JP2010031398A - Electrostatic spinning method and spinning head for electrostatic spinning - Google Patents

Electrostatic spinning method and spinning head for electrostatic spinning Download PDF

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JP2010031398A
JP2010031398A JP2008191864A JP2008191864A JP2010031398A JP 2010031398 A JP2010031398 A JP 2010031398A JP 2008191864 A JP2008191864 A JP 2008191864A JP 2008191864 A JP2008191864 A JP 2008191864A JP 2010031398 A JP2010031398 A JP 2010031398A
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spinning
liquid tank
nozzle
head
stock solution
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JP5237712B2 (en
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Yoshihiro Yamashita
義裕 山下
Hajime Miyake
肇 三宅
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Shiga Prefectural Government.
University of Shiga Prefecture
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University of Shiga Prefecture
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an electrostatic spinning method that does not stain the external surface of nozzle holes and has small power consumption of direct current high-voltage power source: and to provide a spinning head for electrostatic spinning. <P>SOLUTION: In the electrostatic spinning method with which a spinning dope is introduced to a spinning head 2 equipped with nozzles 8 and discharged from the nozzles 8, a discharged spinning dope is drawn under the influence of an electric field, fiberized and collected on a collection surface, the spinning head 2 includes a liquid tank 4, an inlet 6 directly connected to the liquid tank 4 and introduces the spinning dope to the liquid tank 4, and the nozzles 8 conducted to the liquid tank 4, the material of the spinning head 2 comprises an insulating material and a direct current high voltage is applied between the spinning dope and the collection surface. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、静電紡糸方法に関する。   The present invention relates to an electrospinning method.

静電紡糸は、ノズルのノズル孔から吐出させた紡糸用の溶液に電界を作用させて繊維化する紡糸である。静電紡糸は、繊維径がサブミクロンあるいはナノオーダーの繊維を得ることが可能であり、また溶融紡糸が困難な樹脂でも繊維化が可能なので、従来の繊維を用いては実現できなかった用途分野への展開が期待されている。   Electrostatic spinning is spinning in which an electric field is applied to a spinning solution discharged from a nozzle hole of a nozzle to form a fiber. Electrospinning can obtain fibers with submicron or nano-order fiber diameters, and can be made into fibers even with resins that are difficult to melt-spin, so application fields that could not be realized using conventional fibers Expansion to is expected.

静電紡糸による繊維ウエブの製造は、例えば図７に示すように、分配整流ブロック２０２へ計量ポンプ２０１で送られた、紡糸原液であるポリマー溶液を、口金部２０４へ送り、微細なノズル孔２０８を通して押出しながら同時に直流高圧電源２０６により電場をかけて繊維化し、捕集コンベアからなる集積装置２０７上に集積させることにより行われる。この繊維は、３次元のネットワーク構造を成しており、集積装置２０７で集積されて繊維ウエブ２１０となる。（例えば、特許文献1参照）
特開昭６３−１４５４６５号公報 For example, as shown in FIG. 7, the fiber web is manufactured by electrostatic spinning. The polymer solution, which is a spinning solution, sent to the distribution rectifying block 202 by the metering pump 201 is sent to the base portion 204, and fine nozzle holes 208 are produced. At the same time, an electric field is applied by a DC high-voltage power source 206 while being extruded through the fiber, and the fiber is formed and accumulated on a collecting device 207 formed of a collecting conveyor. The fibers have a three-dimensional network structure, and are accumulated by the accumulation device 207 to become a fiber web 210. (For example, see Patent Document 1)
JP-A 63-145465

図７に示すような静電紡糸においては、直流高圧電源２０６の電極をノズル孔２０８に接続することによりポリマー溶液が印加される。従って、ノズル孔２０８は金属のような導電性の素材からなる。また、口金部２０４も金属製であり導電性を有する。   In the electrostatic spinning as shown in FIG. 7, the polymer solution is applied by connecting the electrode of the DC high voltage power source 206 to the nozzle hole 208. Accordingly, the nozzle hole 208 is made of a conductive material such as metal. The base portion 204 is also made of metal and has conductivity.

