WO1998002602A1 - Procede de fabrication de fibres filees avec solvant - Google Patents

Procede de fabrication de fibres filees avec solvant Download PDF

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Publication number
WO1998002602A1
WO1998002602A1 PCT/GB1997/001882 GB9701882W WO9802602A1 WO 1998002602 A1 WO1998002602 A1 WO 1998002602A1 GB 9701882 W GB9701882 W GB 9701882W WO 9802602 A1 WO9802602 A1 WO 9802602A1
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WO
WIPO (PCT)
Prior art keywords
fibre
percent
never
dried
range
Prior art date
Application number
PCT/GB1997/001882
Other languages
English (en)
Inventor
Ian Graveson
Dianne Parker
Susan Janet Taylor
Original Assignee
Courtaulds Fibres (Holdings) Limited
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 Courtaulds Fibres (Holdings) Limited filed Critical Courtaulds Fibres (Holdings) Limited
Priority to AU35495/97A priority Critical patent/AU3549597A/en
Publication of WO1998002602A1 publication Critical patent/WO1998002602A1/fr

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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

  • This invention relates to processes for the manufacture of lyocell fibre which include the step of contacting the fibre in never-dried state with an aqueous solution of an alkali metal hydroxide.
  • Lyocell fibres are known, and their manufacture is described for example in US-A-4 , 416 , 698 , the contents of which are incorporated herein by way of reference.
  • Cellulose is dissolved in a solvent containing a tertiary amine N-oxide (which may also be called for brevity an amine oxide), for example N-methylmorpholine N-oxide (NMMO).
  • NMMO N-methylmorpholine N-oxide
  • the solvent generally also contains a proportion of a non-solvent for cellulose, for example water.
  • the resulting solution is extruded through a suitable die to produce fibres, which are coagulated, washed in water to remove the solvent, and dried.
  • solvent spinning This process of extrusion and coagulation is referred to as "solvent spinning", and the cellulose fibre produced thereby is referred to as "solvent-spun" cellulose fibre or as lyocell fibre.
  • cellulose fibres can be made by extrusion of a solution of a cellulose derivative into a coagulating and regenerating bath.
  • a viscose process In which the cellulose derivative is cellulose xa ⁇ thate.
  • Solvent spinning has a number of advantages over other known processes for the manufacture of elongate cellulose members, such as the viscose process, for example reduced environmental emissions.
  • Lyocell fibres are known to be prone to fibrillation. Fibrillation is a phenomenon which in the main occurs when lyocell fibres are subjected to mechanical forces during wet-processing, and it results in the partial detachment of fine longitudinal fibrils from the fibres. Fibrillation is in general considered to be undesirable in textile end-uses, and efforts have been made to reduce or eliminate fibrillation tendency by chemical aftertreatments , such as those described in US-A-5 , 310 , 424 , or by suitable choice of spinning parameters, as described for example in WO-A-95/02082.
  • Copending unpublished British patent application no. 9611252.9 describes a process for the manufacture of lyocell fibre which includes the characterising step of applying to the reconstituted but never-dried fibre for 20 seconds or more an aqueous liquor which comprises from 10 to 18 percent by weight sodium hydroxide. This process is said to enable the manufacture of lyocell fibre with controlled, in particular reduced, fibrillation tendency.
  • cellulose exhibits a swelling maximum in aqueous sodium hydroxide at a sodium hydroxide concentration of about 10 percent by weight.
  • the present inventors have found that lyocell fibres may tend to shrink in length during treatment in relaxed state with sodium hydroxide, in particular at and around the swelling maximum, and that excessive shrinkage has adverse effects on the tensile properties of the fibres. It is an object of the present invention to provide a method of avoiding such adverse effects on the tensile properties, while retaining the benefits of sodium hydroxide treatment.
  • lyocell fibre is manufactured by a method which includes the step of contacting the fibre in never-dried state with an aqueous solution of an alkali metal hydroxide, and the lengthwise shrinkage of the fibre during the said step is controlled at a value within the range from 5 to 20 percent.
  • a method for the manufacture of lyocell fibre including the steps in sequential order of:
  • the organic solvent is preferably a tertiary amine N-oxide, further preferably N-methylmorpholine N-oxide, and preferably contains a minor proportion of water.
  • the solution preferably comprises from 5 to 30, more preferably from 15 to 25, percent by weight cellulose and from 5 to 20 percent by weight water.
  • the solution may additionally comprise one or more other substances, for example a thermal stabiliser such as propyl gallate, in known manner.
  • the titre of the lyocell fibre may be in the range from 0.5 to 10 decitex.
  • the method of the invention is performed on lyocell fibre in the form of continuous filament yarn or tow and the lengthwise shrinkage of the fibre during the alkali treatment step is controlled by controlling the ratio of the velocities of the fibre as it leaves and enters the said step to be within the range from 0.8:1 to 0.95:1.
  • the method of the invention may be performed on lyocell fibre in the form of continuous filament yarn, tow or staple fibre and the lengthwise shrinkage of the fibre during the alkali treatment step is controlled by suitable choice of the concentration of alkali metal hydroxide and the temperature of the aqueous solution.
