WO2003016601A1 - Dispositif destine a produire des fibres dans le cadre d'un procede de filage electrostatique - Google Patents

Dispositif destine a produire des fibres dans le cadre d'un procede de filage electrostatique Download PDF

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Publication number
WO2003016601A1
WO2003016601A1 PCT/DE2002/002654 DE0202654W WO03016601A1 WO 2003016601 A1 WO2003016601 A1 WO 2003016601A1 DE 0202654 W DE0202654 W DE 0202654W WO 03016601 A1 WO03016601 A1 WO 03016601A1
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WO
WIPO (PCT)
Prior art keywords
spray
electrode
electrodes
plates
polymer
Prior art date
Application number
PCT/DE2002/002654
Other languages
German (de)
English (en)
Inventor
Wolfgang Czado
Original Assignee
Helsa-Werke Helmut Sandler Gmbh & Co. Kg
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Application filed by Helsa-Werke Helmut Sandler Gmbh & Co. Kg filed Critical Helsa-Werke Helmut Sandler Gmbh & Co. Kg
Priority to EP02754394A priority Critical patent/EP1409775B1/fr
Priority to DE50201852T priority patent/DE50201852D1/de
Publication of WO2003016601A1 publication Critical patent/WO2003016601A1/fr

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin

Definitions

  • the present invention relates to a device for producing fibers in an electrostatic spinning process and to a process carried out using this device.
  • Such devices are basically known from the prior art.
  • a polymer in the form of a polymer melt or in the form of a solution is introduced into an electric field and spun into fibers by the action of the electric field.
  • An electrode usually forms a receiving device for the spun fibers, while the counter electrode is designed as a spraying electrode or spray nozzle.
  • the nano and microfibers produced using such a device are not isolated, but are immediately deposited as a fleece.
  • the production of filter materials should be mentioned, for example.
  • the production of a fleece by an electrostatic spinning process is e.g. known from US 4,144,553.
  • Other devices and electrostatic spinning processes are the subject of DE 20 32 072, EP 1 059 106, US 3,994,258, US 4,323,525 and US 4,287,139.
  • a method for electrostatically spinning polymers using this device is also the subject of the invention.
  • a particular advantage of the device according to the invention is that a uniform delivery rate of polymer is ensured over the entire working width of the device without there being any fluctuations in the polymer feed or polymer concentration.
  • the at least one spray electrode or the at least one spray plate has a serrated or corrugated spray edge. It is particularly preferred here if every second tooth or shaft is bent upwards or downwards out of the plane of the spraying electrode or the spraying plate. Such a design of the spray electrode or the spray plate is particularly advantageous compared to a smooth spray edge, since the field effect is increased by the peak effect and thus e.g. a lower high voltage or potential difference between the electrodes is required.
  • Spray electrodes or several spray plates arranged side by side, in particular triangular, trapezoidal, square or rounded Are shape. It is preferred here if the spray electrodes or spray plates are arranged next to one another at a distance in the range from 2 to 10 cm. On the one hand, the peak effect is most pronounced and, on the other hand, the nano and / or microfibers produced by the electrostatic spinning process can be deposited into a particularly regular nonwoven with spray electrodes or spray plates. The same applies, of course, in the aforementioned embodiment with a jagged or corrugated design of the spray electrode or the spray plate. The tips of the spikes or the apexes of the waves are spaced from each other in the range of 2 to 10 cm.
  • the conveyor device is formed by a conveyor roller or a conveyor belt.
  • the conveyor roller or the conveyor belt runs through the polymer solution or melt, with a thin film adhering to the conveyor roller or the conveyor belt.
  • the at least one spray electrode or the at least one spray plate rests at one point on the conveyor roller or the conveyor belt, as a result of which the film of the polymer solution or melt on the conveyor roller or the conveyor belt is scraped off the spray electrode or the spray plate becomes.
  • the polymer solution or the polymer melt runs to the spray edge on the spray electrode or the spray plate, where it sprays evenly due to the high voltage present.
  • this embodiment of the present invention has a conveyor device which is segmented corresponding to the spray electrodes or the spray plates. This ensures that the polymer solution or the polymer melt exclusively in the area of
  • Spray electrodes or spray plates is promoted.
  • the surface of the polymer solution or the polymer melt exposed to the environment is kept as small as possible, so that, for example, unnecessary solvent losses are avoided.
  • the heat loss is kept low, which advantageously contributes to energy savings when operating the device according to the invention.
  • the device according to the invention is closed or encapsulated with a lid such that only the at least one spraying electrode or the at least one spraying plate protrudes from the device. This advantageously further reduces the evaporation of solvents or cooling of the melt.
  • the conveying device is formed by one or more lines or line systems for conveying the polymer solution or the polymer melt from the at least one storage vessel to the at least one spray electrode or the at least one spray plate.
