CN106567145A - Coaxially split dual-core containing microfluid control nozzle and spinning device and spinning method - Google Patents
Coaxially split dual-core containing microfluid control nozzle and spinning device and spinning method Download PDFInfo
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- CN106567145A CN106567145A CN201611004734.2A CN201611004734A CN106567145A CN 106567145 A CN106567145 A CN 106567145A CN 201611004734 A CN201611004734 A CN 201611004734A CN 106567145 A CN106567145 A CN 106567145A
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- syringe
- core
- coaxially
- capillary tube
- twin
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- 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
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- 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
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention provides a coaxially split dual-core containing microfluid control nozzle comprising a chief capillary tube, a first bending capillary tube and a second bending capillary tube; the first bending capillary tube and a second bending capillary tube are arranged inside the chief capillary tube side by side; the bending end of each of the first bending capillary tube and the second bending capillary tube goes through from the side surface of the chief capillary tube; the other end of each of the first bending capillary tube and the second bending capillary tube goes through from an outlet end of the chief capillary tube. The invention also discloses a high voltage electrostatic spinning device applying the nozzle; the spinning device comprises a first syringe pump, a first injection syringe, a second syringe pump, a second injection syringe, a third syringe pump, a third injection syringe, a silica gel flexible pipe, a fiber receiving plate and a high pressure generator. An enforcement method of preparing coaxially split dual-core containing structural nanometer fiber is also provided; under high voltage electrostatic field, high voltage electrostatic spinning technology is carried out to effectively prepare nano fiber having complex structural features containing the coaxially split dual-core.
Description
Technical field
The invention belongs to nanomaterial science field, is related to a kind of device for spinning and spinning process, it is more particularly to a kind of same
Axle includes the microfluidic control shower nozzle of division twin-core, a kind of multithread with the microfluidic control shower nozzle for coaxially including division twin-core
Body electric spinning equipment, and the method that electrospinning single step preparation coaxially includes the structure nano fiber of division twin-core is carried out using the device.
Background technology
High-voltage electrostatic spinning technology abbreviation electrospinning is a kind of nano-fabrication technique of (top-down) from top to bottom, is passed through
Extra electric field power overcomes the surface tension of liquid and viscoelastic power of shower nozzle tip drop and forms jet, in electrostatic repulsion, Coulomb force
Under surface tension collective effect, the liquid jet after being atomized is led within a few tens of milliseconds by high frequency flexural, drawing, division
Thousands of times is stretched, the volatilization of Jing solvents or melt cooling obtain nano-scale fiber in receiving terminal.The technical matters process is simple, manipulation side
Just, select that material ranges are extensive, controllability strong, and sprinkler design can be passed through prepare the Nanowire with microstructure characteristic
Dimension, it is considered to be most possibly realize a kind of method of continuous nano-fibre industrialized production, prepares function using the technology and receives
There is rice fiber good prospect to be expected.
The sharpest edges of electrospinning can be by the design and conversion of spinning header structure, and corresponding knot is effectively prepared in single step
The polymer micro-nanometer fiber of structure feature, this be other various " bottom-up " chemical synthesis process it is impossible.Most
Commonly core sheath structure nanofiber (Moghe AK and Gupta is prepared for spinneret using coaxial capillary metal canula
BS. Co-axial electrospinning for nanofiber structures: Preparation and
applications. Polym. Rev. 2008;48:Prepare 353-377.) and using left-right relation structure spinneret and receive side by side
Rice fiber (Walther A and M ü ller AHE. Janus particles: synthesis, self-assembly,
physical properties, and applications. Chem. Rev.2013;113:5194-5261.).But base
In this concept, also more nanostructured products with labyrinth feature have to be developed.
