DE10016307C2 - Process for the production and processing of a cellulose solution - Google Patents

Process for the production and processing of a cellulose solution

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Publication number
DE10016307C2
DE10016307C2 DE10016307A DE10016307A DE10016307C2 DE 10016307 C2 DE10016307 C2 DE 10016307C2 DE 10016307 A DE10016307 A DE 10016307A DE 10016307 A DE10016307 A DE 10016307A DE 10016307 C2 DE10016307 C2 DE 10016307C2
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DE
Germany
Prior art keywords
characterized
method according
net
cellulose
nmmo
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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 - Fee Related
Application number
DE10016307A
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German (de)
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DE10016307A1 (en
Inventor
Bernd Riedel
Markus Eilers
Eberhard Taeger
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Thuringisches Institut fur Textil und Kunststoff Forschung EV
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Thuringisches Institut fur Textil und Kunststoff Forschung EV
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Application filed by Thuringisches Institut fur Textil und Kunststoff Forschung EV filed Critical Thuringisches Institut fur Textil und Kunststoff Forschung EV
Priority to DE10016307A priority Critical patent/DE10016307C2/en
Publication of DE10016307A1 publication Critical patent/DE10016307A1/en
Application granted granted Critical
Publication of DE10016307C2 publication Critical patent/DE10016307C2/en
Application status is Expired - Fee Related legal-status Critical
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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • C08B1/003Preparation of cellulose solutions, i.e. dopes, with different possible solvents, e.g. ionic liquids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/02Cellulose; Modified cellulose
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof

Abstract

Process for the production and processing of a cellulose solution which is obtained by dissolving the cellulose in a tertiary amine oxide piperidonate, preferably NMMO piperidonate. The cellulose thus dissolved is then deformed, coagulated and the solvent removed. DOLLAR A The tertiary amine oxide is N-methylmorpholine-N-oxide (NMMO). The NMMO piperidonates are produced from aqueous NMMO and piperidone by distilling off water. The cellulose solution can preferably be produced at temperatures between 60 and 130 ° C.

Description

The invention relates to a simplified method for manufacturing provision and processing of a cellulose solution, which by Dissolving the cellulose in a tertiary amine oxide piperidonate, preferably NMMO piperidonate.

State of the art

The advantages of using renewable raw materials for the product tion of plastics, fibers and foils are sufficient known.

Cellulose, which comes from plants, has been used for over 100 years is obtained, the production of textile moldings, for. B. Fibers, filaments or foils. Many decades dominated thereby processes in which the cellulose changes chemically had to be replaced by appropriate ones before it went into solution Molds are extruded and chemically converted to become. The most used method was that Viscose process in which a variety of environmentally harmful Chemicals, by-products and waste products as well as resource-intensive Process design play a role. It was a long time on the Search for suitable direct solvents for cellulose. On such a system that has also been used industrially, is an aqueous solution of a tertiary amine oxide, e.g. B. N- Methylmorpholine-N-oxide, hereinafter NMMO, (e.g. US 4324593, US 4290815, DD 218 104). The spared by such procedures fibers got the generic term LYOCELL. A decision The disadvantage of this system is the relatively high viscosity act of the spinning masses, the a transport within a Process only under defined, technically not easy Conditions allowed. The solving process also requires here an exact temperature control that is difficult to implement in order to  set the residual water content that determines the dissolving process len (EP 0668941, EP 0662204).

DE 28 48 471 was used for the system N-oxide / cellulose Viscosity reduction suggested an aprotic orga liquid with a dipole moment of more than 3.5 Add Debye. The disadvantage of this is that this aproti connections one for the technically feasible Solving process too high volatility.

US 5362867 and US 5929228 have also been changed Release systems presented. In the first one you use alongside the well-known N-methylmorpholine-N-oxide (NMMO) a mixture from recovered caprolactam from polyamide production. The Dependence on upstream production and associated with it possible inhomogeneities due to possible contamination have a detrimental effect on the further process steps out.

