EP0494852B1 - Process for the production of cellulosic articles - Google Patents

Process for the production of cellulosic articles Download PDF

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Publication number
EP0494852B1
EP0494852B1 EP92890004A EP92890004A EP0494852B1 EP 0494852 B1 EP0494852 B1 EP 0494852B1 EP 92890004 A EP92890004 A EP 92890004A EP 92890004 A EP92890004 A EP 92890004A EP 0494852 B1 EP0494852 B1 EP 0494852B1
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Prior art keywords
nozzle
air gap
length
amounts
hole diameter
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EP92890004A
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German (de)
French (fr)
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EP0494852A3 (en
EP0494852A2 (en
Inventor
Stefan Ing. Zikeli
Heinrich Dipl.-Ing. Dr. Firgo
Dieter Dipl.-Ing. Dr. Eichinger
Raimund Jurkovic
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Lenzing AG
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Lenzing AG
Chemiefaser Lenzing AG
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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
    • D01D4/00—Spinnerette packs; Cleaning thereof
    • D01D4/02—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
    • D01D5/06—Wet spinning methods
    • 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
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof

Definitions

  • the present invention relates to a method for producing a cellulosic shaped body, in which a cellulosic amine oxide solution is pressed through a nozzle, then passed through an air gap, optionally stretched therein and finally coagulated in a precipitation bath.
  • fibers with good performance properties can only be obtained from high polymers if a "fiber structure" can be achieved (Ullmann, 5th edition vol. A10, 456).
  • a fiber structure can be achieved (Ullmann, 5th edition vol. A10, 456).
  • melt spinning the fibers are stretched in the warm, plastic state while the molecules are still mobile. Dissolved polymers can be spun dry or wet. In dry spinning, drawing takes place while the solvent escapes or evaporates; the threads extruded into a coagulation bath are drawn during the coagulation. Methods of this type are known and are well described. In all of these cases, it is important that the transition from the liquid state (regardless of whether melt or solution) to the solid state takes place in such a way that the polymer chains or chain packages (i.e. fibrids, fibrils, etc.) are also oriented during thread formation can be.
  • EP-A-295 672 describes the production of aramid fibers, which are introduced, stretched and introduced into a non-coagulating medium via an air gap are then coagulated.
  • DD-PS 218 121 deals with the spinning of cellulose in amine oxides via an air gap, measures being taken to prevent sticking.
  • a disadvantage of this method is that extremely high take-off speeds are required in order to achieve the appropriate textile properties and fineness of the threads. Furthermore, it has been shown in practice that a long air gap on the one hand leads to fiber sticking and on the other hand leads to spinning insecurity and thread breakage in the event of high warpage. Precautions are therefore required to prevent this.
  • a method of this type is described in AT-PS 365 663 (or in equivalent US-PS 4,261,943). For large-scale production, however, the number of holes in a spinneret must be very high. In such a case, precautions to prevent the surface stickiness of the freshly extruded threads which enter the precipitant through an air gap are completely inadequate.
  • the minimum hole diameter of the nozzle used is at most 150 »m, preferably at most 70» m, and the length of the nozzle channel is at least 1000 »m, preferably about 1500» m, where the minimum hole diameter on the outlet side of the nozzle channel is present over at least 1/4, preferably over at least 1/3, of the length of the nozzle channel.
  • the spun thread also has good textile properties: it was found that the elongation at break in particular can be improved. Work capacity - d. H. the product of elongation and strength - behaves inversely proportional to the hole diameter. Furthermore, the loop strength and the associated elongation at break improve, which results in an improved abrasion resistance of the fabrics spun from these fibers. These properties also improve with decreasing hole diameters.
  • the nozzle channel is preferably widened conically on the inlet side and cylindrical on the outlet side.
  • the use of such nozzles is recommended because of the simpler manufacture; it is difficult to z. B. 1500 »m long nozzle with a diameter of only z. B. 100 »m.
  • a nozzle in which the minimum diameter is only provided on the outlet side (e.g. to 1/4 or 1/3 of the length) and which widens conically in the direction of the inlet side is much easier to manufacture and also gives good results.
  • Examples 1 to 3 are only for comparison, Examples 4 to 6 are examples according to the invention. Particularly noteworthy is the excellent value of 47.8 for the conditioned fiber strength in Example 6; Such a value is only reached with a delay of 100 with conventional nozzles!
  • Examples 1 to 3 A comparison of Examples 1 to 3 with Examples 4 to 6 immediately shows that the elongation at break is also improved by using nozzles according to the invention. Furthermore, it can be seen from Examples 4 to 6 that the product of strength and elongation at break (FFk * FDk), the loop strength and the elongation at break increase in the measurement of the loop strength with decreasing hole diameter.
  • a comparison of Example 1 with Example 5 shows that these values can also be improved by using long-channel nozzles according to the invention compared to nozzles with a short channel of the same diameter.
  • Examples 2 and 3 show that with a small nozzle channel length, the fiber properties depend on the distortion in the air gap; they get better as the default increases.
  • Examples 4 and 5 show that, under comparable conditions (warpage, hole diameter), all textile properties - except the elongation at break - are significantly improved by a long-channel nozzle according to the invention.
  • Example 6 shows that by using a small hole diameter of 50 »m, all textile properties are significantly improved.

