KR100652153B1 - Method and device for producing cellulose fibres and cellulose filament yarns - Google Patents

Abstract

The invention relates to a method for producing cellulose fibres or filaments from cellulose according to the dry-wet extrusion process, using aqueous amine oxides as the solvent. According to said method a) cellulose with a cuoxam-DP in the region of between 250 and 3000 is dispersed in an aqueous amine oxide, b) the dispersion obtained is converted at a high temperature by dehydration and shearing into a homogenous solution with a zero shear viscosity in the region of between 600 and 6000 Pa•s at 85 DEG C, c) the solution is fed to at least one spinneret, d) the solution in each spinneret is formed into at least one capillary and the capillary or capillaries of each spinneret are drawn through a non-precipitative medium and are subsequently guided through a spinning bath where the cellulose fibres are precipitated and e) at the end of the spinning bath section, the cellulose fibres are separated from the currents of the spinning bath by deviation and the threads are drawn off. The method is characterised in that the dispersion in step b) is converted into a solution with a relaxation time of between 0.3 and 50 s at 85 DEG C and that the solution in step c) is passed through a flow chamber, common to the spinnerets, in which the residence time of the solution is at least equal to its relaxation time at the spinning temperature.

Description

Method and apparatus for the production of cellulose fiber and cellulose filament yarn {METHOD AND DEVICE FOR PRODUCING CELLULOSE FIBRES AND CELLULOSE FILAMENT YARNS}

The present invention relates to a process for producing cellulose fibers or cellulose filament yarns from cellulose using a dry-wet extrusion process using an aqueous amine oxide, in particular N-methylmorpholine-N-oxide, as a solvent. According to the method, a) dispersing a cellulose or cellulose mixture having quoxam-DP in the range of 250 to 3000 in an aqueous amine oxide, and b) dehydrating and shearing the resulting dispersion at a high temperature of 600 to 6000 Pa at 85 ° C. Converting to a homogeneous solution having a zero shear viscosity in the range of s, c) feeding the solution to at least one spinneret, and d) at each spinneret the solution is formed into at least one capillary The capillary (s) of each spinneret is led through a spinning bath zone where it is drawn through a non-precipitating medium and then the cellulose fibers precipitate, and e) deviation from the flow of the spinneret at the end of the spinneret zone. By separating the cellulose fibers, the yarn is pulled out. The present invention also relates to a spinneret table and a spinneret, a spinneret connected to two vessels by means of a spinneret pump, between the surface of the settling tank and the spinneret in the upper one of the two vessels, according to a wet and dry extrusion method using an aqueous amine oxide. A device for producing cellulose fibers or filament yarns from cellulose using a spinning device comprising a gap, and at least one take-up godet.

US Pat. Nos. 4,246,221 and 4,416,698 dissolve cellulose in tertiary amine oxides containing water, shape these solutions under minimal shear in a spinning capillary and stretch the resulting solution filaments in a large air gap at low draw rates A method of precipitating cellulose in an aqueous spinning bath containing amine oxides and winding the filaments using a Godet is presented. It has also been pointed out that the filaments can interlock with each other in the air gap, and it is proposed to wet the surface of the filaments using rollers. DD-A 218121 proposes the use of polyolefinic ethers as additives in spinning solutions to avoid the problem of filament deadlocking in the air gap.

U. S. Patent No. 5,417, 909 describes the formation of solutions under medium to high shear forces in spinning capillaries, the ejection of solutions in short air gaps under medium to high draw rates, and the filaments or filaments through precipitated cellulose and spinning funnels. The band of is captured and presented in a direct flow. The relatively short air gap prevents filaments from interlacing and allows spinning at capillary densities up to 3 K / mm 2.

International Patent Publication WO 96/20300 describes the relationship between the distance between two radiating capillaries and the spinneret and the distance between one bundle element and the other air gap and the cellulose at an angle of less than 45 degrees. A device for winding fibers is presented.

EP-A 0 832 995 finally proposes a device comprising a swivel focusing element which ensures that the angle between the outermost filament and the center perpendicular to the spinneret is within 20 degrees in a small air gap. have.

