KR20030003925A - An eletronic spinning aparatus, and a process of preparing nonwoven fabric using the thereof - Google Patents

Abstract

PURPOSE: A process of preparing a nonwoven fabric using an electrospinning device containing a nozzle block comprising many pins enabling mass production of nanofibers and a spinning liquid drop apparatus for discontinuously supplying a spinning solution to the nozzle block is provided, which allows mass production of the nonwoven fabric and enables the thickness and width of the nonwoven fabric to be easily controlled. CONSTITUTION: A spinning solution drop apparatus is arranged between a measuring pumper and a nozzle block of an electrospinning device comprising a spinning solution main tank, measuring pumper, nozzle block and collector. The spinning solution drop apparatus is cylindrical in shape and has a spinning solution inducing pipe(3c) and a gas inlet pipe(3b) connected to a filter(3a) at the upper part, a spinning solution outlet pipe(3d) at the lower part and a hollow part for dropping the spinning solution from the spinning solution inducing pipe at the intermediate part.

Description

Electrospinning apparatus and manufacturing method of nonwoven fabric using same {An eletronic spinning aparatus, and a process of preparing nonwoven fabric using the groom}

The present invention relates to an electrospinning apparatus capable of mass-producing nanofibers and a method of manufacturing a nonwoven fabric using the same.

Conventional electrospinning apparatuses described in US 4,044,404 and the like and a method of manufacturing the nonwoven fabric using the same are as follows. Conventional electrospinning apparatus has a spinning liquid main tank (1) for storing the spinning liquid, a metering pump (2) for the quantitative supply of spinning liquid, a plurality of nozzles for discharging the spinning liquid, the fibers are located at the bottom of the nozzle It consists of a collector 6 that integrates, a voltage generator 11 for generating a voltage, and mechanisms for transferring the generated voltage to the nozzle and the collector 6.

Looking at the conventional nonwoven fabric manufacturing method using the electrospinning apparatus in detail, the spinning liquid in the spinning liquid main tank 1 is continuously metered into a plurality of nozzles to which a high voltage is applied through a metering pump.

Subsequently, the spinning liquid supplied to the nozzles is spun and concentrated through the nozzle onto the collector 6 under high voltage to form a single fiber web.

Subsequently, the short fiber web is embossed or needle punched to produce a nonwoven fabric.

Such a conventional electrospinning apparatus and a method of manufacturing a nonwoven fabric using the same have a problem in that the electric force effect imparted is lowered because the spinning liquid is continuously supplied to a nozzle having a high voltage applied thereto.

More specifically, since the electric force applied to the nozzle is dispersed in all the spinning liquid, the electric force does not overcome the interfacial tension of the spinning liquid, and as a result, the fiber forming effect by the electric force is lowered, thereby making it difficult to mass-produce.

In addition, since the spinning liquid is radiated through a plurality of nozzles, that is, it is not divided into nozzle blocks, which makes it difficult to control the width and thickness of the nonwoven fabric.

An object of the present invention is to maximize the electric force effect imparted to the nozzle block (4) during electrospinning, in other words to increase the electric force greater than the interfacial tension of the spinning liquid to enhance the fiber forming effect, the electricity that can mass-produce nanofibers It is intended to provide a spinning device.

Another object of the present invention is to provide a method that can easily control the thickness and width of the nonwoven fabric when manufacturing a nonwoven fabric using an electrospinning device having a nozzle block connecting a large number of pins.

The present invention provides a nozzle block consisting of a plurality of fins and a spinning liquid drop device for discontinuously supplying spinning liquid to the nozzle block (a temporary block of the flow of the spinning liquid at least once) to enable mass production of nanofibers. To provide an electrospinning apparatus having a. In another aspect, the present invention is to provide a method for manufacturing a nonwoven fabric that can easily control the thickness and width of the nonwoven fabric and mass production by using the electrospinning apparatus.

1 is a schematic view of the electrospinning apparatus of the present invention.

Figure 2 (a) is a cross-sectional view of the spinning liquid drop device (3).