ノズル孔２０８が導電性であることによりノズル孔２０８の外周壁面も高電位にあるので、繊維化し空中に放出されたポリマーがその外周壁面に引きつけられて堆積し、ノズル孔２０８の外周壁面が汚れノズル孔の出口近傍にもはみだして紡出の障害になることがある。また、口金部２０４も金属製であり導電性を有するので直流高圧電源２０６の電極に接続された、ノズル孔２０８や口金部２０４のような導電性物質の表面積が大きくなり、その導電性物質の表面から漏洩する電流が多く、直流高圧電源２０６の消費電力が多くなるという問題も生ずる。   Since the nozzle hole 208 is electrically conductive, the outer peripheral wall surface of the nozzle hole 208 is also at a high potential. Therefore, the polymer that is fibrillated and released into the air is attracted to the outer peripheral wall surface and accumulates, and the outer peripheral wall surface of the nozzle hole 208 becomes dirty. There is a possibility that spinning may also occur in the vicinity of the nozzle hole outlet. In addition, since the base part 204 is also made of metal and has conductivity, the surface area of the conductive material such as the nozzle hole 208 and the base part 204 connected to the electrode of the DC high-voltage power source 206 increases, There is also a problem that a large amount of current leaks from the surface and the power consumption of the DC high-voltage power supply 206 increases.

本発明の目的は、ノズル孔の外表面が汚れず、直流高圧電源の消費電力の少ない静電紡糸方法及び静電紡糸用紡糸ヘッドを提供しようとすることである。   An object of the present invention is to provide an electrostatic spinning method and a spinning head for electrostatic spinning in which the outer surface of a nozzle hole is not soiled and the power consumption of a DC high-voltage power supply is low.

本発明の要旨とするところは、紡糸用原液を、ノズルを備えた紡糸ヘッドに導入して前記ノズルから吐出させ、吐出された紡糸用原液に電界を作用させて延伸し繊維化し、捕集面で捕集する静電紡糸方法において、前記紡糸ヘッドが液槽と、該液槽に直結し紡糸用原液を該液槽に導入する導入口と、該液槽に導通する前記ノズルとを含んでなり、前記紡糸ヘッドの素材が絶縁材からなり、紡糸用原液と前記捕集面との間に直流高電圧を印加することを特徴とする静電紡糸方法であることにある。   The gist of the present invention is that a spinning stock solution is introduced into a spinning head equipped with a nozzle and ejected from the nozzle, and an electric field is applied to the ejected spinning stock solution to draw and fiberize the collecting surface. In the electrospinning method collected by the above-mentioned method, the spinning head includes a liquid tank, an inlet port that is directly connected to the liquid tank and introduces a spinning stock solution into the liquid tank, and the nozzle that conducts to the liquid tank. In the electrostatic spinning method, the material of the spinning head is made of an insulating material, and a direct current high voltage is applied between the stock solution for spinning and the collection surface.

また、本発明の要旨とするところは、前記静電紡糸方法に用いられる前記紡糸ヘッドからなる静電紡糸用紡糸ヘッドであることにある。   The gist of the present invention resides in a spinning head for electrospinning comprising the spinning head used in the electrospinning method.

本発明によると、ノズル孔の外表面が汚れず、直流高圧電源の消費電力の少ない静電紡糸方法及び静電紡糸用紡糸ヘッドが提供される。   According to the present invention, an electrostatic spinning method and a spinning head for electrostatic spinning are provided in which the outer surface of the nozzle hole is not soiled and the power consumption of the DC high-voltage power supply is low.

本発明においては、図1に示す紡糸ヘッド２が用いられる。紡糸ヘッド２は、液槽４と、液槽４に直結し紡糸用原液を液槽４に導入する導入口６と、液槽４に導通する複数のノズル８を備える。導入口６には管先１１が取りつけられている。   In the present invention, the spinning head 2 shown in FIG. 1 is used. The spinning head 2 includes a liquid tank 4, an inlet 6 that is directly connected to the liquid tank 4 and introduces the spinning solution into the liquid tank 4, and a plurality of nozzles 8 that are electrically connected to the liquid tank 4. A pipe tip 11 is attached to the introduction port 6.

