EP2530189B1 - Verfahren zur Herstellung von funktionellen Nanofaserschichten sowie Vorrichtung zur Ausführung des Verfahrens - Google Patents

Verfahren zur Herstellung von funktionellen Nanofaserschichten sowie Vorrichtung zur Ausführung des Verfahrens Download PDF

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Publication number
EP2530189B1
EP2530189B1 EP12168226.4A EP12168226A EP2530189B1 EP 2530189 B1 EP2530189 B1 EP 2530189B1 EP 12168226 A EP12168226 A EP 12168226A EP 2530189 B1 EP2530189 B1 EP 2530189B1
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EP
European Patent Office
Prior art keywords
particles
skid plate
nanofibers
collecting electrode
electrode
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Not-in-force
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EP12168226.4A
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English (en)
French (fr)
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EP2530189A1 (de
Inventor
Pavel Pokorný
Petr Louda
David Lukás
Petr Mikes
Lucie Vyslouzilová
Jirí Chvojka
Bozena Hégrová
Richard Lukás
Evzen Amler
Matej Buzgo
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Technicka Univerzita v Liberci
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Technicka Univerzita v Liberci
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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
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/08—Processes in which the treating agent is applied in powder or granular form

Definitions

  • a method for producing a functional nanofiber layer comprising particles of solid and liquid matter by means of electrospinning of a solution or melt of a polymer, at which the produced nanofibers are laid up between a spinning electrode and a collecting electrode onto a base which is the surface of the collecting electrode or a carrying material.
  • a device for producing a functional nanofiber layer comprising particles of a solid or liquid matter by means of electrospinning of a solution or melt of a polymer between a spinning electrode and a collecting electrode, at which the nanofibers being produced are laid up between the spinning electrode and the collecting electrode onto a base which is the surface of the collecting electrode or a carrying material.
  • nanofibrous layers are usually carried out by means of electrospinning or other well-known methods (usually by means of melt-blowing, drawing or centrifugation). Thereat, small particles are brought into a polymer solution or melt, where they are dispersed. Subsequently, the substance being obtained that way is spun.
  • the second method is based on utilizing the so called coaxial electrospinning. Thereat, a material gets incorporated into the fiber cores, which does not need to be spinnable itself.
  • liquid dispersions of particles of a solid matter or globules of liquid of a suitable size can be used for the purpose.
  • the objective of such solutions is the production of nanofibers obtaining the requested qualities by the incorporation of given particles.
  • the material of the particles can also be removed from the fibers, porous fibers with nano-cavities occurring after the material has been washed out being obtained.
  • CN 101586256 A solves a method for the production of porous electrospun fibers with nano-salt equally dispersed in a polymer solution, a component fiber (polymer + nano salt) being obtained by means of electrospinning. By means of subsequent leaching of the saline solution the salt is separated, openings are created and the final porous fiber is produced.
  • Biologically activated carbon fiber for medical purposes and its production is proposed by CN 101736441 A .
  • Electrospinning and high-temperature sintering is carried out to obtain nanoparticles of calcium phosphate with biological activity in the carbon fibers.
  • the diameter of the carbon fibers varies from 50 to 500 nm; the size of nanometric particles of calcium phosphate varies from 10 to 100 nm; the percentage by weight is between 1 and 10 %.
  • Dispersed nanoparticles of calcium phosphate strengthen the bio-bond between the carbon nanofiber and the bone tissue and usually improve the ability of induced bone development.
  • KR 20090058155 A The objective of KR 20090058155 A is the production of antibacteriological, aseptic and at the same time biologically degradable wrapping paper as a means for filtering air or water.
  • the paper is highly temperature-resistant and mechanically strong. It is made of nanofibers produced by means of electrospinning of a solution having antibacteriological and antiseptic qualities. It contains metallic particles and biodegradable fiber-forming polymer.
  • a part of the WO 2008077372 file deals with the method and device for the production of composite fibrous material.
  • fibers of non-ionic polymer are sulphonated. Sulphonated, and thus anionically behaving fibers mix with a polyamide solution in the next step, to make their behaviour cation-active.
  • the fibers are brought into contact with an anionic dispersion of particles, by means of which the particles get bound to the surface area of the fibers and a fiber-particle composite is produced.
