CN113151910A - Curved-edge dish-shaped electrostatic spinning device and using method thereof - Google Patents

Curved-edge dish-shaped electrostatic spinning device and using method thereof Download PDF

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CN113151910A
CN113151910A CN202110355602.9A CN202110355602A CN113151910A CN 113151910 A CN113151910 A CN 113151910A CN 202110355602 A CN202110355602 A CN 202110355602A CN 113151910 A CN113151910 A CN 113151910A
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curved
shaped
electrostatic spinning
dish
nano
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CN113151910B (en
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覃小红
周智勇
王黎明
权震震
张弘楠
王荣武
俞建勇
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Donghua University
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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

Abstract

The invention relates to a curved edge dish-shaped electrostatic spinning device and a using method thereof, belonging to the field of production and preparation of submicron fibers. The electrostatic spinning nozzle is in a curved edge dish shape and is in a container shape with an opening at one end, and the specific using method comprises the following steps: and filling the spinning solution in the spinning tank until the spinning solution is saturated, connecting a high voltage, and under a certain voltage, overcoming the surface tension of the spinning solution, continuously exciting the spinning solution along the edge of a nozzle on the liquid surface to form jet flow, and finally depositing the jet flow on a nano-micron fiber collecting device to obtain the nano-micron fibers. Through the electrostatic spinning nozzle, the problems of low yield, easy blockage and the like of the traditional single-needle electrostatic spinning are effectively solved, and compared with other needle-free electrostatic spinning devices, the electrostatic spinning nozzle can reduce the excitation voltage to a certain extent and provides guarantee for protecting equipment and personal safety of users.

Description

Curved-edge dish-shaped electrostatic spinning device and using method thereof
Technical Field
The invention relates to the technical field of electrostatic spinning, in particular to a curved-edge dish-shaped electrostatic spinning device and a using method thereof.
Background
Nanometer is a length measurement unit of 10-9When the size of the material is in the nanometer scale, the physical properties of the material are obviously changed due to the volume effect, the quantum size effect, the quantum tunneling effect and the dielectric confinement effect, so that some new properties are obtained. The nano-micron fiber has the characteristics of extremely large specific surface area, high porosity and the like, is widely concerned in the fields of high-efficiency filtration, biomedicine, safety protection, electronic devices and the like, and shows huge application and development potential. Currently, techniques for preparing nanofibers include template synthesis, drawing, solvent, chemical vapor deposition, gas-liquid-solid growth, self-assembly, and electrospinning. The electrostatic spinning method has the characteristics of relatively high efficiency in preparation, high process controllability, simple operation, simple equipment, continuous and stable production and the like, and shows great application value.
The electrostatic spinning equipment mainly comprises three parts, namely a high-voltage power supply device, a collecting device and a spinning device. The spinning device is a core component of the device, the traditional single-needle electrostatic spinning nozzle is similar to a medical injector, a certain amount of spinning solution is absorbed, a high voltage is connected to a needle tube of the spinning device, the collecting device is grounded, the spinning solution at the front end of the needle tube overcomes the surface tension of the spinning solution under the action of a high-voltage electric field, is stretched to form jet flow, and finally is split to form nano-micron fibers which are deposited on the collecting device. The deposition form of the composite material is generally disordered fiber net-shaped, isotropy is realized in the plane of a fiber membrane, and the mechanical property of the composite material is poor, so that the composite material becomes a factor for limiting the wide application of the composite material. However, another more important limiting factor is that the yield of the nano-micron fiber prepared by the traditional electrostatic spinning technology is extremely low, generally 0.1-1 g/h, and the large-scale production is difficult to realize.
In order to improve the productivity of electrospinning, multi-needle electrospinning and needle-free electrospinning have been proposed. However, for multi-needle electrostatic spinning, due to the electrostatic shielding effect, the field intensity distribution on different needles has obvious difference, which may cause needle blockage, and cause the problems of difficult normal continuous filament production in the spinning process, different fiber quality and the like. For the needle-free electrostatic spinning technology, the problems are just avoided, and meanwhile, another breakthrough in yield is realized.