図２に示すように、紡糸用原液が原液貯留槽１２から連結管１４を介して紡糸ヘッド２の管先１１を経由して液槽４に導入される。原液槽１２には複数の連結管１４が接続されていてそれぞれが各紡糸ヘッド２に連結されている。連結管１４には本態様にあってはシリコーンゴムのようなエラストマーからなるフレキシブルなチューブ１５が用いられ、管先１１がそのチューブ１５の一端部に指し込まれている。紡糸用原液はノズル８から吐出され、繊維化して捕集面１０に捕集される。ノズル８における紡糸用原液の吐出圧の付与は、原液槽１２の水頭ヘッド圧によるものであってもよい。あるいは原液槽１２の下流に不図示の液送ポンプを設けてその液送圧によるものであってもよい。その他、ノズル８に吐出圧を発生させる手段であればとくに制限はない。   As shown in FIG. 2, the stock solution for spinning is introduced from the stock solution storage tank 12 into the liquid tank 4 through the connecting pipe 14 and the pipe tip 11 of the spinning head 2. A plurality of connecting pipes 14 are connected to the stock solution tank 12 and are connected to the spinning heads 2. In this embodiment, a flexible tube 15 made of an elastomer such as silicone rubber is used for the connecting tube 14, and the tube tip 11 is inserted into one end of the tube 15. The spinning undiluted solution is discharged from the nozzle 8, fiberized, and collected on the collection surface 10. The discharge pressure of the spinning stock solution in the nozzle 8 may be applied by the head pressure of the stock solution tank 12. Alternatively, a liquid feed pump (not shown) may be provided downstream of the stock solution tank 12 and the liquid feed pressure may be used. In addition, there is no particular limitation as long as it is a means for generating discharge pressure at the nozzle 8.

図２の図の拡大部に示すように、金属製の、径０．０５〜１ｍｍほどの細い導線１４の一端部１７が管先１１の外周と、その外周に接するチューブ１５の内周との間を通って液槽４の内部に導入されて、液槽４内の紡糸用原液と接触状態にある。導線１４の他端部１９は液槽４の外部にあって、直流高圧電源２０の正極２２に不図示のリード線を介して接続されている。ノズル８の、ノズル孔の貫通方向の延長方向に捕集面２４が設置され、捕集面２４が直流高圧電源２０のアース極２６に不図示のリード線を介して接続されている。これにより、紡糸ヘッド２内の紡糸用原液と捕集面２４との間に直流高電圧が印加される。図２に示す態様においては捕集面２４は捕集コンベアからなる集積装置２７の捕集面であり、紡出された繊維は、３次元のネットワーク構造を成しており、捕集面２４で集積されて繊維ウエブ２９となる。   As shown in the enlarged portion of the drawing of FIG. 2, one end 17 of a thin conductive wire 14 having a diameter of 0.05 to 1 mm made of metal is formed between the outer periphery of the tube tip 11 and the inner periphery of the tube 15 in contact with the outer periphery. The liquid is introduced into the liquid tank 4 through the space and is in contact with the spinning stock solution in the liquid tank 4. The other end 19 of the conducting wire 14 is outside the liquid tank 4 and is connected to the positive electrode 22 of the DC high-voltage power supply 20 via a lead wire (not shown). A collection surface 24 is installed in the direction of extension of the nozzle 8 through the nozzle hole, and the collection surface 24 is connected to the ground electrode 26 of the DC high-voltage power supply 20 via a lead wire (not shown). As a result, a high DC voltage is applied between the spinning solution in the spinning head 2 and the collection surface 24. In the embodiment shown in FIG. 2, the collection surface 24 is a collection surface of an accumulation device 27 composed of a collection conveyor, and the spun fibers have a three-dimensional network structure. The fiber web 29 is accumulated.

