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
  • 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 invention relates to a spinning device for carrying out the amine oxide process according to the dry / wet spinning process with a spinneret which has spinning holes for extruding filaments, a container with spinning bath liquid, a bundling element which is provided in the spinning bath liquid for bundling the extruded filaments, and an air gap , which is defined as the distance of the spinneret to the surface of the spinning bath liquid.
• the technique of dry / wet spinning is very generally that spinning mass by a molding tool, e.g. a spinneret, in a medium which does not precipitate for the spinning mass, e.g. Air or an inert gas is extruded, wherein if a spinneret is used, filaments are formed which are stretched in this medium and then passed into a spinning bath liquid (coagulation bath) in which the filaments coagulate.
• a molding tool e.g. a spinneret
• a medium which does not precipitate for the spinning mass e.g. Air or an inert gas
• the amine oxide process is generally understood to mean the production of cellulosic moldings using tertiary amine oxides.
• Cellulose is dissolved in a mixture of a tertiary amine oxide and water, the solution is shaped with a molding tool and passed through an aqueous precipitation bath in which the cellulose is precipitated.
• N-Methylmorpholine-N-oxide (NMMO) is primarily used as the amine oxide.
• Other amine oxides are e.g. in EP-A - 0 553 070.
• a method of making moldable cellulose solutions is e.g. known from EP-A-0 356 419.
• the implementation of the amine oxide process using the dry / wet spinning process is known, for example, from DE-A-29 13 589.
• a solution of cellulose in a tertiary amine oxide is shaped in the warm state and the shaped solution by a gaseous medium ( Air) is introduced into the precipitation bath in order to precipitate the cellulose contained, the warm, shaped solution being cooled before being introduced into the precipitation bath.
• the cooling is carried out immediately after molding and preferably consists of blowing the cellulosic molding horizontally with air.
• the method according to the invention allows the cellulose solution to be spun with a high thread density without the spun threads sticking together after exiting the spinneret.
• DD-A-218 121 also relates to a dry / wet spinning process for producing cellulosic fibers from cellulose solutions in tertiary amine oxides. According to this method, too, the cellulose solution is spun in an air gap, that is the distance between the spinneret and the surface of the spinning bath liquid, and is drawn into an aqueous precipitation bath.
• DD-A-218 121 mentions that the air gap can be shortened without adverse consequences for spinning safety if a polyalkylene ether is added to the cellulose solution before spinning. A small air gap is advantageous because the risk of the freshly extruded filaments sticking together is reduced.
• EP-A-0 574 870 describes a dry / wet spinning process for processing solutions of cellulose in tertiary amine oxides and points out the advantage of a small air gap. With this spinning process it is possible, according to the description in the description of this patent application, to spin with a small air gap and with a high number of spinning bores per unit area. Despite these requirements, there should be no sticking of the Filaments are coming. It is recommended that the spun filaments come into contact with the spinning bath liquid in a spinning funnel. Spinning bath liquid is passed through this spinning funnel in cocurrent with the filaments. The axis of the spinning funnel is substantially perpendicular to the plane of the spinneret, and the flow of the spinning bath liquid is directed from top to bottom, the flow generally being caused by the free fall of the spinning bath liquid.
• the warping or drawing of the freshly extruded filaments is achieved in accordance with EP-A-0 574 870 in such a way that the filaments are essentially accelerated to their take-off speed by the spinning bath liquid flowing through the spinning funnel.
• This known spinning device has the disadvantage that the funnel tube of the spinning funnel, due to its relatively narrow diameter, places an upper limit on the filament bundle to be carried out with regard to its overall cross section, which is additionally set unsatisfactorily low for large-scale implementation of the method.
• the funnel tube of the spinning funnel due to its relatively narrow diameter, places an upper limit on the filament bundle to be carried out with regard to its overall cross section, which is additionally set unsatisfactorily low for large-scale implementation of the method.