At present, electrostatic spinning nanofiber batch preparation devices have some reports at home and abroad. Chinese patent 200710036447.4 discloses an air-jet electrostatic spinning device, which forms bubbles on the free liquid surface of a high polymer by introducing air into the bottom of a liquid tank, and the bubbles form taylor cones and multiple jet flows under the action of electric field force to improve the yield of nano fibers, but a plurality of bubble fragments with different shapes and sizes are stretched by the electric field force while the taylor cones formed by the bubbles on a mechanism are broken, so that the diameter distribution of the fibers is wider. The solvent on the free liquid surface of the larger high polymer is extremely easy to volatilize, and the spinning direction is limited; chinese patent 201310032194.9 discloses an umbrella-shaped electrostatic spinning nozzle and an electrostatic spinning method, which can realize mass production of nanofibers, but the free surface of the solution of the umbrella-shaped nozzle is in contact with the atmospheric environment, and the solvent is very volatile, so that the stability of spinning and the quality of the final nanofibers are seriously affected, and the spinning direction is limited; chinese patent 201510278266.7 discloses an air-jet assisted multi-needle electrostatic spinning device, which can improve the yield of nanofibers in unit time, the spinning direction is not limited, but there is a disadvantage that needles are easily blocked, and simultaneously, the arrangement of needles takes into account the mutual influence between electric fields after high-voltage static electricity is applied, so the design of the multi-needle electrostatic spinning device is more complicated and complex, and it is difficult to realize mass production of nanofiber products with narrow fiber diameter distribution.
Disclosure of Invention
The invention aims to solve the technical problem of providing a curved-edge disc-shaped electrostatic spinning device and a using method thereof, solving the problems of larger working voltage and poorer production continuity of the conventional needleless electrostatic spinning spray head, and continuously producing nano-micron fibers at lower voltage; meanwhile, the small-size spray head can be used for efficiently producing the nano-micron fibers in batches, the space utilization rate of the electrostatic spinning spray head is improved, and new possibility is provided for batch production of the nano-micron fibers by using multi-spray-head needle-free electrostatic spinning.
The technical scheme adopted by the invention for solving the technical problems is as follows: provides a curved edge dish-shaped electrostatic spinning device, which comprises a nano-micron fiber collecting device, a liquid supply system, a voltage supply system, a curved edge dish-shaped electrostatic spinning spray head, a lifting and traversing system and a control system, wherein the curved edge dish-shaped electrostatic spinning spray head is made of metal copper, the curved dish-shaped electrostatic spinning nozzle is of a cylindrical structure with an opening at one end, the curved dish-shaped electrostatic spinning nozzle comprises a bottom plate and a plurality of arc-shaped vertical plates, the plurality of arc-shaped vertical plates are enclosed into a ring shape, the bottom of the arc-shaped vertical plates is sealed by the bottom plate, the openings of the arc-shaped vertical plates are all arranged inwards, the center of the bottom plate is provided with a circular through hole, the round through hole is communicated with the liquid supply device, the curved edge dish-shaped electrostatic spinning spray head is arranged on the lifting and transverse moving system, the curved-edge dish-shaped electrostatic spinning nozzle is connected with a voltage supply system, and the nano-micron fiber collecting device is arranged above the curved-edge dish-shaped electrostatic spinning nozzle.
As a supplement to the technical scheme of the invention, the wall thickness of the curved dish-shaped electrostatic spinning nozzle is 0.1-1 mm, and the height is 10 mm.
As a supplement to the technical scheme of the invention, the lifting and traversing system realizes vertical lifting or traversing movement by manually screwing or adopting a stepping motor to drive a lead screw so as to adjust the relative position between the curved-edge disc-shaped electrostatic spinning spray head and the nano-micron fiber collecting device.