紡糸ヘッド２の素材は、絶縁材からなる。絶縁材は、比抵抗が１×１０１０Ω・ｃｍ以上の材料をいう。絶縁材としてはポリエチレン、ポリプロピレンのようなポリオレフィン系樹脂、ポリカーボネート、ポリスチレン、ポリエチレンテレフタレート、ポリブチレンテレフタレートのようなポリエステル系樹脂、ＡＢＳ（アクリル−スチレン−ブタジエン共重合物）などの樹脂が挙げられる。陶磁器のようなセラミックやガラスであってもよい。これらの複合物であってもよい。 The material of the spinning head 2 is made of an insulating material. The insulating material refers to a material having a specific resistance of 1 × 10 10 Ω · cm or more. Examples of the insulating material include polyolefin resins such as polyethylene and polypropylene, polyester resins such as polycarbonate, polystyrene, polyethylene terephthalate and polybutylene terephthalate, and resins such as ABS (acryl-styrene-butadiene copolymer). Ceramics such as ceramics or glass may be used. These composites may be used.

本発明のかかる構成により、ノズル８の外周壁面に直流高圧電源２０の電圧が印加されることがないので、ノズル８の外周壁面へのポリマーの堆積やノズルつまりが防止される。さらに、針金状あるいはリボン状の細い導電性物の先端を紡糸用原液に接触させることにより紡糸用原液を印加しているので、導電部分の表面積が極めて小さく、これにより、電流の空中へのリークが少なくなり直流高圧電源２０の消費電力が極めて小さい。   According to the configuration of the present invention, the voltage of the DC high-voltage power supply 20 is not applied to the outer peripheral wall surface of the nozzle 8, so that polymer accumulation and nozzle clogging on the outer peripheral wall surface of the nozzle 8 are prevented. Furthermore, since the spinning stock solution is applied by bringing the tip of a thin conductive material in the form of a wire or ribbon into contact with the spinning stock solution, the surface area of the conductive portion is extremely small, which causes leakage of current into the air. And the power consumption of the DC high-voltage power supply 20 is extremely small.

本発明においては、図３に示す紡糸ヘッド２ａの要部断面図のように、ノズル８ａが液槽の底壁４ａに着脱自在に取りつけられてもよい。図３においては、ノズル８ａの根元部が円筒状であり、液槽４ａの円筒状のノズル接続部３０が、ノズル８ａの円筒状の根元部３２に着脱自在に嵌入されている。   In the present invention, the nozzle 8a may be detachably attached to the bottom wall 4a of the liquid tank as shown in a cross-sectional view of the main part of the spinning head 2a shown in FIG. In FIG. 3, the base part of the nozzle 8a is cylindrical, and the cylindrical nozzle connection part 30 of the liquid tank 4a is detachably fitted into the cylindrical base part 32 of the nozzle 8a.

本発明においては、図４に示すように、液槽を、液槽上部３４と液槽下部３６とに２つ割にして液槽上部３４と液槽下部３６とが着脱自在に嵌着する構成とすることができる。液槽上部３４には管先１１が一体的に取りつけられている。液槽下部３６にはノズル接続部３０が一体的に取りつけられている。図４は、液槽上部３４の上がわ外壁に補強リブ１５が設けられた態様である。   In the present invention, as shown in FIG. 4, the liquid tank is divided into a liquid tank upper part 34 and a liquid tank lower part 36, and the liquid tank upper part 34 and the liquid tank lower part 36 are detachably fitted. It can be. The pipe tip 11 is integrally attached to the liquid tank upper part 34. A nozzle connecting portion 30 is integrally attached to the liquid tank lower portion 36. FIG. 4 is a mode in which the reinforcing rib 15 is provided on the upper outer wall of the liquid tank upper part 34.

このような２つ割の液槽を用いる場合、図５に示すように、紡糸用原液に電圧を印加するための細長い導線（または薄いリボン状金属箔）４０を液槽上部３４ａと液槽下部３６ａとの嵌合部４１を通して液槽内部と挿通状態とし、導線４０の一端部４４を液槽内部の紡糸用原液と接触させ、他端部を直流高圧電源２０の極に不図示のリード線を介して接続してもよい。   When such a two-divided liquid tank is used, as shown in FIG. 5, an elongated conducting wire (or thin ribbon-like metal foil) 40 for applying a voltage to the spinning undiluted solution is provided with a liquid tank upper part 34a and a liquid tank lower part. 36a is inserted into the liquid tank through the fitting part 41, one end 44 of the conductor 40 is brought into contact with the spinning stock solution in the liquid tank, and the other end is connected to the pole of the DC high-voltage power supply 20 (not shown). You may connect via.

