CN106757415B - A kind of microfluidic control spray head, device for spinning and the spinning process of three-level arrangement - Google Patents
A kind of microfluidic control spray head, device for spinning and the spinning process of three-level arrangement Download PDFInfo
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- CN106757415B CN106757415B CN201611121803.8A CN201611121803A CN106757415B CN 106757415 B CN106757415 B CN 106757415B CN 201611121803 A CN201611121803 A CN 201611121803A CN 106757415 B CN106757415 B CN 106757415B
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- capillary
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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
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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
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The present invention provides a kind of microfluidic control spray heads of three-level arrangement, including a total capillary, the first tortuous capillary and the second tortuous capillary；The section at total capillary outlet end is ellipse, the straightway of first tortuous capillary is arranged in total capillary, the lateral wall of first straight line section is close to an inner sidewall of total capillary, the outlet end of total capillary is stretched out in the outlet end of first tortuous capillary, and the bending part of the first tortuous capillary is pierced by from the side of total capillary；The second straight line section of second tortuous capillary is arranged in total capillary, the lateral wall of second straight line section is close to the inner sidewall of the other side of total capillary, the outlet end of total capillary is stretched out in the outlet end of second tortuous capillary, and the bending part of the second tortuous capillary is pierced by from the side of total capillary.A kind of high-voltage electrostatic spinning device containing above-mentioned spray head is additionally provided, the nanofiber for providing the labyrinth feature of three-level arrangement can be effectivelyed prepared with single step using above-mentioned apparatus.
Description
Technical field
The invention belongs to field of nano material preparation, the microfluidic control spray heads arranged more particularly to a kind of three-level, one
The multi-fluid electric spinning equipment of microfluidic control spray head of the kind with three-level arrangement, and the device is utilized to carry out electrospinning single step preparation three
The method of the structure nano fiber of grade arrangement.
Background technique
High-voltage electrostatic spinning technology (abbreviation electrospinning) is the nano-fabrication technique of a kind of (top-down) from top to bottom, is led to
Cross extra electric field power overcome spray head tip drop surface tension of liquid and viscoelastic power and form jet stream, in electrostatic repulsion, coulomb
Under power and surface tension collective effect, the liquid jet after being atomized is by high frequency flexural, drawing, division, the quilt within a few tens of milliseconds
Drawing-off thousands of times obtains nano-scale fiber in receiving end through solvent volatilization or melt are cooling.The technical matters process is simple, manipulates
Conveniently, selection material ranges are extensive, controllability is strong and can pass through sprinkler design prepares the nanometer with microstructure characteristic
Fiber, it is considered to be a kind of most possible method for realizing continuous nano-fibre industrialized production prepares function using the technology
Nanofiber is expected with good prospect.
The sharpest edges of electrospinning are that corresponding knot can be effectivelyed prepared out by the design and transformation of spinning header structure, single step
The polymer micro-nanometer fiber of structure feature, this is that the chemical synthesis process of various other " bottom-up " is impossible.Most
It the use of coaxial capillary metal sleeve is commonly that spinneret prepares core sheath structure nanofiber (Moghe AK and Gupta
BS. Co-axial electrospinning for nanofiber structures: Preparation and
applications. Polym. Rev. 2008;48:353-377.) received 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 reduces the micro-or nano size of product merely to today to obtain the concept of relevant nanometer effectiveness
Gradually deflect away from mainstream.More attentions all concentrate on nano-device, complicated micro nano structure and relevant nanometer layer at present
In secondary structure-activity relationship.Structural integrity, micro nanometer fiber with labyrinth feature how are be effectivelyed prepared out, and is led to
It is both research hotspot and the micro manufacturing field and novel micro- of nanosecond science and technology that the structure feature for crossing fiber, which goes the function of designing them,
Nanometer product production institute key content to be solved.
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 microfluidic control spray head of three-level arrangement, using spray head assembling electric spinning equipment, implements electrospinning processes, can
The nanofiber that structural integrity, the arrangement of the three-level of size uniformity are be effectivelyed prepared out with single step is new structure nano functional material
Design, preparation and the large-scale production and application of material provide may.
Summary of the invention
For above-mentioned technical problem in the prior art, the present invention provides a kind of microfluidic control sprays of three-level arrangement
Head, device for spinning and spinning process, microfluidic control spray head, device for spinning and the spinning process of this three-level arrangement are wanted
Solve the technical issues of preparing the complex process of the structure nano fiber of three-level arrangement in the prior art.
