CN113913954B - Superfine nanofiber preparation device and method based on solution atomization and electrostatic-airflow take-over drafting - Google Patents
Superfine nanofiber preparation device and method based on solution atomization and electrostatic-airflow take-over drafting Download PDFInfo
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- CN113913954B CN113913954B CN202111185715.5A CN202111185715A CN113913954B CN 113913954 B CN113913954 B CN 113913954B CN 202111185715 A CN202111185715 A CN 202111185715A CN 113913954 B CN113913954 B CN 113913954B
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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
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
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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
- D01D1/00—Treatment of filament-forming or like material
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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
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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Abstract
The invention discloses a device and a method for preparing superfine nano-fibers based on solution atomization and electrostatic-airflow take-over drafting. The method comprises the steps of firstly atomizing a spinning solution into ultra-fine liquid drops by using an atomization technology, then pre-drafting the atomized liquid drops into fine jet flows by using an electrostatic drafting technology, and finally drafting the pre-drafted jet flows into ultra-fine nano fibers by using an electric field attenuated by air flow instead. The invention adopts the spinning method that the spinning solution is atomized into super-micro liquid drops and then directly drafted to form the superfine nano fiber, changes the mode that the Taylor cone splits to form jet flow in the conventional electrostatic spinning, and provides a new mechanism for the formation of the electrostatic spinning nano fiber; meanwhile, the electrostatic-airflow take-over drafting can remarkably enhance the jet drafting force, so that the micro atomized liquid drops can be thinned to be below 100 nm. The extremely fine diameter of the nanofiber enables the nano effect to be more remarkable, and the nanofiber has more outstanding performance advantages when being applied to the fields of filtration, sensing and the like.
Description
Technical Field
The invention belongs to the field of spinning, relates to a nanofiber forming method, and particularly relates to a superfine nanofiber preparation device and method based on solution atomization and electrostatic-airflow succession drafting, which are applied to the fields of filtration, sensing and the like.
Background
The nano-fiber is used as a fiber material, and has the advantages of small diameter, large specific surface area, high porosity and the like, so that the nano-fiber has wide application prospects in the fields of filtration, biology, sensing and the like. At present, methods for preparing nanofibers mainly include a self-assembly method, a phase separation method, a drawing method, a template method, an electrostatic spinning method and the like, and electrostatic spinning is considered to be the simplest and most effective method for industrially preparing nanofibers, and the principle of the method is to draw and thin a polymer solution/melt into nanofibers through electric field force. In the new crown epidemic situation period, a plurality of companies such as national poly-da, jiangxi Xijiuxi, jiangsu nano-fiber and the like successfully develop products such as an electrostatic spinning nano-fiber mask, a protective garment and the like, the filtration efficiency of the product is obviously superior to that of a melt-blown fiber product, and the huge market development potential is displayed.
Although the electrostatic spinning nano-fiber has better market prospect and application value, the electrostatic spinning nano-fiber in the current academia and market refers to the fiber with the diameter of less than 1 μm, and most of the electrostatic spinning nano-fiber which can be stably applied is hundreds of nanometers in length and belongs to submicron grade. The existing research shows that the nanometer effect of the superfine nano-fiber with the size below 100 nm is more obvious, and the superfine nano-fiber can show more outstanding performance advantages when being applied to the fields of filtration, sensing and the like. Therefore, the method for preparing the superfine nano-fiber is developed, the nano effect is fully exerted, the performance advantage is endowed to the fiber material, and the method has important significance for improving the international market competitiveness of nano-fiber in China.
Disclosure of Invention
Aiming at the market demand and the preparation technology bottleneck of the superfine nanofiber, the invention provides a superfine nanofiber preparation device and method based on solution atomization and electrostatic-airflow succession drafting. Firstly, atomizing a spinning solution into ultra-fine droplets by using a bubble atomization technology, then pre-drafting the atomized droplets into fine jet flows by using an electrostatic drafting technology, and finally drafting the pre-drafted jet flows into ultra-fine nanofibers by using an electric field with attenuated airflow succession. The superfine nano fiber has excellent nano effect, shows outstanding performance advantages in the fields of filtration, sensing and the like, and has better application prospect.
