CN107366028B - Electrostatic spinning method for preparing skin-core composite structure nanofibers in batch - Google Patents
Electrostatic spinning method for preparing skin-core composite structure nanofibers in batch Download PDFInfo
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- CN107366028B CN107366028B CN201710629294.8A CN201710629294A CN107366028B CN 107366028 B CN107366028 B CN 107366028B CN 201710629294 A CN201710629294 A CN 201710629294A CN 107366028 B CN107366028 B CN 107366028B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
-
- 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
-
- 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
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
Abstract
The invention relates to an electrostatic spinning method for preparing nano fibers with a skin-core composite structure in batches, which comprises the following steps: (1) forming composite layer spinning solution covered by an upper layer and a lower layer above a spinning nozzle through shell layer spinning solution and core layer spinning solution; (2) under the action of a high-voltage electrostatic field, a large number of skin-core structure Taylor cones are formed; (3) and forming the skin-core composite structure nanofiber on a receiving plate after stretching and curing. The invention can improve the yield of the skin-core composite structure nanofiber and realize the continuous and large-scale preparation of the skin-core composite structure nanofiber, and the used electrostatic spinning device has simple structure and convenient operation, and can eliminate the problem of solvent volatilization at the spinning liquid level in the spinning process and realize the batch preparation of the skin-core composite structure nanofiber.
Description
Technical Field
The invention belongs to the field of coaxial electrostatic spinning, and particularly relates to an electrostatic spinning method for preparing nano fibers with a skin-core composite structure in batches, in particular to an upward-spraying electrostatic spinning method for preparing nano fibers with a skin-core composite structure in batches.
Background
The nanofiber non-woven fabric material prepared by the electrostatic spinning technology has the excellent characteristics of ultra-high specific surface area, high porosity, excellent mechanical property and the like, so that the nanofiber non-woven fabric material has very important application value in various fields such as biomedicine, filtration, catalysis, energy and the like at present, compared with the traditional nanofiber with a single structure, the nanofiber with the skin-core structure has great advantages in various fields such as controllable drug slow release, tissue engineering, a nano sensor, catalysis and the like, has great commercial value and market potential, and is widely concerned by the academic and industrial fields.
The traditional single-needle coaxial electrostatic spinning technology is to improve a single capillary spinneret into a composite capillary spinneret with a concentric shaft configuration, namely, the single capillary spinneret is formed by mutually nesting two capillaries with a coaxial configuration. When coaxial electrostatic spinning is carried out, the shell layer spinning solution and the core layer spinning solution are respectively supplied by two different injection pumps, and the functionalized skin-core composite structure nanofiber can be prepared under the action of a high-voltage electrostatic field. However, the yield of the skin-core composite structure nanofiber prepared by adopting the technology is low, and the mass production of the skin-core composite structure nanofiber cannot be realized.
At present, a certain breakthrough is made in the research of preparing the skin-core composite structure nano fiber in batches by coaxial electrostatic spinning, but a certain problem still exists. Like the small red of the cyst, etc. (the patent number is ZL 201310586614.8) realizes the batch preparation of the nanofiber with the sheath-core structure by utilizing a stepped needleless spinneret, but the spinning liquid surface is open, so that the problem that the solvent on the spinning liquid surface is volatile in the spinning process exists; wuhui et al (patent No. ZL 201410037884.8) adopt an upward spinning flat-plate free liquid surface coaxial electrostatic spinning method, and can prepare multifunctional composite fibers with more uniform structures in batch by increasing the number of core pins and changing core liquid, but the increase of the number of the core pins can generate the problem of electric field interference, and the problem of volatile solvent of the spinning liquid surface in the spinning process is also existed.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides an electrostatic spinning method for preparing nano fibers with a skin-core composite structure in batches, which realizes the batch production of the nano fibers with the skin-core composite structure by utilizing the principle that the double-layer spinning liquid level generates unstable fluctuation under the action of a high-voltage electrostatic field. The spinning method avoids the phenomenon that the traditional coaxial electrostatic spinning technology is easy to block in the spinning process, avoids the problem that a spinning liquid surface solvent is easy to volatilize in the spinning process, and can greatly improve the production efficiency of the skin-core composite structure nanofiber.
In order to achieve the purpose, the invention is realized by the following technical scheme:
an electrostatic spinning method for preparing nano fibers with a skin-core composite structure in batches comprises the following steps:
(1) forming composite layer spinning solution covered by an upper layer and a lower layer above a spinning nozzle through shell layer spinning solution and core layer spinning solution;
(2) under the action of a high-voltage electrostatic field, a large number of skin-core structure Taylor cones are formed;
(3) and forming the skin-core composite structure nanofiber on a receiving plate after stretching and curing.
