CN106435776A - Four-stage coaxial high-voltage electrospinning device and spinning method - Google Patents

Four-stage coaxial high-voltage electrospinning device and spinning method Download PDF

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Publication number
CN106435776A
CN106435776A CN201611004619.5A CN201611004619A CN106435776A CN 106435776 A CN106435776 A CN 106435776A CN 201611004619 A CN201611004619 A CN 201611004619A CN 106435776 A CN106435776 A CN 106435776A
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China
Prior art keywords
capillary
syringe
tortuous
tortuous capillary
level
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CN201611004619.5A
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Chinese (zh)
Inventor
余灯广
李郝林
张曼
郑招斌
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN201611004619.5A priority Critical patent/CN106435776A/en
Publication of CN106435776A publication Critical patent/CN106435776A/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
    • D01D5/0061Electro-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
    • D01D5/0015Electro-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
    • 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
    • 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
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/34Core-skin structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent

Abstract

The invention provides a four-stage coaxial microfluid control nozzle. The nozzle comprises a general capillary tube, a first bent capillary tube, a second bent capillary tube and a third bent capillary tube, wherein the first bent capillary tube is arranged in the general capillary tube, and the other end of the first bent capillary tube runs through the outlet end of the general capillary tube; the second bent capillary tube is arranged in the first bent capillary tube, the outlet end of the second bent capillary tube penetrates out from the outlet end of the first bent capillary tube, and the other end of the second bent capillary tube runs through the first bent capillary tube; and the third bent capillary tube is arranged in the second bent capillary tube, the outlet end of the third bent capillary tube penetrates out from the outlet end of the second bent capillary tube, and the other end of the third bent capillary tube runs through the second bent capillary tube. The invention further provides a high-voltage electrospinning device applying the nozzle, and a method for preparing a four-stage core sheath structure nano-fibers by applying the device to effectively prepare nano-fibers with the four-stage core-sheath structure characteristics in one step.

Description

A kind of level Four coaxial high pressure electrostatic spinning apparatus and spinning process
Technical field
The invention belongs to nanomaterial science field, the coaxial microfluidic control shower nozzle of more particularly to a kind of level Four, a kind of band There is the electric spinning equipment of level Four coaxial microfluidic control shower nozzle and carry the electrospinning dress of level Four coaxial microfluidic control shower nozzle using this Put the preparation method carrying out level Four core sheath structure feature nanofiber.
Background technology
High-voltage electrostatic spinning technology abbreviation electrospinning is the nano-fabrication technique of one kind (top-down) from top to bottom, passes through Extra electric field power overcomes the shower nozzle tip surface tension of liquid of drop and viscoelastic power to form jet, in electrostatic repulsion, Coulomb force Under surface tension collective effect, the liquid jet after being atomized, by high frequency flexural, drawing, division, was led within a few tens of milliseconds Stretch thousands of times, obtain nano-scale fiber through solvent volatilization or melt cooling in receiving terminal.This technical matters process is simple, manipulation side Just, selection material ranges are extensive, controllability is strong and can prepare the Nanowire with microstructure characteristic by sprinkler design Dimension, it is considered to be most possibly realizing a kind of method of continuous nano-fibre industrialized production, applies this technology preparation function to receive Rice fiber has good prospect expection.
The sharpest edges of electrospinning can be by design and the conversion of spinning header structure, and corresponding knot is prepared in single step effectively The polymer micro-nanometer fiber of structure feature, this be other various " bottom-up " chemical synthesis process impossible.? Commonly prepare core sheath structure nanofiber (Moghe AK and Gupta using coaxial capillary metal sleeve for spinneret BS. Co-axial electrospinning for nanofiber structures: Preparation and applications.Polym. Rev.2008;48:353-377.) receive side by side with application left-right relation structure spinneret preparation 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 is to today, the merely concept to obtain relevant nanometer effectiveness for the micro-or nano size of reduction product Gradually deflect away from main flow.More notices all concentrate on nano-device, complicated micro nano structure and relevant nanometer layer at present In secondary structure-activity relationship.How effectively to prepare structural integrity, there is labyrinth feature micro nanometer fiber, and lead to The architectural feature crossing fiber goes the function of designing them to be the study hotspot of nanosecond science and technology, be also micro manufacturing field and new micro- Nanometer product produces the required key content solving.