In EP-A-0 584318 and 0 671492 it is proposed to blow into each of the devices to provide cooling airflow or the spinning chamber to increase the density of the capillaries. EP 795052 proposes air as a refrigerant containing a certain amount of moisture. WO 94/28218 proposes a method and apparatus for blow molding a seal in an air gap, and finally WO 96/21758 proposes a blow molding of a seal in two areas.

Both these methods and apparatus aimed at the largest possible spinneret with very high spinning stability and high capillary density in the spinning of fibers with sufficient air gap. In the spinning of cellulose filament yarns, the demands are relatively low in terms of capillary density, but the limits of fineness depending on the spinneret size clearly lead to higher demands on the winding speed.

In all methods, the non-contact induction of the filament through the air gap, the cooling of the cellulose in the air gap and / or precipitation on the surface by blow molding use of wet gas, the length of the air gap and the like are priorities. The distance the yarn must reach in the spinning chamber and the frictional forces caused by it are largely not taken into account. The turning of the barrel member in EP-A 0 832 995 thus extends the distance of the bath in the angular reduction between the filaments. Partial precipitation of cellulose in the air gap by blow molding with wet air makes the orientation quite difficult. This situation is only considered in US Pat. No. 5,417,909, which uses a spinning funnel to pass the yarn simultaneously with the spinning bath. The frictional force between the yarn / spun yarn increases greatly with distance and speed of the yarn, reducing the mechanical value of the fiber. This situation in the spinning of the fiber is attempting to compensate using a low winding speed.

In the spinning step of the filament yarn of U.S. Patent No. 5,868,985, it is proposed to be able to work at high winding speeds in the direction of the yarn flowing through the yarn passage of 0.5-8 cm. This arrangement, working with an air gap of 18 cm, is only suitable for easy spinning with very low capillary densities, for example as for only short fibers.

It is an object of the present invention to provide a method and apparatus capable of spinning of fibers and multiple spinning of filament yarn having good mechanical properties of the fibers at high capillary density, spinning safety and high winding speed as mentioned at the outset. In particular, it is intended to increase the identity and regularity of the flow through each spinneret compared to conventional methods. Furthermore, it is an object to achieve this purpose without blow molding in capillaries extruded into the air gap using air or similar gases. Other advantages will be appreciated from the description below.

The object is that, as mentioned at the outset, the dispersion in step b) is converted to a solution having a relaxation time of 0.3 to 50 seconds at 85 ° C., and the solution in step c) is a flow chamber common to the spinneret. Passing through, the residence time of the solution is achieved in a process which is at least equal to the relaxation time of the solution at the spinning temperature. Preferred relaxation times range from 1 to 5 seconds at 85 ° C.

Spinning cellulose solutions in hydrous amine oxides results in very pronounced viscoelastic properties. As a result of this, the energy required for the transport and shaping of the spinning solution in the spinning channel is elastically reduced and back-shaping is induced after removing external forces during the relaxation time.

The residence time in the flow chamber exceeding the relaxation time results in complete relaxation and, together with the zero shear viscosity above each spinneret, the current pressure equalizes the volumetric flow through each spinneret.

Measurements of relaxation time from rheological data of cellulose solutions are described in detail in the literature (CH. Michels, Das Papier, 1998 1, S. 3-8). Since cellulose actually exhibits a molar mass distribution, the solution has a relaxation time spectrum. The relaxation time spectrum, ie the relative frequency H ^* for the relaxation time λ of four solutions of different cellulose pulp, is shown in FIG. 1. The relaxation time λ _m is the relaxation time according to the frequency maximum.

In one embodiment according to the invention, cellulose or a mixture of cellulose is pretreated by an enzymatic process. This reduces the variation in the molar mass distribution of certain cellulose pulp. For example, the bimodal distribution of spruce sulfite cellulose is changed to a monomodal distribution.

In another embodiment of the invention for the preparation of a cellulose mixture, first the cellulose with cuoxam-DP is dispersed in water in the region between 600 and 3000, and then the cellulose with cuoxam-DP is between 50 and 600. In the area of and further dispersed, and then the cellulose mixture is separated from water and dried in water to be fed to step a).