  • CZ 300797 B6 relates to a textile comprising at least one layer of polymeric nanofibers obtained by electrospinning from a polymer solution, the polymeric nanofibers comprising particles of a low-molecular matter.
  • the nanofibers of the low-molecular matter are products of a chemical reaction of the low-molecular matter antecedent dissolved in a polymeric solution and a chemical agent applied onto the nanofibers after their spinning.
  • the polymer solution for spinning contains a low-molecular matter antecedent.
  • the low-molecular matter antecedent together with the polymer are pulled into the nanofibers being produced.
  • a suitable chemical agent is used to act on the antecedent contained in the nanofibers, by means of which the low-molecular matter antecedent transforms into a low-molecular matter.
  • CZ 297774 B6 solves the method of the production of photocatalytically active TiO 2 .
  • the production starts from a very cheap raw material - alkaline titanate, which is the by-product of the production of titanium white.
  • the titanate is acted upon by glycol while being heated up and the mixture is then processed by sulphuric acid.
  • the product is photocatalitically active TiO 2 of nanofibrous morphology.
  • a bio-material based on nanofibrous layers consists of at least two nanofibrous layers, covered by living cells growing on their both sides interconnecting those layers.
  • the nanofibrous layers are unwoven and are composed of synthetic polymers or copolymers of monomers selected from a group comprising methacrylic acid esters, methacrylic acid amides, urethanes, vinyl alcohol and monomers derived from lactic acid and its derivatives, and the method of its preparation.
  • the cells are sown on an unwoven layer of nanofibers.
  • CZ 2008-241 A3 makes a wrapping agent public, which is namely a wrapping agent comprising woven or unwoven textile comprising nanofibers and evaporative corrosion inhibitors.
  • CZ20096-148 makes an electrospinning device public, containing two serial separated spinning apparatuses. The first of them generates a supporting layer of nanofibers, microfibers and/or liquid nanoparticles containing polyisobutylene on the carrying material. The second spinning device lays the actual functional layer of nanofibers onto the base. The double device is expensive, actually solving only the perfection of the bond of certain functional nanofiber layers to the carrying material and having only an indirect influence on the qualities of the functional nanofiber layer.
  • the methods and devices according to the prior art are particularly complicated, not dealing with continuous manufacturing of the final composite product, which in the case is a system of nanofibers with particle material invested. Moreover, the quality of the products depends on the required synchronization of the individual steps of its production.
  • the objective of the invention is to relieve the shortages of the prior art or to reduce them to a significant extent and to propose a reasonably priced method of production of a nanofibrous layer allowing to influence its functional qualities by means of adding powdery particle material.
  • the objective of the invention is achieved by means of a method for producing a functional nanofibrous layer comprising particles of either a solid or a liquid matter, the goal of which is that particles are brought into the nanofibrous layer by joint action of gravitational forces, when the particles are guided along an inclined skid plate ended with a sharp edge, and the action of high voltage between a base and the particles which by contacting the charged edge of the skid plate acquire an electric charge consistent with the charged edge, whereby at the same time, ionization of the gaseous environment occurs and electric wind is formed, leading away from the sharp edge of the skid plate, which helps with the transport of the particles being incorporated to the surface area of the collecting electrode.
  • the movement of the particles on the inclined skid plate is facilitated by vibrations of the skid plate.
  • the objective of the invention is also achieved by means of a device for the production of a functional nanofibrous layer comprising solid or liquid matter particles, in which at least one tank with an outlet opening for batching the solid or liquid matter particles is arranged behind the place and/or in the place of deposition of the nanofibers towards the base, the principle of which is that the outlet opening of the tank is coupled with a skid plate equipped with a sharp edge at its end facing the base, the skid plate is connected to a high voltage power supply. That allows to produce a narrow current of electric wind directed away from the sharp edge, which facilitates the transport of suitably sized particles into the wind current and further to the desired place.
  • the skid plate is connected to an outlet member of a vibrator, whose vibrations facilitate the transport of the solid particles.
  • Fig. 1 shows a device according to Background art
