EP2363516A1 - Procédé de fabrication de fibres à partir de dispersions de polymères - Google Patents

Procédé de fabrication de fibres à partir de dispersions de polymères Download PDF

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Publication number
EP2363516A1
EP2363516A1 EP10009103A EP10009103A EP2363516A1 EP 2363516 A1 EP2363516 A1 EP 2363516A1 EP 10009103 A EP10009103 A EP 10009103A EP 10009103 A EP10009103 A EP 10009103A EP 2363516 A1 EP2363516 A1 EP 2363516A1
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EP
European Patent Office
Prior art keywords
polymer
fibers
container
polymer dispersion
poly
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP10009103A
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German (de)
English (en)
Inventor
Judith Dr. Haller
Christian Dr. Waschinski
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Carl Freudenberg KG
Original Assignee
Carl Freudenberg KG
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Filing date
Publication date
Application filed by Carl Freudenberg KG filed Critical Carl Freudenberg KG
Publication of EP2363516A1 publication Critical patent/EP2363516A1/fr
Withdrawn legal-status Critical Current

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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
    • D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets

Definitions

  • the invention relates to processes for the production of polymer fibers, wherein a polymer dispersion is fed to a rotary spinning device.
  • the invention also relates to the use of a polymer dispersion as a fiber raw material for rotational spinning.
  • Polymer fibers are used in the art a variety of applications. Here, microfibers and nanofibers are of particular importance. Such polymer fibers are usually produced by spinning processes. Layers of microfibers or nanofibers are used, for example, as filters, separators or for the absorption of liquids.
  • Fibers with diameters in the micro and nano range are produced in the prior art, inter alia, by rotation spinning. Suitable rotary spinning apparatus and methods are known in the art. They use the centripetal or centrifugal forces that occur during rotation. These forces cause liquid fiber raw material to be thrown in the tangential direction through exit regions from the device becomes.
  • the geometry and diameter of the fibers produced can be influenced by the adjustment of physical parameters. In particular, the centripetal forces are set via the rotational speed of the container, with the discharge openings and the viscosity of the liquid also playing a role.
  • thermoplastic polymers As fiber raw materials melting of thermoplastic polymers are used in the prior art. Therefore, the polymer raw materials and the rotary devices must be heated. Depending on the material used, temperatures of, for example, 100 to 450 ° C are required. This is associated with a high energy consumption. Since the properties of the fibers depend on the viscosity of the fiber raw materials, a constant temperature must be ensured. Thus, special design requirements are made of the rotary devices.
  • polymer solutions are used in the prior art as fiber raw material for rotational spinning.
  • a chemical aftertreatment is necessary, which causes crosslinking of the fibers.
  • the processing of polymer solutions is often carried out in the art at elevated temperature to achieve evaporation of the solvent in fiber production.
  • the DE 10 2005 048 939 A1 discloses rotary spinning apparatus and methods.
  • the devices are associated with a heat source.
  • the exiting fibers are preferably guided by gas streams.
  • Fibrous raw materials used are melts of thermoplastic polymers or solutions of hydrophilic polymers, such as gelatin.
  • the DE 10 2007 011 606 A1 discloses a process for the production of fiber webs, in which gelatin solution is used as fiber raw material.
  • the rotor is operated at 130 ° C and the Gelatin solution heated to 95 ° C before feeding into the device.
  • the fibers are crosslinked after discharge with gaseous formaldehyde.
  • the invention has for its object to provide processes for the production of polymer fibers, which overcome the disadvantages described above.
  • the method should make it possible to produce polymer fibers, in particular micro- and nanofibers, in a simple and efficient manner.
  • the method should be particularly suitable for rotational spinning.
  • the invention is also based on the object to provide an energy-efficient method that can be carried out in particular at low temperature.
  • the design requirements for devices should be kept low.
  • the method should make it possible to process a variety of polymers.
  • the invention relates to a process for the preparation of polymer fibers, wherein a polymer dispersion is fed to a rotary spinning device.
  • the polymer dispersion is processed by rotation spinning into fibers.
  • the fibers may be such limited length (staple fibers) or filaments (filaments).
  • the fiber raw material used is a polymer dispersion. This means that the polymer dispersion is fed into the rotary spinning device and is processed by this into fibers.
  • a polymer dispersion is a colloidally stable dispersion of polymer particles in a liquid, in particular an aqueous phase.