The capillaries extruded in a suitable form pass through the non-precipitated medium almost in parallel, individually, then through the spinneret zone of less than 20 cm in length. The friction between the yarn and the yarn is significantly reduced here by arranging the spinneret and the thread guide described below in a position where the threads do not contact each other and making them mostly parallel through the short spinneret zone. The spinning zone is preferably less than 5 cm. The mass of the bath in the circuit for settling and transporting the yarn is very small, 1.5 to 7 liters per spinneret.

In step e) it is preferred that the cellulose fibers are separated from the flow of the spinning bath by deflecting at an angle of β> 10 ° and the yarn is drawn to a maximum fiber tension of 5 cN / tex. The yarns are separated by β-angle deflection of the laminar flow and falling yarn flow, and are captured under the tension by the winding Godet and adjusted to the desired winding speed v _a . The drawn yarn may be washed and finished and dried with a single filament yarn or joined to thread tow by thread guides to be washed, cut and volumed as a fiber and then worked and dried.

It is also an object of the device as mentioned at the outset to install, according to the invention, a common flow chamber having a volume satisfying the following equation on a spinneret table with spinnerets arranged in one or more rows or groups. Is achieved by:

Where V is the cm 3 unit volume as the flow chamber, v _L is the cm 3 / sec unit as the flow rate of the cellulose solution, and λ _m is the relaxation time of the spinning solution at the maximum frequency of the relaxation time spectrum. The relaxation time λ _m is the intrinsic value of the solution, the measurement of which is described in Ch. In the analysis of michels it is described in particular in the section "Versuchsdurchfuehrung" on pages 3 and 4. This is included in the description herein. At the chamber capacity of this dimension, the uniformity of the flow rate of the spinning solution supplied to one or more of the spinnerets using the spinning pump reaches an optimum value.

Another feature of the invention is the device according to the invention, as mentioned at the outset, characterized in that the width of the air gap and the relaxation time of the spinning solution satisfy the following equation:

Where a is the width of the gap in mm, λ _m is the relaxation time of the spinning solution at the maximum frequency of the relaxation time spectrum, in seconds, and v _a is the winding speed, in units of m / min. It can be seen from the above equation that there is a correlation between the relaxation time and the gap width that increasing the relaxation time can increase the air gap width without reducing the capillary density or winding speed of the spinneret or impairing the safety of the spinning operation. Can be. Thus, the air gap can be increased at the set diameter of the capillary tube with increased relaxation time. That is, the width of the air gap required to achieve high fiber quality with high safety spinning operations (low stretching speed, no capillary deadlock, etc.) can be controlled by the relaxation time of the solution.

Preferably the spinneret, the width of the air gap and the dimension of the spinneret region satisfy the following equation:

Where X is the distance between two adjacent spinneret holes, a is the width of the air gap, w is the length of the spinneret zone, and D is the diameter of the spinneret hole. Each dimension is described in more detail in FIG. 6.

In a preferred embodiment of the device according to the invention, a thread guide member, preferably composed of ceramic, is inserted into the bottom of the upper container. These thread guide members penetrate the bottom of the vessel, through which the set of threaded threads exits the upper spinneret vessel with the spinneret flow. The thread guide member leads to the outlet of the spinning bath in the laminar flow, whereby each fiber bundle is independently captured and accelerated. In a preferred form the spinneret and the thread guide member have the same arrangement. Preferred thread guide members are arranged in rows or groups. In a spinneret table, for example, an array of small spinning hats with a diameter of 12.5 mm or 20 mm and in a single row (preferably filament) or in a plurality of rows (preferably fibres) may be used to In a manner that is connected to the line and is almost parallel and captured from the winding roller or the winding roller. For example, it is desirable for 360-1020 or more capillaries to be arranged in a spinneret area of 90 to 250 m 2 per small cap upon spinning of the fiber. The capillary density is therefore at least about 4 / mm 2.

In a suitable form, the spinneret exhibits the shape of a small cap and the spinneret area occupied by the spin capillary is less than or equal to the inlet area of the thread guide member. Here the thread is mostly parallel and passes through the bath without touching each other.

