CA2213221A1 - Process for the production of cellulose fibres and device for carrying out the process - Google Patents
Process for the production of cellulose fibres and device for carrying out the processInfo
- Publication number
- CA2213221A1 CA2213221A1 CA002213221A CA2213221A CA2213221A1 CA 2213221 A1 CA2213221 A1 CA 2213221A1 CA 002213221 A CA002213221 A CA 002213221A CA 2213221 A CA2213221 A CA 2213221A CA 2213221 A1 CA2213221 A1 CA 2213221A1
- Authority
- CA
- Canada
- Prior art keywords
- filaments
- precipitation agent
- cellulose
- process according
- oxide
- 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
- D01D5/06—Wet spinning methods
-
- 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
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
-
- 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)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Abstract
A process for the production of cellulose fibres, wherein a warm solution of cellulose in a tertiary amine-oxide is spun into filaments, which are conducted across an air gap and thereafter contacted with a precipitation agent to precipitate the cellulose, said filaments being drawn off by exerting a force and being stretched in the air gap, which force is exerted by said precipitation agent by making flow said precipitation agent into the direction where said filaments are drawn off and contacting said filaments with said precipitation agent, characterized in that said precipitation agent is made flow, at the point where it is contacted with said filaments, at a rate which is at least as high as the drawing rate of said filaments. The invention is also concerned with a device for carrying out the process (Fig. 2).
Description
~-Z~
PROCESS FOR THE PRODUCTION OF CELLULOSE FIBRES AND DEVICE FOR
CARRYING OUT THE PROCESS
The invention is concerned with a process for the production of cellulose fibres, wherein a warm solution of cellulose in a tertiary amine-oxide is spun into filamehts, which are conducted across an air gap and thereafter contacted with a precipitation agent to precipitate the cellulose, the filaments being drawn off by exerting a force and being stretched in the air gap, which force is exerted by the precipitation agent by making flow the precipitation agent into the direction where the filaments are drawn off and contacting the filaments with the precipitation agent. The invention is also concerned with a device for carrying out the process.
It is known from US-A 2,179,181 that tertiary amine-oxides are capable of dissolving cellulose and that from these solutions cellulose moulded bodies may be obtained by precipitation. A process for the production of such solutions is known for instance from EP-A - 0 356 419. According to this publication, first a suspension of cellulose is prepared in an aqueous tertiary amine-oxide. The amine-oxide contains up to 40% by mass of water. The aqueous cellulose suspension is heated, and while reducing pressure water is withdrawn up to the point allowing the cellulose to dissolve. The process may be carried out in a thin-film treatment apparatus.
From DE-A - 28 44 163 and DD-A - 218 121 it is known that for the production of cellulose fibres or cellulose films an air gap wherein the extruded fibres may be stretched is provided between the spinneret and the precipitation agent. This stretching is necessary, since it is much more difficult to stretch the filaments after contacting the moulded spinning solution with the aqueous precipitation agent. In the precipitation agent, the fibre structure adjusted in the air gap is fixed.
- ' CA 02213221 1997-08-1 In the air gap however there is a risk that the individual filaments not yet coagulated adhere to each other or fuse together due to their extremely high stickiness, thus making fibre spinning impossible. Evidently, the risk of adhereing to each other is the greater the longer the distance between the spinneret plate and the precipitation agent surface (air gap) is. From WO 93/19230 it is known that it is possible to spin a dense filament bundle in a long air gap when the warm, moulded spinning solution is cooled before being introduced into the precipitation agent, cooling being carried out ; mme~ iately after moulding by means of exposing the solution to a cooling gas stream.
From DD-A - 271 534 a spinning method is known, according to which freshly spun filaments are contacted with the precipitation agent which is made flow in the drawing direction of the filaments.
Also from DE-C - 195 12 053 a method for producing cellulose fibres is known, wherein the freshly extruded filaments are introduced into a precipitation liquid l~min~rly flowing at a predetermined rate at about the same direction as the extruded filaments. The filaments are drawn by a spool.
For the purposes of the present specification and the present claims, the term "air" means not only air as such but also any gas or gas mixture which is inert towards the filaments and does not interfere with spinning in any other way.
Therefore, also a gas different from air may be present in the "air gap".
A process of the type described above is known from EP-A - 0 574 870. This process is carried out using a so-called spinning funnel, wherein stretching of the freshly extruded filaments is achieved by means of a liquid, flowing precipitation agent. The flow of the precipitation agent is caused by gravity. In this process it is disadvantageous that only cellulose solutions of relatively low viscosity, having additionally a relatively low cellulose concentration of only 7,8% by mass, 6,1~ by mass and 10,5% by mass respectively, may be spun. From an economical point of view, cellulose concentrations that low are unsatisfactory, since they reduce the capacity of solution production and cause high concentration costs when regenerating the spent precipitation agent.