• a diameter of 6 mm as is exemplified in EP-A-0 574 870, it is only possible to pass a bundle of filaments consisting of a maximum of 100 filaments through the funnel, as well Spin bath liquid must be transported through the funnel. This in turn means that when using such a spinning funnel, only one spinneret with a maximum of 100 spinning holes can be used.
• the funnel tube must be correspondingly larger, which in turn means that much more spinning bath liquid drains and must be circulated. This high throughput of spin bath liquid leads to turbulent flows in the spin bath, which disrupts the dry / wet spinning process.
• GB-A-1,017,855 describes a device for dry / wet spinning of synthetic polymers.
• the use of a spinning funnel is recommended, through which spinning bath liquid is allowed to flow in cocurrent with the extruded fibers.
• the spinneret is about 0.5 cm above the surface of the spin bath.
• Another measure of the spinnability is the length of time during which one can spin without spinning errors that require technical assistance. Furthermore, even when using spinnerets with a high hole density, the freshly extruded filaments should not stick together in the air gap and the titer should be as constant as possible (small titer fluctuations).
• the spinning device according to the invention for carrying out the amine oxide process according to the dry / wet spinning process with a spinneret, which spinning holes for extruding
• Filaments can be cooled immediately after they have left the spinning holes, a container with spinning bath liquid,
• a bundling element which is provided in the spinning bath liquid for bundling the extruded filaments, and an air gap, which is defined as the distance of the spinneret from the surface of the spinning bath liquid, is characterized in that the bundling element is at a distance from the spinneret such that the angle () that the filaments form perpendicular to the surface of the spinning bath liquid is a maximum of 45 * , and that the relationship
• d Q is the distance (mm) between a spinning hole and its respective adjacent spinning hole on the spinneret
• h is the distance (mm) of the bundling element to the spinneret
• 1 is the air gap (mm)
• the object of the invention can be achieved if the spinning device used is designed in such a way that the above two criteria (angle ⁇ maximum 45 * and the fulfillment of the above inequalities) are met.
• angle ⁇ maximum 45 * and the fulfillment of the above inequalities are met.
• a preferred embodiment of the spinning device according to the invention is characterized in that the bundling element is designed as a deflection element which the filaments are not only bundled, but also redirected.
• the deflecting element is designed such that it does not rotate when the filaments are deflected. According to this embodiment, no rotatable roller or roller is therefore provided as the deflection element. This ensures that torn filaments are not wound on the deflecting element. This makes it easier to carry out the amine oxide process.
• a further preferred embodiment of the spinning device according to the invention is characterized in that the angle ⁇ does not exceed 20 ". It has been shown that it is very important for the spinning safety in the dry / wet spinning process that the draft angle ⁇ in the air gap is as small as possible and preferably does not exceed 20 * , thus minimizing the risk of the filaments sticking in the space between the spinneret and the surface of the spinning bath and increasing the spinning safety.
• the invention also relates to a spinning device for carrying out the amine oxide process by the dry / wet spinning process with a spinneret, which spinning holes for extruding
• Filaments can be cooled immediately after they have left the spinning holes, a container with spinning bath liquid, a deflection element which is provided in the spinning bath liquid for bundling and deflecting the extruded filaments, and an air gap which is the distance from the spinneret to
• Spin bath liquid is defined. which is characterized in that the deflecting element is designed such that it does not rotate when the filaments are deflected.
• spinneret has: an essentially rotationally symmetrical design
• Nozzle body that has a feeder at its center
• Cooling an annular filament sheet by blowing with cooling air is known from WO 95/04173 by the applicant.
• a further preferred embodiment of the spinning device according to the invention is that the container containing the spinning bath liquid is connected to a lifting device with which the container can be moved towards and away from the spinneret in the vertical direction, whereby the distance 1 is changed, and that the bundling element is arranged so that the distance h remains constant despite this movement.
• FIG. 1 denotes a container for holding spinning bath liquid, the surface of the spinning bath liquid being indicated by la.
