WO2012087025A2

WO2012087025A2 - Electrospinning apparatus comprising a spinning tube having a plurality of spounting holes

Info

Publication number: WO2012087025A2
Application number: PCT/KR2011/009935
Authority: WO
Inventors: 김학용; 남기택; 백우일
Original assignee: 전북대학교산학협력단
Priority date: 2010-12-22
Filing date: 2011-12-21
Publication date: 2012-06-28
Also published as: KR20120070780A; WO2012087025A3; WO2012087025A9; KR101172266B1

Abstract

The present invention relates to an electrospinning apparatus comprising a spinning tube having a plurality of spouting holes, in which the spinning tube which is rotatable and having a plurality of spouting holes instead of conventional nozzles is employed as means for electrospinning a spinning solution in the direction of a collector. According to the present invention, electrospinning is performed using both electrostatic force and centrifugal force, thereby increasing discharge amount of unit polygonal tube per unit time and thus significantly improving productivity. Compared to conventional electrospinning apparatuses that use nozzles, the necessity of replacing and cleaning nozzles is eliminated and production processes are thus simplified. As the collector is located above the spinning tube having the plurality of spouting holes, a phenomenon (drop phenomenon) in which the spinning solution in a solution state not a fibrous state drops onto the collector during electrospinning is prevented to improve the quality of the nanofiber web being produced.

Description

Electrospinning apparatus comprising a spinning tube formed with a plurality of discharge holes

The present invention relates to an electrospinning apparatus including a spinning tube having a plurality of discharge holes, and more particularly, to a spinning liquid, and a spinning tube having a structure in which a plurality of discharge holes are formed instead of a conventional nozzle. It relates to an electrospinning apparatus.

Conventional electrospinning apparatuses have mainly adopted a nozzle (Nozzle) fixed as a mechanism for discharging the spinning liquid, as disclosed in Republic of Korea Patent No. 10-0420460.

However, since the conventional electrospinning apparatus electrospins the spinning liquid through a fixed nozzle, the electrospinning is carried out only on the electrostatic force, so that the discharge amount per nozzle per nozzle per unit time is very low at 0.01g, resulting in low productivity. Difficult problems, nozzle replacement and cleaning are very complicated and cumbersome.

In general, the production of nanofibers through electrospinning is in the order of 0.1-1 g per hour, and the solution discharge rate is very low, 1.0-5.0 mL per hour [D. H. H. Renecker et al., Nanptechnology 2006, VOl 17, 1123].

Another conventional electrospinning apparatus is an electrospinning apparatus for electrospinning the spinning liquid (polymethyl methacrylate solution dissolved in chlorobenzene) using only a centrifugal force by using a cylinder rotating at a high speed of 3,000 rpm or more. K. Kern et al., Published in Nano Letters (Nano Letters, 2008, Vol 8, No. 4, 1187-1191).

However, since the conventional electrospinning devices are electrospun using only centrifugal force without using electrostatic force, the yield decreases, and it is difficult to continuously supply the spinning liquid into the cylinder, which makes continuous production difficult.

In another conventional electrospinning apparatus, Jinyuan of Nanzhou University, electrospinning without nozzle using electrostatic force and centrifugal force by supplying polyvinylpyrilidone solution while applying high voltage to a conical container rotating at 50rpm Zhou et al. Are published in a small paper published in Small, 2010 (Small, 2010 Vol 6, 1612-1616).

However, the conventional electrospinning device can improve the output per unit time in the form of a nozzle by utilizing the centrifugal force and the electrostatic force, but it is difficult to continuously produce by supplying the spinning liquid in the conical container, and the lower portion of the conical container There is a problem that the collector is located and the spinning liquid falls into a solution state rather than a fiber form (hereinafter referred to as "drop generation phenomenon").

In addition, a method of electrospinning a system in which a large number of nozzles are arranged on a nozzle plate is well known [H. Y. Kim, WO2005073441, WO2007035011.