The electrostatic spinning method is carried out in electrostatic spinning equipment, the electrostatic spinning equipment comprises a strip-shaped spinning nozzle positioned above a spinning nozzle base, the strip-shaped spinning nozzle is connected with a high-voltage electrostatic generator, a core layer liquid storage tank and a solution recovery tank are respectively arranged on two sides of the spinning nozzle base, a shell layer liquid storage tank is arranged on one side of the core layer liquid storage tank, a receiving plate is arranged above the strip-shaped spinning nozzle, and the receiving plate is grounded.
The cross section of the strip-shaped spinneret is triangular, semicircular or knife-edge, the longitudinal direction of the strip-shaped spinneret is linear or curved, and the width of the strip-shaped spinneret is 1-4 mm.
The cross section of the spinneret base is rectangular, the longitudinal direction of the spinneret base is linear or curved corresponding to the strip-shaped spinneret, and the width of the spinneret base is 4-8 mm.
The outlet of the spinning solution of the liquid storage tank is a slit with the width of 1-5 mm; the core layer spinning solution is placed in a core layer liquid storage tank, and a slit at the outlet of the core layer liquid storage tank is 1-5mm higher than the spinning nozzle; the shell spinning solution is placed in a shell liquid storage tank, and a slit at the outlet of the shell liquid storage tank is 1-5mm higher than that of the core layer liquid storage tank; the inlet of the solution recovery tank is a slit with the width of 5-10mm, is opposite to the liquid storage tank and is arranged on the other side of the spinneret base; the spinning direction is upward, and the receiving plate is located at 500mm above the strip spinneret by 100-.
In the spinning process, firstly, the core layer spinning solution in the core layer liquid storage tank overflows the strip-shaped spinneret after passing through a slit at the outlet of the liquid storage tank to reach a solution recovery tank, and then the shell layer spinning solution in the shell layer liquid storage tank covers the core layer spinning solution overflowing from the slit at the outlet of the liquid storage tank after passing through the slit at the outlet of the liquid storage tank, and overflows the strip-shaped spinneret together with the core layer spinning solution in an up-down covering manner to reach the solution recovery tank.
The high-voltage static voltage output range is 10-100 kV.
The strip-shaped spinneret is made of metal materials; the core layer liquid storage tank and the shell layer liquid storage tank are both made of insulating materials; the solution recovery tank is made of an insulating material; the spinneret base is made of an insulating material; the receiving plate is made of metal materials.
The electrostatic spinning method for preparing the skin-core composite structure nano fibers in batches has the following beneficial effects:
1. the electrostatic spinning method greatly improves the production efficiency of the skin-core composite structure nanofiber;
2. the electrostatic spinning device can avoid the phenomenon that the traditional coaxial electrostatic spinning needle head structure device is easy to block, is easy to clean and has good stability;
3. the electrostatic spinning device can avoid the problem of volatile spinning liquid surface solvent in the spinning process in other coaxial electrostatic spinning technologies.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of a structure of a linear spinneret in the form of a strip having a triangular cross section and a linear longitudinal direction;
FIG. 3 is a schematic view of a structure of a strip spinneret having a triangular cross section and a curved longitudinal section;
FIG. 4 is a schematic view of a structure of a linear spinneret in the longitudinal direction and having a semicircular cross section;
FIG. 5 is a schematic view of a structure of a strip spinneret having a semicircular cross section and a curved longitudinal section;
wherein, 1 is a shell layer liquid storage tank, 2 is a core layer liquid storage tank, 3 is a solution recovery tank, 4 is a spinneret base, 5 is a strip spinneret, 6 is a high-voltage electrostatic generator, and 7 is a receiving plate.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
Referring to fig. 1 to 5, in the electrostatic spinning method for batch preparation of the sheath-core composite structure nanofiber according to the present invention, a shell layer spinning solution and a core layer spinning solution are used to form a composite layer spinning solution covered by an upper layer and a lower layer above a strip-shaped spinneret 5, a large number of sheath-core structure taylor cones are formed under the action of a high voltage electrostatic field, and the sheath-core composite structure nanofiber is formed on a receiving plate after being stretched and cured.
