EP0918893B1 - Cellulosische mikrofaser - Google Patents
Cellulosische mikrofaser Download PDFInfo
- Publication number
- EP0918893B1 EP0918893B1 EP98925319A EP98925319A EP0918893B1 EP 0918893 B1 EP0918893 B1 EP 0918893B1 EP 98925319 A EP98925319 A EP 98925319A EP 98925319 A EP98925319 A EP 98925319A EP 0918893 B1 EP0918893 B1 EP 0918893B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cellulose
- air
- mass
- solution
- spinning
- 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
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Classifications
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- 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 present invention relates to a manufacturing process cellulosic fibers, with cellulose or cellulose in an aqueous tertiary amine oxide to a spinnable solution is solved, this solution using a spinneret Filaments is spun, and the filaments are stretched introduced into a precipitation bath through an air gap to precipitate the dissolved pulp.
- NMMO N-methylmorpholine-N-oxide
- Tertiary amine oxides have long been an alternative Known solvents for cellulose. From U.S. Patent 2,179,181 it is known, for example, that tertiary amine oxides are of high quality Chemical pulp can solve without derivatization and that from these solutions by precipitation cellulosic moldings, how fibers can be obtained. In the US PSen 3,447,939, 3,447,956 and 3,508,941 are other methods described for the production of cellulosic solutions, wherein as Solvents preferably cyclic amine oxides are used. In all of these processes, cellulose is made at elevated temperature physically solved.
- EP-A-0 356 419 by the applicant describes a method described, preferably in a thin film treatment apparatus is carried out in which a suspension of crushed pulp in an aqueous tertiary amine oxide in the form of a thin layer spread over a heating surface is transported, the surface of this thin layer is exposed to a vacuum.
- a suspension of crushed pulp in an aqueous tertiary amine oxide in the form of a thin layer spread over a heating surface is transported, the surface of this thin layer is exposed to a vacuum.
- Water is evaporated via the heating surface and the cellulose can be brought into solution so that a spinnable cellulose solution is discharged.
- Methods for spinning cellulose solutions are e.g. out EP-A-0 671 492 and EP-A-0 659 219 of the applicant known.
- the spinning solution is added through a spinneret Filaments extruded through an air gap into a coagulation bath in which the cellulose precipitates. In the air gap the filaments are stretched. This procedure is commonly known as dry / wet spinning processes.
- the applicant's WO 95/02082 also describes a dry / wet spinning process. This method uses cooling air that has a temperature between 10 ° C and 60 ° C. The humidity of the cooling air supplied is between 20 g H 2 O and 40 g H 2 O per kilogram.
- WO 94/28218 generally proposes the use of spinnerets with 500 to 100,000 holes.
- the temperature of the cooling air is between 0 ° C and 50 ° C.
- the person skilled in the art can see from this literature that the moisture is between 5.5 g H 2 O and 7.5 g H 2 O per kilogram of air. This creates a relatively dry climate in the air gap.
- WO 96/17118 also deals with the climate in the air gap, it being determined that the climate should be as dry as possible, namely 0.1 g H 2 O to 7 g H 2 O per kilogram of air, with a relative humidity of less than 85%. 6 ° C to 40 ° C is suggested as the temperature for the cooling air.
- WO 96/21758 also deals with that to be set climate in the air gap, with a two-stage blowing with different cooling air is proposed, and in the upper Area of the air gap with less humid and cooler air is blown.
- EP-A-0 648 808 describes a molding process a cellulose solution, the cellulosic components the solution a first component made of a cellulose with a Average degree of polymerization (DP) from 500 to 2000 and a second cellulose component with a DP less than 90% of the DP of the first component in the range from 350 to 900 included.
- the weight ratio of the first for the second component should be 95: 5 to 50:50.
- the invention therefore has as its object a method for To provide manufacture of cellulosic fibers, wherein pulp is added in an aqueous tertiary amine oxide a spinnable solution is solved, this solution under Is spun into filaments using a spinneret, and the filaments into one by stretching through an air gap Precipitation bath to be introduced to the dissolved pulp fell, which method allows, fibers with a titer of maximum or less than 1 dtex. These fibers are called microfibers ("Lexicon of textile finishing", H. K. Rouette, volume 2, page 1250 ff; 1995; Laumann'sche Publishing company, ISBN 3-87466-228-4).