In order to solve the technical problem, the invention adopts the following technical scheme:
a spinning device for superfine nanofibers based on solution atomization and electrostatic-airflow take-over drafting comprises a liquid supply device, two spinning units, a gas supply device, two gas nozzles, a high-pressure generation device, a receiving device, a negative pressure fan, a guide roller and a winding device, wherein the liquid supply device is connected with the spinning units; the positive electrode and the negative electrode of the high-voltage generating device are respectively connected with the two spinning units; the air nozzle and the receiving device are respectively arranged right above and below the central axes of the two spinning units, and the receiving device is connected with the negative pressure fan.
Furthermore, the distance between the two spinning units is 2-50 cm, the distance between the receiving device and the air nozzle is 20-100 cm, and the distance between the air nozzle and the horizontal line where the two spinning units are located is 1-10 cm.
Further, the spinning unit consists of a liquid inlet, a liquid chamber, an air inlet, an air chamber and a spinning nozzle; the diameter of the air chamber is 2-10 cm, the diameter of the liquid chamber is 1-9 cm, a certain number of round holes are formed in the wall surface of the liquid chamber along the circumferential direction, the diameter of each round hole is 0.1-5 mm, the hole spacing is 0.1-5 mm, and the diameter of the spinning nozzle is 0.1-9 mm.
Furthermore, the gas nozzle is a hollow round tube with a contraction and expansion structure, the contraction and expansion structure comprises an inlet section, a middle section and an outlet section, the diameter of the middle section is smaller than that of the inlet section and that of the outlet section, and the diameter of the middle section is 1-10 mm.
Furthermore, the receiving device is a round pipe with round holes on the surface, the diameter of the round pipe is 1-1000 mm, the aperture of the round holes on the surface is 1-20 mm, and the hole spacing is 1-10 mm.
Further, the guide roller is 1-1000 mm in diameter, and the winding device is 1-1000 mm in diameter.
The device of the invention is used for preparing superfine nano-fibers based on solution atomization and electrostatic-airflow succession drafting, and the superfine nano-fibers are formed by directly drafting atomized liquid drops. The method comprises the steps of firstly atomizing a spinning solution into superfine droplets by utilizing a bubble atomization technology, then pre-drafting the atomized droplets into fine jet flows by utilizing an electrostatic drafting technology, and finally drafting the pre-drafted jet flows into superfine nano fibers by utilizing an electric field attenuated by air flow instead.
The invention relates to a preparation method of superfine nano-fibers based on solution atomization and electrostatic-airflow take-over drafting, which comprises the following steps:
(1) Dissolving any one or more high molecular polymers capable of electrostatic spinning in a single or mixed organic solvent, and stirring for several hours under a certain temperature condition to obtain a polymer spinning solution with the mass fraction of 2% -30%;
(2) The liquid supply device quantitatively conveys the spinning solution to a liquid chamber of the spinning unit at a constant speed, the gas supply device conveys gas to a gas chamber of the spinning unit according to a certain pressure, and the gas enters the liquid chamber through a circular hole in the wall surface of the liquid chamber. The solution flow is 10-1000 ml/h, and the gas pressure is 0.001-1 MPa. The gas and the solution are mixed in the liquid chamber to form a gas-liquid mixture containing a large number of bubbles, and then the gas-liquid mixture flows out through the spinning nozzle under the pushing action of the solution. After the gas-liquid mixture flows out of the spinning nozzle, a large number of bubbles contained in the gas-liquid mixture are burst under the action of the internal and external pressure difference of the spinning nozzle, and the solution is smashed to be atomized to form ultra-fine liquid drops;