Preferably the ratio of the inlet diameter to the outlet area of the thread guide member is E / e ≧ 1 and the rim is rounded at the outlet. These thread guide members were preferably used for the production of the fibers. They generally extend at least to the total depth of the bottom of the vessel and have a height of 2 to 20 mm.

In another embodiment, the thread guide member exhibits a ratio of height to diameter of the exit area with h / e < 1 and the rim is rounded at the exit. These thread guide members have been used for the manufacture of filament yarns and generally have a height of 2 to 5 mm. The inlet diameter E of the thread guide member or the accompanying bottom opening ranges from 12 cm to 20 cm. The exit diameter of the thread guide member is in the range of 4 mm to 10 mm. The structure of the thread guide member surfaces is such that the yarn and the yarn passing between those surfaces cause minimal friction. This object is also achieved by rounding the rim.

The upper vessel preferably has one feed opening which is connected downstream to a stabilizing chamber. The stabilization chamber may comprise, for example, a flow zone filled with filler and a downstream flow zone without filler, ie a hollow flow zone. The spinning chamber pumped from the stabilization chamber is decelerated to necessarily flow into the laminar flow into the spinning chamber.

In a suitable embodiment, the upper vessel has at least one overflow that can match the overflow height. By displacing the overflow in the vertical direction, it is possible to change the zone of the bath, with the result that further advantages are obtained, especially when starting radiation.

The position of the upper spinneret is preferably opposed to the spinneret which is adjustable in the vertical direction. This arrangement and displacement of the vertical overflow can change the width of the air gap.

It is also possible to adjust the winding goth disposed under the upper spinneret vessel in the vertical direction and / or in the horizontal direction. This makes it possible in particular to adjust the angle β of the thread displacement, in particular from the falling flow of the spinning bath.

The method and apparatus according to the present invention are described in more detail with reference to the drawings and embodiments.

1 is a graph of relaxation time spectra of four different cellulose solutions,

2 is a schematic diagram of an apparatus for carrying out a method according to the invention,

3 is a schematic view from above of the device shown in FIG. 2;

4 is an axial cross-sectional view of one embodiment of a thread guide member preferred in the case of fiber spinning;

5 is an axial cross-sectional view of another embodiment of a thread guide member preferred in the case of filament yarn spinning,

FIG. 6 is a geometrical diagram of a spinning process to illustrate the geometric dimensions of each part of relation (III). FIG.

FIG. 1 shows the relative frequency H * of the relaxation time of four cellulose solutions from different celluloses with aqueous N-methylmorpholine-N-oxide as solvent, details of which are shown in the table included in FIG. Can be. Where λ _m is the relaxation time at the maximum frequency, the unit is second, DP is the degree of polymerization of cuoxam, ηo is the zero shear viscosity of the solution, the unit is Pa · s, and c is the concentration of the cellulose solution in%. The relaxation time λ _m shown in equations (I) and (II) correlates with the width of the air gap and is the current relaxation time at the relative maximum frequency. The solution p9915102 contains a cellulose mixture in which the relaxation time of spruce sulfite cellulose (Quoxam-DP; lambda _m = 1.6 sec) is increased to lambda _m = 2.1 sec by adding a proportion of high molecular weight cellulose.

2 shows a spinning device comprising an upper spinneret 1, a lower spinneret 2 and a spinning device 3. The spinning device 3 comprises a support table with a filter 4, a flow chamber 5 and several spinnerets 6, which are air gaps as the distance between the outlet side and the surface of the spinning bath 7. To form. The bottom of the upper spinneret vessel 1 is reinforced and includes several thread guide members according to the arrangement of the spinneret 6, through which the thread bundle 12 exits the vessel 1.

A vertically and horizontally adjustable winding goth 13 is arranged under the container 1 to deflect all thread bundles of all thread guide members 11 from the yarn stream 14 at an angle β and to wind under moderate tension. . The throttle stream 14 is fed to the lower vessel 2 and returned to the upper vessel 11 via line 16 using a pumping device 15. It is evident that the thread zone 12 through which the thread bundle 12 passes reaches the position of the thread guide member 11 where the thread bundle 12 is separated from the yarn flow 14. Line 16 first enters stabilization chamber 18 partially filled with filler. The spinning bath solution flows from the stabilization chamber 18 through the opening 19 into the vessel 1.