Figure 2 (b) is a perspective view of the spinning liquid drop device (3).

Figure 2 (c) is a plan view of the spinning liquid drop device (3).

2 (d) is an enlarged view of the filter of the spinning liquid dropping apparatus 3.

3 is a process schematic diagram of combining two inventive electrospinning devices.

4 is an electron micrograph of a nonwoven fabric produced by the method of the present invention using a spinning solution in which nylon 6 is dissolved in formic acid.

5 is an enlarged electron micrograph of FIG. 4.

6 is an electron micrograph of a nonwoven fabric produced by the method of the present invention using a spinning solution in which poly (L-lactide) is dissolved in methylene collide.

7 is a diameter distribution diagram of fibers prepared by electrospinning a copolymer spinning solution of poly (glycolide-lactide) by the method of the present invention.

8 is an electron micrograph of a nonwoven fabric prepared by the method of the present invention using a spinning solution in which polyvinyl alcohol is dissolved in tertiary distilled water.

9 is an enlarged electron micrograph of FIG. 8.

10 is an electron micrograph showing a dispersion state of a nonwoven fabric electrospun with a nozzle width distributed at 90 cm.

※ Explanation of main parts in drawings

1: spinning liquid main tank 2: metering pump 3: spinning liquid drop device

4 nozzle block 5 voltage transfer rod 6 collector (conveyor belt)

7,8: support roller 9: embossing roller 10: winding roller

11: voltage generator 3a: filter of the spinning liquid drop device

3b: gas inlet tube 3c: spinning liquid induction tube 3d: spinning liquid discharge tube

The electrospinning apparatus of the present invention for achieving these problems has a cylindrical shape (i) hermetically sealed between the metering pump 2 and the nozzle block 4, and (ii) at the upper end of the spinning liquid induction pipe ( 3c) and a gas inlet tube 3b having a gas inlet and a gas inlet connected to the filter 3a are arranged side by side, and (i) a spinneret discharge tube 3d protrudes at the lower end thereof. (Iii) The middle part is characterized in that the spinning solution dropping device 3 is provided with hollow portions each of which a spinning solution can be dropped from the spinning guide tube 3c.

In addition, in the method of manufacturing the nonwoven fabric of the present invention, before the spinning solution is supplied to the nozzle block 4 under voltage during electrospinning, the spinning solution is passed through the dropping device 3 to block the flow of the spinning solution more than once (drop It is characterized by.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

In the electrospinning apparatus of the present invention, as shown in FIG. 1, the main liquid tank (1) for storing the spinning liquid, the metering pump (2) for supplying the spinning liquid, and a nozzle composed of a plurality of pins are combined in a block form. Nozzle block (4) for discharging the spinning liquid in the form of a fiber, a collector (6) for accumulating the short fibers are located at the bottom of the nozzle block, a voltage generator (11) for generating a high voltage, a voltage generated by the voltage generator It is composed of a voltage transfer rod (5) for transmitting to the upper end of the nozzle block and the spinning liquid drop device (3) located between the metering pump (2) and the nozzle block (4).

The spinning liquid drop device 3 has a cylindrical shape as a whole, as shown in Figs. 3 (a) to 3 (d). At the upper end of the spinning liquid dropping device 3, a spinning liquid induction pipe 3c and a gas inlet pipe 3b for guiding the spinning liquid toward the nozzle block are arranged side by side. At this time, it is preferable to form the spinning liquid induction pipe (3c) slightly longer than the gas inlet pipe (3b).

Gas is introduced from the lower end of the gas inlet pipe, the first gas is introduced portion is connected to the filter (3a) of the shape as shown in Figure 3 (d). At the lower end of the spinning drop device 3, a spinning liquid discharge pipe 3d for guiding the dropped spinning liquid to the nozzle block 4 is formed. The middle part of the spinning drop device 3 is formed in a hollow state so that the spinning liquid can be dropped at the distal end of the spinning guide tube 3c.

The spinning liquid flowing into the spinning liquid dropping device 3 flows down along the spinning liquid induction pipe 3c and is dropped at its distal end to block the flow of the spinning liquid more than once.

