CN108411383B - Porous spherical electrostatic spinning nozzle and spinning method thereof - Google Patents
Porous spherical electrostatic spinning nozzle and spinning method thereof Download PDFInfo
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- CN108411383B CN108411383B CN201810375614.6A CN201810375614A CN108411383B CN 108411383 B CN108411383 B CN 108411383B CN 201810375614 A CN201810375614 A CN 201810375614A CN 108411383 B CN108411383 B CN 108411383B
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- porous spherical
- electrostatic spinning
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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
-
- 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
Abstract
The invention discloses a porous spherical electrostatic spinning nozzle and a spinning method thereof. The porous spherical electrostatic spinning nozzle is a solid sphere with a smooth surface, and a plurality of holes are distributed on the spherical surface of the porous spherical electrostatic spinning nozzle; the porous spherical electrostatic spinning nozzle is connected with the motor I through the transmission shaft, and the lower part of the porous spherical electrostatic spinning nozzle is immersed in the spinning solution in the liquid storage tank. The spinning method comprises the following steps: opening the receiving device; opening the liquid supply device, and injecting the spinning solution into the liquid storage tank through a peristaltic pump; turning on a first motor to enable the porous spherical electrostatic spinning nozzle to rotate in the spinning solution, and enabling the spinning solution to form liquid films in two states on the spherical surface and the hole surface respectively; and opening the high-pressure generator to enable the liquid films on the spherical surface and the hole surface to respectively generate jet flows with different fineness, and stretching, solidifying and depositing the jet flows on the receiving device to form the nano fibers. The invention can prepare the nano-fiber with two or more diameter distributions without using various spinning solutions and adjusting spinning parameters.
Description
Technical Field
The invention relates to a porous spherical electrostatic spinning nozzle and a spinning method thereof, belonging to the technical field of nano fibers and textile machinery.
Background
A series of surprising properties occur when polymer fiber diameters are reduced from the micrometer scale to the submicrometer scale or the nanometer scale. Such as very large volume specific surface area, the volume specific surface area of nanofibers is substantially 1000 times that of microfibers; surface functionalization can be flexibly performed; compared with other known material forms, the material shows excellent effects and mechanical properties, such as surface and interface effects, small-size effects, quantum tunneling effects, rigidity, tensile strength and the like. These outstanding properties make nanofibers the first choice for many important applications, with great potential for development in the fields of high efficiency filtration, biomedical applications, intelligent sensing, etc. Considering the feasibility of operation, stability and controllability (including fiber diameter and distribution), material range, time consumption, etc., electrostatic spinning technology becomes the only method capable of producing continuous polymer nanofibers. With the rise and rapid development of the science of the nano materials, the preparation of the nano fibers by using the electrostatic spinning method becomes a research hotspot of the engineering material science community.
The traditional single-needle electrostatic spinning device is simple and mainly comprises a high-voltage power supply system, a liquid supply system and a collection system. The liquid supply system comprises a micro-injection pump, a medical needle tube and a plain end metal needle head, the flow of the high polymer solution is controlled by the micro-injection pump, the anode of the high-voltage power supply is connected with the plain end metal needle head, and the collection system is a metal flat plate and is grounded. High voltage power supply voltage crescent, the liquid drop of metal syringe needle forms the taylor awl gradually, and when high voltage power supply voltage further increases, the electric field force can overcome effects such as surface tension, the viscous force of high polymer solution and can appear whip phenomenon and reach ground connection metal collection board after forming tiny sharp efflux, and at this in-process, the solvent volatilizees, and the high polymer solidification forms the nanofiber deposit on metal collection board.
The yield of the nanofiber obtained by the traditional electrostatic spinning device is very low, the requirement of the nanofiber in the process of large-scale application is difficult to meet, the problem that the needle head of the single-needle electrostatic spinning device is easy to block exists, and the smooth operation of the nanofiber spinning process can be seriously influenced.
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, the solvent is very volatile, so that the stability of spinning and the quality of the final nanofibers are affected, and the curvature of the solution at the edge of the free liquid level is not adjustable; 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 the shortcoming that needles are easily blocked, and simultaneously, the arrangement mode of needles takes into account the mutual influence between the electric fields after applying high-voltage static electricity, so the design of the multi-needle electrostatic spinning device is more tedious and complicated, and it is difficult to realize mass production of nanofiber products with controllable fiber diameter distribution.