It can be seen from the plan view shown in FIG. 3 that the thread guide members of the bottom face 10 are arranged in a zigzag fashion and the thread bundle 12 is wound in parallel on the winding goth 13.

4 shows a thread guide member 11 of ceramic material for one fiber bundle. It is shown that the cross section of this member narrows in the flow direction. Also in the case of the thread member shown in FIG. It is not shown that the edge of the thread guide member 11 is preferably rounded. The thread bundle immediately separates from the bath flow after passing through the thread guide member.

6 shows an overview of the geometric dimensions included in relation (III). Here reference 6 'is two spinneret holes of diameter D. d is the distance between the centers of the capillaries on the outlet side of the spinneret hole 6 '. x is the distance between the two capillaries and d 'is the distance between the centers of the two capillaries in the inlet. P is the point at which the fiber bundle separates from the spinning stream. β is the deflection angle at which the separation takes place. β ^* is the (very small) angle between two adjacent yarns in the spinning chamber.

Example 1

In a stirring vessel, spruce sulfite cellulose (Quoxam-DP 580, dry content 44.9%) pretreated with 0.49 kg of enzyme method was suspended in 2.6 kg of NMMO (dry content 65.0%) containing 0.44 g of stabilizer. Water is evaporated under shear at 500 ° C., 25-25 mbar. The resulting solution had a composition of 10% cellulose, 78.5% NMMO and 11.5% water, and had no microscopically visible particles, and had a laser diffraction method (B. Kosan; Ch. Cichels Chemical Fibers International 49 [1999] p. 50- Particle size <9 μm is 19 ppm. The shear shear viscosity of the solution was 3450 Pa.s and the relaxation time was 4.1 seconds. Using a spinning pump (1.2ml / U, 25.8Upm) at a flow rate of 31ml / min, two small 30-pin spinning capillaries of 12.5mm diameter and 130mm (L / D ≒ 1) arranged in a row The filament with the hat spinneret was fed to a flow chamber at the spin position. The residence time in the flow chamber with a diameter of 5.4 cm and a height of 0.4 cm was 4.3λ _m . The spinning solution is formed into a thread band under shear of 39 900 1 / s, drawn at a rate of 12.9 at an elongation rate of 220 1 / s in an air gap of 35 mm length, and the cellulose is precipitated in a 3.5 cm long vertical spinning bath. 40 degrees from the generally laminar flow jet of the spinning bath, conveyed by the two thread guide members (e = 5 mm, h = 4 mm) shown in FIG. 5 at the bottom (E = 13 mm) of the upper spinneret container. Deflecting, paralleling, stretching to the winding goth with a thread tension of 2.5 cN / tex, stretching at a speed of 500 m / min, and washing, drying, finishing treatment with a tension of 1.25 cN / tex Wound up.

The filament yarns are characterized by the following parameters:

Fineness 40dtex (30)

Tenacity 43.7 cN / tex

Coefficient of variation 2.3%                 

Elongation 8.5%

Knot breaking load 34.1 cN / tex

Worcester (Slugish) 0.1%

Example 2

0.18 kg of cotton-linter-cellulose was mixed with water in a ratio of 1:20 under shear using a liquor mixer. 4.20 kg of spruce sulfite cellulose (Quoxam-DP 450) was added slowly under further shear to give a homogeneous suspension. The cellulose mixture is separated using a suction press.

In the mixing vessel, the cellulose mixture and 30.42 kg of NMMO (dry content of 84%) were added, and the basicity was adjusted to pH 11.2 by adding NaOH. 7.69 kg of water was evaporated by heating, shearing and vacuum to convert the mixture into a clear solution with 13.0% cellulose, 75.9% NMMO and 11.1% water, 3850 Pa.s of zero shear viscosity and 3.1 s relaxation time.