  • Polymer dispersions are also referred to as latex.
  • the dispersion is characterized by the coexistence of a liquid and a solid polymer phase.
  • the diameter of the polymer particles may for example be between a few tens of nanometers and a few micrometers. According to the invention, the average diameter of the particles is, for example, at least 10 nm, 20 nm or 50 nm.
  • polymer dispersions appear as more or less turbid to white liquids.
  • the colloidal stability of the dispersion is mostly achieved by surfactants, such as surfactants or protective colloids.
  • Polymer dispersions can be prepared by various polymerization methods, such as emulsion polymerization or suspension polymerization, directly from the monomers or by dispersing polymers.
  • the dispersions used according to the invention differ from polymer solutions in which individual polymer molecules are dissolved in solvents.
  • aqueous polymer dispersions Preference is given to aqueous polymer dispersions, since their use can be simple and environmentally friendly. However, it is also possible to use polymer dispersions with organic liquid phases. It is also possible to use polymer dispersions which contain as the liquid phase a mixture of water with an organic solvent, for example an alcohol. The liquid phase (without solids contained therein) preferably consists of water or has a water content of at least 70, 80 or 90% by volume.
  • the polymer dispersion comprises at least one polymer selected from homopolymers or copolymers having monomeric subunits selected from acrylic acid ester (acrylate), methacrylic acid ester (methacrylate), acrylamide, methacrylamide, acrylic acid, methacrylic acid, acrylonitrile, styrene , Butadiene, ethylene, vinyl acetate, vinyl halides, vinyl chloride, vinyl alcohol, vinyl esters, vinyl ethers, ethylene oxide, isoprene, alpha-methylstyrene, vinylsulfonic acid, vinylsulfonenen vinylsulfonic acid esters, or derivatives thereof.
  • the at least one polymer is selected from poly (p-xylylene), polyvinylidene halides, polyesters, polyethers, polyethylene, polypropylene, poly (ethylene / propylene) (EPDM), polyolefins, polycarbonates, polyurethanes, natural polymers, polyacids, polylactate, polycarboxylic acids , Polysulfonic acids, sulfated polysaccharides, polylactides, polyglycosides, polyamides, poly (alkyl) styrenes, polyacrylonitriles, polyacrylamides, polyimides, polyphenylenes, polysilanes, polysiloxanes, polybenzimidazoles, polybenzothiazoles, polyoxazoles, polysulfides, polyesteramides, polyarylenevinylenes, polyetherketones, polyurethanes, polysulfones, ormocerenes, Silicones, wholly aromatic copolyesters,
  • the polymer is selected from styrene-acrylate, styrene-butadiene, pure acrylate and polyvinyl acetate.
  • polymers are used which have non-isolated double bonds.
  • dispersions of thermoplastic polymers are used.
  • copolymers is understood as meaning general polymers which are obtained by polymerization of 2, 3, 4 or more different monomers.
  • Conventional types of copolymers can be used according to the invention, such as random copolymers, alternating copolymers, block copolymers or graft copolymers.
  • Copolymers can be used in which a small proportion of a monomer is copolymerized in order to produce certain properties.
  • the copolymers can be chemically modified after the polymerization, for example be equipped with reactive groups.
  • the polymer dispersion may contain conventional additives such as surfactants such as surfactants, protective colloids, stabilizers, thickeners, plasticizers, salts and dyes.
  • surfactants such as surfactants, protective colloids, stabilizers, thickeners, plasticizers, salts and dyes.
  • the stabilization of polymer dispersions is carried out, for example, with anionic or cationic surfactants by formation of an electrically charged double layer or by steric stabilization with nonionic surfactants or protective colloids.
  • the surfactants may be low molecular weight compounds or polymers and copolymers.
  • the polymer dispersion has a solids content of from 20 to 80% by weight, preferably from 30 to 70% by weight, or from 40 to 60% by weight.
  • the solids content can be determined, for example, according to DIN EN ISO 3251 T. 2-D.
  • the polymer content of the dispersion is about 20 to 80 wt.%.
  • the proportion of polymers in total solids is generally 100% or slightly lower if additives are included.
  • the viscosity of the dispersion at 23 ° C. can be between 40 and 3000 mPas, in particular between 200 and 2000 mPas or between 500 and 1800 mPas.
  • the viscosity can be determined, for example, according to DIN ISO 3219.
  • Suitable polymer dispersions are commercially available, for example.
  • Polymer dispersions based on acrylates are available, for example, from BASF under the brand name Acronal, the use of Acronal 290 D being preferred.
  • the inventive method is carried out with a rotary spinning device.
  • a fiber raw material is discharged from a rotating container by utilizing the Zentripetal mechanism.
  • any device is suitable from the prior art, are processed with the liquid fiber raw materials using rotors to fibers. Preference is given to the use of the devices that are in DE 10 2005 048 939 A1 and DE 10 2007 011 606 A1 to be discribed. The devices described in these documents are hereby incorporated by reference.