(3) And (3) opening the high-voltage generating device, and applying positive voltage and negative voltage to the two spinning units respectively to form a conjugated electric field between the two spinning units. The positive voltage is 0-50 kV, and the negative voltage is-50-0 kV. The ultra-many micro liquid drops sprayed from the two spinning units are respectively charged with positive charges and negative charges in a conjugated electric field, are pre-drafted by the electric field force to form fine jet flows, and move to the central axes of the two spinning units. When the fine jet flows meet at the central axis, the charges are neutralized;
(4) The gas supply device quantitatively delivers gas to the gas nozzle at a constant speed, and the gas enters from the inlet section and is sprayed out through the outlet section. After the structure of the conveyed gas is changed in three stages through the gas nozzle, the gas speed is obviously improved, and the gas speed at the inlet is more than 5 m/s. The ejected high-speed gas meets the fine jet flow which is pre-drawn at the central axis of the two spinning units, the fine jet flow is driven to move along the flowing direction of the high-speed gas by attraction, the fine jet flow is drawn and refined into superfine nano fibers, and the fiber diameter is less than 100 nm;
(5) And (3) opening a negative pressure fan to form negative pressure suction on the surface of the receiving device, so that the superfine nanofibers formed in the step (4) are deposited on the surface of the receiving device under the combined action of the negative pressure suction and the high-speed gas drafting force to form a nanofiber film, and then the nanofiber film is conveyed to a winding device under the action of a guide roller to obtain a continuous nanofiber package. The flow rate of the negative pressure fan is more than 1000 ml/h. The rotating speed of the receiving device is more than 0.1 m/h, the rotating speed of the guide roller is more than 0.1 m/h, and the rotating speed of the winding device is more than 0.1 m/h.
The invention has the beneficial effects that: the invention adopts the spinning method that the spinning solution is firstly atomized into super-micro liquid drops and then directly drafted to form the superfine nano fiber, changes the mode that the Taylor cone splits to form jet flow in the conventional electrostatic spinning, and provides a new mechanism for the formation of the electrostatic spinning nano fiber; meanwhile, the electrostatic-airflow alternative drafting can obviously enhance the jet drafting force, so that the tiny atomized liquid drops can be thinned to be below 100 nm, and reliable theoretical guidance and technical support are provided for developing the preparation technology of the superfine nano fibers. The extremely fine diameter of the nanofiber enables the nano effect to be more remarkable, and the nanofiber has more outstanding performance advantages when being applied to the fields of filtering, sensing and the like.
Drawings
FIG. 1 is a schematic diagram of an apparatus for forming ultra-fine nanofibers based on solution atomization and electrostatic-pneumatic succeed drafting;
FIG. 2 is a schematic diagram of a spinning unit structure;
FIG. 3 is a schematic view of the structure of the air nozzle;
FIG. 4 is an electron microscope image of very fine polyacrylonitrile nanofibers.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
As shown in fig. 1, the spinning apparatus for superfine nanofibers based on solution atomization and electrostatic-air flow alternative drafting of the present embodiment includes a liquid supply device 1, a spinning unit 2, an air supply device 3, an air nozzle 4, a high voltage generation device 5, a receiving device 6, a negative pressure fan 7, a guide roller 8 and a winding device 9, wherein the liquid supply device 1 is connected to the spinning unit 2, the two spinning units 2 are horizontally disposed opposite to each other with a distance of 2-50 cm, and the spinning unit 2 and the air nozzle 4 are respectively connected to the air supply device 3; the positive electrode and the negative electrode of the high-voltage generating device 5 are respectively connected with the two spinning units 2; the air nozzle 4 and the receiving device 6 are respectively arranged right above and right below the central axis of the two spinning units 2, the distance between the receiving device 6 and the air nozzle 4 is 20-100 cm, the distance between the air nozzle 4 and the horizontal line of the two spinning units 2 is 1-10 cm, and the receiving device 6 is connected with a negative pressure fan 7.