The disadvantage of the conventional electrospinning method is that the production of nanofibers per unit hole is very low, and there is a problem in that nozzle cleaning is cumbersome.

The problem of the present invention is to use a combination of electrostatic and centrifugal force to solve the above problems, a plurality of discharge holes are formed in place of the conventional nozzle and by electrospinning the spinning liquid with a spinning spinning tube per unit spinning tube per unit time The discharge amount is increased, the productivity is greatly improved, the trouble of nozzle replacement and cleaning can be eliminated, the drop occurrence phenomenon can be effectively prevented, and the spinning solution is supplied continuously to provide an electrospinning device capable of continuous production.

In order to achieve the above object, in the present invention, the spinning liquid main tank (a) storing and storing the spinning liquid, the spinning liquid stored and stored in the spinning liquid main tank (b) and the tube block (d) and a plurality of discharges The spinning solution supply pump (c) for supplying the spinning tube (e) having holes (h) formed therein, the spinning solution is supplied to the spinning tube (e) while storing the spinning solution supplied from the spinning main tank (b). A tube block (d), a plurality of discharge holes (h) are formed, the spinning tube is arranged on the tube block (d) to rotate and electrospin the spinning liquid in the direction of the collector through the discharge holes (h) (e) a spinning tube support (f) in the form of a tube supporting the spinning tube (e) while being rotated in a state arranged on the tube block (d) in combination with the spinning tube (e), and the spinning tube ( e) rotating at the state of high voltage, The collector for integrating the nanofibers electrospun from the discharge holes (h) formed in the tube (e), the high voltage generator (a) and the motor (g) for applying a high voltage to each of the tube block (d) and the collector and the A plurality of discharge holes are formed, comprising a spinning tube support rotating device comprising a motor and a gear connecting the radiating tube support (f) and one kind of power transmission mechanism (p) selected from the belt. It provides an electrospinning device consisting of electrospinning devices comprising a spinning tube.

According to the present invention, electrospinning is performed using a combination of electrostatic and centrifugal forces, thereby increasing the amount of discharge per unit spinning tube per unit time, thereby greatly improving productivity, and eliminating the need for nozzle replacement and cleaning compared to using a nozzle. Since the collector is located on the top of the spinning tube, the effect of improving the quality of the nanofiber web produced by preventing the dropping (drop phenomenon) of the spinning liquid on the collector in the form of a solution rather than fibrous during electrospinning is achieved. have.

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

FIG. 2 is an enlarged view of a portion of the spinning tube e and the spinning tube support f arranged in the tube block d in FIG.

3 to 9 are cross-sectional views showing an arrangement of discharge holes h formed on the spinning tube e constituting the electrospinning device of the present invention.

10 (a) to 10 (z) are enlarged cross-sectional views of one example of a cross-sectional shape of the discharge hole h formed on the spinning tube e.

a: high voltage generator b: spinning liquid main tank

c: spinning liquid supply pump d: tube block

e: spinning tube f: spinning tube support

h: discharge hole formed on the spinning tube

g: motor p: power train

i: collector k: bearing

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

First, the present invention, as shown in Figure 1, the spinning liquid main tank (a) for storing and storing the spinning liquid, the spinning liquid stored and stored in the spinning liquid main tank (b) tube block (d) and a plurality of Spinning liquid supply pump (c) for supplying to the spinning tube (e) formed with the discharge holes (h), while supplying the spinning liquid supplied from the spinning liquid main tank (b) to the spinning tube (e), Hanging tube block (d), a plurality of discharge holes (h) are formed, the radiation is arranged on the tube block (d) to rotate the spinning liquid electrospinning the spinning liquid in the direction of the collector through the discharge holes (h) A tube (e), a spinning tube support (f) in the form of a tube supporting the spinning tube (e) while rotating in an arrangement on the tube block (d) in a state coupled with the spinning tube (e), the spinning Located at the top of the tube (e) while rotating under a high voltage applied, spinning tube (e) A collector for integrating the nanofibers electrospun from the discharge holes (h) formed, a high voltage generator (a) and a motor (g) and the motor (g) for applying a high voltage to each of the tube block (d) and the collector; It comprises a spinning tube formed with a plurality of discharge holes characterized in that consisting of a spinning tube support rotating device consisting of one of the power transmission mechanism (p) selected from the gear and belt connecting the spinning tube support (f) It consists of electrospinning devices.