  • the method according to the invention differs from the known methods, since according to the state of the art fiber dispersions do not use polymer dispersions but polymer melts or polymer solutions.
  • the fibers are laid on a storage device to a fiber fabric after discharging from the rotary spinning device.
  • the device comprises a container for receiving raw fiber material, wherein the container is set in rotation and wherein the container outlet areas for the Having fiber raw material, wherein the outlet regions are associated with guide means for directional, contactless guidance of the exiting the container fiber raw material.
  • a device is for example in DE 10 2005 048 939 A1 represented ( FIG. 1 , Paragraphs [0048] to [0052]).
  • the guide means comprise at least one gas flow.
  • the fibers are transported by a gas stream. If the gas stream is laminar, the fibers can be stretched and formed between the laminar layers. It is also possible to use a gas flow field which comprises a plurality of gas flows. For example, the fibers may be stretched in a first flow, redirected in a second flow and cooled in a third flow and / or functionalized by a chemical treatment. The individual flows may have different temperatures and / or speeds. As the gas, air or inert gases such as nitrogen are preferably used, and the use of air is generally easier and less expensive.
  • the guide means are associated with fans, such as fans or pumps. With these fibers can be blown or sucked.
  • the container may be formed as a truncated cone-like hollow body.
  • the hollow body may be arranged such that it tapers upwards. This specific embodiment ensures that a melt of the fiber raw material does not spill out of the container during the rotation of the container.
  • the container can be filled, for example, from above. This allows the container to be filled during its rotation. In that regard, a continuous manufacturing process is feasible.
  • the container could be associated with demolition edges, which cause gas flows or turbulence deflected, deflected or interrupted become.
  • the separation edges could be circumferentially arranged on the container and be configured as radially projecting projections.
  • the exit areas of the container could be designed as passages. It is conceivable that the passages are circular, oval or rectangular. Depending on the shape of the passages, the fiber geometry can be influenced.
  • the passages have, for example, a diameter or a width of up to 500 ⁇ m. This dimensioning is advantageous for the production of nanofibers and microfibers.
  • the passages are positioned, for example, at a distance of one centimeter from each other. It is also conceivable that the passages are arranged in several rows one above the other. As a result, the throughput of fiber raw material can be increased in a particularly simple manner. By reducing or increasing the diameter, it is possible to produce nano- or microfibers in the range of 50 nm to 200 microns.
  • the container can, for example, rotate at up to 25,000 revolutions per minute. At this high speed, it is possible to produce nanofibers with a diameter of 50 nm. By choosing the rotational speed and viscosity of the fiber raw material, fibers with a larger diameter can also be produced.
  • the rotation spinning takes place at 200 to 10,000 rpm, in particular at 200 to 5000 rpm or 300 to 1000 rpm.
  • the container may have a heat source.
  • Suitable heat sources are, for example, radiant heaters, infrared radiators or hot air blowers. With such heat sources, the heat radiation can act on the fiber raw material even at high speeds of the container.
  • the heat source can also be integrated in the container. According to the invention, however, it has been found that polymer dispersions are processed into fibers at room temperature can. This is advantageous since compared to conventional methods with polymer melts the energy consumption is significantly reduced. It is therefore preferable to carry out the process without supplying heat.
  • the apparatus for fiber production has no heat source for heating the fiber raw material and / or the rotor.
  • the polymer dispersion is processed at a temperature of 15 to 80 ° C, in particular at 15 to 50 ° C, preferably at 20 to 40 ° C and more preferably at room temperature, whereby in particular the temperature of the dispersion in the rotating container is called.
  • the device is preferably associated with a storage device for receiving fiber raw material.
  • the storage device can be configured as a platform on which the fibers can be deposited to form a batt.
  • the storage device may also be a rotating device, are received on the fibers for coating a cylindrical body or for producing a winding mat.
  • the electrical potential difference is used to support the production of nanofibers.
  • the effects of the centripetal forces and the electric field that is, the fiber raw material is on the one hand by the centripetal forces in thin Threads thrown tangentially away from the rotating container and split by the electric field.