  • the one or more lines or line systems for conveying the polymer solution or the polymer melt from the at least one storage vessel to the at least one spray electrode or the at least one spray plate.
  • Line systems for conveying the polymer solution or polymer melt from the at least one storage vessel are preferably attached to the deepest point of the storage vessel and the polymer solution or polymer melt is conveyed through these lines or line system solely by gravity, the polymer solution or the polymer melt at the end of the lines or
  • the conveying device further comprises a conveying pump for conveying the polymer solution or the polymer melt through the lines or line systems located on the storage vessel.
  • the one or more lines or line systems have outlet openings for the polymer solution or polymer melt in the form of nozzles, in particular in the form of regulatable or adjustable nozzles.
  • the one or more lines or line systems are optional, including any existing nozzles are provided with a heating device, which in particular facilitates the processing of a polymer melt and the susceptibility to failure of the Device reduced. It is particularly preferred if the nozzle or nozzles have an additional solvent supply or supply line and / or an additional compressed air supply line. This enables a solvent supply to the nozzles for cleaning purposes.
  • one or more brushes can be arranged on the nozzle or on the nozzles, which brushes can optionally be rotated.
  • a solvent can be introduced into the nozzle by means of a corresponding supply or feed line or it can be dripped onto the nozzle tip from the outside. It is also possible to e.g. to be cleaned by means of rotating brushes or by means of a blast of compressed air, with solvent optionally being added to the compressed air.
  • spray electrodes or spray plates are particularly subject to the problem of incrustations
  • several spray electrodes or spray plates are arranged on a holding or transport device, the holding or transport device being designed in particular as a circulating belt or as a transport wheel, and the transport device, including the spray electrodes or spray plates at least partially immersed in a cleaning bath for the latter.
  • the transport device is then actuated at certain time intervals, ie new spray electrodes or spray plates are used for electrostatic spinning, while spray electrodes and spray plates which have already been used and are encrusted are immersed in a cleaning bath.
  • the incrustations on the spray electrodes or spray plates can also be completely dried instead of a solvent bath and then removed by a brush or a scraper.
  • spray electrodes or spray plates which can be used only once, a plurality of spray electrodes or spray plates being arranged in a feed device for the same and designed to be detachable by feed. In the operation of this embodiment, a spray electrode or a spray plate is used until there is no longer sufficient efficiency due to incrustations formed.
  • the feed device is then actuated either in a predetermined time interval or controlled by an operator and the used spray electrode or the used spray element is released from the device according to the invention and a new spray electrode or a new spray plate is brought into an operating position for electrostatic spinning of a polymer.
  • the particular advantage of this embodiment is that additional handling of solvents and a corresponding cleaning of the spray electrodes or spray plates can be omitted, as a result of which a higher level of operational safety is achieved, because the effort to completely clean the spray plates or
  • Spray electrodes is comparatively large if the quality of the product, i.e. the fibers or nonwovens produced should be ensured.
  • the counter electrode is preferably formed by a rigid sheet, an electrically conductive, circumferential band or a fleece. It is particularly preferred if the counter electrode is formed by an electrically conductive, circumferential band made of wire mesh or metal foil, this band moving in particular with a carrier material on which the fibers produced by the electrostatic spinning are placed. This avoids the application of tensile forces on the carrier material. It is most preferred if the counter electrode is formed from electrospun fibers of opposite polarity. This carrier material is then simultaneously coated on the top and bottom by two spray devices with fibers of opposite polarity. This creates a much more effective filter material, since a higher charge density can be achieved and both the positive and negative charges are firmly fixed in the fibers.
  • Polymer solutions of various concentrations e.g. Form fibers of different diameters.
  • the prescribed device for electrostatic spinning of polymers is used, the spinning taking place in an electrostatic field with a potential difference between the at least one spraying electrode or the at least one spraying plate and the counter electrode in the range from 5 kV to 1000 kV. Preferably in a field from 10 kV to 100 kV and most preferably in a field from 10 to 50 kV.
  • different spray electrodes or. Spray plates spun different polymer solutions or polymer melts simultaneously and / or different potential differences are applied to different spray electrodes or spray plates during spinning.