As a supplement to the technical scheme of the invention, the vertical lifting moving range of the lifting and transversely moving system is 1-10 mm, and the horizontal transversely moving range is +/-20 mm.
As a supplement to the technical scheme of the invention, the nano-micron fiber collecting device is a metal roller capable of realizing rotation speed adjustment, and is positioned right above the curved-edge dish-shaped electrostatic spinning nozzle, and one end of the metal roller is grounded by using a metal wire.
As a supplement to the technical scheme of the invention, the curved edge dish-shaped electrostatic spinning nozzle is connected with a power supply system through a metal wire, and the power supply system comprises a positive high-voltage direct-current power supply and a negative high-voltage direct-current power supply.
As a supplement to the technical scheme of the invention, the round through hole is communicated with the liquid supply device through an insulating conduit.
As a supplement to the technical scheme of the invention, the device also comprises a control system, and the control system is respectively connected with the nano-micron fiber collecting device, the liquid supply system, the voltage supply system and the lifting and traversing system. The liquid supply device is controlled by the control system to adjust the liquid supply speed and the liquid supply amount.
As a supplement to the technical scheme of the invention, a maximum virtual circle is drawn along the outlines of a plurality of arc-shaped vertical plates, and the diameter of the virtual circle and the outer diameter of the arc-shaped vertical plates satisfy the following formula:
Figure BDA0003003651770000031
wherein n is the arc riser quantity, and R is the radius of arc riser outline, and R is the radius of virtual circle.
As a supplement to the technical scheme of the invention, the application method of the curved dish-shaped electrostatic spinning device comprises the following steps:
step 1: adjusting the working distance from the working surface of the curved-edge dish-shaped electrostatic spinning nozzle to the lower surface of the metal roller through a lifting and transverse moving system;
step 2: adding spinning solution into a curved dish-shaped electrostatic spinning nozzle until the liquid level is basically saturated;
and step 3: setting a liquid supply rate, a transverse moving rate of the lifting and transverse moving system and a transverse moving range on the control system;
and 4, step 4: turning on a power supply of the nano-micron fiber collecting device, setting the rotating speed of the metal roller, and turning on a working switch of the metal roller;
and 5: turning on a power switch of a voltage supply system, and setting a high-voltage power supply to be the required spinning voltage;
step 6: generating a large number of jet flows along the edge of the inner wall of the arc-shaped vertical plate, wherein the jet flows towards the metal roller, then the jet flows are split into nano-micron fibers, and finally the nano-micron fibers are deposited on the metal roller;
and 7: the shutdown operation, firstly, the voltage parameter of the high-voltage power supply is adjusted to be 0, the power supply of the voltage supply system is closed, the rotating speed of the roller is adjusted to be 0, and the power supply of the nano-micron fiber collecting device is closed;
and 8: obtaining the nano-micron fiber membrane.
Has the advantages that: the invention relates to a curved-edge dish-shaped electrostatic spinning device and a using method thereof, which effectively avoid the problems of electrostatic shielding, needle blockage and the like which can occur in the needle type electrostatic spinning process, and a curved-edge dish-shaped spray head is convenient to clean, replace and process, thereby obviously reducing the voltage required by electrostatic spinning, greatly improving the yield of electrostatic spinning nano-micron fibers, and obtaining the fibers with thinner fineness and better uniformity.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic structural view of a curved-edge dish-shaped electrospinning spray head according to the present invention;
FIG. 3 is a schematic diagram of the relationship between parameters of the curved dish-shaped electrospinning nozzle according to the present invention.
