EP1224343B1 - Procede de production de corps faconnes en cellulose - Google Patents

Procede de production de corps faconnes en cellulose Download PDF

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Publication number
EP1224343B1
EP1224343B1 EP00978960A EP00978960A EP1224343B1 EP 1224343 B1 EP1224343 B1 EP 1224343B1 EP 00978960 A EP00978960 A EP 00978960A EP 00978960 A EP00978960 A EP 00978960A EP 1224343 B1 EP1224343 B1 EP 1224343B1
Authority
EP
European Patent Office
Prior art keywords
cellulose
bleached
group content
tcf
ecf
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
EP00978960A
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German (de)
English (en)
Other versions
EP1224343A1 (fr
Inventor
Ralf-Uwe Bauer
Uwe Kind
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.)
LL Plant Engineering AG
Original Assignee
ZiAG Plant Engineering GmbH
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Filing date
Publication date
Application filed by ZiAG Plant Engineering GmbH filed Critical ZiAG Plant Engineering GmbH
Publication of EP1224343A1 publication Critical patent/EP1224343A1/fr
Application granted granted Critical
Publication of EP1224343B1 publication Critical patent/EP1224343B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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

  • the invention relates to a process for the production of shaped cellulose articles, such as fibers, filaments or films, from TCF or ECF bleached pulp, which comprises dissolving the bleached pulp in an aqueous tertiary amine oxide to form a moldable cellulose solution, the cellulose solution deformed and by Coagulation of the deformed solution forms the molding.
  • the invention further relates to the use of a TCF- or ECF-bleached pulp for the production of cellulose moldings.
  • TCF-bleached pulp in the Lyocell process leads to moldings with a higher degree of whiteness than the use of an ECF-bleached pulp. Both pulps are provided with similarly high output whiteness by 90% and high purities, particularly with respect to lignin content. It therefore appeared questionable whether the TCF pulp generally gives better whiteness of the cellulosic shaped bodies produced from this pulp than does an ECF pulp.
  • the object of the present invention is to provide a process for the production of cellulosic moldings with reduced cellulose degradation starting from TCF- or ECF-bleached pulp.
  • the reduction of cellulose degradation should be achieved without any special measures in Lyocellmaschine substantially. Further advantages of the invention will become apparent from the following description.
  • Pulp and fiber whitenesses of various pulp samples were determined which were either ECF or TCF bleached.
  • the determination of the whiteness of the pulp was carried out according to DIN 53145, part 2.
  • the determination of the whiteness of the fiber was carried out according to the method described in WO 97/23666, page 6.
  • the average degree of polymerization of the pulps by the cuoxam method was about 550.
  • the whitenesses measured on the pulp and on the fiber are summarized in Table 1.
  • Table 1 Whiteness / pulp source production method Initial grade of pulp Whiteness of the braided fiber Cellunier F Fa. Rayonier USA ECF (ElementaryChiller-Free) 89.9 55.0 Temfilm Example 1 Fa.
  • one to reduce of cellulose degradation in the process employs a TCF bleached pulp having a carboxyl group content in the range of 1 to 35 ⁇ mol / g or an ECF bleached pulp having a carboxyl group content in the range of 1 to 50 ⁇ mol / g. It has been found that the lower the carboxyl group content of the pulp used, the less is the cellulose degradation in the course of the production and processing of the extrusion solution. In order to achieve a low degradation of the cellulose and the amine oxide in the lyocell process, TCF- and ECF-bleached pulps whose carboxyl group content lies in the stated ranges are used in the spinning solution production. Pulps with the stated carboxyl group contents can be produced by different pulp manufacturers. As a result of the reduced degradation of the dope components, fewer coloring constituents are also formed, so that, secondarily, the whiteness of the shaped bodies formed is also improved.
  • a TCF-bleached pulp having a carboxyl group content in the range of 15 to 30 ⁇ mol / g or an ECF-bleached pulp having an arboxyl group content in the range of 25 to 35 ⁇ mol / g is used.
  • the determination of the carboxyl group content of the cellulose to be used can be carried out according to Döring, verg1. K. Goetze, man-made fibers by the viscose process, 2nd volume 3rd ed., 1997, p. 1079.
  • NMMO-MH N-methylmorpholine N-oxide monohydrate
  • the amount of the organic compound may be in the range of 0.01 to 0.5 mass% based on the amount of the solvent. Suitable organic compounds are known from EP-A-0 047 929. A commonly used compound is isopropyl gallate.
  • the cellulose degradation is limited to a proportion in the range of 3 to 20% by mass, based on the pulp used.
  • the degraded cellulose content is in the range of 8 to 15 mass%.
  • the invention further relates to the use of a TCF-bleached pulp or an ECF-bleached pulp having a carboxyl group content in the range of 1 to 35 .mu.mol / g and 1 to 50 .mu.mol / g to form a cellulose solution in a tertiary amine oxide-containing solvent for the Production of Moldings by the Lyocell Process.
  • the use of these pulps not only reduces the degradation in the course of the lyocell process, but also increases the whiteness of the shaped bodies formed.
  • Long fiber sulfite pulp was bleached by alkaline peroxide-enhanced oxygen extraction, then ozone and peroxide in a known manner.
  • the bleaching methods are described, for example, in RP Singh, The Bleaching of Pulp, TAPPI Press, Atlanta, USA. In this case, three different carboxyl group contents were set (Examples 1 to 3). Three more samples of the pulp were bleached with hypochlorite. On the pulps, the degree of polymerization and the initial degree of whiteness were determined by the methods given above, including the carboxyl and carbonyl group content of the pulp. From the bleached pulps spinning solutions with 13% cellulose, 10.5% water and 76.5% NMMO were prepared in a known manner.
  • the solutions were spun at 95 ° C. by a dry-wet method with a nozzle of 65 ⁇ m hole diameter. On the obtained fibers, the degree of polymerization and the degree of whiteness were determined. The degree of polymerization was determined by the cuoxam method, the degree of fiber whiteness by the method given above. The determined numerical values are given in Table 2.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Paper (AREA)