An economical fibre production achieving a high production capacity however re~uires processing of dopes having a higher cellulose concentration. Moreover, the dope output is to be as high as possible. Such a process however cannot be carried out using the known spinning funnel, since for this purpose it would have to be produced in an inappropriate size.
It is the object of the present invention to further develop a process of the type mentioned above in such a way that a high output may be achieved and highly concentrated, very viscous cellulose solutions may be processed.
The process according to the invention for the production of cellulose fibres, wherein a solution of cellulose in a tertiary amine-oxide is spun into filaments in warm condition, which filaments are conducted across an air gap and thereafter contacted with a precipitation agent to precipitate the cellulose, the filaments being drawn off by exerting a force and being stretched in the air gap, which force is exerted by the precipitation agent by making flow the precipitation agent into the direction where the filaments are drawn off and contacting the filaments with the precipitation agent is characterized in that the precipitation agent, at the point where it is contacted with the filaments, is made flow at a rate which is at least as high as the drawing rate of the filaments and particularly higher than the drawing rate of the filaments.
- ' CA 02213221 1997-08-1~
-By means of the process according to the invention, cellulose solutions having a cellulose concentration of at least 12% by mass, preferably 13-15% by mass, may be advantageously spun.
The invention is based on the finding that it is possible to stretch very viscous cellulose solutions having cellulose concentrations of at least 12% by mass without any mechanical stretching device such as a drawing gallette, i.e.
exclusively by means of the kinetic energy transferred to the filaments by the flowing precipitation agent. For this purpose, the filaments are passed through a so-called injector, whereinto a precipitation agent accelerating the filaments is injected at a pressure being above ambient pressure.
In this process, the drawing rate results in the known manner from the desired titre of the filaments, the concentration of the cellulose solution and the output of the cellulose solution.
The filaments are preferably moistened with the precipitation agent before being contacted with the flowing precipitation agent which exerts on them the force for drawing them off.
The precipitation agent whereby the filaments are moistened may be the same precipitation agent whereby the force for stretching is exerted on the filaments, or it may be a different one.
To allow spinning a dense filament bundle it is convenient to expose the ~ilaments in the air gap to a cooling gas stream, cooling being carried out immediately after spinning. The cooling gas stream may be moist air.
In the process according to the invention, N-methylmorpholine-N-oxide is advantageously used as the tertiary amine-oxide.
The invention is also concerned with a process for the production of a nonwoven, which is characterized in that the cellulose fibres produced according to the invention are laid to a nonwoven which is consolidated.
The nonwoven may be consolidated by treatment with a jet of water. It also may be advantageously consolidated by soaking it with an aqueous solution of a tertiary amine-oxide capable of dissolving cellulose to start to dissolve the cellulose superficially and by subsequently pressing the soaked nonwoven at elevated temperature, whereafter the solution of tertiary amine-oxide is washed out of the pressed nonwoven.
The invention is also concerned with a device for carrying out the process according to the invention, said device comprising: an outlet to receive the precipitation agent and the filaments, a channel connected to the outlet wherein the filaments are conducted, said device being characterized in that the channel leads into an acceleration area wherein the filaments are accelerated using a precipitation agent which is introduced by means of a feeding leading into the acceleration area at a pressure which is higher than atmospheric pressure.
The invention is further concerned with a spinning device comprising a spinneret, a feeding for cooling gas and the device indicated above, for carrying out the amine-oxide process according to the dry/wet-spinning process.
The invention is also concerned with the use of an injector comprising:
- a channel wherein freshly extruded cellulose filaments are conducted, - an acceleration area whereinto the channel leads, so that the filaments may be fed to the acceleration area, and CA 02213221 1997-08-1~
- a feeding for precipitation agents, which feeding leads into the acceleration area so that the precipitation agent may be fed to the acceleration area when producing cellulose filaments according to the dry/wet-spinning process, wherein a solution of cellulose in an aqueous tertiary amine-oxide is moulded into filaments which are stretched in an air gap and afterwards contacted with the precipitation agent.
The invention is explained in more detail by means of the drawing, Figure 1 showing the use according to the invention of an injector for dry/wet-spinning of solutions of cellulose in a tertiary amine-oxide. Figure 2 shows a preferred embodiment of the device according to the invention.
In Figure 1, 1 refers to a heatable (heating not shown) spinneret fed with dope 3, i.e. warm cellulose having a temperature of approximately lOO-C to 120~C, through feeding pipe 2. Pump 4 serves to dose the dope and adjust the pressure necessary for extruding. Filaments 5 extruded from spinneret 1 through spinning holes 16 are cooled using an inert gas 6, pre~erably air, which is directed towards filaments 5 delivered by spinneret 1 by means of gas nozzles 7. By means of exposing the filaments to that gas stream, spinnerets having a high hole density may be used, while the adhesion of the filaments to each other during the spinning process is avoided.