The figure is as follows: 1. the device comprises a nano-micron fiber collecting device, a liquid supply system, a voltage supply system, a curved-edge dish-shaped electrostatic spinning spray head, a lifting and transverse moving system, a liquid supply system, a curved-edge dish-shaped electrostatic spinning spray head, a lifting and transverse moving system, a liquid supply system, an insulating guide pipe, a liquid supply system, a liquid supply.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The embodiment of the invention relates to a curved-edge dish-shaped electrostatic spinning device and a using method thereof, as shown in figures 1-3, the curved-edge dish-shaped electrostatic spinning device comprises a nano-micron fiber collecting device 1, a liquid supply system 2, a voltage supply system 3, a curved-edge dish-shaped electrostatic spinning spray head 4, a lifting and traversing system 5 and a control system, wherein the curved-edge dish-shaped electrostatic spinning spray head 4 is made of metal copper, the curved-edge dish-shaped electrostatic spinning spray head 4 is of a cylindrical structure with an open end, the curved-edge dish-shaped electrostatic spinning spray head 4 comprises a bottom plate 10 and a plurality of arc-shaped vertical plates 11, the plurality of arc-shaped vertical plates 11 are enclosed into a ring shape, the bottom of each arc-shaped vertical plate 11 is sealed by the bottom plate 10, each arc-shaped vertical plate 11 is similar to a petal, the plurality of arc-shaped vertical plates 11 form the shape of a whole flower, the openings of the arc-shaped vertical plates 11 are all arranged inwards, the center of the bottom plate 10 is provided with a circular through hole 9, the round through hole 9 is communicated with the liquid supply device 2, the curved dish-shaped electrostatic spinning nozzle 4 is arranged on the lifting and transverse moving system 5, the curved dish-shaped electrostatic spinning nozzle 4 is connected with the voltage supply system 3, and the nano-micron fiber collection device 1 is arranged above the curved dish-shaped electrostatic spinning nozzle 4.
The wall thickness of the curved dish-shaped electrostatic spinning spray head 4 is 0.1-1 mm, and the height is 10 mm.
The lifting and transverse moving system 5 realizes vertical lifting or transverse moving by manually screwing or adopting a stepping motor to drive a screw rod so as to adjust the relative position between the curved-edge disc-shaped electrostatic spinning nozzle 4 and the nano-micron fiber collecting device 1.
The vertical lifting moving range of the lifting and transverse moving system 5 is 1-10 mm, and the horizontal transverse moving range is +/-20 mm.
The nano-micron fiber collecting device 1 is a metal roller capable of realizing rotation speed adjustment, and is positioned right above the curved-edge disc-shaped electrostatic spinning nozzle 4, and one end of the metal roller is grounded by using a metal wire.
The curved edge dish-shaped electrostatic spinning nozzle 4 is connected with a power supply system 3 through a metal wire 7, and the power supply system 3 comprises a positive high-voltage direct-current power supply and a negative high-voltage direct-current power supply.
The round through hole 9 is communicated with the liquid supply device 2 through an insulating conduit 6.
The device also comprises a control system, and the control system is respectively connected with the nano-micron fiber collecting device 1, the liquid supply system 2, the voltage supply system 3 and the lifting and traversing system 5. The liquid supply device 2 is controlled by a control system to adjust the liquid supply speed and the liquid supply amount.
Draw the biggest virtual circle along the profile of a plurality of arc riser 11, the diameter of virtual circle and the external diameter of arc riser 11 satisfy the following formula:
Figure BDA0003003651770000051
wherein n is the quantity of arc riser 11, and R is the radius of arc riser 11 outline, and R is the radius of virtual circle. This can be better understood with reference to fig. 3.
