CN1180142C - Method for producing cellulose fibers - Google Patents
Method for producing cellulose fibers Download PDFInfo
- Publication number
- CN1180142C CN1180142C CNB018118291A CN01811829A CN1180142C CN 1180142 C CN1180142 C CN 1180142C CN B018118291 A CNB018118291 A CN B018118291A CN 01811829 A CN01811829 A CN 01811829A CN 1180142 C CN1180142 C CN 1180142C
- Authority
- CN
- China
- Prior art keywords
- air
- temperature
- fiber
- spinning
- cellulose
- 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 - Fee Related
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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
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (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 DEG C < T < 90 DEG C.
Description
The present invention relates to the method that a kind of claim 1 is summarized.
The method of this kind produce cellulose fibers is referred to as " amine oxide method " or " Lyocell method ".
" Lyocell " be BISFA (BISFA) authorize those by with cellulose dissolution in a kind of organic solvent but without the stage that generates derivative, and extrude the generic name of the fibrid cellulose fiber that fiber produces by this solution.So-called " organic solvent ", the mixture that is understood to include organic compound and water is interior.This kind fiber also claims " solvent spinning fibre ".As organic solvent, on commercial scale, use N-methylmorpholine-N-oxide at present.
Known, the performance of Lyocell fiber and the stability of spinning technique thereof are subjected to the condition effect in the so-called air-gap between spinneret and the coagulating bath liquid level to a great extent.
For example, learn a kind of method of after shaping, cooling off the tow of extruding immediately with one air-flow from PCT-WO 93/19230.Hereinafter, this air-flow is referred to as " cooling air ".In the embodiment of PCT-WO 93/19230, the temperature of cooling air is-6 ℃～24 ℃.
PCT-WO 94/28218 describes the method among a kind of PCT-WO of being similar to 93/19230.According to the document, the temperature of cooling air is maintained at and is lower than 50 ℃.
Learn a kind of method from PCT-WO 95/02082, by this method, the humidity of air should be maintained within a certain range according to certain mathematic(al) representation in orifice diameter, every hole spinning quality output, filament number, air-gap width and the air-gap.In the embodiment of PCT-WO 95/02082, do not provide the information of cooling air temperature.Only usually point out temperature between 10 ℃～60 ℃ at declaratives, preferably between 20 ℃～40 ℃.
PCT-WO 96/17118 relates to the water capacity of cooling off air.The highest cooling air temperature that provides in the document is about 40 ℃.
According to PCT-WO 96/21758, the temperature of cooling air can be between 0 ℃～40 ℃.In PCT-WO 97/38153, the temperature of cooling air be it is said-10 ℃～50 ℃.
PCT-WO 98/58103 describes, and is having under the situation of extruding silk in a large number,, when the spinneret that uses has a large amount of spinneret orifice, will produce very moist atmosphere in air-gap that is.For guarantee spinning process under such condition, also keep stable, PCT-WO 98/58103 suggestion, spinning solution should comprise a kind of cellulose and/or another kind of polymer with higher molecular weight of special ratios before being about to spinning.
The existing problem of spinning fibre cellulose solution in NMMO is, has under the full-bodied situation at solution, and spinning solution must spinning under the temperature that improves.The high viscosity of spinning solution appears at, and for example, when cellulose concentration is high in the solution, and that this considers that from angle of economy yes is desirable.When the pulp that high viscosity also appears at use has at high proportion macromolecule (amount) cellulose.
Yet the temperature of spinning solution when the spinning fiber number is little, for example, during less than the fiber of 1 dtex (dtex), also must maintain high level.Under the situation of this kind fiber, the tow in the air-gap must be drawing to extra high degree.If do not improve the spinning solution temperature, this moment spinning solution viscosity for realizing this kind drawing-off also with too high.
Generally speaking, spinning duration, the temperature of spinning solution should be between 80 ℃～120 ℃, especially 100 ℃～120 ℃.But, therefore do not wish to improve the temperature of cellulose solution in view of the solution of cellulose in NMMO is heat-labile and is tending towards taking place exothermal decomposition reactions.
The present invention also aims to provide a kind of method that belongs to this generic name category, by this method, full-bodied cellulose solution spinning preferably and can produce little Denier fiber preferably.
This purpose is achieved in that promptly, and the temperature (T) of cooling air meets 60 ℃＜T＜90 ℃ before contacting with tow.
Surprisingly, prove that during the cooling air of the higher temperature in adopting the scope of temperature in claim 1, the cellulose solution of viscosity higher is spinning well also, not necessarily will improve the temperature of spinning solution.Such as the yet spinning well of little Denier fiber of 0.9 dtex, do not need to improve the temperature of spinning solution.
In addition, compare, adopt the fiber of higher temperature cooling air production to have higher-strength numerical value with the fiber that adopts lower temperature cooling air under same spinning solution temperature, to produce.
Preferably, the water capacity of this cooling air is between 4g water/kg air～15g water/kg air.
Particularly, the inventive method is fit to the fiber of production fiber number less than 1 dtex.
Example 1:
Have in employing under the cooling conditions of air of different temperatures, have 15wt% cellulose (pulp: Cellunier F, manufacturer: Rayonnier), the spinning solution of 10wt% water and 75wt%NMMO is spun into fiber.
Measure the minimum fiber fiber number that can produce separately: for this reason, by improving hauling speed breaks end to determine fiber until fiber maximum hauling speed (m/min).Write down this speed and calculate fiber number according to the computational methods of describing among the PCT-WO 98/58103 with it.
And then, determine following intensity of spinning fiber of conditioning state respectively.
| The spinning solution temperature (℃) | Cooling air temperature (℃) | Lowest Denier (dtex) | Conditioning state strength (cN/ dtex) |
| 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 |
Be clear that from table be higher than under 60 ℃ the cooling air temperature, minimum obtainable fiber number reduces greatly.Have, fibre strength obviously improves again.
