Winding device and winding method

Abstract

The invention relates to a device for solidifying and winding cellulose multifilaments, comprising an extrusion unit with at least 10 openings for forming filaments, a coagulation unit for solidifying the filaments, and a thread winder for winding the cellulose filaments, characterized in that the device contains no or only a partial washing unit for washing the cellulose filaments or for extracting a cellulose solvent from the cellulose filaments between the coagulation unit and the thread winder; and a method for winding cellulose multifilaments.

Description

[0001] The invention relates to a device for the post-treatment of solvent-spun cellulose fibers. background

[0002] Due to the positive properties of cellulose fibers (moisture absorption, breathability, biodegradability), which synthetic fibers cannot adequately match, the demand for both natural and synthetically produced cellulose fibers is expected to continue increasing. Cotton production capacity, in particular, can no longer keep pace with the growing demand, despite the cultivation of cotton hybrids and increased yields. Therefore, alternative, synthetically produced cellulose fibers are needed. The use of cellulose-based fibers is also essential from an ecological perspective. Cotton cultivation requires significant amounts of water and high-quality arable land. Available land is in fierce competition with food production. Lifecycle analyses conclude that the CO₂ footprint of synthetically produced cellulose fibers is significantly lower than that of cotton.Accordingly, the pulp industry has already reacted to the expected increased demand for soluble pulp.

[0003] The production of cellulose fibers is currently based primarily on the viscose process. Due to strict environmental regulations, significant viscose production capacities have been closed in Europe and the United States since the 1980s. From an ecological perspective, it is questionable whether viscose technology should continue to be used for capacity expansion, as the use of large quantities of sulfur compounds and sodium hydroxide leads to hazardous gaseous byproducts that severely pollute the environment.

[0004] Consequently, sulfur-free manufacturing processes were developed and proposed for the production of cellulose fibers. The use of N-methylmorpholine N-oxide (NMMO) monohydrate as a solvent for cellulose was developed as a sulfur-free fiber manufacturing process on a commercial scale and is used to produce so-called lyocell fibers.

[0005] Lyocell as a generic name has been recognized by the BISFA (Bureau for the Standardization of Rayon and Synthetic Fibers, Brussels) and in the USA (by the Federal Trade Commission).

[0006] In the lyocell production process, chemical celluloses are first suspended in an NMMO-water mixture. Subsequently, the water content of the suspension is gradually reduced at elevated temperature and under reduced pressure conditions until the solvent system corresponds to an NMMO monohydrate in which cellulose is soluble.

[0007] Subsequently, spinning solution (typical cellulose concentrations 8-20%) is extruded through an air gap into a coagulation bath, where solvent exchange takes place, resulting in the precipitation of the initially dissolved cellulose as thread-like products.

[0008] In the viscose process, this takes place directly in a coagulation medium (wet spinning). Alternatively, when spinning a lyocell solution (NM-MO-water-cellulose), extrusion can be performed in a gas gap, followed by coagulation. After die extrusion, the extruded continuous filaments pass through a gas gap, allowing the extrudate to remain briefly as a liquid, highly viscous, cooled filament in the air gap. By stretching the continuously spun filaments, the resulting shapes are drawn in the air gap to up to 15 times their original length before they enter the coagulation zone and precipitate (dry-jet-wet spinning). Dry-wet spinning as a lyocell process is described, for example, in US 4246221 A, US 4416698 A, WO 93 / 019230 A1, WO 94 / 028218 A1, WO 97 / 33020 A1, WO 2002 / 012599 A1, WO 2003 / 014436 A1, WO 2003 / 057951 A1, WO 2013 / 030399 A1, WO 2013 / 030400 A1, WO 2014 / 057022 A1, WO 2020 / 043860 A1.

[0009] The lyocell process typically uses tertiary amine oxides, such as N-methylmorpholine N-oxide (NMMO), or ionic solubilizers ("ionic liquids", US 6824599, DE 102004031025) as solvents to dissolve the cellulose. Since the solvent is expensive, attempts are made to recover it from the spinning process and, in particular, in a downstream washing process (WO 2020 / 234330 A1).

[0010] Due to the high solvent recovery rates required for process efficiency, improving energy efficiency is crucial and presents a constant challenge for solvent recovery, particularly during the washing process. This applies to the Lyocell process as well as to processes using ionic liquids for dissolving and spinning cellulose. Problems can arise if the process parameters of fiber filament washing are not precisely controlled, as yarn irregularities resulting from increased solvent and degradation residues in the filament yarns can lead to quality defects such as uneven whiteness and varying dyeing behavior due to impurities.

[0011] The production of lyocell filaments is generally a continuous process involving several steps, as described, for example, in EP 1500724 B1: (A) dissolving cellulose in a solvent mixture, (B) extruding the spinning solution through a spinneret, followed by passing through an air gap and then coagulating the spinning solution in a coagulation bath to obtain a multifilament (dry-jet-wet spinning), (C) washing out the solvent through an aqueous water wash bath, (D) continuously treating the multifilament through an oil treatment device and through a swirling nozzle, and (E) drying and then winding.

[0012] In EP 1657327 A1, the continuously produced cellulose multifilaments are also subjected to a water wash to remove the solvent. During the filament production process, a specific temperature control of the coagulation or spinning bath is maintained to ensure complete removal of the solvent NMMO during the washing process. Optimal washing temperatures for the fiber washing are approximately 35°C. After washing with water, the multifilaments are continuously dried using a drying roller. The washed, dried, and post-treated filaments are then wound onto reels.

[0013] Solvent recovery in a washing process following wet-dry spinning is described in greater detail in US 2013 / 0101843 A1, US 2011 / 0252762 A1, and EP 3467161 A1. After spinning, the cellulose filaments are continuously fed over several rollers and washed. The filaments are then fed over several rollers into a dryer, where multi-stage drying takes place. The dry cellulose filaments are finally wound onto reels. According to EP 3467161 A1, washing the filaments to remove the solvent is performed using driven rollers sprayed with washing fluid. Drying the filaments is achieved using a multitude of drum dryers arranged with differently set and controlled drum speeds to ensure that filament elongation is kept low and constant during the drying process to prevent filament damage.

[0014] The post-processing of commercially usable cellulose filaments and yarns requires careful washing and drying, during which the forces acting on the tensile filaments and the washing and drying conditions are precisely controlled. Commercially usable cellulose filaments should be free of filament damage, homogeneous in structure and chemical composition, and easily post-processed (e.g., uniformly dyeable). The washing process, in particular, is a costly procedure to recover the (expensive) solvent.

[0015] EP3467161A1 states that the fragile filament structure must be handled very gently throughout all process steps. The stresses and forces acting on the filament during the entire manufacturing process must be avoided or significantly minimized to prevent breakage or damage. The need for sufficiently long washing cycles, combined with the high thread speeds required for efficient operation, results in relatively long washing cycles in serial production. To ensure gentle filament handling, correspondingly elaborate precautions must be taken. Insufficient protective measures will lead to quality limitations. Insufficiently long washing cycles result in residual solvents remaining in the filament, which also negatively impacts quality.

[0016] Therefore, there is a need for more cost-effective methods to obtain cellulose filaments and yarns suitable for commercial use. Summary of the invention

[0017] The present invention relates to a device for solidifying and winding cellulose multifilaments, comprising a spinning unit (with an extrusion unit having at least 10 openings for forming filaments and a coagulation unit for solidifying the filaments) and a thread winder for winding the cellulose filaments, characterized in that the device contains no or only a partial washing unit for washing the cellulose filaments or for extracting a cellulose solvent from the cellulose filaments between the coagulation unit and the thread winder.

[0018] The invention further relates to a method for the production and processing of cellulose filaments comprising a spinning process (dry-wet spinning process or wet spinning process) for the production of cellulose filaments, wherein the cellulose filaments contain cellulose solvents, optionally partial washing of the cellulose filaments or optionally partial extraction of a cellulose solvent from the cellulose filaments, whereby the solvent content of the cellulose filaments is reduced and the cellulose filaments remain moist, and winding of the washed and moist cellulose filaments.

[0019] Furthermore, the invention relates to a method for the production and processing of cellulose multifilaments, comprising forming at least 10 cellulose filaments and solidifying the at least 10 cellulose filaments in a coagulation unit, wherein the solidified cellulose filaments are moist and contain solvents of cellulose, and winding the moist, solvent-containing cellulose filaments. The invention also relates to a method for processing freshly spun cellulose multifilaments, wherein a cellulose multifilament comprises at least 10 cellulose filaments, comprising winding at least one solvent-containing cellulose multifilament onto a spool.

[0020] The invention also relates to cellulose filaments obtainable according to the inventive method. For example, the cellulose filaments can be wound while wet and dried in the wound state. A cellulose filament can have periodic indentations, with the indentations occurring every 5 µm to 1000 pm. The periodic indentations can occur in groups of, for example, 10 or more, e.g., 10 to 1000 indentations.

[0021] The invention further relates to a cross-coil with at least one moist wound cellulose multifilament, wherein the cellulose multifilament comprises at least 10 cellulose filaments, wherein the cross-coil has a coil body as a support which is cylindrical, and the cellulose multifilament is wound onto the coil body with a laying angle of 5°-20° or with a cross angle of 10°-40°.

[0022] The following detailed description applies equally to the apparatus, method, cross-coil, and cellulose filament. For example, preferred method features also correspond to properties or suitability of the apparatus or its corresponding components, and preferred apparatus features also correspond to means used in the method according to the invention. The cross-coil with wound cellulose filaments and the cellulose filament are products of the method. All preferred features are combinable with one another unless explicitly excluded. All method features, including those mentioned above, are combinable with one another. All apparatus features, including those mentioned above, are combinable with one another. Figures

[0023] In the Figures 1 and 2The components of a device according to the invention are shown schematically. A spinning unit (1) for cellulose filaments (1d) is shown, comprising an extrusion plate (1d) with extrusion openings and a coagulation bath (1c). A deflecting roller (2) for deflecting cellulose filaments produced in the spinning unit is also shown. There are various types of coagulation baths, which are used in Figure 2 only shown as a block. It is customary for the deflection roller (5) to be positioned directly in the coagulation bath (1c). This is in Figure 1The cellulose filaments are guided through an optional partial washing unit (3) and, via a further deflection roller (5), into the filament winder (4). There, the cellulose filaments are wound onto a spool (4a). A spool with wound cellulose filaments (4b) is shown. The cellulose filaments can be wound crosswise. A changing filament guide (4c) can be provided to position the cellulose filaments during the winding process. A separate spool washer (6) can be provided for washing a spool with wound cellulose filaments. For this purpose, the spools with cellulose filaments are removed from the filament winder (4) and brought to the spool washer (6).

[0024] Figure 3An SEM image shows several cellulose filaments produced according to the invention. Indentations spaced 100 pm apart are visible on the filaments. These were created by the inventive method (in particular, the crossed winding in a moist, solvent-containing state, followed by washing and drying).

[0025] In Figure 4 A SEM image of a cryobreak of a single filament is shown. Detailed description of the invention

[0026] The invention relates to a device for the post-treatment of solvent-spun cellulose filaments, in particular cellulose multifilaments or cellulose filament yarns. The post-treatment comprises the winding of solvent-containing cellulose filaments. Solvent-spun cellulose filaments are produced in a dry-wet spinning plant / process or in a wet spinning plant / process and still contain solvents from cellulose immediately after production (as mentioned in the background, tertiary amine oxides, in particular NMMO, or ionic liquids).

[0027] A dry-wet spinning process (also called dry-jet-wet spinning) typically includes the following steps: i) Shaping the cellulose solution: This can be done, for example, by extruding the cellulose solution through extrusion dies. An extrusion line usually has a plate with these extrusion dies.The size of the extrusion openings can influence the diameter of the formed cellulose filaments (another factor influencing the diameter is the stretching of the cellulose filaments); ii) Treating the formed cellulose solution in a gas gap: Here, stretching of the cellulose solution can occur; and iii) Solidifying the cellulose solution into cellulose forms (especially cellulose filaments, also called cellulose threads): Solidification usually takes place in a coagulation unit – here, the cellulose solution is introduced into a fluid that removes cellulose solvent from the cellulose solution, causing it to solidify and form the cellulose filaments. The removal of cellulose solvent in the coagulation unit is not complete – solvent remains in the cellulose filaments, but in a smaller quantity than is necessary to dissolve the cellulose.According to these process steps, a wet-dry spinning plant can include i) an extrusion device, ii) a gas gap, and iii) a coagulation bath. Such processes and wet-dry spinning plants are extensively described in the aforementioned background literature. Numerous variations are known, all of which can be used for the present invention.

