CA2413706A1 - Process for the production of cellulosic fibres - Google Patents
Process for the production of cellulosic fibres Download PDFInfo
- Publication number
- CA2413706A1 CA2413706A1 CA002413706A CA2413706A CA2413706A1 CA 2413706 A1 CA2413706 A1 CA 2413706A1 CA 002413706 A CA002413706 A CA 002413706A CA 2413706 A CA2413706 A CA 2413706A CA 2413706 A1 CA2413706 A1 CA 2413706A1
- Authority
- CA
- Canada
- Prior art keywords
- fibres
- temperature
- air
- filaments
- 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.)
- Abandoned
Links
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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Paper (AREA)
Abstract
The invention relates to a method for producing cellulose fibres. According to said method, a solution of cellulose in a tertiary amino oxide is extruded through the spinning holes of a spinneret and the extruded filaments are fed into a precipitation bath whilst being drawn via an air gap. The filaments are exposed to a gaseous stream in the air gap. The invention is characterised in that the temperature (T) of the gas prior to the contact with the filaments is represented by the formula: 60 ~C < T < 90 ~C.
Description
Process for the Production of Cellulosic Fibres The invention relates to a process according to the preamble of claim 1.
Such processes for the production of cellulosic fibres are known under the names of "amine-oxide process" or "Lyocell process".
"Lyocell" is the generic name BISFA (The International Bureau for the Standardization of man-made fibres) has given to cellulose fibres which are produced by dissolving cellulose in an organic solvent without formation of a derivative and extruding fibres from that solution.
By "an organic solvent", a mixture of an organic chemical and water is understood therein.
Such fibres are also known by the term of "solvent-spun fibres". As an organic solvent, N-methyl-morpholino-N-oxide is used today on a commercial scale.
It is known that the properties of Lyocell fibres as well as the stability of the spinning process are substantially influenced by the conditions prevailing in the so-called air gap between the spinning nozzle and the precipitation-bath surface.
For example, it is known from PCT-WO 93/19230 to cool the extruded filaments immediately after the forming by means of a gas stream. In the following, this gas stream is referred to as "cooling air". In the examples of PCT-WO 93/19230, the temperature of the cooling air is -6°C to 24°C.
PCT-WO 94/28218 describes a similar process as does PCT-WO 93/19230. According to that document, the temperature of the cooling air is to be kept below 50°C.
From PCT-WO 95/02082 there is known a process according to which the spinning-hole diameter, the spinning-mass output per hole, the titer of the individual filament, the width of the air gap and the humidity of the air in the air gap are to be kept in certain ranges by a mathematical expression. In the examples of PCT-WO 95/02082, no information on the temperature of the cooling air is given. In the description there are generally indicated temperatures of between 10°C and 60°C, preferably of between 20°C and 40°C.
PCT-WO 96/17118 deals with the humidity content of the cooling air. The highest cooling-air temperature indicated in that document is around 40°C.
Such processes for the production of cellulosic fibres are known under the names of "amine-oxide process" or "Lyocell process".
"Lyocell" is the generic name BISFA (The International Bureau for the Standardization of man-made fibres) has given to cellulose fibres which are produced by dissolving cellulose in an organic solvent without formation of a derivative and extruding fibres from that solution.
By "an organic solvent", a mixture of an organic chemical and water is understood therein.
Such fibres are also known by the term of "solvent-spun fibres". As an organic solvent, N-methyl-morpholino-N-oxide is used today on a commercial scale.
It is known that the properties of Lyocell fibres as well as the stability of the spinning process are substantially influenced by the conditions prevailing in the so-called air gap between the spinning nozzle and the precipitation-bath surface.
For example, it is known from PCT-WO 93/19230 to cool the extruded filaments immediately after the forming by means of a gas stream. In the following, this gas stream is referred to as "cooling air". In the examples of PCT-WO 93/19230, the temperature of the cooling air is -6°C to 24°C.
