight -10 ten thousand dalton), be dissolved in 1 milliliter and be dissolved in lmL 9:In 1, THF/DMF (v/v) solvent, prepared 16wt%PVC solution, using ParafilmTM Solution bottle cap magnetic agitation 24 hours Left and right, stand-by;
2) spinning process:Adjust micro propulsion pump parameter:2.5 milliliters of capacity, 1.2 mls/hour of fltting speed, run, Open rotary apparatuss, adjusting rotating speed makes slow-roll stabilization, contains into 3000ml ethanol, regulating liquid surface is apart from syringe needle in square container 15cm, opens high voltage power supply, 14 kilovolts of regulation voltage level, starts spinning, so that coma is entered in reception liquid ethanol;
3) separate spinning fibre:PVC coma in ethanol is transferred to equipped with the beaker of ultra-pure water, solution will be received Each component permutation goes out three-dimensional orientation electrospinning fibre, and repeated several times eliminate the impurity such as the ethanol in three-dimensional fiber;
4) the three-dimensional electrospinning fibre group containing ultra-pure water that above-mentioned steps obtain is put into -80 DEG C of refrigerator freezings to tying completely Ice;
5) frozen samples that above-mentioned steps obtain are put into freeze dryer and carry out frozen dried, finally give PVC three-dimensional fiber Timbering material.Three-dimensional electrospinning fibre support material manufactured in the present embodiment is merrily and lightheartedly fluffy, and outward appearance is in spongy homogeneous clusters, hole A diameter of 10 μm~100 μm, fibre diameter is 0.3~3 μm.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.It should be pointed out that it is right For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out Some improvement and modification, these improve and modify and also fall in the protection domain of the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention. Multiple modifications to these embodiments will be apparent from for those skilled in the art, as defined herein General Principle can be realized without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention It is not intended to be limited to the embodiments shown herein, and be to fit to and principles disclosed herein and features of novelty phase one The scope the widest causing.

Claims (10)

1. a kind of device preparing electrospinning fibre, including:Electrospun cabinet, high voltage power supply, propulsion pump, Electrospun reception device and rotation Turn support, described Electrospun reception device includes circumferential receptacle device and runing rest;
The top of described Electrospun cabinet is provided with perforate, and propulsion pump lower end is fixed with syringe, and described syringe passes through described opening Hole is arranged inside described Electrospun cabinet;
It is provided with spinning vessel immediately below the internal and described syringe of described Electrospun cabinet;
The circumferential receptacle device being loaded with reception liquid in described spinning vessel and not being totally submerged in described reception liquid;
The runing rest of described Electrospun reception device is arranged at described spinning vessel upper end, described circumferential receptacle device coaxial sleeve Outside in described runing rest;
Described spinning vessel outer bottom is provided with conductive layer;
Described conductive layer is connected with the negative pole of described high voltage power supply, and described syringe is connected with the positive pole of described high voltage power supply, institute State the outside that high voltage power supply is arranged at described Electrospun cabinet.
2. device according to claim 1 is it is characterised in that the metal needle of described syringe and described reception liquid liquid level Distance be 5~25cm.
3. device according to claim 1 it is characterised in that described spinning vessel be square container, described square container Length be more than 30cm, highly for 10~30cm.
4. device according to claim 1 is it is characterised in that the conductive material of described conductive layer is stannum film.
5. device according to claim 1 is it is characterised in that described reception liquid is selected from ethanol, methanol, acetone, water, diformazan One of base Methanamide, chloroform, dichloromethane and oxolane or two kinds.
6. device according to claim 1 it is characterised in that be provided with the metal needle of described syringe insulation thin Piece, described heat insulating lamella is at the bottom 3~10cm of described metal needle.
7. the method preparing electrospinning fibre using the device described in any one of claim 1~6, comprises the following steps:
High polymer is mixed with solvent, obtains spinning solution;
Described spinning solution is placed in syringe, opens high voltage power supply, propulsion pump and runing rest, start spinning;
Reception liquid in coma on circumferential receptacle device is separated, obtains coma;
Lyophilizing after described coma is freezed, obtains electrospinning fibre.
8. method according to claim 7 is it is characterised in that described high polymer is selected from shitosan, sodium alginate, polyethylene Alcohol, collagen, protein, polylactic acid, polycaprolactone, polyaniline, polrvinyl chloride, polyethylene, polyethylene terephthalate and poly- One or more of poly lactic coglycolic acid;The concentration of described spinning solution is 6wt%~15wt%.
9. method according to claim 7 is it is characterised in that described supply voltage is 5~25 kilovolts, described propulsion pump Fltting speed is 0.1~2.5ml/h.
10. method according to claim 7 is it is characterised in that the step obtaining coma is specially:
Coma on circumferential receptacle device is transferred to equipped with the reception liquid in the beaker of ultra-pure water, displacing in coma, Repeated several times, obtain the coma containing ultra-pure water.
CN201610809663.7A 2016-09-08 2016-09-08 Device and method for producing eletrospinning fibers Pending CN106400133A (en)

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