As shown in fig. 2, the spinning unit 2 is composed of a liquid inlet 14, a liquid chamber 15, an air inlet 16, an air chamber 17 and a spinning nozzle 20; the diameter of the air chamber 17 is 2-10 cm, the diameter of the liquid chamber 15 is 1-9 cm, a certain number of round holes 18 are formed in the wall surface of the liquid chamber 15 along the circumferential direction, the diameter of each round hole 18 is 0.1-5 mm, the hole spacing is 0.1-5 mm, and the diameter of the spinning nozzle 20 is 0.1-9 mm.
As shown in fig. 3, the gas nozzle 4 is a hollow circular tube with a converging-diverging structure, the converging-diverging structure is composed of three stages, namely an inlet section 21, a middle section 22 and an outlet section 23, the diameter of the middle section 22 is smaller than that of the inlet section 21 and that of the outlet section 23, and the diameter of the middle section 22 is 1-10 mm.
The receiving device 6 is a round pipe with a round hole on the surface, the diameter of the round pipe is 1-1000 mm, the aperture of the round hole on the surface is 1-20 mm, the hole distance is 1-10 mm, the diameter of the guide roller 8 is 1-1000 mm, and the diameter of the winding device 9 is 1-1000 mm.
Example 2
The preparation steps of the ultrafine nanofibers based on solution atomization and electrostatic-air flow alternative drafting of this example are as follows:
(1) Dissolving Polyacrylonitrile (PAN) powder in an N, N-dimethylformamide solvent, and stirring for 6 hours at 80 ℃ to obtain a PAN spinning solution with the mass fraction of 4%;
(2) The liquid supply device 1 quantitatively conveys the PAN spinning solution to a liquid chamber 15 of the spinning unit 2 at a constant speed, and the solution flow is 300 ml/h. The gas supply device 3 delivers gas to a gas chamber 17 of the spinning unit 2 at a certain pressure, and the gas enters the liquid chamber through a circular hole 18 on the wall surface of the liquid chamber 15, and the gas pressure is 0.3 MPa. The gas and PAN spinning solution mix in the liquid chamber to form a gas-liquid mixture 19 containing a large number of bubbles, which then flows out through the spinning nozzle 20 under the driving action of the PAN spinning solution. After the gas-liquid mixture flows out of the spinning nozzle, a large number of bubbles contained in the gas-liquid mixture are burst under the action of the internal and external pressure difference of the spinning nozzle, and the solution is smashed to be atomized to form ultra-fine liquid drops 10.
(3) And (3) opening the high voltage generating device 5, and applying positive voltage and negative voltage to the two spinning units respectively to form a conjugated electric field between the two spinning units. The positive voltage was 35 kV, and the negative voltage was-35 kV. The ultra-many micro liquid drops sprayed from the two spinning units are respectively charged with positive charges and negative charges in a conjugated electric field, are pre-drafted by the electric field force to form fine jet flows 11, and move to the central axes of the two spinning units. When the fine jets meet at the central axis, the charge is neutralized.
(4) The gas supply device 3 uniformly and quantitatively conveys gas to the gas nozzle 4, and the gas enters from the inlet section and is sprayed out through the outlet section. After the structure of the conveyed gas is changed in three stages through the gas nozzle, the gas speed is obviously improved, and the inlet gas speed is 100 m/s. The ejected high-speed gas meets the fine jet flow of the pre-drafting at the central axis of the two spinning units, the fine jet flow is driven to move along the flowing direction of the high-speed gas by attraction, and the fine jet flow is drafted and refined into the superfine nano-fiber 12.
(5) And (3) opening a negative pressure fan 7 to form negative pressure suction on the surface of the receiving device, so that the superfine nanofibers 12 formed in the step (4) are deposited on the surface of the receiving device under the combined action of the negative pressure suction and the high-speed gas drafting force to form a nanofiber film 13, and then the nanofiber film is conveyed to a winding device 9 under the action of a guide roller 8 to obtain continuous packages. The flow rate of the negative pressure fan is 3000 ml/h. The rotating speed of the receiving device is 2 m/h, the rotating speed of the guide roller is 2 m/h, and the rotating speed of the winding device is 2 m/h.