Looking at the principle that the spinning liquid is dropped (drop), when the gas is introduced into the upper end of the closed spinning liquid drop device 3 along the filter (3d) and the gas inlet pipe (3b), the spinning liquid is induced by gas vortex, etc. The pressure in the tube 3c becomes naturally irregular, and the spinning liquid drops due to the pressure difference that occurs.

As the gas introduced in the present invention, an inert gas such as air or nitrogen may be used.

On the other hand, the nozzle block 4 is arranged in a block unit consisting of two or more pins (pin). The number of pins formed in one nozzle block 4 is preferably 2-100,000, more preferably 20-2,000. The nozzle pin may have a circular or shaped cross section and may have a needle shape. The nozzle pins can be arranged in circumferential, lattice, or line. More preferably, they are arranged in a line.

Next, look at a method of manufacturing a nonwoven fabric using the electrospinning apparatus of the present invention.

First, the thermoplastic resin or the thermosetting resin spinning liquid stored in the main tank 1 is metered by the metering pump 2 and supplied to the spinning liquid dropping device 3 by quantity. In this case, the thermoplastic or thermosetting resin for preparing the spinning solution may be polyester resin, acrylic resin, phenol resin, epoxy resin, nylon resin, poly (glycolide / L-lactide) copolymer, poly (L-lactide) resin, Polyvinyl alcohol resin, polyvinyl chloride resin and the like can be used. As the spinning solution, any of the above resin melts or solutions may be used.

In this way, the spinning liquid supplied into the spinning liquid dropping device 3 passes through the spinning liquid dropping device 3 while being discontinuously, in other words, the clouding of the spinning liquid is blocked at least once in accordance with the above-described mechanism. The high voltage of is supplied to the hanging nozzle block (4).

Subsequently, the nozzle block 4 discharges the spinning liquid onto the short fibers through the nozzle, and accumulates it on the collector 6 under high voltage to produce a nonwoven web.

At this time, the voltage transfer rod 5 and the collector 6 installed at the upper end of the nozzle block 4 in order to promote the fiber formation by the electric force is applied 1kV or more, more preferably 20kV or more generated from the voltage generator 11 Walk. It is more advantageous in terms of productivity to use an endless belt as the collect 6.

In this way, when the nonwoven fabric formed by continuously processing the nonwoven web formed on the collector 6 with the embossing roller 9 is wound on the winding roller 10, the nonwoven fabric manufacturing process is completed.

In the manufacturing method of the present invention, the spinning solution is dropped at least once when the spinning solution is supplied to the nozzle block 4 using the spinning solution drop device 3, thereby maximizing fiber formation. As a result, the fiber-forming effect by the electric force is increased, it is possible to mass-produce nanofibers and nonwoven fabrics. In addition, the manufacturing method of the present invention can freely change and adjust the width and thickness of the nonwoven fabric by arranging nozzles composed of a plurality of pins in a block form.

In the case where two or more electrospinning apparatuses of the present invention are arranged and used, polymers of various components can be freely combined with each other, making it easier to manufacture a hybrid nonwoven fabric.

According to the method of the present invention, the diameter of the fiber spun by melt spinning is 1,000 nm or more, and the diameter of the fiber spun by solution spinning is 1 to 500 nm. The solution spinning method includes both wet spinning and dry spinning.

Non-woven fabric composed of nanofibers is used for various purposes such as artificial leather, sanitary napkins, filters, medical materials such as artificial blood vessels, winter vests, semiconductor wipers, and battery nonwoven fabrics.

Hereinafter, the present invention will be described in more detail with reference to Examples.

