CN109750360B - Self-cleaning spiral electrostatic spinning nozzle and use method thereof - Google Patents
Self-cleaning spiral electrostatic spinning nozzle and use method thereof Download PDFInfo
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Abstract
The invention relates to a self-cleaning spiral electrostatic spinning nozzle and a using method thereof. The invention adopts the spiral cleaning sleeve made of polytetrafluoroethylene, so that the surface of the spinning cutter head can be immediately screwed, and meanwhile, the electric field of the spinning nozzle is not interfered; the technology can enable the spray head to be always loaded with new liquid on the basis of not interfering the regulation and control of the electric field, improve the uniformity of the concentration distribution of the spinning liquid on the surface of the spray head in the spinning process, clean the spray head immediately, avoid the situation that the solution concentration at the local edge is too high and is solidified, and ensure the stability of the long-time continuous spinning of equipment.
Description
Technical Field
The invention belongs to the technical field of nano fibers and textile machinery, and particularly relates to a self-cleaning spiral electrostatic spinning nozzle 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 solution free surface of the umbrella-shaped nozzle is in contact with the atmospheric environment, and the solvent is very volatile, so that the spinning stability and the final nanofiber quality are affected, and the phenomena of edge solution solidification and wire drawing are easily caused in long-time spinning; 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 solidification phenomenon of the edge solution is easy to occur in the needle-free electrostatic spinning process, and the wire drawing phenomenon often occurs in long-time continuous spinning under a high-voltage electric field. These problems all reduce the quality of electrospun nanofibers and even affect the stable process of continuous spinning for a long time. The spinning nozzle needs to be stopped and cleaned intermittently in the industrial production process, the operation is complex, and the spinning solution is easy to waste and pollute.
Disclosure of Invention
The invention aims to solve the technical problems that the concentration of a continuous spinning solution of a needle-free electrostatic spinning nozzle fluctuates, the concentration distribution of the spinning solution on the surface of the nozzle is uneven in the spinning process, the diameter distribution of spinning fibers is wide, and the spinning is stopped and cleaned after solidified spinning impurities appear in long-time spinning.
The technical scheme adopted by the invention for solving the technical problem is as follows: a self-cleaning spiral electrostatic spinning nozzle comprises a spiral spinning tool bit, a spiral cleaning sleeve and a liquid sealing piston; 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 cleaning sleeve consists of a spiral line with the outline of a spiral spinning cutter head, a similar triangular ring and a cylindrical central shaft; the spiral cleaning sleeve and the spiral spinning cutter head are concentrically arranged and are arranged on the spiral spinning cutter head; the liquid sealing pistons are arranged at two ends of the spiral cleaning sleeve. The spray head is ensured to be cleaned immediately by the reciprocating rotation of the spiral cutter head in the spiral cleaning sleeve.
Further, the upper part of the spiral cleaning sleeve is an open part and a closed part, the open part is formed by horizontally cutting off a spiral part at the upper horizontal part within a screw pitch range, the open part and the closed part are distributed on the whole spiral cleaning sleeve at intervals one by one, and the liquid sealing pistons are arranged at the open parts at the two ends of the spiral cleaning sleeve.
Furthermore, a slit channel with the width of 0-15mm is arranged between the spiral cleaning sleeve and the spiral spinning cutter head, and the side lines of the opening part are all provided with 0-10mm round corners.
Further, the spiral cleaning sleeve is made of polytetrafluoroethylene.
Furthermore, the diameter of the profile spiral line of the spiral spinning cutter head is 80-500mm, and the thread pitch is 10-100 mm; the profile section triangle is an isosceles triangle, the bottom is 20-100mm, the height is 40-200mm, and round corners of 5-10mm are inverted at the base angle spiral lines at two positions of the triangle.
Further, the spiral spinning cutter head is made of copper.