4 small caps with 90 spin capillaries of 120 mm (L / D ≒ 1), 20 mm in diameter, arranged in a spinning solution at a flow rate of 157 ml / min using a spin pump (4.8 ml / U, 32.7 Upm) The filament with the spinneret was fed to a flow chamber at the spinning position. The residence time in the flow chamber with dimensions of 13.9 × 4.0 × 0.35 cm was 2.3λ _m .

The spinning solution is formed into thread bands under a shear of 42 900 1 / s, drawn at a rate of 11.7 at an elongation rate of 245 1 / s in a 28 mm long air gap, and the cellulose is precipitated in a 4.0 cm long vertical spinning bath. 50 degrees from the generally laminar flow jet of the spinning bath, conveyed by the two thread guide members (e = 7mm, h = 4mm) shown in FIG. 5 at the bottom (E = 18mm) of the upper spinneret container. Deflected, paralleled and wound to the winding goth with the thread tension of ˜3 cN / tex and stretched at a speed of 450 m / min, followed by washing, drying and finishing with the yarn tension ≥1.5 cN / tex And wound up.

The filament yarn exhibited the following properties:

Fineness 150dtex (90)

Toughness 41.7 cN / tex

Coefficient of variation 3.2%

Elongation 9.1%

28.9% of brass breaking loads

Worcester (sludge) 0.1%

Example 3

7.66 kg / h of spruce sulfite cellulose (cuoxam-DP 480, dry content 50%) and 29.0 kg / h N-methylmorpholine-N-oxide (NMMO, dry content 84%), which were activated and stabilized by an enzymatic method, were prepared. It was fed to a heated CO-ROTATING-PROCESSOR 25 CONTI (LIST AG ARISDORF) and dispersed to a homogenization mixture. The mixture was fed to a DISKOTHERM B 63 CONTI (LIST AG ARISDORF) type heat dispensing system using a dosing pump, which evaporated 4.7 kg / h of water at 90 ° C. and 20 mbar vacuum to give 12.9% cellulose, NMMO 76.3. A homogenous cellulose solution 27.0 kg / h having a composition of% and 11.7% of water was obtained. This solution has a zero shear viscosity of 3100 Pa.s and a relaxation time of 1.9 s at 95 ° C.

Flow chamber 13 (9.2x6.2x0.8 = 45.cm3) (retention time) was passed through a spinneret filter with 451 ml / min spinning solution having a temperature of 85 ° C using a spinning pump (9.6 ml / U; 47 Upm). T = 3λ _m ), reaching 13 small spinning caps with 350 spinning capillaries arranged in three rows and each having a diameter of 100 μm. At a shear rate of 16 850 1 / s, the solution is molded in 4550 spinneret channels and stretched at a rate of 9.5 at an elongation rate of 90 1 / s in an air gap of 20 mm, and the cellulose is precipitated in a 6 cm length bath. The yarn is separated from the laminar flow current bath stream at an angle of 35 ° and wound up using a winding goth at a winding speed of 120 m / min and sent to subsequent processing and drying.

On the bottom of the spinneret vessel a ceramic threaded guide member was placed on the spinneret table, similar to the arrangement of a small cap.

The obtained staple fiber had the following mechanical properties:

Fineness 1.3dtex

Toughness (Dry State) 43.5 cN / tex

Toughness (wet state) 36.5 cN / tex

Shinto (Dry) 14.5%

Elongation (Wet) 15.1%

Loop Breaking Load 15.6 cN / tex                 

Staple Length 38mm

Example 4

In a turbo mixer, 0.23 of high molecular weight spruce sulfite cellulose (cuoxam-DP 1100) was mixed with water in a ratio of 1:16. A small amount of 4.45 kg of spruce sulfite cellulose with a Cuoxam DP of 480 was added to make a homogeneous suspension. A homogeneous mixture of cellulose mixtures was separated from water using a sieve belt apparatus to obtain 9.36 kg of cellulose with a dry content of 50%. This cellulose mixture was added in a heated dose of CO2ROTATING-PROCESSOR 25 CONTI (LIST AG ARISDORF) in a 1 hour dose with 35.9 kg of NMMO (84% dry matter) simultaneously containing 10 g of stabilizer, and 2.26 kg of Dispersed while removing water to make a homogenization mixture. 43.0 kg / h of the mixture was sent to a DICKOTHERM B 63 CONTI (LIST ARISDORF) heated kneading apparatus using a mixture dosing device, thereby removing 4.0 kg / h of water at a temperature of 93 ° C. and a pressure of 22 mbar to give 12.0% of cellulose. A homogeneous cellulose solution having a composition of 77.3% NMMO and 10.7% water was obtained. This solution has a zero shear viscosity of 3750 Pa.s and a relaxation time of 2.1 s.