Development of Nano-technology merely reduces the micro-or nano size of product to obtain the concept of relevant nanometer effectiveness to today
Main flow has gradually been deflected away from.More attention all concentrate on nano-device, complicated micro nano structure and relevant nanometer layer at present
In secondary structure activity relationship.Structural integrity, the micro nanometer fiber with labyrinth feature how are effectively prepared, and is led to
The architectural feature for crossing fiber goes to design study hotspot that their function is both nanosecond science and technology, and micro manufacturing field and new micro-
The key content solved needed for nanometer product production.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of microfluid for coaxially including division twin-core
Control shower nozzle and device for spinning, spinning process, described this kind of microfluidic control shower nozzle for coaxially including division twin-core and
Device for spinning, spinning process prepare the complex process of the structure nano fiber for coaxially including division twin-core during prior art is solved
Technical problem.
The invention provides it is a kind of coaxially include division twin-core microfluidic control shower nozzle, including a total capillary tube, first
Tortuous capillary and the second tortuous capillary;The first described tortuous capillary and the second described tortuous capillary are set up in parallel
In described total capillary tube, one end of the bending of the first described tortuous capillary and the second described tortuous capillary from
The side of described total capillary tube passes, the other end of the first described tortuous capillary and the second described tortuous capillary
The port of export from described total capillary tube is passed and flushes setting.
Further, the other end of the first described tortuous capillary and the second described tortuous capillary passes institute
0.2 mm of the port of export of the total capillary tube stated, in width between the first described tortuous capillary and the second described tortuous capillary
Distance on degree direction is 0.2 mm, the first described tortuous capillary and the second described tortuous capillary respectively with it is described
The inwall of total capillary tube distance in the direction of the width is 0.2 mm.
Further, the entrance point of described total capillary tube is provided with an interface, sets on the lateral wall of described interface
It is all provided with the lateral wall of the bending section for being equipped with spiral reinforcement, the first described tortuous capillary and the second tortuous capillary
It is equipped with the projection of annular.
Further, the length of described total capillary tube is 70 mm;The length of the first tortuous capillary is 75 mm;Second
The length of tortuous capillary is 80 mm;Described total capillary tube, adopt between the first tortuous capillary and the second tortuous capillary
Epoxy resin is gluing together and to be sealed.
Present invention also offers a kind of high-voltage electrostatic spinning device, including the first syringe pump, the first syringe, the second injection
Pump, the second syringe, the 3rd syringe pump, the 3rd syringe, the first silica gel hose, the second silica gel hose, fiber receiver board, high pressure
Generator, a kind of microfluidic control shower nozzle for coaxially including division twin-core described in claim 1, described the first syringe peace
It is mounted in the first described syringe pump, the first described syringe and the described microfluidic control for coaxially including division twin-core are sprayed
Head connection, described the second syringe are arranged in the second described syringe pump, and described the second syringe is by described the
One silica gel hose and the described microfluidic control shower nozzle connection for coaxially including division twin-core, the 3rd described syringe are arranged on
In the 3rd described syringe pump, described the 3rd syringe passes through the second described silica gel hose and described coaxially includes division
The microfluidic control shower nozzle connection of twin-core, described high tension generator and the described microfluidic control for coaxially including division twin-core
Shower nozzle connects, and the lower end of the described microfluidic control shower nozzle for coaxially including division twin-core is provided with fiber receiver board.
Receive present invention also offers being prepared using above-mentioned high-voltage electrostatic spinning device and coaxially including the structure for dividing twin-core
The method of rice fiber, adds in the first syringe, and the 3rd
The 3rd spinning liquid is added in syringe, by high voltage electrostatic field, you can prepare the structure for coaxially including division twin-core
Nanofiber.
