EP1129241B1 - Procede de production de fibres cellulosiques - Google Patents
Procede de production de fibres cellulosiques Download PDFInfo
- Publication number
- EP1129241B1 EP1129241B1 EP99947074A EP99947074A EP1129241B1 EP 1129241 B1 EP1129241 B1 EP 1129241B1 EP 99947074 A EP99947074 A EP 99947074A EP 99947074 A EP99947074 A EP 99947074A EP 1129241 B1 EP1129241 B1 EP 1129241B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- wash
- baths
- bath
- fibers
- washing
- 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
Links
- 239000000835 fiber Substances 0.000 title claims description 38
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000005406 washing Methods 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229920002678 cellulose Polymers 0.000 claims description 7
- 239000001913 cellulose Substances 0.000 claims description 7
- 150000003512 tertiary amines Chemical class 0.000 claims description 5
- 239000006172 buffering agent Substances 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims 1
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000007788 liquid Substances 0.000 description 13
- 150000001412 amines Chemical class 0.000 description 8
- 229920000433 Lyocell Polymers 0.000 description 6
- 239000004745 nonwoven fabric Substances 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 239000007844 bleaching agent Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 206010061592 cardiac fibrillation Diseases 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000002600 fibrillogenic effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IVNPXOUPZCTJAK-UHFFFAOYSA-N 4-methylmorpholin-4-ium;hydroxide Chemical compound O.CN1CCOCC1 IVNPXOUPZCTJAK-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Images
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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
-
- 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 cellulosic fibers from solutions of Cellulose in an aqueous tertiary amine oxide.
- a mixture, in particular, as the organic solvent from a tertiary amine oxide and water excellent for the production of Lyocell fibers or other moldings is excellent for the production of Lyocell fibers or other moldings.
- the amine oxide used is predominantly N-methylmorpholine-N-oxide (NMMO) used.
- NMMO N-methylmorpholine-N-oxide
- Other suitable amine oxides are in the EP-A 0 553 070.
- Process for the production of cellulosic moldings from a Solutions of the cellulose in a mixture of NMMO and water are e.g. in the US PS 4,246,221 or disclosed in PCT-WO 93/19230. The cellulose solution is made extruded into a spinneret, stretched in an air gap and out of solution in one aqueous precipitation bath precipitated.
- amine oxide process This process is hereinafter referred to as the "amine oxide process” or “Lyocellclar”, with the abbreviation "NMMO” in the following all tertiary amine oxides are meant that can dissolve cellulose.
- NMMO tertiary amine oxides are meant that can dissolve cellulose.
- PCT-WO 92/14871 describes a method for washing after Fibers produced by amine oxide processes.
- the fibers are cut into staple fibers only in a later process stage.
- PCT-WO 92/14871 points out that it can be derived from the Viscose process for the production of cellulosic fibers is known to be one of the washing stages is designed as a bleaching stage in which an alkaline pH prevails. However, it is known in the amine oxide process that all washing liquids for the recovery of NMMO are recycled. It is also in this context from the PCT-WO 92/14871 known that the washing baths are connected to each other and fresh washing liquid added in the last washing bath and countercurrent to Direction of transport of the fiber cable is guided to the first wash bath. Because the entry Additional chemicals in larger quantities in this circuit is undesirable Amine oxide process does not implement a bleaching stage in the washing liquid circuit become. It is only possible to use a bleach bath independently of each other To provide related wash baths. So if in the following of "Wash baths" is meant, such an independent bleach bath is not meant.
- Another problem with washing the fibers made by the amine oxide process is that adhering NMMO must be completely removed from the fiber.
- the object of the present invention is to provide a method, in which the NMMO is washed out of the fiber with as little effort as possible can be.