[0028] In wet spinning, cellulose filaments are produced in a similar manner using a wet spinning system. The shaping of the cellulose solution is carried out in the same way as in the wet-dry process, particularly by extrusion. Instead of a gas gap, the shaped cellulose solution is solidified immediately in step iii). Solidification occurs as in the wet-dry process, except for the absence of a gas gap, especially using a coagulation system such as a coagulation bath. Wet spinning and wet-dry spinning processes are described, for example, in Azimi et al., Cellulose (2022) 29:3079-3129, US 2022 / 0112628 A1 and US 11,208,739.

[0029] Various arrangements of extrusion openings, gas gap, and coagulation bath are known in the wet-dry process of cellulose. The most common is the use of a basin as the coagulation bath, as shown in WO 93 / 019230 A1. Here, the coagulation bath can be in a basin containing a deflector, in particular a deflector roller, which deflects the solidified cellulose filaments upwards so that the cellulose filaments can be drawn off over the top of the basin. This principle is also found, for example, in US 7364681B2 and other documents mentioned above. Other arrangements are also possible, such as a funnel-shaped coagulation bath, in which the cellulose filaments are passed through a funnel-shaped bath and drawn off at the bottom through a hole in the funnel (US 5639484 A). Both configurations are possible and are shown schematically in Fig. 1 and Fig. 2This is roughly illustrated. After the coagulation bath in the device / coagulation using the wet-dry process, the cellulose filaments are solid and no longer in a liquid state. The optional subsequent washing is therefore not coagulation, but rather serves to wash out some of the cellulose solvent. This can alter the plasticity of the cellulose filament and thus improve its coiling in the wet state (i.e., without drying). Washing can also be used to extract cellulose solvent from the cellulose filaments.

[0030] The invention relates in particular to the treatment of cellulose multifilaments produced in a spinning process or spinning plant, specifically immediately after their production, where the cellulose filaments of the multifilaments still contain solvent; that is, the cellulose filaments are already coagulated but still contain significant amounts of solvent, which affects the plasticity of the cellulose filaments. Conventionally, the solvent is removed from the cellulose filaments as quickly as possible so that expensive solvent is recovered and finished, further-processable cellulose filaments are obtained. According to the invention, it has been found that such immediate washing processes are inefficient. According to the invention, the solvent-containing cellulose filaments are wound up. In the wound state, e.g., on a spool, the solvent-containing threads can be washed out much more efficiently.A coil is also called a tube or bobbin.

[0031] The invention enabled the elongation of cellulose filaments to be increased by up to 50%, which significantly facilitates the further processing of the produced filaments into end-customer products. Secondly, the strength of the cellulose filaments could also be increased by up to 20%, which is likewise advantageous for further processing.

[0032] The production of cellulose multifilaments is typically carried out industrially to obtain filament bundles or yarns that are desirable on the market, i.e., those with sufficient strength and flexibility. Previously, for example in the literature cited at the beginning, it was assumed that multifilaments must be washed (i.e., solvents completely removed) and dried quickly after production before being wound onto reels. The aforementioned production description is common for the manufacture of staple or continuous filaments. According to the invention, the multifilament is wound onto reels while still moist and containing solvents. Due to the plasticity of moist, solvent-containing multifilaments, deformation can occur during this process.These deformations have not proven to be disadvantageous, but rather beneficial, as the finished product has a better feel and the coloring of filaments produced according to the invention is more efficient, requiring fewer chemicals for coloring. Furthermore, processing is simplified, and there are fewer filament defects in production, such as filament breaks, tears, or the like. These effects are particularly noticeable with filament bundles. The cellulose multifilament preferably consists of 10 or more, 20 or more, 30 or more, particularly preferably 50 or more, or 75 or more, or even more preferably 100 or more, individual cellulose filaments. Accordingly, the extrusion system has 10 or more, 20 or more, 30 or more, particularly preferably 50 or more, or 75 or more, or even more preferably 100 or more extrusion openings.

[0033] In particular, the invention relates to a device for solidifying and winding threads, comprising a spinning unit for cellulose filaments, a deflecting roller for deflecting cellulose filaments produced in the spinning unit, and a thread winder for winding the cellulose filaments, wherein the device includes no or only a partial washing unit for washing the cellulose filaments or for extracting the cellulose solvent from the cellulose filaments between the spinning unit and the thread winder.The invention also relates to a device for solidifying and winding cellulose multifilaments, comprising an extrusion system with at least 10 openings (nozzle openings) for forming filaments, a coagulation system for solidifying the filaments, and a thread winder for winding the cellulose filaments, characterized in that the device contains no or only a partial washing system for washing the cellulose filaments between the coagulation system and the thread winder.

[0034] Because no or only a partial washing system is provided, the cellulose filament is still moist and contains solvents when the thread winder is used. Solvent refers to solvents from cellulose. A partial washing system can, for example, only wash out solvents from the outer areas of the cellulose filaments. This leads to a reduction in the plasticity of the outer areas of the cellulose filaments. Such partial washing can be achieved by limiting the length of the partial washing system. For example, the partial washing system can have a maximum length of 5 m, preferably a maximum of 3 m, or even a maximum of 2 m. A maximum length of 1 m is particularly preferred. The length refers to the section over which a cellulose filament is treated with a washing liquid (e.g., water) in the partial washing system. In the device according to the invention, this section includes the structural measures for the treatment, such as...A wash bath (bath length) or, in the case of spraying, the length over which spray nozzles are arranged. The washing medium in the partial washing system (partial washer) can contain solvents, or the process can include partial washing with a solvent-containing medium.

[0035] The device may optionally include one, several, or all of the following elements, preferably in this order in the production direction: spinning mass supply, spinning pump, heat exchanger, nozzle block with sieve, distribution plate and nozzle, gas gap, blown air supply into the gas gap, blown air exhaust from the gas gap, blown air guide plates at the gas gap, contact precipitation, deflector, partial washing unit, deflector (roller), yarn winder. The yarn winder may be configured with multiple winding stations.

[0036] The invention further relates to a method for the production and processing of cellulose filaments, comprising spinning processes for the production of cellulose filaments, wherein the cellulose filaments contain solvents of cellulose, no or partial washing of the cellulose filaments, whereby the solvent content of the cellulose filaments is reduced, and the cellulose filaments remain moist and solvent-containing, and winding of the moist, solvent-containing cellulose filaments. The invention further relates to a method for the production and processing of cellulose multifilaments, comprising forming at least 10 cellulose filaments and solidifying the at least 10 cellulose filaments in a coagulation plant, wherein the solidified cellulose filaments are moist and contain solvents of cellulose, and winding of the moist, solvent-containing cellulose filaments.Preferably, the process comprises partial washing of the cellulose filaments, whereby the solvent content of the cellulose filaments is reduced but not completely removed, and the cellulose filaments remain moist. Partial washing allows the solvent-containing cellulose filaments to have a core area with a higher solvent concentration than an outer area. Washing the multifilaments on the spool has proven to be particularly efficient, especially compared to conventional washing in the production line as described, for example, in WO 2020 / 136109 A1 or WO 2021 / 105275 A1, or on a reel as described in EP 3812489 A1. According to the invention, such deflection rollers are preferably avoided.

[0037] Therefore, the invention also relates to a method for processing freshly spun cellulose filaments, in particular cellulose multifilaments, wherein solvent-containing cellulose filaments are wound up, especially on a spool. The solvent-containing cellulose filaments can have a core region with a higher solvent concentration than in a peripheral region of the cellulose filaments. The freshly spun cellulose filaments originate from a spinning process. Subsequently, no or only partial washing of the already solidified cellulose filaments can take place, as mentioned above. Peripheral region and core region refer to the filament cross-section.

[0038] The thread cross-section is usually round, but can also have other shapes, depending on the shape of the extrusion openings in the wet-dry process. Preferably, the thread cross-section is circular or elliptical.

[0039] In both dry-wet and wet spinning processes, the cellulose solution is forced (extruded) through the extrusion dies at a specific extrusion speed. The cellulose solution is a highly viscous liquid and can withstand certain tensile forces. This is utilized for the aforementioned stretching in the gas gap during the dry-wet spinning process. For stretching, the cellulose filaments are drawn off at a certain speed. This tensile force on the (solid) cellulose filaments continues to extrude in both the dry-wet and wet spinning processes, and in the dry-wet process, it also causes the cellulose solution to stretch in the gas gap. In conventional, industrially used lyocell processes, the draw-off speed is achieved not only by a draw-off device but also continuously via driven rollers.In the conventional lyocell process, the cellulose filaments (also called cellulose threads) would be subjected to multiple strong forces if these forces were not balanced during the process, particularly by driven rollers. As shown, for example, in US20130101843A1, the cellulose threads run over numerous rollers, especially in washing units that completely remove cellulose solvents, and in drying units. If these rollers were not driven, the forces exerted on the cellulose threads would be too great and would cause thread breakage. To prevent this, the conventional lyocell process uses driven guide rollers. This means that the take-off speed is determined by the guide roller closest to the extrusion unit, which also acts as a drive roller. These frictional forces are more pronounced in cellulose multifilaments because the individual cellulose filaments also rub against each other.Therefore, the advantages of the invention, namely gentle handling of cellulose filaments, are particularly pronounced in the case of cellulose multifilaments.

[0040] The cellulose solution for extrusion is preferably a mixture of cellulose, solvent, and water. An example of a spinning solution is: cellulose: 12.9%; solvent, e.g., NMMO: 76.3%; water: 10.8% (all percentages by weight).

[0041] According to the invention, the number of deflection devices, in particular the deflection rollers, is minimized because no or only a simplified partial washing and no drying are carried out before winding / before the yarn winder. Due to the small number of deflection devices / deflection rollers, it is not necessary to drive the deflection devices / deflection rollers, since the small number also results in only minimal forces being exerted on the cellulose filaments.

[0042] In the apparatus and method, the yarn winder can provide the take-off speed for the spinning unit, or a yarn winder can be used in the method to take off the cellulose filaments in the spinning process, particularly from the coagulation unit. This can be done directly or indirectly via one or more intermediate filament deflectors (also called deflection devices or deflectors). Preferably, the number of deflectors, such as deflection rollers, between the yarn winder and the spinning unit is limited; for example, a maximum of 5 deflectors, such as deflection rollers, or a maximum of 4, 3, or 2 deflectors, such as deflection rollers, may be provided. Preferably, the number of deflectors, particularly deflection rollers, is also limited in the spinning unit or is completely avoided, as, for example, in a funnel coagulation bath (US 5639484 A) or a draining coagulation bath (WO 96 / 030566 A1).The spinning machine can have 0, 1 or 2 deflectors, preferably deflection rollers, preferably 0 or 1. Preferably the entire inventive device has 0, 1, 2, 3, 4, 5, or 6 deflectors, in particular deflection rollers, preferably 1, 2, 3 or 4.

[0043] Preferably, the wet-dry process is used. The thread winder can then supply or control the take-off speed for stretching in the gas gap.

[0044] Preferably, one or more, preferably two, three, four, five, or all, of the deflection rollers are rotatably mounted and / or driven without a motor. Due to the free rotation and the absence of a motor, the rollers exert no pulling force on the cellulose filaments. Frictional forces on the threads are minimized by the rotatable mounting. Preferably, there is no motorized deflection roller between the dry / wet spinning unit and the thread winder. Motorized deflection rollers can cause filament defects in the cellulose filaments, especially in multifilaments, and are therefore preferably avoided. Rotatably mounted deflection rollers rotate with the cellulose filaments attached to them, preferably without slippage.

[0045] Preferably, after their production in the spinning process, particularly after solidification / coagulation, the cellulose filaments are deflected by a deflector, preferably a deflection roller, which is preferably not motorized. This allows the cellulose filaments to be deflected in their guide direction towards the partial wash or the yarn winder. Deflectors, also called deflection devices, can be deflection rollers or deflection edges. Deflection rollers are preferred. Preferably, no deflection edges are used.

[0046] Preferably, after washing, the cellulose filaments are deflected by a deflector (deflection device), preferably a deflection roller, before winding. Preferably, this deflection roller is not motorized or rotatably mounted. This allows the cellulose filaments to be deflected in their guiding direction towards the yarn winder.

[0047] Deflection pulleys preferably have an outer diameter of 0.4 mm to 4 cm, preferably of 0.6 mm to 3 cm.