Further, the method that above-mentioned preparation coaxially includes the structure nano fiber of division twin-core, comprises the steps:
1), the step of a preparation spinning liquid, described the first spinning liquid is polyvinylpyrrolidine that mass percent concentration is 8%
The ethanol solution of ketone;Ethanol solution of second spinning liquid for Eudragit E100 that mass percent concentration is 13%;3rd spins
Ethanol solution of the silk liquid for Eudragit L100 that mass percent concentration is 13%;
2) first, second, and third spinning liquid obtained by step 1 is added separately in corresponding syringe, is then turned on the first note
Penetrate pump, the second syringe pump and the 3rd syringe pump;
3) the sheath flow quantity for controlling the first syringe is that the core flow quantity of 2.0 ml/h, control second and the 3rd syringe is
0.1 ml/h opens high tension generator, and it is 15 cm that adjustment fibre board receives distance, and voltage is upgraded to 15kV carries out electrospinning, obtains final product
Polyvinylpyrrolidone epitheca is wrapped up while being Eudragit E100, the division twin-core for Eudragit L100 is multiple in addition
Close structure nano fiber.
The present invention is on the basis of test of many times, it then follows the behavior characteristicss of fluid and basic natural rule under high voltage electric field
Rule, finds out a kind of microfluidic control shower nozzle for coaxially including division twin-core, using the shower nozzle assembling electric spinning equipment, implements electrospinning
Technique, can effectively be prepared the nanofiber for coaxially including division twin-core of structural integrity, size uniformity, be new with single step
Design, preparation and the large-scale production of structure nano functional material and application are provided may.
The present invention is compared with prior art, and its technological progress is significant.The height for coaxially including division twin-core of the present invention
Pressure electrospinning process application be simple and convenient to operate, it is easily controllable, in high-pressure electrostatic off field, using the method implement high pressure it is quiet
Electrospinning, can effectively prepare the nanofiber with the labyrinth feature for coaxially including division twin-core with single step,
And extensive amplification production can be carried out by increasing spinneret quantity.
Description of the drawings
Fig. 1 is a kind of monnolithic case schematic diagram of the microfluidic control shower nozzle for coaxially including division twin-core of the present invention, and 1- is total
Capillary tube, 2- tortuous capillaries, 3- tortuous capillaries, 4- interfaces, 5- annular protrusions, 6- epoxy resin.
Fig. 2 is a kind of outlet shooting figure of the microfluidic control shower nozzle for coaxially including division twin-core of the present invention.
Fig. 3 is a kind of structural representation of high-voltage electrostatic spinning device of the invention, and 7- high tension generators, 8- first is injected
Pump, the second syringe pumps of 9-, the 3rd syringe pumps of 10-, 11- coaxially include the microfluid electric injector of division twin-core, 12- fibers and receive
Plate, 13- the first high resiliency silica gel hoses, the first syringes of 14-, the second syringes of 15-, the 3rd syringes of 16-, 17- second are high
Elastic silica gel flexible pipe.
Fig. 4 is the connection of a kind of microfluidic control shower nozzle for coaxially including division twin-core of the present invention and whole fluid injectors
Mode.
Fig. 5 is the compound Taylor that the structure nano fiber for coaxially including division twin-core is prepared using the electric spinning equipment of the present invention
Diagram cone sample.
Fig. 6 is the structure nano fiber scanning electron microscope Electronic Speculum that division twin-core is coaxially included obtained by Application Example
Figure.
Fig. 7 is the structure nano fiber transmission electron microscope Electronic Speculum that division twin-core is coaxially included obtained by Application Example
Figure.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can be made various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
The invention provides a kind of microfluidic control shower nozzle for coaxially including division twin-core, including 1, first bending of total capillary tube
Capillary tube 2 and the second tortuous capillary 3;The first described tortuous capillary 2 and the second described tortuous capillary 3 are set up in parallel
In described total capillary tube 1, one end of the bending of the first described tortuous capillary 2 and the second described tortuous capillary 3
Side from described total capillary tube 1 passes, the first described tortuous capillary 2 and the second described tortuous capillary 3
Other end is passed from the port of export of described total capillary tube 1 and flushes setting.
