US20070210481A1 - Lyocell Method and Device Involving the Control of the Metal Ion Content - Google Patents

Lyocell Method and Device Involving the Control of the Metal Ion Content Download PDF

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Publication number
US20070210481A1
US20070210481A1 US11/569,056 US56905605A US2007210481A1 US 20070210481 A1 US20070210481 A1 US 20070210481A1 US 56905605 A US56905605 A US 56905605A US 2007210481 A1 US2007210481 A1 US 2007210481A1
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Prior art keywords
cellulose
metal ion
content
treatment medium
type
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Stefan Zikeli
Werner Schumann
Lutz Glaser
Michael Longin
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LL Plant Engineering AG
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ZiAG Plant Engineering GmbH
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Assigned to ZIMMER AKTIENGESELLSCHAFT reassignment ZIMMER AKTIENGESELLSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GLASER, LUTZ, SCHUMANN, WERNER, ZIKELI, STEFAN, LONGIN, MICHAEL
Publication of US20070210481A1 publication Critical patent/US20070210481A1/en
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00—Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00—Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • C08B1/003—Preparation of cellulose solutions, i.e. dopes, with different possible solvents, e.g. ionic liquids
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D13/00—Complete machines for producing artificial threads
    • D01D13/02—Elements of machines in combination
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D4/00—Spinnerette packs; Cleaning thereof
    • D01D4/02—Spinnerettes
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/20—Cellulose-derived artificial fibres