PCT-WO 94/28218 describes a similar process as does PCT-WO 93/19230. According to that document, the temperature of the cooling air is to be kept below 50°C.
From PCT-WO 95/02082 there is known a process according to which the spinning-hole diameter, the spinning-mass output per hole, the titer of the individual filament, the width of the air gap and the humidity of the air in the air gap are to be kept in certain ranges by a mathematical expression. In the examples of PCT-WO 95/02082, no information on the temperature of the cooling air is given. In the description there are generally indicated temperatures of between 10°C and 60°C, preferably of between 20°C and 40°C.
PCT-WO 96/17118 deals with the humidity content of the cooling air. The highest cooling-air temperature indicated in that document is around 40°C.
According to PCT-WO 96/21758, the temperature of the cooling air may be 0°C to 40°C. In PCT-WO 97/38153, the temperature of the cooling air is indicated as being -10°C to 50°C.
PCT-WO 98/58103 describes that in the case of a large number of extruded filaments, i.e., when spinning nozzles with a great number of spinning holes are used, a very humid climate in the air gap results. To ensure the stability of the spinning process also under those conditions, PCT-WO 98/58103 suggests that the spinning solution immediately before spinning should contain a specific proportion of cellulose and/or another polymer having a higher molecular weight.
One problem in spinning cellulose solutions in NMMO is that in the case of solutions having a high viscosity, the spinning solution has to be spun at increased temperatures. High viscosities of the spinning solution result for example when the cellulose concentration in the solution is high, which of course is desired from an economical point of view.
High viscosities further result when pulps having high proportions of high-molecular cellulose are used.
However, the temperature of the spinning solution has to be kept high also when fibres having a smaller titer, e.g. smaller than 1 dtex, are to be spun. In the case of such fibres, the filaments in the air gap have to be stretched to a particularly high degree.
Without increasing the temperature of the spinning solution, the viscosity of the spinning solution would also here be too high for this stretching.
Usually, during spinning, the temperature of the spinning solution should be 80°C to 120°C, in particular 100°C to 120°C. Since solutions of cellulose in NMMO are thermally unstable and tend to undergo exothermal decomposition reactions, it is, however, not desired to increase the temperature of the cellulose solution.
The present invention has as its object to provide a process according to the generic term, whereby cellulose solutions having a high viscosity can be spun better and fibres having small titers can be produced better.
This object is achieved in that for the temperature (T) of the cooling air before the contact with the filaments 60°C < T < 90°C is correct.
Surprisingly, it has been shown that when using cooling air having higher temperatures in the range of claim 1, also higher-viscous cellulose solutions can be spun well, without having to increase the temperature of the spinning solution. Also fibres having small titers, e.g. 0.9 dtex, can be spun well without increasing the temperature of the spinning solution.
Furthermore, fibres which are produced using cooling air with higher temperatures have higher strength values than fibres which at the same temperature of the spinning solution are produced using cooling air with a lower temperature.
Preferably, the cooling air has a humidity content of 4g of H20/kg of air up to 1 Sg of H20/kg of air.
In particular, the process according to the invention is suitable for the production of fibres having a titer of less than 1 dtex.
Example l:
A spinning solution having 15% by weight cellulose (pulp: Cellunier F, manufacturer:
Rayonnier), 10% by weight water and 75% by weight NMMO was spun into fibres while using cooling air with different temperatures.
The respective minimally obtainable titer of the fibres was measured: For this, the maximum drawing-off speed (m/min) of the fibres is determined by increasing the drawing-off speed up until the fibre breaks. This speed is noted and utilized for calculating the titer according to the calculation method described in PCT-WO 98/58103.
Further, the strength of the spun fibres in the conditioned state was determined, respectively.