The present invention is on the basis of test of many times, it then follows the behavioural characteristic of fluid and basic natural rule under high voltage electric field Rule, finds out a kind of level Four coaxial microfluidic control shower nozzle, applies this shower nozzle assembling electric spinning equipment, implements electrospinning processes, permissible Structural integrity, size uniformity level Four coaxial rice fiber are prepared in single step effectively, be new structure nano-functional material design, Preparation and large-scale production and application provide may.
Content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of level Four coaxial high pressure electrostatic spinning apparatus And spinning process, described this level Four coaxial high pressure electrostatic spinning apparatus and spinning process will solve can not make in prior art The technical problem of standby level Four core sheath structure nanofiber.
The invention provides a kind of coaxial microfluidic control shower nozzle of level Four, a kind of coaxial microfluidic control shower nozzle of level Four, its It is characterised by:Including a total capillary, the first tortuous capillary and the second tortuous capillary and the 3rd tortuous capillary;Described The external diameter of the first tortuous capillary is less than the internal diameter of described total capillary;The external diameter of the second described tortuous capillary is less than institute The internal diameter of the first tortuous capillary stated;The external diameter of the 3rd described tortuous capillary is less than the internal diameter of the second tortuous capillary; The straightway of the first described tortuous capillary is arranged in described total capillary, the bending of described the first tortuous capillary Portion passes from the side wall of the entrance point of described total capillary, and the other end of the first described tortuous capillary passes described Total capillary the port of export;The straightway of the second described tortuous capillary is arranged in the first described tortuous capillary, The port of export of the second described tortuous capillary passes from the port of export of the first tortuous capillary, described second bending capillary The other end of pipe passes the first described tortuous capillary;The bend of the second described tortuous capillary is from described total hair Pass on the side wall of the entrance point of tubule;The straightway of the 3rd described tortuous capillary is arranged on the second described bending capillary Guan Zhong, the port of export of the 3rd described tortuous capillary passes from the port of export of the second tortuous capillary, and described the 3rd is curved The other end of bent capillary passes the second described tortuous capillary;The bend of the 3rd described tortuous capillary is from described The side wall of the entrance point of total capillary on pass;The first described tortuous capillary, the second tortuous capillary and the 3rd bend It is provided with annular protrusion on the lateral wall of bend entrance point of capillary;Described total capillary and the first bending capillary Pipe, the second tortuous capillary, the straightway of the 3rd tortuous capillary are coaxially disposed.
Further, the entrance point of described total capillary is provided with an interface, and the described lateral wall of interface sets It is equipped with spiral reinforcement.
Further, the port of export of the first described tortuous capillary passes the port of export 0.2mm of described total capillary; The port of export of the second described tortuous capillary passes the port of export 0.2mm of the first described tortuous capillary;Described the 3rd The port of export of tortuous capillary passes the port of export 0.2mm of the second described tortuous capillary,.
Further, the length of described total capillary is 70 mm, and the length of the first described tortuous capillary is 75 mm;The length of the second described tortuous capillary is 80 mm;The length of the 3rd described tortuous capillary is 85 mm;Described First tortuous capillary and the second tortuous capillary 15 and part outside in total capillary for the 3rd tortuous capillary adopt epoxy Resin is gluing and seals.
