EP0902852B1 - Procede de production d'un fil cellulosique - Google Patents

Procede de production d'un fil cellulosique Download PDF

Info

Publication number
EP0902852B1
EP0902852B1 EP97927053A EP97927053A EP0902852B1 EP 0902852 B1 EP0902852 B1 EP 0902852B1 EP 97927053 A EP97927053 A EP 97927053A EP 97927053 A EP97927053 A EP 97927053A EP 0902852 B1 EP0902852 B1 EP 0902852B1
Authority
EP
European Patent Office
Prior art keywords
yarns
aqueous alkaline
solution
treatment
alkaline solution
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
EP97927053A
Other languages
German (de)
English (en)
Other versions
EP0902852A1 (fr
Inventor
Abdulmajid Hashemzadeh
Peter Raidt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Akzo Nobel NV
Original Assignee
Akzo Nobel NV
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Akzo Nobel NV filed Critical Akzo Nobel NV
Publication of EP0902852A1 publication Critical patent/EP0902852A1/fr
Application granted granted Critical
Publication of EP0902852B1 publication Critical patent/EP0902852B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • 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 invention relates to a method for producing a cellulosic yarn by spinning a possibly still water and optionally a stabilizer-containing solution of cellulose in a tertiary amine oxide to fibers or filaments, cases, Washing and drying.
  • WO95 / 24524 discloses a method for color properties to improve fabrics from so-called Lyocell yarns.
  • Lyocell yarns are solvent-spun cellulose yarns that by spinning a solution of cellulose in one organic solvents are produced. With the solvent it is essentially an aqueous tertiary amine oxide, for example N-methylmorpholine-N-oxide (NMMO).
  • NMMO N-methylmorpholine-N-oxide
  • fabrics from the named Cellulose yarns undergo mercerization, i.e. with a treated alkaline solution. This mercerization corresponds in principle the one that is common for cotton fabrics and it will an aqueous NaOH solution with a Concentration of 10 to 30% by weight at room temperature or slightly elevated temperature (e.g.
  • WO95 / 24524 in which aqueous NaOH solutions with a concentration of 14% by weight or 25 % By weight was used, the treatment of tissues was carried out from Lyocell yarns at room temperature over a period of 45 Seconds. This gave tissues after dyeing had a deeper shade than non-mercerized ones Tissue.
  • the invention was therefore based on the object of a method for Production of cellulosic yarns by spinning one possibly still water and possibly containing a stabilizer Solution of cellulose in a tertiary amine oxide to fibers or Filaments, cases, washing and drying are available too with the disadvantages described above at least be reduced.
  • the treatment is preferably carried out with the aqueous alkaline Solution over a period of 1 to 15 seconds, especially preferably 1 to 10 seconds, in particular 2 to 6 seconds.
  • An aqueous NaOH or KOH solution is preferably used.
  • the concentration of alkali in the aqueous alkaline solution should be between 0.5 and 20% by weight, preferably between 10 and 14 % By weight.
  • the aqueous alkaline solution can be more inorganic or organic auxiliaries, such as in particular Contain emulsifiers, salts, glycerin or the like.
  • the treatment temperature has a range from 0 to 60 ° C proven to be favorable, with 20 to 60 ° C, in particular 40 to 60 ° C are preferred.
  • treatment with the aqueous alkaline solution to yarns that were previously made have not been dried.
  • the treatment is therefore preferably carried out after washing the yarn. Implementation of the treatment with the aqueous alkaline solution before washing, i.e. to felling is also possible, but complicates Recovery of the tertiary amine oxide from the wash water, because in the subsequent washing the tertiary amine oxide and Alkaline solution get into the wash water.
