EP1483435B1 - Hollow-fiber spinning nozzle - Google Patents

Hollow-fiber spinning nozzle Download PDF

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Publication number
EP1483435B1
EP1483435B1 EP03706500A EP03706500A EP1483435B1 EP 1483435 B1 EP1483435 B1 EP 1483435B1 EP 03706500 A EP03706500 A EP 03706500A EP 03706500 A EP03706500 A EP 03706500A EP 1483435 B1 EP1483435 B1 EP 1483435B1
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EP
European Patent Office
Prior art keywords
plate
needle
hollow fiber
bore
spinning nozzle
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.)
Expired - Lifetime
Application number
EP03706500A
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German (de)
French (fr)
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EP1483435A1 (en
Inventor
Torsten Keller
Jens-Holger Stahl
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Fresenius Medical Care Deutschland GmbH
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Fresenius Medical Care Deutschland GmbH
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Priority to EP09008291A priority Critical patent/EP2112256B1/en
Publication of EP1483435A1 publication Critical patent/EP1483435A1/en
Application granted granted Critical
Publication of EP1483435B1 publication Critical patent/EP1483435B1/en
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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
    • D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
    • 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
    • D01D4/00—Spinnerette packs; Cleaning thereof
    • D01D4/02—Spinnerettes
    • D01D4/022—Processes or materials for the preparation of spinnerettes
    • 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
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • D01D5/34—Core-skin structure; Spinnerette packs therefor
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S425/00—Plastic article or earthenware shaping or treating: apparatus
    • Y10S425/217—Spinnerette forming conjugate, composite or hollow filaments
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
    • Y10T156/10—Methods of surface bonding and/or assembly therefor
    • Y10T156/1052—Methods of surface bonding and/or assembly therefor with cutting, punching, tearing or severing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49428—Gas and water specific plumbing component making
    • Y10T29/49432—Nozzle making
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/4998—Combined manufacture including applying or shaping of fluent material