The inventor also discloses a series of batch electrostatic spinning devices, which comprise ZL 201710684508.1 electrostatic spinning devices with dynamically controlled spinning solution curvature and use methods thereof, ZL 201710044752.1 spiral groove-shaped electrostatic spinning devices with spiral grooves and use methods thereof, ZL 201710044800.7 annular rotary brush type electrostatic spinning devices with annular rotary brushes and use methods thereof, ZL 201710046822.7 spherical rotary brush type electrostatic spinning devices with annular rotary brushes and use methods thereof, ZL 201610629977.9 linear groove-shaped needle-free electrostatic spinning devices with annular slots and spinning methods thereof, ZL 201610296863.7 double-annular slot-shaped electrostatic spinning devices with annular slots and methods thereof, ZL 201510831359.8 sawtooth-shaped annular needle-free electrostatic spinning devices with annular slots and use methods thereof, and the like, wherein the patents are based on regulation and optimization of single diameter distribution of nanofibers. In many applications of filtration, energy, sensing, biomedicine and the like which are concerned in academia and industry, the electrostatic spinning nanofiber aggregate structure can be finely regulated and controlled to further improve the product performance, and meanwhile, the batch preparation of the electrostatic spinning nanofiber aggregate structure is very important.
Disclosure of Invention
The invention aims to solve the technical problem of providing a porous spherical electrostatic spinning spray head and a using method thereof, solves the problems of uncontrollable fiber multistage diameter distribution and single nanofiber membrane structure in the existing batch electrostatic spinning process, and realizes one-step batch preparation of controllable multistage diameter distribution nanofibers.
The technical scheme adopted by the invention for solving the technical problems is as follows: the porous spherical electrostatic spinning spray head is characterized in that the porous spherical electrostatic spinning spray head is a solid sphere with a smooth surface, and a plurality of holes are distributed on the spherical surface of the porous spherical electrostatic spinning spray head; the porous spherical electrostatic spinning nozzle is connected with the motor I through a transmission shaft, the lower part of the porous spherical electrostatic spinning nozzle is immersed in the spinning solution in the liquid storage tank, the spinning solution is connected with the anode of the high-voltage generator, and the liquid supply device is communicated with the bottom of the liquid storage tank through a peristaltic pump; a receiving device is arranged above the porous spherical electrostatic spinning nozzle.
Preferably, the solid sphere is made of copper or stainless steel, and the diameter of the solid sphere is 30-200 mm.
Preferably, the holes are uniformly and symmetrically distributed on the spherical surface, the number of the holes is 1-1000, the diameter of the holes is 1-10 mm, and the depth of the holes is 1-30 mm.
Preferably, the hole is a chamfer structure extending towards the outer edge at the spherical surface, and the depth of the chamfer structure is 0-10 mm.
Preferably, the material of the reservoir is polytetrafluoroethylene.
Preferably, the voltage regulation range of the high voltage generator is 0-120 kV.
Preferably, the drive shaft is arranged coaxially with the diameter of the solid sphere.
Preferably, the rotating speed of the first motor is 0-15 r/min.
Preferably, the receiving device comprises a metal roller with a second motor, and the metal roller is grounded or connected with the negative pole of the high-voltage generator.
More preferably, the diameter of the metal roller is 100-1200 mm, and the rotating speed of the second motor is 0-120 r/min.
The invention also provides an electrostatic spinning method, which is characterized in that the porous spherical electrostatic spinning nozzle is adopted, and the method comprises the following steps:
step 1): adjusting the distance between the receiving device and the porous spherical electrostatic spinning nozzle, and opening the receiving device;
step 2): opening the liquid supply device, and injecting the spinning solution into the liquid storage tank through a peristaltic pump;
step 3): turning on a first motor, setting the rotating speed, and enabling the porous spherical electrostatic spinning nozzle to rotate in the spinning solution, wherein the spinning solution forms liquid films in two states on the spherical surface and the hole surface respectively;
step 4): and opening the high-voltage generator, slowly increasing the voltage to the required spinning voltage to enable the liquid films on the surfaces of the spherical surface and the hole to respectively generate a first jet flow and a second jet flow with different fineness, wherein the jet flows fly to the receiving device under the action of a high-voltage electrostatic field, and after the solvent is volatilized, the jet flows are stretched, solidified and deposited on the receiving device to form the nano fibers.