Example 1

In a 96% sulfuric acid solution, a nylon 6 chip having a relative viscosity of 2.3 was dissolved in formic acid at 20% to prepare a spinning solution. While storing the spinning solution in the main tank (1), the metering pump (2) is quantitatively metered and supplied to the spinning solution drop device (3) of Figure 2 to discontinuously switch the flow of spinning solution. Subsequently, the spinning solution was supplied to a nozzle block 4 under a voltage of 50 kV and spun into fibers through the nozzle, and the spun fibers were accumulated on the collector 6 to have a width of 60 cm and a weight of 3.0 g / A nonwoven web of 2 m 2 is produced. At this time, the number of pins per nozzle block was set to 200, and such a nozzle block was used by arranging 200 blocks. Simco's Model C H 50 was used as the voltage generator. The discharge amount per pin was set at 0.0027 g / min (discharge amount per nozzle block: 0.54 g / min) so that the total discharge amount was 108 g / min. One nozzle block was subdivided into ten pieces, and one spinning solution drop device (3) was installed for every 20 pins. Drop speed was set at 3 second intervals. Subsequently, the nonwoven web is embossed while being transported at a speed of 60 m / min to produce a nonwoven fabric. Tensile strength, tensile elongation and electron micrograph of the prepared nonwoven fabric are shown in Table 1.

Example 2

Poly (L-lactide) having a viscosity average molecular weight of 450,000 was dissolved in methylene chloride to prepare a spinning solution. While storing the spinning solution in the main tank (1), the metering pump (2) is quantitatively metered and supplied to the spinning solution drop device (3) of Figure 2 to discontinuously switch the flow of spinning solution. Subsequently, the spinning solution was supplied to a nozzle block 4 under a voltage of 50 kV and spun into fibers through a nozzle, and the spun fibers were accumulated on the collector 6 to be 60 cm in width and 6.9 g / weight. A nonwoven web of 2 m 2 is produced. At this time, the number of pins per nozzle block was 400, and such a block was used in an array of 20 blocks. Simco's Model C H 50 was used as the voltage generator. The discharge amount per pin was set at 0.0026 g / min so that the total discharge amount was 20.8 g / min. One nozzle block was further subdivided into ten and one spinning solution drop device (3) was installed for every 40 pins. Drop speed was set at 3.2 second intervals. Subsequently, the nonwoven web is embossed while being transported at a speed of 5 m / min to produce a nonwoven fabric. Tensile strength, tensile elongation and electron micrograph of the prepared nonwoven fabric are shown in Table 1.

Example 3

A spinning solution was prepared by dissolving a poly (glycolide-lactide) copolymer (molar ratio: 50/50) having a viscosity average molecular weight of 450,000 in methylene chloride. While storing the spinning solution in the main tank (1), the metering pump (2) is quantitatively metered and supplied to the spinning solution drop device (3) of Figure 2 to discontinuously switch the flow of spinning solution. Subsequently, the spinning solution was supplied to a nozzle block 4 subjected to a voltage of 50 kV and spun into fibers through the nozzle, and the spun fibers were accumulated on the collector 6 to be 60 cm in width and 8.53 g in weight. A nonwoven web of 2 m 2 is produced. At this time, the number of pins per nozzle block was 400, and such a block was used in an array of 20 blocks. Simco's Model C H 50 was used as the voltage generator. The discharge amount per pin was set to 0.0032 g / min (discharge amount per nozzle block: 1.28 g / min) so that the total discharge amount was 25.6 g / min. One nozzle block was further subdivided into ten and one spinning solution drop device (3) was installed for every 40 pins. Drop speed was set at 2 second intervals. Subsequently, the nonwoven web is embossed while being transported at a speed of 5 m / min to produce a nonwoven fabric. Tensile strength, tensile elongation and electron micrograph of the prepared nonwoven fabric are shown in Table 1.