Definitions

  • the invention relates to a hollow fiber spinneret according to the preamble of claim 1.
  • Hollow-fiber spinnerets are already known which serve for the production of polymeric hollow-fiber membranes.
  • such hollow fiber spinnerets 10 consist of a base body 12 made of metal, in which a plurality of bores 14, 16, 18, 22 are introduced.
  • a tube 20 is fitted, in which a Hurllstoff- or support means channel 22 is formed for introducing the precipitant or support means.
  • the holes 16 and 18 form Massezu thoroughlykanäle for a polymer, which exits via an annular channel 22, which also consists of a corresponding hole, yes.
  • methods of conventional metal working are used.
  • the nozzle structure created by the assembly of both nozzle parts with an inaccuracy, for example, the geometry of the annulus 22 added up from the manufacturing errors in the manufacture of the body 12 and the tube 20.
  • an inaccuracy for example, the geometry of the annulus 22 added up from the manufacturing errors in the manufacture of the body 12 and the tube 20.
  • mounting errors added which also contribute to an inaccuracy can lead the geometry.
  • the known in the art hollow fiber spinnerets are not arbitrarily reduced in size.
  • the object of the invention is therefore to provide hollow fiber spinnerets with which even fine capillary membranes can be produced, wherein the manufacturing tolerances are minimized and the manufacturing process for these hollow fiber spinnerets is significantly cheaper.
  • this object is achieved by the combination of the features of claim 1.
  • a completely new design for hollow fiber spinnerets is provided because the invention avoids conventional metalworking and uses microstructure techniques.
  • at least two plate-shaped bodies structured by microstructure technology are joined together to form the hollow-fiber spinneret.
  • a second unstructured plate is preferably added to a first plate formed by microstructure technology, wherein the second plate is patterned only after application to the first plate.
  • the plates are connected flat to each other.
  • a hollow fiber spinneret consists of two plates, wherein in the first plate the Massezu Foodkanäle, a mass flow equalization zone, a precipitant / Stauerschzu Georgiabohrung and a needle stump are excluded, while in the second plate a nozzle structure with mass annular gap and a needle with a precipitant / Stauerschbohrung are excluded.
  • the second plate additionally contains the MassezuGermankanäle and the mass flow homogenization zone: There accounts for these elements and the needle stump on the first plate.
  • a special feature of this construction is that the needle of the spinneret is connected to the first plate only at one end face.
  • a hollow-fiber spinneret with which a simple capillary hollow-fiber membrane can be produced, advantageously have the following dimensions: Thickness of the first plate: 0.250 - 1.500 mm Thickness of the second plate: 0.050-1.500 mm Outer diameter of the needle: 0,020 -1,500 mm Length of the needle incl.
  • Needle stump 0.100 - 2.000 mm Diameter of the precipitation agent bore: 0.010 - 1.000 mm Length of precipitation agent hole: 0.150 - 2.500 mm Outer diameter of the annular gap: 0.040 - 3.000 mm Length of the annular gap: 0.050 - 1.500 mm Height of the spinneret: 0.300 - 3.000 mm Edge length of the spinneret: 1,000 -. 25.00 mm.
  • a further preferred embodiment of the invention consists of three plates, wherein the first plate contains feed channels, a homogenization zone and a needle stub with a central feed bore, a second plate which adjoins the first plate, feed channels, a homogenization zone and a further needle stub with a having a concentric annular channel and a needle extension having a central bore, and wherein a third plate, which in turn adjoins the second plate, a nozzle structure comprising a central bore and two concentric annular gaps.
  • Capillary membranes with coextruded bilayers can be produced by means of this hollow-fiber spinneret according to the invention.
  • the hollow fiber spinneret is composed of three individual plates, wherein the first plate has a central feed bore, a parallel to the first plate second feed channels and arranged on these equalization zones and a needle stub with concentric annular channel and a central bore and wherein the third plate adjoining the second plate has a nozzle structure consisting of a central bore and two concentric annular gaps.
  • the outer diameter of the multi-channel hollow fiber spinneret is less than 1 mm.
  • the outer diameter of the multi-channel hollow fiber spinneret is less than or equal to 0.45 mm.
  • FIG. 2 a hollow fiber spinneret 10 according to a first embodiment of the invention is shown.
  • the entire body 26 is composed of two individual plates 30 and 32.
  • ground supply channels 34, a mass flow equalization zone 36, a precipitating agent supply bore 38 and a needle stub 40 are formed by a corresponding etching operation, which will be described later in detail.
  • the three-dimensional design of here in FIG. 2 shown hollow fiber spinneret results from FIG. 4 , There it can be seen that the Massezu Foodkanäle, ie the channels for supplying the considered the considered here.
  • the mass flow equalization zone 36 results as an annular space around the needle stub 40 around.
  • the Desillatorizu operationsbohrung 38 is widened in its pointing to the top of the area, as can be seen in particular of Figure 2.
  • monocrystalline silicon for example, has a thickness of the first plate of 0.4 mm, a thickness of the second plate of 0.1 mm, an outer diameter of the needle of 0.05 mm, a length of the needle including the needle stump of 0.15 mm Diameter of Desillatoribohrung 38 in the extended range of 0.1 mm, an outer diameter of the annular gap 42 of 0.1 mm and a length of the annular gap 42 of 0.1 mm.
  • the height of the main body 26, ie the height of the entire spinneret 10, is accordingly 0.5 mm, while an edge length of the main body 26 of the spinneret 10 is 2 mm.
  • hollow fiber spinnerets In the production of hollow fiber spinnerets by means of microstructure technology is assumed by 2 round wafer discs with 100 to 300 mm diameter. From these wafers, many spinneret structures are simultaneously produced. The individual hollow fiber spinnerets 10 are then obtained by dicing the finished wafers. The separated split spinnerets can each contain a single nozzle structure, as shown here, but also several nozzle structures in a nozzle structure composite. This is achieved by not separating all of the nozzle structures formed on the wafer from one another, but rather that a plurality of nozzle structures together form a multiple nozzle unit, which are cut along the outer contour of the wafer.
  • the production of the spinnerets 10 begins with the structuring on both sides of a first wafer, which receives the elements 34, 36, 38, 40 of the plate 30 of the spinneret 10.
  • the structures are fabricated by a series of standard lithography techniques, ie photoresist masks, SiO, Si-N or the like, and standard etching techniques.
  • RIE reactive ion etching
  • D-RIE reactive ion deep etching
  • cryo-etching Particularly suitable are special deep etching methods such as D-RIE and cryo-etching.
  • the lithographic masks for the front and back must be aligned visually.
  • the second wafer, from which the second plate is to be produced is bonded to the correspondingly structured first wafer. In this case, all bonding methods can be used, anodic bonding, direct bonding or the like.
  • the nozzle structure 48 with annular gap 42 and precipitation agent bore 46 is produced in a two-stage etching process.
  • the first step only the deeper precipitation agent hole is advanced.
  • both structures are then finished etched.
  • the above-mentioned lithography and etching processes are again used, although the use of the deep etching process is even more advisable here than during the processing of the first wafer.
  • the individual spinnerets are cut out of the wafer by suitable separation methods, such as wafer sawing or laser processing.
  • a hollow fiber spinneret 10 for producing a hollow fiber coextruded from two layers is shown.
  • a hollow fiber spinneret 10 with a base body 100 consisting of three individual plates 102, 104 and 106 is shown.
  • the individual plates in turn consist of monocrystalline silicon.
  • a feed channel 108 is excluded for the precipitant.
  • feed channels 110, 112 for a first polymer are provided, which open into an associated homogenization zone 114.
  • the equalization zone 114 surrounds a corresponding needle stump 116.
  • a precipitant hole 118 is also excluded, which is surrounded by a further needle stub 120 and an annular space 122. Furthermore, further feed channels 124 with subsequent homogenization zone 126 are excluded in the second plate 104. Finally, the third plate 106 has two annular gaps 128 and 130 for the respective polymeric materials to be co-extruded, and a needle 132 with precipitant well 134. In the variants of Figs 3a, 3b and 3c the supply channels 124 are each configured differently. While in the embodiment according to the FIG. 3a the feed channel 124 for the second polymer is provided only in the second plate 104, which runs in the variant according to the FIG.
  • the three plates 102, 104 and 106 are in turn connected to the main body 100 by a suitable bonding method, advantageously direct bonding. Otherwise corresponds to the manufacturing method for the hollow fiber spinneret 10 according to the Figures 3 and 5 , analogous to that, as already stated by the FIG. 2 and 4 was explained in detail.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
  • Spinning Or Twisting Of Yarns (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

A hollow fiber spinning nozzle comprises a base element with precipitating agent/support agent as well as inlet channels together with a nozzle structure with an outflow opening and a needle with a borehole for a precipitating agent. The base element comprises at least two microstructured flat bodies brought together.