[0048] Preferably, the winding process (on the yarn winder) creates tension on the cellulose filaments, which continues until the spinning process, particularly during consolidation, and determines the take-off speed of the cellulose filaments during the spinning process, especially after consolidation, preferably the take-off speed from the coagulation unit. This continuation of tension is achieved by the rotatably mounted or non-motorized deflection rollers – and their small number (maximum partial washing, no drying / no dryer). A partial washer can be designed very simply. In particular, the partial washer avoids separate deflection elements such as rollers. For example, the cellulose filament can be guided under a water shower.

[0049] Preferably, the cellulose filaments are drawn off from the spinning process, preferably from a wet-dry process, and particularly preferably after solidification or coagulation, at a draw-off speed of 100 m / min to 500 m / min. The extrusion speed is lower and can be, for example, 10–150 m / min. Higher draw-off speeds result from the stretching process.

[0050] The formed cellulose solution can be stretched / stretched in the air gap to 2-20 times, preferably 3-15 times, in particular to 4-10 times, its original length (length immediately after extrusion).

[0051] Preferably, the partial washing system has one, two, or more washing channels. One washing channel can be positioned for washing a cellulose multifilament. If several multifilaments are produced in parallel, preferably one washing channel is provided for each multifilament. In the washing channels, the multifilaments are washed to remove some of the cellulose solvent.

[0052] Preferably, the partial washing system has two or more washing channels, and two washing channels are positioned at an angle of 0° to 150°, preferably 5° to 50°, to each other. The angle is the angle between the washing channel axes of the two washing channels, enclosed by washing channel axes defined along the multifilaments. The angle opens in the production direction, i.e., away from the coagulation unit and towards the yarn winder.

[0053] Preferably, the partial washing unit is positioned with a gradient of 0% to 373%, more preferably 5% to 100%. The gradient is essentially downwards in the production direction, i.e., in the direction from the coagulation bath to the filament winder or in the filament take-off direction. Washing fluid can thus flow off by gravity in the filament take-off direction, i.e., in a co-current flow.

[0054] Preferably, the partial washing system has two or more washing channels, one of which is positioned for washing a cellulose multifilament. The two or more washing channels can be positioned at different gradients relative to each other.

[0055] Preferably, the cellulose filaments are formed using a cellulose solution containing a cellulose solvent at a concentration of 60% to 85%. Preferably, the formed cellulose filaments are treated in the coagulation unit with a coagulation fluid containing a cellulose solvent at a concentration of 0% to 30%, preferably 5% to 25%. Preferably, the cellulose filaments have a cellulose solvent content of 30% to 60%, preferably 40% to 55% (all wt%) after coagulation. Preferably, after solidification in a coagulation unit, the cellulose filaments are partially washed until the cellulose solvent content is reduced to 10% to 40%, preferably 20% to 30% (all wt%). These solvent concentrations in different fluids or at different process stages can be combined.In this process, the proportion of cellulose solvent is continuously reduced. Initially, a cellulose solution is present, which is extruded and shaped. This is typically done at high temperatures, e.g., above 75°C, or at room temperature (e.g., with ionic liquids). The temperature depends on the solvent. This solution solidifies / coagulates by reducing the proportion of cellulose solvent and the temperature. The proportion is then further reduced by partial washing. In the process according to the invention, the cellulose solvent is only completely removed after the material is wound / rewound into a compact, coiled form, e.g., onto a spool.

[0056] Preferably, the filament winder incorporates a variable-angle filament guide. A variable-angle filament guide is preferably suitable for controlling the winding angle of the filament. The winding angle is the angle of the filaments on the spool. Preferably, the winding is cross-wound and inclined. Preferably, a further deflector, more preferably a deflection roller, is located directly before or after the variable-angle filament guide. This further deflector can guide the cellulose filament to the variable-angle filament guide. A deflector or deflection device before the variable-angle filament guide can, for example, also be designed and installed in a non-straight, slightly curved, or specially shaped configuration to compensate for variations in the filament path. A deflector or deflection device after the variable-angle filament guide can be used to press cellulose filament onto a spool on which the cellulose filaments are wound. This pressure can be, for example, 3 to 30 N.The changing thread guide can direct the cellulose filament to different positions within the thread winder. This allows the filament to be guided and deposited at different positions on a spool. This enables winding patterns to be set at a selected density via the thread winder's rotation axis. Preferably, the cellulose filament is wound crosswise onto a spool. This crosswise winding is accomplished by the changing thread guide. Preferably, the thread winder has a spool for winding the cellulose filaments. The changing thread guide is essentially a cellulose filament guide and is preferably driven by a motor, e.g., a stepper motor, a linear guide drive, or motors that enable linear movement of the changing thread guide based on a rotary motion. The drive of the changing thread guide can also be magnetically coupled or achieved through the use of various mechanisms.The moist cellulose filament is guided linearly along an axis by the changing thread guide. This is achieved by moving the changing thread guide back and forth along an axis. A deflector (e.g., a pressure roller) then presses the filament onto the spool winding device and winds it onto the spool body. The linear guidance of the cellulose filament strand along the changing axis, combined with the pressure of the rotating changing pressure roller against the filament winder (which rotates at a preset speed), winds the resulting moist cellulose coagulate, either as a single filament or a filament strand (a filament strand can consist of several individual filaments, e.g., 1000 or more), onto the motor-driven spool body, forming a moist cellulose filament spool.The yarn winder can simultaneously serve as a take-up device, after the spinning process, for adjusting the desired individual or total filament thickness (drawing). A variable yarn guide on a yarn winder for yarns with adjustable yarn guide stroke and stepless, collective adjustment of the bobbin flank angle is described, for example, in US 3730448 A.

[0057] Preferably, the thread winder has a spool for winding the cellulose filaments, preferably the spool being driven by a motor. Preferably, the spool is clamped. The spool can wind the cellulose filaments onto a bobbin by rotating the spool around a bobbin axis. The spool is rotationally symmetrical with respect to its circumference and can be cylindrical or conical. The bobbin can also have holes or perforations, which need not be rotationally symmetrical, but may be.

[0058] The winding speed can be automatically controlled depending on the set take-off speed, as well as the extrudate (extrusion openings) and spool diameter. To create an ideal winding pattern, the tension between take-off and winding can be dynamically adjusted. After the winding process, the spool, along with the cellulose filament, can be removed and used or stored.

[0059] The cellulose filaments preferably have a solvent concentration of 10% to 40%, preferably 20% to 35% (all weight %), when wound up, e.g. after partial washing.

[0060] Preferably, the cellulose filaments are wound with a packing density of 0.8 g / cm³ to 1.3 g / cm³ (moist cellulose filaments) and / or the cellulose filaments are wound with a packing density of 0.2 g / cm³ to 0.7 g / cm³ (based on dried cellulose filaments). The packing density can be determined by the thread guidance on the spool; for example, a cross-winding pattern can be used to adjust the spacing between the cellulose filament windings. A variable-width thread guide is preferably used for this purpose. This guide can determine the position of the wound cellulose filaments on a spool. According to the invention, the cellulose filament thread can be wound in such a way that the adjacent threads are separated from each other and formed into a continuous cellulose filament spool body with uniform tension. For solvent-spun cellulose filaments, the density of the filaments on a pack is preferably adjusted to 0.3 to 0.6 g / cm³ < spool volume.The packing density is achieved by appropriately selecting the winding parameters. The main parameters include the winding method and the angle of the applied filament. To achieve the packing density according to the invention, the "distributed wind" or "wild winding" technique has proven suitable. The cross-winding angle of the filament is preferably in the range of 20° to 28°. Preferably, the cellulose filaments are wound cylindrically or conically at the ends of the spool. The tangential tension in the crossed winding can, for example, have a value of 3 to 500 cN, preferably 5 to 50 cN, and more preferably between 10 and 20 cN.

[0061] Individual cellulose filament windings are not laid onto the spool at a constant winding ratio (spool revolutions per double stroke of the thread guide), but rather at a constant angle (laying angle). This angle is defined by measuring a surface projection of the spool between a straight line that intersects the spool axis perpendicularly and the path of the cellulose filament. This winding technique lays the cellulose filament onto the spool particularly gently and, above all, loosely, resulting in a very low density of the resulting yarn cake. This, in turn, makes the cake particularly easy to wash in subsequent laundry. Furthermore, this method allows the cellulose filament to cross over previously laid cellulose filaments, creating a cross-winding effect.Cross-winding gives the spool high mechanical strength and is particularly suitable for winding onto spool bodies without side walls. Preferably, the cellulose filaments are wound at a lay angle of 5°–20°, more preferably 10°–14°. In the case of crossed winding, where different layers of filaments are wound at opposite angles, twice the lay angle corresponds to the angle between the different filament layers. The angle between the filaments can be 10°–40°, more preferably 15°–30°.

[0062] The invention also relates to a cross-wound spool with at least one wet-wound cellulose multifilament, wherein the cellulose multifilament comprises at least 10 cellulose filaments, the cross-wound spool having a cylindrical spool body as a support, and the cellulose multifilament being wound onto the spool body with a lay-up angle of 4°–20° or with a cross-angle of 10°–40°. The cellulose multifilament can be dried and present on the spool in a dried state. The lay-up angle is formed by the normal to the cylindrical axis of the spool body and the laid-up multifilaments, at least in a central part of the spool. In the outer regions of the spool, the filaments can be wound at a different angle for deflection and retraction.

[0063] In the inventive method, the coil winding can be carried out in stages. An initial base winding (e.g., in a start-up process) can be applied, which is wound with a slightly different winding angle. This initial winding is placed on the empty coil former and serves the purpose of building the winding up as close as possible to the ideal cylindrical final shape. After this initial winding, a constant winding angle is maintained, as described above. The winding angle is the angle between the cellulose filament and the perpendicular to the coil axis (also called the axis of rotation). Preferably, the cellulose filaments are wound in a start-up process (base winding) and a subsequent main winding, wherein the winding angles in the start-up and main winding processes differ from each other by 0.5° to 10°, preferably by 0.5° to 3°.

[0064] It has been shown that the bobbin winds more efficiently if it is not perfectly cylindrical, but rather has angled edges at the ends. The edge angle is used for this purpose. Winding at an edge angle of less than 90°, for example, between 60° and 85°, results in a particularly gentle winding of the thread's turning points, as these points do not overlap but are instead pushed further and further towards the center of the bobbin as it grows.

[0065] The packing density of the spool is defined by the mass of the cellulose filaments on the spool in the dry state divided by the enclosing volume of the cellulose filaments on the spool.

[0066] The thread winder can be a device for receiving and depositing moist, solvent-containing cellulose filaments.

[0067] The device can be further supplemented by a separate spool washer. The separate spool washer is used for washing cellulose filaments wound on a spool. Preferably, the wound multifilaments are washed on the spool, preferably with a washing liquid flow rate of 1000 to 10000 liters per minute and / or 2 to 50 liters per minute per kilogram of dry cellulose filament.

[0068] In preferred embodiments, the cellulose filaments are post-treated after winding by washing, rinsing, bleaching, dyeing, cross-linking, and drying processes. This post-treatment of the cellulose filaments takes place in the wound state, particularly on a spool. The cellulose filaments are preferably wound at a laying angle of 5°–20°, more preferably 10°–20°.

[0069] The thread winder can be speed-controlled or tension-controlled, with the device preferably having a dancer arm. With speed control, the winding speed is adjusted to achieve the desired take-off speed. For this purpose, a take-off mechanism can be installed upstream of the thread winder to determine the take-off speed. In tension-controlled operation, the filament tension can be kept constant by a dancer arm (optionally with a dancer arm roller). This compensates for tension variations that would occur due to the movement of the changing thread guide.

[0070] In the thread winder / process step of winding the cellulose filaments, the cellulose filaments can be wound onto a spool, preferably mechanically clamped. After one spool has been fully wound, another spool can receive the wound cellulose filaments. The thread winder can have a spool changer for switching between spools. A spool changer can, for example, have two or more spool carriers. These spool carriers hold spools, one of which holds the cellulose filaments (the "active spool carrier" or "active spool"). The changing thread guide can be associated with the active spool carrier or the active spool. One or more spool carriers can be provided for quick repositioning to the position of the active spool carrier. Such provided spools (carriers) are also called standby spools. For example, the spool carriers can be arranged on a rotatable support, such as a disk.Rotating the holder changes the position of the spool supports. Spool supports are, for example, bolts on which the clamped spools can rotate for winding.