Present invention also offers a kind of electric spinning equipment, including the first syringe pump, the first syringe, the second syringe pump, second Syringe, the 3rd syringe pump, the 3rd syringe, the 4th syringe pump, the 4th syringe, the first silica gel hose, the second silica gel hose, 3rd silica gel hose, fiber receiver board, DC static high pressure generator, and the coaxial microfluid control of the level Four described in claim 1 Shower nozzle processed;The first described syringe is arranged in the first described syringe pump, the first described syringe and described level Four Coaxial microfluidic control shower nozzle connects, and the second described syringe is arranged in the second described syringe pump, described the second note Emitter passes through the first silica gel hose and described level Four coaxial microfluidic control shower nozzle connects, and the 3rd described syringe is arranged on In the 3rd described syringe pump, the 3rd described syringe passes through the second silica gel hose and the coaxial microfluidic control of described level Four Shower nozzle connects, and the 4th described syringe is arranged in the 4th described syringe pump, and the 4th described syringe passes through the 3rd silicon Glue flexible pipe and the connection of described level Four coaxial microfluidic control shower nozzle, described DC static high pressure generator and described level Four Coaxial microfluidic control shower nozzle connects, and the lower end of described level Four coaxial microfluidic control shower nozzle is provided with a fiber and receives Plate.
Present invention also offers the method preparing level Four Coaxial Nanofibers using above-mentioned electric spinning equipment, in the first injection Add the first spinning liquid in device, in the second syringe, add the second spinning liquid, in the 3rd syringe, add the 3rd spinning solution Body, adds the 4th spinning liquid in the 4th syringe, by high voltage electrostatic field, you can single step is prepared with level Four core sheath Structure nano fiber.
Specifically, the method for above-mentioned preparation level Four core sheath structure nanofiber, comprises the steps:
1) step of a preparation spinning solution, the first spinning solution be polyvinylpyrrolidone mass percent concentration be 8% second Alcoholic solution;Second spinning solution is the mixed ethanol solution of polyvinylpyrrolidone and phosphotungstic acid, in mixed solution, polyethylene pyrrole The mass percent concentration of pyrrolidone is 8%, and the mass percent concentration of phosphotungstic acid is 0.1%;3rd spinning solution is polyethylene pyrrole The mixed ethanol solution of pyrrolidone and phosphotungstic acid, in mixed solution, the mass percent concentration of polyvinylpyrrolidone is 8%, The mass percent concentration of phosphotungstic acid is 0.3%;4th spinning solution is molten for the mixed ethanol of polyvinylpyrrolidone and phosphotungstic acid Liquid, in mixed solution, the mass percent concentration of polyvinylpyrrolidone is 8%, and the mass percent concentration of phosphotungstic acid is 1%;
2) the first spinning solution of step 1 gained is added separately in corresponding syringe to the 4th spinning solution, is then turned on first To the 4th syringe pump;
3) control each laminar flow amount to be respectively 1.5,0.6,0.3,0.2mL/h from the first syringe to the 4th syringe, open direct current HV generator, voltage is upgraded to 18kV and carries out electrospinning arranged side by side, obtain final product the nanofiber with level Four core sheath structure feature.
The principle of the present invention is:The level Four coaxial configuration of level Four coaxial microfluidic control shower nozzle is to prepare corresponding construction nanometer Material provides a macroscopical masterplate, in high-pressure electrostatic off field, by the interaction of high-voltage electrostatic field and fluid, several milliseconds it The interior solid nano fiber that liquid spinning dope is drawn into clear in structure.On the other hand, shower nozzle each layer outlet height is inconsistent, has Effect prevents phase counterdiffusion at nozzle position for the fluid between layers.Above-mentioned principle collective effect it is ensured that high-pressure electrostatic off field, From macroscopical masterplate to accurate " duplication " of microcosmic level Four core sheath structure nanofiber.
The present invention compares with prior art, and its technological progress is significant.A kind of level Four coaxial high pressure electrostatic spinning of the present invention Method application be simple and convenient to operate, easily controllable, level Four core sheath structure can effectively be prepared with single step under high voltage electric field and receive Rice fiber, and production can be amplified on a large scale by increasing spinneret quantity.
Brief description
Fig. 1 is a kind of monnolithic case schematic diagram of the coaxial microfluidic control shower nozzle of level Four of the present invention, the total capillary of 13-, 16- First tortuous capillary, 15- second tortuous capillary, 14- the 3rd tortuous capillary.