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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)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Woven Fabrics (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Description

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung eines cellulosischen Formkörpers, bei dem eine cellulosische Aminoxidlösung durch eine Düse gepreßt, anschließend durch einen Luftspalt geführt, in diesem gegebenenfalls verstreckt und schließlich in einem Fällbad koaguliert wird.The present invention relates to a method for producing a cellulosic shaped body, in which a cellulosic amine oxide solution is pressed through a nozzle, then passed through an air gap, optionally stretched therein and finally coagulated in a precipitation bath.

Es ist bekannt, daß Fasern mit guten Gebrauchseigenschaften aus Hochpolymeren nur dann erhalten werden, wenn eine "Faserstruktur" erzielt werden kann (Ullmann, 5. Auflage Vol. A10, 456). Unter anderem ist es dazu nötig, mikroorientierte Bereiche im Polymeren, beispielsweise Fibride, in der Faser auszurichten. Diese Orientierung wird vom Herstellungsverfahren bestimmt und beruht auf physikalischen oder physikochemischen Vorgängen. In vielen Fällen bewirkt eine Verstreckung diese Orientierung.It is known that fibers with good performance properties can only be obtained from high polymers if a "fiber structure" can be achieved (Ullmann, 5th edition vol. A10, 456). Among other things, it is necessary to align micro-oriented areas in the polymer, for example fibrids, in the fiber. This orientation is determined by the manufacturing process and is based on physical or physicochemical processes. In many cases, stretching causes this orientation.

In welchem Verfahrensabschnitt und unter welchen Bedingungen diese Verstreckung erfolgt, ist ausschlaggebend für die erhaltenen Fasereigenschaften. Beim Schmelzspinnen werden die Fasern im warmen plastischen Zustand, während die Moleküle noch beweglich sind, verstreckt. Gelöste Polymere können trocken oder naß gesponnen werden. Beim Trockenspinnen erfolgt die Verstreckung, während das Lösungsmittel entweicht bzw. verdampft; die in ein Fällbad extrudierten Fäden werden während der Koagulierung verstreckt. Verfahren dieser Art sind bekannt und reichlich beschrieben. In all diesen Fällen ist es aber wichtig, daß der Übergang vom flüssigen Zustand (unabhängig, ob Schmelze oder Lösung) zum festen Zustand so erfolgt, daß während der Fadenbildung auch eine Orientierung der Polymerketten oder -kettenpakete (sprich Fibride,Fibrillen usw.) erzielt werden kann.The stage of the process and the conditions under which this stretching takes place are decisive for the fiber properties obtained. In melt spinning, the fibers are stretched in the warm, plastic state while the molecules are still mobile. Dissolved polymers can be spun dry or wet. In dry spinning, drawing takes place while the solvent escapes or evaporates; the threads extruded into a coagulation bath are drawn during the coagulation. Methods of this type are known and are well described. In all of these cases, it is important that the transition from the liquid state (regardless of whether melt or solution) to the solid state takes place in such a way that the polymer chains or chain packages (i.e. fibrids, fibrils, etc.) are also oriented during thread formation can be.