  • aqueous alkaline solution After treatment with the aqueous alkaline solution should the yarn in an aqueous acidic solution, such as an acetic acid solution, neutralized, washed again and then dried.
  • an aqueous acidic solution such as an acetic acid solution
  • tertiary amine oxide preferably used N-methylmorpholine-N-oxide (NMMO) and the cellulose solution may contain propyl gallic acid as Stabilizer.
  • NMMO N-methylmorpholine-N-oxide
  • L (1-10) The main reason for this effect is the increase in the crystallite size L (1-10) .
  • This crystal dimension in particular is influenced by treatment with an aqueous alkaline solution.
  • L (1-10) has values in the range from 3 to 4 nm. Treating the yarns with aqueous alkaline solution results in a 50% increase in L (1-10) .
  • the wet abrasion test equipment For measuring the tendency to fibrillation of cellulosic yarns serves the wet abrasion test apparatus shown schematically in the figure.
  • the wet abrasion test equipment consists of essentially from those designated by reference numerals 1 to 6 Elements that are described in more detail below.
  • the yarn 2 is fixed in a PVC block 1.
  • the abrasion will generated by the yarn 2 via a rotating glass rod 5 with 6 mm diameter, on which a ceramic rod 4th with 2.5 mm diameter is attached.
  • the glass rod 5 is in a distance of 80 mm to the PVC block 1.
  • the Glass rod 5 and with it the ceramic rod 4 rotate with one Speed of 25 revolutions per minute.
  • the distance of the weight 6 to the glass rod 5 is 60 mm.
  • the wet scrub test was carried out on the following Examples carried out over a minute or two. With defined and reproducible fibrillation of the apparatus was graded on a scale from 1 to 6 microscopic evaluation of the scrubbed yarn area rated.
  • Primary fibrillation means that only on the fiber surface Fibrils are observed.
  • Secondary fibrillation means that the fibrils are also in the deeper layers of the filaments can be observed. The stronger the secondary fibrillation progresses, the longer and the fibrils become thicker.
  • the wet abrasion test was carried out for each of the following examples carried out five times each and an average grade calculated.
  • a high weight loss is economical disadvantageous and also makes recovery very difficult the alkaline solution if this after cleaning again to be used in the process.
  • the solved Cellulose concentrates in the aqueous over time alkaline solution.
  • the separation of dissolved cellulose As such, the aqueous alkaline solution is already there difficult.
  • a separation of the dissolved cellulose for example via centrifugation or filtration, but is definitely with higher costs and with loss of alkaline solution connected so that the lowest possible weight loss is sought should be in order to minimize cellulose in the to dissolve aqueous alkaline solution.
  • weight loss also affects Yarn properties and leads to filament or fiber breaks and Lint formation, which in turn affects the processability of the yarn negatively influenced and leads to a reduction in quality.
  • Example 4 While in Examples 1 to 3 the yarns are in a bath aqueous NaOH immersed for a certain time and thus stress-free treatment with the aqueous alkaline Solution were subjected in Example 4 each dried yarns (trial Nos. 1 to 4) and not before dried yarns (Experiment Nos. 5 to 13) continuously a bath with aqueous NaOH was drawn through. In contrast to Examples 1 to 3 were carried out according to Example 4 thus not tension-free, but in such a way that the yarn under one Tension in the order of 2 to 10 cN stood. The However, tensile stress should not exceed 10 cN if possible, otherwise the yarn could be stretched again the desired effect of reducing the would reduce fibrillation.
  • Tables 5 and 6 show textile data of yarns produced according to the invention (Table 5) and of comparison yarns (Table 6).
  • the treatment with the aqueous alkaline solution was carried out continuously, as described in Example 4.