  • Fig. 2 shows a design comprising two particle tanks
  • Fig. 3 shows a device according to the invention using the combined effect of gravity, vibrations electric wind and Coulomb forces to incorporate the particles
  • Figs. 4 and 5 show a device according to background art using the effect of an electrospraying system to incorporate the particles and a continuously operating device processing two types of nanofibers and two types of incorporated particles.
  • An exemplary embodiment of the device according to background art for incorporating solid or liquid matter particles into a nanofibrous layer at electrospinning comprises a spinning electrode 1 equipped with an output nozzle 11 for importing the processed polymer into an electic field between a spinning electrode 1 connected to the positive pole 10 of a high voltage power supply and a collecting electrode 2 comprising a rotating collector connected to the negative pole 20 of a high voltage power supply.
  • the cylindrical or other surface of the collecting electrode 2 is either covered in a non-represented carrying material or makes up a surface onto which the nanofibers are laid up directly, being removed after finishing the production of the respective layer.
  • a tank 3 is placed, being filled with fine particles of material, which are meant to be incorporated into the final composite nanofibrous material.
  • the tank 3 is advantageously connected to the positive pole 10 of the high voltage power supply.
  • the tank 3 can be gravitational.
  • the tank is coupled with a non-represented vibrational device.
  • the tank 3 is equipped with a lockable outlet 31.
  • the device represented in Fig. 2 is supplemented by another tank 4 for particles having qualities different from those deposited in tank 3.
  • a tank 5 for particles is placed, the lower part of which is connected to a bottom comprising a skid plate 6, having a sharp edge 61 neighbouring the collecting electrode 2 and the outlet nozzle 11 of the spinning electrode 1.
  • the edge 61 is connected to the positive pole of the power supply.
  • the wall of the tank 5 is finishes in a lockable outlet 51 in its lowest place.
  • the skid plate 6 is connected to an outlet member of a non-represented vibrator.
  • Fig. 4 the device according to the background art is represented, the tank for particles of which is made up of an electrospraying system 7 with a reservoir 71 for the spraying liquid, the outlet tube 72 of which is brought close to the collecting electrode 2 and the outlet nozzle 11 of the spinning electrode 1.
  • the electrospraying nozzle 73 is directed into the area of the collecting electrode 2 , onto which the nozzle 11 of the spinning electrode 1 is directed as well.
  • the outlet tube 72 is connected to the positive pole 10 of the high voltage power supply.
  • devices included comprising electrical means for the atomization of particles and their transport towards the surface of the collecting electrode, which are represented in Fig. 3 and 4 , is supplemented by supportive pneumatic means.
  • Those comprise a compressed air feeding pipeline the outlet nozzle of which neighbours the outlet opening 51 of the tank 5 of particles or the outlet tube 72 orifice directed towards the surface of the collecting electrode 2 .
  • a device according to the invention is represented, intended for a continuous production of a nanofibrous layer with incorporated particles.
  • a part of the collecting electrode 2 is belted with a band of carrying material 8, led by a pair 81 of intake rollers before the collecting electrode 2 and by a pair 82 of off-take rollers after the collecting electrode 2 .
  • another spinning electrode 12 is placed in the vicinity of the part of the collecting electrode 2 circuit opposite to the spinning electrode 1
  • FIG. 6 another embodiment of the device according to the background art is represented, intended for a continuous production of a nanofibrous layer with incorporated particles.
  • the motion of the carrying material 8 band in the S1 direction is mediated by means of a pair 83 of feed rollers and a pair 84 of detaching rollers.
  • the spinning electrode 1, the tank 4 for particles, the spinning electrode 12 and the tank 4 for particles are placed gradually in the S1 direction of the carrying material 8 band's motion above the carrying material 8.
  • two collecting electrodes 13 are placed under the spinning electrodes 1 , 10 and two collecting electrodes 14 are placed under the tanks 3, 4.
  • two spinning electrodes 1, 12 are placed in a row, having tanks 4 and 3 for particles in a row after them.
  • a layer of nanofibers distributed in a commonly known way comes under the outlet opening 31 of the tank 3 for particles after the collector 2 has been turned in the S2 direction.
  • the particles are poured into a layer of nanofibers by means of gravitation and/or the effect of the voltage difference occurring between the tank 3 for particles and the collecting electrode 2.