A use method of a curved-edge dish-shaped electrostatic spinning device comprises the following steps:
step 1: the working distance from the working surface of the curved dish-shaped electrostatic spinning nozzle 4 to the lower surface of the metal roller is adjusted through the lifting and transverse moving system 5;
step 2: adding spinning solution into the curved dish-shaped electrostatic spinning nozzle 4 until the liquid level is basically saturated;
and step 3: the control system is provided with a liquid supply speed, a transverse moving speed and a transverse moving range of the lifting and transverse moving system 5;
and 4, step 4: turning on a power supply of the nano-micron fiber collecting device 1, setting the rotating speed of the metal roller, and turning on a working switch of the metal roller;
and 5: turning on a power switch of a voltage supply system 3, and setting a high-voltage power supply to be the required spinning voltage;
step 6: a large number of jet flows 8 are generated along the edge of the inner wall of the arc-shaped vertical plate 11, the jet flows 8 move towards the metal roller, then are split into nano-micron fibers, and finally are deposited on the metal roller;
and 7: the shutdown operation, firstly adjusting the voltage parameter of the high-voltage power supply to be 0, closing the power supply of the voltage supply system, adjusting the rotating speed of the roller to be 0, and closing the power supply of the nano-micron fiber collecting device 1;
and 8: obtaining the nano-micron fiber membrane.
Preparing a spinning solution: the curved edge disc-shaped nozzle is utilized to produce polyacrylonitrile submicron fiber, a certain amount of polyacrylonitrile is taken and dissolved in N-N dimethylformamide solution, and spinning solution with the mass fraction of 12 wt% is prepared.
Experiment: adjusting the collecting distance from the working surface of the curved-edge dish-shaped spray head to the roller to be 18 cm; pouring the spinning solution into a curved edge dish-shaped nozzle until the liquid level is basically saturated; setting the liquid supply rate to be 20ml/h, the transverse moving rate to be 20cm/min and the transverse moving range to be +/-15 cm on a control system; turning on a power supply of the collecting device, and setting the rotating speed of the roller to be 750 r/min; turning on a roller switch, adjusting the parameters of a high-voltage power supply to be set to 30 KV; generating a plurality of jet flows along the curved dish-shaped edge, wherein the jet flows to the collecting device; a large amount of nano-micron fibers can be obtained on the collecting device, and the product is in a film shape on the macro scale.

Claims (10)

1. The utility model provides a curved edge dish-shaped electrostatic spinning device which characterized in that: comprises a nano-micron fiber collecting device (1), a liquid supply system (2), a voltage supply system (3), a curved-edge disc-shaped electrostatic spinning nozzle (4), a lifting and traversing system (5) and a control system, wherein the curved-edge disc-shaped electrostatic spinning nozzle (4) is made of metal copper, the curved-edge disc-shaped electrostatic spinning nozzle (4) is of a cylindrical structure with one open end, the curved-edge disc-shaped electrostatic spinning nozzle (4) comprises a bottom plate (10) and a plurality of arc-shaped vertical plates (11), the plurality of arc-shaped vertical plates (11) are encircled into a ring shape, the bottom of the arc-shaped vertical plates (11) is sealed by the bottom plate (10), openings of the arc-shaped vertical plates (11) are all arranged inwards, a circular through hole (9) is formed in the center of the bottom plate (10), the circular through hole (9) is communicated with the liquid supply device (2), and the curved-edge disc-shaped electrostatic spinning nozzle (4) is installed on the lifting and traversing system (5), the curved-edge dish-shaped electrostatic spinning nozzle (4) is connected with a voltage supply system (3), and the nano-micron fiber collecting device (1) is arranged above the curved-edge dish-shaped electrostatic spinning nozzle (4).
2. The curved dish-shaped electrospinning device of claim 1, wherein: the wall thickness of the curved dish-shaped electrostatic spinning spray head (4) is 0.1-1 mm, and the height is 10 mm.
3. The curved dish-shaped electrospinning device of claim 1, wherein: the lifting and transverse moving system (5) realizes vertical lifting or transverse moving by manually screwing or adopting a stepping motor to drive a screw rod so as to adjust the relative position between the curved-edge dish-shaped electrostatic spinning spray head (4) and the nano-micron fiber collecting device (1).
4. The curved dish-shaped electrospinning device of claim 1, wherein: the vertical lifting moving range of the lifting and transverse moving system (5) is 1-10 mm, and the horizontal transverse moving range is +/-20 mm.