Description

Die Erfindung betrifft eine Hohlfaser-Spinndüse nach dem Oberbegriff des Anspruchs 1.The invention relates to a hollow fiber spinneret according to the preamble of claim 1.

Es sind bereits Hohlfaser-Spinndüsen bekannt, die zur Herstellung von polymeren Hohlfasermembranen dienen. Wie in der Figur 1 gemäß der beigefügten Zeichnung dargestellt, bestehen derartige Hohlfaser-Spinndüsen 10 aus einem Grundkörper 12 aus Metall, in welchen mehrere Bohrungen 14, 16, 18, 22 eingebracht sind. In die Bohrung 14 ist ein Röhrchen 20 eingepasst, in welchem ein Fällmittel- bzw. Stützmittelkanal 22 zum Einbringen des Fällmittels bzw. Stützmittels ausgebildet ist. Die Bohrungen 16 und 18 bilden Massezuführkanäle für ein Polymer, das über einen Ringkanal 22, der ja ebenfalls aus einer entsprechenden Bohrung besteht, austritt. Bei der Herstellung der bekannten Hohlfaser-Spinndüsen 10 werden Verfahren der üblichen Metallbearbeitung angewandt. Hier entsteht also die Düsenstruktur durch den Zusammenbau beider Düsenteile, wobei sich eine Ungenauigkeit, beispielsweise der Geometrie des Ringraums 22 aufsummiert aus den Fertigungsfehlern beim Fertigen des Grundkörpers 12 und des Röhrchens 20. Es treten darüber hinaus mögliche Montagefehler hinzu, die ebenfalls zu einer Ungenauigkeit der Geometrie führen können. Schließlich sind die gemäß dem Stand der Technik bekannten Hohlfaser-Spinndüsen nicht beliebig verkleinerbar.Hollow-fiber spinnerets are already known which serve for the production of polymeric hollow-fiber membranes. Like in the FIG. 1 shown in the accompanying drawing, such hollow fiber spinnerets 10 consist of a base body 12 made of metal, in which a plurality of bores 14, 16, 18, 22 are introduced. In the bore 14, a tube 20 is fitted, in which a Fällmittel- or support means channel 22 is formed for introducing the precipitant or support means. The holes 16 and 18 form Massezuführkanäle for a polymer, which exits via an annular channel 22, which also consists of a corresponding hole, yes. In the production of the known hollow-fiber spinnerets 10, methods of conventional metal working are used. Here, therefore, the nozzle structure created by the assembly of both nozzle parts, with an inaccuracy, for example, the geometry of the annulus 22 added up from the manufacturing errors in the manufacture of the body 12 and the tube 20. There are also possible mounting errors added, which also contribute to an inaccuracy can lead the geometry. Finally, the known in the art hollow fiber spinnerets are not arbitrarily reduced in size.

Aufgabe der Erfindung ist es daher, Hohlfaser-Spinndüsen an die Hand zu geben, mit denen auch feine Kapillarmembranen herstellbar sind, wobei die Fertigungstoleranzen minimiert werden und das Herstellverfahren für diese Hohlfaser-Spinndüsen deutlich verbilligt wird.The object of the invention is therefore to provide hollow fiber spinnerets with which even fine capillary membranes can be produced, wherein the manufacturing tolerances are minimized and the manufacturing process for these hollow fiber spinnerets is significantly cheaper.

Erfindungsgemäß wird diese Aufgabe durch die Kombination der Merkmale des Anspruchs 1 gelöst. Somit wird eine vollständig neuartige Konstruktionsweise für Hohlfaser-Spinndüsen geschaffen, da sich die Erfindung von der konventionellen Metallbearbeitung abwendet und Verfahren der Mikrostrukturtechnik anwendet. Erfindungsgemäß werden nämlich mindestens zwei mittels Mikrostrukturtechnik strukturierte plattenförmige Körper zu der Hohlfaser-Spinndüse zusammengefügt. Dabei wird bevorzugt auf eine erste mittels Mikrostrukturtechnik gebildete Platte eine zweite unstrukturierte Platte gefügt, wobei die zweite Platte erst nach dem Aufbringen auf die erste Platte strukturiert wird. Die Platten werden flächig miteinander verbunden. Mit der neuen Fertigungsmethode eröffnet sich eine Vielzahl von Vorteilen. Zunächst lässt sich eine wesentlich kleinere Abmessung der Düsenstruktur mittels der Mikrostrukturtechnik realisieren. Darüber hinaus ist eine wesentlich höhere Präzision hinsichtlich der Düsenstruktur realisierbar. Diese Präzision kommt dadurch zustande, dass die Düsenstruktur in einem Schritt entsteht. Sie ist nur durch die Genauigkeit der zu Grunde liegenden Lithographiemaske, die bei der Mikrostrukturtechnik verwendet wird, beschränkt. Derartige Lithographiemasken lassen sich jedoch mit Toleranzen von 100 nm extrem genau fertigen. Ein weiterer Vorteil des erfindungsgemäßen Verfahrens liegt in den wesentlich geringeren Produktionskosten der Spinndüsen.According to the invention this object is achieved by the combination of the features of claim 1. Thus, a completely new design for hollow fiber spinnerets is provided because the invention avoids conventional metalworking and uses microstructure techniques. In accordance with the invention, at least two plate-shaped bodies structured by microstructure technology are joined together to form the hollow-fiber spinneret. In this case, a second unstructured plate is preferably added to a first plate formed by microstructure technology, wherein the second plate is patterned only after application to the first plate. The plates are connected flat to each other. The new manufacturing method opens up a multitude of advantages. First, a much smaller dimension of the nozzle structure can be realized by means of microstructure technology. In addition, a much higher precision with respect to the nozzle structure can be realized. This precision is achieved by creating the nozzle structure in one step. It is limited only by the accuracy of the underlying lithographic mask used in microstructure technology. However, such lithography masks can be manufactured extremely precisely with tolerances of 100 nm. Another advantage of the method according to the invention lies in the significantly lower production costs of the spinnerets.