Temperature Temperature of Minimum Titer Strength of the the (dtex) Conditioned (cN/tex) Spinning SolutionCooling Air (C) C
100 20 2.01 38.1 100 50 1.70 38.7 100 60 1.59 40.1 100 70 1.36 39.8 100 80 1.32 40.6 From the table it is apparent that at temperatures of the cooling air of above 60°C, the minimally obtainable titer decreases considerably. Further, the strength of the fibres increases considerably.
Example 2:
A spinning solution having 14.6% by weight cellulose (pulp: Borregaard LVU), 9.5% by weight water and 75.9% by weight NMMO was spun in a continuous experimental plant into fibres having a titer of 1.3 dtex. At different temperatures of the cooling air used it was measured which spinning-mass temperature was necessary to be able to produce without disturbances fibres having that titer.
Temperature of Spinning-mass Temperature Required the (C) Coolin Air C
From the table it is apparent that when using cooling air with a temperature of 65°C, it is possible to produce the fibres at a considerably lower temperature of the spinning solution.
Example 3:
A spinning solution having 15% by weight cellulose (pulp: Alicell VLV, manufacturer:
Western Pulp), 10% by weight water and 75% by weight NMMO was spun into fibres while using cooling air with different temperatures. As described in Example 1, the minimally obtainable titer of the fibres as well as the strength of the spun fibres in the conditioned state were determined:
Temperature Temperature of Minimum Titer Strength of the the (dtex) Conditioned (cN/tex) Spinning SolutionCooling Air (C) C
100 20 1.34 37.4 100 50 1.05 39.2 100 70 0.98 40.4 100 80 0.92 39.1 ~
From the table it is apparent that when using cooling air with higher temperatures, it is well possible to produce fibres having a titer of less than 1 dtex.
PCT-WO 98/58103 describes that in the case of a large number of extruded filaments, i.e., when spinning nozzles with a great number of spinning holes are used, a very humid climate in the air gap results. To ensure the stability of the spinning process also under those conditions, PCT-WO 98/58103 suggests that the spinning solution immediately before spinning should contain a specific proportion of cellulose and/or another polymer having a higher molecular weight.
One problem in spinning cellulose solutions in NMMO is that in the case of solutions having a high viscosity, the spinning solution has to be spun at increased temperatures. High viscosities of the spinning solution result for example when the cellulose concentration in the solution is high, which of course is desired from an economical point of view.
High viscosities further result when pulps having high proportions of high-molecular cellulose are used.
However, the temperature of the spinning solution has to be kept high also when fibres having a smaller titer, e.g. smaller than 1 dtex, are to be spun. In the case of such fibres, the filaments in the air gap have to be stretched to a particularly high degree.
Without increasing the temperature of the spinning solution, the viscosity of the spinning solution would also here be too high for this stretching.
Usually, during spinning, the temperature of the spinning solution should be 80°C to 120°C, in particular 100°C to 120°C. Since solutions of cellulose in NMMO are thermally unstable and tend to undergo exothermal decomposition reactions, it is, however, not desired to increase the temperature of the cellulose solution.
The present invention has as its object to provide a process according to the generic term, whereby cellulose solutions having a high viscosity can be spun better and fibres having small titers can be produced better.
This object is achieved in that for the temperature (T) of the cooling air before the contact with the filaments 60°C < T < 90°C is correct.
Surprisingly, it has been shown that when using cooling air having higher temperatures in the range of claim 1, also higher-viscous cellulose solutions can be spun well, without having to increase the temperature of the spinning solution. Also fibres having small titers, e.g. 0.9 dtex, can be spun well without increasing the temperature of the spinning solution.
Furthermore, fibres which are produced using cooling air with higher temperatures have higher strength values than fibres which at the same temperature of the spinning solution are produced using cooling air with a lower temperature.
Preferably, the cooling air has a humidity content of 4g of H20/kg of air up to 1 Sg of H20/kg of air.
In particular, the process according to the invention is suitable for the production of fibres having a titer of less than 1 dtex.