Example 2:
Borregaard LVU), the spinning solution of 9.5wt% water and 75.9wt%NMMO is spun into the fiber of fiber number 1.3 dtexs in continuous experimental apparatus has 14.6wt% cellulose (pulp:.Adopting under the different cooling air temperature conditions, which kind of spinning material temperature measures needs to produce the fiber with this fiber number, and unlikely interference production process.
| Cooling air temperature (℃) | The spinning material temperature that requires (℃) |
| 22 | 116 |
| 65 | 109 |
From table, be clear that, when to adopt temperature be 65 ℃ cooling air, might be under much lower spinning solution temperature producd fibers.
Example 3:
Western Pulp), the spinning solution of 10wt% water and 75wt%NMMO is spun into fiber have in employing under the cooling conditions of air of different temperatures, have 15wt% cellulose (pulp: Alicell VLV, manufacturer:.Described in example 1, determine the minimum fibre number of producing and spin the intensity of fiber under the conditioning state:
| The spinning solution temperature (℃) | Cooling air temperature (℃) | Lowest Denier (dtex) | Conditioning state strength (cN/ dtex) |
| 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 table, be clear that, when adopting the cooling air of higher temperature, might produce the fiber of fiber number well less than 1 dtex.
Claims (4)
1. the method for a produce cellulose fibers, comprise: the solution of cellulose in tertiary amino oxides is extruded by the spinneret orifice of spinneret, the tow of extruding is introduced in the coagulating bath through air-gap under traction, tow is exposed in air-gap in one air-flow, it is characterized in that the temperature T of gas meets 60 ℃＜T＜90 ℃ before contacting with tow.
2. the method for claim 1 is characterized in that, this gas is air.
3. the method for claim 2 is characterized in that, the water capacity of moving air is between 4g water/kg air～15g water/kg air.
4. the method for any one in the claim 1～3 is characterized in that, produces the silk of fiber number less than 1 dtex.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ATA1121/2000 | 2000-06-29 | ||
| AT0112100A AT408355B (en) | 2000-06-29 | 2000-06-29 | Process for producing cellulosic fibres |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1439065A CN1439065A (en) | 2003-08-27 |
| CN1180142C true CN1180142C (en) | 2004-12-15 |
Family
ID=3685802
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB018118291A Expired - Fee Related CN1180142C (en) | 2000-06-29 | 2001-06-28 | Method for producing cellulose fibers |
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) | AU2001267127B2 (en) |
| BR (1) | BR0112036A (en) |
| CA (1) | CA2413706A1 (en) |
| DE (1) | DE50102613D1 (en) |
| NO (1) | NO20026186D0 (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 |
| WO2018156352A1 (en) | 2017-02-21 | 2018-08-30 | 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 |
| DE59502659D1 (en) * | 1994-12-02 | 1998-07-30 | Akzo Nobel Nv | METHOD FOR PRODUCING CELLULOSIC SHAPED BODIES AND A YARN FROM CELLULOSIC FILAMENTS |
| US6210801B1 (en) * | 1996-08-23 | 2001-04-03 | Weyerhaeuser Company | Lyocell fibers, and compositions for making same |
| US6221487B1 (en) * | 1996-08-23 | 2001-04-24 | The Weyerhauser Company | Lyocell fibers having enhanced CV properties |
| 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 EP EP01944725A patent/EP1299583B1/en not_active Expired - Lifetime
- 2001-06-28 JP JP2002506280A patent/JP2004501296A/en not_active Abandoned
- 2001-06-28 CA CA002413706A patent/CA2413706A1/en not_active Abandoned
- 2001-06-28 AU AU2001267127A patent/AU2001267127B2/en not_active Ceased
- 2001-06-28 WO PCT/AT2001/000212 patent/WO2002000975A1/en active IP Right Grant
- 2001-06-28 AU AU6712701A patent/AU6712701A/en active Pending
- 2001-06-28 DE DE50102613T patent/DE50102613D1/en not_active Expired - Fee Related
- 2001-06-28 TR TR2004/01926T patent/TR200401926T4/en unknown
- 2001-06-28 CN CNB018118291A patent/CN1180142C/en not_active Expired - Fee Related
- 2001-06-28 BR BR0112036-0A patent/BR0112036A/en not_active IP Right Cessation
- 2001-06-28 TW TW090115807A patent/TW534932B/en not_active IP Right Cessation
-
2002
- 2002-12-23 NO NO20026186A patent/NO20026186D0/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 |
|---|---|
| CN1439065A (en) | 2003-08-27 |
| WO2002000975A1 (en) | 2002-01-03 |
| DE50102613D1 (en) | 2004-07-22 |
| AU6712701A (en) | 2002-01-08 |
| AU2001267127B2 (en) | 2005-03-24 |
| NO20026186L (en) | 2002-12-23 |
| TW534932B (en) | 2003-06-01 |
| BR0112036A (en) | 2003-05-13 |
| US20030173700A1 (en) | 2003-09-18 |
| EP1299583B1 (en) | 2004-06-16 |
| TR200401926T4 (en) | 2004-09-21 |
| EP1299583A1 (en) | 2003-04-09 |
| ATA11212000A (en) | 2001-03-15 |
| JP2004501296A (en) | 2004-01-15 |
| CA2413706A1 (en) | 2002-12-24 |
| AT408355B (en) | 2001-11-26 |
| NO20026186D0 (en) | 2002-12-23 |
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| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20041215 Termination date: 20190628 |
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| CF01 | Termination of patent right due to non-payment of annual fee |