Besondere Ausgestaltungen der Erfindung ergeben sich aus den sich an den Hauptanspruch anschließenden Unteransprüchen.Particular embodiments of the invention will become apparent from the subsequent claims to the main claim.

Grundsätzlich lassen sich natürlich für die Realisierung der Hohlfaser-Spinndüsen nach der Erfindung alle Materialien der Mikrostrukturtechnik einsetzen, sofern diese anisotrop geätzt und gebondet werden können. Besonders vorteilhaft sind aber einkristallines Silizium, Galliumarsenid (GaAs) oder Germanium einsetzbar.In principle, of course, all materials of microstructure technology can be used for the realization of the hollow-fiber spinnerets according to the invention, provided that they can be anisotropically etched and bonded. However, it is particularly advantageous to use monocrystalline silicon, gallium arsenide (GaAs) or germanium.

Gemäß einer besonderen Ausführungsform der Erfindung besteht eine Hohlfaser-Spinndüse aus zwei Platten, wobei in der ersten Platte die Massezuführkanäle, eine Massestrom-Vergleichmäßigungszone, eine Fällmittel/Stützmittelzuführbohrung und ein Nadelstumpf ausgenommen sind, während in der zweiten Plattte eine Düsenstruktur mit Masse-Ringspalt und eine Nadel mit einer Fällmittel/Stützmittelbohrung ausgenommen sind.According to a particular embodiment of the invention, a hollow fiber spinneret consists of two plates, wherein in the first plate the Massezuführkanäle, a mass flow equalization zone, a precipitant / Stützmittelzuführbohrung and a needle stump are excluded, while in the second plate a nozzle structure with mass annular gap and a needle with a precipitant / Stützmittelbohrung are excluded.

Alternativ ist auch eine Konstruktion denkbar, bei der die zweite Platte zusätzlich die Massezuführkanäle und die Massestrom-Vergleichmäßigungszone enthält: Dort entfallen auf der ersten Platte diese Elemente und der Nadelstumpf. Ein besonderes Merkmal dieser Konstruktion ist es, dass die Nadel der Spinndüse nur an einer Stirnfläche mit der erste Platte verbunden ist.Alternatively, a construction is conceivable in which the second plate additionally contains the Massezuführkanäle and the mass flow homogenization zone: There accounts for these elements and the needle stump on the first plate. A special feature of this construction is that the needle of the spinneret is connected to the first plate only at one end face.

Diese bevorzugten Ausgestaltungen für eine Hohlfaser-Spinndüse, mit der eine einfache Kapillar-Hohlfasermembran herstellbar ist, weisen vorteilhaft folgende Abmessungen auf: Dicke der ersten Platte : 0,250 - 1,500 mm Dicke der zweiten Platte: 0,050 -1,500 mm Außendurchmesser der Nadel: 0,020 -1,500 mm Länge der Nadel incl. Nadelstumpf: 0,100 - 2,000 mm Durchmesser der Fällmittelbohrung: 0,010 - 1,000 mm Länge der Fällmittelbohrung: 0,150 - 2,500 mm Außendurchmesser des Ringspalts: 0,040 - 3,000 mm Länge des Ringspalts: 0,050 - 1,500 mm Höhe der Spinndüse: 0,300 - 3,000 mm Kantenlänge der Spinndüse: 1,000 -. 25,00 mm. These preferred embodiments for a hollow-fiber spinneret, with which a simple capillary hollow-fiber membrane can be produced, advantageously have the following dimensions: Thickness of the first plate: 0.250 - 1.500 mm Thickness of the second plate: 0.050-1.500 mm Outer diameter of the needle: 0,020 -1,500 mm Length of the needle incl. Needle stump: 0.100 - 2.000 mm Diameter of the precipitation agent bore: 0.010 - 1.000 mm Length of precipitation agent hole: 0.150 - 2.500 mm Outer diameter of the annular gap: 0.040 - 3.000 mm Length of the annular gap: 0.050 - 1.500 mm Height of the spinneret: 0.300 - 3.000 mm Edge length of the spinneret: 1,000 -. 25.00 mm.