Further, the other end of the first described tortuous capillary 2 and the second described tortuous capillary 3 is passed
0.2 mm of the port of export of described total capillary tube 1, the first described tortuous capillary 2 and the second described tortuous capillary 3 it
Between distance in the direction of the width be 0.2 mm, the first described tortuous capillary 2 and the second described tortuous capillary 3 and institute
The inwall of the total capillary tube 1 stated distance in the direction of the width is 0.2 mm, and its outlet side shooting figure is as shown in Figure 2.
Further, the entrance point of described total capillary tube 1 is provided with an interface 4, on the lateral wall of described interface 4
On the lateral wall of the bending section for being provided with spiral reinforcement, the first described tortuous capillary 2 and the second tortuous capillary 3
It is provided with the projection 5 of annular.
Further, the internal diameter of described interface 4 successively decreases from outside to inside successively.
Further, the length of described total capillary tube 1 is 70 mm;The length of the first tortuous capillary 2 is 75 mm;The
The length of two tortuous capillaries 3 is 80 mm;Described total capillary tube 1, the first tortuous capillary 2 and the second tortuous capillary 3 it
Between together and seal using epoxy resin 6 is gluing.
Embodiment 2
A kind of high-voltage electrostatic spinning device of the shower nozzle assembling of Application Example 1, its composition schematic diagram is as shown in figure 3, including high
Pressure generator 7, the first syringe pump 8, the second syringe pump 9, the 3rd syringe pump 10, the microfluid electric injector for coaxially including division twin-core
11st, fiber receiver board 12, the first high resiliency silica gel hose 13, the first syringe 14, the second syringe 15, the 3rd syringe 16,
Second high resiliency silica gel hose 17.
Using the high-voltage electrostatic spinning device with the microfluidic control shower nozzle for coaxially including division twin-core to three fluid streams
Implement electrospinning, concretely comprise the following steps:First syringe 14 is arranged in the first syringe pump 8, is added a kind of in the first syringe 14
Epitheca spinning liquid, the first syringe 14 are directly connected to the interface 4 of the microfluidic control shower nozzle 11 for coaxially including division twin-core.The
Two syringes 15 are arranged in the second syringe pump 9, add a kind of spinning liquid of second inner core, spin in the second syringe 15
Silk liquid is imported in the first tortuous capillary 2 by the first high resiliency silica gel hose 13.3rd syringe 16 is arranged on the 3rd note
Penetrate in pump 10, in the 3rd syringe 16, add another kind of spinning liquid of inner core, spinning liquid to pass through the second high resiliency silica gel
Flexible pipe 17 is imported in the second tortuous capillary 3.High tension generator 7 and coaxially include division twin-core microfluidic control shower nozzle
11 are directly connected to, and 11 lower end of shower nozzle is provided with a fiber receiver board 12, receive the hardboard that flat board 12 is aluminium foil parcel, should
Receive plate earthing.
Fig. 4 is each syringe connection high resiliency silica gel hose 13,17.
Application Example 1
It is using a kind of high-voltage electrostatic spinning device enforcement electrospinning of the shower nozzle assembling of the application described in embodiment 2, coaxial to prepare
The structure nano fiber of division twin-core is included, step is as follows:
1st, the preparation of spinning liquid
First spinning liquid, mass percent concentration are 8% polyvinylpyrrolidone (PVP) ethanol solution, and its compound method is such as
Under:Will the PVP of 8g be added in the ethanol of 92g, stir the PVP ethanol solution for obtaining final product that mass percent concentration is 8%;
Second spinning liquid, mass percent concentration is the ethanol solution of 13% Eudragit E100, and its compound method is as follows:
Will the Eudragit E100 of 13 g be added in the ethanol of 78g, it is 13% to stir and obtain final product mass percent concentration
Eudragit E100 solution;
3rd spinning liquid, mass percent concentration is the ethanol solution of 13% Eudragit L100, and its compound method is as follows:
Will the Eudragit L100 of 13 g be added in the ethanol of 78g, it is 13% to stir and obtain final product mass percent concentration
Eudragit L100 solution;
2nd, first, second, and third spinning liquid obtained by step 1 is added separately in corresponding syringe, is then turned on the first note
Penetrate pump 8, the second syringe pump 9 and the 3rd syringe pump 10;
3rd, the sheath flow quantity for controlling the first syringe 14 is 2.0 ml/h, controls the core of the second syringe 15 and the 3rd syringe 16
Flow quantity is 0.1 ml/h and opens high tension generator 7, and it is 15 cm that adjustment fibre board 12 receives distance, and voltage is upgraded to 15kV
Electrospinning is carried out, the structure nano fiber for coaxially including division twin-core is obtained final product.Drop before applied voltage and applying in preparation process
The composite construction taylor cone produced after voltage is as shown in Figure 5.