本発明の他の態様においては、図６に示すように、原液貯留槽１２（図２）と管先１１（図１など）とを連結する、エラストマーを素材とする絶縁性の連結管１４の少なくとも一部を短い金属管５０に置き換えて、金属管５０と直流高圧電源２０の電極とをリード線５２を介して電気的に接続して、紡糸用原液に電圧を印加してもよい。   In another aspect of the present invention, as shown in FIG. 6, an insulating connecting pipe 14 made of an elastomer is used to connect the stock solution storage tank 12 (FIG. 2) and the pipe tip 11 (FIG. 1, etc.). At least a part of the metal tube 50 may be replaced with the short metal tube 50, and the metal tube 50 and the electrode of the DC high-voltage power supply 20 may be electrically connected via the lead wire 52 to apply a voltage to the spinning dope.

本発明のさらに他の態様においては、原液貯留槽１２（図２）内の紡糸用原液に電極小片を投入し、電極小片をリード線を介して直流高圧電源２０の極に接続して紡糸用原液に電圧を印加してもよい。   In still another embodiment of the present invention, a small piece of electrode is put into the spinning stock solution in the stock solution storage tank 12 (FIG. 2), and the small piece of electrode is connected to the pole of the DC high-voltage power supply 20 via a lead wire for spinning. A voltage may be applied to the stock solution.

ポリエチレンを素材とする、図４に示す形状の液槽上部３４と液槽下部３６とからなる液槽と、図３に示すポリエチレンを素材とするノズル８ａを用い、図２に示す構成で紡出を行った。   Spinning with the structure shown in FIG. 2 using a liquid tank made of polyethylene as a raw material and comprising a liquid tank upper part 34 and a liquid tank lower part 36 having the shape shown in FIG. 4 and a nozzle 8a made of polyethylene shown in FIG. Went.

液槽の下底に１０個のノズルを１０ｍｍ間隔で配した。各ノズルの出口の内径は０．６ｍｍ、長さは４０ｍｍである。ノズルと紡糸用原液との印加電圧を１０ｋＶとして紡出を行った。紡出開始時に吐出量が１ｃｃ／ｍｉｎ／ノズルとなるように原液槽１２の水頭高さを調整した。   Ten nozzles were arranged at 10 mm intervals on the bottom of the liquid tank. The inner diameter of each nozzle outlet is 0.6 mm and the length is 40 mm. Spinning was carried out at an applied voltage of 10 kV between the nozzle and the stock solution for spinning. The head height of the stock solution tank 12 was adjusted so that the discharge rate was 1 cc / min / nozzle at the start of spinning.

捕集された繊維ウエブ２９の目付けが０．２ｇ／ｍ２になるように紡出開始時に捕集面２４の速度を調整し、連続紡出を行った。３０分間の紡出後も、ノズルの外周壁面へのポリマーの付着はごく僅かであり、吐出量の減少もごく僅かであった。 The speed of the collection surface 24 was adjusted at the start of spinning so that the basis weight of the collected fiber web 29 was 0.2 g / m 2 , and continuous spinning was performed. Even after spinning for 30 minutes, the polymer adhered to the outer peripheral wall surface of the nozzle was negligible, and the decrease in the discharge amount was negligible.

比較例Comparative example

実施例と同様にして紡出を行った。ただし、ノズルの素材をステンレスとし、導線１４を用いず、ノズルと直流高圧電源の極とを接続することにより紡糸用原液に電圧を印加した。   Spinning was carried out in the same manner as in the Examples. However, the nozzle was made of stainless steel, and a voltage was applied to the spinning dope by connecting the nozzle and the pole of the DC high-voltage power source without using the lead wire 14.

１０分間後に、ノズルの外周壁面へポリマーの付着が認められ吐出量の減少やノズル先端から液だれを生ずるなど紡出に支障をきたした。   After 10 minutes, adhesion of the polymer was recognized on the outer peripheral wall surface of the nozzle, which caused problems in spinning, such as a decrease in the discharge amount and dripping from the nozzle tip.