The porous spherical electrostatic spinning nozzle provided by the invention can realize that the high polymer spinning solution simultaneously forms two spinning solution film states on the surface of the nozzle, one is a liquid film formed on the surface of a spherical hole, and the other is a liquid film distributed on the spherical surface. The method further realizes the multi-jet distribution regulation and control of the surface of the spray head and the controllable regulation and control of the multi-stage distribution of the diameters of the nanofibers, and then realizes the one-step batch production of the nanofibers with controllable multi-stage diameter distribution.
Drawings
FIG. 1 is a schematic view of a porous spherical electrostatic spinning nozzle provided by the present invention during spinning;
FIG. 2 is a schematic structural view of a porous spherical electrospinning nozzle;
fig. 3 is a perspective view of a porous spherical electrospinning spray head.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
As shown in fig. 1-3, the porous spherical electrospinning nozzle used in examples 1-3 is a solid sphere with a smooth surface, and the material of the core sphere is copper or stainless steel, and the diameter of the core sphere is 30-200 mm; a plurality of holes 13 are distributed on the spherical surface 12; the holes 13 are uniformly and symmetrically distributed on the spherical surface 12, the number of the holes 13 is 1-1000, the diameter of the holes is 1-10 mm, and the depth of the holes is 1-30 mm. The hole 13 is a chamfer structure extending towards the outer edge at the spherical surface 12, and the depth of the chamfer structure is 0-10 mm. The porous spherical electrostatic spinning nozzle 5 is connected with a first motor 3 through an insulated transmission shaft 4 (the rotating speed of the first motor 3 is 0-15 r/min), and the transmission shaft 4 and the diameter of the solid sphere are coaxially arranged. The lower part of the porous spherical electrostatic spinning nozzle 5 is immersed in the spinning solution 14 in the liquid storage tank 2, the spinning solution 14 is connected with the anode of the high-voltage generator 1, and the liquid supply device 16 is communicated with the bottom of the liquid storage tank 2 through the peristaltic pump 15; a receiving device is arranged above the porous spherical electrostatic spinning nozzle 5. The liquid storage tank 2 is made of polytetrafluoroethylene. The voltage regulation range of the high voltage generator 1 is 0-120 kV. The receiving device comprises a metal roller 7 with a second motor 6, and the metal roller 7 is grounded 9 or connected with the negative pole of the high-voltage generator 1. The diameter of the metal roller 7 is 100-1200 mm, and the rotating speed of the second motor 6 is 0-120 r/min.
Example 1
An electrostatic spinning method comprises the following steps:
the spinning solution 14 is a polymer solution prepared from Polyacrylonitrile (PAN) and N-N Dimethylformamide (DMF) to prepare the nanofiber with controllable multistage diameter distribution. The mass fraction of the prepared PAN high polymer solution is 10 percent.
Selecting a spray head with the diameter of 60 mm; holes 13 are distributed on the spherical surface 12; the holes 13 are evenly and symmetrically distributed on the spherical surface 12, the number of the holes 13 is 60, the diameter of the holes is 4mm, and the depth of the holes is 10 mm. The hole 13 is a chamfer structure extending towards the outer edge at the spherical surface 12, and the depth of the chamfer structure is 1 mm.
Grounding 9 the metal roller 7, and adjusting the distance between the metal roller 7 and the porous spherical electrostatic spinning nozzle 5 to be 20 cm; turning on the second motor 6, and setting the rotating speed of the metal roller 7 to be 60 r/min; opening a switch of the liquid supply device 16, and injecting the spinning liquid 14 into the liquid storage tank 2 through the peristaltic pump 15; turning on a first motor 3, setting the rotating speed to be 0.5r/min, driving a porous spherical electrostatic spinning nozzle 5 to rotate in a spinning solution 14 by the first motor 3 through a transmission shaft 4, and respectively forming liquid films in two states on the surfaces of a spherical surface 12 and a hole 13; opening a switch of the high-voltage generator 1, and slowly increasing the voltage to 65 kV; the first jet flow 10 and the second jet flow 11 with different fineness are respectively generated on the liquid films on the surfaces of the spherical surface 12 and the holes 13; the jet flies to the metal roller 7 under the action of a high-voltage electrostatic field, the solvent is volatilized, and the jet is stretched, solidified and deposited on the metal roller 7 to form the nano-fibers 8.