Fig. 2 is a kind of outlet shooting figure of the coaxial microfluidic control shower nozzle of level Four of the present invention.
Fig. 3 is the electric spinning equipment structural representation of the present invention, 1- DC static high pressure generator, 2- first syringe pump, 3- Second syringe pump, 4- the 3rd syringe pump, 5- the 4th syringe pump, 6- fiber receiver board, 7- level Four coaxial microfluidic control shower nozzle, 8- First high resiliency silica gel hose, 9- first syringe, 10- second syringe, 11- the 3rd syringe, 12- the 4th syringe, 18- Second high resiliency silica gel hose, 19- the 3rd high resiliency silica gel hose.
Fig. 4 is a kind of level Four coaxial microfluidic control shower nozzle of the present invention and whole fluid injector connected modes.
Fig. 5 is that the electric spinning equipment of the present invention prepares compound Taylor's diagram cone that level Four coaxial configuration nanofiber process shoots Sample.
Fig. 6 is Application Example gained level Four core sheath structure nanofiber SEM electron microscope;
Fig. 7 is Application Example gained level Four core sheath structure nanofiber transmission electron microscope electron microscope.
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 restriction the scope of the present invention.In addition, it is to be understood that after having read the content of present invention instruction, people in the art Member can make 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 coaxial microfluidic control shower nozzle of level Four, including a total capillary 13, the first tortuous capillary 16 With the second tortuous capillary 15 and the 3rd tortuous capillary 14;The external diameter of the first described tortuous capillary 16 is less than described total The internal diameter of capillary 13;The external diameter of the second described tortuous capillary 15 is less than the internal diameter of the first described tortuous capillary 16; The external diameter of the 3rd described tortuous capillary 14 is less than the internal diameter of the second tortuous capillary 15;
The straightway of the first described tortuous capillary 16 is arranged in described total capillary 13, described the first bending capillary The bend of pipe 16 passes from the side wall of the entrance point of described total capillary 13, described the first tortuous capillary 16 another Outer one end passes the port of export of described total capillary 13;The straightway of the second described tortuous capillary 15 is arranged on described In first tortuous capillary 16, the port of export of described the second tortuous capillary 15 is from the port of export of the first tortuous capillary 16 Pass, the other end of the second described tortuous capillary 15 passes the first described tortuous capillary 16;Described second is curved The bend of bent capillary 15 passes from the side wall of the entrance point of described total capillary 13;The 3rd described tortuous capillary 14 straightway is arranged in the second described tortuous capillary 15, and the port of export of described the 3rd tortuous capillary 14 is from second Pass in the port of export of tortuous capillary 15, the other end of the 3rd described tortuous capillary 14 passes the second described bending Capillary 15;The bend of the 3rd described tortuous capillary 14 is worn from the side wall of the entrance point of described total capillary 13 Go out;The described bend entrance point of the first tortuous capillary 16, the second tortuous capillary 15 and the 3rd tortuous capillary 14 Annular protrusion 18 is provided with lateral wall;Described total capillary 13 and the first tortuous capillary 16, the second tortuous capillary 15th, the straightway of the 3rd tortuous capillary 14 is coaxially disposed.
Further, the junction sealing of the second described tortuous capillary 15 and the first described tortuous capillary 16 sets Put;The junction sealing setting of the 3rd described tortuous capillary 14 and the second described tortuous capillary 15.
Further, the entrance point of described total capillary 13 is provided with an interface 17, the outside of described interface 17 Spiral reinforcement is provided with wall.The internal diameter of described interface 17 successively decreases from outside to inside successively.
Further, the junction sealing of the first described tortuous capillary 16 and the second described tortuous capillary 15 sets Put;The junction sealing setting of the 3rd described tortuous capillary 14 and the second described tortuous capillary 15.