In US 5929228 the way is followed, along with the NMMO Proportions of a mixture of N-methylol-caprolactam and tetra- Add methyl ammonium chloride to the solvent system. The technical, occupational safety and ecological control Such a system is complicated due to the complexity Properties, especially of tetra-methylammonium chloride, very complex.

The use of unsubstituted or with nitrogen Alkyl groups monosubstituted carboxamides as co- Solvent is described in WO 99/60026, the Alkyl groups must not have more than 4 carbon atoms. This Substances tend to form in connection with NMMNO well crystallizing complexes that when cooling the manufactured cellulose solutions to a disadvantageous one freeze the solution combined with a partial gel tion, lead. It is particularly disadvantageous that when thawing the frozen cellulose solution these formed when freezing  Gel structures only through the action of shear forces and Heat in a solution suitable for further processing state must be reset.

The aim of the invention is to overcome these disadvantages of cellulose oil to eliminate solutions.

It was surprisingly found that Cellu loose in tertiary amine oxide piperidonates, preferably NMMO Piperidonaten, dissolves and from these advantageous solutions by deformation, coagulation and subsequent removal let the solvent be molded. open This advantage is due to the fact that the Piperido nate a cheaper internal structure of the cellulose solution causes.

Compared to the known solutions based on NMMO, the Solutions do not crystallize, even when they cool down and stand out beyond that as a result of the comparison larger molecular volume of the piperidonates and thus associated greater distance between the solvated Cellulose molecules, due to a lower structural viscosity out.

Piperidone is an amphiprotic cyclic solvent with 5 CH 2 groups arranged in a ring. Piperidone forms complexes with different compositions via hydrogen bonds with tertiary amine oxides, which, regardless of whether the piperidone is present in the complex as lactam or in its tautomeric form as lactim, are referred to as piperidones.

Water-based NMMO with piperidone is used to manufacture them mixed and with the addition of heat from the solution in the Vacuum the water through an intermediate column deducted. A syrup-like melt forms when it cools down  from which with great delay at lower temperatures ever according to the composition of NMMO piperidonate or NMMO piperidonate Crystallize mixtures.

Such piperidonates or Piperidonate mixtures suitable, the content of piperidone 60 wt .-% does not exceed.

The cellulose can be dissolved by

  • a) piperidonates with a defined composition made from aqueous NMMO and piperidone by distillation lation of the water and subsequent cleaning by Um crystallization,
  • b) Piperidonate mixtures made from aqueous NMMO and Piperidone by distilling off the water until it reaches Errei a sufficient quality of soldering for cellulose.

The piperidonates or the piperidonate mixtures can be diluted contain agents.

Any dilutions still present in the solutions Aprotic organic solvents such as z. B. dimethyl sulfoxide, dimethylformamide, N-methylpyrrolidone and dimethylacetamide, or amphiprotic solvents such as z. B. the piperidone and / or water and / or lower alcohol le, or the tertiary amine oxide itself.

Due to the higher boiling point of the Piperi by more than 150 ° C dons versus water can be the composition of piperido technically safe.

Cellulosic materials that are used in the process are preferred chemical fiber pulp, cotton linters, softwood sulfite, softwood sulfate and / or hardwood pulps from the Sulfite or sulfate digestion processes different Polymerization. The pulp can be one or in Form of mixtures of different degrees of polymerization used  become. Pulps are also treated with Druckex explosion technology, electron beams or enzymes can be used.

To better illustrate the invention, the following is intended in a particularly advantageous embodiment according to (b) how to make a cellulose solution Fibers deformed, the cellulose by the action of a Koagu regeneration medium and the solvent was selected and is recovered. As a tertiary amine oxide NMMO used.

The starting point is pulp, as previously described mentioned part. The pulp becomes a preparation acted for better accessibility to the Secure solvent or its precursor. The Mechanical pulp with the help of shredders or mills be crushed and added in this form. A another variant of the pretreatment of the pulp is that this in an aqueous solution due to intensive shearing is crushed and the resulting pulp closing by dewatering to a defined humidity is set before it is mixed in with the solvent system Touch comes. The pulp can be in the phase of watery treatment with the outcrop and the accessible cellulose-promoting chemicals (alkalis, Acids, surfactants) or enzymes are treated.