  • water-soluble polymers e.g. Polyvinyl alcohol, polyvinyl pyrrolidine, polyethylene oxide and its copolymers, cellulose and its derivatives, starch and mixtures of these polymers.
  • Polymers which are soluble in organic solvents can also be spun in the device according to the invention.
  • Polystyrene, polycarbonate, polyvinyl chloride, polyacrylate, polymethacrylate, polyvinyl acetate, polyvinyl acetal, polyvinyl ether, polyurethane, polyamide, polysulfone, polyether sulfone, polyacrylonitrile, cellulose derivatives and mixtures of these polymers are particularly worth mentioning here.
  • Polymers spinnable from the melt are e.g. Thermoplastics such as polyolefins, polyester, polyoxymethylene, polychlorotrifluoroethylene,
  • Polyphenylene sulfide, polyaryl ether ketone, polyvinylidene fluoride and mixtures of these polymers are added which are able to take up or stabilize a charge.
  • these are metal, without carbon or graphite powder, dyes (especially those with amino groups that can resonate with delocalized electron systems; metallocenes, amino and phosphines. Powders of other, electrically conductive materials such as electrically conductive polymers and ceramics are also suitable ,
  • Figure 1 is a schematic representation of a first embodiment of the device according to the invention.
  • Figure 2 is a schematic plan view of a conveyor roller with adjacent spray electrodes or spray plates;
  • FIG. 3 is a schematic representation of an embodiment in which the
  • Spray electrodes or spray plates are arranged on a transport device
  • FIG. 4 shows a second embodiment of the present invention, in which the spray electrodes or spray plates are arranged on a transport wheel and pass through a cleaning bath;
  • FIG. 5 shows an embodiment in which the spray electrodes or
  • FIG. 1 shows a first embodiment of the device according to the invention for the electrostatic spinning of polymers.
  • a conveyor device 1 formed by a conveyor roller is arranged in a storage container for the polymer solution or the polymer melt 2, the conveyor roller 1 conveying polymer solution or polymer melt from the storage vessel and transferring it to the adjacent spraying electrode 3, generally also referred to as a spraying plate.
  • a high-voltage generator 4 generates the potential difference required between the spray electrode 3 and the counter electrode 5, so that the polymer contained in the storage vessel 2 is spun into fibers 6 in the electrostatic field.
  • FIG. 2 shows a schematic top view of a conveyor roller 1 with spray electrodes 3 attached.
  • a plurality of spray electrodes 3 are arranged next to one another at a distance.
  • FIG. 3 shows an embodiment of the present invention, in which the spray electrodes 3a are arranged on a conveyor belt 7.
  • electrostatic spinning i.e. during operation of the device, polymer solution or polymer melt runs from line 9 onto spray electrode 3a, which has a corresponding potential difference with respect to the counter electrode, so that fibers 6 are detached from spray electrode 3a.
  • FIG. 5 finally shows a schematic illustration of an embodiment in which the spray electrodes 3b are contained in a feed device (not shown) along the line 9 for the supply of the polymer solution or polymer melt.
  • the spray electrodes are moved in the direction of the arrow in the feed device until the first spray electrode 3 b reaches the operating position. Then polymer solution or polymer melt is conveyed through line 9 to the spray electrode 3 b located in the operating position. Since this is for Counter electrode has a corresponding potential difference
  • a 5% polystyrene solution in dichloromethane is mixed with 0.5 rhodamine G6 and spun at 50 revolutions of the conveyor roller (diameter 7 cm) per minute.
  • the spray plates are directly opposite each other at a distance of 20 cm, the carrier fleece (micro-spunbond polypropylene fleece with 60 g / m 2 ) is in the middle at a speed of 0.5 m / min. passed.
  • a high voltage of + or - 15 kV is applied to the spray plates.
  • the carrier fleece coated in this way has a deposition rate of 50% of the 0.3-0.5 ⁇ m fraction of NaCl. Measured at a flow rate of 50 l / min. and a flow area of 100 cm 2 .
  • the air resistance of the carrier fleece was increased under these conditions by the coating from 8 to 16 Pa.
  • the spray plates are directly opposite each other at a distance of 20 cm, the carrier fleece (micro-spunbond polypropylene fleece with 60 g / m 2 ) is in the middle at a speed of 0.5 m / min. passed.
  • a high voltage of + or - 15 kV is applied to the spray plates.
  • the carrier fleece coated in this way has a deposition rate of 65% of the 0.3-0.5 ⁇ m fraction of NaCl. Measured at a flow rate of 50 l / min. and a flow area of 100 cm 2 .
  • the air resistance of the carrier fleece was increased under these conditions by the coating from 8 to 16 Pa.
  • a 5% polystyrene solution in dichloromethane is spun with 5 g / l chlorine and at 60 revolutions of the conveyor roller (diameter 7 cm) per minute.
  • the spray plates are directly opposite each other at a distance of 20 cm, the carrier fleece (micro-spunbond polypropylene fleece with 60 g / m 2 ) is in the middle at a speed of 0.5 m / min. passed.
  • a high voltage of + or - 15 kV is applied to the spray plates.
  • the carrier fleece coated in this way had a deposition rate of 60% of the 0.3-0.5 ⁇ m fraction of NaCl. Measured at a flow rate of 50 l / min. and a flow area of 100 cm 2 .
  • the air resistance of the carrier fleece was increased under these conditions by the coating from 8 to 15 Pa.