Claims (8)

  1. Procédé pour la fabrication de matériaux moulés en cellulose, comme par exemple la confection de fibres, de filaments ou de feuilles, en cellulose blanchie TCF (totalement sans chlore) ou ECF (sans chlore élémentaire), par lequel la cellulose blanchie sera dissoute dans un amine-oxyde tertiaire aqueux, formant une solution cellulosique apte au moulage et par la coagulation de cette solution formée, sera transformée en un matériau moulé, caractérisé par le fait que pour réduire la dégradation de la cellulose dans ce procédé, une cellulose blanchie TCF avec un contenu de groupe carboxyle dans la gamme de 1 à 35 µmol / g ou une cellulose blanchie ECF avec un contenu de groupe carboxyle dans la gamme de 1 à 50 µmol/g sera utilisée.
  2. Procédé selon la revendication 1, caractérisé par l'utilisation d'une cellulose blanchie TCF avec un contenu de groupe carboxyle dans la gamme de 15 à 30 µmol / g dans la phase de dissolution.
  3. Procédé selon la revendication 1, caractérisé par l'utilisation d'une cellulose blanchie ECF avec un contenu de groupe carboxyle dans la gamme de 25 à 35 µmol / g dans la phase de dissolution.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé par le fait que N-oxyde de N-méthylmorpholine est utilisé à la place de l'amine-oxyde tertiaire.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé par la formation d'une solution cellulosique avec un contenu d'alcalis ou de composés organiques, ces derniers ayant au moins 4 atomes de carbone, au moins deux liaisons doubles conjuguées et au moins deux substituants -X-H, dont X désigne O ou NR, et R désigne l'hydrogène ou un groupe alkyle, ayant 1 à 4 atomes de carbone.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé par le fait que la dégradation de la cellulose est limitée à une fraction dans la gamme de 3 à 20%, par rapport à la cellulose utilisée.
  7. Utilisation d'une cellulose blanchie TCF, ayant un contenu de groupe carboxyle dans la gamme de 1 à 35 µmol / g, afin d'obtenir une solution cellulosique dans un solvant contenant un amine-oxyde tertiaire pour la confection de matériaux moulés selon le procédé de Lyocell.
  8. Utilisation d'une cellulose blanchie ECF, ayant un contenu de groupe carboxyle dans la gamme de 1 à 50 µmol / g, afin d'obtenir une solution cellulosique dans un solvant contenant un amine-oxyde tertiaire pour la confection de matériaux moulés selon le procédé de Lyocell.
EP00978960A 1999-10-07 2000-09-29 Procede de production de corps faconnes en cellulose Expired - Lifetime EP1224343B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19948401 1999-10-07
DE19948401A DE19948401C1 (de) 1999-10-07 1999-10-07 Verfahren zur Herstellung von Cellulose-Formkörpern
PCT/DE2000/003408 WO2001025515A1 (fr) 1999-10-07 2000-09-29 Procede de production de corps façonnes en cellulose

Publications (2)

Publication Number Publication Date
EP1224343A1 EP1224343A1 (fr) 2002-07-24
EP1224343B1 true EP1224343B1 (fr) 2006-02-01