- This task is accomplished by a process for producing cellulosic fibers from solutions the cellulose dissolved in an aqueous tertiary amine oxide, the extruded fibers passed over a precipitation bath and cut and the cut fibers in the form of a Fleece passed over several wash baths and then dried, which Wash baths communicate with each other and being fresh wash liquid in the last Wash bath is given up and countercurrent to the direction of transport of the nonwoven is led to the first washing bath, and which method is characterized in that the pH of each of the wash baths is maintained above 8.5. For the purposes of In the present invention, a pH of more than 8.5 is referred to as "alkaline pH" designated.
- the invention relates to so-called "washing sections" of several together related washes. According to the pH of the Wash liquid of each of the related wash baths higher than 8.5 being held. Baths that are not connected to the washing baths and therefore not can be fed with the same washing liquid, e.g. separate treatment or Bleach baths are not included in the present invention.
- the adjustment of the pH in the wash baths can be done by the Basic buffering substances are added.
- the addition of Sodium hydroxide solution preferred.
- the necessary amount of caustic soda, which of Process parameters such as depends on the pH value of the fleece or the moisture in the fleece, can easily be determined for the person skilled in the art on the basis of the respective circumstances. In the amount added is regulated in a simple manner on the basis of the pH of the wash baths.
- the sodium hydroxide solution can only be in one of the wash baths or in several places be added to the laundry. It turns out that the addition of alkali to the wash baths no negative influence on the subsequent process steps such as cleaning the Has wash baths and solvent recovery.
- the temperature of the wash water is preferably about 20 ° C to 90 ° C.
- wash the fleece this can be done through the washing baths filled with washing liquid be performed.
- the wash baths can also be designed such that Washing liquid is sprayed onto the fleece.
- the total liquor ratio of the washing liquid to the nonwoven fabric is advantageously 1.5: 1 to 40: 1.
- 1 schematically denotes a method for washing a nonwoven fabric freshly spun cut lyocell fibers.
- the nonwoven (10) is e.g. on a sieve belt (not shown) through the different washing baths (there are 5 washing baths in FIG. 1).
- the washing liquid flows down back into the respective container.
- Fresh wash water 13 becomes the last bath (Container 5) fed.
- the wash water circulates in the respective baths, taking the rate the circulation within a bath may be higher than the rate of supply of the fresh one Wash water in the last wash bath. Excess wash water becomes countercurrent
- the direction of transport of the nonwoven fabric is fed to the upstream wash bath.
- nonwoven fabric is rolled using pairs of rollers, e.g. the pair of rollers (11, 12) pressed.
- the washed nonwoven becomes further post-treatment stages supplied or dried.
- the wash water of the first becomes the precipitation bath and the cleaning and recovery of NMMO fed.
- a nonwoven fabric was made from freshly spun Lyocell fibers in five wash baths using slightly alkaline water as Washing liquid without additional measures according to the general given above Procedure washed.
- the fleece was pressed to a water content of approximately 200%. After the last wash bath, the fleece was brought to a water content of approx. 100% squeezed and then dried.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
- Paper (AREA)
- Nonwoven Fabrics (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Claims (6)
- Procédé de production de fibres cellulosiques, à partir de solutions de la cellulose dans un amynoxyde tertiaire, aqueux, les fibres extrudées étant guidées à travers un bain de précipitation et découpées, et les fibres découpées, ayant la forme d'un matelas, étant guidées à travers une pluralité de bains de lavage et étant ensuite séchées, lesdits bains de lavage étant reliés ensemble et du liquide de lavage neuf étant amené au dernier bain de lavage et guidé à contre-courant par rapport à la direction de transport du matelas de fibres, jusqu'au premier bain de lavage, caractérisé en ce que la valeur de pH de chacun des bains de lavage est maintenue à une valeur supérieure à 8,5.
- Procédé selon la revendication 1, caractérisé en ce que la valeur de pH de chacun des bains de lavage est maintenue entre 9 et 11
- Procédé selon l'une des revendications 1 ou 2, caractérisé en ce que le réglage de la valeur de pH dans les bains de lavage se fait par addition de substances à effet tampon et basique.