The invention also provides a method for carrying out electrostatic spinning by using the self-cleaning spiral electrostatic spinning nozzle, which mainly comprises the following steps:
1) grounding the metal cylindrical roller or connecting the metal cylindrical roller with the negative electrode of the high-voltage generator, connecting the spiral spinning cutter head with the positive electrode of the high-voltage generator, and adjusting the distance between the metal cylindrical roller and the spiral spinning cutter head;
2) opening a driving motor of the metal cylindrical roller and setting the rotating speed of the roller;
3) immersing the bottom of a self-cleaning spiral electrostatic spinning nozzle in a spinning solution tank and setting a rotating speed, 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 spiral spinning cutter head at the opening part of the spiral cleaning sleeve;
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 diameter of the metal cylindrical roller is 80mm-1200 mm; the rotating speed of the motor is 0-100 r/min.
Furthermore, the voltage regulation range of the high-voltage generator is 0-100 KV.
Further, the spiral spinning cutter head is driven by a motor and rotates in a reciprocating mode in the spiral cleaning sleeve, the rotating angular speed is 0-30r/min, and the reciprocating rotating angle is +/-360 degrees.
The invention has the advantages that the spiral cleaning sleeve made of polytetrafluoroethylene can enable the spray head to be always loaded with new liquid on the basis of not interfering the regulation and control of an electric field, the uniformity of the concentration distribution of the spinning liquid on the surface of the spray head in the spinning process is improved, meanwhile, the spray head is cleaned immediately, the situation that the solution concentration at the local edge is too high and is solidified is avoided, and the stability of the long-time continuous spinning of equipment is ensured.
Drawings
FIG. 1 is a schematic view of a self-cleaning spiral electrostatic spinning nozzle
FIG. 2 is a schematic view of a cleaning sleeve and a spiral spinning blade
1. The device comprises a high-pressure generator, 2, a motor, 3, jet flow, 4, a motor, 5, a metal cylindrical roller, 6, nano fibers, 7, a ground, 8, a spiral spinning cutter head, 9, a spiral cleaning sleeve, 10, a spinning liquid groove, 11, high polymer spinning liquid, 12, a liquid sealing piston, 13, an opening part of the spiral cleaning sleeve, and 14, a sealing part of the spiral cleaning sleeve.
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.
The invention provides a self-cleaning spiral electrostatic spinning nozzle which comprises a spiral spinning cutter head 8, a spiral cleaning sleeve 9 and a liquid sealing piston 12.
As shown in fig. 2, the spiral spinning cutter head 8 is composed of a spiral body with a spiral line profile 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, the height is 40-200mm, and round corners of 5-10mm are inverted at the base angle spiral lines at two positions of the triangle. The spiral spinning cutter head 8 is made of copper and is connected with the anode of the high-voltage generator 1, and the voltage regulating range of the high-voltage generator 1 is 0-100 KV.
As shown in fig. 2, the spiral cleaning sleeve 9 is composed of a spiral line with the outline of the spiral spinning head 8, a similar triangular ring and a cylindrical central shaft in cross section, is made of polytetrafluoroethylene, and is concentrically arranged with the spiral spinning head 8. The spiral cleaning sleeve 9 covers the spiral spinning cutter head 8, and a slit passage with the width of 0-15mm is arranged between the spiral cleaning sleeve and the spiral spinning cutter head. The upper part of the spiral cleaning sleeve 9 is provided with an opening part 13 and a closing part 14, the opening part 13 is formed by horizontally cutting off a horizontal upper spiral part within a range of screw pitches, and the opening part 13 and the closing part 14 are alternately distributed on the whole spiral cleaning sleeve 9. The open part 13 side lines of the spiral cleaning sleeve 9 are all provided with 0-10mm round corners.
As shown in figure 1, the liquid sealing piston 12 is arranged at the open part 13 at the two ends of the spiral cleaning sleeve 9, so that the spinning liquid 11 can not coat the spiral cutter bits at the two ends of the liquid sealing piston 12 during the reciprocating rotation of the spiral cutter bit 8.