Eine weitere bevorzugte Ausgestaltung der Erfindung besteht aus drei Platten, wobei die erste Platte Zuführkanäle, eine Vergleichmäßigungszone und einen Nadelstumpf mit einer zentralen Zuführbohrung enthält, eine zweite Platte, die sich an die erste Platte anschließt, Zuführkanäle, eine Vergleichmäßigungszone und einen weiteren Nadelstumpf mit einem konzentrischen Ringkanal sowie eine Nadelverlängerung mit einer zentralen Bohrung aufweist, und wobei eine dritte Platte, die sich wiederum an die zweite Platte anschließt, eine Düsenstruktur bestehend aus einer zentralen Bohrung und zwei konzentrischen Ringspalten aufweist. Mittels dieser erfindungsgemäßen Hohlfaser-Spinndüse lassen sich Kapillarmembranen mit koextrudierten Doppelschichten herstellen.A further preferred embodiment of the invention consists of three plates, wherein the first plate contains feed channels, a homogenization zone and a needle stub with a central feed bore, a second plate which adjoins the first plate, feed channels, a homogenization zone and a further needle stub with a having a concentric annular channel and a needle extension having a central bore, and wherein a third plate, which in turn adjoins the second plate, a nozzle structure comprising a central bore and two concentric annular gaps. Capillary membranes with coextruded bilayers can be produced by means of this hollow-fiber spinneret according to the invention.

Eine alternative Ausführungsvariante ergibt sich dadurch, dass die Hohlfaser-Spinndüsen aus drei einzelnen Platten aufgebaut ist, wobei die erste Platte eine zentrale Zuführungsbohrung aufweist, eine sich an die erste Platte anschließende zweite Platte parallele Zuführkanäle und zu diesen angeordnete Vergleichmäßigungszonen sowie ein Nadelstumpf mit konzentrischem Ringkanal und eine zentrale Bohrung aufweist und wobei die an die zweite Platte anschließende dritte Platte eine Düsenstruktur bestehend aus einer zentralen Bohrung und zwei konzentrischen Ringspalten aufweist.
Vorteilhaft ist der äußere Durchmesser der Mehrkanal-Hohlfaser-Spinndüse kleiner als 1 mm. Besonders vorteilhaft ist der äußere Durchmesser der Mehrkanal-Hohlfaser-Spinndüse kleiner oder gleich 0,45 mm. Mit dieser ist eine Dialysemembran mit einem Innendurchmesser von 200-300 µm herstellbar.An alternative embodiment results from the fact that the hollow fiber spinneret is composed of three individual plates, wherein the first plate has a central feed bore, a parallel to the first plate second feed channels and arranged on these equalization zones and a needle stub with concentric annular channel and a central bore and wherein the third plate adjoining the second plate has a nozzle structure consisting of a central bore and two concentric annular gaps.
Advantageously, the outer diameter of the multi-channel hollow fiber spinneret is less than 1 mm. Particularly advantageously, the outer diameter of the multi-channel hollow fiber spinneret is less than or equal to 0.45 mm. With this a dialysis membrane with an inner diameter of 200-300 microns can be produced.

Weitere Einzelheiten und Vorteile der Erfindung ergeben sich aus den in der Zeichnung dargestellten Ausführungsbeispielen. Es zeigen:

Figur 1:
einen schematischen Schnitt durch eine Hohlfaser-Spinndüse gemäß einer Ausführungsform nach dem Stand der Technik,
Figur 2:
einen schematischen Schnitt durch eine Hohlfaser-Spinndüse nach einer ersten Ausgestaltung der Erfindung,
Figur 3:
eine schematische Schnittdarstellung einer Hohlfaser-Spinndüse nach einer zweiten Ausführungsvariante der Erfindung, wobei drei Varianten der Anordnung der Massezuführkanäle gezeigt sind,
Figur 4:
eine teilweise geschnittene dreidimensionale Darstellung einer Hohlfaser-Spinndüse gemäß Figur 2 und
Figur 5:
eine teilweise geschnittene dreidimensionale Darstellung einer Hohlfaser-Spinndüse gemäß der Ausführungsvariante nach Figur 3.
Further details and advantages of the invention will become apparent from the embodiments illustrated in the drawings. Show it:
FIG. 1:
a schematic section through a hollow fiber spinneret according to an embodiment of the prior art,
FIG. 2:
a schematic section through a hollow fiber spinneret according to a first embodiment of the invention,
FIG. 3:
1 is a schematic sectional view of a hollow fiber spinneret according to a second embodiment of the invention, wherein three variants of the arrangement of the ground feed channels are shown,
FIG. 4:
a partially sectioned three-dimensional representation of a hollow fiber spinneret according to FIG. 2 and
FIG. 5:
a partially cut three-dimensional view of a hollow fiber spinneret according to the embodiment according to FIG. 3 ,

In Figur 2 ist eine Hohlfaser-Spinndüse 10 nach einer ersten Ausgestaltung der Erfindung gezeigt. Hier ist der gesamte Grundkörper 26 aus zwei einzelnen Platten 30 und 32 zusammengesetzt. In der ersten Platte 30 sind Massezuführkanäle 34, eine Massenstrom-Vergleichmäßigungszone 36, eine Fällmittelzuführungsbohrung 38 und ein Nadelstumpf 40 durch einen entsprechenden Ätzvorgang, der später noch im einzelnen beschrieben wird, gebildet. Die dreidimensionale Ausgestaltung der hier in Figur 2 dargestellten Hohlfaser-Spinndüse ergibt sich aus Figur 4. Dort ist zu sehen, dass die Massezuführkanäle, d.h. die Kanäle zur Zuführung der auszufällenden polymeren Masse im hier dargestellten Ausführungsbeispiel kreuzförmig angeordnet sind. Die Massestrom-Vergleichmäßigungszone 36 ergibt sich als Ringraum um den Nadelstumpf 40 herum. Die Fällmittelzuführungsbohrung 38 ist in ihrem zur Oberseite hinweisenden Bereich verbreitert, wie das insbesondere der Figur 2 zu entnehmen ist.In FIG. 2 a hollow fiber spinneret 10 according to a first embodiment of the invention is shown. Here, the entire body 26 is composed of two individual plates 30 and 32. In the first plate 30, ground supply channels 34, a mass flow equalization zone 36, a precipitating agent supply bore 38 and a needle stub 40 are formed by a corresponding etching operation, which will be described later in detail. The three-dimensional design of here in FIG. 2 shown hollow fiber spinneret results from FIG. 4 , There it can be seen that the Massezuführkanäle, ie the channels for supplying the auszufällenden polymeric mass are arranged crosswise in the embodiment shown here. The mass flow equalization zone 36 results as an annular space around the needle stub 40 around. The Fällmittelzuführungsbohrung 38 is widened in its pointing to the top of the area, as can be seen in particular of Figure 2.