Filaments 5 are introduced into channel 9 of injector 17 and finally reach an acceleration area 10 of injector 17, wherein the filaments are contacted with a precipitation agent which flows rapidly downwards towards diffuser 11, whereby the cellulose is precipitated. At the same time, the filaments are accelerated. The precipitation agent employed for accelerating is pressed into injector 17 by means of feeding pipe 14. Due to the acceleration of the filaments as they approach diffuser 11, the filaments are drawn downwards at a higher rate than they are delivered by spinneret 1, which results in a stretching of the filaments. The stretched filaments are discharged from injector 17 through diffuser 11 and may be deposited for instance on a screen (not shown).
Conducting the filaments through injector 17 is not shown in Figure 1.
In the embodiment of the invention shown in Figure 1, the air gap extends from the bottom of spinneret 1 to the end of channel 9, i.e. the point where channel 9 enters acceleration area 10. The length of channel 9 is not limited and may also be shorter than shown in Figure 1.
Figure 2 shows a preferred embodiment of the device according to the invention. In this Figure, device portions already described in Figure 1 are referred to by the same reference numbers.
Filaments 5 extruded from spinneret 1 are introduced into a device comprising substantially an injector portion 18 whereupon a kind of spinning funnel 19 is placed. The mechanical connection of injector portion 18 with spinning funnel 19 may be established e.g. by means of a screw connection.
Filaments 5 extruded from spinneret 1 reach precipitation agent 15 of spinning funnel 19 across an air gap defined through the distance of the bottom of spinneret 1 from the surface of precipitation agent 15, are conducted through channel 9a and finally reach acceleration area 10 of injector 18, wherein the filaments are accelerated by the precipitation agent which flows rapidly downwards towards diffuser 11. The precipitation agent employed for acceleration is pressed into injector 18 through feeder 14.
Due to the acceleration of the filaments as they approach diffuser 11, the filaments are drawn downwards at a higher rate than they are delivered by spinneret 1, resulting in a stretching of the filaments in the air gap.
CA 02213221 1997-08-1~
In spinning funnel 19 there is a feeding 12 for precipitation agents pumped through channel 13 into cone 8. It should be paid attention to adjust the amounts of precipitation agents fed to spinning funnel 19 through feedings 12 and 14 and discharged from injector 18 through diffuser 11 to each other such that the desired stretching in the air gap is achieved while simultaneously preventing a drop of liquid level 15 and thus a widening of the air gap.
In Figure 2, the surface of precipitation agent 15 is shown level with the upper edge of spinning funnel 19. It is evident to those skilled in the art that this surface may be provided also at a somewhat lower level, in which case the air gap naturally will be correspondingly wider.
By means of the following Examples, the invention is described in more detail.
Example 1 In a heatable and evacuatable stirring vessel, a spinnable cellulose solution having a cellulose content of 12~ (NMMO:
77~; H2O~ ) was produced from sulphite pulp and aqueous NMMO in a way known to those skilled in the art. This solution was extruded into filaments at 130~C from a spinneret having 888 holes (hole diameter: 80 ~m).
The air gap was 22 mm.
Precipitation agent was injected into feeding 14 in an amount of 1008 l/minute. The speed of the precipitation agent at the acceleration area lo at the exit o~ the channel 9a was at about 378 m/minute achieving a stretching and drawing of 9.9.
Achieving a stretching of of 9.9 means that the filaments are drawn off at a rate amounting to 9.9 times the rate whereat the filaments are delivered from the spinneret and enter the -- ' CA 02213221 1997-08-1~
_g_ air gap wherein they are stretched. Thus stretching is defined by:
Rate of final drawing Stretching =
Rate at spinneret outlet The fibres produced had a titre of 1.30 dtex.
Examples 2 - 4 The procedure described in Example 1 was carried out with the exception that the amount of precipitation agent injected per hour and the rate of the precipitation agent given in the following table were employed. The achieved stretching is also given in the table.
Table Precipitation agent Stretching Titre Injection Rate (dtex) Example 2792 l/h 396 m/min 5.3 2.45 Example 3828 l/h ~14 m/min 6.9 1.87 Example 4720 l/h 360 m/min 9.3 1.39 Example 5 The filament bundle produced in Example 2 was allowed to wind on a travelling screen producing a nonwoven having a area weight of 40 g/m2. The liquid permeability of this nonwoven was measured according to the EDANA (European Disposables and Nonwovens Association) Standard 150.2-93 using a LISTER
apparatus (methodology: a determined amount (5 ml) of test liquid (0.9% NaCl solution) is applied to the nonwoven at a constant delivery rate. The time the nonwoven requires to discharge this liquid is electronically measured.) The average of 10 measurements was 1.47 sec.