  • the shape of the fibers and in particular the fiber diameter depend on the settings of the device and the nature of the polymer dispersion. Decisive in particular are the viscosity, the surface tension and the temperature of the dispersion, the rotational speed and the size of the discharge openings. In this case, additives, for example surfactants, can be added to the dispersion to modify the surface tension.
  • the average diameter of the fibers is between 10 nm and 1000 ⁇ m, in particular between 50 nm and 500 ⁇ m. In one embodiment, nanofibers of average diameter between 10 and 1000 nm are produced. In another embodiment, microfibers with a mean diameter of from 1 to 500 ⁇ m are produced.
  • the fibers can be dried after being discharged, for example in the air stream.
  • the fibers after discharge, have a tackiness sufficient to bond the fibers together at contact points.
  • the fibers After being discharged from the device, the fibers can be chemically aftertreated, for example cross-linked. However, such a post-treatment requires an additional step and the use of process chemicals, which is associated with increased effort and costs.
  • the fibers are not chemically post-treated after discharge from the rotary spinning machine, in particular not crosslinked.
  • the production of fibers can be carried out in a simple manner, without chemical crosslinking is required.
  • the fibers may be modified by a chemical aftertreatment.
  • the aftertreatment may be a crosslinking or other modification that does not serve for crosslinking and / or fiber stability.
  • the fibers may be chemically hydrophilized or hydrophobed or treated so as to alter the electrical properties.
  • the scrims may serve as semifinished products and be further processed, for example reinforced or consolidated, and / or bonded in laminates with each other or with other materials.
  • the layers may have, for example, basis weights between 20 and 500 g / m 2 .
  • the basis weight can be determined, for example, according to DIN 53854.
  • the layers can be made to have low porosity and high surface area so that fabrics formed therefrom have very good filtering, damping or absorption properties depending on their use.
  • the layers can be used, for example, in air filters, liquid filters, as acoustic damping elements, as wound dressings, as cleaning agents or as battery separators.
  • a substrate can also be coated with a scrim by the method according to the invention.
  • the invention also provides the use of a polymer dispersion as a fiber raw material for rotational spinning.
  • Starting material makes it easy to produce a variety of different polymer fibers. It opens up a wide range of new applications for rotational spinning. For example, polymers or additives can be processed, which have only a limited temperature resistance.
  • the process according to the invention can be used at room temperature or at a comparatively low temperature.
  • the melting of thermoplastic polymers is not required. This is associated with a considerable energy saving, especially in large-scale processes.
  • the rotary spinning devices can be operated without a heat source, whereby the design effort is reduced.
  • the polymer dispersion used was 20 g of styrene acrylate (trade name Acronal 290D, BASF). This has a solids content of about 50 wt.% And a viscosity of 700 to 1500 mPas.
  • the dispersion contains 7% by weight of polyvinyl alcohol (based on the total solids content).
  • the dispersion was processed with a rotor spinning device, which in Fig. 1 from DE 10 2007 011 606 A1 shown and explained in the corresponding description.
  • the process was carried out at room temperature.
  • the spinning device comprises a spinning rotor, which is set in rotation by a drive unit about a vertical axis of rotation.
  • the spinning rotor has a container for receiving the polymer dispersion, which is added during the spinning process continuously via a funnel from an inlet channel.
  • the container has at its outer periphery a plurality of openings through which the spin dispersion is discharged in filament form by centrifugal force.
  • the spinning rotor together with the drive unit and the depositing device are arranged in a housing which delimits a spinning space from the environment.
  • the spinning rotor is operated at a rotational speed of 640 rpm.
  • a depositing device in the form of a cylinder wall is provided, which catches the fibers.
  • the fibers are deposited as fleece on the depositing device. Due to the predetermined over the distance flight time at a certain rotational speed, the fibers are solidified to the extent that the fibrous shape is substantially retained when hitting the depositing device, on the other hand can still form the areas in which two or more fibers or filaments stick together.
  • Fibers having a filament thickness of about 1.5 ⁇ m were obtained. The thickness was determined by light microscopy and SEM images. The fiber fabric is in Fig. 1 shown. In further experiments it was found that polymer dispersions of Acronal 290D, which were additionally mixed with 0.5 to 2 volumes of water, could not be made into fibers.
EP10009103A 2010-03-05 2010-09-02 Procédé de fabrication de fibres à partir de dispersions de polymères Withdrawn EP2363516A1 (fr)