Further, the port of export of the first described tortuous capillary 16 passes the port of export of described total capillary 13 0.2mm;The port of export of the second described tortuous capillary 15 passes the port of export 0.2mm of the first described tortuous capillary 16; The port of export of the 3rd described tortuous capillary 14 passes the port of export 0.2mm of the second described tortuous capillary 15, and level Four is same It is as shown in Figure 2 that the exit portion side of axle microfluidic control shower nozzle shoots pattern.
Further, the length of described total capillary 13 is 70 mm, and the length of the first described tortuous capillary 16 is 75 mm;The length of the second described tortuous capillary 15 is 80 mm;The length of the 3rd described tortuous capillary 14 is 85 mm;The first described tortuous capillary 16 and the second tortuous capillary 15 and the 3rd tortuous capillary are outside total capillary 13 Part is gluing and seal using epoxy resin.
Embodiment 2
A kind of electric spinning equipment with the coaxial microfluidic control shower nozzle of the level Four described in embodiment 1, its composition schematic diagram such as Fig. 3 Shown, including DC static high pressure generator 1, the first syringe pump 2, the second syringe pump 3, the 3rd syringe pump 4, the 4th syringe pump 5, Fiber receiver board 6, level Four coaxial microfluidic control shower nozzle 7, the first high resiliency silica gel hose 8, the first syringe 9, second are injected Device 10, the 3rd syringe 11, the 4th syringe 12, total capillary 13, the second high resiliency silica gel hose 19, the second high resiliency silica gel Flexible pipe 20.
Add the first outermost layer spinning liquid in the first syringe 9 on the first syringe pump 2, the first syringe 9 is straight Connect and connect with the interface 17 of level Four coaxial microfluidic control shower nozzle 7, add the in the second syringe 10 on the second syringe pump 3 Two kinds outer layer spinning liquid, the second syringe 10 passes through the first high resiliency silica gel hose 8 and the first tortuous capillary 16 connects, The third third layer spinning liquid from outside to inside, the 3rd syringe 11 is added in the 3rd syringe 11 on the 3rd syringe pump 4 Connected by the second high resiliency silica gel hose 19 and the first tortuous capillary 15, the 4th syringe 12 on the 4th syringe pump 5 Interior addition the 4th inner core spinning liquid, the 4th syringe 12 passes through the 3rd high resiliency silica gel hose 20 and the first tortuous capillary 14 Connect.By respective syringe pump by coaxial for spinning liquid simultaneous implantation level Four microfluidic control shower nozzle 7.High pressure generator 1 and four The coaxial microfluidic control shower nozzle 5 of level connects.Level Four coaxial microfluidic control shower nozzle 5 lower end is provided with a fiber receiver board 6, connects The hardboard being wrapped up for aluminium foil by flat board 4, this accepts plate earthing.Start high direct voltage electrostatic generator 1 and increase appropriate electrical Pressure, you can single step is prepared effectively with level Four core sheath structure nanofiber.
Application Example 1
Electric spinning equipment using the coaxial microfluidic control shower nozzle of the level Four described in embodiment 2 carries out electrospinning to two fluids, to make Get everything ready and have the nanofiber of level Four core sheath structure feature, it comprises the following steps that:
1st, the preparation of spinning solution
First spinning solution, mass percent concentration is 8% polyvinylpyrrolidone (PVP) ethanol solution, and its compound method is such as Under:The PVP of 8g will be added in the ethanol of 92g, stir and obtain final product the PVP ethanol solution that mass percent concentration is 8%;
Second spinning solution, mass percent concentration be 8% polyvinylpyrrolidone (PVP) and low phosphorus wolframic acid ethanol molten Liquid, its compound method is as follows:PVP the and 0.1g phosphotungstic acid of 8g will be added in the ethanol of 91.9g, stir and obtain final product quality Percent concentration is 8% PVP ethanol solution;
3rd spinning solution, mass percent concentration be 8% polyvinylpyrrolidone (PVP) and middle concentration phosphotungstic acid ethanol molten Liquid, its compound method is as follows:The PVP of 8g and 0.3 g phosphotungstic acid will be added in the ethanol of 91.7g, stir and obtain final product matter Amount percent concentration is 8% PVP ethanol solution;
4th spinning solution, mass percent concentration be 8% polyvinylpyrrolidone (PVP) and high concentration phosphorus wolframic acid ethanol molten Liquid, its compound method is as follows:The PVP of 8g and 1.0 g phosphotungstic acids will be added in the ethanol of 91g, stir and obtain final product quality Percent concentration is 8% PVP ethanol solution;
2nd, the first spinning solution of step 1 gained is added separately in corresponding syringe to the 4th spinning solution, is then turned on first To the 4th syringe pump 2,3,4,5;
3rd, control each laminar flow amount to be respectively 1.5,0.6,0.3,0.2 mL/h from the first syringe 9 to the 4th syringe 12, open High direct voltage electrostatic generator 1, voltage is upgraded to 18kV and carries out electrospinning arranged side by side, obtain final product the nanometer with level Four core sheath structure feature Fiber.