The spiral spinning cutter head 8 is driven by the motor 2 and can rotate in a reciprocating mode in the spiral cleaning sleeve 9, the rotating angular speed is 0-30r/min, and the reciprocating rotating angle is +/-360 degrees.
The invention also provides a method for carrying out electrostatic spinning by using the self-cleaning spiral electrostatic spinning nozzle, which 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, and adjusting the distance between the metal cylindrical roller 5 and the spiral spinning cutter head 8;
2) opening a driving motor 4 of a metal cylindrical roller 5, and setting the rotating speed of the roller;
3) immersing the bottom of a self-cleaning spiral electrostatic spinning nozzle in a spinning solution tank 10 and setting a rotating speed, wherein the spinning solution tank 10 stores high polymer spinning solution 11;
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 of the spiral spinning cutter head 8 at the opening part 13 of the spiral cleaning sleeve 9;
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 3 is stretched, solidified and deposited on the metal cylinder roller 5 to form a large number of nano fibers 6.
Preferably, the diameter of the metal cylindrical roller 5 is 80mm-1200mm, and the rotating speed of the speed-adjustable motor 4 for driving the metal roller 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 the metal roller, and adjusting the distance between the metal cylindrical roller and the spiral spinning cutter head 8 to be 20 cm; the driving motor 4 of the metal cylindrical roller of the receiving device is started, and the rotating speed of the roller is set to be 60 r/min; setting the rotating speed of a spiral spinning cutter head 8 to be 3 r/min; turning on a switch of the high-voltage generator 1, and slowly increasing the voltage to 50 KV; a large number of jet flows 3 are generated on the spinning solution surface of the spiral spinning cutter head of the opening part 13 of the spiral cleaning sleeve 9; the jet flow 3 flies to the metal roller 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 to form a large number of nano fibers 6.
Example 2
This example is similar to example 1, except that: the mass fraction of the prepared PAN high polymer solution is 12 percent; the distance between the metal cylindrical roller and the spiral spinning cutter head 8 is 22 cm; the rotating speed of the metal cylindrical roller is 80 r/min; the rotating speed of the spiral spinning cutter head 8 is 5 r/min; the voltage of the high voltage generator 1 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 self-cleaning spiral electrostatic spinning nozzle comprises a spiral spinning tool bit (8), and is characterized by also comprising a spiral cleaning sleeve (9) and a liquid sealing piston (12); 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 cleaning sleeve (9) consists of a spiral line with the outline of a spiral spinning cutter head (8), a similar triangular ring and a cylindrical central shaft in the cross section; the spiral cleaning sleeve is concentrically arranged with the spiral spinning cutter head and is arranged on the spiral spinning cutter head; seal liquid piston (12) and set up clean cover (9) both ends of spiral, clean cover (9) upper portion of spiral is opening portion (13) and closing part (14), opening portion (13) are cut off by the horizontal upper portion spiral portion level of a pitch within range and form, and opening portion (13) and closing part (14) alternate distribution one by one is on whole clean cover (9) of spiral, it sets up to seal liquid piston (12) the clean cover (9) both ends of spiral opening portion (13).
2. The self-cleaning screw type electrospinning nozzle of claim 1, wherein a slit passage with a width of 0-15mm is formed between the screw cleaning sleeve (9) and the screw spinning head (8), and the open part (13) has rounded corners with 0-10mm in side lines.
3. Self-cleaning spiral electrospinning spray head according to any of claims 1 to 2, characterized in that the spiral cleaning sleeve (9) is made of polytetrafluoroethylene.
4. The self-cleaning screw type electrospinning nozzle of claim 1, wherein the diameter of the contour spiral of the screw spinning head (8) is 80 to 500mm, and the pitch is 10 to 100 mm; the profile section triangle is an isosceles triangle, the bottom is 20-100mm, the height is 40-200mm, and round corners of 5-10mm are chamfered at the spiral line of the two bottom angles of the triangle.