Um das schlagartige Verdampfen eines Lösungsmittels aus einem Faden während des Trockenspinnens zu verhindern,gibt es mehrere Möglichkeiten.There are several ways to prevent the sudden evaporation of a solvent from a thread during dry spinning.

Die Problematik der sehr raschen Koagulation des Polymeren beim Naßspinnen (wie z. B. im Falle von cellulosischen Aminoxidlösungen) konnte jedoch bisher nur durch Kombination von Trocken- und Naßspinnen gelöst werden.However, the problem of the very rapid coagulation of the polymer during wet spinning (such as in the case of cellulosic amine oxide solutions) has so far only been able to be solved by combining dry and wet spinning.

So ist bekannt, Lösungen von Polymeren über einen Luftspalt in das Koagulationsmedium einzubringen. In der EP-A-295 672 ist die Herstellung von Aramidfasern, die über einen Luftspalt in ein nicht-koagulierendes Medium eingebracht, verstreckt und anschließend koaguliert werden, beschrieben.It is known, for example, to introduce solutions of polymers into the coagulation medium via an air gap. EP-A-295 672 describes the production of aramid fibers, which are introduced, stretched and introduced into a non-coagulating medium via an air gap are then coagulated.

Die DD-PS 218 121 hat das Verspinnen von Cellulose in Aminoxiden über einen Luftspalt zum Gegenstand, wobei Vorkehrungen, die das Verkleben verhindern, vorgesehen sind.DD-PS 218 121 deals with the spinning of cellulose in amine oxides via an air gap, measures being taken to prevent sticking.

Gemäß der US-PS 4 501 886 wird eine Lösung von Cellulose-triacetat mittels eines Luftspaltes gesponnen.According to US Pat. No. 4,501,886, a solution of cellulose triacetate is spun by means of an air gap.

In der US-PS 3 414 645 ist ebenfalls die Herstellung von aromatischen Polyamiden aus Lösungen, in einem Trocken-Naß-Spinnverfahren beschrieben.US Pat. No. 3,414,645 also describes the preparation of aromatic polyamides from solutions in a dry-wet spinning process.

Bei all diesen Verfahren wird im Luftspalt eine gewisse Orientierung erzielt, denn alleine das Ausfließenlassen einer zähflüssigen Lösung durch eine kleine Öffnung nach unten zwingt aufgrund der Schwerkraft den Lösungsteilchen eine Orientierung auf. Diese Orientierung durch die Schwerkraft kann noch erhöht werden, wenn die Extrudiergeschwindigkeit der Polymerlösung und die Abzugsgeschwindigkeit des Fadens so eingestellt sind, daß eine Verstreckung erzielt wird.With all of these methods, a certain orientation is achieved in the air gap, because just letting a viscous solution flow out through a small opening downwards forces the solution particles to find their way due to gravity. This orientation by gravity can be increased if the rate of extrusion of the polymer solution and the rate of withdrawal of the thread are adjusted so that drawing is achieved.

