EP0799333B1 - Fibres et fils de cellulose presentant une propension reduite a la formation de fibrilles - Google Patents

Fibres et fils de cellulose presentant une propension reduite a la formation de fibrilles Download PDF

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Publication number
EP0799333B1
EP0799333B1 EP95943196A EP95943196A EP0799333B1 EP 0799333 B1 EP0799333 B1 EP 0799333B1 EP 95943196 A EP95943196 A EP 95943196A EP 95943196 A EP95943196 A EP 95943196A EP 0799333 B1 EP0799333 B1 EP 0799333B1
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EP
European Patent Office
Prior art keywords
yarns
fibers
process according
treatment
carried out
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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
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EP95943196A
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German (de)
English (en)
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EP0799333A1 (fr
Inventor
Abdulmajid Hashemzadeh
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Akzo Nobel NV
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Akzo Nobel NV
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
    • 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
    • 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
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core
    • 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
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/2964—Artificial fiber or filament
    • Y10T428/2965—Cellulosic

Definitions

  • the invention relates to cellulosic fibers or yarns reduced tendency to form fibrils and a procedure for the production of such fibers or yarns, the Fibers preferably after the NMMO thread formation process getting produced.
  • This solution is then filtered and passed through a nozzle, preferably with the interposition of an air gap, in a mostly aqueous precipitation bath extruded, whereby by Coagulation of the shaped bodies such as threads, yarns, films and the like. arise.
  • These moldings are then washed to still remove existing tertiary amine oxide. Subsequently the molded body can be dried and processed in the usual way, e.g. be wound up, etc.
  • the NMMO process stands out from the classic ones Process for the production of cellulosic moldings all from the fact that it is essentially physical processes, so at least theoretically no chemical reactions take place and no chemical ones By-products arise that are disposed of as waste products or back into the starting products by chemical methods should be converted.
  • the NMMO process therefore belongs basically to the very environmentally friendly processes.
  • the actual starting product is a renewable one Raw material, and the cellulosic end product is biodegradable.
  • the cellulosic fibers especially those made by the NMMO process become fibrillated, especially when wet tend to, especially when mechanical forces are on the fibers act. This includes when dyeing the case, it also occurs already when washing the fibers, if they leave after of the coagulation bath freed from solvent that is still present should be.
  • the existing fibrils are made of course with all further processing operations, also in dry condition, more or less unpleasant noticeable.
  • fibril formation for the Achieve special surface effects can, but for most uses is fibril formation undesirable.
  • the object of the invention is therefore cellulosic fibers and to provide yarns, especially those which were obtained according to the NMMO method, which via have a reduced tendency to form fibrils, which but at the same time have a very good dyeability that is called a dyeability, which is essentially the dyeability of untreated fibers corresponds or only insignificantly is reduced, and their mechanical textile data, especially the stretch compared to untreated fibers are not or only slightly deteriorated.
  • Task of The invention is also a corresponding method for To provide access to such fibers that are economical, reproducible Results that work continuously, one high spinning speed allowed and no subsequent related cleaning or neutralization levels needed.
  • This object is achieved by a manufacturing method of cellulosic fibers or yarns with reduced Tendency to fibril formation by treating but not yet washed after the thread forming process dried fibers or yarns with a crosslinking agent, characterized in that the fibers or yarns with amino, polyalkylene oxide, epoxy or carboxyl functional modified, reactive polysiloxanes with self-crosslinking same treated.
  • the reactive siloxanes are preferably combined in known in particular but with low formaldehyde or free crosslinkers used.
  • the reactive polysiloxanes are preferably side chain modified.
  • fibers or yarns are treated which were obtained according to the NMMO method.
  • Siloxane solutions can be aqueous, alcoholic or aqueous / alcoholic Solutions are available; the solutions can also be found at Use of other solvents such as toluene, acetone and the like. have been produced.