PROCESS FOR THE PRODUCTION OF CELLULOSE FIBRES AND DEVICE FOR
CARRYING OUT THE PROCESS
The invention is concerned with a process for the production of cellulose fibres, wherein a warm solution of cellulose in a tertiary amine-oxide is spun into filamehts, which are conducted across an air gap and thereafter contacted with a precipitation agent to precipitate the cellulose, the filaments being drawn off by exerting a force and being stretched in the air gap, which force is exerted by the precipitation agent by making flow the precipitation agent into the direction where the filaments are drawn off and contacting the filaments with the precipitation agent. The invention is also concerned with a device for carrying out the process.
It is known from US-A 2,179,181 that tertiary amine-oxides are capable of dissolving cellulose and that from these solutions cellulose moulded bodies may be obtained by precipitation. A process for the production of such solutions is known for instance from EP-A - 0 356 419. According to this publication, first a suspension of cellulose is prepared in an aqueous tertiary amine-oxide. The amine-oxide contains up to 40% by mass of water. The aqueous cellulose suspension is heated, and while reducing pressure water is withdrawn up to the point allowing the cellulose to dissolve. The process may be carried out in a thin-film treatment apparatus.
From DE-A - 28 44 163 and DD-A - 218 121 it is known that for the production of cellulose fibres or cellulose films an air gap wherein the extruded fibres may be stretched is provided between the spinneret and the precipitation agent. This stretching is necessary, since it is much more difficult to stretch the filaments after contacting the moulded spinning solution with the aqueous precipitation agent. In the precipitation agent, the fibre structure adjusted in the air gap is fixed.
- ' CA 02213221 1997-08-1 In the air gap however there is a risk that the individual filaments not yet coagulated adhere to each other or fuse together due to their extremely high stickiness, thus making fibre spinning impossible. Evidently, the risk of adhereing to each other is the greater the longer the distance between the spinneret plate and the precipitation agent surface (air gap) is. From WO 93/19230 it is known that it is possible to spin a dense filament bundle in a long air gap when the warm, moulded spinning solution is cooled before being introduced into the precipitation agent, cooling being carried out ; mme~ iately after moulding by means of exposing the solution to a cooling gas stream.
From DD-A - 271 534 a spinning method is known, according to which freshly spun filaments are contacted with the precipitation agent which is made flow in the drawing direction of the filaments.
Also from DE-C - 195 12 053 a method for producing cellulose fibres is known, wherein the freshly extruded filaments are introduced into a precipitation liquid l~min~rly flowing at a predetermined rate at about the same direction as the extruded filaments. The filaments are drawn by a spool.
For the purposes of the present specification and the present claims, the term "air" means not only air as such but also any gas or gas mixture which is inert towards the filaments and does not interfere with spinning in any other way.
Therefore, also a gas different from air may be present in the "air gap".
A process of the type described above is known from EP-A - 0 574 870. This process is carried out using a so-called spinning funnel, wherein stretching of the freshly extruded filaments is achieved by means of a liquid, flowing precipitation agent. The flow of the precipitation agent is caused by gravity. In this process it is disadvantageous that only cellulose solutions of relatively low viscosity, having additionally a relatively low cellulose concentration of only 7,8% by mass, 6,1~ by mass and 10,5% by mass respectively, may be spun. From an economical point of view, cellulose concentrations that low are unsatisfactory, since they reduce the capacity of solution production and cause high concentration costs when regenerating the spent precipitation agent.
An economical fibre production achieving a high production capacity however re~uires processing of dopes having a higher cellulose concentration. Moreover, the dope output is to be as high as possible. Such a process however cannot be carried out using the known spinning funnel, since for this purpose it would have to be produced in an inappropriate size.
It is the object of the present invention to further develop a process of the type mentioned above in such a way that a high output may be achieved and highly concentrated, very viscous cellulose solutions may be processed.
The process according to the invention for the production of cellulose fibres, wherein a solution of cellulose in a tertiary amine-oxide is spun into filaments in warm condition, which filaments are conducted across an air gap and thereafter contacted with a precipitation agent to precipitate the cellulose, the filaments being drawn off by exerting a force and being stretched in the air gap, which force is exerted by the precipitation agent by making flow the precipitation agent into the direction where the filaments are drawn off and contacting the filaments with the precipitation agent is characterized in that the precipitation agent, at the point where it is contacted with the filaments, is made flow at a rate which is at least as high as the drawing rate of the filaments and particularly higher than the drawing rate of the filaments.