Ein Verfahren dieser Art ist in der AT-PS 387 792 (bzw. den dazu äquivalenten US-PSen 4 246 221 und 4 416 698) beschrieben. Eine Lösung von Cellulose in NMMO (NMMO = N-Methylmorpholin-N-oxid) und Wasser wird geformt, im Luftspalt verstreckt und anschließend ausgefällt. Die Verstreckung wird bei einem Streckverhältnis von mindestens 3 vorgenommen. Dazu ist eine Luftspaltlänge von 5-70 cm notwendig.A method of this type is described in AT-PS 387 792 (or the equivalent US Pat. Nos. 4,246,221 and 4,416,698). A solution of cellulose in NMMO (NMMO = N-methylmorpholine-N-oxide) and water is formed, stretched in the air gap and then precipitated. The stretching is carried out at a stretch ratio of at least 3. This requires an air gap length of 5-70 cm.

Ein Nachteil dieses Verfahrens besteht darin, daß extrem hohe Abzugsgeschwindigkeiten erforderlich sind, um entsprechende textile Eigenschaften und Feinheit der Fäden zu erzielen. Weiters hat sich in der Praxis gezeigt, daß ein langer Luftspalt einerseits zu Faserverklebungen und anderseits bei hohen Verzügen auch zu Spinnunsicherheit und Fadenbruch führt. Es sind daher Vorkehrungen nötig, dies zu verhindern. Ein Verfahren dieser Art ist in der AT-PS 365 663 (bzw. in der äquivalenten US-PS 4 261 943) beschrieben. Für eine Großproduktion muß aber die Lochzahl in einer Spinndüse sehr hoch sein. In so einem Fall sind Vorkehrungen zur Verhinderung der Oberflächenklebrigkeit der frisch extrudierten Fäden, die durch einen Luftspalt in das Fällungsmittel gelangen, völlig unzureichend.A disadvantage of this method is that extremely high take-off speeds are required in order to achieve the appropriate textile properties and fineness of the threads. Furthermore, it has been shown in practice that a long air gap on the one hand leads to fiber sticking and on the other hand leads to spinning insecurity and thread breakage in the event of high warpage. Precautions are therefore required to prevent this. A method of this type is described in AT-PS 365 663 (or in equivalent US-PS 4,261,943). For large-scale production, however, the number of holes in a spinneret must be very high. In such a case, precautions to prevent the surface stickiness of the freshly extruded threads which enter the precipitant through an air gap are completely inadequate.

Es ist Aufgabe der vorliegenden Erfindung, ein Spinnverfahren zu schaffen, mit dem trotz Verwendung eines kurzen Luftspaltes eine rasch koagulierende Lösung zu Fäden mit verbesserten Fasereigenschaften versponnen werden kann.It is an object of the present invention to provide a spinning process with which, despite the use of a short air gap, a rapidly coagulating solution can be spun into threads with improved fiber properties.

Diese Aufgabe wird durch ein Verfahren der eingangs genannten Art erfindungsgemäß dadurch gelöst, daß der minimale Lochdurchmesser der verwendeten Düse höchstens 150 »m, vorzugsweise höchstens 70 »m, und die Länge des Düsenkanals mindestens 1000 »m, vorzugsweise etwa 1500 »m, beträgt wobei der minimale Lochdurchmesser auf der Austrittsseite des Düsenkanals über mindestens 1/4, vorzugsweise über mindestens 1/3 der Länge des Düsenkanals vorhanden ist.This object is achieved according to the invention by a method of the type mentioned in the introduction in that the minimum hole diameter of the nozzle used is at most 150 »m, preferably at most 70» m, and the length of the nozzle channel is at least 1000 »m, preferably about 1500» m, where the minimum hole diameter on the outlet side of the nozzle channel is present over at least 1/4, preferably over at least 1/3, of the length of the nozzle channel.