Example 2
An electrostatic spinning method comprises the following steps:
the spinning solution 14 is a polymer solution prepared from Polyacrylonitrile (PAN) and N-N Dimethylformamide (DMF) to prepare the nanofiber with controllable multistage diameter distribution. The mass fraction of the prepared PAN high polymer solution is 14%.
Selecting a spray head with the diameter of 60 mm; holes 13 are distributed on the spherical surface 12; the holes 13 are evenly and symmetrically distributed on the spherical surface 12, the number of the holes 13 is 60, the diameter of the holes is 6mm, and the depth of the holes is 10 mm. The hole 13 is a chamfer structure extending towards the outer edge at the spherical surface 12, and the depth of the chamfer structure is 1 mm.
Grounding 9 the metal roller 7, and adjusting the distance between the metal rotary roller 7 and the porous spherical electrostatic spinning nozzle 5 to be 22 cm; turning on the second motor 6, and setting the rotating speed of the metal roller 7 to be 80 r/min; opening a switch of the liquid supply device 16, and injecting the spinning liquid 14 into the liquid storage tank 2 through the peristaltic pump 15; turning on a first motor 3, setting the rotating speed to be 1r/min, driving a porous spherical electrostatic spinning nozzle 5 to rotate in a spinning solution 14 by the first motor 3 through a transmission shaft 4, and respectively forming liquid films in two states on the surfaces of a spherical surface 12 and a hole 13; opening a switch of the high-voltage generator 1, and slowly increasing the voltage to 75 kV; the first jet flow 10 and the second jet flow 11 with different fineness are respectively generated on the liquid films on the surfaces of the spherical surface 12 and the holes 13; the jet flies to the metal roller 7 under the action of a high-voltage electrostatic field, the solvent is volatilized, and the jet is stretched, solidified and deposited on the metal roller 7 to form the nano-fibers 8.
Example 3
An electrostatic spinning method comprises the following steps:
the spinning solution 14 is a polymer solution prepared from Polyacrylonitrile (PAN) and N-N Dimethylformamide (DMF) to prepare the nanofiber with controllable multistage diameter distribution. The mass fraction of the prepared PAN high polymer solution is 10 percent.
Selecting a spray head with the diameter of 60 mm; holes 13 are distributed on the spherical surface 12; the holes 13 are evenly and symmetrically distributed on the spherical surface 12, the number of the holes 13 is 60, the diameter of the holes is 4mm, and the depth of the holes is 5 mm. The hole 13 is a chamfer structure extending towards the outer edge at the spherical surface 12, and the depth of the chamfer structure is 1 mm.
Grounding 9 the metal roller 7, and adjusting the distance between the metal roller 7 and the porous spherical electrostatic spinning nozzle 5 to be 16 cm; turning on the second motor 6, and setting the rotating speed of the metal roller 7 to be 40 r/min; opening a switch of the liquid supply device 16, and injecting the spinning liquid 14 into the liquid storage tank 2 through the peristaltic pump 15; turning on a first motor 3, setting the rotating speed to be 0.5r/min, driving a porous spherical electrostatic spinning nozzle 5 to rotate in a spinning solution 14 by the first motor 3 through a transmission shaft 4, and respectively forming liquid films in two states on the surfaces of a spherical surface 12 and a hole 13; opening a switch of the high-voltage generator 1, and slowly increasing the voltage to 65 kV; the first jet flow 10 and the second jet flow 11 with different fineness are respectively generated on the liquid films on the surfaces of the spherical surface 12 and the holes 13; the jet flies to the metal roller 7 under the action of a high-voltage electrostatic field, the solvent is volatilized, and the jet is stretched, solidified and deposited on the metal roller 7 to form the nano-fibers 8.