- ' CA 02213221 1997-08-1~
-By means of the process according to the invention, cellulose solutions having a cellulose concentration of at least 12% by mass, preferably 13-15% by mass, may be advantageously spun.
The invention is based on the finding that it is possible to stretch very viscous cellulose solutions having cellulose concentrations of at least 12% by mass without any mechanical stretching device such as a drawing gallette, i.e.
exclusively by means of the kinetic energy transferred to the filaments by the flowing precipitation agent. For this purpose, the filaments are passed through a so-called injector, whereinto a precipitation agent accelerating the filaments is injected at a pressure being above ambient pressure.
In this process, the drawing rate results in the known manner from the desired titre of the filaments, the concentration of the cellulose solution and the output of the cellulose solution.
The filaments are preferably moistened with the precipitation agent before being contacted with the flowing precipitation agent which exerts on them the force for drawing them off.
The precipitation agent whereby the filaments are moistened may be the same precipitation agent whereby the force for stretching is exerted on the filaments, or it may be a different one.
To allow spinning a dense filament bundle it is convenient to expose the ~ilaments in the air gap to a cooling gas stream, cooling being carried out immediately after spinning. The cooling gas stream may be moist air.
In the process according to the invention, N-methylmorpholine-N-oxide is advantageously used as the tertiary amine-oxide.
The invention is also concerned with a process for the production of a nonwoven, which is characterized in that the cellulose fibres produced according to the invention are laid to a nonwoven which is consolidated.
The nonwoven may be consolidated by treatment with a jet of water. It also may be advantageously consolidated by soaking it with an aqueous solution of a tertiary amine-oxide capable of dissolving cellulose to start to dissolve the cellulose superficially and by subsequently pressing the soaked nonwoven at elevated temperature, whereafter the solution of tertiary amine-oxide is washed out of the pressed nonwoven.
The invention is also concerned with a device for carrying out the process according to the invention, said device comprising: an outlet to receive the precipitation agent and the filaments, a channel connected to the outlet wherein the filaments are conducted, said device being characterized in that the channel leads into an acceleration area wherein the filaments are accelerated using a precipitation agent which is introduced by means of a feeding leading into the acceleration area at a pressure which is higher than atmospheric pressure.
The invention is further concerned with a spinning device comprising a spinneret, a feeding for cooling gas and the device indicated above, for carrying out the amine-oxide process according to the dry/wet-spinning process.
The invention is also concerned with the use of an injector comprising:
- a channel wherein freshly extruded cellulose filaments are conducted, - an acceleration area whereinto the channel leads, so that the filaments may be fed to the acceleration area, and CA 02213221 1997-08-1~
- a feeding for precipitation agents, which feeding leads into the acceleration area so that the precipitation agent may be fed to the acceleration area when producing cellulose filaments according to the dry/wet-spinning process, wherein a solution of cellulose in an aqueous tertiary amine-oxide is moulded into filaments which are stretched in an air gap and afterwards contacted with the precipitation agent.
The invention is explained in more detail by means of the drawing, Figure 1 showing the use according to the invention of an injector for dry/wet-spinning of solutions of cellulose in a tertiary amine-oxide. Figure 2 shows a preferred embodiment of the device according to the invention.
In Figure 1, 1 refers to a heatable (heating not shown) spinneret fed with dope 3, i.e. warm cellulose having a temperature of approximately lOO-C to 120~C, through feeding pipe 2. Pump 4 serves to dose the dope and adjust the pressure necessary for extruding. Filaments 5 extruded from spinneret 1 through spinning holes 16 are cooled using an inert gas 6, pre~erably air, which is directed towards filaments 5 delivered by spinneret 1 by means of gas nozzles 7. By means of exposing the filaments to that gas stream, spinnerets having a high hole density may be used, while the adhesion of the filaments to each other during the spinning process is avoided.
Filaments 5 are introduced into channel 9 of injector 17 and finally reach an acceleration area 10 of injector 17, wherein the filaments are contacted with a precipitation agent which flows rapidly downwards towards diffuser 11, whereby the cellulose is precipitated. At the same time, the filaments are accelerated. The precipitation agent employed for accelerating is pressed into injector 17 by means of feeding pipe 14. Due to the acceleration of the filaments as they approach diffuser 11, the filaments are drawn downwards at a higher rate than they are delivered by spinneret 1, which results in a stretching of the filaments. The stretched filaments are discharged from injector 17 through diffuser 11 and may be deposited for instance on a screen (not shown).
Conducting the filaments through injector 17 is not shown in Figure 1.
In the embodiment of the invention shown in Figure 1, the air gap extends from the bottom of spinneret 1 to the end of channel 9, i.e. the point where channel 9 enters acceleration area 10. The length of channel 9 is not limited and may also be shorter than shown in Figure 1.