The present invention provides a kind of microfluidic control spray heads of three-level arrangement, including total capillary, first curved hairs
Tubule and the second tortuous capillary；The section at total capillary outlet end is ellipse, first tortuous capillary
Including a first straight line section and first bending part, the first straight line section is arranged in total capillary, institute
The lateral wall for the first straight line section stated is close to an inner sidewall of total capillary, and first tortuous capillary goes out
The outlet end of total capillary is stretched out at mouthful end, and the bending part of first tortuous capillary is from total capillary
Side is pierced by；Second tortuous capillary includes a second straight line section and second bending part, and described second is straight
Line segment is arranged in total capillary, and the lateral wall of the second straight line section is close to other the one of total capillary
The inner sidewall of side, the outlet end of the outlet end stretching of second tortuous capillary total capillary, described second
The bending part of tortuous capillary is pierced by from the side of total capillary, the first straight line section and the second straight line
There is gap between section.
Further, the outlet end of first tortuous capillary is concordant with the outlet end of total capillary, and described
The outlet end of two tortuous capillaries is also concordant with the outlet end of total capillary.
Further, the length of total capillary is 70 mm, and the input end of total capillary is provided with one
Interface, spiral reinforcing rib is provided on the lateral wall of the interface, and the length of first tortuous capillary is 55
mm；The length of second tortuous capillary is 55 mm；The interface, the first tortuous capillary, the second tortuous capillary
It is connected place with total capillary and is all made of the sealing of epoxy resin gluing.
Further, it is respectively provided on the lateral wall of the bending part of first tortuous capillary and the second tortuous capillary
There is the protrusion of annular.
The present invention also provides a kind of high-voltage electrostatic spinning devices, including the first syringe pump, the first syringe, the second injection
Pump, the second syringe, third syringe pump, third syringe, fiber receiver board, high pressure generator and described in claim 1 three
The microfluidic control spray head of grade arrangement, first syringe are mounted in first syringe pump, first note
Emitter is connected with the microfluidic control spray head, and second syringe is mounted in second syringe pump, described
The second syringe microfluidic control spray head described by the connection of silica gel hose, the third syringe is mounted on institute
In the third syringe pump stated, the third syringe microfluidic control spray head described by second silica gel hose connection,
The high pressure generator is connected with the microfluidic control spray head, and the lower end of the microfluidic control spray head is provided with fibre
Tie up receiver board.
The present invention also provides the method for the structure nano fiber using above-mentioned electric spinning equipment preparation three-level arrangement, the
The intermediate spinning liquid of the first arrangement is added in one syringe, the spinning liquid on second of one side is added in the second syringe,
The spinning liquid of the third another side is added in third syringe, by high voltage electrostatic field, can single step be effectively prepared
The structure nano fiber of three-level arrangement out.
Further, the method for the structure nano fiber of above-mentioned preparation three-level arrangement, includes the following steps:
1) the step of preparation spinning solution, the first spinning solution be mass percent concentration be 13%Eudragit L100 and
The ethanol solution of 2% phosphotungstic acid；Second spinning solution is that mass percent concentration is 13%Eudragit E100 and 1% nano-silica
Change the alcohol suspension of titanium；Third spinning solution is the Eudragit L100 ethanol solution that mass percent concentration is 13%；
2) resulting first, second, and third spinning solution of step (1) is added separately in corresponding syringe, is then turned on
First syringe pump, the second syringe pump and third syringe pump；
3) the sheath flow quantity for controlling the first syringe is 1.5 ml/h, the core flow quantity point of control second and third syringe
Not Wei 0.5 and 0.3 ml/h open high pressure generator, adjustment fiberboard receive distance be 15 cm, by voltage be upgraded to 14kV carry out
The structure nano fiber that electrospinning arranges to get three-level.
The principle of the present invention is: the specific structural features of the microfluidic control spray head of three-level arrangement are to prepare corresponding construction to receive
Rice material provides a macroscopical template, high-pressure electrostatic off field, by the interaction of high-voltage electrostatic field and fluid, at several milliseconds
Within liquid spinning dope is drawn into solid nano fiber clear in structure.On the other hand, the fluid of spray outlet three-level arrangement
An ellipse complete curve closing structure is formed under high voltage electric field, on the one hand this closing structure is conducive to high voltage electric field pair
On the other hand the uniform synchro-draw of three kinds of fluids keeps having enough contacts area between three kinds of fluids of arrangement, effectively
It prevents from separating caused by " identical charges repel each other " between fluid.Above-mentioned principle collective effect, it is ensured that high-pressure electrostatic off field, from macroscopic view
Accurate " duplication " of the template to microcosmic three-level arrangement architecture feature nanofiber.