The strip spinneret 5 is arranged above the spinneret base 4, the cross section of the strip spinneret 5 can be triangular, semicircular or knife-edge shaped, the longitudinal direction of the strip spinneret 5 is linear or curved, and the width of the strip spinneret 5 is 1-4 mm. The cross section of the spinneret base 4 is rectangular, the spinneret base 4 is linear or curved corresponding to the strip-shaped spinneret 5 in the longitudinal direction, and the width of the spinneret base is 4-8 mm. The outlet of the spinning solution of the liquid storage tank is a slit with the width of 1-5mm, the spinning solution of the core layer is arranged in the liquid storage tank 2 of the core layer, and the slit at the outlet of the liquid storage tank 2 of the core layer is 1-5mm higher than the upper part of the strip-shaped spinning nozzle 5; the shell spinning solution is placed in the shell liquid storage tank 1, and the slit at the outlet of the shell liquid storage tank 1 is 1-5mm higher than that of the core layer liquid storage tank. The solution recovery tank 3 is provided with a slit with the width of 5-10mm at the inlet, is opposite to the liquid storage tank and is arranged at the other side of the spinning nozzle base 4. The spinning direction is upward, i.e. the receiving plate 7 is located 100-500mm directly above the strip spinneret 5.
In the spinning process, the spinning solution of the core layer in a core layer liquid storage tank 2 firstly overflows a strip-shaped spinning nozzle 5 to a solution recovery tank 3 through a slit at an outlet of the liquid storage tank, then the spinning solution of the shell layer in a shell layer liquid storage tank 1 covers the spinning solution of the core layer overflowing from the slit at the outlet of the liquid storage tank through the slit at the outlet of the liquid storage tank, and overflows the strip-shaped spinning nozzle 5 to the solution recovery tank 3 together with the spinning solution of the core layer in an up-down covering manner.
The proportion of the shell layer fiber and the core layer fiber in the skin-core composite structure nanofiber can be adjusted through the overflow amount and the overflow speed of the shell layer spinning solution and the core layer spinning solution from the slits at the outlets of the respective liquid storage tanks, and the viscosity and the conductivity of the spinning solutions, and the spinning solution of the core layer is preferably higher in density and higher in conductivity than the shell layer spinning solution in the spinning process.
In the present invention
The electrostatic spinning device comprises a strip-shaped spinning nozzle 5, a spinning nozzle base 4, a shell layer liquid storage tank 1, a core layer liquid storage tank 2, a solution recovery tank 3, a receiving plate 7 and a high-voltage electrostatic generator 6. The strip-shaped spinneret 5 is made of metal materials, the spinneret base 4 is made of insulating materials, the shell layer liquid storage tank 1 and the core layer liquid storage tank 2 are made of insulating materials, the solution recovery tank 3 is made of insulating materials, and the receiving plate 7 is made of metal materials. The strip spinneret 5 is connected with the anode of a high-voltage electrostatic generator 6, the output range of the high-voltage electrostatic voltage is 10-100kV, and a receiving plate 7 is grounded.
In the embodiment, a Polyacrylonitrile (PAN) solution with the mass concentration of 10% is selected as a core layer solution, a Polyurethane (PU) solution with the mass concentration of 14% is adopted as a shell layer solution, a core layer spinning solution firstly overflows from a slit at an outlet of a core layer liquid storage tank 2 at a certain flow rate and passes over the upper edge of a strip-shaped spinneret 5, and then enters a solution recovery tank 3; then, the shell layer spinning solution overflows from a slit at the outlet of the shell layer liquid storage tank 1 at a certain flow velocity, then covers the core layer spinning solution, and passes through a strip-shaped spinning nozzle 5 together with the core layer spinning solution in an up-down covering state to enter a solution recovery tank 3; when the upper edge of the strip-shaped spinning nozzle 5 forms stable upper and lower layer spinning solution coverage, the high-voltage electrostatic generator 6 starts to apply a certain voltage, so that the upper and lower composite layer spinning solutions on the upper edge of the strip-shaped spinning nozzle 5 form unstable fluctuation under the action of a high-voltage electrostatic field, a plurality of sheath-core composite structure Taylor cones formed on the spinning solution surface generate sheath-core composite structure jet flow, and the sheath-core composite structure nanofiber is formed after stretching and drying.
The invention can improve the yield of the skin-core composite structure nanofiber and realize the continuous and large-scale preparation of the skin-core composite structure nanofiber, and the used electrostatic spinning device has simple structure and convenient operation, and can eliminate the problem of solvent volatilization at the spinning liquid level in the spinning process and realize the batch preparation of the skin-core composite structure nanofiber.
The above-mentioned embodiments are only used for explaining the inventive concept of the present invention, and do not limit the protection of the claims of the present invention, and any insubstantial modifications of the present invention using this concept shall fall within the protection scope of the present invention.