Figure 2 shows a preferred embodiment of the device according to the invention. In this Figure, device portions already described in Figure 1 are referred to by the same reference numbers.
Filaments 5 extruded from spinneret 1 are introduced into a device comprising substantially an injector portion 18 whereupon a kind of spinning funnel 19 is placed. The mechanical connection of injector portion 18 with spinning funnel 19 may be established e.g. by means of a screw connection.
Filaments 5 extruded from spinneret 1 reach precipitation agent 15 of spinning funnel 19 across an air gap defined through the distance of the bottom of spinneret 1 from the surface of precipitation agent 15, are conducted through channel 9a and finally reach acceleration area 10 of injector 18, wherein the filaments are accelerated by the precipitation agent which flows rapidly downwards towards diffuser 11. The precipitation agent employed for acceleration is pressed into injector 18 through feeder 14.
Due to the acceleration of the filaments as they approach diffuser 11, the filaments are drawn downwards at a higher rate than they are delivered by spinneret 1, resulting in a stretching of the filaments in the air gap.
CA 02213221 1997-08-1~
In spinning funnel 19 there is a feeding 12 for precipitation agents pumped through channel 13 into cone 8. It should be paid attention to adjust the amounts of precipitation agents fed to spinning funnel 19 through feedings 12 and 14 and discharged from injector 18 through diffuser 11 to each other such that the desired stretching in the air gap is achieved while simultaneously preventing a drop of liquid level 15 and thus a widening of the air gap.
In Figure 2, the surface of precipitation agent 15 is shown level with the upper edge of spinning funnel 19. It is evident to those skilled in the art that this surface may be provided also at a somewhat lower level, in which case the air gap naturally will be correspondingly wider.
By means of the following Examples, the invention is described in more detail.
Example 1 In a heatable and evacuatable stirring vessel, a spinnable cellulose solution having a cellulose content of 12~ (NMMO:
77~; H2O~ ) was produced from sulphite pulp and aqueous NMMO in a way known to those skilled in the art. This solution was extruded into filaments at 130~C from a spinneret having 888 holes (hole diameter: 80 ~m).
The air gap was 22 mm.
Precipitation agent was injected into feeding 14 in an amount of 1008 l/minute. The speed of the precipitation agent at the acceleration area lo at the exit o~ the channel 9a was at about 378 m/minute achieving a stretching and drawing of 9.9.
Achieving a stretching of of 9.9 means that the filaments are drawn off at a rate amounting to 9.9 times the rate whereat the filaments are delivered from the spinneret and enter the -- ' CA 02213221 1997-08-1~
_g_ air gap wherein they are stretched. Thus stretching is defined by:
Rate of final drawing Stretching =
Rate at spinneret outlet The fibres produced had a titre of 1.30 dtex.
Examples 2 - 4 The procedure described in Example 1 was carried out with the exception that the amount of precipitation agent injected per hour and the rate of the precipitation agent given in the following table were employed. The achieved stretching is also given in the table.
Table Precipitation agent Stretching Titre Injection Rate (dtex) Example 2792 l/h 396 m/min 5.3 2.45 Example 3828 l/h ~14 m/min 6.9 1.87 Example 4720 l/h 360 m/min 9.3 1.39 Example 5 The filament bundle produced in Example 2 was allowed to wind on a travelling screen producing a nonwoven having a area weight of 40 g/m2. The liquid permeability of this nonwoven was measured according to the EDANA (European Disposables and Nonwovens Association) Standard 150.2-93 using a LISTER
apparatus (methodology: a determined amount (5 ml) of test liquid (0.9% NaCl solution) is applied to the nonwoven at a constant delivery rate. The time the nonwoven requires to discharge this liquid is electronically measured.) The average of 10 measurements was 1.47 sec.
Claims (10)
1. A process for the production of cellulose fibres, wherein a warm solution of cellulose in a tertiary amine-oxide is spun into filaments, which are conducted across an air gap and thereafter contacted with a precipitation agent to precipitate the cellulose, said filaments being drawn off by exerting a force and being stretched in said air gap, which force is exerted by said precipitation agent by making flow said precipitation agent into the direction where said filaments are drawn off and contacting said filaments with said precipitation agent, characterized in that said precipitation agent is made flow, at the point where it is contacted with said filaments, at a rate which is at least as high as and particularly higher than the drawing rate of said filaments.
2. A process according to Claim 1, characterized in that said filaments are moistened with said precipitation agent before being contacted with the flowing precipitation agent exerting upon them the force for drawing them off.
3. A process according to one of the Claims 1 or 2, characterized in that said filaments are cooled in said air gap by exposing them to a cooling gas stream, said cooling being carried out immediately after spinning.
4. A process according to one of the Claims 1 to 3, characterized in that as said tertiary amine-oxide N-methylmorpholine-N-oxide is used.