Applications Claiming Priority (1)

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DE201010010553 DE102010010553A1 (de) 2010-03-05 2010-03-05 Verfahren zur Herstellung von Fasern aus Polymerdispersionen

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8685424B2 (en) 2010-10-14 2014-04-01 Zeus Industrial Products, Inc. Antimicrobial substrate
US9034031B2 (en) 2009-08-07 2015-05-19 Zeus Industrial Products, Inc. Prosthetic device including electrostatically spun fibrous layer and method for making the same
US9198999B2 (en) 2012-09-21 2015-12-01 Merit Medical Systems, Inc. Drug-eluting rotational spun coatings and methods of use
US9655710B2 (en) 2011-01-28 2017-05-23 Merit Medical Systems, Inc. Process of making a stent
US9827703B2 (en) 2013-03-13 2017-11-28 Merit Medical Systems, Inc. Methods, systems, and apparatuses for manufacturing rotational spun appliances
US9856588B2 (en) 2009-01-16 2018-01-02 Zeus Industrial Products, Inc. Electrospinning of PTFE
US9987833B2 (en) 2012-01-16 2018-06-05 Merit Medical Systems, Inc. Rotational spun material covered medical appliances and methods of manufacture
US10010395B2 (en) 2012-04-05 2018-07-03 Zeus Industrial Products, Inc. Composite prosthetic devices
US10028852B2 (en) 2015-02-26 2018-07-24 Merit Medical Systems, Inc. Layered medical appliances and methods
US10507268B2 (en) 2012-09-19 2019-12-17 Merit Medical Systems, Inc. Electrospun material covered medical appliances and methods of manufacture
US10799617B2 (en) 2013-03-13 2020-10-13 Merit Medical Systems, Inc. Serially deposited fiber materials and associated devices and methods

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2001578A (en) * 1977-07-29 1979-02-07 Ici Ltd Spinning fibres
US4485055A (en) * 1981-07-22 1984-11-27 Basf Aktiengesellschaft Reproducible production of shaped articles of various geometries from polymer dispersions, melts or solutions
WO2004090206A1 (fr) * 2003-04-03 2004-10-21 E.I. Dupont De Nemours And Company Procede de formation de materiau uniforme par rotation
US20050136253A1 (en) * 2003-12-18 2005-06-23 Michael John G. Rotary spinning processes for forming hydroxyl polymer-containing fibers
DE102005048939A1 (de) 2005-07-01 2007-01-11 Carl Freudenberg Kg Vorrichtung, Anordnung und Verfahren zur Herstellung von Fasern und eine solche Fasern umfassende Anordnung
DE102007011606A1 (de) 2007-03-02 2008-09-04 Carl Freudenberg Kg Faser-Wirrgelege