1 is a schematic view of the electrospinning apparatus according to the present invention, the radiation tube support (f) is omitted without showing in detail the state connected to the power transmission mechanism (p).

The spinning tube support f is rotated by a spinning tube support rotating device consisting of a motor g and a power transmission mechanism p, whereby the spinning tube e coupled with the spinning tube support f is also rotated. Done.

The rotation speed of the spinning tube (e) is generally 50 rpm or more.

If the rotation speed is too low, the centrifugal force is low, the nanofiber forming ability is lowered. If the rotation speed is too high, a drop phenomenon occurs in which the spinning solution is injected into the solution itself, not nanofibers, in the discharge hole (h) formed in the spinning tube (e). Not preferred.

However, since the appropriate number of rotations of the spinning tube (e) depends on the diameter, number, number of array rows, and arrangement of the discharge holes (h) formed in the spinning tube (e), in the present invention, the number of rotations is limited to a specific range. It is not.

Specifically, the spinning tube supports f rotate in connection with the motor g by a power transmission mechanism p, which is a gear or a belt.

As a specific embodiment, each of the radiating tube supports f is provided with gears, which are power transmission mechanisms p, engaged with each other, as shown in FIG. 2, and one of the gears is connected to the motor g. Rotate in engagement with another connected gear.

FIG. 2 is a detailed enlarged view of the portion of the spinning tube e and the spinning tube support f arranged on the tube block d in FIG. 1.

As shown in FIG. 2, a bearing k is attached to each of the radiation tube supports f.

The bearing (k) is preferably made of ceramics, metals or high-performance polymers, etc., depending on the corrosiveness of the solvent used to produce the spinning solution.

In another specific embodiment, each of the polygonal tube supports f is rotated in connection with the motor g by a belt which is a power transmission mechanism p.

The radiation tube (e) may be integrally fixed to the radiation tube supporter (f) in a non-separable manner, or may be secured to be detachable in a one-touch manner, but it may be detachably fixed. It is preferable because it is easy to clean and replace parts.

The spinning tube support f is preferably a cylindrical tube, having a diameter of 3 mm or more, but is not necessarily cylindrical.

In the spinning tube e, a plurality of discharge holes h are arranged on the spinning tube e as exemplarily shown in FIGS. 3 to 9.

Specifically, the discharge holes (h) formed in the spinning tube (e) are arranged in the circumferential direction or diagonal direction on the spinning tube (e).

3 to 9 are cross-sectional schematic diagrams illustrating the arrangement method of the discharge holes h and the cross-sectional shape of the discharge holes h formed on the spinning tube e.

Specifically, as shown in FIG. 3, the discharge holes h having a slit shape may be arranged in the form of alternately changing the long axis / short axis direction on the same concentric circle along the circumferential direction on the radiation tube e.

In addition, as illustrated in FIG. 4, the slit-shaped discharge holes h may be arranged along the circumferential direction on the radiation tube e in the long axis / short axis direction on the same concentric circle.

In addition, as shown in FIG. 5, the discharge holes h having a slit shape may be arranged on the radiating tube e in a manner of changing the long axis / short axis direction by different concentric circles along the circumferential direction.

In addition, as shown in FIG. 6, the discharge holes h in the form of arrow marks may be arranged on the radiation tube e in the same direction in the discharge holes h facing each other in all concentric circles along the circumferential direction. As illustrated in FIG. 7, the discharge holes h in the form of arrow marks may be arranged in different directions on the radiating tube e to face each other in different concentric circles along the circumferential direction. .