The first stage is through continuous or discount thorough mixing of the components water, NMMO, piperidone and cellulose made a mash. The cellulose concents mash is usually between 4 and 23% (Dimensions). In addition to cellulose, other soluble or insoluble, organic or inorganic compounds, such as for example pigments, dyes, ion exchangers, soot, Stabilizers, ceramic powders, are added.  

The resulting mash is placed in an evaporator Apply a vacuum with appropriate temperature control sheared. It is irrelevant whether the apparatus after the Principle of a thin layer or other wave apparatus is designed. According to the invention at a temperature between 60-140 ° C, preferably 80-130 ° C, and under pressure from 30-150 mbar.

The cellulose concentration in the solution is between 5 and 25%.

For further additional thermal stabilization and Suppression of chain breakdown of cellulose, especially at higher temperatures, stabilizers, such as. B. Gallic acid propyl ester, preferably up to a content of Add 1% based on cellulose to the spinning solution. The Spinning solution obtained is transported over a temperature line pressed with the help of a pump over a filter element and then directly or through a molding tool passed an air gap into a precipitation bath. The subsequent one Wash the adhering solvent NMMO / piperidone shoots with water, which is the concurrent principle tration of the spinning bath controls. A common one for cellulosi cal fibers / filaments known post-treatment procedure follows [finishing, drying, if necessary (in between) Bleaching and cutting].

The precipitation bath, consisting of NMMO, piperidone and as a direct one Coagulation medium water and / or low molecular weight alcohols, is given for reprocessing. The reprocessing closes the processes of removing undissolved foreign matter substances through filters and from dissolved foreign substances Anion and cation exchange resins as well as the concentration vaporizer systems. The rain so obtained Mixture can in turn be the stage of mash production  provided in the required concentration the. The resulting concentrate from the stage of coagulation Onsmittelverdampfung is also in the cycle of washing stage after the coagulation bath.

Through the described circuit management, it is possible to Recovery rate for NMMO and piperidone to ≧ 99.5% observed.

The individual process stages in the aforementioned process execution are thus:

  • - Preparation or pre-treatment of the cellulosic Aus gear to improve accessibility or Dissolving properties,
  • - Mixing and homogenizing the cellulose in one solution medium precursor,
  • - Removal of water by evaporation under vacuum and Shear if necessary with the addition of one or more stabilizers,
  • - Transport and filtration of the solution through pipes, Storage containers, filtration devices,
  • - Extrusion of the cellulose solution obtained through a mold tool directly or with the interposition of an air gap tes in an aqueous or alcohol-containing precipitation bath closing laundry to remove the solvent,
  • - Application of the cellulose molding obtained for embossing special properties,
  • - The precipitation bath obtained by cleaning and concentration again in the appropriate quality of the used Lö precursor is brought.
Examples example 1

350 g NMMNO, 55 g water and 310 g piperidone are combined in one Rotary evaporator heated to 120 ° C and the water under distilled off slowly by applying a vacuum. The distillati residue (NMMO piperidonate) is cooled to 70 ° C. In the syrupy melt obtained is 90 g of a fine ground pulp DP 480 introduced and then with mixed intensively with a propeller stirrer. 250 g the homogeneous ne pulp suspension in a duplex laboratory kneader IKA registered and at 110 ° C internal temperature and one Shaft speed of 20 rpm sheared for 20 min. There is one clear viscous cellulose solution that cools down to room temperature temperature not crystallized and freezes.

Example 2

370 g of pulp with a Cuoxam DP of 520 in a mixture of 1830 g NMMO, 774 g piperidone and 720 g Homogenized water. The temperature of the mixture is 50 ° C. The resulting homogeneous mash is sheared, Apply heat and apply a vacuum as long as possible until a homogeneous solution of the cellulose is observed. The process ran at a final vacuum of 30 mbar and one Temperature of the reaction mass of max. 95 ° C.