[0071] Preferably, the device has one or more standby spools, particularly in conjunction with the winder. Standby spools are in a position without filament feed / without changeover thread guide. Standby spools can be provided for switching to the position of a fully wound spool. Preferably, the device has a spool-changing system that can change the position of two or more spools, whereby one spool is moved into a winding position and / or one spool is moved away from a winding position.

[0072] Preferably, the device has a spool transfer system suitable for changing spools by linear and / or rotary motion. In this process, spools can be changed by linear and / or rotary motion. Preferably, a standby spool is positioned next to a wound spool by rotation, so that a changeover filament guide begins to wind cellulose filaments onto the standby spool without interruption. This transfers the cellulose filament from one spool to the other. The cellulose filament transferred from the previously wound spool to the standby spool can be cut during the filament transfer between the spools. For this purpose, the device can have a cutting device. The fully wound spool can be moved by a linear motion to allow for a smaller design of the winding device.

[0073] A wound cellulose filament pack preferably has a circumference of 60 mm to 600 mm; preferably, the wet spool circumference is in the range of 100–300 mm or 150–250 mm. The cellulose filament spool bodies produced according to the invention preferably have a length of 50 mm to 500 mm. While different winding conditions may be suitable for different filament types, it has been found that the following is ideal for the production of solvent-impregnated, precision-wound spools with a density of 0.3 to 0.5 g / cm³ (based on dry cellulose filaments), and / or with a minimum circumference of at least 120 mm and / or a length of the cellulose filament pack of 120 to 160 mm: firstly, for washing out the organic solvents, and secondly, for producing the primary, secondary, and tertiary wound cellulose filament spools, and thirdly, for unwinding in further textile and technical applications.The primary winding of the cellulose filament spool (or primary winding) refers to the spool / filaments wound directly after production and for the first time. These filaments from the primary winding can be unwound and rewound. These are referred to as the secondary winding. These filaments from the secondary winding can also be unwound and rewound. These are referred to as the tertiary winding. Various treatment steps can be performed between these windings, such as solvent extraction (washing) – this time complete or nearly complete – various other treatments, and drying.

[0074] Preferably, the device further comprises a spool washer. The spool washer is used for washing cellulose filaments wound on a spool. Accordingly, the method according to the invention preferably includes the step of washing wound cellulose filaments, particularly preferably cellulose filaments wound on a spool. During this washing process, cellulose solvent is removed from the cellulose filaments as completely as possible, particularly by displacement during washing. The washing liquid is preferably an aqueous fluid, especially water. Washing the wound cellulose filaments can be designed very flexibly with regard to temperature, pressure, washing medium flow rate (usually water or aqueous liquid), and time. This is an advantage of the method according to the invention, since the process parameter during unwinding, as described in US 2013 / 0101843 A1, does not need to be taken into account.In these continuous processes, the thread must continue to be handled very carefully directly on the extracted cellulose filament, as the thread under tensile stress can easily develop filament defects such as cracks.

[0075] After washing, the cellulose filaments on the spools are moist but no longer contain solvents, or only a small amount (e.g., less than 0.1% by weight solvent). These moist, coiled cellulose filaments can be further processed or dried. Preferably, the moist cellulose filaments are treated before drying, for example, by washing, anting, crosslinking, bleaching, and / or dyeing. This treatment is carried out while the filaments are coiled, for example, on a (cross-)spool. Anting while coiled can be performed, for example, in a spool washer or during mechanical dewatering. Such treatment steps are more efficient on moist cellulose filaments that have not been previously dried. Drying appears to alter the cellulose structure, and not all parts of the cellulose filaments are equally accessible when subsequently treated with liquid for bleaching or dyeing dried cellulose.The device according to the invention can have corresponding treatment chambers for bleaching, dyeing, impregnating, and crosslinking. Furthermore, a spool dryer, e.g., a high-frequency heater, microwave dryer, hot air dryer, or drying chamber, is preferably provided. These chambers are specifically designed for spools, and a spool holder may be included. In the process according to the invention, the wound cellulose filaments, particularly those on a spool, can be treated according to the process steps described above. Preferably, the moist wound and / or wound cellulose filaments have a relative humidity of 50% to 170%, more preferably 100% to 140% (all weight percent).

[0076] The solvent-containing cellulose filaments, wound into yarn spools, are preferably subjected to a further post-treatment step after winding. This post-treatment step can consist of subjecting the moist yarn spool to further swelling in a solvent bath. Solvent baths can be, for example, dilute amine oxide solutions or ionic liquids. The resulting yarn spools can also be immersed in other solvent baths that accelerate or delay the crystallization of the cellulose filaments.

[0077] Cellulose can be subjected to substitution reactions. The aim of these reactions on freshly spun, moist, and highly reactive cellulose filaments is to produce products with modified properties. This can broaden the range of applications for cellulose filaments. Esterification, etherification, and grafting reactions are all possible substitution reactions.

[0078] Preferably, the wound multifilaments on the spool are dewatered, preferably by mechanical dewatering, e.g., centrifugation, and / or drying by heat and / or vacuum. Preferably, mechanical dewatering is carried out to a water content of 30%–70% (by weight) followed by drying. Drying, including partial drying, can be carried out using convective, contact, radiation, electric, high-frequency, or microwave drying methods. Optionally, after or between dewatering steps, the cellulose filaments can be rewound onto a different spool. This improves the packing density after water loss. After drying, the filaments can be subjected to heat fixation.

[0079] A spool with crossed wound cellulose filaments is also called a cross-wound spool. The descriptions herein, and especially those that follow, relate to spools and, in particular, to the cross-wound spool. The laying angle of the filaments is preferably 5°–20°, as described above. Preferably, this results in a cross angle of 10°–40° for different filament layers. On a cross-wound spool according to the invention, the cellulose filaments may contain cellulose solvents. A cross-wound spool according to the invention can be formed and / or processed, e.g., washed or dried, according to a method according to the invention.

[0080] The spools preferably have a perforated spool body. The spool body can have a multitude of holes through which or into which washing liquid, treatment liquid, or a gas can pass for drying. This allows the cellulose filaments wound on the spool body to be treated continuously from both the outside and the inside (via the perforations / holes). The multitude of holes can, for example, be 30 or more, or 50 or more. This can be scaled according to the size of the spool body. The spool bodies can also consist of surface-closed hollow cylinder elements, perforated metal or plastic cores, or spring-like spool bodies onto which the continuously formed filament is wound. Preferably, the spool body is made of polypropylene. Preferably, the spool body is a hollow cylinder, preferably with a wall thickness of 0.5 mm to 5 mm.Preferably the coil body is perforated, preferably with openings which exclude 10% to 60%, preferably 20% to 50% of the coil surface.

[0081] Preferably, the cellulose filaments on the spool are wound with a packing density corresponding to 20-60% (volume %), preferably 25-35% (volume %), of dry cellulose filaments. The volume refers to the volume occupied by the cellulose filaments and the spaces between the filaments. An enclosing volume around the filaments can also be defined.

[0082] In preferred embodiments, the coil former has a modulus of elasticity of 1200 MPa to 1300 MPa and / or a tensile strength of 33 to 37 MPa measured according to ISO 527-2, and / or withstands a compressive force of 450 N to 550 N according to EN 12080. Preferably, the coil former is made of polypropylene.

[0083] Preferably, the solvent for cellulose is a tertiary amine oxide, preferably N-methylmorpholine N-oxide (NMMO), or an ionic solvent, preferably with an ammonium, pyrimidium, or imidazolium cation, particularly preferably 1,3-dialkylimidazolium, especially preferably 1,3-dimethylimidazolium, 1-ethyl-3-methylimidazolium, 1-methyl-3-propylimidazolium, 1-isopropyl-3-methylimidazolium, 1-butyl-3-methylimidazolium, 1-methyl-3-pentylimidazolium, 1-hexyl-3-methylimidazolium, 1-heptyl-3-methylimidazolium, 1-methyl-3-octylimidazolium, 1-decyl-3-methylimidazolium, 1-methyl-3-benzylimidazolium, 1-methyl-3-(3-phenylpropyl)imidazolium. 1-(2-Ethyl)hexyl-3-methylimidazolium, 1-methyl-3-nonylimidazolium, 1-methyl-3-decylimidazolium, 1,2,3-trimethylimidazolium, 1-ethyl-2,3-dimethylimidazolium or 1-butyl-2,3-dimethylimidazolium, particularly preferably butyl-3-methylimidazolium, 1-Ethyl-3-methyl-imidazolium, 1-butyl-2,3-dimethylimidazolium, 1-butyl-3,5-dimethylpyridinium,or 1-butyl-3-methylimidazolium. E.g., 1-butyl-3,5-dimethylpyridinium bromide, 1-butyl-3-methylimidazolium hexafluorophosphate, 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide. Other known cellulose solvents and solvent systems, cellulose manufacturing processes, such as urea / sodium hydroxide, sodium hydroxide / zinc, dimethylacetamide / lithium chloride, dimethyl sulfoxide / paraformaldehyde can be used. The ions can be coupled with common counterions (anions) such as fluoride, chloride, bromide, thiocyanate, dicyanamide, nitrate, methyl phosphate, acetate, formate, propionate, benzoate, thioglycolate, methyl sulfate, hydrogen sulfate. Cellulose solvents are described, for example, in Négrier et al. (DOI:10.1039 / d2su00084a), Elsayed et al. (Cellulose 28: 533-547, (2021)), Azimi et al. (Cellulose 29: 3079-3129, (2022)), Swatloski et al. (J. Am. Chem. Soc. 2002, 124, 18, 4974-4975), WO2018 / 138416, WO2023 / 104635, US 7,858,802, US 8,163,215. The ionic liquids described therein can be used to prepare cellulose solutions and for the production of cellulose fibers according to the invention. 1-Butyl-3-methylimidazolium (Bmim) or 1-Ethyl-3-methylimidazolium (Emim) are preferred. Likewise, highly purified ionic liquids, so-called CBILS® Carbonate Based Ionic Liquids, such as 1,3-dialkylimidazolium, can also be used as solvents. Other potential cations are ammonium or pyridinium, imidazolium, phosphonium, morpholine, [TMGH]+, [DBNH]+, [DBUH]+. The coagulation liquid can contain water, in particular a mixture of water and a solvent for cellulose.

[0084] Further solvents and methods for dissolving and processing cellulose are described, for example, in WO2022 / 112425A1 and WO2022 / 144506A1. The resulting cellulose solutions can also be processed into cellulose filaments using the device according to the invention.

[0085] The cellulose filaments obtained by spinning are preferably a multifilament or bundled together, e.g., 10 or more, 30 or more, 50 or more, 100 or more, or 200 or more. These cellulose filaments can be processed together as yarn in such bundles. For this purpose, the cellulose filaments are produced in parallel. The extrusion apparatus can have the same number of extrusion openings as the number of filaments produced in parallel, e.g., 10 or more, 30 or more, 50 or more, or 100 or more. Parallel spinning / extrusion is described, for example, in WO 94 / 028218 A1.

[0086] The invention further relates to a cellulose filament that is wound while wet and dried in the wound state. The invention also relates to a cellulose filament that can have periodic indentations, with the indentations occurring every 5 µm to 1000 pm. The periodic indentations can occur, for example, 100 times or more, 1000 times or more, or 10,000 times or more. Such cellulose filaments are obtainable according to the inventive process. The cellulose filament can be present in a yarn of 10 or more, 30 or more, or 50 or more cellulose filaments, e.g., 100 or more cellulose filaments (multifilament). The cellulose filament according to the invention has a different structure than continuously produced cellulose filaments that are immediately washed and dried. Due to the winding in a wet, solvent-containing state, the cellulose exhibits a different, slower crystallization or solidification behavior.According to the invention, the cellulose has an amorphous structure. Furthermore, plastic deformation is noticeable during cross-winding, which is why the filament can have indentations every 5 µm to 1000 pm, preferably every 10 µm to 500 pm, and particularly preferably every 30 pm to 120 pm. The indentations can be present in one area, alongside other areas with fewer indentations. The area with indentations corresponds to the central part of the spool with the cross-winding. In the outer region of the spool, filaments are deflected, and fewer indentations can be present in corresponding areas on the filament. An area with periodic indentations can, for example, comprise 10, 20, or 30 indentations. It has been found that the primarily wound, coiled, and swollen cellulose filaments (moist and containing solvents) are surface-modified by the layered cross-winding of the cellulose filaments.The windings of different layers of moist cellulose filaments intersect, therefore only touching at isolated points, and modify the surfaces of the swollen fiber mass through mutual indentations. The induced plastic deformation of moist cellulose fibers refers to the irreversible change in the shape of the extruded cellulose material under the influence of external forces during primary winding. An initial plastic deformation of the cellulose fibers remains as a permanent change, as their internal structures, particularly the crystal structures of the precipitated regenerated cellulose, rearrange themselves accordingly. An indentation can, for example, be 3%–30% of the diameter, preferably 5%–20% or 8%–15%.