Example 3
The preparation steps of the ultrafine nanofibers based on solution atomization and electrostatic-air flow alternative drafting of this example are as follows:
(1) Dissolving Polyacrylonitrile (PAN) powder in an N, N-dimethylformamide solvent, and stirring for 6 hours at 80 ℃ to obtain a PAN spinning solution with the mass fraction of 12%;
(2) The liquid supply device quantitatively conveys the PAN spinning solution to a liquid chamber of the spinning unit at a constant speed, and the solution flow rate is 300 ml/h. The air supply device conveys air to an air chamber of the spinning unit according to a certain pressure, the air enters the liquid chamber through a round hole in the wall surface of the liquid chamber, and the air pressure is 0.3 MPa. The gas and the PAN spinning solution are mixed in the liquid chamber to form a gas-liquid mixture containing a large number of bubbles, and then the gas-liquid mixture flows out through the spinning nozzle under the pushing action of the PAN spinning solution. After the gas-liquid mixture flows out of the spinning nozzle, a large number of bubbles contained in the gas-liquid mixture are burst under the action of the internal and external pressure difference of the spinning nozzle, and the solution is smashed to be atomized to form ultra-fine liquid drops.
(3) And (3) opening the high-voltage generating device, and applying positive voltage and negative voltage to the two spinning units respectively to form a conjugated electric field between the two spinning units. The positive voltage was 35 kV, and the negative voltage was-35 kV. The ultra-many micro liquid drops sprayed from the two spinning units are respectively charged with positive charges and negative charges in a conjugated electric field, are pre-drafted by the electric field force to form fine jet flows, and move to the central axes of the two spinning units. When the fine jets meet at the central axis, the charge is neutralized.
(4) The gas supply device quantitatively delivers gas to the gas nozzle at a constant speed, and the gas enters from the inlet section and is sprayed out through the outlet section. After the structure of the conveyed gas is changed in three stages through the gas nozzle, the gas speed is obviously improved, and the inlet gas speed is 100 m/s. The sprayed high-speed gas meets the pre-drawn fine jet flow at the central axis of the two spinning units, the fine jet flow is driven to move along the flowing direction of the high-speed gas by attraction, and the fine jet flow is drawn and refined into superfine nano fibers.
(5) And (5) opening a negative pressure fan to form negative pressure suction on the surface of the receiving device, so that the superfine nanofibers formed in the step (4) are deposited on the surface of the receiving device under the combined action of the negative pressure suction and the high-speed gas drafting force to form a nanofiber film, and then the nanofiber film is conveyed to a winding device under the action of a guide roller to obtain continuous packages. The flow rate of the negative pressure fan is 3000 ml/h. The rotating speed of the receiving device is 2 m/h, the rotating speed of the guide roller is 2 m/h, and the rotating speed of the winding device is 2 m/h.
Example 4
The preparation procedure of the very fine nanofibers based on solution atomization and electrostatic-pneumatic take-over drawing of this example is as follows:
(1) Dissolving Polyacrylonitrile (PAN) powder in an N, N-dimethylformamide solvent, and stirring for 6 hours at 80 ℃ to obtain a PAN spinning solution with the mass fraction of 8%;
(2) The liquid supply device quantitatively conveys the PAN spinning solution to a liquid chamber of the spinning unit at a constant speed, and the solution flow rate is 300 ml/h. The air supply device conveys air to an air chamber of the spinning unit according to a certain pressure, the air enters the liquid chamber through a round hole in the wall surface of the liquid chamber, and the air pressure is 0.5 MPa. The gas and PAN spinning solution are mixed in the liquid chamber to form a gas-liquid mixture containing a large number of bubbles, and then the gas-liquid mixture flows out through the spinning nozzle under the pushing action of the PAN spinning solution. After the gas-liquid mixture flows out of the spinning nozzle, a large number of bubbles contained in the gas-liquid mixture are burst under the action of the internal and external pressure difference of the spinning nozzle, and the solution is broken and atomized to form ultra-fine liquid drops.