  • the collecting electrode 2 can perform several revolutions when producing a single fibrous film, whereupon sandwich material gets produced, in the layers of nanofibers of which the poured particles are incorporated in the gaps between the nanofibers.
  • the tank 5 for particles is placed as close as possible to the spinning electrode 1 or its outlet nozzle 11 .
  • the particles lying directly on the skid plate 6 are moved through the outlet opening 51 towards the edge 61 of the skid plate 6.
  • Such movement of particles may be facilitated by vibrations of the skid plate 6 .
  • the sharp edge 61 connected to the positive pole 10 of the efficient high voltage power supply charges the powdery particles electrically. Ionization of the gaseous environment occurs and electric wind is formed.
  • the current of electric wind in the S3 direction away from the edge 61 is very narrow (forming a so called stream); that is why quick flux occurs in the vicinity of it, helping transport suitably sized particles into the current and further to a required place, i.e. to the surface area of the collecting electrode 2 virtually simultaneously with the stream of nanofibers leaving the outlet nozzle 11 of the spinning electrode 1.
  • the like electric charge obtained by the particles contacting the charged edge 61 is utilized.
  • the like charged particles then repel each other and obstruct the bunching of minute particles.
  • those charged particles are gravitated towards the collecting electrode by Coulomb forces, which also supports their motion.
  • the electrospraying system according to Fig. 4 uses a strong electric field to transport the particles. By means of it, the surface level of the spraying liquid transported through the outlet tube 72 from the reservoir 71 for the spraying liquid gets unbalanced, whereupon small droplets occur through so called electrospraying. Those droplets occurring after a contact with the charged edge of the nozzle 73 of the outlet tube 72 get seized by the current of the electric wind and transported to a required place. In this case, that is straight into the area where the fibers making up the nanofibrous layer are laid up simultaneously. The composite nanofibrous material is simultaneously produced in one place of the base material.
  • the oppositely charged counter-electrode As the potential of the charged edge forming the electric wind is related to the ground consisting in e.g. the frame of the machine, the floor of the room etc.
  • An analogical electrospraying system may also be using already existing particular materials sputtered electrostatically onto the surface of the collecting electrode virtually simultaneously with the nanofibers.
  • a device utilized with another commonly known method comprises a surface-structured rotating roller, carrying the particles in cavities made on its surface and pouring them into the nanofibrous layer being formed.
  • Fig. 1 to 4 The embodiments represented in Fig. 1 to 4 and their modifications related to the mutual arrangement of the spinning electrodes and tanks for particles allow to produce extensive sandwich material of a required thickness, which may comprise layers of nanofibers of different kinds, by means of multiple rotations of the collecting electrode 2 in the S2 direction.
  • the collecting electrode 2 of the device according to Fig. 5 is partly banded with a carrying material 8 band. Its continuous motion in the S4 direction is derived from the rotation of the collecting electrode 2 in the S2 direction or the interaction of the pair 81 of the input rollers and the pair 82 of the off-take rollers, which are linked to non-represented driving means.
  • a layer of nanofibers produced by the spinning electrode 1 is primarily produced, followed by the particles from tanks 4, 3 being gradually incorporated into that layer and overlayed by a layer of nanofibers produced by the spinning electrode 12 afterwards.
  • the band of carrying material 8 covered in a multicomponent nanofibrous layer is taken off by means of a pair 82 of off-take rollers for storing purposes or further processing.
  • a band of carrying material 8 is lead through a lengthwise arranged spinning chamber 9 virtually horizontally in the S1 direction, being driven by means of a pair 83 of feed rollers supported by a pair 84 of detaching rollers.
  • the band of carrying material 8 After the band of carrying material 8 has entered the spinning chamber 9 the first nanofibrous layer, the first kind of particles, the second nanofibrous layer and the second kind of particles are gradually distributed onto it.
  • the produced multicomponent nanofibrous material is detached from the spinning chamber 9 by means of a pair 84 of detaching rollers.
  • the resulting multicomponent nanofibrous material can be modified through changing the order of spinning electrodes 1 , 12 and tanks 4, 3. That way, a second layer of nanofibers produced by means of spinning electrode 12 can be added to the first layer of nanofibers produced by means of spinning electrode 1 and the first kind of particles from tank 4 and subsequently the second kind of particles from tank 3 can be poured.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Nonwoven Fabrics (AREA)