[0087] In preferred embodiments, the moist, solvent-containing cellulose filament is wound up to a length of at least 50 m. Preferably, the length is at least 100 m, more preferably 100 m to 5 km, and more preferably 200 m to 2.5 km, e.g. 300 m to 1.5 km.

[0088] A cellulose filament produced according to the invention preferably has a fineness of 0.5 dtex to 10 dtex, more preferably 0.8 dtex to 5 dtex, and more preferably about 1-2 dtex. For bundled filaments, the overall fineness is specified. For example, a bundle (or yarn) of 100 filaments, each with a fineness of 1 dtex, has a fineness of 100 dtex (100 × 1 dtex). The fineness of a single filament (individual fiber) is preferably 0.5 dtex to 7 dtex, more preferably 0.8 dtex to 6 dtex. Preferably, bundles with a fineness of 20 dtex to 3000 dtex are wound up, according to the invention, in a moist state. Dtex and further filament specifications are in accordance with BISFA (Terminology of Man-Made Fibres). Preferably, a cellulose filament has a filament thickness of 4 pm to 30 pm, particularly preferably 7 µm to 25 µm, even more preferably 9 pm to 20 µm, especially preferably 11 pm to 15 µm.Such threads are fine enough for applications in the textile industry and are also well-suited for processing in the apparatus according to the invention in the field of technical applications. The cellulose filaments produced according to the invention also have a higher strength (at the same thickness or fineness) of approximately 20%. This allows for the production of finer threads according to the invention (with comparable strength). Surprisingly, the process according to the invention yielded a very bright (white) cellulose filament product, since the washing process carried out after the primary winding is very efficient and gentle on the fibers, and the solvent can be completely removed from the fibers. This prevents yellowing, eliminating the need for subsequent bleaching steps.As a result, the resulting cellulose fibers have improved mechanical properties, such as elongation and strength, as well as improved whiteness and thus better dyeing properties. This process is also more environmentally friendly than alternative fiber filament manufacturing methods that require a bleaching step.

[0089] The invention thus also relates to a cellulose filament which was wound while wet and dried in the wound state. Preferably, the cellulose filament has at least 10 periodic indentations in a given area, wherein the indentations are present every 5 µm to 1000 pm in that area. Preferably, the cellulose filament has a degree of crystallinity of 40%-50%, more preferably 41%-49%, or 42%-48%, or 43%-47%, or 44%-46%, preferably about 45%.

[0090] X-ray structure investigations of the cellulose filaments produced according to the invention have shown that the orientation parameter OG(004) is below 0.93 and the integral orientation parameter of the cellulose filament OGI, which can be derived from this, is in the range between 64% and 78%. Surprisingly, compared to conventionally produced cellulose filaments, the inventive method for producing the cellulose filaments yielded filaments with reduced Hermann orientation factors. This indicates a less pronounced alignment of the cellulose fibers in a specific direction, or, conversely, the less pronounced alignment results in a more random distribution and orientation of the cellulose structure within the filaments. The orientation of the cellulose filaments could be influenced by the inventive method.The quality and performance of the manufactured cellulose filaments are closely related to mechanical properties such as tensile strength, elongation, and stainability. Compared to prior art cellulose filaments, which have orientation factors of 0.97 and above, the cellulose filaments manufactured according to the invention exhibit orientation factors below 0.96. In preferred embodiments of the invention, the cellulose filaments have an orientation factor of less than 0.965, preferably 0.963 or less, more preferably 0.961 or less, even more preferably 0.960 or less, and particularly preferably 0.959 or less. In special embodiments, the Hermann orientation factor fc of the cellulose filaments is less than 0.965, preferably 0.951–0.958. The Hermann orientation factor can be determined, for example, by wide-angle X-ray scattering (WAXS) or small-angle X-ray scattering (SAXS).

[0091] Preferably, the cellulose filament has a thread thickness of 0.7 dtex to 10 dtex. It can be present in a cellulose filament bundle (multifilament) with a total density of 10 dtex to 3000 dtex.

[0092] After washing, the cellulose filaments (preferably as bundles) can be unwound and wound onto another spool (secondary winding). These rewinding processes can be used to carry out further treatment steps on the cellulose filament bundle, such as annealing, impregnation, etc. Preferably, the secondary winding is also carried out while wet, but after the solvent has been removed, i.e., without solvent or possibly only residual amounts of solvent. Alternatively, the filaments are dried on the first spool after production (primary spool) without being rewound onto the secondary spool, so that the secondary spool is created from the primary spool. Preferably, drying takes place on the secondary spool. The dried cellulose filaments can then be rewound onto a new spool (tertiary winding).

[0093] The following numbered embodiments are preferred aspects of the invention. These can be combined with each other and with the claims. 1. A device for solidifying and winding cellulose multifilaments, comprising an extrusion unit with at least 10 openings for forming filaments, a coagulation unit for solidifying the filaments, and a filament winder for winding the cellulose filaments, characterized in that the device contains no or only a partial washing unit for washing the cellulose filaments or for extracting a cellulose solvent from the cellulose filaments between the coagulation unit and the filament winder. 2. Device according to 1, wherein the partial washing unit has a maximum length of 5 m. 3. Device according to 1 or 2, wherein the partial washing unit has one, two, or more washing channels or fluid beds, one washing channel or fluid bed being positioned for washing a cellulose multifilament or for extracting a cellulose solvent from a cellulose multifilament. 4. Device according to 3,wherein the partial washing unit has two or more washing channels and two washing channels are positioned at an angle of 0° to 150°, preferably 5° to 50°, to each other. 5. Device according to any one of 1 to 4, wherein the partial washing unit is positioned with a gradient of 0% to 373%, preferably 5% to 100%. 6. Device according to any one of 1 to 5, wherein the partial washing unit has two or more washing channels, one of which is positioned for washing a cellulose multifilament, and wherein the two or more washing channels are positioned with different gradients to each other. 7. Device according to any one of 1 to 6, wherein the filament winder is a device for receiving and depositing the moist, solvent-containing cellulose filaments. 8. Device according to any one of 1 to 7, wherein the filament winder provides the take-off velocity of the formed filaments from the coagulation unit. 9. Device according to one of 1 to 8 with a deflection device,preferably a deflecting roller for deflecting cellulose threads which are solidified in the coagulation unit. 10. Device according to 9, wherein the deflecting roller is rotatably mounted and / or is not driven by a motor. 11. Device according to any one of 1 to 10, wherein there is no motor-driven deflecting roller between the coagulation unit and the thread winder. 12. Device according to any one of 1 to 11, wherein a changing thread guide is located on the thread winder. A changing thread guide is preferably suitable for carrying out the filament winding with controlled laying angle. 13. Device according to 12, wherein a further deflecting device, preferably a deflecting roller, is located directly before or after the changing thread guide. 14. Device according to any one of 1 to 13, wherein the thread winder has a spool for winding the cellulose filaments, preferably wherein the spool is driven by a motor. 15. Device according to any one of 1 to 14, wherein the device has a16. Device according to any one of 1 to 15, wherein the device has one or more spools wound in parallel and / or one, two, or more spools are provided with one or two or more changing thread guides. 17. Device according to 16, with a spool transfer system suitable for changing spools by linear and / or rotary motion. 18. Device according to any one of 1 to 17, wherein the device further comprises a spool washer for washing or extracting cellulose solvents from cellulose filaments wound on a spool. 19. Device according to any one of 1 to 18, wherein the thread winder is speed-controlled or tension-controlled.wherein the device preferably has no dancer arm. 20. Method for the production and processing of cellulose multifilaments comprising forming at least 10 cellulose filaments and solidifying the at least 10 cellulose filaments in a coagulation unit, wherein the solidified cellulose filaments are moist and contain cellulose solvents, and winding the moist, solvent-containing cellulose filaments. 21. Method according to 20, further comprising partially washing the cellulose filaments or partially extracting cellulose solvents from the cellulose filaments, whereby the cellulose solvent content of the cellulose filaments is reduced but not completely removed, and the cellulose filaments remain moist. 22. Method according to one of 20 or 21, wherein the cellulose filaments are deflected after solidification at a deflecting device, wherein the deflecting device preferably23. A method according to one of 20 to 22, wherein the cellulose filaments are deflected after washing and before winding at a deflecting device, preferably a deflecting roller, wherein the deflecting device, preferably the deflecting roller, is preferably not motorized. 24. A method according to one of 20 to 23, wherein the winding creates a tension on the cellulose filaments, which continues until solidification and, after solidification, determines the unwinding speed of the cellulose filaments. 25. A method according to one of 20 to 24, wherein, after solidification, the cellulose filaments are unwinded at an unwinding speed of 100 m / min to 500 m / min. 26. A method according to one of 20 to 25, wherein the forming of the cellulose filaments is carried out with a cellulose solution.which has a cellulose solvent in a concentration of 60% to 85%; and / or wherein, in the coagulation unit, the formed cellulose filaments are treated with a coagulation fluid which has a cellulose solvent in a concentration of 0% to 30%, preferably 5% to 25%; and / or the cellulose filaments after the coagulation unit have a cellulose solvent content of 30% to 60%, preferably 40% to 55% (all wt.%). 27. Method according to one of 20 to 26, wherein, after solidification in a coagulation unit, the cellulose filaments are partially washed or cellulose solvent is partially extracted, wherein washing or extraction continues until the cellulose solvent content in the cellulose filaments is reduced to 10% to 40%, preferably to 20% to 30% (all wt.%). 28. Method for processing freshly spun cellulose multifilaments, wherein a cellulose multifilament comprises at least 10 cellulose filaments,Comprehensive winding of at least one solvent-containing cellulose multifilament onto a spool. 29. Method according to one of 20 to 28, wherein the solvent-containing cellulose filaments have a core region with a higher solvent concentration than in a peripheral region of the cellulose filaments. 30. A process according to one of 20 to 29, wherein the solvent for cellulose is a tertiary amine oxide, preferably N-methylmorpholine N-oxide, or an ionic solvent, preferably with an ammonium, pyrimidium, or imidazolium cation, particularly preferably 1,3-dialkylimidazolium, especially preferably 1,3-dimethylimidazolium, 1-ethyl-3-methylimidazolium, 1-methyl-3-propylimidazolium, 1-isopropyl-3-methylimidazolium, 1-butyl-3-methylimidazolium, 1-methyl-3-pentylimidazolium, 1-hexyl-3-methylimidazolium, 1-heptyl-3-methylimidazolium, 1-methyl-3-octylimidazolium, 1-decyl-3-methylimidazolium, 1-methyl-3-benzylimidazolium, 1-Methyl-3-(3-phenylpropyl)imidazolium,1-(2-Ethyl)hexyl-3-methylimidazolium, 1-methyl-3-nonylimidazolium, 1-methyl-3-decylimidazolium, 1,2,3-trimethylimidazolium, 1-ethyl-2,3-dimethylimidazolium or 1-butyl-2,3-dimethylimidazolium, particularly preferably butyl-3-methylimidazolium, 1-Ethyl-3-methyl-imidazolium, 1-butyl-2,3-dimethylimidazolium, 1-butyl-3,5-dimethylpyridinium, or 1-butyl-3-methylimidazolium. E.g. 1-butyl-3,5-dimethylpyridinium bromide, 1-butyl-3-methylimidazolium hexafluorophosphate, 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide. 31. A method according to one of 20 to 30, wherein the cellulose filaments are wound with a packing density of 0.8 g / cm³ to 1.3 g / cm³ (moist cellulose filaments) and / or wherein the cellulose filaments are wound with a packing density of 0.2 g / cm³ to 0.7 g / cm³ (based on dried cellulose filaments). 32. A method according to one of 20 to 31, wherein the cellulose filaments are wound at a laying angle of 5°–20°, preferably 10°–14°,33. A method according to any one of 20 to 32, wherein the cellulose filaments are post-treated after winding by washing, annealing, bleaching, dyeing, crosslinking, impregnation, and drying processes. This post-treatment of the cellulose filaments is carried out in the wound state, in particular on a spool. 34. A method according to any one of 20 to 33, wherein the cellulose filaments are wound in a start-up process and a subsequent main process, wherein the winding angles in the start-up process and in the main process differ from each other by 0.5° to 10°, preferably by 0.5° to 3°. 35. A method according to any one of 20 to 34, wherein the wound multifilaments are washed on the spool, preferably with a washing fluid flow rate of 1000 to 10000 liters per minute and / or 2 to 50 liters per minute per kilogram of dry cellulose filament. 36. Procedure according to one of 20 to 35,wherein the wound multifilaments on the spool are dewatered, preferably by mechanical dewatering, e.g., centrifugation, and / or drying by heat, radiation, and / or negative pressure. 37. Cross-wound spool with at least one moist wound cellulose multifilament, wherein the cellulose multifilament comprises at least 10 cellulose filaments, the cross-wound spool having a cylindrical spool body as a support, and the cellulose multifilament being wound onto the spool body at a laying angle of 5°–20°. 38. Cross-wound spool according to 37, wherein the cellulose filaments are wound with a packing density corresponding to 20–60% (by volume), preferably 25–35% (by volume), of dry cellulose filaments. 39. Cross-wound spool according to 37 or 38, wherein the cellulose filaments contain cellulose solvents. 40. Cross coil according to one of 37 to 39, wherein the coil body is a hollow cylinder, preferably with a wall thickness of 0,5 mm to 5 mm. 41. Cross coil according to one of 37 to 40, wherein the coil former is perforated, preferably with openings which exclude 10% to 60%, preferably 20% to 50% of the coil surface. 42. Cross coil according to one of 37 to 41, which is formed and / or processed by a method according to 20 to 36, e.g., extracted, treated, or washed. 43. Cross coil according to one of 37 to 42, with a coil former having a modulus of elasticity of 1200 MPa to 1300 MPa and / or with a tensile strength of 33 to 37 MPa measured according to ISO 527-2, and / or withstanding a compressive force of 450 N to 550 N according to EN 12080. 44. Cellulose filament that was wound while containing cellulose solvents and / or moist and / or treated (e.g., by washing, rinsing, bleaching, dyeing, crosslinking, or impregnation processes) and dried in the wound state. 45. Cellulose filament with a region of periodic indentations, wherein indentations,46. ​​Cellulose filament with a degree of crystallinity of 40%–50%, preferably 41%–49%, or 42%–48%, or 43%–47%, or 44%–46%, preferably about 45%. 47. Cellulose filament with a Hermann orientation factor fc of less than 0.965, e.g., less than 9.60, preferably 0.951–0.958. 48. Cellulose filament with the properties of 44, 45, 46, and / or 47. 49. Cellulose filament according to 44 to 48 with a filament thickness of 0.7 dtex to 10 dtex, and / or in a cellulose filament bundle with a total titer of 10 dtex to 3000 dtex. 50. Cellulose filament obtainable by a process according to one of 20 to 36, preferably additionally as in one of 44 to 49. ,