- the invention provides in particular the task of staple fibers of the genus Lyocell with a maximum or less than 1 dtex titer to provide.
- Cellulose molecules with a molecular weight of at least 5x10 5 are referred to as "long chain" for the purposes of the present description and claims.
- a preferred embodiment of the method according to the invention is therefore characterized in that the filaments with air be blown immediately after they leave the spinneret and that this air has a moisture content of less than 5 g water / kg air.
- the tertiary amine oxide preferably N-methyl-morpholine-N-oxide used.
- the invention also relates to the use of a spinnable solution of cellulose in an aqueous tertiary amine oxide which is less than 0.20% by mass, in particular less than 0.05% by mass, based on the mass of the solution, of cellulose with a molecular weight of at least 5x10 5 , for the production of cellulosic fibers with a maximum titer of 1 dtex.
- the tertiary amine oxide is N-methyl-morpholine-N-oxide best proven.
- the invention leads to a cellulosic fiber Genus Lyocell, the one Titers in the range from 1.0 dtex to 0.3 dtex, especially in the Range of 1.0 dtex and 0.5 dtex, and preferably in the range of 1.0 dtex and 0.8 dtex. Accordingly, too staple fibers with a length of in particular 1 cm to 10 cm.
- the molecular weight profile of a pulp can be determined using Gel permeation chromatography (GPC) can be obtained, whereby in the "Differential Weight Fraction" in [%] as a graph Ordinate against molecular weight [g / mol; logarithmic Application] is applied.
- GPC Gel permeation chromatography
- the size "differential weight fraction” describes the percentage frequency fraction of the molar mass fraction.
- the measuring apparatus is implemented by means of measures familiar to the person skilled in the art calibrated.
- the signals are evaluated according to Zimm, using the Zimm formula if necessary, set in the evaluation software.
- FIG. 1a For the Viscokraft LV pulp (manufacturer: International Paper) the molecular weight profile in FIG. 1a is exemplary shown.
- the diagram of Fig. 1a shows that this pulp largely consists of molecules with one There is a molecular weight of about 100,000 and that this Pulp practically no parts with a molecular weight of more than 500,000.
- a 15% cellulose solution from this pulp only (production see below) in an aqueous amine oxide ( spinning mass) that used in the present invention.
- Fig. 1b shows the molecular weight profile of the pulp Alistaple LD 9.2 (manufacturer: Western Pulp).
- This pulp has a maximum molar mass frequency at around 200,000, and the graph also shows that this A high proportion (about 25%) of molecules with a pulp Has molecular weight greater than 500,000.
- a spinning mass, who exclusively use such a pulp to 15 Contains% by mass, has about 4% (based on the mass of Solution; Degradation not taken into account during solution production) Cellulose molecules with a molecular weight of larger than 500,000 and thus does not correspond to that according to the invention is used.
- the shredded pulp is in aqueous, 50% NMMO suspended, in a kneader (Type: IKA laboratory kneader HKD-T; Manufacturer: IKA-Labortechnik) and impregnate for one hour calmly. Then by heating the Kneader with a heating medium heated to 130 ° C and through Reduce the pressure of water evaporated until the pulp has completely gone into solution.
- a kneader Type: IKA laboratory kneader HKD-T; Manufacturer: IKA-Labortechnik
- a spinning apparatus is used in plastics processing Common melt index device from Davenport used.
- This device consists of a heatable, temperature-controllable Steel cylinder into which the spinning mass is poured becomes.
- a piston loaded with a weight is the spinning mass by the at the bottom of the Steel cylinder attached spinneret that has a hole with a Has diameter of 100 microns, extruded.
- the one placed in the spinning apparatus Spinning mass (cellulose content: 15%) extruded through the spinning hole and over an air gap 3 cm in length led an aqueous precipitation bath, deflected, over a godet deducted, which is provided behind the precipitation bath, and thereby stretched.
- the spinning mass output through the nozzle is 0.030 g / min.
- the spinning temperature is 80 ° C to 120 ° C.