Example 4

A polyvinyl alcohol having a number average molecular weight of 20,000 was dissolved in tertiary distilled water to prepare a spinning solution. While storing the spinning solution in the main tank (1), the metering pump (2) is quantitatively metered and supplied to the spinning solution drop device (3) of Figure 2 to discontinuously switch the flow of spinning solution. Subsequently, the spinning solution was supplied to a nozzle block 4 subjected to a voltage of 50 kV and spun into fibers through the nozzle, and the spun fibers were accumulated on the collector 6 to have a width of 60 cm and a weight of 3.87 g / A nonwoven web of 2 m 2 is produced. At this time, the number of pins per nozzle block was 400, and such a block was used in an array of 20 blocks. Simco's Model C H 50 was used as the voltage generator. The discharge amount per pin was set to 0.0029 g / min (discharge amount per nozzle block: 1.28 g / min) so that the total discharge amount was 23.2 g / min. One nozzle block was further subdivided into ten and one spinning solution drop device (3) was installed for every 40 pins. Drop speed was set at 2.5 second intervals. Subsequently, the nonwoven web is embossed while being transported at a speed of 10 m / min to produce a nonwoven fabric. Tensile strength, tensile elongation and electron micrograph of the prepared nonwoven fabric are shown in Table 1.

Property evaluation result division Tensile strength (kg / cm) Tensile Elongation (%) Electron micrograph Example 1 180 25 4 and 5 Example 2 180 25 6 Example 3 100 28 7 Example 4 120 32 8 and 9

※ The tensile strength and tensile elongation are the result measured by ASTM D 1117 method.

The present invention can mass-produce a nonwoven fabric composed of nanofibers, and can easily adjust the thickness and width of the nonwoven fabric. In addition, when two or more electrospinning apparatuses of the present invention are combined, a multicomponent polymer can be freely combined, and thus a hybrid nonwoven fabric can be easily manufactured.

Claims (10)

Spinning liquid main tank (1), metering pump (2), nozzle block (4), a collector (6), a voltage generator (11) and the voltage that are located at the bottom of the nozzle block (4) to accumulate fibers 1. An electrospinning device composed of mechanisms for transmitting a voltage generated in the generator to the nozzle block 4 and the collector 6, between the metering pump 2 and the nozzle block 4; (Iii) has a closed cylindrical shape, (Ii) an upper end portion of the spinning liquid induction tube 3c and a gas inlet tube 3b in which gas is introduced into the lower end and the gas inlet is connected to the filter 3a are arranged side by side; (Iii) At the lower end thereof, a spinning liquid discharge pipe 3d protrudes, (Iii) An electrospinning apparatus, characterized in that a middle portion is provided with a spinning liquid dropping device (3), each of which has a hollow portion in which the spinning liquid can be dropped from the spinning liquid induction pipe (3c). 2. An electrospinning apparatus according to claim 1, wherein the nozzles are arranged in block units consisting of two or more pins or needles. The electrospinning apparatus according to claim 1 or 2, wherein the number of pins of one nozzle block is 2 to 100,000. The electrospinning apparatus according to claim 1 or 2, wherein the shape of the nozzle pins is a circular or a deformed cross section. The electrospinning apparatus according to claim 1 or 2, wherein the nozzle pins are arranged circumferentially, latticely or in a row. In manufacturing the nonwoven fabric by electrospinning the thermoplastic resin or thermosetting resin spinning liquid from the nozzle block 4 onto the collector 6 and subsequently embossing it, the metering pump 2 in the spinning liquid main tank 1 Before supplying the spinning solution supplied via the quantitatively to the nozzle block 4 under voltage; (Iii) has a closed cylindrical shape, (Ii) an upper end portion of the spinning liquid induction tube 3c and a gas inlet tube 3b in which gas is introduced into the lower end and the gas inlet is connected to the filter 3a are arranged side by side; (Iii) At the lower end thereof, a spinning liquid discharge pipe 3d protrudes, (Iii) A method for producing a nonwoven fabric, characterized in that the intermediate part passes through each of the spinning solution dropping apparatuses 3, each of which has a hollow portion through which the spinning solution can be dropped from the spinning guide tube 3c. . The method for manufacturing a nonwoven fabric according to claim 6, wherein the nozzles are arranged in block units consisting of two or more pins. Method according to claim 6, characterized in that air or inert gas is introduced into the spinning liquid dropping device (3). The method for producing a nonwoven fabric according to claim 6, wherein the spinning solution is a melt or a solution. 7. A method for producing a nonwoven fabric as claimed in claim 6, characterized in that an endless belt is used as the collector (6).