Abstract

La présente invention concerne un dispositif destiné à produire des fibres (6) dans le cadre d'un procédé de filage électrostatique, ledit dispositif comprenant un réservoir destiné à une solution polymère ou à une masse polymère en fusion, un système d'acheminement (1) disposé dans le réservoir, au moins une électrode de pulvérisation (3; 3a; 3b) ou au moins une tôle de pulvérisation et une contre-électrode (5), l'électrode/les électrodes de pulvérisation ou la/les tôle(s) de pulvérisation étant disposé(s) contre le système d'acheminement (1) de sorte que la solution polymère ou matière polymère en fusion acheminée depuis le réservoir par le système d'acheminement (1), s'écoule sur l'électrode/les électrodes de pulvérisation (3; 3a; 3b) ou sur la/les tôle(s) de pulvérisation. L'invention a également pour objet un procédé destiné au filage électrostatique de polymères par utilisation du dispositif de l'invention.
PCT/DE2002/002654 2001-07-25 2002-07-19 Dispositif destine a produire des fibres dans le cadre d'un procede de filage electrostatique WO2003016601A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP02754394A EP1409775B1 (fr) 2001-07-25 2002-07-19 Dispositif destine a produire des fibres dans le cadre d'un procede de filage electrostatique
DE50201852T DE50201852D1 (de) 2001-07-25 2002-07-19 Vorrichtung zur herstellung von fasern in einem elektrostatischen spinnverfahren

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10136256.0 2001-07-25
DE10136256A DE10136256B4 (de) 2001-07-25 2001-07-25 Vorrichtung zur Herstellung von Fasern in einem elektrostatischen Spinnverfahren

Publications (1)

Publication Number Publication Date
WO2003016601A1 true WO2003016601A1 (fr) 2003-02-27

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Country Status (3)

Country Link
EP (1) EP1409775B1 (fr)
DE (2) DE10136256B4 (fr)
WO (1) WO2003016601A1 (fr)