The present invention is compared with prior art, and technological progress is significant.The high-pressure electrostatic of three-level arrangement of the invention is spun
Silk method application is simple and convenient to operate, is easily controllable, can be effectively prepared out the knot of three-level arrangement with single step under high voltage electric field
Structure nanofiber, and extensive amplification production can be carried out by increasing spinneret quantity.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the microfluid electric injector of three-level arrangement of the invention, the total capillary of 1-, 2- first
Tortuous capillary, the second tortuous capillary of 3-, 4- connector, 5- bulge loop, 6- epoxy resin.
Fig. 2 is a kind of outlet shooting figure of the microfluid electric injector of three-level arrangement of the invention.
Fig. 3 is the structural schematic diagram of more jet stream electric spinning equipments of the microfluid electric injector arranged containing three-level of the invention,
The microfluid EFI that 7- high pressure generator, the first syringe pump of 8-, the second syringe pump of 9-, 10- third syringe pump, 11- three-level arrange
Head, 12- fiber receiver board, the first syringe of 13-, the second syringe of 14-, 15- third syringe, 16- the first high resiliency silica gel
Hose；17- the second high resiliency silica gel hose.
Fig. 4 is the electricity using the structure nano fiber of the microfluid electric injector electric spinning equipment preparation three-level arrangement of three-level arrangement
Spinning process shooting figure；
Fig. 5 is the structure nano fiber scanning electron microscope electron microscope of the arrangement of three-level obtained by Application Example；
Fig. 6 is the structure nano fiber transmission electron microscope electron microscope of the arrangement of three-level obtained by Application Example.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
As shown in Figure 1, the present invention provides a kind of microfluidic control spray head of three-level arrangement, including a total capillary 1,
First tortuous capillary 2 and the second tortuous capillary 3.
The section of 1 outlet end of total capillary is ellipse；First tortuous capillary 2 includes one first
Straightway and first bending part, the first straight line section are arranged in total capillary 1, the first straight line
The lateral wall of section is close to an inner sidewall of total capillary 1, and institute is stretched out in the outlet end of first tortuous capillary 2
The bending part of the outlet end for the total capillary 1 stated, first tortuous capillary 2 is worn from the side of total capillary 1
Out；
Second tortuous capillary 3 includes a second straight line section and second bending part, and described second is straight
Line segment is arranged in total capillary 1, in addition the lateral wall of the second straight line section is close to total capillary 1
The inner sidewall of side, the outlet end of total capillary 1 is stretched out in the outlet end of second tortuous capillary 3, described
The bending part of second tortuous capillary 3 is pierced by from the side of total capillary 1, the first straight line section and described
There is gap between two straightways.
Further, the outlet end of first tortuous capillary 2 is concordant with the outlet end of total capillary 1,
The outlet end of second tortuous capillary 3 is concordant with the outlet end of the first tortuous capillary 1.
Further, the length of total capillary 1 is 70 mm, and the input end of total capillary 1 is provided with one
A interface 4 is provided with spiral reinforcing rib, the length of first tortuous capillary 2 on the lateral wall of the interface 4
For 55 mm；The length of second tortuous capillary 3 is 55 mm；Total capillary 1,2 and of the first tortuous capillary
Second tortuous capillary 3 and 4 place of being linked of interface are all made of 6 adhesive sealing of epoxy resin.
Further, on the lateral wall of the bending part tail end of first tortuous capillary 2 and the second tortuous capillary 3
It is provided with the protrusion 5 of annular.
Embodiment 2
A kind of high-voltage electrostatic spinning device of application spray head assembling, composition schematic diagram is as shown in figure 3,7- high pressure
Raw device, the first syringe pump of 8-, the second syringe pump of 9-, 10- third syringe pump, the microfluid electric injector of 11- three-level arrangement, 12- are fine
Tie up receiver board, the first syringe of 13-, the second syringe of 14-, 15- third syringe, 16- the first high resiliency silica gel hose；17-
Second high resiliency silica gel hose.