Claims (5)
1. An electrostatic spinning method for preparing nano fibers with a skin-core composite structure in batches is characterized by comprising the following steps:
(1) forming composite layer spinning solution covered by an upper layer and a lower layer above a spinning nozzle through shell layer spinning solution and core layer spinning solution;
(2) under the action of a high-voltage electrostatic field, a large number of skin-core structure Taylor cones are formed;
(3) forming the skin-core composite structure nanofiber on a receiving plate after stretching and curing;
the electrostatic spinning method is carried out in electrostatic spinning equipment, the electrostatic spinning equipment comprises a strip-shaped spinning nozzle positioned above a spinning nozzle base, the strip-shaped spinning nozzle is connected with a high-voltage electrostatic generator, a core layer liquid storage tank and a solution recovery tank are respectively arranged on two sides of the spinning nozzle base, a shell layer liquid storage tank is arranged on one side of the core layer liquid storage tank, a receiving plate is arranged above the strip-shaped spinning nozzle, and the receiving plate is grounded;
in the spinning process, firstly, the core layer spinning solution in the core layer liquid storage tank overflows the strip-shaped spinneret after passing through a slit at the outlet of the liquid storage tank to reach a solution recovery tank, then the shell layer spinning solution in the shell layer liquid storage tank covers the core layer spinning solution overflowing from the slit at the outlet of the liquid storage tank after passing through the slit at the outlet of the liquid storage tank, and overflows the strip-shaped spinneret together with the core layer spinning solution in an up-and-down covering manner to reach the solution recovery tank;
in the spinning process, the spinning solution of the core layer has higher density and conductivity than the spinning solution of the shell layer.
2. The electrospinning method of mass producing core-sheath composite structured nanofibers according to claim 1, wherein: the cross section of the strip-shaped spinneret is triangular, semicircular or knife-edge, the longitudinal direction of the strip-shaped spinneret is linear or curved, and the width of the strip-shaped spinneret is 1-4 mm.
3. The electrospinning method of mass producing core-sheath composite structured nanofibers according to claim 1, wherein: the cross section of the spinneret base is rectangular, the longitudinal direction of the spinneret base is linear or curved corresponding to the strip-shaped spinneret, and the width of the spinneret base is 4-8 mm.
4. The electrospinning method of mass producing core-sheath composite structured nanofibers according to claim 1, wherein: the high-voltage static voltage output range is 10-100 kV.
5. The electrospinning method of mass producing core-sheath composite structured nanofibers according to claim 1, wherein: the strip-shaped spinneret is made of metal materials; the core layer liquid storage tank and the shell layer liquid storage tank are both made of insulating materials; the solution recovery tank is made of an insulating material; the spinneret base is made of an insulating material; the receiving plate is made of metal materials.
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| CN109137095B (en) * | 2018-10-26 | 2021-11-30 | 邳州市鑫盛创业投资有限公司 | Collecting table of electrospinning fiber jet forming device |
| CN109957846B (en) * | 2019-04-08 | 2021-05-14 | 嘉兴学院 | Wide-diameter distribution nanofiber based on coaxial electrostatic spinning and preparation method thereof |
| CN110629297A (en) * | 2019-09-26 | 2019-12-31 | 南通纺织丝绸产业技术研究院 | Free liquid level spinning method for multi-polymer blending |
| CN111485296B (en) * | 2020-05-19 | 2021-01-05 | 南京鼓楼医院 | Preparation method and application of bionic multi-component fiber |
| CN111472057A (en) * | 2020-05-29 | 2020-07-31 | 苏州大学 | Spinning device with core-shell structure capable of preparing nanofibers in batches |
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| WO2014074565A1 (en) * | 2012-11-07 | 2014-05-15 | Massachusetts Institute Of Technology | Formation of core-shell fibers and particles by free surface electrospinning |
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| CN100410429C (en) * | 2003-12-10 | 2008-08-13 | 同济大学 | Electrostatic spinning apparatus with multi-spraying heads for preparing coaxial composite continuous nanometer/micron fibre |
| US8968626B2 (en) * | 2011-01-31 | 2015-03-03 | Arsenal Medical, Inc. | Electrospinning process for manufacture of multi-layered structures |
| US9194058B2 (en) * | 2011-01-31 | 2015-11-24 | Arsenal Medical, Inc. | Electrospinning process for manufacture of multi-layered structures |
| WO2014062627A1 (en) * | 2012-10-15 | 2014-04-24 | Arsenal Medical, Inc. | Systems and methods for facilitating the generation of core-sheath taylor cones in electrospinning |
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| WO2014074565A1 (en) * | 2012-11-07 | 2014-05-15 | Massachusetts Institute Of Technology | Formation of core-shell fibers and particles by free surface electrospinning |
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