Also, as shown in FIG. 8, different shapes, for example, a slit shape and an asterisk shape, may be arranged alternately on the same concentric circle along the circumferential direction on the radiation tube e, as shown in FIG. 9. Likewise, discharge holes h of the same shape are arranged on the inner concentric circle along the circumferential direction on the radiation tube e, for example, asterisk, and different from the discharge holes arranged on the inner concentric circle on the outer concentric circle, eg For example, the slit discharge holes h may be arranged.

Since the size of the discharge holes h and the distance between the discharge holes h vary depending on the shape and arrangement method of the discharge holes h, the present invention is not particularly limited thereto.

In other words, the cross-sectional shape of the discharge hole (h) formed in the spinning tube (e) has a circular, slit-shaped, two or more angles as exemplarily shown in Figure 10 (a) to Figure 10 (z). Polygons, Hangul consonant forms, Hangul vowel forms, English alphabet forms, numeric forms such as 1, 2, Greek numeral forms, Greek character forms, various marker forms such as arrows, and the like, and are illustrated by way of example in FIGS. 8 to 9. As described above, two or more discharge holes h having different shapes may be arranged together on the same radiation tube e.

As the collector furnace, an endless belt, a drum or a roller is used.

If the collector is an endless belt, a nanofiber web is produced, and if it is a drum or roller, a nanofiber filament is produced.

In this case, the electrospun nanofibers are arranged in the direction of rotation of the collector in the form of a drum or roller, and the nanofiber filaments are manufactured by concentrating the arranged nanofibers.

The spinning tube supports (f) are arranged in a straight or diagonal direction on the tube block (d), so that more spinning tube supports (f) can be arranged on the tube block (d) to increase productivity per unit time. Increase and the device is simplified.

Next, with reference to Figure 1 looks at an example of a method for producing a nanofiber web with an electrospinning apparatus according to the present invention.

After dissolving in a polymer solvent, a predetermined amount of spinning liquid stored in the spinning liquid main tank (b) is supplied to the tube block (d) through which a high voltage is applied through a supply pump (c). In this way, the spinning liquid supplied to the tube block d is attached to the spinning tube support f on the tube block d through the discharge holes h formed in the spinning tube e, which rotates. The nanofibers are fabricated by integrating the nanofibers onto the collector by electrospinning toward the rotating collector while being placed at the top and a high voltage is applied thereto.

When the nanofiber web is manufactured as described above, electrospinning is performed by using both electrostatic and centrifugal forces to increase the discharge amount per spinning tube per unit time, thereby greatly improving productivity, and the cumbersome nozzle replacement and cleaning due to the conventional nozzle. The operation can be omitted, and the collector is located on the top of the spinning tube (e) to prevent the drop phenomenon to improve the quality of the nanofiber web.

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

However, the present invention is not limited by the following examples.

Example 1

First, polyvinyl alcohol (Aldrich, USA) was dissolved in distilled water by 10% by weight to prepare a spinning solution.

Next, as shown in FIG. 1, a high voltage is applied to a predetermined amount of the spinning liquid stored in the spinning liquid main tank b through the supply pump c, and the discharge holes h of the slit type are arranged and formed as shown in FIG. 4. The spinning tube (e) and the spinning tube support (f) were fed to the tube block (d) arranged in a closed state.

The slit-shaped discharge hole h has a width of 0.5 mm, a length of 3 mm, and the radiation tube e has a diameter of 50 mm, and the eighteen concentric circles are arranged along the circumferential direction of the radiation tube e. The discharge holes h are arranged, and 36 discharge holes are arranged in the outer concentric circles, and 54 discharge holes are arranged as a whole.

A voltage of 45 kV was applied to the tube block d.

Subsequently, as described above, the spinning liquid supplied to the tube block (d) is arranged in the spinning tube (e) and formed by electrospinning in the direction of the collector located above the spinning tube (e) through the discharge holes (h) formed. Nanofiber webs were prepared by integrating the nanofibers onto the collector.

At this time, the discharge amount per unit time per spinning tube (e) was 18g / min.

At this time, a voltage of 45 kV was applied to the collector and the collector was rotated at a rotation speed of 3.6 m / min.