The cellulose solution obtained was analyzed and characterized using the following parameters:

cellulose content 11.8% water content 4.5% NMMO Piperidonategehalt 83.7% micrograph no visible particles at 50x magnification in the microscope viscosity 4200 Pa.s melting point less than 30 ° C

The solution obtained was at a temperature of 80 ° C pressed through a spinneret and through an air gap in a precipitation bath spun in water. The hole diameter of the Nozzle bores were 75 µm, the spinning speed was 36 m / min. The resulting fiber cable was washed out, ge cut and prepared.

The textile-physical values were measured as follows:

titres 0.13 tex Strength dry / wet 45/36 cN / tex Elongation dry / wet 12/13% Loop tensile strength 14.5 cN / tex wet modulus 250 cN / tex
Comparative Example 2

It became a cellulose solution analogous to Example 2, but without the piperidone component.

Specifically, the mixture was homogenized into a mash: 370 g Cellulose, 2389 g NMMO and 776 g water.

The evaporation conditions corresponded to those of Example 1; it 400 g of water were evaporated.

The solution obtained was characterized as follows:

cellulose content 11.8% water content 12.0% NMMO content 76.2% micrograph no visible particles at 50x magnification in the microscope viscosity 6500 Pa.s melting point 72 ° C

The fiber values determined analogously under the same conditions of spinning were as follows:

titres 0.13 tex Strength dry / wet 41/35 cN / tex Elongation dry / wet 12 / 13.5% Loop tensile strength 12.4 cN / tex wet modulus 235 cN / tex
Example 3

The following components were homogenized analogously to Example 2:
350 g pulp, Cuoxam DP 500, 1417 g NMMO, 500 g water, 1199 g piperidone, 2 g propyl gallic acid.

The subsequent treatment of the homogenized mash was carried out under the conditions of Example 1 leads until 500 g of water were distilled off.

The solution obtained was characterized as follows:

cellulose content approx. 12% NMMO Piperidonatgehalt approx. 88% micrograph no visible particles at 50x magnification in the microscope viscosity 4520 Pa.s melting point less than 25 ° C

Claims (35)