Aus den Figuren 2 und 4 ist auch der Aufbau der zweiten Platte 32 zu entnehmen, die eine Masse-Austrittsöffnung 42 aufweist, der unmittelbar an die Massestrom-Vergleichmäßigungszone 36 anschließt. Diese Masse-Austrittsöffnung bzw. der Masse-Ringspalt 42 ergibt mit der Nadel 44 mit Fällmittelbohrung 46 die hochpräzise Düsenstruktur 48. Das in den Figuren 2 und 4 dargestellte Ausführungsbeispiel aus einkristallinem Silizium hat beispielsweise eine Dicke der ersten Platte von 0,4 mm, eine Dicke der zweiten Platte von 0,1 mm, einen Außendurchmesser der Nadel von 0,05 mm, eine Länge der Nadel inklusive Nadelstumpf von 0,15 mm, ein Durchmesser der Fällmittelbohrung 38 im erweiterten Bereich von 0,1 mm, einen Außendurchmesser des Ringspalts 42 von 0,1 mm und eine Länge des Ringspalts 42 von 0,1 mm. Die Höhe des Grundkörpers 26, d.h. die Höhe der gesamten Spinndüse 10, beträgt demnach 0,5 mm, während eine Kantenlänge des Grundkörpers 26 der Spinndüse 10 2 mm beträgt.From the Figures 2 and 4 is also the construction of the second plate 32 can be seen, which has a mass outlet opening 42 which connects directly to the mass flow equalization zone 36. This mass outlet opening or the mass-annular gap 42 results with the needle 44 with Fällmittelbohrung 46, the high-precision nozzle structure 48. The in the Figures 2 and 4 illustrated embodiment monocrystalline silicon, for example, has a thickness of the first plate of 0.4 mm, a thickness of the second plate of 0.1 mm, an outer diameter of the needle of 0.05 mm, a length of the needle including the needle stump of 0.15 mm Diameter of Fällmittelbohrung 38 in the extended range of 0.1 mm, an outer diameter of the annular gap 42 of 0.1 mm and a length of the annular gap 42 of 0.1 mm. The height of the main body 26, ie the height of the entire spinneret 10, is accordingly 0.5 mm, while an edge length of the main body 26 of the spinneret 10 is 2 mm.

Bei der Herstellung von Hohlfaser-Spinndüsen mittels Mikrostrukturtechnik wird von 2 runden Waferscheiben mit 100 bis 300 mm Durchmesser ausgegangen. Aus diesen Wafern werden gleichzeitig viele Spinndüsenstrukturen hergestellt. Die einzelnen Hohlfaser-Spinndüsen 10 erhält man dann durch Zerteilen der fertig bearbeiteten Wafer. Die vereinzelten geteilten Spinndüsen können jeweils eine einzige Düsenstruktur, wie hier dargestellt, aber auch mehrere Düsenstrukturen in einem Düsenstrukturverbund enthalten. Dies erreicht man dadurch, dass nicht alle Düsenstrukturen, die auf dem Wafer gebildet wurden, voneinander getrennt werde, sondern dass mehrere Düsenstrukturen zusammen eine Mehrfach-Düseneinheit bilden, die entlang ihrer Außenkontur vom Wafer ausgeschnitten werden.In the production of hollow fiber spinnerets by means of microstructure technology is assumed by 2 round wafer discs with 100 to 300 mm diameter. From these wafers, many spinneret structures are simultaneously produced. The individual hollow fiber spinnerets 10 are then obtained by dicing the finished wafers. The separated split spinnerets can each contain a single nozzle structure, as shown here, but also several nozzle structures in a nozzle structure composite. This is achieved by not separating all of the nozzle structures formed on the wafer from one another, but rather that a plurality of nozzle structures together form a multiple nozzle unit, which are cut along the outer contour of the wafer.