  • the lengthwise shrinkage of the fibre is conveniently measured by treating a sample of never-dried fibre cut to known length, for example 25 cm long, in relaxed state with the aqueous solution, followed by washing and drying, and comparing the length of the dried fibre with that of the cut fibre prior to the alkali treatment step.
  • the alkali metal hydroxide is preferably sodium hydroxide, although other compounds such as potassium hydroxide may alternatively be used.
  • the aqueous solution of alkali metal hydroxide may comprise from 5 to 18, preferably from 8 to 13, percent by weight sodium hydroxide.
  • the temperature of the aqueous solution of alkali metal hydroxide is preferably in the range from 0 to 60°C, more preferably from 20 to 30 °C. It will be appreciated that routine experimentation may be required in the second embodiment of the invention to select conditions of concentration and temperature which ensure that the lengthwise shrinkage of the fibre falls within the desired range .
  • the aqueous solution of alkali metal hydroxide may be applied to the fibre by any convenient conventional means, for example using a circulating bath, wicking roller or spray.
  • a circulating bath When a circulating bath is used, the residence time of the fibre therein may conveniently be in the range from 5 to 120 seconds.
  • alkali metal hydroxide is washed from the fibre.
  • the fibre is washed with hot water, preferably followed by a sour wash with dilute aqueous acid so that the fibre pH is below 7.
  • the fibre is washed with an aqueous acid solution.
  • the acid may be a mineral acid such as hydrochloric acid or sulphuric acid, the concentration thereof in the aqueous acid solution being in the range from 0.1 to 20, preferably from 1 to 15, percent by volume, or it may be an organic acid such as acetic acid, the concentration thereof in the aqueous acid solution being in the range from 25 to 75, preferably from 40 to 60, percent by volume.
  • the washing liquor may be applied to the fibre by any convenient means, for example using a circulating bath, wicking roller or spray.
  • a circulating bath for example, wicking roller or spray.
  • the residence time of the fibre in such a circulating bath may conveniently be in the range from 5 to 120 seconds.
  • the method of the invention has the advantage that it permits control over and maintenance of fibre tensile properties at the same time as it imparts the advantages which flow from treatment of never-dried lyocell fibres with aqueous alkali as described in the aforementioned British patent applications.
  • Dry lyocell fibre (approx 0.05 g) is cut to 10 mm lengths and placed in an industrial blender together with 400 ml tap The blender is then operated for a time between 30 second and 3 minutes to induce fibrillation; the time required depends inter alia on the nature of the blender blade and j 3 chosen so that a standard sample of commercial lyocell fib -e (available from Courtaulds Fibres (Holdings) Limited under the Trade Mark TENCEL) exhibits a fibrillation index in the range 6.5 to 8.0. The fibre is then collected and dried and assessed for degree of fibrillation.
  • Fibrillation Index There is no universally accepted standard for assessment of fibrillation, and the following method was used to assess Fibrillation Index (F.I.).
  • F.I. Fibrillation Index
  • a series of samples of fibre having nil and increasing degrees of fibrillation was identified.
  • a standard length of fibre from each sample was then measured, and the number of fibrils (fine hairy spurs extending from the main body of the fibre) along the standard length was counted.
  • the length of each fibril was measured, and an arbitrary number, being the product of the number of fibrils multiplied by the average length of each fibril, was determined for each fibre.
  • the fibre exhibiting the highest value of this product was identified as being the most fibrillated fibre and was assigned an arbitrary Fibrillation Index of 10.
  • the wholly unfibrillated fibre was assigned a Fibrillation Index of zero, and the remaining fibres were graded from 0 to 10 based on the microscopically measured arbitrary numbers.
  • the measured fibres were then used to form a standard graded scale.
  • To determine the Fibrillation Index for any other sample of fibre five or ten fibres were visually compared under the microscope with the standard graded fibres. The visually determined numbers for each fibre were then averaged to give a Fibrillation Index for the sample under test. It will be appreciated that visual determination and averaging is many times quicker than measurement, and it has been found that skilled fibre technologists are consistent in their rating of fibres.
  • fabrics containing fibre with F.I. 2 or more may have a "frosted" appearance.
  • a desirable target for fibre F.I. is 1 or less, preferably 0.5 or less, in fabric, including laundered fabric.
  • fibre was 20 treated with 9-13% NaOH solutions at 10°C, shrinkage being measured at around 40%; or with 9 or 11% NaOH solutions at 5°C, shrinkage being measured at around 50%.
  • the fibres were severely weakened, and F.I.s were unmeasureable because the fibres disintegrated during 25 testing.
  • Lyocell fibre was spun and washed as in Example 1.
  • the fibre in tow form was then passed first through a bath containing 11% w/v aqueous sodium hydroxide 30 at 25 "C and next through a bath containing 15% v/v aqueous sulphuric acid at ambient temperature, either under tension or in relaxed state.
  • roller speeds into and out of the NaOH bath were 2.69 and 2.16 m/min respectively, corresponding to a controlled shrinkage of 19.3%.
  • the fibre was then rinsed and dried as in Example 1.
  • the results shown in Table 2 were obtained :
  • the fibre treated under tension exhibited a good combination of properties in comparison with that treated in relaxed state, and both samples exhibited a good combination of properties in comparison with the control.