1. Process for the production of moldings based on cellulose, characterized in that cellulose is dissolved in tertiary amine oxide piperidonates, then deformed, coagulated and the solvent is removed.
2. The method according to claim 1, characterized in that the tertiary amine oxide Is N-methylmorpholine-N-oxide (NMMO).
3. The method according to claim 1 and 2, characterized in that that the NMMO piperidonates from aqueous NMMO and pipe ridon produced by distilling water the.
4. The method according to claim 1 and 3, characterized net that the NMMO piperidonates are an integer and / or has a fractional molar composition and used individually or as mixtures.
5. The method according to claim 1 to 4, characterized net that a cellulose with a medium molecular weight of 40,000 to 350,000 is used.
6. The method according to claim 1 to 5, characterized net that mixtures of celluloses of different moles Specular weights are used.
7. The method according to claim, 1 to 6, characterized in net that cellulose pulps are used, made of hard or soft wood according to the sulfite, sul fat, or the Organocell process.
8. The method according to claim, 1 to 6, characterized in net that used as cellulose cotton linters becomes.  
9. The method according to claim 1 to 8, characterized in that the cellulose with enzymes, radiation or a Explosion technology is treated.
10. The method according to claim 1 to 9, characterized in that that the pulp or cotton linters before the Lö is shredded and / or ground.
11. The method according to claim 1 to 9, characterized in that the pulp or cotton linters before the Lö shredded and / or ground se process, in aqueous Phase with chemicals (alkalis, acids, surfactants) or then treated with enzymes, through intense Shear crushed again and the resulting one Pulp pulp then by dewatering on a defined moisture content is set.
12. The method according to claim 1 to 11, characterized in net that besides cellulose there are others in the system soluble or insoluble, organic or inorganic Compounds such as pigments, dyes, ion exchange shear, soot, ceramic powder.
13. The method according to claim 1 to 12, characterized in net that at least one or more stabilizers too be set.
14. The method according to claim 1 to 13, characterized in net that NaOH is used as a stabilizer.
15. The method according to claim 1 to 13, characterized in net that as a stabilizer mixture NaOH and gallic acid propyl ester is used.
16. The method according to claim 1 to 15, characterized in net that as a stabilizer aldehyde group-binding sub punch, such as hydrazine derivatives, semicarbazides, hydroxyla min or their salts are added.  
17. The method according to claim 1 to 16, characterized in net that the solution preparation under vacuum and Sche tion in a commercially available thin-film apparatus or a single or multi-shaft reactor with mixing and Shear effect occurs.
18. The method according to claim 1 to 17, characterized in net that the shear rates were between 100-10000 1 / s gene.
19. The method according to claim 1 to 18, characterized in net that the cellulose solution has a concentration of 5 contains up to 25% cellulose.
20. The method according to claim 1 to 19, characterized in net that in addition to the NMMO piperidonate one or more Diluents are contained in the cellulose solution.
21. The method according to claim 1 to 20, characterized in net that a diluent is water.
22. The method according to claim 1 to 20, characterized in net that a diluent is an aprotic organi is a solvent.
23. The method according to claim 1 to 20, characterized in net that a diluent is an amphiprotic solvent is medium.
24. The method according to claim 1 to 23, characterized in net that with the manufacture of the cellulose solution Temperatures between 20 and 140 ° C, preferably between between 60 and 130 ° C.
25. The method according to claim 1 to 24, characterized in net that all piping and / or apparatus in which there is cellulose solution, active or passive tempe be riert, the temperature between 50 and 140 ° C. can lie.  
26. The method according to claim 1 to 25, characterized in net that the solution emerging from the mold jet is fed directly into the precipitation bath.
27. The method according to claim 1 to 25, characterized in that the solution jet emerging from the mold pass through an air gap before entering the precipitation bath is tested.
28. The method according to claim 1 to 25 and 27, characterized records that the solder emerging from the mold before entering the precipitation bath by a Air gap passed and with the help of a moving gas feed medium, which may contain additives, is tempered.
29. The method according to claim 1 to 28, characterized in net that the solution temperature in the mold between 20 ° C and 140 ° C.
30. The method according to claim 1 to 29, characterized in net that the precipitation bath from water and / or alcohol and Piperidone and tertiary amine oxide.
31. The method according to claim 1 to 30, characterized in net that from the cellulose solutions fibers, filaments, Foils, nonwovens and membranes can be produced.
32. The method according to claim 1 to 31, characterized in net that the molded body mechanically and / or chemically and / or treated thermally.
33. The method according to claim 1 to 32, characterized in net that the precipitation bath obtained by mechanical Fil tration and / or activated carbon treatment and / or Io exchange stages, consisting of cation and / or anion-active exchange columns or membrane modules, ge is cleaned.  
34. The method according to claim 1 to 33, characterized in net that the solvent recovery by a Va Kuume evaporation plants and / or membrane plants.
35. The method according to claim 1 to 34, characterized in net that if necessary in the cellulose process condensates in the washing process the.
DE10016307A 2000-03-31 2000-03-31 Process for the production and processing of a cellulose solution Expired - Fee Related DE10016307C2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE10016307A DE10016307C2 (en) 2000-03-31 2000-03-31 Process for the production and processing of a cellulose solution

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE10016307A DE10016307C2 (en) 2000-03-31 2000-03-31 Process for the production and processing of a cellulose solution
PCT/DE2001/001177 WO2001074906A1 (en) 2000-03-31 2001-03-28 Method for producing and processing a cellulose solution
CN 01807577 CN1422282A (en) 2000-03-31 2001-03-28 Method for producing and processing a cellulose solution
AU6202301A AU6202301A (en) 2000-03-31 2001-03-28 Method for producing and processing a cellulose solution

Publications (2)

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DE10016307A1 DE10016307A1 (en) 2001-10-18
DE10016307C2 true DE10016307C2 (en) 2002-05-08