[0094] The following example shows an experiment using the method described in the Figures 1 and 2 Device shown with partial washing.

[0095] The device / method according to the invention were tested with a cellulose solution (viscous spinning mass) consisting, for example, of cellulose, NMMO, and water in a composition comprising 14.0% cellulose, 10.20% water, and 75.80% N-methylmorpholine N-oxide (all wt%). The cellulose solution was formed by extrusion and passed through a gas gap. Further cellulose solutions tested were spun in compositions ranging from 8% to 16% cellulose, a water content between 13.4% and 9.2%, and a tertiary amine oxide (NMMO) content between 78.6% and 74.9%. Experiments showed that cellulose with an average degree of polymerization of DP 550 is readily processable.The intrinsic viscosity (IV) of the celluloses used ranged between 350 ml / g and 770 ml / g, with a polymer dispersion index (PDI) of 2.0–10.0, preferably in the PDI range of 2–7, and an alpha content in the cellulose of 86–98%. For experimental purposes, celluloses with average degrees of polymerization (DP) in the range of DP 400 to DP 1600 were used (DP determination by capillary viscometry according to DIN 54270).

[0096] The concentration of cellulose material in the ionic liquids used typically ranges from 1 to 20 wt%, depending on the degree of polymerization. Some studies have shown that higher concentrations of up to 20 wt% can be achieved, particularly when high-performance dispersants or special processing techniques are used. The choice of cellulose concentration in the ionic liquids depends on various factors, including the intended application, the type of cellulose, the solubility properties of the ionic liquid, and processing parameters such as temperature and treatment time of the cellulosic substrate. Higher cellulose concentrations have been shown to result in more viscous solutions, while lower concentrations (in the range of 12–17%) are better suited for the processing steps of the cellulose solution.The water content of cellulose solutions in ionic liquids can typically range from a few percent to 10 wt%. Ionic cellulose solutions can also be produced in a relatively dry consistency, particularly if they are manufactured, stored, and processed under an inert gas atmosphere. It is advantageous that the water content of cellulose solutions in ionic liquids is precisely adjusted, controlled, and monitored, as excessive water content impairs the quality of the ionic cellulose solution and the materials produced from it. It has been shown that a low water content leads to better cellulose dissolution and, overall, more stable cellulose solutions, while a relatively high water content increases the viscosity of the cellulose solution and leads to undesirable effects such as poor dissolution of the cellulose substrate and consequently poor spinning conditions.The ionic liquids used also enabled the processing of recycled pulp, cotton, and cellulose substrates from recycled textile and waste materials into filament strands. However, the raw materials used were cleaned and pretreated to remove impurities and improve their solubility in the ionic liquid. This can include steps such as crushing, grinding, extraction, washing, and / or removal of foreign substances.

[0097] The device according to the invention also enabled the processing of pulps with a hemicellulose content between 3% and 20% and glucomannan and xylan contents between 1% and 10%. The pulps used had a carboxyl and carbonyl group content of 15–40 pmol / g each, heavy metal contents of less than 10 mg / kg, and alkali and alkaline earth contents in the range of 100–500 mg / kg pulp. A description of the pulp analysis can be found, for example, in the reference at http: / / www.gruberscript.net / 23Zellstoffanalyse_chemisch.pdf. The organization TAPPI (Technical Association of the Pulp and Paper Industry) also develops and recommends, for example, the following measurement methods for pulp analysis: TAPPI T 204: Determination of the alkali resistance of pulp (cold-insoluble substance content). TAPPI T 236: Determination of kappa number of pulp; TAPPI T 237: Determination of the carboxyl group number of pulp.

[0098] To stabilize and prevent the degradation of the cellulose and the cellulose solvent (tertiary amine oxides, ionic liquids), radical scavenger chemicals such as propyl gallate, bases such as sodium hydroxide, and hydroxylamine are added in appropriate quantities according to the state of the art.

[0099] A spinning machine unit can be comprised of a single spinning station or multiple spinning stations connected together. The spinning / shaping of the cellulose solution is carried out using the dry-jet-wet spinning process. The cellulose solution (spinning mass) forced through the individual spinning capillaries in the extrusion device is extruded into an air gap located below the spinneret and drawn to achieve the desired fiber properties and quality requirements. The extruded cellulose solution can be drawn in the air gap using a moving gas stream, preferably conditioned air. After drawing, the drawn cellulose solution enters the coagulation bath below to precipitate the cellulose into filament or thread form.The cellulose is precipitated in an aqueous coagulation bath, while at the same time the solvent is partially extracted from the thread / filament and collected in the coagulation bath.

[0100] The following parameters were tested for the dry-wet process:

[0101] After coagulation, a partial wash is performed in the form of solvent extraction. The aim here is to partially remove the solvent from the cellulose filaments. Water is the preferred washing medium. The washing medium and the filament bundle pass together over a fluid bed / wash bath. A structured surface of the fluid bed (washing channel) creates and maintains turbulence in the washing medium, intensifying the washing effect. Additionally, the temperature of the washing medium can be increased to accelerate mass transfer.

[0102] The aqueous, solvent-containing, and highly swollen cellulose fiber bundle (cellulose multifilament) is continuously fed to a winding machine (primary winding) via guides after coagulation and washing. Here, the cellulose filaments are pulled forward and wound spirally in a crosswise pattern. Winding can be performed on any cylindrical or frustoconical bobbin (empty bobbin, tube, or other type of spool). Perforated bobbins of varying material compositions can also be used.

[0103] The following parameters were tested for partial washing and winding:

[0104] The apparatus for carrying out the invention is by no means limited to the devices and methods illustrated, but other conventional fiber production devices can also be used to transport the fiber bundle, guiding the cellulose fiber to a winding system. This means that other suitable devices for linearly guiding a fiber between the coagulation bath, washing, fiber surface stabilization, and winding or further processing can also be used.

[0105] Advantageous for the production of the product spool during the primary winding is the winding of the moist, highly swollen fiber filament cake in the form of a cross-spool, whereby the endlessly produced cellulose filament is continuously guided crosswise over a certain product spool length.

[0106] When winding, it is important to ensure that the initially moist fiber bundles are not compressed and wound too tightly, as this will adversely affect the subsequent treatment steps and damage the fiber bundle.

[0107] The fiber guidance from the extrusion nozzle to the primary winding is designed in such a way that the sensitive, primary spun fiber bundle is not damaged by shear forces.

[0108] The angle of the cross-wound filament is also adjusted accordingly to maintain a desired spool circumference, whereby, according to the invention, the cross-wound length of the product spool decreases in a specific ratio with increasing spool diameter, i.e., that an edge angle β of 90–70°, preferably 72–80°, results, or that the winding is adjusted so that the laying angle is 5–20°, preferably 10–14°. It has been shown that an initial laying angle of 13.5° over an initial length of 500–2000 m, followed by a uniform transition to a laying angle of 12° over a length of 500–7000 m, provides good treatment for the filament bundle.

[0109] The following parameters were tested for cross-winding: Test number speed Starting angle Initial length Laying angle Winder Note - m / min ° km ° Grades 1-3 7-1 230 27 7 11.5 1.5 7-2 240 27 3 12.5 2 7-3 235 28 5 12 1 7-4 230 29 7 12.5 1.5 7-5 235 28 5 12 1.5 7-6 240 29 7 11.5 1 7-7 240 27 7 12.5 1 7-8 230 27 7 12.5 2.5 7-9 230 29 3 11.5 2.5 7-10 230 29 7 11.5 2.5 7-11 240 29 3 12.5 3 7-12 240 29 3 11.5 1.5 7-13 235 28 5 12 2.5 7-14 240 27 3 11.5 1.5 7-15 230 29 3 12.5 1.5 7-16 230 27 3 11.5 1.5 7-17 230 27 3 12.5 1 7-18 235 28 5 12 3 7-19 240 27 7 11.5 2 Note: 1 - very good, 5 - bad

[0110] In the inventive method, a yarn winding machine is used, wherein the cellulose filament supply is provided by a continuous spinning machine.

[0111] The swollen cellulose filaments are fed to the winding station at a fixed speed to ensure uniform winding. The yarn winder is equipped with devices to control the winding speed. Additionally, the ratio of extrusion speed to winding speed is kept constant. This ratio, also known as the draw ratio, determines the desired production specification of the continuous filament yarn, expressed in units such as dtex or den. Selecting a suitable draw ratio also prevents overstretching or slack in the yarn during the winding process.Surprisingly, it was found that by adjusting the distance between the spool and the specially shaped, non-motorized deflection device(s), the change in filament yarn length caused by the oscillation process results in negligible titer fluctuations, making the cellulose filament bundle ideally suited for textile and technical applications. The yarn is laid onto a cylindrical or conical spool body by means of an oscillating yarn guide, through which the yarn is continuously fed back and forth. The linear movement of the yarn and the rotation of the spool support ensure that the continuously produced cellulose filament yarn is laid evenly on the typically perforated winding spool in a cylindrical, conical, or other desired geometric shape, while still moist and containing cellulose solvent.Spool holding systems consisting of at least one fixed spool unit are preferred. It is advantageous to use rotating spool holder systems, which consist of several individual spool holder systems for holding the wound spool or empty spool, and to connect the primary winding of the moist cellulose filaments with the continuously carried out spinning or thread manufacturing process.

[0112] The bobbin holding system or driven rotary thread winder comprises a turntable, a linearly operating thread displacement mechanism (changing device), and a drive rotation mechanism required for the automatically initiated rotation of the empty and product bobbin spindles arranged on the turntable. The turntable is rotatably connected to the fixed mounting plate, with at least one, preferably several, and even more preferably two bobbin spindles installed on the turntable.

[0113] The linear thread displacement and guidance mechanism (changing device) can be arranged in a housing that pivots towards the bobbin case. The force and rotation mechanism is located on the back of the mounting plate and is in transmission connection with the bobbin spindles. The bobbins (tubes, bobbins) are mechanically fixed (clamped) onto the rotating bobbin spindles.