Abstract

La présente invention permet de maîtriser la tendance à la fibrillation de fibres filées avec solvant; elle consiste à appliquer une solution aqueuse d'hydroxyde alcalin sur la fibre à l'état non déshydraté dans des conditions telles que la retrait en longueur de la fibre au cours de cette étape est maintenu dans une plage de valeurs allant de 5 à 20 pour cent.
PCT/GB1997/001882 1996-07-12 1997-07-11 Procede de fabrication de fibres filees avec solvant WO1998002602A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU35495/97A AU3549597A (en) 1996-07-12 1997-07-11 Method for the manufacture of lyocell fibre

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9614679.0 1996-07-12
GBGB9614679.0A GB9614679D0 (en) 1996-07-12 1996-07-12 Manufacture of fibre

Publications (1)

Publication Number Publication Date
WO1998002602A1 true WO1998002602A1 (fr) 1998-01-22

Family

ID=10796808

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1997/001882 WO1998002602A1 (fr) 1996-07-12 1997-07-11 Procede de fabrication de fibres filees avec solvant

Country Status (3)

Country Link
AU (1) AU3549597A (fr)
GB (1) GB9614679D0 (fr)
WO (1) WO1998002602A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000018991A1 (fr) * 1998-09-29 2000-04-06 Lenzing Aktiengesellschaft Procede de production de fibres cellulosiques
WO2015101543A1 (fr) 2014-01-03 2015-07-09 Lenzing Aktiengesellschaft Fibre cellulosique

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992014871A1 (fr) * 1991-02-15 1992-09-03 Courtaulds Plc Procede de production de fibres
WO1995024524A1 (fr) * 1994-03-09 1995-09-14 Courtaulds Fibres (Holdings) Limited Traitement de fibres
WO1995028516A1 (fr) * 1994-04-15 1995-10-26 Courtaulds Fibres (Holdings) Limited Traitement pour fibres
WO1997023668A1 (fr) * 1995-12-21 1997-07-03 Courtaulds Fibres (Holdings) Limited Fabrication d'articles cellulosiques

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992014871A1 (fr) * 1991-02-15 1992-09-03 Courtaulds Plc Procede de production de fibres
WO1995024524A1 (fr) * 1994-03-09 1995-09-14 Courtaulds Fibres (Holdings) Limited Traitement de fibres
WO1995028516A1 (fr) * 1994-04-15 1995-10-26 Courtaulds Fibres (Holdings) Limited Traitement pour fibres
WO1997023668A1 (fr) * 1995-12-21 1997-07-03 Courtaulds Fibres (Holdings) Limited Fabrication d'articles cellulosiques

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000018991A1 (fr) * 1998-09-29 2000-04-06 Lenzing Aktiengesellschaft Procede de production de fibres cellulosiques
US6645409B2 (en) 1998-09-29 2003-11-11 Lenzing Aktiengesellschaft Process for the production of cellulosic fibres
WO2015101543A1 (fr) 2014-01-03 2015-07-09 Lenzing Aktiengesellschaft Fibre cellulosique
US10883196B2 (en) 2014-01-03 2021-01-05 Lenzing Aktiengesellschaft Cellulose fiber

Also Published As

Publication number Publication date
AU3549597A (en) 1998-02-09
GB9614679D0 (en) 1996-09-04

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