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CN (1) CN1422282A (en)
AU (1) AU6202301A (en)
DE (1) DE10016307C2 (en)
WO (1) WO2001074906A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8317503B2 (en) 2004-05-13 2012-11-27 Lenzing Aktiengesellschaft Device for producing Lyocell fibers

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DE10200405A1 (en) 2002-01-08 2002-08-01 Zimmer Ag Cooling blowing spinning apparatus and process
DE10204381A1 (en) 2002-01-28 2003-08-07 Zimmer Ag Ergonomic spinning system
DE10206089A1 (en) 2002-02-13 2002-08-14 Zimmer Ag bursting
DE10314878A1 (en) * 2003-04-01 2004-10-28 Zimmer Ag Method and device for producing post-stretched cellulose filaments
JP5371441B2 (en) * 2005-12-23 2013-12-18 ビーエーエスエフ ソシエタス・ヨーロピアBasf Se Solvent system based on molten ionic liquid, its production and its use to produce regenerated carbohydrates
CN103305570B (en) * 2013-06-07 2015-06-24 常州大学 Method for pre-treating corn stalks by diluted hydrochloric acid auxiliary oxide morpholine-N-oxide
TWI547609B (en) * 2013-08-29 2016-09-01 財團法人紡織產業綜合研究所 Preparation method of high cellulose concentratlon spinning dope and manufacturing method of non-woven fabric
EA024329B1 (en) * 2013-09-27 2016-09-30 Сумгаитский Государственный Университет Process for cellulose activation
AT515174B1 (en) * 2013-10-15 2019-05-15 Chemiefaser Lenzing Ag Cellulose suspension, process for its preparation and use
EA025957B1 (en) * 2013-12-23 2017-02-28 Сумгаитский Государственный Университет Process for cellulose activation

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2848471A1 (en) * 1977-11-25 1979-06-07 Akzona Inc A process for producing articles based on cellulose
US5362867A (en) * 1992-05-27 1994-11-08 Formosa Chemicals & Fibre Corporation Method of making cellulose yarn solution
DE4420304C1 (en) * 1994-06-10 1995-09-21 Fraunhofer Ges Forschung Flexible cellulose, low modulus cellulose fibres for textile applications
DE69400311T2 (en) * 1993-05-28 1996-11-28 Courtaulds Fibres Holdings Ltd Transport of cellulose solutions through pipelines
US5929228A (en) * 1998-02-09 1999-07-27 Cheng; Meng-Song Cellulose solution with low viscosity and process of preparing the same
WO1999060026A1 (en) * 1998-05-19 1999-11-25 Tencel Limited Cellulosic solutions and their uses

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2848471A1 (en) * 1977-11-25 1979-06-07 Akzona Inc A process for producing articles based on cellulose
US5362867A (en) * 1992-05-27 1994-11-08 Formosa Chemicals & Fibre Corporation Method of making cellulose yarn solution
DE69400311T2 (en) * 1993-05-28 1996-11-28 Courtaulds Fibres Holdings Ltd Transport of cellulose solutions through pipelines
DE4420304C1 (en) * 1994-06-10 1995-09-21 Fraunhofer Ges Forschung Flexible cellulose, low modulus cellulose fibres for textile applications
US5929228A (en) * 1998-02-09 1999-07-27 Cheng; Meng-Song Cellulose solution with low viscosity and process of preparing the same
WO1999060026A1 (en) * 1998-05-19 1999-11-25 Tencel Limited Cellulosic solutions and their uses

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8317503B2 (en) 2004-05-13 2012-11-27 Lenzing Aktiengesellschaft Device for producing Lyocell fibers
US8580167B2 (en) 2004-05-13 2013-11-12 Lenzing Aktiengesellschaft Lyocell method comprising an adjustment of the processing duration based on the degree of polymerization

Also Published As

Publication number Publication date
DE10016307A1 (en) 2001-10-18
AU6202301A (en) 2001-10-15
WO2001074906A1 (en) 2001-10-11
CN1422282A (en) 2003-06-04

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