Durch Verwendung derartiger Langkanaldüsen mit geringem Durchmesser wird bereits in den Düsenkanälen durch Scherkräfte eine Orientierung des Polymeren erzielt. Dadurch kann der anschließende Luftspalt kurz gehalten werden: seine Länge beträgt zweckmäßigerweise höchstens 35, vorzugsweise höchstens 10mm. Dadurch wird die Störanfälligkeit stark reduziert; es gibt nur wesentlich geringere Titerschwankungen und damit keine Fadenrisse mehr; benachbarte Fäden können infolge des kürzeren Luftspaltes nicht mehr verkleben, sodaß die Lochdichte in der Spinndüse erhöht werden kann, wodurch die Produktivität steigt.By using such long-channel nozzles with a small diameter, an orientation of the polymer is achieved in the nozzle channels by shear forces. This allows the subsequent air gap to be kept short: its length is expediently at most 35 mm, preferably at most 10 mm. This greatly reduces the susceptibility to faults; there are only significantly fewer fluctuations in titer and therefore no more thread breaks; Because of the shorter air gap, neighboring threads can no longer stick together, so that the hole density in the spinneret can be increased, which increases productivity.

Schließlich hat der gesponnene Faden auch gute textile Eigenschaften: Es wurde gefunden, daß insbesondere die Bruchdehnung verbessert werden kann. Das Arbeitsvermögen - d. h. das Produkt aus Dehnung und Festigkeit - verhält sich dabei umgekehrt proportional zum Lochdurchmesser. Weiters verbessert sich die Schlingenfestigkeit und die dazugehörende Bruchdehnung, was sich in einer verbesserten Scheuerbeständigkeit der aus diesen Fasern ersponnenen Gewebenäußert. Diese Eigenschaften verbessern sich ebenfalls bei sinkenden Lochdurchmessern.Finally, the spun thread also has good textile properties: it was found that the elongation at break in particular can be improved. Work capacity - d. H. the product of elongation and strength - behaves inversely proportional to the hole diameter. Furthermore, the loop strength and the associated elongation at break improve, which results in an improved abrasion resistance of the fabrics spun from these fibers. These properties also improve with decreasing hole diameters.

Vorzugsweise ist der Düsenkanal auf der Eintrittsseite kegelförmig erweitert und auf der Austrittsseite zylinderförmig. Die Verwendung derartiger Düsen ist wegen der einfacheren Herstellbarkeit empfehlenswert; es ist schwierig, eine z. B. 1500 »m lange Düse durchgehend mit einem Durchmesser von nur z. B. 100 »m herzustellen. Eine Düse, bei der der minimale Durchmesser nur auf der Austrittsseite vorgesehen ist (z. B. auf 1/4 oder 1/3 der Länge) und die sich in Richtung Eintrittsseite kegelförmig erweitert, ist wesentlich leichter herstellbar und liefert auch gute Ergebnisse.The nozzle channel is preferably widened conically on the inlet side and cylindrical on the outlet side. The use of such nozzles is recommended because of the simpler manufacture; it is difficult to z. B. 1500 »m long nozzle with a diameter of only z. B. 100 »m. A nozzle in which the minimum diameter is only provided on the outlet side (e.g. to 1/4 or 1/3 of the length) and which widens conically in the direction of the inlet side is much easier to manufacture and also gives good results.

Anhand der folgenden Beispiele wird die Erfindung näher erläutert:
   2276 g Zellstoff (Feststoff- oder Trockengehalt 94 %, DP=750 [DP = Durchschnittlicher Polymerisationsgrad]) und 0,02 % Rutin als Stabilisator werden in 26 139 g 60%iger wässeriger N-Metyhlmorpholinoxid-Lösung suspendiert. Während 2 Stunden wird bei 100°C und einem Vakuum bis zu 50 bis 300 mbar 9415 g Wasser abdestilliert. Die dabei entstandene Lösung wird anhand der Viskosität und unter dem Mikroskop beurteilt.The invention is explained in more detail using the following examples:
2276 g of pulp (solid or dry content 94%, DP = 750 [DP = average degree of polymerization]) and 0.02% rutin as stabilizer are suspended in 26 139 g of 60% aqueous N-methylmorpholine oxide solution. 9415 g of water are distilled off at 100 ° C. and under a vacuum of up to 50 to 300 mbar for 2 hours. The resulting solution is assessed on the basis of viscosity and under a microscope.