Flow chamber 13 (9.2x6.2x0.8 = 45.6 cm 3) (retention time t) was passed through a spinneret filter with 457 ml / min spinning solution having a temperature of 85 ° C. using a spinning pump (9.6 ml / U; 57 Upm). = 2.4λ _m ) and reach five small spinning caps with 1020 spinning capillaries, arranged in three rows and each having a diameter of 80 μm. At a shear rate of 13770 1 / s, the solution is molded in 5100 spinneret channels and stretched at a rate of 8.8 at an elongation rate of 67 1 / s in an air gap of 22 mm, cellulose precipitates in a 5 cm length bath, The yarns are separated at a 30 ° angle from the laminar flow bath, drawn off at a winding speed of 100 m / min using a winding goth, combined with fiber tow, washed, cut into staple fibers, subsequently processed and dried. Five thread guide members were arranged in two rows in the upper spinneret vessel with dimensions h = 20 mm, E = 20 mm, e = 10 mm according to FIG. 5. Transfer of the cooled bath (6-8 ° C.) using a membrane pump was carried out at 35 l / min between the lower and upper spinneret vessels.

The obtained staple fiber had the following mechanical properties:

Fineness 1.7dtex

Toughness (Dry State) 42.8 cN / tex

Toughness (wet state) 35.9 cN / tex

Shinto (Dry) 15.5%

Elongation (Wet) 15.9%

Loop Breaking Load 15.1 cN / tex

Staple Length 38mm

Claims (17)

A process for producing cellulose fibers or cellulose filaments from cellulose by a dry-wet extrusion process using an aqueous amine oxide, in particular N-methylmorpholine-N-oxide, as a solvent, a) dispersing a cellulose or cellulose mixture with cuprammonium DP in the range of 250 to 3000 in an aqueous amine oxide, b) converting the obtained dispersion into a homogeneous solution having a zero shear viscosity in the range of 600 to 6000 Pa.s at 85 ° C., while removing water at high temperature, c) transferring said solution to at least one spinneret, d) shaping the solution to form at least one capillary at each spinneret, stretching the capillary (s) of each nozzle through a non-precipitating medium and then passing through a precipitation bath to precipitate cellulose fibers Making a step, and e) drawing off the fibers by separating the cellulose fibers by deviation from the settler stream at the end of the settler zone. Including, The dispersion in step b) is converted into a solution at a relaxation time in the range of 0.3 seconds to 50 seconds at 85 ° C., The solution in step c) is passed through an inflow chamber, wherein the residence time of the solution is at least equal to the relaxation time at the spinning temperature. Process for producing cellulose fiber or cellulose filament. Claim 2 was abandoned when the setup registration fee was paid. The method of claim 1, The method for producing cellulose fibers or cellulose filaments, characterized in that the cellulose or cellulose mixture is pretreated by an enzyme method. The method of claim 1, To prepare the cellulose mixture, firstly, cellulose with copper ammonia DP in the range of 600 to 3000 is dispersed in water, followed by dispersion by addition of cellulose with copper ammonia DP in the range of 250 to 600, and then wet from the press. The method of producing a cellulose fiber or a cellulose filament, wherein the cellulose mixture of is used in step a) after water removal. The method of claim 1, Passing the capillaries individually and substantially parallel to the non-precipitable medium, and then passing the settling tank less than 20 cm in length to produce cellulose fibers or cellulose filaments. The method of claim 1, Wherein said cellulose fiber in step e) is deflected from the settling stream at an angle of β> 10 ° and drawn off at a maximum thread tension of 5 cN / tex. An apparatus for producing cellulose fibers or cellulose filaments from cellulose by a wet and dry extrusion process using an aqueous amine oxide as a solvent, Spinning package 3 with spinneret plate and spinneret 6, A settling tank in two vessels 1 and 2 connected by a settling tank pump 15, A gap a between the spinneret 6 and the surface 7 of the settling tank in the upper vessel of the two vessels 1, 2, and Draw-off speed roller (13) Including, A cellulose fiber or cellulose characterized in that a common inlet chamber 5 is installed on a spinneret plate in which one or more rows or groups of spinnerets 6 are arranged, the volume of which is represented by the following formula: Filament's Manufacturing Device:

(I) Wherein V is in cm 3 as the volume of the inlet chamber,

Is the flow rate of the cellulose solution in cm 3 / s, and λ _m is the relaxation time of the spinning solution at the maximum frequency of the relaxation time spectrum. An apparatus for producing cellulose fibers or cellulose filaments from cellulose by a wet and dry extrusion process using an aqueous amine oxide as a solvent, Spinning package 3 with spinneret plate and spinneret 6,  A settling tank in two vessels 1 and 2 connected by a settling tank pump 15, A gap a between the spinneret 6 and the surface 7 of the settling tank in the upper vessel of the two vessels 1, 2, and Drawing Off Speed Rollers (13) Including, The width of the gap (a) and the relaxation time of the spinning solution is defined in the following formula device for producing a cellulose fiber or cellulose filament:

(II) (Wherein a is the width of the gap in mm, λ _m is the relaxation time of the spinning solution at the maximum frequency of the relaxation time spectrum, v _a is the drawing off rate and the unit is m / min). Claim 8 was abandoned when the registration fee was paid. The method according to claim 6 or 7, Apparatus for producing cellulose fibers or cellulose filaments, characterized in that the dimensions of the spinneret 6, the width of the gap a and the sedimentation tank zone w are defined by the following formula:

(Ⅲ) (Where X is the distance between two adjacent nozzle holes 6 ', a is the width of the air gap, w is the length of the settling zone, and D is the diameter of the nozzle hole). Claim 9 was abandoned upon payment of a set-up fee. The method according to claim 6 or 7, Apparatus for producing cellulose fibers or cellulose filaments, characterized in that the fiber guide member (11) made of ceramic is inserted into the bottom face (10) of the upper settling vessel (1). Claim 10 was abandoned upon payment of a setup registration fee. The method of claim 9, Apparatus for producing cellulose fibers or cellulose filaments, characterized in that the fiber guide member (11) is arranged in rows or groups. Claim 11 was abandoned upon payment of a setup registration fee. The method of claim 9, The shape of the spinneret (6) is a hat shape, the nozzle area covered with the spin capillary tube is less than the inlet area of the fiber guide member (11), characterized in that the manufacturing apparatus of cellulose fibers or cellulose filaments. Claim 12 was abandoned upon payment of a registration fee. The method of claim 9, The diameter ratio of the inlet region and the outlet region of the fiber guide member (11) is E / e ≥ 1, and the edge at the outlet is rounded, the manufacturing apparatus of cellulose fibers or cellulose filaments. Claim 13 was abandoned upon payment of a registration fee. The method of claim 9, The ratio of the height to the inner diameter of the outlet region of the fiber guide member (11) is h / e <1, and the edges at the inlet and the outlet are rounded, characterized in that the apparatus for producing cellulose fibers or cellulose filaments. The method according to claim 6 or 7, Apparatus for producing cellulose fibers or cellulose filaments, characterized in that the upper settling vessel (1) has an inlet opening (19) downstream of the settling chamber (18). The method according to claim 6 or 7, Apparatus for producing a cellulose fiber or cellulose filament, characterized in that the upper sedimentation tank vessel (1) has at least one overflow (overflow) is adjustable height, The method according to claim 6 or 7, Apparatus for producing cellulose fibers or cellulose filaments, characterized in that the position of the upper settling vessel 1 is adjustable in the vertical direction with respect to the spinning package 3, The method according to claim 6 or 7, Apparatus for producing cellulose fibers or cellulose filaments, characterized in that the drawing off roller (13) provided below the upper settling vessel (1) is adjustable in the vertical direction and / or horizontal direction.

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