[0114] If a thread winder has a revolving bobbin winding and holding system, when the desired bobbin weight (or other bobbin parameters such as length, diameter, etc.) is reached, the finished bobbin can be rotated around a centrally arranged axis of rotation, in a turret-like fashion, and turned into a finishing position in which the reserve bobbin body was located.

[0115] The empty reserve spool body is then rotated into the product production position by a turret-like turn. This ensures that the continuous cellulose filament spinning process is not interrupted. A rotating spool holding system can also be replaced by a non-rotating yarn winding system, in which case, after the finished spool, the moist, solvent-containing product spool is exchanged for an empty spool. This results in a brief interruption of the regular spinning process. For both rotating and non-rotating spool holding systems, the deflection can be caused by the movement of the changing device or by the movement of the rotating spool itself, resulting from the increase in diameter during the winding process.

[0116] According to the thread winder, which is able to automatically change the spool, when a spool with moist, highly swollen cellulose fiber yarn has been produced, it is rotated from the production position to the holding position, and the stand-by spool is rotated from the holding position to the production position in a turret-like fashion.

[0117] Since the yarn is automatically cut after the standby spool is rotated from the holding position to the producing position and vice versa, it can be wound onto the newly rotated spool. The spool, primarily wound and filled with moist cellulose yarn, is removed manually or automatically downwards, upwards, or to the side.

[0118] The winding of the produced yarn therefore begins anew, since, as mentioned above, by simultaneously replacing and rotating the full production spool, the reserve spool is moved from the reserve position into the production or starting position, allowing the fiber production process to continue continuously with the new winding.

[0119] The cellulose fiber yarn spool is now in the finishing position, with the desired and set production weight, and can be fed into the further processing of the process.

[0120] By using a multi-spool carrier system, the primary winding process can continue once the desired spool weight is reached, as the yarn winder has an automatic system for collecting the fiber cake. In the inventive method, an automatic changer that rotates through full spools or a simple mechanism to secure only the spool can be used. Alternative: Simple winding station: If a simple winding mechanism of a yarn winder is used, the primary winding must be interrupted by stopping the winding station when the desired production weight is reached. This also means that the continuously running spinning process must be interrupted before an empty reserve spool can be placed on for the next winding operation.

[0121] By employing a separate fiber production process according to the invention, which is not known in the prior art, with primary winding of a moist, solvent-containing, swollen cellulose fiber yarn, the continuously running yarn production process can be continued by using an automatically guided yarn winding process. The production efficiency of the process is increased while simultaneously reducing labor intensity and labor costs.

[0122] Modern yarn winders are often automated and equipped with controls to monitor the winding process. This can include adjusting parameters such as speed, tension, lay-up angle, winding density, yarn run detectors, etc. Spool body - Washing the wound cellulose filaments:

[0123] The winding core of the inserted coil, in the form of a bobbin, can be made of plastic, metal, or cardboard, either as a solid body or a perforated coil former. Metallic coil formers can be made of solid cylindrical or frustoconical aluminum, natural aluminum, powder-coated aluminum, stainless steel (ground on one side, bright on the other), or dimensionally stable plastics such as polypropylene (PP), as well as other plastics.

[0124] If perforated coil bodies are used in the process, the perforation of the coil body can be round hole, square hole, round oblong hole, rectangular oblong hole, as well as in all possible special hole shapes such as hexagon, square hole, diamond hole, triangular hole, keyhole, star hole and / or in combination as well as in any shape.

[0125] If a perforated spool body is used in the inventive method, the perforated spool area of ​​the empty spool should be approximately 10–40% of the total spool surface area. Preferably in the range of 15–30%, more preferably in the range of 20–30%. This enables a rinsing or washing liquid flow rate of 1,000–10,000 liters / min per spool and a spool liquid flow rate of 10–50 liters / min per spool, or, based on the surface area, 50–500 liters / min per m² of spool surface area or 2–50 liters / min per kg of dry cellulose filament cake (cake washing liquid).

[0126] The following parameters were tested for washing the wound cellulose filaments: Attempt coil former perforated surface to total surface Number of spools used in laundry Rinsing liquid flow rate z, empty Flush liquid flow rate Flushing fluid flow rate per surface Cake washing liquid Washing result n % Liters / min per coil Liters / min per coil Liters / (min*m²<) Liters / (min*kg) School grade 1 A 10 1 2355 96 68.3 4.0 3 2 A 10 2 1920 11.9 104.9 5.5 4 3 A 10 5 2010 8.5 53.5 3.9 4 4 A 10 5 4320 10.6 83.2 5.7 3 5 A 10 10 6900 11.9 104.9 3.7 4 6 A 10 10 5250 9.4 65.5 5.3 4 7 A 10 50 5505 7.8 45.1 2.8 5 8 A 10 50 6075 11.5 98.0 3.6 5 10 B 22 1 1800 19.4 126.2 10.7 3 11 B 22 2 2580 25.5 219.3 8.3 2 12 B 22 5 6480 26.0 226.9 13.6 2 13 B 22 5 3780 17.6 104.3 11.6 2 14 B 22 10 4080 25.5 219.3 16.8 3 15 B 22 50 7200 26.6 238.6 18.0 3 16 C 28 1 2640 32.8 283.9 19.5 1 17 C 28 2 6180 36.1 345.1 18.2 2 18 C 28 5 3540 22.4 132.7 14.6 1 19 C 28 10 7740 23.5 146.3 79 2 20 C 28 50 4140 30.5 246.4 14.3 2 21 D 37 1 6660 33.3 222.0 11.7 1 22 D 37 2 4680 37.4 279.6 17.2 1 23 D 37 5 3120 36.3 263.2 13.6 2 24 D 37 10 4680 45.9 421.4 259 1 25 D 37 25 6840 34.8 242.2 19.1 2 26 D 37 50 3780 28.9 166.7 18.0 2 School grade: 1 - very good, 5 - poor

[0127] Better washing results were achieved with perforated coils.

[0128] Plastic spools for dyeing textile yarns, also known as plastic dyeing cones, plastic dyeing tubes, etc., can also be used in the primary and secondary winding according to the invention.

[0129] Positive properties of plastic textile yarn dyeing spools include their relatively light manufacturing process, chemical stability, insulating properties, and excellent strength. This is achieved because the plastic dyeing spools, for example those made of polypropylene, can be reinforced with glass fibers during the injection molding process. This ensures higher temperature resistance and dimensional stability. Their long-term thermal resistance is approximately 120 °C, making them suitable for hot water or hot water under increased pressure.

[0130] In the primary winding step according to the invention, coil formers are used in diameter dimensions of 30 to 80 mm, in coil former lengths of 150 - 300 mm, in the materials polypropylene (PP), high temperature resistant polypropylene (HT-PP), or in the material mixture of polycarbonate (PC) and acrylonitrile butadiene styrene (PC / ABS).

[0131] Other coil formers that can be used in the primary winding process according to the invention are called "dye springs" or "one-way dye springs." These are also perforated and can be used as stackable disposable coil formers or reusable coil formers. The various perforations give the coils a certain elasticity in the radial direction. These "springs" serve to hold the moist cellulosic continuous filament securely and in shape during the washing and post-treatment processes.

[0132] The spools used should be compressible to minimize mechanical stress on the filament yarn during the washing process. This mechanical stress occurs when the solvent is replaced by detergent during washing, which can cause shrinkage or expansion of the spool cake. The wound spools can also be subsequently covered with nonwoven fabric for further use in the washing process. This facilitates efficient processing during secondary winding.

[0133] Parallel washing machines are available for washing the wound cellulose fibers. In these machines, the cross-wound reels are washed solvent-free in stages. The reels are placed on special supports into the parallel, batch-operated washing machines and pass through various washing stages, with each stage (washing cycle) lasting approximately 15-120 minutes on average. The washing liquor is kept moist with a batch volume of 2-8 liters per kilogram of cellulose substrate. The liquor is heated to a temperature of approximately 90 °C and pressurized to 1.1-3 bar. The parallel washing machines are operated an average of 2-50 times per day to achieve an annual production capacity of, for example, 5,000 tons.

[0134] The solvent-free washed cross-wound coils emerging from the washing units can then be subjected to a pre-drying step and / or mechanical dewatering. Alternatively, the solvent-free washed cross-wound coils can undergo further treatments before the pre-drying step, as described above. By arranging several washing units in parallel, the process is converted into a "quasi-continuous washing process." The system components can be used, on the one hand, to remove the solvent from the cellulose substrates; on the other hand, if appropriate, further fiber substrate treatments, such as dyeing, are also possible in the multi-purpose units, with the operations being carried out separately. The required heat can be supplied by direct or indirect heating with steam, water, gas, electricity, or oil.

[0135] The washing liquid derived from the washing process, containing the aforementioned cellulose solvents, such as amine oxides or ionic liquids, is recycled to the spinning process and the spinning bath as a diluent and precipitating agent. The process according to the invention is not limited to recycling the enriched wash water into the spinning process; rather, specially installed washing liquors, purification, and recovery processes can run in parallel with the yarn production process or independently. For example, washing liquors, filtrations, ion exchange systems, membrane processes, and evaporation processes can be used to separate solids and water or for liquid / liquid separation. Corresponding apparatus and processes can be used individually or in combination.

[0136] The following parameters were tested for washing the wound cellulose filaments: Key figure Unit 9-1 9-2 9-3 94 9-5 9-6 9-7 9-8 9-9 9-10 9-11 9-12 Packing density in the car wash % 50 53 64 50 23 32 81 71 79 57 77 74 Fleet ratio - 1:10 1:10 1:10 1:40 1:20 120 1:20 L3 1:6 1:6 16 1:6 Number of washing levels - 4 5 3 3 4 5 8 9 5 6 8 5 Duration of washing cycles min 49 59 48 4 49 10 6 16 43 13 31 52 Pressure drop across the cake bear 13 24 0.5 0.1 L6 0.2 0.6 0.3 1.7 17 21 1.8 Result of the washing School grade 2 3 1 3 2 3 5 1 4 5 3 3

[0137] The washing process is carried out by pressure washing, whereby the washing liquid can move both from the inside out and from the outside in. The packing density of the product spool in the washing system, together with the resulting pressure drop, determines the effectiveness of the washing and the resulting number of washing stages. Between washing stages, the detergent is exchanged in the opposite direction. The packing densities in the trials ranged from 50% to 83%. The liquor ratio ranged from 1:3 to 1:40, with the best washing results achieved in trials 9-3 and 9-8. Sufficient washing time, combined with an adequate liquor ratio and moderate pressure, is likely responsible for the good washing results. Pre-drying or centrifugation:

[0138] After washing, the moist, now (essentially) solvent-free cellulose filament can be mechanically separated.

[0139] In this process, a centrifuge rotating the spool generates a centrifugal force strong enough to separate the water from the swollen cellulose filament yarns, causing it to exit the spool radially. A rotational speed of 6500 rpm has been shown to produce a suitable and sufficiently dry filament cake, reducing the moisture content from an initial 230% to as low as 130%. This offers a significant advantage for subsequent processing steps, as it reduces the required drying energy. However, the same treatment can also be achieved by performing an intermediate drying step.

[0140] The following parameters were tested for the centrifugation of the cellulose filaments: Key figure Unit 9-1 9-2 9-3 9-4 9-5 Initial moisture content rel.% 229 191 190 199 210 Residual moisture rel.% 105 122 192 163 135 Rotational speed of the coil in the centrifuge rpm 3500 7000 4300 5000 6500

[0141] If the coils are subjected to thermal dewatering to reduce their water content, the coils from the cake washing process must be removed from the pressure washing unit and fed into a dryer. However, the pressure washing tank can also be connected to a steam and compressed air supply to largely remove surface water before drying.

[0142] Before reducing the water content by thermally heating the coil bodies, the product coils of the cake washing process can be removed from the perforated pressure washing tubes and subjected to mechanically guided dewatering, such as centrifugation, and thus pre-dried.

[0143] For drying, the cellulose filament spools are either removed directly from the cake washing or from the centrifuge, subjected to the treatments mentioned above, and fed into the drying step.

[0144] The subsequent drying process can be carried out in a high-frequency oven, microwave dryer, tray dryer, or similar appliance, where the desired moisture content can be adjusted or the drying process can be completed. In these ovens, additional dry air or hot air can be blown in and extracted to even out the heating and to remove any steam and moisture that may be produced.