Parameter der Spinnlösung:Spinning solution parameters:

Cellulose Buckey V5 (α = 97,8 %, Viskosität bei 25°C und 0,5 Masse-% Zellstoffdichte: 10,8 cP)Cellulose Buckey V5 (α = 97.8%, viscosity at 25 ° C and 0.5 mass% cellulose density: 10.8 cP) 10 %10% Wasserwater 12 %12% NMMONMMO 78 %78% Komplexe Viskosität der Spinnmasse bei 95°C RV20, Oszillation mit w=0,31 [1/s]Complex viscosity of the spinning mass at 95 ° C RV20, oscillation with w = 0.31 [1 / s] 1680 Pas1680 Pas

Anschließend wird diese Lösung bei einer Spinntemperatur von 75°C durch eine Spinndüse gepreßt, einen 9 mm langen Luftspalt geführt und schließlich in einem Fällbad, welches aus einer 20%igen wässerigen NMMO-Lösung besteht, koaguliert. Tabelle 1 enthält die bei diesem Versuch erzielten Eigenschaften der Fasern und die dazugehörenden Prozeßparameter.

Figure imgb0001
This solution is then pressed through a spinneret at a spinning temperature of 75 ° C., passed through a 9 mm long air gap and finally coagulated in a precipitation bath which consists of a 20% aqueous NMMO solution. Table 1 contains the properties of the fibers achieved in this test and the associated process parameters.
Figure imgb0001

Die Beispiele 1 bis 3 dienen nur zum Vergleich, die Beispiele 4 bis 6 sind erfindungsgemäße Beispiele. Besonders hervorgehoben werden soll der hervorragende Wert von 47,8 für die konditionierte Faserfestigkeit bei Beispiel 6 werden; ein derartiger Wert wird bei herkömmlichen Düsen erst bei einem Verzug von 100 erreicht!Examples 1 to 3 are only for comparison, Examples 4 to 6 are examples according to the invention. Particularly noteworthy is the excellent value of 47.8 for the conditioned fiber strength in Example 6; Such a value is only reached with a delay of 100 with conventional nozzles!

Aus einem Vergleich der Beispiele 1 bis 3 mit den Beispielen 4 bis 6 ist unmittelbar ersichtlich, daß durch den Einsatz erfindungsgemäßer Düsen auch die Bruchdehnung verbessert wird. Weiters ist aus den Beispielen 4 bis 6 ersichtlich, daß das Produkt aus Festigkeit und Bruchdehnung (FFk*FDk), die Schlingenfestigkeit sowie die Bruchdehnung bei der Messung der Schlingenfestigkeit mit sinkendem Lochdurchmesser steigen. Ein Vergleich von Beispiel 1 mit Beispiel 5 (bei diesen beiden Beispielen ist der Lochdurchmesser gleich) zeigt, daß diese Werte auch durch den Einsatz erfindungsgemäßer Langkanaldüsen gegenüber Düsen mit kurzem Kanal gleichen Durchmessers verbessert werden.A comparison of Examples 1 to 3 with Examples 4 to 6 immediately shows that the elongation at break is also improved by using nozzles according to the invention. Furthermore, it can be seen from Examples 4 to 6 that the product of strength and elongation at break (FFk * FDk), the loop strength and the elongation at break increase in the measurement of the loop strength with decreasing hole diameter. A comparison of Example 1 with Example 5 (in these two examples the hole diameter is the same) shows that these values can also be improved by using long-channel nozzles according to the invention compared to nozzles with a short channel of the same diameter.