Application Example 2
Level Four core sheath structure nanofiber prepared by Application Example 1 is carried out see after the metal spraying of surface using field scan Electronic Speculum Examine, result is as shown in Figure 6.Prepared level Four core sheath structure collecting nanofibers uniformly and assume good linear condition, directly Footpath is 720 ± 150nm.Using high-resolution projection electron microscope, prepared level Four core sheath structure nanofiber is seen Examine, result is as shown in fig. 7, due to the effect of contrast preparation phosphotungstic acid, the level Four core sheath structure of nanofiber is clear.
The above is only the citing of embodiments of the present invention it is noted that ordinary skill for 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)

1. a kind of coaxial microfluidic control shower nozzle of level Four it is characterised in that:Including a total capillary, the first tortuous capillary and Two tortuous capillaries and the 3rd tortuous capillary;The external diameter of the first described tortuous capillary is less than the interior of described total capillary Footpath;The external diameter of the second described tortuous capillary is less than the internal diameter of the first described tortuous capillary;The 3rd described curved hairs The external diameter of tubule is less than the internal diameter of the second tortuous capillary;The straightway of the first described tortuous capillary is arranged on described total In capillary, the bend of the first described tortuous capillary passes from the side wall of the entrance point of described total capillary, institute The other end of the first tortuous capillary stated passes the port of export of described total capillary;The second described tortuous capillary Straightway is arranged in the first described tortuous capillary, and the port of export of the second described tortuous capillary bends capillary from first Pass in the port of export of pipe, the other end of the second described tortuous capillary passes the first described tortuous capillary;Described The bend of the second tortuous capillary pass from the side wall of the entrance point of described total capillary;The 3rd described curved hairs The straightway of tubule is arranged in the second described tortuous capillary, and the port of export of the 3rd described tortuous capillary is curved from second Pass in the port of export of bent capillary, the other end of the 3rd described tortuous capillary passes the second described bending capillary Pipe;The bend of the 3rd described tortuous capillary passes from the side wall of the entrance point of described total capillary;Described It is provided with ring on the lateral wall of bend entrance point of one tortuous capillary, the second tortuous capillary and the 3rd tortuous capillary Shape is raised;Described total capillary and the first tortuous capillary, the second tortuous capillary, the 3rd tortuous capillary straightway with Axle is arranged.
2. a kind of coaxial microfluidic control shower nozzle of level Four according to claim 1 it is characterised in that:Described total capillary Entrance point be provided with an interface, the described lateral wall of interface is provided with spiral reinforcement.
3. a kind of coaxial microfluidic control shower nozzle of level Four according to claim 1 it is characterised in that:The first described bending The port of export of capillary passes the port of export 0.2mm of described total capillary;The port of export of the second described tortuous capillary is worn Go out the port of export 0.2mm of the first described tortuous capillary;The port of export of the 3rd described tortuous capillary passes described the The port of export 0.2mm of two tortuous capillaries.