5. The self-cleaning spiral electrospinning spray head of claim 1, wherein the spiral spinning blade (8) is made of copper.
6. A method of electrospinning using the self-cleaning helical electrospinning spray head of claim 1, consisting essentially 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 cutter head (8) with the positive electrode of the high-voltage generator (1), and adjusting the distance between the metal cylindrical roller (5) and the spiral spinning cutter head (8);
2) opening a driving motor (4) of the metal cylindrical roller (5), and setting the rotating speed of the roller;
3) immersing the bottom of a self-cleaning spiral electrostatic spinning spray head in a spinning solution tank (10) and setting the rotating speed, wherein the spinning solution tank (10) stores high polymer spinning solution (11);
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 surface of the spinning solution of a spiral spinning cutter head (8) of an opening part (13) of a spiral cleaning sleeve (9);
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 (3) is stretched, solidified and deposited on the metal cylindrical roller (5) to form a large number of nano fibers (6).
7. The electrospinning method according to claim 6, wherein the diameter of the metal cylindrical drum (5) is 80mm to 1200 mm; the rotating speed of the motor (4) is 0-100 r/min.
8. The electrospinning method according to claim 6, wherein the voltage regulation range of the high voltage generator (1) is 0-100 KV.
9. The electrospinning method according to claim 6, wherein the helical spinning blade (8) is driven by the motor (2) to reciprocate in the helical cleaning sleeve (9) at a rotational angular velocity of 0 to 30r/min and a reciprocating rotational angle of ± 360 degrees.
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| JP2011026720A (en) * | 2009-07-22 | 2011-02-10 | Teijin Techno Products Ltd | Spinneret-cleaning system |
| CN102828259A (en) * | 2012-09-18 | 2012-12-19 | 天津工业大学 | Saw tooth type needle-free electrostatic spinning device |
| CN203187801U (en) * | 2013-02-07 | 2013-09-11 | 赵曙光 | Spiral nano-fiber generator |
| CN103484953A (en) * | 2013-09-11 | 2014-01-01 | 天津工业大学 | Disc-type needle-free electrostatic spinning device |
| CN103590121A (en) * | 2013-11-22 | 2014-02-19 | 北京化工大学 | Linear jet flow nozzle-free type electrostatic spinning device |
| CN103774250A (en) * | 2014-01-27 | 2014-05-07 | 上海云同纳米科技中心(普通合伙) | Electrostatic nanofiber generator |
| 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 |
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| CZ20032421A3 (en) * | 2003-09-08 | 2004-11-10 | Technická univerzita v Liberci | Process for producing nanofibers of polymer solution by electrostatic spinning and apparatus for making the same |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011026720A (en) * | 2009-07-22 | 2011-02-10 | Teijin Techno Products Ltd | Spinneret-cleaning system |
| CN102828259A (en) * | 2012-09-18 | 2012-12-19 | 天津工业大学 | Saw tooth type needle-free electrostatic spinning device |
| CN203187801U (en) * | 2013-02-07 | 2013-09-11 | 赵曙光 | Spiral nano-fiber generator |
| CN103484953A (en) * | 2013-09-11 | 2014-01-01 | 天津工业大学 | Disc-type needle-free electrostatic spinning device |
| CN103590121A (en) * | 2013-11-22 | 2014-02-19 | 北京化工大学 | Linear jet flow nozzle-free type electrostatic spinning device |
| CN103774250A (en) * | 2014-01-27 | 2014-05-07 | 上海云同纳米科技中心(普通合伙) | Electrostatic nanofiber generator |
| 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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Effective date of registration: 20211129 Address after: 1882 Yan'an west road, Changning District, Shanghai Patentee after: DONGHUA University Patentee after: NARI Weikang (Shanghai) Technology Co., Ltd Address before: 201620 No. 2999 North Renmin Road, Songjiang new town, Songjiang District, Shanghai. Patentee before: DONGHUA University Patentee before: Nantong Dingyu Textile Machinery Technology Co., Ltd |