Die Herstellung der Spinndüsen 10 beginnt mit der beidseitigen Strukturierung eines ersten Wafers, der die Elemente 34, 36, 38, 40 der Platte 30 der Spinndüse 10 aufnimmt. Die Strukturen werden mit einer Folge von Standard-Lithographieverfahren, d.h. Masken aus Photoresist, SiO, Si-N oder ähnlichem, und Standard-Ätzverfahren gefertigt. Bei den Standard-Ätzverfahren sind insbesondere das reaktive Ionen-Ätzen (RIE), das reaktive lonen-Tiefenätzen (D-RIE) und das Kryo-Ätzen zu nennen. Besonders geeignet sind spezielle Tiefenätzverfahren wie das D-RIE und das Kryo-Ätzen. Die Lithographie-Masken für die Vorder- und Rückseite müssen optisch zueinander ausgerichtet werden. Anschließend wird der zweite Wafer, aus dem die zweite Platte hergestellt werden soll, auf den entsprechend strukturierten ersten Wafer gebondet. Dabei können sämtliche Bondverfahren eingesetzt werden, das Anodische Bonden, das Direktbonden oder ähnliches.The production of the spinnerets 10 begins with the structuring on both sides of a first wafer, which receives the elements 34, 36, 38, 40 of the plate 30 of the spinneret 10. The structures are fabricated by a series of standard lithography techniques, ie photoresist masks, SiO, Si-N or the like, and standard etching techniques. In the standard etching processes, in particular reactive ion etching (RIE), reactive ion deep etching (D-RIE) and cryo-etching are to be mentioned. Particularly suitable are special deep etching methods such as D-RIE and cryo-etching. The lithographic masks for the front and back must be aligned visually. Subsequently, the second wafer, from which the second plate is to be produced, is bonded to the correspondingly structured first wafer. In this case, all bonding methods can be used, anodic bonding, direct bonding or the like.

Besonders geeignet ist aber das Direktbonden, da die höchsten Festigkeiten erreicht werden und damit ein guter Halt der Nadel auf der ersten Platte gewährleistet wird. Im nächsten Schritt wird die Düsenstrukur 48 mit Ringspalt 42 und Fällmittelbohrung 46 in einem zweistufigen Ätzverfahren hergestellt. Im ersten Schritt wird nur die tiefere Fällmittelbohrung vorangetrieben. Im zweiten Schritt werden dann beide Strukturen fertig geätzt. Zur Anwendung kommen dabei wieder die genannten Lithographie- und Ätzverfahren, wobei hier die Verwendung der Tiefenätzverfahren noch eher angeraten ist als bei der Bearbeitung des ersten Wafers. Im letzten Schritt werden die einzelnen Spinndüsen, wie bereits zuvor beschrieben, durch geeignete Trennverfahren, wie Wafer-Sägen oder Laserbearbeitung aus dem Wafer herausgeschnitten.However, direct bonding is particularly suitable since the highest strengths are achieved and thus a good hold of the needle on the first plate is ensured. In the next step, the nozzle structure 48 with annular gap 42 and precipitation agent bore 46 is produced in a two-stage etching process. In the first step, only the deeper precipitation agent hole is advanced. In the second step, both structures are then finished etched. The above-mentioned lithography and etching processes are again used, although the use of the deep etching process is even more advisable here than during the processing of the first wafer. In the last step, as described above, the individual spinnerets are cut out of the wafer by suitable separation methods, such as wafer sawing or laser processing.

Anhand der Figuren 3 und 5 werden weitere alternative Ausgestaltungen der Erfindung erläutert. Hier ist eine Hohlfaser-Spinndüse 10 zur Herstellung einer aus zwei Schichten koextrudierten Hohlfaser gezeigt. Hier ist eine Hohlfaser-Spinndüse 10 mit eines Grundkörpers 100 bestehend aus drei einzelnen Platten 102, 104 und 106 gezeigt. Die einzelnen Platten bestehen wiederum aus einkristallinem Silizium. In der ersten Platte 102 ist ein Zuführkanal 108 für das Fällmittel ausgenommen. Zusätzlich sind Zuführkanäle 110, 112 für ein erstes Polymer vorgesehen, die in eine zugehörige Vergleichmäßigungszone 114 einmünden. Die Vergleichmäßigungszone 114 umgibt einen entsprechenden Nadelstumpf 116.Based on Figures 3 and 5 further alternative embodiments of the invention will be explained. Here, a hollow fiber spinneret 10 for producing a hollow fiber coextruded from two layers is shown. Here, a hollow fiber spinneret 10 with a base body 100 consisting of three individual plates 102, 104 and 106 is shown. The individual plates in turn consist of monocrystalline silicon. In the first plate 102, a feed channel 108 is excluded for the precipitant. In addition, feed channels 110, 112 for a first polymer are provided, which open into an associated homogenization zone 114. The equalization zone 114 surrounds a corresponding needle stump 116.