Claims (5)

  1. Verfahren zur Erzeugung einer Funktionsnanoschicht, die die Partikel eines festen oder flüssigen Stoffes durch elektrisches Verspinnen der Polymerlösung oder -schmelze aufweist, bei dem die gebildeten Nanofasern zwischen der Spinnelektrode (1) und der Sammelelektrode (2) auf eine Unterlage gelagert werden, die die Oberfläche der Sammelelektrode (2) oder ein tragendes Material (8) ist, wobei in so gebildete Schicht unmittelbar nach deren Erzeugung in der Richtung gegen die Unterlage zwischen ihre Nanofasern die Partikel eines festen oder flüssigen Stoffes eingetragen werden, die in den Spalten zwischen den Nanofasern gelagert werden, dadurch gekennzeichnet, dass die Eintragung von Partikeln in die Nanofaserschicht durch gemeinsame Schwerkraftwirkung, wann die Partikel auf einer geneigten Gleitplatte (6) geführt werden, die mit einer scharfen Kante (61) beendet ist, und durch die Wirkung der Hochspannung zwischen der Unterlage und den Partikeln erfolgt, die im Kontakt mit der geladenen Kante (61) der Gleitplatte (6) elektrische mit der geladenen Kante (61) übereinstimmende Aufladung erhalten, wobei es zugleich zur Ionisierung des gasförmigen Umfeldes und zur Entstehung der elektrischen Luft kommt, die von der scharfen Kante (61) der Gleitplatte (6) gerichtet ist, was dem Transport des eingetragenen Partikels zur Oberfläche der Sammelelektrode (2) beiträgt.
  2. Verfahren nach dem Anspruch 1, dadurch gekennzeichnet, dass die Bewegung der Partikel auf der geneigten Gleitplatte (6) durch die Vibrationen dieser Rutschplatte (6) unterstützt wird.
  3. Einrichtung zur Erzeugung einer Funktionsnanofaserschicht, die Partikel eines festen oder flüssigen Stoffes durch das elektrische Verspinnen der Polymerlösung oder -schmelze zwischen der Spinnelektrode (1) und der Sammelelektrode (2) aufweist, bei der die gebildeten Nanofasern zwischen der Spinnelektrode (1) und der Sammelelektrode (2) auf eine Unterlage gelagert werden, die die Oberfläche der Sammelelektrode (2) oder ein tragendes Material (8) ist, wobei hinter der Stelle und/oder in der Stelle der Lagerung der Nanofasern gegen die Unterlage mindestens ein Speicher (5) mit einer Ausgangsöffnung (51) zur Dosierung der Partikel des festen oder flüssigen Stoffes angeordnet ist, dadurch gekennzeichnet, dass die Ausgangsöffnung (51) des Speichers (5) mit der Gleitplatte (6) gekoppelt ist, die am der Unterlage zugewandten Ende eine scharfe Kante (61) aufweist, wobei die Gleitplatte (6) an die Hochspannungsquelle angeschlossen ist.
  4. Einrichtung nach dem Anspruch 3, dadurch gekennzeichnet, dass die Gleitplatte (6) ans Ausgangsglied des Vibrators angeschlossen ist.
  5. Einrichtung nach dem Anspruch 3 oder 4, dadurch gekennzeichnet, dass hinter der Stelle der Lagerung der eingetragenen Partikel eine Spinnelektrode (1, 12) gelagert ist.
EP12168226.4A 2011-06-01 2012-05-16 Verfahren zur Herstellung von funktionellen Nanofaserschichten sowie Vorrichtung zur Ausführung des Verfahrens Not-in-force EP2530189B1 (de)

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CZ20110328A CZ2011328A3 (cs) 2011-06-01 2011-06-01 Zpusob vytvárení funkcní nanovlákenné vrstvy a zarízení k provádení zpusobu

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EP2530189B1 true EP2530189B1 (de) 2018-06-13

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CZ2011328A3 (cs) 2012-01-11
EP2530189A1 (de) 2012-12-05

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