Family

ID=7924866

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00978960A Expired - Lifetime EP1224343B1 (fr) 1999-10-07 2000-09-29 Procede de production de corps faconnes en cellulose

Country Status (15)

Country Link
US (1) US7175792B1 (fr)
EP (1) EP1224343B1 (fr)
KR (1) KR100661454B1 (fr)
CN (1) CN1180141C (fr)
AT (1) ATE317027T1 (fr)
AU (1) AU1645601A (fr)
BR (1) BR0014529B1 (fr)
CA (1) CA2385227A1 (fr)
DE (2) DE19948401C1 (fr)
EA (1) EA200200382A1 (fr)
MY (1) MY129236A (fr)
NO (1) NO20021588L (fr)
TW (1) TW522178B (fr)
WO (1) WO2001025515A1 (fr)
ZA (1) ZA200203556B (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100359050C (zh) * 2004-11-16 2008-01-02 唐山三友集团化纤有限公司 高白强力细旦粘胶短纤维及其生产工艺
CN101649061B (zh) * 2009-07-13 2012-06-27 潍坊恒联玻璃纸有限公司 一种航空仪表盘专用纤维素膜的制备方法
KR102313567B1 (ko) * 2014-03-11 2021-10-19 스마트폴리머 게엠베하 직접 용해 방법에 따라 제조된 난연성 셀룰로스 성형체

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3034685C2 (de) * 1980-09-13 1984-07-05 Akzo Gmbh, 5600 Wuppertal Cellulose-Form- und Spinnmasse mit geringen Anteilen an niedermolekularen Abbauprodukten
US4480089A (en) * 1983-06-14 1984-10-30 Purdue Research Foundation Modified cellulose products by bleaching
DD218104B5 (de) * 1983-10-17 1996-06-13 Thueringisches Inst Textil Verfahren zur Herstellung thermisch stabiler Cellulose-Aminoxidloesungen
DE4308524C1 (de) * 1992-06-16 1994-09-22 Thueringisches Inst Textil Verfahren zur Herstellung von Cellulosefasern und -filamenten nach dem Trocken-Naßextrusionsverfahren
DE4219658C3 (de) * 1992-06-16 2001-06-13 Ostthueringische Materialpruef Verfahren zur Herstellung von Cellulosefasern -filamenten und -folien nach dem Trocken-Naßextrusionsverfahren
DE4441468C2 (de) * 1994-11-22 2000-02-10 Ostthueringische Materialpruef Verfahren zur Herstellung einer homogenen Lösung von Cellulose in wasserhaltigem N-Methylmorpholin-N-oxid
AT402827B (de) * 1995-12-22 1997-09-25 Chemiefaser Lenzing Ag Celluloseformkörper und verfahren zu seiner herstellung
TR200102472T2 (tr) * 1999-02-24 2002-03-21 Sca Hygiene Products Gmbh Oksidize selloz i‡erikli elyaf materyaller ve bunlardan imal edilen rnler.
US6524348B1 (en) * 1999-03-19 2003-02-25 Weyerhaeuser Company Method of making carboxylated cellulose fibers and products of the method
DE19953591A1 (de) * 1999-11-08 2001-05-17 Sca Hygiene Prod Gmbh Metallvernetzbare oxidierte cellulosehaltige Faserstoffe und daraus hergestellte Produkte
US20030051834A1 (en) * 2001-06-06 2003-03-20 Weerawarna S. Ananda Method for preparation of stabilized carboxylated cellulose
US7052540B2 (en) * 2004-03-11 2006-05-30 Eastman Chemical Company Aqueous dispersions of carboxylated cellulose esters, and methods of making them

Also Published As

Publication number Publication date
NO20021588D0 (no) 2002-04-04
NO20021588L (no) 2002-04-04
ZA200203556B (en) 2003-02-26
TW522178B (en) 2003-03-01
CN1377428A (zh) 2002-10-30
MY129236A (en) 2007-03-30
WO2001025515A1 (fr) 2001-04-12
KR100661454B1 (ko) 2006-12-27
CN1180141C (zh) 2004-12-15
DE50012169D1 (de) 2006-04-13
ATE317027T1 (de) 2006-02-15
US7175792B1 (en) 2007-02-13
BR0014529A (pt) 2002-08-27
DE19948401C1 (de) 2001-05-03
EA200200382A1 (ru) 2002-10-31
AU1645601A (en) 2001-05-10
CA2385227A1 (fr) 2001-04-12
BR0014529B1 (pt) 2011-08-09
EP1224343A1 (fr) 2002-07-24
KR20020037378A (ko) 2002-05-18

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