In der zweiten Platte 104 ist ebenfalls eine Fällmittelbohrung 118 ausgenommen, die von einem weiterem Nadelstumpf 120 und einem Ringraum 122 umgeben ist. Weiterhin sind weitere Zuführkanäle 124 mit anschließender Vergleichmäßigungszone 126 in der zweiten Platte 104 ausgenommen. Schließlich weist die dritte Platte 106 zwei Ringspalten 128 und 130 für die jeweiligen polymeren Materialien, die koextrudiert werden sollen, auf, sowie eine Nadel 132 mit Fällmittelbohrung 134. Bei den Varianten der Figur 3a, Figur 3b und Figur 3c sind die Zuführkanäle 124 jeweils anders ausgestaltet. Während in der Ausführungsvariante gemäß der Figur 3a der Zuführungskanal 124 für das zweite Polymer lediglich in der zweiten Platte 104 vorgesehen ist, verläuft der in der Variante gemäß der Figur 3b sowohl durch die zweite Platte 104 wie auch durch die dritte Platte 106. In der Ausführungsvariante gemäß der Figur 3c verläuft der Zuführkanal 124 für das zweite Polymer durch die zweite Platte 104 und die erste Platte 102, wie hier in der Figur 3c dargestellt. Die Darstellung gemäß Figur 5 entspricht dem Schnitt gemäß Figur 3a, wobei hier deutlich wird, dass 8 Zuführkanäle 112 sternförmig angeordnet sind, während lediglich 4 Zuführkanäle 124 kreuzförmig angeordnet sind.In the second plate 104, a precipitant hole 118 is also excluded, which is surrounded by a further needle stub 120 and an annular space 122. Furthermore, further feed channels 124 with subsequent homogenization zone 126 are excluded in the second plate 104. Finally, the third plate 106 has two annular gaps 128 and 130 for the respective polymeric materials to be co-extruded, and a needle 132 with precipitant well 134. In the variants of Figs 3a, 3b and 3c the supply channels 124 are each configured differently. While in the embodiment according to the FIG. 3a the feed channel 124 for the second polymer is provided only in the second plate 104, which runs in the variant according to the FIG. 3b either through the second plate 104 as well as through the third plate 106. In the embodiment according to the Figure 3c For example, the second polymer feed passage 124 extends through the second plate 104 and the first plate 102 as shown in FIG Figure 3c shown. The representation according to FIG. 5 corresponds to the section according to FIG. 3a , wherein it is clear here that 8 feed channels 112 are arranged in a star shape, while only 4 feed channels 124 are arranged in a cross shape.

Die drei Platten 102, 104 und 106 werden wiederum durch ein geeignetes Bondverfahren, vorteilhaft ein Direktbonden, miteinander zum Grundkörper 100 verbunden. Ansonsten entspricht das Herstellverfahren für die Hohlfaser-Spinndüse 10 gemäß der Figuren 3 und 5, analog demjenigen, wie es bereits anhand der Figur 2 und 4 im einzelnen erläutert wurde.The three plates 102, 104 and 106 are in turn connected to the main body 100 by a suitable bonding method, advantageously direct bonding. Otherwise corresponds to the manufacturing method for the hollow fiber spinneret 10 according to the Figures 3 and 5 , analogous to that, as already stated by the FIG. 2 and 4 was explained in detail.

Claims (9)

  1. A hollow fiber spinning nozzle in which coagulation agent/support agent passages and mass supply passages and a nozzle structure connected to these and having a mass discharge opening and a needle with a coagulation agent/support agent bore are formed in a base body,
    characterized in that
    at least two plate-shaped bodies structured by means of microstructure technology are joined together to form the base body.
  2. A hollow fiber spinning nozzle in accordance with claim 1, wherein it consists of mono-crystalline silicon, gallium arsenide (GaAs) or germanium.
  3. A hollow fiber spinning nozzle in accordance with either of claims 1 or 2, wherein the mass discharge opening is an annular gap.
  4. A hollow fiber spinning nozzle in accordance with any of claims 1 to 3, wherein it consists of two plates, with the mass supply passages, a mass flow homogenization zone, a coagulation agent/support agent supply bore and a needle stub being cut out in the first plate, while in the second plate a nozzle structure with a mass annular gap and a needle with a coagulation agent/support agent bore are cut out.
  5. A hollow fiber spinning nozzle in accordance with any of claims 1 to 3, wherein it consists of two plates, with a coagulation agent/support agent supply bore being cut out in the first plate, while in the second plate mass supply passages, a mass flow homogenization zone and a nozzle structure with a mass annular gap and a needle with a coagulation agent/support agent bore are cut out.
  6. A hollow fiber spinning nozzle in accordance with either of claims 4 or 5, wherein its individual components have the following dimensions: Thickness of the first plate: 0.250 - 1.500 mm Thickness of the second plate: 0.050 - 1.500 mm Outer diameter of the needle: 0.020 - 1.500 mm Length of the needle, incl. needle stub: 0.100 - 2.000 mm Diameter of the coagulation agent bore: 0.010 - 1.000 mm Length of the coagulation agent bore: 0.150 - 2.500 mm Outer diameter of the annular gap: 0.040 - 3.000 mm Length of the annular gap: 0.050 - 1.500 mm Height of the spinning nozzle: 0.300 - 3.000 mm Edge length of the spinning nozzle: 1.000 - 25.00 mm.
  7. A hollow fiber spinning nozzle in accordance with any of claims 1 to 3, wherein it consists of three plates, with the first plate including supply passages, a homogenization zone and a needle stub with a central supply bore, a second plate which adjoins the first plate having supply passages, a homogenization zone and a further needle stub with a concentric ring passage as well as a needle extension with a central bore and with a third plate which in turn adjoins the second plate, having a nozzle structure consisting of a central bore and two concentric annular gaps.
  8. A hollow fiber spinning nozzle in accordance with any of claim 1 to 3, wherein the base body is made up of three individual plates, with the first plate having a central supply bore, a plate adjoining the first plate having parallel supply passages and homogenization zones associated with these as well as a needle stub with a concentric ring passage and a central bore and with the third plate adjoining the second plate having a nozzle structure consisting of a central bore and two concentric annular gaps.
  9. A hollow fiber spinning nozzle in accordance with either of claims 7 or 8, wherein the outer diameter of the multi-passage hollow fiber spinning nozzle is smaller than 1 mm, preferably smaller than or equal to 0.45 mm.
EP03706500A 2002-03-13 2003-02-13 Hollow-fiber spinning nozzle Expired - Lifetime EP1483435B1 (en)

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