Die Beispiele 2 und 3 zeigen, daß bei kleiner Düsenkanallänge die Fasereigenschaften vom Verzug im Luftspalt abhängen; sie werden mit steigendem Verzug besser. Die Beispiele 4 und 5 zeigen, daß bei vergleichbaren Verhältnissen (Verzug, Lochdurchmesser) durch eine erfindungsgemäße Langkanaldüse alle textilen Eigenschaften - ausgenommen die Bruchdehnung - wesentlich verbessert werden. Beispiel 6 zeigt, daß durch Anwendung eines kleinen Lochdurchmessers von 50 »m alle textilen Eigenschaften wesentlich verbessert werden.Examples 2 and 3 show that with a small nozzle channel length, the fiber properties depend on the distortion in the air gap; they get better as the default increases. Examples 4 and 5 show that, under comparable conditions (warpage, hole diameter), all textile properties - except the elongation at break - are significantly improved by a long-channel nozzle according to the invention. Example 6 shows that by using a small hole diameter of 50 »m, all textile properties are significantly improved.

Claims (4)

  1. A method for the production of a cellulose shaped body, in which a cellulose amine oxide solution is pressed through a nozzle, is then guided through an air gap, is stretched in the latter if necessary and is finally coagulated in a precipitation bath, characterised in that the minimum hole diameter of the nozzle which is used amounts to at most 150 »m, preferably at most 70 »m, and the length of the nozzle canal amounts to at least 1000 »m, preferably approximately 1500 »m, in which the minimum hole diameter is present on the outlet side of the nozzle canal over at least 1/4, preferably over at least 1/3 of the length of the nozzle canal.
  2. A method according to Claim 1, characterised in that the length of the air gap amounts to at most 35 mm, preferably at most 10 mm.
  3. A method according to Claim 1 or 2, characterised in that the nozzle canal is widened in a conical shape on the inlet side and is cylindrical on the outlet side.
  4. A method according to Claim 3, characterised in that the angle of divergence of the conical widening amounts to 8°.
EP92890004A 1991-01-09 1992-01-09 Process for the production of cellulosic articles Expired - Lifetime EP0494852B1 (en)

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AT32/91 1991-01-09
AT0003291A AT395863B (en) 1991-01-09 1991-01-09 METHOD FOR PRODUCING A CELLULOSIC MOLDED BODY

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EP0494852A2 EP0494852A2 (en) 1992-07-15
EP0494852A3 EP0494852A3 (en) 1993-03-17
EP0494852B1 true EP0494852B1 (en) 1995-05-17

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CS2292A3 (en) 1992-08-12
US5252284A (en) 1993-10-12
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FI97155C (en) 1996-10-25
ZA9110195B (en) 1992-10-28
SK279852B6 (en) 1999-04-13
PL169309B1 (en) 1996-06-28
ATA3291A (en) 1992-08-15
FI920072L (en) 1992-07-10
JPH04308220A (en) 1992-10-30
FI97155B (en) 1996-07-15
DK0494852T3 (en) 1995-07-10
SI9112009A (en) 1994-12-31
FI920072A0 (en) 1992-01-08
NO920108L (en) 1992-07-10
CA2059043A1 (en) 1992-07-10
HU212340B (en) 1996-05-28
PH29990A (en) 1996-10-29
BG60111B2 (en) 1993-10-29
PL293115A1 (en) 1992-08-24
RU2072006C1 (en) 1997-01-20
TR27259A (en) 1994-12-22
AT395863B (en) 1993-03-25
ES2072746T3 (en) 1995-07-16
CZ282528B6 (en) 1997-08-13
NO920108D0 (en) 1992-01-08
DE59202175D1 (en) 1995-06-22
YU47623B (en) 1995-10-24
RO107701B1 (en) 1993-12-30
YU200991A (en) 1994-01-20
BR9200043A (en) 1992-09-08
MX9200080A (en) 1992-07-01
NO303696B1 (en) 1998-08-17
EP0494852A3 (en) 1993-03-17
EP0494852A2 (en) 1992-07-15
HU9200064D0 (en) 1992-04-28

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