(3) And (3) opening the high-voltage generating device, and applying positive voltage and negative voltage to the two spinning units respectively to form a conjugated electric field between the two spinning units. The positive voltage was 35 kV, and the negative voltage was-35 kV. The ultra-many micro liquid drops sprayed from the two spinning units are respectively charged with positive charges and negative charges in a conjugated electric field, are pre-drawn by the electric field force to form fine jet flows, and move to the central axes of the two spinning units. When the fine jets meet at the central axis, the charge is neutralized.
(4) The gas supply device quantitatively delivers gas to the gas nozzle at a constant speed, and the gas enters from the inlet section and is sprayed out through the outlet section. After the structure of the conveyed gas is changed in three stages through the gas nozzle, the gas velocity is obviously improved, and the inlet gas velocity is 150 m/s. The sprayed high-speed gas meets the pre-drawn fine jet flow at the central axis of the two spinning units, the fine jet flow is driven to move along the flowing direction of the high-speed gas by attraction, and the fine jet flow is drawn and refined into superfine nano fibers.
(5) And (5) opening a negative pressure fan to form negative pressure suction on the surface of the receiving device, so that the superfine nanofibers formed in the step (4) are deposited on the surface of the receiving device under the combined action of the negative pressure suction and the high-speed gas drafting force to form a nanofiber film, and then the nanofiber film is conveyed to a winding device under the action of a guide roller to obtain continuous packages. The flow rate of the negative pressure fan is 3000 ml/h. The rotating speed of the receiving device is 2 m/h, the rotating speed of the guide roller is 2 m/h, and the rotating speed of the winding device is 2 m/h.
Example 5
The preparation procedure of the very fine nanofibers based on solution atomization and electrostatic-pneumatic take-over drawing of this example is as follows:
(1) Dissolving Polyamide (PA) powder in a formic acid solvent, and stirring for 6 hours at 60 ℃ to obtain a PA spinning solution with the mass fraction of 8%;
(2) The liquid supply device quantitatively conveys the PA spinning solution to a liquid chamber of the spinning unit at a constant speed, and the solution flow is 200 ml/h. The air supply device conveys air to an air chamber of the spinning unit according to a certain pressure, the air enters the liquid chamber through a round hole in the wall surface of the liquid chamber, and the air pressure is 0.3 MPa. The gas is mixed with the PA spinning solution in the liquid chamber to form a gas-liquid mixture containing a large number of bubbles, and then the gas-liquid mixture flows out through the spinning nozzle under the pushing action of the PA spinning solution. After the gas-liquid mixture flows out of the spinning nozzle, a large number of bubbles contained in the gas-liquid mixture are burst under the action of the internal and external pressure difference of the spinning nozzle, and the solution is smashed to be atomized to form ultra-fine liquid drops.
(3) And (3) opening the high-voltage generating device, and applying positive voltage and negative voltage to the two spinning units respectively to form a conjugated electric field between the two spinning units. The positive voltage was 20 kV, and the negative voltage was-20 kV. The ultra-many micro liquid drops sprayed from the two spinning units are respectively charged with positive charges and negative charges in a conjugated electric field, are pre-drafted by the electric field force to form fine jet flows, and move to the central axes of the two spinning units. When the fine jets meet at the central axis, the charge is neutralized.
(4) The gas supply device quantitatively delivers gas to the gas nozzle at a constant speed, and the gas enters from the inlet section and is sprayed out through the outlet section. After the structure of the conveyed gas is changed in three stages through the gas nozzle, the gas speed is obviously improved, and the inlet gas speed is 100 m/s. The ejected high-speed gas meets the fine jet flow of the pre-drafting at the central axis of the two spinning units, the fine jet flow is driven to move along the flowing direction of the high-speed gas by attraction, and the fine jet flow is drafted and refined into the superfine nano-fiber.