表１に実施例、比較例それぞれにおける繊維ウエブの目付けの経時変化を示す。   Table 1 shows changes with time of the basis weight of the fiber web in each of the examples and comparative examples.

Figure 2010031398
Figure 2010031398

その他、本発明は、主旨を逸脱しない範囲で当業者の知識に基づき種々なる改良、修正、変更を加えた態様で実施できるものである。   In addition, the present invention can be carried out in a mode in which various improvements, modifications, and changes are added based on the knowledge of those skilled in the art without departing from the spirit of the present invention.

本発明の静電紡糸方法において用いられる紡糸ヘッドの態様の一例を示す構造説明図である。It is structure explanatory drawing which shows an example of the aspect of the spinning head used in the electrostatic spinning method of this invention. 本発明の静電紡糸方法における紡糸の態様の一例を示す装置レイアウトの説明図である。It is explanatory drawing of the apparatus layout which shows an example of the aspect of spinning in the electrostatic spinning method of this invention. 本発明の静電紡糸方法において用いられる紡糸ヘッドの態様の他の一例を示す要部断面図である。It is principal part sectional drawing which shows another example of the aspect of the spinning head used in the electrostatic spinning method of this invention. 本発明の静電紡糸方法において用いられる紡糸ヘッドの態様のさらに他の一例を示し、図４（ａ）は斜視図、図４（ｂ）は要部正面図、図４（ｃ）は図４（ｂ）のＡ−Ａ方向の断面図である。FIG. 4 shows still another example of the mode of the spinning head used in the electrostatic spinning method of the present invention, FIG. 4 (a) is a perspective view, FIG. 4 (b) is a front view of the main part, and FIG. 4 (c) is FIG. It is sectional drawing of the AA direction of (b). 本発明の静電紡糸方法における紡糸用原液に電圧を印加する態様の一例を示す要部断面模式図である。It is a principal part cross-sectional schematic diagram which shows an example of the aspect which applies a voltage to the stock solution for spinning in the electrostatic spinning method of this invention. 本発明の静電紡糸方法における紡糸用原液に電圧を印加する態様の他の一例を示す要部断面模式図である。It is a principal part cross-sectional schematic diagram which shows another example of the aspect which applies a voltage to the stock solution for spinning in the electrostatic spinning method of this invention. 従来の静電紡糸装置の態様を示す模式図である。It is a schematic diagram which shows the aspect of the conventional electrostatic spinning apparatus.

符号の説明Explanation of symbols

２：紡糸ヘッド
４：液槽
６：導入口
８：ノズル
１１：管先 2: Spinning head 4: Liquid tank 6: Inlet 8: Nozzle 11: Pipe tip

Claims (2)

紡糸用原液を、ノズルを備えた紡糸ヘッドに導入して前記ノズルから吐出させ、吐出された紡糸用原液に電界を作用させて延伸し繊維化し、捕集面で捕集する静電紡糸方法において、前記紡糸ヘッドが液槽と、該液槽に直結し紡糸用原液を該液槽に導入する導入口と、該液槽に導通する前記ノズルとを含んでなり、前記紡糸ヘッドの素材が絶縁材からなり、紡糸用原液と前記捕集面との間に直流高電圧を印加することを特徴とする静電紡糸方法。 In an electrospinning method in which a spinning stock solution is introduced into a spinning head equipped with a nozzle and discharged from the nozzle, and an electric field is applied to the discharged spinning stock solution to draw and fiberize it and collect it on a collecting surface. The spinning head includes a liquid tank, an inlet directly connected to the liquid tank for introducing a spinning stock solution into the liquid tank, and the nozzle electrically connected to the liquid tank, and the material of the spinning head is insulated. An electrostatic spinning method comprising a material and applying a direct high voltage between a spinning stock solution and the collection surface. 請求項１に記載の静電紡糸方法に用いられる前記紡糸ヘッドからなる静電紡糸用紡糸ヘッド。 A spinning head for electrospinning comprising the spinning head used in the electrospinning method according to claim 1.
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