Application Example 2
Surface is carried out to the structure nano fiber for coaxially including division twin-core prepared by Application Example 1 using field scanning Electronic Speculum
Observe after metal spraying, as a result as shown in Figure 6.The prepared structure nano fiber for coaxially including division twin-core is collected uniform and is presented
Good linear condition, a diameter of 570 ± 60 nm.Coaxially included point to prepared using high resolution transmission electron microscopy
The structure nano fiber for splitting twin-core is observed, as a result as shown in fig. 7, the structure knot for coaxially including division twin-core of nanofiber
Structure is clear.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, on the premise of without departing from the technology of the present invention principle, some improvement can also be made, these improvement also should be regarded as this
The protection domain of invention.
Claims (7)
- It is 1. a kind of coaxially to include the microfluidic control shower nozzle for dividing twin-core, it is characterised in that:Including a total capillary tube, the first bending Capillary tube and the second tortuous capillary;The first described tortuous capillary and the second described tortuous capillary are disposed in parallel in institute In the total capillary tube stated, one end of the bending of the first described tortuous capillary and the second described tortuous capillary is from described The side of total capillary tube pass, the other end of the first described tortuous capillary and the second described tortuous capillary from The port of export of described total capillary tube is passed and flushes setting.
- 2. it is according to claim 1 it is a kind of coaxially include division twin-core microfluidic control shower nozzle, it is characterised in that:It is described The first tortuous capillary and the other end of the second described tortuous capillary pass the port of export of described total capillary tube 0.2 mm, the distance between the first described tortuous capillary and the second described tortuous capillary in the direction of the width are 0.2 Mm, the first described tortuous capillary and the second described tortuous capillary are respectively with the inwall of described total capillary tube in width Distance on direction is 0.2 mm.
- 3. it is according to claim 1 it is a kind of coaxially include division twin-core microfluidic control shower nozzle, it is characterised in that:It is described The entrance point of total capillary tube be provided with an interface, be provided with spiral reinforcement, institute on the lateral wall of described interface The first tortuous capillary stated and the projection that annular is provided with the lateral wall of the bending section of the second tortuous capillary.
- 4. it is according to claim 1 it is a kind of coaxially include division twin-core microfluidic control shower nozzle, it is characterised in that:It is described Total capillary tube length be 70 mm;The length of the first tortuous capillary is 75 mm;The length of the second tortuous capillary is 80 mm;It is described total capillary tube, gluing together and close using epoxy resin between the first tortuous capillary and the second tortuous capillary Envelope.
- 5. a kind of high-voltage electrostatic spinning device, it is characterised in that:Including the first syringe pump, the first syringe, the second syringe pump, Two syringes, the 3rd syringe pump, the 3rd syringe, the first silica gel hose, the second silica gel hose, fiber receiver board, high pressure occur Device, a kind of microfluidic control shower nozzle for coaxially including division twin-core described in claim 1, the first described syringe are arranged on In the first described syringe pump, the first described syringe and the described microfluidic control shower nozzle for coaxially including division twin-core connect Connect, the second described syringe is arranged in the second described syringe pump, the second described syringe passes through the first described silicon Glue flexible pipe and the described microfluidic control shower nozzle connection for coaxially including division twin-core, the 3rd described syringe are arranged on described The 3rd syringe pump in, described the 3rd syringe is by the second described silica gel hose and described coaxially includes division twin-core The connection of microfluidic control shower nozzle, described high tension generator and the described microfluidic control shower nozzle for coaxially including division twin-core Connection, is provided with fiber receiver board in the lower end of the described microfluidic control shower nozzle for coaxially including division twin-core.