- the minimally spinnable is used to simulate the spinning behavior Titer taken. This is the maximum take-off speed (m / min) determined. The take-off speed is like this increased for a long time until the thread breaks. That speed is noted and for the calculation of the titer see below Formula used. The higher this value is, the better is the spinning behavior and the finer the obtained Fiber.
- Fig. 2 shows the spinning behavior of cellulose solutions with varying proportions of long chain molecules, where as Ordinate the minimum titer (dtex) and as the abscissa the Concentration of the respective cellulose solution on cellulose molecules with a molecular weight of at least 500,000 is applied. The concentrations were just before determined by spinning.
- the proportion of long chain molecules was determined by adding corresponding amounts of Alistaple LD 9.2 to Viscokraft LV set.
- the cellulose concentration of the solution was in 15 mass% in all cases.
- the spinning behavior was determined for each cellulose solution both at a humidity in the air gap of 30 g H 2 O (curve “a") and at 0 g H 2 O (dry) (straight line “b").
Description
Zellstoff | Temp. | Feuchte | max. Abzugsgeschw. | Titer |
Alistaple LD 9.2 | ||||
" | 105 | 0 | 31 | 1,78 |
" | 105 | 20 | 40 | 1,37 |
" | 105 | 47 | 62 | 0,87 |
" | 115 | 0 | 38 | 1,43 |
" | 115 | 20 | 42 | 1,29 |
" | 115 | 47 | 83 | 0,66 |
" | 120 | 0 | 40 | 1,35 |
" | 120 | 20 | 59 | 0,92 |
" | 120 | 47 | 83 | 0,66 |
Zellstoff | Temp. | Feuchte | max. Abzugsgeschw. | Titer |
Viscokraft LV (unbestrahlt) | 105 | 0 | 156 | 0,35 |
" | 105 | 20 | 176 | 0,31 |
" | 105 | 47 | 43 | 1,27 |
" | 115 | 0 | 176 | 0,31 |
" | 115 | 20 | 99 | 0,55 |
" | 115 | 47 | 63 | 0,86 |
" | 120 | 0 | 170 | 0,32 |
" | 120 | 22 | 83 | 0,66 |
" | 120 | 47 | 52 | 1,05 |
Zellstoffmischung (Alistaple/Viscokraft) | Feuchte | max. /Abzugsgeschw. | Titer |
30/70 | 30 | 116 | 0,47 |
30/70 | 50 | 118 | 0,46 |
30/70 | 70 | 127 | 0,43 |
- daß ein Zusammenhang zwischen Verspinnbarkeit und Konzentration an langkettigen Molekülen besteht;
- daß bei trockener Luft im Luftspalt (Gerade "b") die Verspinnbarkeit annähernd linear immer besser wird, wenn die Konzentration an langkettigen Molekülen abnimmt;
- daß bei feuchter Luft im Luftspalt (Kurve "a") die Verspinnbarkeit mit abnehmender Konzentration an langkettigen Molekülen zunächst auch immer besser wird, sich ab einer Konzentration von etwa 0,25 Masse-% jedoch wieder verschlechtert, wobei diese Verschlechterung ab 0,05 Masse-% besonders ausgeprägt ist.
- die Konzentration an Cellulosemolekülen mit einem Molekulargewicht von mindestens 5x105, und
- der Feuchtigkeitsgehalt der Luft im Luftspalt.
Claims (4)
- Verfahren zur Herstellung cellulosischer Fasern, wobei Cellulose in einem wässerigen tertiären Aminoxid zu einer spinnbaren Lösung gelöst wird, diese Lösung unter Verwendung einer Spinndüse zu Filamenten versponnen wird, und die Filamente unter Verstreckung durch einen Luftspalt in ein Fällbad eingebracht werden, um die gelöste Cellulose zu fällen,
dadurch gekennzeichnet, daßzum Verspinnen eine Lösung eingesetzt wird, die weniger als 0,20 Masse-%, insbesondere weniger als 0,05 Masse-%, bezogen auf die Masse der Lösung, Cellulose mit einem Molekulargewicht von mindestens 5x105 aufweist, unddie Luft im Luftspalt einen Feuchtigkeitsgehalt von kleiner als 5 g Wasser/kg Luft aufweist. - Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Filamente mit Luft beblasen werden, unmittelbar nachdem sie die Spinndüse verlassen haben, und daß diese Luft einen Feuchtigkeitsgehalt von kleiner als 5 g Wasser/kg Luft aufweist.
- Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß als tertiäres Aminoxid N-Methylmorpholin-N-oxid eingesetzt wird.
- Verwendung einer spinnbaren Lösung von Cellulose in einem wässerigen tertiären Aminoxid, welche weniger als 0,20 Masse-%, insbesondere weniger als 0,05 Masse-%, bezogen auf die Masse der Lösung, Cellulose mit einem Molekulargewicht von mindestens 5x105 aufweist, zur Herstellung cellulosischer Fasern mit einem Titer von maximal 1 dtex.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT98925319T ATE251238T1 (de) | 1997-06-17 | 1998-06-17 | Cellulosische mikrofaser |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT105597 | 1997-06-17 | ||
AT1055/97 | 1997-06-17 | ||
AT105597A AT405532B (de) | 1997-06-17 | 1997-06-17 | Cellulosische mikrofaser |
PCT/AT1998/000150 WO1998058102A1 (de) | 1997-06-17 | 1998-06-17 | Cellulosische mikrofaser |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0918893A1 EP0918893A1 (de) | 1999-06-02 |
EP0918893B1 true EP0918893B1 (de) | 2003-10-01 |
Family
ID=3505615
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98925319A Expired - Lifetime EP0918893B1 (de) | 1997-06-17 | 1998-06-17 | Cellulosische mikrofaser |
Country Status (7)
Country | Link |
---|---|
EP (1) | EP0918893B1 (de) |
AT (1) | AT405532B (de) |
AU (1) | AU7750498A (de) |
DE (1) | DE59809792D1 (de) |
ES (1) | ES2206936T3 (de) |
PT (1) | PT918893E (de) |
WO (1) | WO1998058102A1 (de) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6221487B1 (en) | 1996-08-23 | 2001-04-24 | The Weyerhauser Company | Lyocell fibers having enhanced CV properties |
US6235392B1 (en) | 1996-08-23 | 2001-05-22 | Weyerhaeuser Company | Lyocell fibers and process for their preparation |
AT506268B1 (de) | 2008-01-11 | 2014-08-15 | Chemiefaser Lenzing Ag | Mikrofaser |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB9421261D0 (en) * | 1994-10-21 | 1994-12-07 | Courtaulds Plc | Non-woven fabrics |
TW389799B (en) * | 1995-08-29 | 2000-05-11 | Asahi Chemical Ind | Cellulose multifilament yarn and fabric made thereof |
GB9605504D0 (en) * | 1996-03-15 | 1996-05-15 | Courtaulds Plc | Manufacture of elongate members |
EP0920548B1 (de) * | 1996-08-23 | 2002-10-02 | Weyerhaeuser Company | Lyocellfasern und verfahren zu ihrer herstellung |
-
1997
- 1997-06-17 AT AT105597A patent/AT405532B/de not_active IP Right Cessation
-
1998
- 1998-06-17 AU AU77504/98A patent/AU7750498A/en not_active Abandoned
- 1998-06-17 WO PCT/AT1998/000150 patent/WO1998058102A1/de active IP Right Grant
- 1998-06-17 PT PT98925319T patent/PT918893E/pt unknown
- 1998-06-17 EP EP98925319A patent/EP0918893B1/de not_active Expired - Lifetime
- 1998-06-17 DE DE59809792T patent/DE59809792D1/de not_active Expired - Fee Related
- 1998-06-17 ES ES98925319T patent/ES2206936T3/es not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
DE59809792D1 (de) | 2003-11-06 |
AU7750498A (en) | 1999-01-04 |
PT918893E (pt) | 2004-02-27 |
AT405532B (de) | 1999-09-27 |
WO1998058102A1 (de) | 1998-12-23 |
ES2206936T3 (es) | 2004-05-16 |
ATA105597A (de) | 1999-01-15 |
EP0918893A1 (de) | 1999-06-02 |
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