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2001578A (en) * 1977-07-29 1979-02-07 Ici Ltd Spinning fibres
US4485055A (en) * 1981-07-22 1984-11-27 Basf Aktiengesellschaft Reproducible production of shaped articles of various geometries from polymer dispersions, melts or solutions
WO2004090206A1 (fr) * 2003-04-03 2004-10-21 E.I. Dupont De Nemours And Company Procede de formation de materiau uniforme par rotation
US20050136253A1 (en) * 2003-12-18 2005-06-23 Michael John G. Rotary spinning processes for forming hydroxyl polymer-containing fibers
DE102005048939A1 (de) 2005-07-01 2007-01-11 Carl Freudenberg Kg Vorrichtung, Anordnung und Verfahren zur Herstellung von Fasern und eine solche Fasern umfassende Anordnung
DE102007011606A1 (de) 2007-03-02 2008-09-04 Carl Freudenberg Kg Faser-Wirrgelege

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9856588B2 (en) 2009-01-16 2018-01-02 Zeus Industrial Products, Inc. Electrospinning of PTFE
US9034031B2 (en) 2009-08-07 2015-05-19 Zeus Industrial Products, Inc. Prosthetic device including electrostatically spun fibrous layer and method for making the same
US8685424B2 (en) 2010-10-14 2014-04-01 Zeus Industrial Products, Inc. Antimicrobial substrate
US10653511B2 (en) 2011-01-28 2020-05-19 Merit Medical Systems, Inc. Electrospun PTFE coated stent and method of use
US9655710B2 (en) 2011-01-28 2017-05-23 Merit Medical Systems, Inc. Process of making a stent
US10653512B2 (en) 2011-01-28 2020-05-19 Merit Medical Systems, Inc. Electrospun PTFE coated stent and method of use
US11623438B2 (en) 2012-01-16 2023-04-11 Merit Medical Systems, Inc. Rotational spun material covered medical appliances and methods of manufacture
US10675850B2 (en) 2012-01-16 2020-06-09 Merit Medical Systems, Inc. Rotational spun material covered medical appliances and methods of manufacture
US9987833B2 (en) 2012-01-16 2018-06-05 Merit Medical Systems, Inc. Rotational spun material covered medical appliances and methods of manufacture
US10005269B2 (en) 2012-01-16 2018-06-26 Merit Medical Systems, Inc. Rotational spun material covered medical appliances and methods of manufacture
US10010395B2 (en) 2012-04-05 2018-07-03 Zeus Industrial Products, Inc. Composite prosthetic devices
US10507268B2 (en) 2012-09-19 2019-12-17 Merit Medical Systems, Inc. Electrospun material covered medical appliances and methods of manufacture
US11541154B2 (en) 2012-09-19 2023-01-03 Merit Medical Systems, Inc. Electrospun material covered medical appliances and methods of manufacture
US9198999B2 (en) 2012-09-21 2015-12-01 Merit Medical Systems, Inc. Drug-eluting rotational spun coatings and methods of use
US9827703B2 (en) 2013-03-13 2017-11-28 Merit Medical Systems, Inc. Methods, systems, and apparatuses for manufacturing rotational spun appliances
US10799617B2 (en) 2013-03-13 2020-10-13 Merit Medical Systems, Inc. Serially deposited fiber materials and associated devices and methods
US10953586B2 (en) 2013-03-13 2021-03-23 Merit Medical Systems, Inc. Methods, systems, and apparatuses for manufacturing rotational spun appliances
US10028852B2 (en) 2015-02-26 2018-07-24 Merit Medical Systems, Inc. Layered medical appliances and methods
US11026777B2 (en) 2015-02-26 2021-06-08 Merit Medical Systems, Inc. Layered medical appliances and methods

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