• spinning mass is extruded through the spinneret 3 and the extruded filaments 4, 5 are drawn off via the air gap 1 into the spinning bath liquid in which they coagulate.
• the deflection element 2 which is a non-rotatable, cylindrical rod, the coagulated filaments are bundled, deflected and pulled off obliquely upwards.
• the distance between the underside of the spinneret 3 and the surface la of the spinning bath liquid is defined as the air gap 1.
• the angle defined above, which the filaments form perpendicular to the surface of the spinning bath liquid, is denoted by ⁇ .
• the reference numeral 4 denotes a filament which comes from a spinning hole which is located on the outer edge of a circular ring formed by the spinning holes in the spinneret 3, i. is the radius (mm) of the circle, which limits the circular ring formed by the spinning holes to the outside.
• d Q the distance of this spinning hole to its neighboring spinning hole 5 is designated, whereby the distance between the respective centers of the two neighboring spinning holes is meant.
• h is the distance between the deflecting element 2 and the spinneret 7, and 1 is the air gap.
• the container 1 stands on a lifting device (not shown) with which the container 1 moves vertically and the size of the air gap 1 can thereby be changed in a simple manner.
• Figure 2 essentially shows the spinning device of Figure
• the non-rotatable deflection element 2 is connected via a rigid arm 6 to a fixed element 7, which is not connected to the container 1, so that the element 7 is not moved when the container 1 is raised or lowered.
• the element 7 can be a wall, for example.
• Two positions of the container 1 are shown in FIG. 2, the lower position being indicated by dashed lines.
• the device for lifting and lowering the container 1 is not shown. It is clear from FIG. 2 that the air gap can be shortened or lengthened by raising and lowering the container 1, the distance h remaining the same at the same time.
• FIG. 3 shows a further embodiment of the spinning device according to the invention.
• the deflection element 2 is anchored to the floor 8 by means of a rigid arm 9.
• the arm 9 protrudes through a corresponding opening
• a jacket 10 is provided for sealing, which is simply pushed together when the container 1 is lowered by means of a device, not shown.
• Example 1 documents the advantageous effect of a non-rotatable deflection element on the spinnability.
• a spinning device was used which essentially corresponded to FIG. 1, but a spinning funnel according to EP-A-0 574 870 was used as the bundling element.
• the spinneret used was that described in WO 95/04173, the disclosure of which is incorporated by reference.
• This previously known spinneret (number of holes: 3960; hole diameter: 100 ⁇ m; outer diameter of the nozzle (outermost row of holes) d .: 145 mm) has an essentially rotationally symmetrical nozzle body, which has a supply for cooling gas, a supply for cellulose solutions (13, 5% cellulose; temp .: 120 "C), an annular, deep-drawn spinning insert made of precious metal with spinning holes, which spinning insert is trough-shaped in cross-section, and has a baffle plate for directing a cooling gas stream onto cellulose filaments which are extruded from the spinning holes (output: 0.025 g / min), so that the cooling gas flow (24 m 3 / h) hits the extruded cellulose filaments essentially perpendicularly.
• the spinning holes are essentially uniformly spaced apart from one another in the spinning insert (hole-hole spacing d Q : 1000 / im) had a length of 15 mm.
• the air in the air gap had a temperature of 24.5'C and a water hold 4.5 g water / kg air.
• Table 1 shows that up to an angle of approx. 40 *, no reduction in the final take-off speed and therefore no deterioration in the spinnability can be observed. From an angle of 45 * , however, the maximum final withdrawal speed is significantly reduced. At an angle of around 61 * , the solution is no longer spinnable.
• a spinning device was used which corresponded to FIG. 2, and the spinning nozzle used was again the one described schematically in WO 95/04173 (number of holes: 28,392; hole diameter: 100 ⁇ m; outer diameter of the nozzle (outermost row of holes)): 155 mm; hole-hole spacing d_: 500 ⁇ m).