5. The curved dish-shaped electrospinning device of claim 1, wherein: the nano-micron fiber collecting device (1) is a metal roller capable of realizing rotation speed adjustment, and is positioned right above the curved-edge dish-shaped electrostatic spinning nozzle (4), and one end of the metal roller is grounded by using a metal wire.
6. The curved dish-shaped electrospinning device of claim 1, wherein: the curved edge dish-shaped electrostatic spinning nozzle (4) is connected with a power supply system (3) through a metal wire (7), and the power supply system (3) comprises a positive high-voltage direct-current power supply and a negative high-voltage direct-current power supply.
7. The curved dish-shaped electrospinning device of claim 1, wherein: the round through hole (9) is communicated with the liquid supply device (2) through an insulating conduit (6).
8. The curved dish-shaped electrospinning device of claim 1, wherein: the device also comprises a control system, wherein the control system is respectively connected with the nano-micron fiber collecting device (1), the liquid supply system (2), the voltage supply system (3) and the lifting and transverse moving system (5).
9. The curved dish-shaped static electricity of claim 1Spinning device, its characterized in that: drawing a maximum virtual circle along the outlines of the arc-shaped vertical plates (11), wherein the diameter of the virtual circle and the outer diameter of the arc-shaped vertical plates (11) satisfy the following formula:
Figure FDA0003003651760000021
(wherein, n is the number of the arc vertical plates (11), R is the radius of the outer contour of the arc vertical plates (11), and R is the radius of the virtual circle).
10. The use method of the curved dish-shaped electrospinning device according to claim 1, comprising the steps of:
step 1: the working distance from the working surface of the curved dish-shaped electrostatic spinning nozzle (4) to the lower surface of the metal roller is adjusted through the lifting and transverse moving system (5);
step 2: adding spinning solution into the curved dish-shaped electrostatic spinning nozzle (4) until the liquid level is basically saturated;
and step 3: the control system is provided with a liquid supply speed, a transverse moving speed and a transverse moving range of the lifting and transverse moving system (5);
and 4, step 4: turning on a power supply of the nano-micron fiber collecting device (1), setting the rotating speed of the metal roller, and turning on a working switch of the metal roller;
and 5: a power switch of the voltage supply system (3) is turned on, and a high-voltage power supply is set to be the required spinning voltage;
step 6: a large number of jet flows (8) are generated along the edge of the inner wall of the arc-shaped vertical plate (11), the jet flows (8) move towards the metal roller, then are split into nano-micron fibers, and finally are deposited on the metal roller;
and 7: the shutdown operation is that firstly, the voltage parameter of the high-voltage power supply is adjusted to be 0, the power supply of the voltage supply system is closed, the rotating speed of the roller is adjusted to be 0, and the power supply of the nano-micron fiber collecting device (1) is closed;
and 8: obtaining the nano-micron fiber membrane.
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EP3491178A1 (en) * 2017-01-06 2019-06-05 SABIC Global Technologies B.V. Apparatus for continuous needleless electrospinning a nanoscale or submicron scale polymer fiber web onto a substrate
CN110670155A (en) * 2019-09-20 2020-01-10 上海松冒实业有限公司 Petal-shaped nanofiber production device and method
CN111058102A (en) * 2020-01-03 2020-04-24 西安工程大学 Disc-shaped needle-free electrostatic spinning device and working method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103451749A (en) * 2012-05-30 2013-12-18 湖南博弈飞装备新材料研究所 Continuous electrostatic spinning system and method for preparing fine fibers
JP3184886U (en) * 2013-03-21 2013-07-25 國興 李 Screw fiber generator and electrostatic rod spinning equipment
CN103290493A (en) * 2013-06-24 2013-09-11 苏州大学 Electrostatic spinning device and method for mass nanometer/micrometer fibers
CN203583025U (en) * 2013-12-05 2014-05-07 厦门大学 Electrostatic spinning device
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CN111058102A (en) * 2020-01-03 2020-04-24 西安工程大学 Disc-shaped needle-free electrostatic spinning device and working method thereof

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