Landscapes

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

Claims (10)

  1. Procédé de fabrication de fils cellulosiques par filage d'une solution de cellulose dans un oxyde d'amine tertiaire contenant éventuellement encore de l'eau et éventuellement un agent stabilisant, donnant des fibres ou filaments, coagulation, lavage et séchage de ceux-ci, caractérisé par le fait que l'on traite les fils, avant de les sécher, pendant une durée d'immersion inférieure à 20 secondes avec une solution aqueuse alcaline.
  2. Procédé selon la revendication 1, caractérisé par le fait que le traitement avec la solution aqueuse alcaline dure de 1 à 10 secondes, de préférence de 2 à 6 secondes.
  3. Procédé selon la revendication 1 ou 2, caractérisé par le fait que l'on utilise comme solution aqueuse alcaline une solution de NaOH ou de KOH.
  4. Procédé selon la revendication 1, 2 ou 3, caractérisé par le fait que la concentration de la solution aqueuse en alcali est comprise entre 0,5 et 20 % en poids, de préférence entre 10 et 14 % en poids.
  5. Procédé selon l'une ou plusieurs des revendications 1 à 4, caractérisé par le fait que la solution aqueuse alcaline contient d'autres adjuvants inorganiques ou organiques.
  6. Procédé selon la revendication 5, caractérisé par le fait que l'on utilise comme adjuvants des agents émulsionnants, des sels ou du glycérol.
  7. Procédé selon l'une ou plusieurs des revendications 1 à 6, caractérisé par le fait que le traitement est réalisé à une température comprise entre 0 et 60 °C, de préférence entre 20 et 60 °C.
  8. Procédé selon l'une ou plusieurs des revendications 1 à 7, caractérisé par le fait que le traitement avec la solution aqueuse alcaline est réalisé après le lavage des fils.
  9. Procédé selon l'une ou plusieurs des revendications 1 à 8, caractérisé par le fait que les fils sont neutralisés, après traitement avec la solution aqueuse alcaline, dans une solution aqueuse acide, et sont ensuite lavés puis séchés.
  10. Procédé selon l'une ou plusieurs des revendications 1 à 9, caractérisé par le fait que l'on utilise comme oxyde d'amine tertiaire le N-oxyde de la N-méthylmorpholine.
EP97927053A 1996-05-30 1997-05-27 Procede de production d'un fil cellulosique Expired - Lifetime EP0902852B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19621602 1996-05-30
DE19621602 1996-05-30
PCT/EP1997/002742 WO1997046745A1 (fr) 1996-05-30 1997-05-27 Procede de production d'un fil cellulosique

Publications (2)

Publication Number Publication Date
EP0902852A1 EP0902852A1 (fr) 1999-03-24
EP0902852B1 true EP0902852B1 (fr) 2000-03-01

Family

ID=7795617

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97927053A Expired - Lifetime EP0902852B1 (fr) 1996-05-30 1997-05-27 Procede de production d'un fil cellulosique

Country Status (10)

Country Link
US (1) US6042767A (fr)
EP (1) EP0902852B1 (fr)
JP (1) JP2000511598A (fr)
AT (1) ATE190098T1 (fr)
AU (1) AU3168297A (fr)
DE (1) DE59701182D1 (fr)
ES (1) ES2145609T3 (fr)
ID (1) ID18177A (fr)
TW (1) TW382030B (fr)
WO (1) WO1997046745A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT411769B (de) * 2002-07-12 2004-05-25 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer formkörper
US20050278868A1 (en) * 2004-05-21 2005-12-22 Tetsutaro Fumisi Method of producing cotton fiber product having smooth surfaces and cotton-regenerated cellulose compound yarn or fabric
TWI667378B (zh) 2014-01-03 2019-08-01 奧地利商蘭精股份有限公司 纖維素纖維
EP3494254B1 (fr) 2016-08-04 2021-09-29 PVH Corp. Tissus et vêtements sans repassage, et leur procédé de finition

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9103297D0 (en) * 1991-02-15 1991-04-03 Courtaulds Plc Fibre production method
US5662858A (en) * 1993-04-21 1997-09-02 Lenzing Aktiengesellschaft Process for the production of cellulose fibres having a reduced tendency to fibrillation
GB9404510D0 (en) * 1994-03-09 1994-04-20 Courtaulds Fibres Holdings Ltd Fibre treatment
GB9407496D0 (en) * 1994-04-15 1994-06-08 Courtaulds Fibres Holdings Ltd Fibre treatment