Electrospinning preparation, tool are implemented to three fluid streams using the electric spinning equipment of the microfluidic control spray head with three-level arrangement
Steps are as follows for body: the first syringe 13 is mounted in the first syringe pump 8, and the first spinning liquid is added in syringe 13, injection
Device 13 is directly connected to the interface end of the microfluidic control spray head 11 of three-level arrangement.Second syringe 14 is mounted on the second syringe pump 9
It is interior, the second spinning suspension is added in syringe 9, spinning liquid imports three-level arrangement by the first high resiliency silica gel hose 16
Microfluidic control spray head 11 tortuous capillary 2 in.Third syringe 15 is mounted in third syringe pump 10, in syringe 15
Middle addition third spinning liquid, spinning liquid import the microfluidic control spray of three-level arrangement by the second high resiliency silica gel hose 17
In first 11 tortuous capillary 3.High pressure generator 7 and the microfluidic control spray head 11 of three-level arrangement are directly connected to by conducting wire,
11 lower end of spray head is provided with a fiber receiver board 12, receiving distance is 15 cm, receives the cardboard that plate 12 is aluminium foil package
Plate, this receives plate earthing.
Application Example 1
Using a kind of high-voltage electrostatic spinning device implementation electrospinning of application spray head assembling as described in example 2, with preparation
The structure nano fiber of three-level arrangement, steps are as follows:
(1), the preparation of spinning solution
First spinning solution, mass percent concentration are the ethanol solution of 13%Eudragit L100 and 2% phosphotungstic acid, are matched
Method processed is as follows: the phosphotungstic acid of the Eudragit E100 of 13 g and 2 g being added in the ethyl alcohol of 75 g, is stirred evenly i.e.
Obtain the ethanol solution of Eudragit E100 and 4% phosphotungstic acid that mass percent concentration is 13%；
Second spinning solution, mass percent concentration is 13%Eudragit E100 and the ethyl alcohol of 1% nano-titanium dioxide is outstanding
Supernatant liquid；Its preparation method is as follows: the Eudragit E100 of 13 g and 1 nano-titanium dioxide are added to the ethyl alcohol of 76 g
In, stir evenly the alcohol suspension up to mass percent concentration for 13%Eudragit E100 and 1% nano-titanium dioxide；
Third spinning solution, the Eudragit L100 ethanol solution that mass percent concentration is 13%, preparation method are as follows:
The Eudragit E100 of 13 g is added in the ethyl alcohol of 77 g, stirring evenly up to mass percent concentration is 13%
The alcohol suspension of Eudragit E100；
4) resulting first, second, and third spinning solution of step (1) is added separately in corresponding syringe, is then turned on
First syringe pump, the second syringe pump and third syringe pump；
5) flow of the first syringe is controlled as 1.5 ml/h, and the core flow quantity of control second and third syringe is respectively
0.5 and 0.3 ml/h opens high pressure generator, and it is 15 cm that adjustment fiberboard, which receives distance, and voltage is upgraded to 14kV and carries out electrospinning,
Up to the structure nano fiber of three-level arrangement.
Application Example 2
Surface metal spraying is carried out to the structure nano fiber that three-level prepared by Application Example 1 arranges using field scan Electronic Speculum
After observe, as a result as shown in Figure 5.The structure nano fiber of prepared three-level arrangement is collected uniformly and good linear shape is presented
State, diameter are 710 ± 130 nm.The structure nano arranged using high resolution transmission electron microscopy prepared three-level is fine
Dimension is observed, and as a result as shown in fig. 6, the structure that arrange of the left, center, right three-level of nanofiber is clear in structure, left side is because of containing
Nano-titanium dioxide and it is different from right side, it is intermediate because bigger gray scale is presented containing developer phosphotungstic acid.
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, without departing from the technical principles of the invention, several improvement can also be made, these improvement also should be regarded as this
The protection scope of invention.
Claims (6)
1. a kind of microfluidic control spray head of three-level arrangement, it is characterised in that: including total capillary, first tortuous capillary
With the second tortuous capillary；The section at total capillary outlet end is ellipse, and first tortuous capillary includes
One first straight line section and first bending part, the first straight line section is arranged in total capillary, described
The lateral wall of first straight line section is close to an inner sidewall of total capillary, the outlet end of first tortuous capillary
Concordant with the outlet end of total capillary, the first bending part of first tortuous capillary is from total capillary
Side be pierced by；Second tortuous capillary include a second straight line section and second bending part, described second
Straightway is arranged in total capillary, in addition the lateral wall of the second straight line section is close to total capillary
The inner sidewall of side, the outlet end of second tortuous capillary is concordant with the outlet end of the first tortuous capillary,
Second bending part of second tortuous capillary is pierced by from the side of total capillary, the first straight line section and
There is gap between the second straight line section.