[0145] Drying devices equipped as high-frequency dryers have proven to be superior to mechanical drying devices (EP 0075797 B1). Furthermore, the necessary singulation or combination of the coils for further processing, such as packaging, can be easily integrated into a subsequent automated process after drying.

[0146] The moist primary product reels, emerging from the cake washing process step where solvent removal in a pressure vessel and / or further chemical treatment takes place, are fed into a drying system. The pressure vessel itself, or several adjacent pressure vessels, can serve as the drying system.

[0147] The cellulose fiber spools fed into the drying system, already mounted on a perforated spool sleeve after coming from the cake washing process, can be placed on perforated tubes of a pressure tube dryer. The drying agent, such as hot air, is then passed through these tubes. The hot air exiting the perforated tubes subsequently flows through the perforated washing spools for pre-drying or final drying of the produced cellulose fibers.

[0148] The cellulose filaments can be rewound after or during the processing steps, i.e., transferred to other spool bodies (secondary and tertiary winding). It is advantageous for the process flow to partially dry the cellulose filaments before secondary winding. According to the invention, intermediate drying is carried out by removing a portion of the water bound in the spool using a thermal, mechanical, or other method. The drying process is designed so that the escaping water is transported away very gently and homogeneously across the entire cross-section. On the one hand, as much water as possible must be removed, and on the other hand, enough water must remain on the spool so that it can be easily unwound during secondary winding. A relative humidity in the range of 50–200% (particularly preferably 120–150%) is preferred.Preferably, this partial drying should be carried out in such a way that homogeneous moisture is achieved across the entire coil.

[0149] Surprisingly, it was discovered during the experiments that a spool that had dried completely after washing could no longer be unwound, or only with great difficulty. For this reason, a suitable release agent, such as fatty acid esters, mineral oils, silicone oils, and other suitable substances, is applied to the filament using a suitable technical device, such as an oil roller, during secondary winding. Before secondary winding, the filament is in an initially moist or, preferably, a partially dried state.

[0150] For this purpose, the coil is unwound and subjected to the treatment described above, and then rewound onto a coil blank. The winding should be done in such a way that the coil retains its shape, but also very loosely, so that it is suitable for the subsequent process steps. A cake density of approximately 0.3–0.5 kg / L has proven very useful in this regard.

[0151] During the trials, it was found that drying in the wound state proved to be particularly gentle and advantageous for the fiber properties. According to the invention, drying is achieved by supplying energy in a thermal, electromagnetic, convective, or other suitable form. Preferably, the drying process is carried out as homogeneously as possible until a desired residual moisture content is reached, which allows for trouble-free rewinding. Surprisingly, it was found that the packing density decreases during drying. This effect contributes to gentle drying and thus promotes the production of high-quality fibers.

[0152] During drying, the packing density decreases. To obtain a stable coil as the final product, the coil is preferably rewound a second time (tertiary winding) to achieve a final shape preferred by the customer. The winding parameters are selected to produce a stable final coil. The relative humidity for this process step is between 60-90%, preferably between 75-85%.

[0153] A final conditioning process can then be carried out, e.g., storage at the desired humidity or drying to achieve the appropriate final fiber moisture content. Drying is again achieved by supplying energy in a thermal, electromagnetic, convective, or other suitable form.

[0154] Quantitative determination of the degree of crystallinity xc and the crystallite sizes D (hkl) by wide-angle X-ray scattering (WAXS): To obtain an isotropic preparation, the fibers were manually cut into a fine powder with scissors and then prepared in a 2 mm thick sample carrier between two PET films (isotropic powder preparation). The wide-angle X-ray analysis was performed with a Bruker-AXS D5000 dual-circuit diffractometer in symmetrical transmission using monochromatic (Ge(111) primary monochromator) Cu-Kα radiation (λ = 0.15406 nm) at 30 mA and 40 kV. The diffractograms were recorded in the 2Θ angle range of 4°–104° (step size Δ2Θ = 0.2°, measurement time / Δ2Θ: 55 s). The sample rotated around the sample standard at 15 rpm during the measurement. The entire angular range was measured three times to improve the statistics.

[0155] Using WAXS7 software, based on the Ruland-Vonk method for determining the degree of crystallinity, the degree of crystallinity xc and a disorder parameter k, which is a measure of the lattice defects in the crystallites, were determined from the normalized scattering curves. The mean crystallite sizes D (hkl) were determined from the half-widths of the crystalline X-ray reflections of the lateral principal reflections (1-10), (110), (020), and (004) according to the Scherrer formula: D hkl = 0.9 λ / β cos Θ (λ = 0.15406 nm, β = full width at half maximum) Tabel: Sample no. degree of crystallinity xc [%] k [10 -2< nm -2< ] modification 1 46 1,7 Cellulose-II 2 48 1,7 Cellulose-II 3 44 1,6 Cellulose-II 4 48 1,9 Cellulose-II 5 47 1,7 Cellulose-II Sample number Crystallite sizes D (hkl) [nm] (1-10) (110) (020) (110)+(020) (004) 1 4,2 4,2 3, 9 8,1 8, 8 2 4,5 4,4 3, 9 8,3 9, 8 3 4,4 4,4 3,4 7,8 9, 4 4 4,4 4,1 4,1 8,2 10,2 5 4,6 4,5 3,6 8,1 9, 5 Scanning electron microscopy (SEM)

[0156] For surface analysis, the fibers were horizontally bonded to the sample carrier using an electrically conductive substrate. To create cryogenic fractures, a fiber bundle was immersed in liquid nitrogen and broken after freezing. The fiber bundle was then mounted vertically on a conductive substrate on the sample carrier. Finally, the fiber samples were sputtered with a platinum layer (4 nm thick) to prevent electrostatic charging. The investigations were performed using a GeminiSEM 300 SEM (Zeiss, Germany), operated at an accelerating voltage of 5 kV and the lowest possible beam current to minimize radiation damage and fiber charging. SEM results of the fiber surface and cryogenic fracture are presented in the Figures 3 and 4 shown. Crystalline fiber orientation

[0157] Wide-angle X-ray scattering (WAXS) measurements were performed to determine the fiber orientation.

[0158] A layer of parallel cellulose fibers was fixed with cyanoglue to a fiber sample holder with a hole diameter of 2.3 cm (oriented fiber preparation). To determine Hermans' orientation factor fc as well as other orientation parameters (OG (hkl) and OGI (hkl) ), the distribution of the (004) lattice plane reflection (chain direction reflection) of the cellulose structure was measured.

[0159] First, the exact angular position of the maximum of the (004) reflection at 2Θ ~ 34.6° was determined using a Θ / 2Θ scan. Subsequently, with Θ and 2Θ constant, the distribution of the (004) lattice planes was recorded using a Φ spinner scan in the Φ angle range of 60° to 120° (assumed maximum of the distribution at 90°). The measurement was performed on a Bruker-AXS D5000 dual-circuit diffractometer in symmetrical transmission using monochromatic (Ge(111) primary monochromator) Cu-Kα radiation (λ = 0.15406 nm) at 30 mA and 40 kV. The step size ΔΦ was 0.2°, and the measurement time was 180 s / ΔΦ.

[0160] To quantitatively analyze the orientation of the (004) lattice planes and thus the distribution of the oriented cellulose molecule axes of the crystalline regions in the fiber direction, the orientation parameters fc and OG(hkl) were determined. Before calculating the crystalline Hermans orientation factor fc, a linear background was subtracted from the scattering curves. Since the background is formed by the isotropically distributed lattice planes, neglecting the small amount of air scattering, an integral orientation parameter OGI(hkl) can be used as a measure of the proportion of oriented lattice planes to the total number of scattering lattice planes. OGI hkl = ∫ I hkl ori / ∫ I hkl ori + ∫ I hkl iso (I (hkl)ori = intensity oriented lattice plane (hkl), I (hkl)iso = intensity isotropic lattice plane (hkl)) can be determined.

[0161] The fiber orientation of two samples was determined. The first sample is a conventionally produced reference sample with continuous processing, immediate in-line washing and drying, and winding; and the second sample is produced according to the invention with moist, solvent-based winding followed by subsequent washing and drying. The results of the calculation of the various orientation parameters are given in the following table. sample FWHM [°] OG(004) OGI(004) FC comparison sample 12,264 0, 932 80 0, 965 sample according to the invention 14,321 0, 920 73 0, 954

[0162] Comparing the determined orientation parameters OG(004) of the two fiber samples, the fiber sample according to the invention exhibits a significantly lower orientation compared to the reference sample. The half-width of the distribution curve is significantly higher, resulting in lower values ​​for the orientation parameters OG(004) and fc. The proportion of oriented regions (OGI) is also lower than in the reference sample. Reference symbol list

[0163] 1 Spinning unit 2 Deflection roller 3 Partial washing unit 4 Yarn winder 5 Further deflection roller 6 Spool washer 1a Extrusion plate 1b Gas gap 1c Coagulation bath 1d Cellulose filaments 4a Spool 4b Winded cellulose filaments 4c Change yarn guide

Claims

1. A device for solidifying and winding cellulose multifilaments, comprising an extrusion unit with at least 10 openings for forming filaments, a coagulation unit for solidifying the filaments, and a thread winder for winding the cellulose filaments, characterized by the fact that The device contains no or only a partial washing system for washing the cellulose filaments or for extracting a cellulose solvent from the cellulose filaments between the coagulation system and the thread winder.

2. Device according to claim 1, wherein the partial washing system has a maximum length of 5 m.

3. Device according to claim 1 or 2, wherein the partial washing system has one, two or more washing channels or fluid beds, wherein a washing channel or fluid bed is positioned for washing a cellulose multifilament or for extracting a cellulose solvent from a cellulose multifilament.

4. Device according to one of claims 1 to 3 with a deflecting device, preferably a deflecting roller, for deflecting cellulose threads which are solidified in the coagulation plant; wherein preferably the deflecting roller is rotatably mounted and / or is not driven by a motor; and / or wherein there is no motorized deflecting roller between the coagulation plant and the thread winder.

5. Device according to one of claims 1 to 4, wherein a changing thread guide is provided on the thread winder.

6. Device according to one of claims 1 to 5, wherein the device has one, two or more spools, wherein two or more spools are wound in parallel and / or one, two or more spools are provided with a changing thread guide.

7. Device according to any one of claims 1 to 6, wherein the device further comprises a spool washer for washing or extracting cellulose solvents from cellulose filaments wound on a spool.

8. A method for the production and processing of cellulose multifilaments comprising forming at least 10 cellulose filaments and solidifying the at least 10 cellulose filaments in a coagulation plant, wherein the solidified cellulose filaments are moist and contain solvents of cellulose, and winding the moist, solvent-containing cellulose filaments.

9. The method of claim 8, further comprising partially washing or extracting the cellulose solvent from the cellulose filaments, whereby the cellulose solvent content of the cellulose filaments is reduced but not completely removed and the cellulose filaments remain moist.

10. Method according to claim 8 or 9, wherein the winding creates a tension on the cellulose filaments which continues until solidification and determines the unwinding speed of the cellulose filaments after solidification.

11. Method for processing freshly spun cellulose multifilaments, wherein a cellulose multifilament comprises at least 10 cellulose filaments, comprising winding at least one solvent-containing cellulose multifilament onto a spool.

12. Method according to any one of claims 8 to 11, wherein the cellulose filaments have a packing density of 0.8 g / cm³ 3 up to 1.3 g / cm³ 3 moist cellulose filaments are wound and / or wherein the cellulose filaments are packed with a density based on dried cellulose filaments of 0.2 g / cm³ 3 up to 0.7 g / cm³ 3are wound up; and / or wherein the cellulose filaments are wound up at a laying angle of 5°-20°, preferably 10-14°.

13. Method according to any one of claims 8 to 12 wherein the wound multifilaments are washed on a spool, preferably with a washing liquid throughput of 1000 to 10000 liters per minute and / or 2 to 50 liters per minute and per kilogram of dry cellulose filament; and / or wherein the wound multifilaments are dewatered on the spool.

14. Cross-coil with at least one moist wound cellulose multifilament, wherein the cellulose multifilament comprises at least 10 cellulose filaments, wherein the cross-coil has a coil body as a support which is cylindrical, and the cellulose multifilament is wound onto the coil body with a laying angle of 5°-20°.

15. Cellulose filament which has been wound while containing cellulose solvent and / or wet and dried in the wound state, and has a region with periodic indentations, wherein indentations in the region are present every 5 µm to 1000 µm; and / or has a Hermann orientation factor fc of less than 0.965, preferably of 0.951 - 0.958.

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