(5) And (5) opening a negative pressure fan to form negative pressure suction on the surface of the receiving device, so that the superfine nanofibers formed in the step (4) are deposited on the surface of the receiving device under the combined action of the negative pressure suction and the high-speed gas drafting force to form a nanofiber film, and then the nanofiber film is conveyed to a winding device under the action of a guide roller to obtain continuous packages. The flow rate of the negative pressure fan is 3000 ml/h. The rotating speed of the receiving device is 1 m/h, the rotating speed of the guide roller is 1 m/h, and the rotating speed of the winding device is 1 m/h.
The method comprises the steps of firstly atomizing a spinning solution into ultra-fine liquid drops by using an atomization technology, then pre-drafting the atomized liquid drops into fine jet flows by using an electrostatic drafting technology, and finally drafting the pre-drafted jet flows into ultra-fine nano fibers by using an electric field with airflow replacing attenuation. The invention adopts the spinning method that the spinning solution is firstly atomized into super-micro liquid drops and then directly drafted to form the superfine nano fiber, changes the mode that the Taylor cone splits to form jet flow in the conventional electrostatic spinning, and provides a new mechanism for the formation of the electrostatic spinning nano fiber; meanwhile, the electrostatic-airflow take-over drafting can obviously enhance the jet drafting force, so that the micro atomized liquid drops can be thinned to be below 100 nm, the nanometer effect of the superfine nanofiber is more obvious due to the superfine diameter of the nanofiber, and the superfine nanofiber has more outstanding performance advantages when being applied to the fields of filtration, sensing and the like.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A spinning device of superfine nano-fiber based on solution atomization and electrostatic-airflow succession drafting is characterized in that: the device comprises a liquid supply device (1), spinning units (2), a gas supply device (3), gas nozzles (4), a high-pressure generating device (5), a receiving device (6), a negative pressure fan (7), guide rollers (8) and a winding device (9), wherein the liquid supply device (1) is connected with the spinning units (2), the number of the spinning units (2) is two, the two spinning units (2) are horizontally and oppositely arranged, and the spinning units (2) and the gas nozzles (4) are respectively connected with the gas supply device (3); the positive electrode and the negative electrode of the high-voltage generating device (5) are respectively connected with the two spinning units (2); the air nozzle (4) and the receiving device (6) are respectively arranged right above and right below the central axes of the two spinning units (2), and the receiving device (6) is connected with a negative pressure fan (7);
the distance between the two spinning units (2) is 2-50 cm, the distance between the receiving device (6) and the air nozzle (4) is 20-100 cm, and the distance between the air nozzle (4) and the horizontal line where the two spinning units (2) are located is 1-10 cm;
the gas nozzle (4) is a hollow round tube with a contraction and expansion structure, the contraction and expansion structure consists of three stages, namely an inlet section (21), a middle section (22) and an outlet section (23), the diameter of the middle section (22) is smaller than that of the inlet section (21) and that of the outlet section (23), and the diameter of the middle section (22) is 1-10 mm;
the spinning unit (2) is composed of a liquid inlet (14), a liquid chamber (15), an air inlet (16), an air chamber (17) and a spinning nozzle (20); the diameter of the air chamber (17) is 2-10 cm, the diameter of the liquid chamber (15) is 1-9 cm, a certain number of round holes (18) are formed in the wall surface of the liquid chamber (15) along the circumferential direction, the diameter of each round hole (18) is 0.1-5 mm, the hole spacing is 0.1-5 mm, and the diameter of the spinning nozzle (20) is 0.1-9 mm;
the two spinning units are respectively applied with positive voltage and negative voltage to form a conjugate electric field between the two spinning units, ultra-many tiny liquid drops sprayed from the two spinning units are respectively charged with positive charges and negative charges in the conjugate electric field, and are pre-drawn by electric field force to form tiny jet flows which move to the central axes of the two spinning units.