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WO2005024101A1 (fr) * 2003-09-08 2005-03-17 Technicka Univerzita V Liberci Procede de production de nanofibres par filage electrostatique a partir d'une solution polymere et dispositif associe
WO2006131081A1 (fr) * 2005-06-07 2006-12-14 Elmarco, S.R.O. Procédé et dispositif de fabrication de nanofibres à partir de la solution polymère par filage électrostatique
CZ300345B6 (cs) * 2007-07-17 2009-04-22 Elmarco, S. R. O. Zpusob zvláknování kapalné matrice, zarízení pro výrobu nanovláken elektrostatickým zvláknováním kapalné matrice a zvláknovací elektroda pro takové zarízení
GB2462112A (en) * 2008-07-24 2010-01-27 Stfc Science & Technology Producing fibres and droplets, using an electric field and moving band
US7815427B2 (en) 2007-11-20 2010-10-19 Clarcor, Inc. Apparatus and method for reducing solvent loss for electro-spinning of fine fibers
CN101985793A (zh) * 2010-11-22 2011-03-16 北京化工大学 静电纺丝法连续制备无纺布制品的装置
US7967588B2 (en) 2007-11-20 2011-06-28 Clarcor Inc. Fine fiber electro-spinning equipment, filter media systems and methods
CN102704192A (zh) * 2012-06-25 2012-10-03 天津工业大学 一种多辊实心针电极纳米纤维非织造布生产装置
CN102704193A (zh) * 2012-06-25 2012-10-03 威程(天津)科技有限公司 一种多实心针电极纳米纤维非织造布生产装置
CN103065543A (zh) * 2013-01-20 2013-04-24 青岛大学 一种便携式熔体静电纺丝教学演示装置
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CN104894661A (zh) * 2015-07-06 2015-09-09 苏州大学 一种静电纺丝装置
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CZ308360B6 (cs) * 2009-08-06 2020-06-24 Elmarco S.R.O. Rotační zvlákňovací elektroda
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DE10310435B3 (de) * 2003-02-05 2004-06-03 Helsa-Werke Helmut Sandler Gmbh & Co. Kg Filterelement und Verfahren zu seiner Herstellung
DE102007027014A1 (de) 2007-06-08 2008-12-18 Rainer Busch Vorrichtung zur Herstellung von Nano- und Microfasern durch elektrostatisches Spinnen einer durch Zentrifugalkräften in radialer Richtung aufgeschichteten Polymerlösung
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KR101143934B1 (ko) 2003-09-08 2012-05-09 테크니카 유니베르지타 브이 리베르치 정전방사를 이용한 고분자 용액으로부터 나노섬유 제조방법및 그 제조장치
US7585437B2 (en) 2003-09-08 2009-09-08 Technicka Universita V Liberci Method of nanofibres production from a polymer solution using electrostatic spinning and a device for carrying out the method
WO2005024101A1 (fr) * 2003-09-08 2005-03-17 Technicka Univerzita V Liberci Procede de production de nanofibres par filage electrostatique a partir d'une solution polymere et dispositif associe
CN1849418B (zh) * 2003-09-08 2012-07-04 利伯西科技大学 利用静电纺丝从聚合物溶液生产纳米纤维的方法和用于实施该方法的设备
AU2004270787B2 (en) * 2003-09-08 2010-06-17 Technicka Univerzita V Liberci A method of nanofibres production from a polymer solution using electrostatic spinning and a device for carrying out the method
WO2006131081A1 (fr) * 2005-06-07 2006-12-14 Elmarco, S.R.O. Procédé et dispositif de fabrication de nanofibres à partir de la solution polymère par filage électrostatique
CZ300345B6 (cs) * 2007-07-17 2009-04-22 Elmarco, S. R. O. Zpusob zvláknování kapalné matrice, zarízení pro výrobu nanovláken elektrostatickým zvláknováním kapalné matrice a zvláknovací elektroda pro takové zarízení
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EP1409775B1 (fr) 2004-12-22
DE10136256A1 (de) 2003-04-24
DE10136256B4 (de) 2005-03-31
EP1409775A1 (fr) 2004-04-21

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