• the cellulose solution used had 13.5% cellulose and had a temperature of 120 * C.
• the output was 0.025 g / min.
• the air gap 1 had a length of 20 mm.
• the air in the air gap had a temperature of 12 * C and a water content of 5 g water / kg air.
• the filaments were deflected on a cylindrical, non-rotatable rod 2 and pulled obliquely upwards out of the spinning bath.
• Example 2 The same spinning device was used as described in Example 2, but the air gap 1 was set constant at 30 mm. The distance h was again varied. On the basis of the occurrence of spinning defects (filament tears, extreme sticking of the filaments to one another), the spinning security of the solution was characterized under the specified conditions.
• a high level of spinning security is given if practically no spinning defects occur in a period of more than 15 minutes. If spinning errors occur in a period of 15 minutes or before, spinning on a technical scale is only possible with constant technical assistance.
• the spinning safety is characterized by a time specification, the specification "> 15 min” in Table 3 below meaning that good spinnability (practically no spinning defects within 15 minutes) was given.
• An indication of e.g. " ⁇ 10 min” means that massive spinning errors occur before 10 minutes after the start of spinning, which force the spinning to be interrupted.
• Rotationally symmetrical, rotatable deflection elements of various designs were tested.
• filaments are wound up in the deflection roller within a short time.
• the cause of the winding is apparently that there are sometimes individual thread breaks in the spinning bath, which are caught by a rotating deflection roller, are carried by the deflection roller and lead to ever larger windings by carrying other filaments.
• the spun filaments are damaged because the filaments wound on the deflection roller have to be removed again by mechanical intervention, which leads to a deterioration in the end product.

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Mechanical Engineering (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
• Artificial Filaments (AREA)
• Inorganic Fibers (AREA)

Priority Applications (21)

Applications Claiming Priority (2)

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Cited By (8)

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Citations (7)

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• 1994
  • 1994-12-22 AT AT0239194A patent/ATA239194A/de not_active Application Discontinuation
• 1995
  • 1995-11-27 JP JP8520070A patent/JPH09509704A/ja not_active Ceased
  • 1995-11-27 HU HU9602257A patent/HU220328B/hu not_active IP Right Cessation
  • 1995-11-27 CZ CZ19962305A patent/CZ288127B6/cs not_active IP Right Cessation
  • 1995-11-27 DE DE59510336T patent/DE59510336D1/de not_active Expired - Fee Related
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  • 1995-11-27 WO PCT/AT1995/000229 patent/WO1996020300A2/de active IP Right Grant
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  • 1995-11-27 AU AU38632/95A patent/AU703733B2/en not_active Ceased
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  • 1995-12-19 CA CA002183230A patent/CA2183230A1/en not_active Abandoned
  • 1995-12-19 WO PCT/AT1995/000244 patent/WO1996019598A2/de active IP Right Grant
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  • 1995-12-19 AT AT95940073T patent/ATE166677T1/de active
  • 1995-12-19 AT AT0902195A patent/ATA902195A/de not_active Application Discontinuation
  • 1995-12-19 EP EP95940073A patent/EP0746641B1/de not_active Expired - Lifetime
  • 1995-12-19 JP JP8519353A patent/JPH09509703A/ja active Pending
  • 1995-12-19 EP EP97119866A patent/EP0832995A3/de not_active Withdrawn
  • 1995-12-19 GB GB9617016A patent/GB2301060A/en not_active Withdrawn
  • 1995-12-19 CN CN95192617A patent/CN1146218A/zh active Pending
  • 1995-12-19 DE DE59502340T patent/DE59502340D1/de not_active Expired - Fee Related
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• 1996
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  • 1996-08-21 FI FI963269A patent/FI963269A0/fi not_active IP Right Cessation
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• 1998
  • 1998-09-28 HK HK98111006A patent/HK1010401A1/xx not_active IP Right Cessation
• 2000
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