Example l:
A spinning solution having 15% by weight cellulose (pulp: Cellunier F, manufacturer:
Rayonnier), 10% by weight water and 75% by weight NMMO was spun into fibres while using cooling air with different temperatures.
The respective minimally obtainable titer of the fibres was measured: For this, the maximum drawing-off speed (m/min) of the fibres is determined by increasing the drawing-off speed up until the fibre breaks. This speed is noted and utilized for calculating the titer according to the calculation method described in PCT-WO 98/58103.
Further, the strength of the spun fibres in the conditioned state was determined, respectively.
Temperature Temperature of Minimum Titer Strength of the the (dtex) Conditioned (cN/tex) Spinning SolutionCooling Air (C) C
100 20 2.01 38.1 100 50 1.70 38.7 100 60 1.59 40.1 100 70 1.36 39.8 100 80 1.32 40.6 From the table it is apparent that at temperatures of the cooling air of above 60°C, the minimally obtainable titer decreases considerably. Further, the strength of the fibres increases considerably.
Example 2:
A spinning solution having 14.6% by weight cellulose (pulp: Borregaard LVU), 9.5% by weight water and 75.9% by weight NMMO was spun in a continuous experimental plant into fibres having a titer of 1.3 dtex. At different temperatures of the cooling air used it was measured which spinning-mass temperature was necessary to be able to produce without disturbances fibres having that titer.
Temperature of Spinning-mass Temperature Required the (C) Coolin Air C
From the table it is apparent that when using cooling air with a temperature of 65°C, it is possible to produce the fibres at a considerably lower temperature of the spinning solution.
Example 3:
A spinning solution having 15% by weight cellulose (pulp: Alicell VLV, manufacturer:
Western Pulp), 10% by weight water and 75% by weight NMMO was spun into fibres while using cooling air with different temperatures. As described in Example 1, the minimally obtainable titer of the fibres as well as the strength of the spun fibres in the conditioned state were determined:
Temperature Temperature of Minimum Titer Strength of the the (dtex) Conditioned (cN/tex) Spinning SolutionCooling Air (C) C
100 20 1.34 37.4 100 50 1.05 39.2 100 70 0.98 40.4 100 80 0.92 39.1 ~
From the table it is apparent that when using cooling air with higher temperatures, it is well possible to produce fibres having a titer of less than 1 dtex.
Claims (4)
1. A process for the production of cellulosic fibres by extruding a solution of cellulose in a tertiary amine oxide through spinning holes of a spinning nozzle and conducting the extruded filaments into a precipitation bath via an air gap while they are drawn off, the filaments in the air gap being exposed to the flow of a gas, characterized in that for the temperature (T) of the gas before the contact with the filaments 60°C < T
< 90°C is correct.
< 90°C is correct.
2. A process according to claim 1, characterized in that the gas is air.
3. A process according to claim 2, characterized in that the flowing air has a humidity content of 4g of H2O/kg of air up to 15g of H2O/kg of air.