5. A process according to Claim 4, characterized in that said solution to be spun has a cellulose concentration of at least 12%, preferably 13-15%, by mass.
6. A process for the production of a nonwoven, characterized in that said cellulose fibres produced according to the process according to one or more of the Claims 1 to 5 are laid to a nonwoven which is consolidated.
7. A process according to Claim 6, characterized in that said nonwoven is consolidated by soaking it with an aqueous solution of a tertiary amine-oxide capable of dissolving cellulose to superficially start to dissolve said cellulose and by subsequently pressing said soaked nonwoven at elevated temperature, whereafter said solution of tertiary amine-oxide is washed out of said pressed nonwoven.
8. A device for carrying out the process according to one of the Claims 1 to 7, comprising an outlet (8) to receive the precipitation agent (15) and the filaments (5), a channel (9a) connected to outlet (8) wherein said filaments (5) are conducted, characterized in that said channel (9a) leads into an acceleration area (10) wherein said filaments (5) are accelerated using a precipitation agent which is introduced by means of a feeding (14) leading into said acceleration area (10) at a pressure which is higher than atmospheric pressure.
9. A spinning device for carrying out the process according to the dry/wet-spinning process comprising a spinneret (1), a feeding (7) for cooling gas (6) and a device according to Claim 8.
10. Use of an injector comprising:
- a channel (9) wherein freshly extruded cellulose filaments are conducted, - an acceleration area (10) whereinto channel (9) leads, so that said filaments may be fed to said acceleration area, and - a feeding (14) for precipitation agents, which feeding (14) leads into acceleration area (10) so that said precipitation agent may be fed to acceleration area (10) when producing cellulose filaments according to the dry/wet-spinning process, wherein a solution of cellulose in an aqueous tertiary amine-oxide is moulded into filaments which are stretched in an air gap and afterwards contacted with a precipitation agent.
- a channel (9) wherein freshly extruded cellulose filaments are conducted, - an acceleration area (10) whereinto channel (9) leads, so that said filaments may be fed to said acceleration area, and - a feeding (14) for precipitation agents, which feeding (14) leads into acceleration area (10) so that said precipitation agent may be fed to acceleration area (10) when producing cellulose filaments according to the dry/wet-spinning process, wherein a solution of cellulose in an aqueous tertiary amine-oxide is moulded into filaments which are stretched in an air gap and afterwards contacted with a precipitation agent.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ATA2107/95 | 1995-12-27 | ||
| AT0210795A AT402947B (en) | 1995-12-27 | 1995-12-27 | METHOD FOR PRODUCING CELLULOSIC FIBERS AND DEVICE FOR IMPLEMENTING THE METHOD |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2213221A1 true CA2213221A1 (en) | 1997-07-10 |
Family
ID=3527917
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002213221A Abandoned CA2213221A1 (en) | 1995-12-27 | 1996-12-20 | Process for the production of cellulose fibres and device for carrying out the process |
Country Status (11)
| Country | Link |
|---|---|
| EP (1) | EP0811087B1 (en) |
| JP (1) | JPH11501371A (en) |
| CN (1) | CN1181788A (en) |
| AT (2) | AT402947B (en) |
| AU (1) | AU1185797A (en) |
| BR (1) | BR9607047A (en) |
| CA (1) | CA2213221A1 (en) |
| DE (1) | DE59601184D1 (en) |
| ES (1) | ES2129992T3 (en) |
| NO (1) | NO973763L (en) |
| WO (1) | WO1997024476A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116334778A (en) * | 2023-05-26 | 2023-06-27 | 吉林富博纤维研究院有限公司 | Preparation method of high-performance PAN-based carbon fiber precursor |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6235392B1 (en) | 1996-08-23 | 2001-05-22 | Weyerhaeuser Company | Lyocell fibers and process for their preparation |
| US6221487B1 (en) | 1996-08-23 | 2001-04-24 | The Weyerhauser Company | Lyocell fibers having enhanced CV properties |
| CN1061106C (en) * | 1997-12-09 | 2001-01-24 | 宜宾丝丽雅集团有限公司 | Method for producing cellulose fiber by dissolvant method |