  • Aqueous microemulsions are aqueous dispersions particularly suitable. Microemulsions are understood to mean particularly fine-particle emulsions in which the particle sizes of the distributed liquid particles predominantly in the Are in the nanometer range, e.g. at 40 nm.
  • the emulsions can be conventional ionic or nonionic Contain emulsifiers.
  • the treatment according to the invention preferably takes place at a temperature of 180 to 250 ° C instead, taking treatment times from 0.5 seconds to 5 minutes, in particular 10 seconds to 20 seconds may be preferred.
  • the Treatment on a hot contact plate is special advantageous.
  • the method according to the invention can be advantageous perform continuously.
  • the fiber After soaking, spraying or applying the siloxane the fiber is expediently passed between two rollers, to squeeze off excess solution or dispersion.
  • the fiber is then fed to a zone in which is at an elevated temperature. Preferably points this route has a temperature of 180 to 250 ° C.
  • This Treatment at the elevated temperature involves at the same time a drying of the fibers.
  • the applied siloxane crosslinks which consists essentially of self-networking, i.e. a crosslinking of the polysiloxane with the OH groups Cellulose is not found or only to a minor extent instead of.
  • Fibers or yarn e.g. passed over a contact heating plate be at a temperature of, for example 250 ° C is set.
  • the treatment time is usually even shorter than that for a conventional convection dryer is the case. So times of about 0.5 to 1 to 2 seconds are sufficient, to bring about self-networking and the fiber too dry.
  • contact heating plate it is also possible in addition to the contact heating plate still use hot air.
  • Another option is there by treating the fibers with rays, e.g. with microwaves, UV light and the like.
  • the method according to the invention can for example be as follows be performed:
  • Partial water separation creates a spinning solution
  • the composition cellulose 14%, water 11%, NMMO 74.86%.
  • the spinning solution also contains 0.14% as a stabilizer Propyl gallic acid.
  • This spinning solution which has a temperature of 120 ° C, is by means of a spinning pump through a spinneret with 50 Holes - the single hole diameter is 130 ⁇ m - in pressed an air gap.
  • the air gap has a length of 18 cm. A stretching of 15.9 takes place in the air gap instead of; then the filaments in an aqueous Precipitation bath coagulates.
  • the threads are withdrawn from the precipitation bath and into a Wash section led in which the remaining in the thread NMMO is washed out. After leaving the washing section part of the water stripped; in addition the fiber blown with a jet of air at room temperature so that the fiber still has a residual water content of approx. 300%.
  • An aqueous dispersion is placed over a rotating godet of the active siloxane applied. After passing one The fiber is squeezed by a convection dryer passed, which has a temperature of 250 ° C. The fiber stays in the dryer for 10 seconds.
  • the fiber After leaving the dryer, the fiber is used a nozzle to a moisture content of 11%.
  • a common finishing agent is applied at the same time.
  • the number L that is used to assess the dyeability was measured as follows:
  • the measurement of the dyeability of the tissues was carried out using the Minolta Chroma-Meter Cr-300, Cr-310 and CR-331 performed.
  • the value L is a measure of the brightness of the colored Product. The lower this value is, the better it is Dyeability.
  • Table 2 shows the values on one same yarn as in Table 1 were obtained with the difference that the treated yarns before the Treatment has been dried, i.e. no primary swelling owned more.
  • the tear times are compared to the untreated Yarn practical at the lower concentrations unchanged.
  • One is only at elevated concentrations Notice improvement, but in no way to the Improvement can reach, which not yet dried yarns can be obtained.
  • the invention further relates to cellulosic fibers and / or yarns with a reduced tendency to form fibrils, characterized in that the fibers or yarns are one the fibers still possessing the primary swelling
  • a coating consisting of essentially self-crosslinked at least bifunctional reactive siloxanes as defined in claim 1, consists.
  • the amount of the coating is preferably 0.1 up to 1% by weight based on the cellulosic fibers or Yarns.
  • the fibers are further characterized in that they one, compared to the untreated fibers or Yarning, no or insignificant reduction in elongation and have dyeability. They are also characterized by that they are compared to the untreated fibers have at least twice the tear time.
  • the fibers or yarns are preferably produced by the NMMO thread forming process.
  • the breaking time is a measure of the tendency of the fibers or yarns to fibrillate (see Tables I and II).
  • a bundle (1) of 50 filaments which is fixed at one end with a thread clamp (2), is guided through a thread guide (3).
  • the bundle (1) is adjusted with a Y-piece (4) in relation to an ejector (10).