Also Published As

Publication number Publication date
ID18177A (id) 1998-03-12
AU3168297A (en) 1998-01-05
US6042767A (en) 2000-03-28
TW382030B (en) 2000-02-11
ES2145609T3 (es) 2000-07-01
JP2000511598A (ja) 2000-09-05
DE59701182D1 (de) 2000-04-06
EP0902852A1 (fr) 1999-03-24
ATE190098T1 (de) 2000-03-15
WO1997046745A1 (fr) 1997-12-11

Similar Documents

Publication Publication Date Title
DE69511532T2 (de) Behandlung von fasern
DE860389C (de) Verfahren zur Herstellung von Gebilden aus regenerierter Cellulose
US5403530A (en) Elongate member production method
DE969389C (de) Verfahren zur Herstellung von baumwollaehnlichen Faeden, Fasern oder Baendchen durch Verformung von Viscose
DE69322170T2 (de) Faserbehandlung
EP0853146A2 (fr) Procédé de production de fibres cellulosiques et fibres cellulosiques
DE69007682T2 (de) Verfahren zur Herstellung von färbbaren poly(paraphenylen-terephtalamid) Fasern mit kationischen Farbstoffen.
EP0799333B1 (fr) Fibres et fils de cellulose presentant une propension reduite a la formation de fibrilles
DE1669427B1 (de) Verfahren zum Herstellen von schwer entflammbaren Faeden oder Fasern aus regenerierter Cellulose
DE974548C (de) Verfahren zur Herstellung von Gebilden, wie Faeden oder Filmen, aus regenerierter Cellulose
CH685944A5 (de) Verfahren zur Herstellung von Cellulosefasern mit verringerter Fibrillierneigung.
EP0902852B1 (fr) Procede de production d'un fil cellulosique
DE971618C (de) Verfahren zur Herstellung von Viscosekunstseidenfaeden
DE1258544B (de) Verfahren zur Herstellung von Regeneratcellulosefasern und -faeden
DE69925988T2 (de) Verfahren zur behandlung von kulierware
DE1083016B (de) Verfahren zur Herstellung von kuenstlichen Gebilden, wie Faeden oder Filme, aus Viscose
DE568571C (de) Verfahren zur Herstellung kuenstlicher Faeden oder Faserbuendel aus Viskose mit hoherFestigkeit und Dehnung
WO1997004148A1 (fr) Fibres de cellulose
DE1234916B (de) Verfahren zur Herstellung von aus regenerierter Cellulose bestehenden Faeden, Fasernoder Folien
EP0783602B1 (fr) Fibre cellulosique
AT367805B (de) Verfahren zur herstellung von fasern aus regenerierter zellulose
EP0888467B1 (fr) Procede de production de fibres cellulosiques a tendance reduite a la fibrillation
AT160368B (de) Verfahren zur Herstellung von Kunstfasern.
DE1135614B (de) Verfahren zur Herstellung von Cellulosehydratfaeden
AT118594B (de) Verfahren zur Erhöhung der Dehnbarkeit und Elastizität von künstlichen Fäden.

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19981105

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT DE ES FR GB IT NL

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

17Q First examination report despatched

Effective date: 19990618

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

ITF It: translation for a ep patent filed
AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT DE ES FR GB IT NL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20000301

REF Corresponds to:

Ref document number: 190098

Country of ref document: AT

Date of ref document: 20000315

Kind code of ref document: T

ET Fr: translation filed
REF Corresponds to:

Ref document number: 59701182

Country of ref document: DE

Date of ref document: 20000406

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 20000328

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2145609

Country of ref document: ES

Kind code of ref document: T3

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20020501

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20020502

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20020520

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20020522

Year of fee payment: 6

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20020606

Year of fee payment: 6

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030527

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030527

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030528

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20031202

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20030527

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040130

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20030528

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20050527