CN109881268B - Spiral electrostatic spinning nozzle with controllable spinning solution curvature and application method thereof - Google Patents
Spiral electrostatic spinning nozzle with controllable spinning solution curvature and application method thereof Download PDFInfo
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- CN109881268B CN109881268B CN201910217391.5A CN201910217391A CN109881268B CN 109881268 B CN109881268 B CN 109881268B CN 201910217391 A CN201910217391 A CN 201910217391A CN 109881268 B CN109881268 B CN 109881268B
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Abstract
The invention relates to a spiral electrostatic spinning nozzle with controllable spinning solution curvature and a using method thereof. The spiral spinning cutter head consists of a spiral body with a spiral line outline and a triangular section and a cylindrical central shaft; the spiral groove sleeve consists of a spiral line with the outline of a spiral spinning cutter head, an unclosed isosceles trapezoid ring with a bottomless section and a cylindrical central shaft, and the two are concentrically arranged. The invention adopts the spiral groove sleeve made of polytetrafluoroethylene, so that the curvature of the spinning solution on the surface of the spiral spinning cutter head does not fluctuate obviously, and the electric field of the spinning nozzle is not interfered. The technology can stabilize the free liquid level of the spinning solution on the basis of not interfering the regulation and control of an electric field, regulate and control the curvature of the spinning solution, reduce the volatilization of a solvent and realize the batch preparation of narrow-distribution submicron fibers and nano fibers.
Description
Technical Field
The invention belongs to the technical field of nano fibers and textile machinery, and particularly relates to a spiral electrostatic spinning nozzle with controllable spinning solution curvature and a using method thereof.
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 prior patents also disclose a series of spiral jets immersed in the spinning dope, which do not constrain the curvature of the spinning dope at the exit point and do not provide good control of the fiber diameter.
Disclosure of Invention
The invention aims to solve the technical problems that the shape of a spinning solution on the surface of the conventional spiral immersion type nozzle is not constrained, the movement path of jet flow is unstable in the spinning process, the free liquid level of the spinning solution to be spun is too large, and the solvent of the spinning solution to be spun is volatile, and simultaneously, the precise design regulation of the electric field and the curvature of the spinning solution in the electrostatic spinning process is realized, and the large-batch preparation of narrow-distribution submicron fibers and nano fibers is realized.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a spiral electrostatic spinning nozzle with controllable spinning solution curvature comprises a spiral spinning tool bit and a spiral groove sleeve fixedly mounted on the spiral spinning tool bit.
Further, the spiral spinning cutter head consists of a spiral body with a spiral line outline and a triangular section and a cylindrical central shaft; the diameter of the outline spiral line of the spiral spinning cutter head is 80-500mm, and the thread pitch is 10-100 mm; the profile section triangle of the spiral spinning cutter head is an isosceles triangle, the bottom is 20-100mm, and the height is 40-200 mm; the profile is a spiral line, and the spiral body with the triangular section is chamfered with fillets with the radius of 5-10mm at the spiral line of the bottom angles at two positions of the triangle.
Further, the spiral spinning cutter head is made of copper.
Further, the spiral groove sleeve is composed of a spiral line with the outline of a spiral spinning cutter head, an unclosed isosceles trapezoid ring without an upper bottom and a cylindrical central shaft, and the spiral groove sleeve and the spiral spinning cutter head are concentrically arranged; the top end of the spiral groove sleeve is provided with a smooth fillet with the radius of 5-10 mm; the spiral groove sleeve and the spiral spinning cutter head form a slit passage with the width of 0-10 mm.
Furthermore, the spiral groove sleeve is made of polytetrafluoroethylene.
Further, a method for carrying out electrostatic spinning by using a spiral electrostatic spinning nozzle with controllable spinning solution curvature mainly comprises the following steps:
1) grounding the metal cylindrical roller or connecting the metal cylindrical roller with the negative electrode of a high-voltage generator, connecting a spiral spinning cutter head with the positive electrode of the high-voltage generator, and adjusting the distance between the metal cylindrical roller and a spiral electrostatic spinning nozzle with controllable spinning solution curvature;
2) opening a driving motor of the metal cylindrical roller and setting the rotating speed of the metal cylindrical roller;
3) immersing the bottom of a spiral electrostatic spinning nozzle with controllable spinning solution curvature in a spinning solution tank and setting the rotating speed of the nozzle, wherein the spinning solution tank stores high polymer spinning solution;
4) opening a switch of the high-voltage generator, and slowly increasing the voltage to the required spinning voltage;
5) a large number of jet flows are generated on the surface of the spinning solution of the upper spiral spinning cutter head;
6) the jet flow flies to the metal cylinder roller under the action of the high-voltage electrostatic field, the solvent is volatilized, and the jet flow is stretched, solidified and deposited on the metal cylinder roller to form a large number of nano fibers.