2. Spinning apparatus according to claim 1, characterised in that: the receiving device (6) is a round pipe with round holes on the surface, the diameter is 1-1000 mm, the aperture of the round holes on the surface is 1-20 mm, and the hole distance is 1-10 mm.
3. Spinning apparatus according to claim 1, characterised in that: the diameter of the guide roller (8) is 1-1000 mm, and the diameter of the winding device (9) is 1-1000 mm.
4. A process for the preparation of very fine nanofibers by means of the spinning apparatus according to any of claims 1 to 3, based on solution atomization and electrostatic-pneumatic drawing-in succession, characterized in that: firstly, atomizing a spinning solution into ultra-fine droplets by using a bubble atomization technology, then pre-drafting the atomized droplets into fine jet flows by using an electrostatic drafting technology, and finally drafting the pre-drafted jet flows into ultra-fine nanofibers by using an electric field with attenuated airflow succession.
5. The process for preparing ultrafine nanofibers according to claim 4, comprising the steps of:
(1) Dissolving any one or more high molecular polymers capable of electrostatic spinning in a single or mixed organic solvent to obtain a polymer spinning solution with the mass fraction of 2-30%;
(2) The liquid supply device quantitatively conveys spinning solution to a liquid chamber of the spinning unit at a constant speed, the gas supply device conveys gas to a gas chamber of the spinning unit, the gas enters the liquid chamber through a round hole in the wall surface of the liquid chamber, the solution flow is 10-1000 ml/h, and the gas pressure is 0.001-1 MPa; the gas and the solution are mixed in the liquid chamber to form a gas-liquid mixture (19) containing a large number of bubbles, and then the gas-liquid mixture flows out through the spinning nozzle under the pushing action of the solution; after the gas-liquid mixture flows out of the spinning nozzle, a large number of bubbles contained in the gas-liquid mixture are burst under the action of the internal and external pressure difference of the spinning nozzle, and the solution is smashed to be atomized to form ultra-fine liquid drops (10);
(3) Opening the high-voltage generating device, applying positive voltage and negative voltage to the two spinning units respectively to form a conjugate electric field between the two spinning units, wherein the positive voltage is 0-50 kV, the negative voltage is-50-0 kV, the ultra-many micro liquid drops sprayed from the two spinning units are respectively charged with positive charges and negative charges in the conjugate electric field, are pre-drawn by electric field force to form fine jet flow (11) and move to the central axis of the two spinning units; when the fine jet flows meet at the central axis, the charges are neutralized;
(4) The gas supply device quantitatively conveys gas to the gas nozzle at a constant speed, the gas enters from the inlet section and is sprayed out from the outlet section, the conveyed gas is remarkably improved in speed after the structure of the three stages of the gas nozzle is changed, the speed of the inlet gas is more than 5 m/s, the sprayed high-speed gas meets the pre-drawn fine jet flow at the central axis of the two spinning units, the fine jet flows are attracted and driven to move along the flowing direction of the high-speed gas, the fine jet flow is drawn and refined into superfine nano fibers (12), and the diameter of the superfine nano fibers (12) is less than 100 nm;
(5) And (3) opening a negative pressure fan to form negative pressure suction on the surface of the receiving device, so that the superfine nanofibers formed in the step (4) are deposited on the surface of the receiving device under the combined action of the negative pressure suction and the high-speed gas drafting force to form a nanofiber film (13), and then the nanofiber film is conveyed to a winding device under the action of a guide roller to obtain a continuous nanofiber package.
6. The process for producing ultrafine nanofibers according to claim 5, wherein: in the step (5), the flow rate of the negative pressure fan is more than 1000 ml/h, the rotating speed of the receiving device is more than 0.1 m/h, the rotating speed of the guide roller is more than 0.1 m/h, and the rotating speed of the winding device is more than 0.1 m/h.
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