- Procédé la revendication 3, caractérisé en ce qu'une lessive de soude est ajoutée à au moins l'un des bains de lavage.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que le matelas de fibres, après avoir quitté un bain de lavage, est exprimé avant d'entrer au bain de lavage suivant.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que la température du liquide de lavage est dans la plage de 20°C à 90°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT99947074T ATE258238T1 (de) | 1998-09-29 | 1999-09-28 | Verfahren zur herstellung cellulosischer fasern |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT161498 | 1998-09-29 | ||
| AT0161498A AT406588B (de) | 1998-09-29 | 1998-09-29 | Verfahren zur herstellung cellulosischer fasern |
| PCT/AT1999/000229 WO2000018991A1 (fr) | 1998-09-29 | 1999-09-28 | Procede de production de fibres cellulosiques |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1129241A1 EP1129241A1 (fr) | 2001-09-05 |
| EP1129241B1 true EP1129241B1 (fr) | 2004-01-21 |
Family
ID=3517237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP99947074A Expired - Lifetime EP1129241B1 (fr) | 1998-09-29 | 1999-09-28 | Procede de production de fibres cellulosiques |
Country Status (11)
| Country | Link |
|---|---|
| US (1) | US6645409B2 (fr) |
| EP (1) | EP1129241B1 (fr) |
| KR (1) | KR20010075371A (fr) |
| CN (1) | CN1143011C (fr) |
| AT (1) | AT406588B (fr) |
| AU (1) | AU6066899A (fr) |
| BR (1) | BR9914108A (fr) |
| DE (1) | DE59908380D1 (fr) |
| ID (1) | ID28499A (fr) |
| TW (1) | TW577941B (fr) |
| WO (1) | WO2000018991A1 (fr) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT410319B (de) * | 2001-07-25 | 2003-03-25 | Chemiefaser Lenzing Ag | Celluloseschwamm und verfahren zu dessen herstellung |
| JP2005535966A (ja) * | 2002-08-09 | 2005-11-24 | インテル・コーポレーション | アライメントまたはブロードキャスト命令を含むマルチメディア・コプロセッサの制御メカニズム |
| DE102004007617B4 (de) * | 2004-02-17 | 2007-02-08 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zur Herstellung eines Vliesstoffes, Vliesstoff und dessen Verwendung |
| US7693817B2 (en) * | 2005-06-29 | 2010-04-06 | Microsoft Corporation | Sensing, storing, indexing, and retrieving data leveraging measures of user activity, attention, and interest |
| KR100769973B1 (ko) * | 2006-12-28 | 2007-10-25 | 주식회사 효성 | 수세 공정 특성을 가진 산업용 셀룰로오스 멀티필라멘트의제조 방법 수세 공정 |
| AT504649B1 (de) * | 2007-07-11 | 2008-07-15 | Chemiefaser Lenzing Ag | Vorrichtung und verfahren zur behandlung einer fasermasse |
| AT505904B1 (de) * | 2007-09-21 | 2009-05-15 | Chemiefaser Lenzing Ag | Cellulosesuspension und verfahren zu deren herstellung |
| AT507051B1 (de) | 2008-06-27 | 2015-05-15 | Chemiefaser Lenzing Ag | Cellulosefaser und verfahren zu ihrer herstellung |
| AT519489B1 (de) | 2016-10-21 | 2021-11-15 | Chemiefaser Lenzing Ag | Verfahren und Vorrichtung zum Herstellen von Vliesen auf Cellulosebasis, die direkt aus Lyocell-Spinnlösung gebildet werden |
| KR101972271B1 (ko) * | 2018-09-05 | 2019-04-24 | 박한수 | 인조 모발용 원사를 제조하는 방법 및 장치 |
| EP3828320A1 (fr) | 2019-11-26 | 2021-06-02 | Lenzing Aktiengesellschaft | Lavage à contre-courant |