Furthermore, the receiving device comprises a metal rotary drum and a driving motor for driving the metal rotary drum to rotate, the diameter of the metal rotary drum is 80mm-1200mm, and the rotating speed of the driving motor is 0-100 r/min.
Further, the rotating angular speed of the spiral electrostatic spinning nozzle with controllable spinning solution curvature is 0-15 r/min.
Furthermore, the voltage regulation range of the high-voltage generator is 0-100 KV.
The invention has the beneficial effects that: the spiral groove sleeve made of polytetrafluoroethylene is adopted, so that the curvature of the spinning solution on the surface of the spiral spinning tool bit does not fluctuate obviously, and meanwhile, the electric field of a spinning nozzle is not interfered. The technology is simple and easy to implement, can stabilize the free liquid level of the spinning solution on the basis of not interfering the regulation and control of an electric field, regulate and control the curvature of the spinning solution, reduce the volatilization of a solvent and realize the batch preparation of narrow-distribution submicron fibers and nano fibers.
Drawings
FIG. 1 is a schematic drawing of spinning with a spiral electrostatic spinning nozzle with controllable spinning solution curvature.
FIG. 2 is a schematic view of a spiral spinning head.
Fig. 3 is a schematic view of a spiral fluted bushing.
FIG. 4 is a schematic view of a spiral electrostatic spinning nozzle with controllable curvature of the spinning solution;
FIG. 5 is a schematic cross-sectional view of a spiral electrostatic spinning nozzle with controllable curvature of the spinning solution.
1. The spinning device comprises a high-voltage generator, 2, a spinning liquid groove, 3, jet flow, 4, a driving motor, 5, a metal rotary drum, 6, nano fibers, 7, a ground, 8, a spiral spinning tool bit, 9, a spiral groove sleeve, 10, high polymer spinning liquid, 11 and the surface of the spinning liquid.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 2, 3, 4 and 5, a spiral electrostatic spinning nozzle with controllable spinning solution curvature comprises a spiral spinning cutter head 8 and a spiral groove sleeve 9; the spiral spinning cutter head 8 consists of a spiral body with a spiral line outline and a triangular section and a cylindrical central shaft; the diameter of the outline spiral line is 80-500mm, and the thread pitch is 10-100 mm; the profile section triangle is an isosceles triangle, the bottom is 20-100mm, and the height is 40-200 mm; the profile is a spiral line, and the spiral body with the triangular section is chamfered with fillets with the radius of 5-10mm at the spiral line of the bottom angles at two positions of the triangle. The spiral groove sleeve 9 is composed of a spiral line with the outline of a spiral spinning tool bit 8, an unclosed isosceles trapezoid ring without an upper bottom and a cylindrical central shaft, and the spiral groove sleeve 9 and the spiral spinning tool bit 8 are concentrically arranged; the top end of the spiral groove sleeve 9 is provided with a smooth fillet with the radius of 5-10 mm; the spiral groove sleeve 9 and the spiral spinning cutter head 8 form a slit passage with the width of 0-10 mm.
The spiral spinning tool bit 8 is made of copper, the spiral groove sleeve 9 is made of polytetrafluoroethylene, and the spiral groove sleeve 9 is fixedly mounted on the spiral spinning tool bit 8 to form a spiral electrostatic spinning nozzle with controllable spinning solution curvature.