  • the ejector (10) is followed by a thread guide (5) with which the bundle (1) is deflected, which is loaded with a weight 6 of 20 grams at its second end.
  • the distance between the first thread guide (3) and the Y-piece (4) and between the Y-piece (4) and the ejector inlet is approx. 3 cm in each case.
  • the distance between the ejector outlet and the second thread guide (5) is approximately 11 cm.
  • the ejector (10) has a length of 22 mm.
  • the ejector (10) has an inlet gap (11) with a square cross section for the bundle (1).
  • the width b e and the height h e of the entry gap (11) are 1 mm.
  • the thread channel (12) extending through the entire ejector (10) has opposite liquid supply channels (14, 14 ') in the two side walls (13, 13'). Through these liquid supply channels (14, 14 ') water flows at a temperature of about 25 ° C at an angle a of 15 ° relative to the axis of the bundle (1).
  • the water flows with a volume flow of 45 l / h in total into the thread channel (12) and exits the ejector (10) at the outlet gap (15).
  • the width b z of the liquid supply channels (14, 14 ') is 0.6 mm and their height h z 1 mm.
  • the length l z of the feed channels (14, 14 ') is 6 mm.
  • the width b of the thread channel (12) from the confluence of the liquid supply channels (14, 14 ') to the outlet gap (15) is 1.2 mm.
  • the height h is 1 mm.
  • the supply with water takes place through bores (16, 16 ') with a diameter of 4 mm from the underside of the ejector (10).
  • the ejector (10) is closed from above with a cover, not shown, lying flat.
  • the filament bundle (1) 1 inserted into the device parts and with the Weight loaded.
  • the water supply in the ejector (10) represents the beginning of the time measurement.
  • the time measurement is ended at the time the weight drops, i.e. if the bundle breaks.
  • individual measurements were carried out, and the given data mean values from these 10 represent the tear time Measurements. The higher this value is, the lower it is fibrillation.
  • Functionally reactive in the context of the invention means that when treating the fibers with the coating agent, at which an elevated temperature is preferably used, a networking of the applied agent with itself takes place something like a self-condensation and that practically no crosslinking with the cellulose, i.e. with the Hydroxyl groups of cellulose takes place.
  • Self-crosslinking is preferably carried out at pH values of 4 to 12.
  • Reactive polysiloxanes operating under the conditions of Self-networking can be used, e.g. in Textilveredlung 20 (1985) No. 1, pages 8 to 12.
  • the amino, polyalkylene oxide and epoxide functional modified reactive siloxanes are discussed in this review exemplified by formulas that the Figures 7, 9, 10 correspond.
  • Carboxyl functional modified polysiloxanes have a side chain modification correspondingly the carboxyl group. It will preferably those that are functionally modified on the side chain Polysiloxanes used.
  • the polysiloxanes can simply be side chain modified, i.e. they just point functional groups of a certain kind, but it is also possible to use double modified siloxanes, i.e. Polysiloxanes, which have different functional groups have.
  • the end groups of the modified polysiloxanes are preferred Hydroxyl, alkoxy and saturated alkyl groups especially the methyl group.
  • Polysiloxanes with the vinyl group as an end group are less within the scope of the invention suitable.
  • the functionally modified polysiloxanes which are used according to the invention, are all commercially available available products.
  • Page 10 shown amino functional silicones as they can be used according to the invention.
  • Further usable functional silicones are in the prospectus remove.
  • Suitable microemulsions are also there offered, e.g. the silicone microemulsion CT96E on page 14 of the prospectus.
  • silicones in the attachment mentioned there for crosslinking for cellulose fibers that no longer have a primary swelling have, i.e. have already been dried, e.g. to the To give fibers a water-repellent finish.
  • Treatment under self-networking conditions however, according to the invention on the fibers, threads and yarns between the washing section that connects to the spinning bath and carried out the dryer. That is called Treatment takes place on the not yet dried fibers instead of.
  • Filaments within the scope of the invention also include i.e. Understand endless fibers.
  • fibers, filaments and yarns obtained in the still have their original elongation and have excellent dyeability and beyond an unexpectedly high reduction in the tendency to form fibrils have.
  • the fibers can be in the usual way processed, i.e. wound into yarns of various titers can be processed. Tissues, Knitted fabrics and other textile fabrics manufactured due to their low tendency to fibrillate distinguished from other products.
  • fibers, Filaments and yarns from all common cellulosic Raw materials products such as cotton linters, cellulose and the like. produce.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Claims (16)