4. A process according to anyone of claims 1 to 3, characterized in that filaments having a titer of less than 1 dtex are produced.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT0112100A AT408355B (en) | 2000-06-29 | 2000-06-29 | Process for producing cellulosic fibres |
| ATA1121/2000 | 2000-06-29 | ||
| PCT/AT2001/000212 WO2002000975A1 (en) | 2000-06-29 | 2001-06-28 | Method for producing cellulose fibres |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2413706A1 true CA2413706A1 (en) | 2002-12-24 |
Family
ID=3685802
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002413706A Abandoned CA2413706A1 (en) | 2000-06-29 | 2001-06-28 | Process for the production of cellulosic fibres |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US20030173700A1 (en) |
| EP (1) | EP1299583B1 (en) |
| JP (1) | JP2004501296A (en) |
| CN (1) | CN1180142C (en) |
| AT (1) | AT408355B (en) |
| AU (2) | AU6712701A (en) |
| BR (1) | BR0112036A (en) |
| CA (1) | CA2413706A1 (en) |
| DE (1) | DE50102613D1 (en) |
| NO (1) | NO20026186L (en) |
| TR (1) | TR200401926T4 (en) |
| TW (1) | TW534932B (en) |
| WO (1) | WO2002000975A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT506268B1 (en) | 2008-01-11 | 2014-08-15 | Chemiefaser Lenzing Ag | MICROFIBRE |
| US10920274B2 (en) | 2017-02-21 | 2021-02-16 | Apdn (B.V.I.) Inc. | Nucleic acid coated submicron particles for authentication |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATA53792A (en) * | 1992-03-17 | 1995-02-15 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING CELLULOSIC MOLDED BODIES, DEVICE FOR IMPLEMENTING THE METHOD AND USE OF A SPINNING DEVICE |
| US5902532A (en) * | 1994-12-02 | 1999-05-11 | Akzo Nobel Nv | Process for manufacturing cellulose objects |
| US6221487B1 (en) * | 1996-08-23 | 2001-04-24 | The Weyerhauser Company | Lyocell fibers having enhanced CV properties |
| US6210801B1 (en) * | 1996-08-23 | 2001-04-03 | Weyerhaeuser Company | Lyocell fibers, and compositions for making same |
| AT405531B (en) * | 1997-06-17 | 1999-09-27 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING CELLULOSIC FIBERS |
| AT408656B (en) * | 1998-06-04 | 2002-02-25 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING CELLULOSIC MOLDED BODIES |
-
2000
- 2000-06-29 AT AT0112100A patent/AT408355B/en not_active IP Right Cessation
-
2001
- 2001-06-28 AU AU6712701A patent/AU6712701A/en active Pending
- 2001-06-28 EP EP01944725A patent/EP1299583B1/en not_active Expired - Lifetime
- 2001-06-28 CA CA002413706A patent/CA2413706A1/en not_active Abandoned
- 2001-06-28 BR BR0112036-0A patent/BR0112036A/en not_active IP Right Cessation
- 2001-06-28 AU AU2001267127A patent/AU2001267127B2/en not_active Ceased
- 2001-06-28 CN CNB018118291A patent/CN1180142C/en not_active Expired - Fee Related
- 2001-06-28 DE DE50102613T patent/DE50102613D1/en not_active Expired - Fee Related
- 2001-06-28 TW TW090115807A patent/TW534932B/en not_active IP Right Cessation
- 2001-06-28 WO PCT/AT2001/000212 patent/WO2002000975A1/en active IP Right Grant
- 2001-06-28 JP JP2002506280A patent/JP2004501296A/en not_active Abandoned
- 2001-06-28 TR TR2004/01926T patent/TR200401926T4/en unknown
-
2002
- 2002-12-23 NO NO20026186A patent/NO20026186L/en not_active Application Discontinuation
- 2002-12-27 US US10/330,779 patent/US20030173700A1/en not_active Abandoned
Also Published As
| Publication number | Publication date |
|---|---|
| ATA11212000A (en) | 2001-03-15 |
| EP1299583B1 (en) | 2004-06-16 |
| TW534932B (en) | 2003-06-01 |
| CN1180142C (en) | 2004-12-15 |
| CN1439065A (en) | 2003-08-27 |
| BR0112036A (en) | 2003-05-13 |
| NO20026186D0 (en) | 2002-12-23 |
| US20030173700A1 (en) | 2003-09-18 |
| AU2001267127B2 (en) | 2005-03-24 |
| AT408355B (en) | 2001-11-26 |
| DE50102613D1 (en) | 2004-07-22 |
| TR200401926T4 (en) | 2004-09-21 |
| JP2004501296A (en) | 2004-01-15 |
| WO2002000975A1 (en) | 2002-01-03 |
| NO20026186L (en) | 2002-12-23 |
| AU6712701A (en) | 2002-01-08 |
| EP1299583A1 (en) | 2003-04-09 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FZDE | Discontinued |