As shown in fig. 1, when electrostatic spinning is performed by using a spiral electrostatic spinning nozzle with controllable spinning solution curvature, the method mainly comprises the following steps:
1) grounding 7 the metal cylindrical roller 5 or connecting the metal cylindrical roller with the negative electrode of the high-voltage generator 1, connecting the spiral spinning tool bit 8 with the positive electrode of the high-voltage generator 1, and adjusting the distance between the metal cylindrical roller 5 and a spiral electrostatic spinning nozzle with controllable spinning solution curvature;
2) opening a driving motor 4 of the metal cylindrical roller 5, and setting the rotating speed of the metal cylindrical roller 5;
3) immersing the bottom of a spiral electrostatic spinning nozzle with controllable spinning solution curvature in a spinning solution tank 2 and setting the rotating speed of the nozzle, wherein the spinning solution tank 2 stores high polymer spinning solution 10;
4) opening a switch of the high-voltage generator 1, and slowly increasing the voltage to the required spinning voltage;
5) a large number of jets 3 are generated on the spinning solution surface 11 of the upper spiral spinning cutter head;
6) the jet flow 3 flies to the metal cylinder roller 5 under the action of the high-voltage electrostatic field, the solvent is volatilized, and the jet flow is stretched, solidified and deposited on the metal cylinder roller 5 to form a large number of nano fibers 6.
The voltage regulating range of the high voltage generator 1 is 0-100KV, the spiral electrostatic spinning nozzle with controllable spinning solution curvature rotates at the angular speed of 0-15r/min, the diameter of the metal cylindrical roller is 80mm-1200mm, and the rotating speed of the driving motor 4 is 0-100 r/min.
Example 1
Then, the nano-fiber is prepared by using a high polymer solution prepared from Polyacrylonitrile (PAN) and N-N Dimethylformamide (DMF). The mass fraction of the prepared PAN high polymer solution is 10 percent. Grounding 7 the metal roller 5, and adjusting the distance between the metal cylindrical roller 5 and the spiral electrostatic spinning nozzle with controllable spinning solution curvature to be 20 cm; opening a driving motor 4 of a metal cylindrical roller 5 of a receiving device, and setting the rotating speed of the roller to be 60 r/min; setting the rotating speed of a spiral electrostatic spinning nozzle with controllable spinning solution curvature to be 10 r/min; turning on a switch of the high-voltage generator 1, and slowly increasing the voltage to 50 KV; a large number of jets 3 are generated on the spinning solution surface 11 of the upper spiral spinning head 8; the jet flow 3 flies to the metal roller 5 under the action of a high-voltage electrostatic field, the solvent is volatilized, and the jet flow 3 is stretched, solidified and deposited on the metal roller 5 to form a large number of nano fibers 6.
Example 2
This example is similar to example 1, except that: preparing PAN high polymer solution with the mass fraction of 12%; the distance between the metal cylindrical roller 5 and the spiral electrostatic spinning nozzle with controllable spinning solution curvature is 18 cm; the rotating speed of the metal cylindrical roller 5 is 80 r/min; the rotating speed of the spiral electrostatic spinning nozzle with controllable spinning solution curvature is 12 r/min; the high voltage generator 1 voltage is 55 KV.
Example 3
This example is similar to example 1, except that: the mass fraction of the prepared PAN high polymer solution is 14 percent; the distance between the metal cylindrical roller 5 and the spiral electrostatic spinning nozzle with controllable spinning solution curvature is 22 cm; the rotating speed of the metal cylindrical roller 5 is 80 r/min; the rotating speed of the spiral electrostatic spinning nozzle with controllable spinning solution curvature is 15 r/min; the high voltage generator 1 voltage is 55 KV.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A spiral electrostatic spinning nozzle with controllable spinning solution curvature comprises a spiral spinning tool bit (8) and is characterized in that a spiral groove sleeve (9) is fixedly mounted on the spiral spinning tool bit (8), and the spiral spinning tool bit (8) consists of a spiral body with a spiral line outline and a triangular section and a cylindrical central shaft; the spiral groove sleeve (9) is composed of a spiral line with the outline of the spiral spinning cutter head (8), an unclosed isosceles trapezoid ring with a bottomless cross section and a cylindrical central shaft, and the spiral groove sleeve (9) and the spiral spinning cutter head (8) are concentrically arranged.
2. The spin dope curvature controllable spiral electrostatic spinning nozzle according to claim 1, wherein the diameter of the contour spiral of the spiral spinning cutter head (8) is 80-500mm, and the pitch is 10-100 mm; the profile section triangle of the spiral spinning cutter head (8) is an isosceles triangle, the bottom is 20-100mm, the height is 40-200mm, and fillets with the radius of 5-10mm are chamfered at the spiral line of the two bottom corners of the triangle.
3. The spiral type electrospinning nozzle according to claim 1 or 2, wherein the spiral spinning nozzle tip (8) is made of copper.