| CN112593305A (zh) * | 2020-12-04 | 2021-04-02 | 四川辉腾科技股份有限公司 | 一种芳纶ⅲ纤维纺丝水洗装置及其使用方法 |
| KR20250109158A (ko) * | 2024-01-09 | 2025-07-16 | 코오롱인더스트리 주식회사 | 라이오셀 소재, 흡연 물품용 필터, 흡연 물품 및 이들의 제조방법 |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4246221A (en) | 1979-03-02 | 1981-01-20 | Akzona Incorporated | Process for shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent |
| DE3536537A1 (de) | 1985-10-12 | 1987-04-16 | Wolff Walsrode Ag | Verfahren zur reinigung von produkten aus regenerierter cellulose |
| GB9103297D0 (en) | 1991-02-15 | 1991-04-03 | Courtaulds Plc | Fibre production method |
| AT396930B (de) | 1992-01-23 | 1993-12-27 | Chemiefaser Lenzing Ag | Aminoxide |
| ATA53792A (de) | 1992-03-17 | 1995-02-15 | Chemiefaser Lenzing Ag | Verfahren zur herstellung cellulosischer formkörper, vorrichtung zur durchführung des verfahrens sowie verwendung einer spinnvorrichtung |
| US5585052A (en) * | 1994-08-10 | 1996-12-17 | The Dow Chemical Company | Process for the preparation of polybenzazole staple fiber |
| AT402741B (de) | 1995-10-13 | 1997-08-25 | Chemiefaser Lenzing Ag | Verfahren zur herstellung cellulosischer fasern |
| DE19600572B4 (de) * | 1996-01-09 | 2005-03-10 | Fraunhofer Ges Forschung | Verfahren zur Herstellung von Cellulosefasern und die mit diesem Verfahren hergestellten Fasern |
| GB9611252D0 (en) * | 1996-05-30 | 1996-07-31 | Courtaulds Fibres Holdings Ltd | Fibre manufacture |
| GB9614679D0 (en) * | 1996-07-12 | 1996-09-04 | Courtaulds Fibres Holdings Ltd | Manufacture of fibre |
| GB9615431D0 (en) * | 1996-07-23 | 1996-09-04 | Courtaulds Fibres Holdings Ltd | Fibre manufacture |
-
1998
- 1998-09-29 AT AT0161498A patent/AT406588B/de not_active IP Right Cessation
-
1999
- 1999-09-28 BR BR9914108-6A patent/BR9914108A/pt not_active Application Discontinuation
- 1999-09-28 AU AU60668/99A patent/AU6066899A/en not_active Abandoned
- 1999-09-28 DE DE59908380T patent/DE59908380D1/de not_active Expired - Fee Related
- 1999-09-28 WO PCT/AT1999/000229 patent/WO2000018991A1/fr not_active Ceased
- 1999-09-28 KR KR1020017003839A patent/KR20010075371A/ko not_active Abandoned
- 1999-09-28 EP EP99947074A patent/EP1129241B1/fr not_active Expired - Lifetime
- 1999-09-28 CN CNB998114847A patent/CN1143011C/zh not_active Expired - Lifetime
- 1999-09-28 ID IDW20010718A patent/ID28499A/id unknown
- 1999-10-01 TW TW088116969A patent/TW577941B/zh not_active IP Right Cessation
-
2001
- 2001-03-21 US US09/814,152 patent/US6645409B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| US6645409B2 (en) | 2003-11-11 |
| ATA161498A (de) | 1999-11-15 |
| KR20010075371A (ko) | 2001-08-09 |
| BR9914108A (pt) | 2001-06-12 |
| TW577941B (en) | 2004-03-01 |
| ID28499A (id) | 2001-05-31 |
| US20020008331A1 (en) | 2002-01-24 |
| AT406588B (de) | 2000-06-26 |
| EP1129241A1 (fr) | 2001-09-05 |
| AU6066899A (en) | 2000-04-17 |
| CN1320176A (zh) | 2001-10-31 |
| WO2000018991A1 (fr) | 2000-04-06 |
| CN1143011C (zh) | 2004-03-24 |
| DE59908380D1 (de) | 2004-02-26 |
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