- 6. the structure nano fiber of division twin-core is coaxially included using the high-voltage electrostatic spinning device preparation described in claim 5 Method, it is characterised in that:Add in the first syringe, The 3rd spinning liquid is added in 3rd syringe, by high voltage electrostatic field, you can prepare and coaxially include division twin-core Structure nano fiber.
- 7. it is as claimed in claim 6 to prepare the method for coaxially including the structure nano fiber for dividing twin-core, it is characterised in that bag Include following steps:1)The step of one preparation spinning liquid, described the first spinning liquid are polyvinylpyrrolidine that mass percent concentration is 8% The ethanol solution of ketone;Ethanol solution of second spinning liquid for Eudragit E100 that mass percent concentration is 13%;3rd spins Ethanol solution of the silk liquid for Eudragit L100 that mass percent concentration is 13%;2)First, second, and third spinning liquid obtained by step 1 is added separately in corresponding syringe, the first note is then turned on Penetrate pump, the second syringe pump and the 3rd syringe pump;3)The sheath flow quantity for controlling the first syringe is that the core flow quantity of 2.0 ml/h, control second and the 3rd syringe is 0.1 ml/h opens high tension generator, and it is 15 cm that adjustment fibre board receives distance, and voltage is upgraded to 15kV carries out electrospinning, obtains final product Polyvinylpyrrolidone epitheca is wrapped up while being Eudragit E100, the division twin-core for Eudragit L100 is multiple in addition Close structure nano fiber.
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CN110004506A (en) * | 2019-04-17 | 2019-07-12 | 中国科学院长春应用化学研究所 | A kind of micro-fluidic device for spinning and method |
CN110079877A (en) * | 2019-05-30 | 2019-08-02 | 上海理工大学 | The coaxial spinneret device of four kinds of electrospinning multistage composites |
CN111020880A (en) * | 2019-12-04 | 2020-04-17 | 广西民族大学 | Colon-targeted sinomenine hydrochloride sustained-release nanofiber membrane as well as preparation method and application thereof |
CN113897691A (en) * | 2021-11-16 | 2022-01-07 | 上海理工大学 | Preparation method of bead nanofiber with composite structure |
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CN103966680A (en) * | 2014-05-04 | 2014-08-06 | 东华大学 | Method for preparing drug sustained release nanofibers |
CN104611773A (en) * | 2015-01-19 | 2015-05-13 | 上海理工大学 | Eccentric sleeve type parallel spinning head and application thereof |
CN105384138A (en) * | 2015-10-27 | 2016-03-09 | 江西科技师范大学 | Core-shell type ultra-micro electrode prepared through coaxial electrostatic spinning and preparation method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN110004506A (en) * | 2019-04-17 | 2019-07-12 | 中国科学院长春应用化学研究所 | A kind of micro-fluidic device for spinning and method |
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CN110079877B (en) * | 2019-05-30 | 2020-06-23 | 上海理工大学 | Four-component electrospinning multi-stage composite coaxial spinning head device |
CN111020880A (en) * | 2019-12-04 | 2020-04-17 | 广西民族大学 | Colon-targeted sinomenine hydrochloride sustained-release nanofiber membrane as well as preparation method and application thereof |
CN113897691A (en) * | 2021-11-16 | 2022-01-07 | 上海理工大学 | Preparation method of bead nanofiber with composite structure |
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Application publication date: 20170419 |