4. The spin dope curvature controllable spiral electrospinning jet head of claim 1, wherein the spiral groove tube (9) has a smooth rounded corner at its top end with a radius of 5-10 mm; the spiral groove sleeve (9) and the spiral spinning cutter head (8) form a slit channel with the width of 0-10 mm.
5. The spiral electrospinning nozzle according to claim 1 or 4, wherein the spiral grooved tube (9) is made of polytetrafluoroethylene.
6. A method of electrospinning using the spiral electrospinning nozzle of claim 1 having a controllable curvature of the dope, comprising the steps of:
1) grounding (7) the metal cylindrical roller (5) or connecting the metal cylindrical roller with the negative electrode of the high-voltage generator (1), connecting the spiral spinning tool bit (8) with the positive electrode of the high-voltage generator (1), and adjusting the distance between the metal cylindrical roller (5) and the spiral electrostatic spinning nozzle with controllable spinning solution curvature;
2) opening a driving motor (4) of the metal cylindrical roller (5), and setting the rotating speed of the metal cylindrical roller (5);
3) immersing the bottom of a spiral electrostatic spinning nozzle with controllable spinning solution curvature in a spinning solution tank (2) and setting the rotating speed of the nozzle, wherein the spinning solution tank (2) stores high polymer spinning solution (10);
4) opening a switch of the high-voltage generator (1), and slowly increasing the voltage to the required spinning voltage;
5) a large number of jet flows (3) are generated on the spinning solution surface (11) of the upper spiral spinning cutter head;
6) the jet flow (3) flies to the metal cylindrical roller (5) under the action of a high-voltage electrostatic field, the solvent is volatilized, and the jet flow is stretched, solidified and deposited on the metal cylindrical roller (5) to form a large number of nano fibers (6).
7. The method of electrospinning according to the spiral type electrospinning nozzle having a controlled dope curvature according to claim 6, wherein the diameter of the metal cylindrical drum (5) is 80mm to 1200mm, and the rotation speed of the driving motor (4) is 0 to 100 r/min.
8. The method of electrospinning according to claim 6, wherein the spinning solution curvature-controllable spiral electrospinning nozzle rotates at an angular velocity of 0 to 15 r/min.
9. The method of electrospinning according to the spiral type electrospinning nozzle having a controlled dope curvature according to claim 6, wherein the voltage regulation range of the high voltage generator (1) is 0 to 100 KV.
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| FR2902114A1 (en) * | 2006-06-12 | 2007-12-14 | Promiles Snc | POLYMERIC FILAMENT HAVING AT LEAST ONE LONGITUDINAL ETOFFE CHANNEL COMPRISING THESE FILAMENTS, ARTICLE FORMED THEREFROM, AND METHOD OF MAKING SAID FILAMENT |
| CN102828259A (en) * | 2012-09-18 | 2012-12-19 | 天津工业大学 | Saw tooth type needle-free electrostatic spinning device |
| CN103484953A (en) * | 2013-09-11 | 2014-01-01 | 天津工业大学 | Disc-type needle-free electrostatic spinning device |
| CN204608225U (en) * | 2015-04-08 | 2015-09-02 | 刘千祥 | A kind of synchronous circulating type helixseal belting for electrostatic spinning |
| CN107620127A (en) * | 2016-07-14 | 2018-01-23 | 天津工业大学 | A kind of needle-less electrostatic spinning component based on fractal structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140377391A1 (en) * | 2013-06-25 | 2014-12-25 | Paul Kaohing Lee | Electro Fiber Pulling Apparatus with Spiral Rod |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2902114A1 (en) * | 2006-06-12 | 2007-12-14 | Promiles Snc | POLYMERIC FILAMENT HAVING AT LEAST ONE LONGITUDINAL ETOFFE CHANNEL COMPRISING THESE FILAMENTS, ARTICLE FORMED THEREFROM, AND METHOD OF MAKING SAID FILAMENT |
| CN102828259A (en) * | 2012-09-18 | 2012-12-19 | 天津工业大学 | Saw tooth type needle-free electrostatic spinning device |
| CN103484953A (en) * | 2013-09-11 | 2014-01-01 | 天津工业大学 | Disc-type needle-free electrostatic spinning device |
| CN204608225U (en) * | 2015-04-08 | 2015-09-02 | 刘千祥 | A kind of synchronous circulating type helixseal belting for electrostatic spinning |
| CN107620127A (en) * | 2016-07-14 | 2018-01-23 | 天津工业大学 | A kind of needle-less electrostatic spinning component based on fractal structure |
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