In addition, the width of the collector was 2,2m, the distance between the collector and the spinning tube (e) was adjusted to 27cm.

In addition, the spinning tube (e) was rotated at 150rpm by connecting to the motor by a belt which is a power transmission mechanism.

Thus, the average diameter of the nanofibers was 220 nm, and the weight of the nanofiber webs was 41.5 g / m 2.

The diameters of the nanofibers constituting the nanofiber web were very uniform, and no drop phenomenon occurred.

The present invention is a method that can produce a large amount of nanofibers, in particular, the productivity is greatly improved, can eliminate the hassle of nozzle replacement and cleaning, can effectively prevent the occurrence of drop, continuous supply of spinning liquid As industrially available.

Claims

  Spinning liquid main tank (a) for storing and storing the spinning liquid,

  Spinning liquid supply pump (c) for supplying the spinning liquid stored and stored in the spinning liquid main tank (b) to the spinning tube (e) formed with a tube block (d) and a plurality of discharge holes (h),

  A tube block (d) for supplying to the spinning tube (e) while storing the spinning liquid supplied from the spinning liquid main tank (b), the high voltage is applied,

  A plurality of discharge holes (h) are formed, the discharge tube (e) is arranged on the tube block (d) to rotate the electrospinning of the spinning liquid in the collector direction through the discharge holes (h)

  Spinning tube support (f) in the form of a tube supporting the spinning tube (e) while rotating in the state arranged on the tube block (d) coupled to the spinning tube (e)

  Located at the top of the spinning tube (e) while rotating in a high voltage applied state, the collector for integrating the nanofibers electrospun from the discharge holes (h) formed in the spinning tube (e)

  High voltage generator (a) for applying a high voltage to each of the tube block (d) and the collector and

  And a spinning tube support rotating device comprising a motor (g) and a gear and belt connecting the motor (g) and the spinning tube support (f), one kind of power transmission mechanism (p) selected. Electrospinning apparatus comprising a radiation tube formed with a plurality of discharge holes.
According to claim 1, wherein each of the radiating tube support (f) is provided with gears, which are power transmission mechanism (p) in engagement with each other, one of the gears in engagement with another gear connected to the motor (g) Electrospinning apparatus comprising a radiation tube formed with a plurality of discharge holes, characterized in that there is.
The electrospinning apparatus according to claim 1, wherein each of the radiation tube supports (f) is connected to the motor (g) by a belt which is a power transmission mechanism.
The electrospinning apparatus of claim 1, wherein a bearing (k) is attached to each of the spinning tube supports (f).
The method of claim 1, wherein the radiation tube support (f) is coupled to the radiation tube (e) in a fixed state and a detachable state selected from one of the plurality of discharge tube formed discharge holes, characterized in that Electrospinning apparatus comprising.
The method of claim 1, wherein the cross-sectional shape of the discharge hole (h) formed in the radiation tube (e) is circular, slit, polygonal with two or more angles, Korean form, English alphabet form, numeric form, Greek numeral form, Electrospinning apparatus comprising a spinning tube formed with a plurality of discharge holes, characterized in that the one type selected from the Greek and marker forms.
The plurality of discharge holes of claim 1, wherein the discharge holes h formed in the radiation tube e are arranged in one direction selected from the circumferential direction and the diagonal direction on the radiation tube e. Electrospinning apparatus comprising a spin tube formed.
2. The plurality of discharge holes of claim 1, wherein two or more discharge holes h having different cross-sectional shapes are arranged in one direction selected from the circumferential direction and the diagonal direction on the radiation tube e. Electrospinning apparatus comprising a spin tube formed.
The method of claim 1, wherein the radiation tube (e) comprises a discharge tube formed with a plurality of discharge holes, characterized in that arranged in one direction selected from the linear direction and diagonal direction on the tube block (d) Spinning device.
The electrospinning apparatus of claim 1, wherein the collector is one selected from an endless belt, a drum, and a roller.