  1. Procédé pour la fabrication de fibres ou fils cellulosiques ayant une tendance réduite à la fibrillation, par traitement des fibres ou fils lavés en sortie de l'étape de formation des fibres mais non encore séchés, avec un agent de réticulation, caractérisé par le fait que l'on traite les fibres ou fils avec des polysiloxanes réactifs fonctionnalisés par des groupes amino, polyalkylèneoxy, époxy ou carboxy, et l'autoréticulation de ceux-ci.
  2. Procédé selon la revendication 1, caractérisé par le fait que l'on utilise des polysiloxanes réactifs fonctionnalisés au niveau des chaínes latérales.
  3. Procédé selon l'une des revendications 1 à 2, caractérisé par le fait que l'on réalise le traitement en utilisant en outre des agents de réticulation connus, en particulier des agents de réticulation pauvres en formaldéhyde ou exempts de formaldéhyde.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé par le fait que l'on traite des fibres ou fils obtenus par une étape de formation de fibres selon un procédé utilisant le N-oxyde de N-méthylmorpholine (procédé NMMO).
  5. Procédé selon une des revendications 1 à 4, caractérisé par le fait que l'on utilise pour le traitement des fibres ou fils une dispersion aqueuse ou une solution ayant une concentration en siloxane réactif comprise entre 0,1 et 5 % en poids.
  6. Procédé selon une des revendications 1 à 5, caractérisé par le fait que l'on utilise pour le traitement des fibres ou fils une microémulsion aqueuse.
  7. Procédé selon une des revendications 1 à 6, caractérisé par le fait que l'on réalise le traitement à une température allant de 180 à 250 °C.
  8. Procédé selon une des revendications 1 à 7, caractérisé par le fait que l'on réalise le traitement sur une plaque de contact chaude.
  9. Procédé selon une des revendications 1 à 7, caractérisé par le fait que l'on réalise le traitement sur des galettes chaudes.
  10. Procédé selon une des revendications 1 à 7, caractérisé par le fait que l'on réalise le traitement dans de l'air chaud.
  11. Procédé selon une des revendications 1 à 7, caractérisé par le fait que l'on réalise le traitement dans de l'air chaud en combinaison avec une plaque de contact chaude et/ou des galettes chaudes.
  12. Procédé selon une des revendications 1 à 11, caractérisé par le fait que le traitement est un traitement en continu.
  13. Fibres ou fils cellulosiques ayant une tendance réduite à la fibrillation, caractérisés par le fait que les fibres ou fils portent un revêtement appliqué sur les fibres ou fils présentant encore un gonflement primaire, lequel revêtement est constitué essentiellement de polysiloxanes réactifs fonctionnalisés par des groupes amino, polyalkylèneoxy, époxy ou carboxy.
  14. Fibres ou fils selon la revendication 13, caractérisé par le fait que le revêtement est présent à raison de 0,1 à 1 % en poids rapporté au poids des fibres, filaments ou fils cellulosiques.
  15. Fibres, filaments ou fils selon la revendication 13 ou 14, caractérisés par un temps de rupture au moins deux fois plus long que le temps de rupture de fibres ou fils par ailleurs identiques mais ne portant pas de revêtement de siloxanes réactifs, au moins bifonctionnels, autoréticulés.
  16. Fibres ou fils cellulosiques selon une ou plusieurs des revendications 13 à 15, caractérisés par le fait que les fibres ou fils ont été préparés selon un procédé de formation de fibres utilisant le N-oxyde de N-méthylmorpholine (procédé NMMO).
EP95943196A 1994-12-23 1995-12-22 Fibres et fils de cellulose presentant une propension reduite a la formation de fibrilles Expired - Lifetime EP0799333B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4446307 1994-12-23
DE4446307 1994-12-23
PCT/EP1995/005109 WO1996020302A1 (fr) 1994-12-23 1995-12-22 Fibres et fils de cellulose presentant une propension reduite a la formation de fibrilles