| AT406386B (en) | 1998-07-28 | 2000-04-25 | Chemiefaser Lenzing Ag | METHOD AND DEVICE FOR PRODUCING CELLULOSIC MOLDED BODIES |
| DE10025230A1 (en) * | 2000-05-22 | 2000-11-02 | Lurgi Zimmer Ag | Extrusion of continuous filaments or film from a solution of water with cellulose and a tertiary amine oxide has a structured air drawing action in the air gap after the extrusion channel to increase the material strength |
| DE10025231A1 (en) | 2000-05-22 | 2000-11-02 | Lurgi Zimmer Ag | Extrusion of continuous filaments or film from a solution of water with cellulose and a tertiary amine oxide has a structured air drawing action in the air gap after the extrusion channel to increase the material strength |
| DE10060876B4 (en) * | 2000-12-07 | 2006-03-09 | Zimmer Ag | Precipitation device for a spinning plant |
| JP4593370B2 (en) * | 2005-06-02 | 2010-12-08 | 帝人テクノプロダクツ株式会社 | Dry and wet spinning equipment |
| US20090312731A1 (en) * | 2006-04-28 | 2009-12-17 | Lenzing Aktiengesellschaft | Nonwoven Melt-Blown Product |
| AT503625B1 (en) | 2006-04-28 | 2013-10-15 | Chemiefaser Lenzing Ag | WATER-IRRADIZED PRODUCT CONTAINING CELLULASIC FIBERS |
| ES2625035B1 (en) * | 2015-12-18 | 2018-06-21 | Universidad De Extremadura | PRODUCTION OF VISCOELASTIC CAPILLARY JETS BY GASEOUS FOCUS |
| EP3470557A1 (en) * | 2017-10-12 | 2019-04-17 | Lenzing Aktiengesellschaft | Spinning device and method for stringing up in a spinning device |
| CN110424423B (en) * | 2019-08-22 | 2022-02-08 | 深圳市如茵生态环境建设有限公司 | Fiber spinning system |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT962284B (en) * | 1971-08-30 | 1973-12-20 | Asahi Chemical Ind | PROCEDURE FOR THE MANUFACTURE OF NON-WOVEN FABRIC WITH CONTINUOUS FILAMENTS WITH THE METHOD OF WET SPINNING UNDER TENSION |
| DD271534B5 (en) * | 1988-04-26 | 2002-07-11 | Thueringisches Inst Textil | Process for the spinning of polymer solutions |
| PL285328A1 (en) * | 1989-05-31 | 1991-01-28 | Chemiefaser Lenzing Ag | Apparatus for and method of expsing fibre cables to treatment with a liquid |
| 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 |
| JPH07268718A (en) * | 1994-03-29 | 1995-10-17 | Asahi Chem Ind Co Ltd | Method for wet spinning regenerated cellulosic fiber |
-
1995
- 1995-12-27 AT AT0210795A patent/AT402947B/en not_active IP Right Cessation
-
1996
- 1996-12-20 AT AT96942981T patent/ATE176011T1/en not_active IP Right Cessation
- 1996-12-20 AU AU11857/97A patent/AU1185797A/en not_active Abandoned
- 1996-12-20 EP EP96942981A patent/EP0811087B1/en not_active Expired - Lifetime
- 1996-12-20 CA CA002213221A patent/CA2213221A1/en not_active Abandoned
- 1996-12-20 CN CN96193341.0A patent/CN1181788A/en active Pending
- 1996-12-20 DE DE59601184T patent/DE59601184D1/en not_active Expired - Fee Related
- 1996-12-20 BR BR9607047A patent/BR9607047A/en not_active Application Discontinuation
- 1996-12-20 ES ES96942981T patent/ES2129992T3/en not_active Expired - Lifetime
- 1996-12-20 JP JP9523913A patent/JPH11501371A/en active Pending
- 1996-12-20 WO PCT/AT1996/000260 patent/WO1997024476A1/en active IP Right Grant
-
1997
- 1997-08-15 NO NO973763A patent/NO973763L/en not_active Application Discontinuation
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116334778A (en) * | 2023-05-26 | 2023-06-27 | 吉林富博纤维研究院有限公司 | Preparation method of high-performance PAN-based carbon fiber precursor |
| CN116334778B (en) * | 2023-05-26 | 2023-07-21 | 吉林富博纤维研究院有限公司 | Preparation method of high-performance PAN-based carbon fiber precursor |
Also Published As
| Publication number | Publication date |
|---|---|
| ATA210795A (en) | 1997-02-15 |
| EP0811087A1 (en) | 1997-12-10 |
| NO973763D0 (en) | 1997-08-15 |
| EP0811087B1 (en) | 1999-01-20 |
| ATE176011T1 (en) | 1999-02-15 |
| BR9607047A (en) | 1997-12-30 |
| WO1997024476A1 (en) | 1997-07-10 |
| NO973763L (en) | 1997-08-15 |
| ES2129992T3 (en) | 1999-06-16 |
| JPH11501371A (en) | 1999-02-02 |
| CN1181788A (en) | 1998-05-13 |
| AU1185797A (en) | 1997-07-28 |
| AT402947B (en) | 1997-09-25 |
| DE59601184D1 (en) | 1999-03-04 |
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Legal Events
| Date | Code | Title | Description |
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| FZDE | Discontinued |