Claims (8)
1. The porous spherical electrostatic spinning spray head is characterized in that the porous spherical electrostatic spinning spray head (5) is a solid sphere with a smooth surface, and a plurality of holes (13) are distributed on a spherical surface (12) of the porous spherical electrostatic spinning spray head; the porous spherical electrostatic spinning nozzle (5) is connected with the motor I (3) through the transmission shaft (4), the lower part of the porous spherical electrostatic spinning nozzle (5) is immersed in spinning liquid (14) in the liquid storage tank (2), the spinning liquid (14) is connected with the anode of the high-voltage generator (1), and the liquid supply device (16) is communicated with the bottom of the liquid storage tank (2) through the peristaltic pump (15); a receiving device is arranged above the porous spherical electrostatic spinning nozzle (5); the solid sphere is made of metal copper or stainless steel, and the diameter of the solid sphere is 30-200 mm; the holes (13) are uniformly and symmetrically distributed on the spherical surface (12), the number of the holes (13) is 1-1000, the diameter of the holes is 1-10 mm, and the depth of the holes is 1-30 mm; the hole (13) is of a chamfer structure extending towards the outer edge at the spherical surface (12), and the depth of the chamfer structure is 0-10 mm.
2. A porous spherical electrospinning jet head according to claim 1, wherein the reservoir (2) is made of teflon.
3. The porous spherical electrospinning jet head of claim 1, wherein the voltage regulation range of the high voltage generator (1) is 0 to 120 kV.
4. A porous spherical electrospinning spray head according to claim 1 wherein the drive shaft (4) is arranged coaxially with the diameter of a solid sphere.
5. The porous spherical electrospinning nozzle of claim 1, wherein the rotational speed of the first motor (3) is 0 to 15 r/min.
6. Porous spherical electrospinning spray head according to claim 1, characterized in that the receiving means comprise a metal roller (7) with motor two (6), the metal roller (7) being connected to ground (9) or to the negative pole of the high voltage generator (1).
7. The porous spherical electrospinning spray head according to claim 6, wherein the diameter of the metal roller (7) is 100 to 1200mm, and the rotation speed of the second motor (6) is 0 to 120 r/min.
8. An electrospinning method using the porous spherical electrospinning nozzle according to any one of claims 1 to 7, comprising the steps of:
step 1): adjusting the distance between the receiving device and the porous spherical electrostatic spinning nozzle (5), and opening the receiving device;
step 2): opening the liquid supply device (16), and injecting the spinning solution (14) into the liquid storage tank (2) through a peristaltic pump (15);
step 3): turning on a first motor (3), setting the rotating speed, enabling a porous spherical electrostatic spinning nozzle (5) to rotate in a spinning solution (14), and enabling the spinning solution (14) to form liquid films in two states on the surfaces of a spherical surface (12) and holes (13) respectively;
step 4): and (2) opening the high-voltage generator (1), slowly increasing the voltage to the required spinning voltage, enabling liquid films on the surfaces of the spherical surface (12) and the hole (13) to respectively generate a first jet flow (10) and a second jet flow (11) with different fineness, flying to the receiving device under the action of a high-voltage electrostatic field, and after the solvent is volatilized, stretching, solidifying and depositing the jet flows on the receiving device to form the nano fibers (8).
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| CN110629307A (en) * | 2019-09-26 | 2019-12-31 | 南通纺织丝绸产业技术研究院 | Spinning method capable of improving yield of nano fibers |
| CN111394805A (en) * | 2020-03-09 | 2020-07-10 | 东华大学 | Sea urchin-shaped electrostatic spinning nozzle and spinning method thereof |
| CN112981557B (en) * | 2021-02-08 | 2022-05-13 | 苏州大学 | Waterwheel type bubble spinning device |
| CN115974597A (en) * | 2023-01-31 | 2023-04-18 | 广西贺州农贝贝农牧科技有限公司 | Environment-friendly livestock and poultry manure high-temperature aerobic fermentation chamber and fermentation process thereof |
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| CZ294274B6 (en) * | 2003-09-08 | 2004-11-10 | Technická univerzita v Liberci | Process for producing nanofibers from polymeric solution by electrostatic spinning and apparatus for making the same |
| CN102191574B (en) * | 2011-05-19 | 2012-09-05 | 厦门大学 | Nano fiber batch manufacturing device |
| CN105734694B (en) * | 2016-03-08 | 2018-04-24 | 西安工程大学 | A kind of air pressure is to liquid formula electrostatic spinning apparatus and its method for preparing nanometer fiber net |
| CN106811811B (en) * | 2017-01-20 | 2019-01-11 | 东华大学 | A kind of brush mass electrostatic spinning apparatus of ball shape rotary and its application method |
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