Publications (2)

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EP0799333A1 EP0799333A1 (fr) 1997-10-08
EP0799333B1 true EP0799333B1 (fr) 2000-06-07

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EP95943196A Expired - Lifetime EP0799333B1 (fr) 1994-12-23 1995-12-22 Fibres et fils de cellulose presentant une propension reduite a la formation de fibrilles

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US (2) US6048479A (fr)
EP (1) EP0799333B1 (fr)
JP (1) JPH10511439A (fr)
AT (1) ATE193737T1 (fr)
AU (1) AU4433996A (fr)
CA (1) CA2207856A1 (fr)
DE (1) DE59508458D1 (fr)
TW (1) TW293043B (fr)
WO (1) WO1996020302A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006030342A1 (de) * 2006-06-30 2008-01-03 Momentive Performance Materials Gmbh & Co. Kg Verfahren zur Herstellung von Cellulosefasern mit verringerter Kristallinität

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GB2307203B (en) * 1993-04-21 1997-09-10 Chemiefaser Lenzing Ag Process for the production of cellulose fibres having a reduced tendency to fibrillation
US20060078847A1 (en) * 2000-09-29 2006-04-13 Kwan Norman H Dental implant system and additional methods of attachment
US6432270B1 (en) 2001-02-20 2002-08-13 Kimberly-Clark Worldwide, Inc. Soft absorbent tissue
US6511580B1 (en) 2001-11-15 2003-01-28 Kimberly-Clark Worldwide, Inc. Soft absorbent tissue containing derivitized amino-functional polysiloxanes
US6576087B1 (en) 2001-11-15 2003-06-10 Kimberly-Clark Worldwide, Inc. Soft absorbent tissue containing polysiloxanes
US6599393B1 (en) 2001-11-15 2003-07-29 Kimberly-Clark Worldwide, Inc. Soft absorbent tissue containing hydrophilically-modified amino-functional polysiloxanes
US6582558B1 (en) 2001-11-15 2003-06-24 Kimberly-Clark Worldwide, Inc. Soft absorbent tissue containing hydrophilic polysiloxanes
US6514383B1 (en) 2001-11-15 2003-02-04 Kimberly-Clark Worldwide, Inc. Soft absorbent tissue containing derivitized amino-functional polysiloxanes
WO2009031869A2 (fr) * 2007-09-07 2009-03-12 Kolon Industries, Inc. Fibres à base de cellulose et câble à pneus les comprenant
US10011931B2 (en) 2014-10-06 2018-07-03 Natural Fiber Welding, Inc. Methods, processes, and apparatuses for producing dyed and welded substrates
KR102591968B1 (ko) 2016-03-25 2023-10-20 네추럴 파이버 웰딩 인코포레이티드 용접된 기재를 제조하기 위한 방법, 공정, 및 장치
CA3021729A1 (fr) 2016-05-03 2017-11-09 Natural Fiber Welding, Inc. Methodes, procedes et appareils permettant de produire des substrats colores et soudes

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US3952134A (en) * 1970-03-23 1976-04-20 Celanese Corporation Continuous filament product
DE2616797C3 (de) * 1976-04-15 1981-03-12 Chemische Fabrik Pfersee Gmbh, 8900 Augsburg Verfahren zum Imprägnieren und Beschichten von Textilien mit Polymeren, die reaktive Gruppen enthalten
US5520869A (en) * 1990-10-12 1996-05-28 Courtaulds Plc Treatment of fibre
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US5593483A (en) * 1995-03-27 1997-01-14 Advanced Chemical Technologies, Inc. Water repellent composition for cellulose containing materials and method for producing same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006030342A1 (de) * 2006-06-30 2008-01-03 Momentive Performance Materials Gmbh & Co. Kg Verfahren zur Herstellung von Cellulosefasern mit verringerter Kristallinität

Also Published As

Publication number Publication date
WO1996020302A1 (fr) 1996-07-04
AU4433996A (en) 1996-07-19
DE59508458D1 (de) 2000-07-13
US6048479A (en) 2000-04-11
CA2207856A1 (fr) 1996-07-04
JPH10511439A (ja) 1998-11-04
US6180234B1 (en) 2001-01-30
EP0799333A1 (fr) 1997-10-08
TW293043B (fr) 1996-12-11
ATE193737T1 (de) 2000-06-15

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