4. a kind of coaxial microfluidic control shower nozzle of level Four according to claim 1 it is characterised in that:Described total capillary Length be 70 mm, the length of described the first tortuous capillary is 75 mm;The length of the second described tortuous capillary is 80 mm;The length of the 3rd described tortuous capillary is 85 mm;Described the first tortuous capillary, the second tortuous capillary and 3rd tortuous capillary is gluing and seal using epoxy resin in the part of total capillary lateral outer.
5. a kind of electric spinning equipment it is characterised in that:Including the first syringe pump, the first syringe, the second syringe pump, the second injection Device, the 3rd syringe pump, the 3rd syringe, the 4th syringe pump, the 4th syringe, the first silica gel hose, the second silica gel hose, the 3rd Silica gel hose, fiber receiver board, DC static high pressure generator, and the spray of the coaxial microfluidic control of the level Four described in claim 1 Head;The first described syringe is arranged in the first described syringe pump, and the first described syringe and described level Four are coaxial Microfluidic control shower nozzle connects, and the second described syringe is arranged in the second described syringe pump, described the second syringe Connected by the first silica gel hose and described level Four coaxial microfluidic control shower nozzle, the 3rd described syringe is arranged on described The 3rd syringe pump in, described the 3rd syringe passes through the second silica gel hose and described level Four coaxial microfluidic control shower nozzle Connect, the 4th described syringe is arranged in the 4th described syringe pump, it is soft that the 4th described syringe passes through the 3rd silica gel Pipe and described level Four coaxial microfluidic control shower nozzle connect, and described DC static high pressure generator and described level Four are coaxial Microfluidic control shower nozzle connects, and the lower end of described level Four coaxial microfluidic control shower nozzle is provided with a fiber receiver board.
6. utilize claim 4 described in electric spinning equipment prepare level Four Coaxial Nanofibers method it is characterised in that:First Add the first spinning liquid in syringe, in the second syringe, add the second spinning liquid, in the 3rd syringe, add the 3rd spinning Silk liquid, adds the 4th spinning liquid in the 4th syringe, by high voltage electrostatic field, you can single step is prepared with level Four Core sheath structure nanofiber.
7. the method for preparation level Four core sheath structure nanofiber according to claim 5 is it is characterised in that include following walking Suddenly:
1)The step of one preparation spinning solution, the first spinning solution be polyvinylpyrrolidone mass percent concentration be 8% second Alcoholic solution;Second spinning solution is the mixed ethanol solution of polyvinylpyrrolidone and phosphotungstic acid, in mixed solution, polyethylene pyrrole The mass percent concentration of pyrrolidone is 8%, and the mass percent concentration of phosphotungstic acid is 0.1%;3rd spinning solution is polyethylene pyrrole The mixed ethanol solution of pyrrolidone and phosphotungstic acid, in mixed solution, the mass percent concentration of polyvinylpyrrolidone is 8%, The mass percent concentration of phosphotungstic acid is 0.3%;4th spinning solution is molten for the mixed ethanol of polyvinylpyrrolidone and phosphotungstic acid Liquid, in mixed solution, the mass percent concentration of polyvinylpyrrolidone is 8%, and the mass percent concentration of phosphotungstic acid is 1%;
2)First spinning solution of step 1 gained is added separately in corresponding syringe to the 4th spinning solution, is then turned on first To the 4th syringe pump;
3)Control each laminar flow amount to be respectively 1.5,0.6,0.3,0.2 mL/h from the first syringe to the 4th syringe, open direct current HV generator, voltage is upgraded to 18kV and carries out electrospinning arranged side by side, obtain final product the nanofiber with level Four core sheath structure feature.
CN201611004619.5A 2016-11-15 2016-11-15 Four-stage coaxial high-voltage electrospinning device and spinning method Pending CN106435776A (en)

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CN107366028A (en) * 2017-07-28 2017-11-21 浙江工业大学之江学院 A kind of batch prepares the electrospinning process of core-sheath composite structure nanofiber
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