2. a kind of microfluidic control spray head of three-level arrangement according to claim 1, it is characterised in that: total capillary
The length of pipe is 70 mm, and the input end of total capillary is provided with an interface, is arranged on the lateral wall of the interface
There is spiral reinforcing rib, the length of first tortuous capillary is 55 mm；The length of second tortuous capillary
For 55 mm；First tortuous capillary and the second tortuous capillary are inserted into total capillary place and use epoxy resin gluing
Sealing.
3. a kind of microfluidic control spray head of three-level arrangement according to claim 1, it is characterised in that: described first is curved
The protrusion of annular is provided on the lateral wall of the bending part tail end of bent capillary and the second tortuous capillary.
4. 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, third syringe pump, third syringe, fiber receiver board, high pressure generator and three-level described in claim 1 arrangement
Microfluidic control spray head, first syringe is mounted in first syringe pump, first syringe and
The microfluidic control spray head connection, second syringe are mounted in second syringe pump, and described second
The syringe microfluidic control spray head described by the connection of silica gel hose, the third syringe are mounted on described the
In three syringe pumps, the third syringe microfluidic control spray head described by second silica gel hose connection is described
High pressure generator is connected with the microfluidic control spray head by conducting wire, and the lower end of the microfluidic control spray head is provided with
Fiber receiver board.
5. the method for the structure nano fiber using high-voltage electrostatic spinning device as claimed in claim 4 preparation three-level arrangement,
It is characterized by: the first spinning solution among the first arrangement is added in the first syringe, second is added in the second syringe
Second spinning solution on kind one side, the interior third spinning solution that the third another side is added of third syringe, is made by high-voltage electrostatic field
With, can single step be effectively prepared out three-level arrangement structure nano fiber.
6. the method for the structure nano fiber of preparation three-level arrangement as claimed in claim 5, it is characterised in that including walking as follows
It is rapid:
1) the step of preparation spinning solution, the first spinning solution are that mass percent concentration is 13%Eudragit L100 and 2% phosphorus
The ethanol solution of wolframic acid；Second spinning solution is that mass percent concentration is 13%Eudragit E100 and 1% nano-titanium dioxide
Alcohol suspension；Third spinning solution is the Eudragit L100 ethanol solution that mass percent concentration is 13%；
2) resulting first, second, and third spinning solution of step (1) is added separately in corresponding syringe, is then turned on first
Syringe pump, the second syringe pump and third syringe pump；
3) the sheath flow quantity of the first syringe is controlled as 1.5 ml/h, and the core flow quantity of control second and third syringe is respectively
0.5 and 0.3 ml/h opens high pressure generator, and adjustment fiber receiver board receives distance, and voltage is upgraded to 14kV and carries out electrospinning, i.e.,
Obtain the structure nano fiber of three-level arrangement.
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| CN201611121803.8A CN106757415B (en) | 2016-12-08 | 2016-12-08 | A kind of microfluidic control spray head, device for spinning and the spinning process of three-level arrangement |
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| CN201611121803.8A CN106757415B (en) | 2016-12-08 | 2016-12-08 | A kind of microfluidic control spray head, device for spinning and the spinning process of three-level arrangement |
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| CN109385694B (en) * | 2018-09-21 | 2020-02-14 | 华中科技大学 | Spiral graphene fiber and preparation method and application thereof |
| CN109518284B (en) * | 2018-11-26 | 2021-12-31 | 青岛大学 | Functional fiber, microfluidic spinning device thereof and fiber preparation method |
| CN112708949B (en) * | 2020-12-23 | 2022-07-22 | 广西大学 | Preparation method of high-strength nano cellulose fiber based on microfluid assembly |
| CN117230537B (en) * | 2023-11-13 | 2024-02-13 | 江苏新视界先进功能纤维创新中心有限公司 | Melt differential electrospinning core-shell nanofiber filament preparation device |
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| CN103966680A (en) * | 2014-05-04 | 2014-08-06 | 东华大学 | Method for preparing drug sustained release nanofibers |
| CN105926055B (en) * | 2016-06-23 | 2018-06-15 | 浙江大学 | The electrospinning process of regulation and control micro/nano-fibre configuration of surface in situ |
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