Definitions

  • the invention relates to a method for producing a Lyocell fibre from a spinning mass which is produced by adding a treatment medium to a cellulose, to a cellulose suspension and/or a cellulose solution.
  • the invention also relates to a device for the production of Lyocell fibers with a mixing device in which a cellulose, a cellulose suspension and/or a cellulose solution can be charged with a treatment medium.
  • Lyocell technology Methods and devices of this kind are known from the Lyocell technology. With the Lyocell technology threads, fibers, films and membranes are extruded as endless molded bodies from the spinning mass containing cellulose, water and tertiary amine oxide. On account of its environmental friendliness, the Lyocell technology is increasingly replacing the conventional viscose methods.
  • the environmental friendliness of the Lyocell method stems from the solution of the cellulose without derivatisation in an organic, aqueous solvent. From this cellulose solution endless molded bodies, for example fibers and film, are then extruded.
  • Lyocell was issued by the BISFA (International Bureau for the Standardisation of Man-made Fibers). In the state of the art the Lyocell method is now well documented.
  • tertiary amine oxides are known as solvents for cellulose from U.S. Pat. No. 2,179,181 which solvents can dissolve cellulose without derivatisation. From these solutions, the cellulose molded bodies solvents can be obtained by precipitation.
  • NMMNO N-methylmorpholine-N-oxide
  • N-methylpiperidine-N-oxide N-methylpyrrolidone oxide, dimethylcyclohexylamine oxide and others can be used as the amine oxide.
  • Mixing in the mixing chamber occurs between 65° C. and 85° C.
  • the cellulose is mixed with the aqueous solution of the tertiary amine oxide in a device, whereby the mixing device exhibits a mixing tool and a container which rotates during mixing.
  • the mixing tool is improved such that it is formed as a paddle, rail or helix and during mixing preferably prevents the formation of deposits on the inner surface of the container.
  • a buffer device is described, which comprises a mixing vessel and a conveyor worm as a discharging device. In this way, a continuous production of the cellulose solution is facilitated despite the cellulose being fed in batches.
  • WO-A-96/33934 has now been further advanced by the method of WO-96/33221, in which a homogeneous cellulose suspension is produced from milled cellulose and an aqueous amine oxide solution in one single step.
  • the pulverised cellulose is brought into contact with the liquid, aqueous tertiary amine oxide and a first mixture is formed.
  • the first mixture is spread in layers on a surface and transported under intensive mixing over this surface. This process can be carried out continuously.
  • Other methods in which the cellulose solution is treated in the form of a thin layer are also known from EP-A-0356419, DE-A-2011493 and WO-A-94/06530.
  • the system NMMNO/cellulose/water in the highly concentrated NMMNO region has the property of releasing metal ions from the process apparatus, such as lines, filters, and pumps, which reduces the system stability.
  • WO-A-96/27035 a method for the production of cellulose molded bodies is described in which at least some of the materials in contact with the cellulose solution contain at least 90% of an element from the group of titanium, zirconium, chrome and nickel down to a depth of at least 0.5 ⁇ m.
  • the important aspect with regard to WO-A-96/27035 is that the rest of the composition of the apparatus and piping, where it comes into contact with the cellulose solution, does not contain any copper, molybdenum, tungsten or cobalt. According to WO-A-96/27035, this measure should prevent exothermic decomposition reactions.
  • DE-A-44 39 149 Another way of producing the cellulose solution is followed in DE-A-44 39 149 which forms the closest state of the art.
  • the cellulose is pretreated enzymatically.
  • the cellulose can be disintegrated under shearing in water before the pretreatment.
  • the pretreated cellulose is separated from the liquor and the separated cellulose is introduced into a melt of NMMNO and water.
  • the separated liquor can be fed back to the pretreatment after supplementing the water and enzyme losses.
  • this type of process management has proven to be impracticable, because the cellulose solution obtained in this way is unstable.
  • the object of the invention is therefore to improve the known methods and devices of the Lyocell technology such that, with the highest level of environmental compatibility, the method can be carried out independent of the type of cellulose used in a stable manner and with consistent quality.
  • This object is solved for the aforementioned method in that the content of at least one type of destabilising metal ions in the cellulose, in the cellulose suspension and/or in the cellulose solution is monitored and adjusted below a stability limit.
  • this object is solved according to the invention in that a sensor, by which the content of at least one type of destabilising metal ion can be acquired in the cellulose, cellulose suspension and/or cellulose solution and a control signal representing the content of at least one type of destabilising metal ion can be output, and a control device are provided through which the metal ion content of the cellulose, cellulose suspension and/or cellulose solution can be adjusted to below a stability limit in dependence of the control signal.
  • the solution according to the invention is simple and enables any type of cellulose to be used for the spinning mass during the cellulose processing used in the production of Lyocell fibers, irrespective of its content of metal ions destabilising the cellulose suspension and/or cellulose solution, so that it is no longer necessary to carefully select the cellulose according to its content of destabilising metal ions, in particular iron (Fe 3+ ) and copper (Cu 2+ ) ions before its processing, or to mix several types of cellulose.
  • Lyocell fibers eliminates the problem of the cellulose processing in that only certain cellulose compositions can be used, which are specially suitable for the Lyocell process and correspondingly expensive, such as, for example, the celluloses produced according to the method of DE-T-699 13 117.
  • any celluloses can be used in the course of the Lyocell method, in particular also celluloses with a high to very high content of destabilising metal ions, which until now could not or could only with expensive additional measures be processed, because they have led to an instable cellulose suspension and/or cellulose solution with the risk of an exothermic reaction.
  • the main source of the metal ions which destabilize the cellulose suspension and/or the cellulose solution appears to be the cellulose itself.
  • the method according to the invention and the device according to the invention can both be used with the Lyocell method, in which the cellulose is directly pulped in an aqueous solution of a tertiary amine oxide or in a tertiary amine oxide and cellulose solution is produced from it, and also with methods in which initially a cellulose suspension is produced containing essentially water and cellulose and only then a tertiary amine oxide or an aqueous solution therefrom is added to form a cellulose solution.
  • the stability limit for the metal ion content is determined in dependence of the composition of the cellulose suspension and/or cellulose solution, their temperature and their residence time in the plant from the pulper through to the extrusion of the Lyocell fibers.
  • Each type of metal ion can exhibit different high stability limits. The less a certain type of metal ion destabilizes the cellulose suspension and/or cellulose solution, the higher the stability limit can be.
  • the stability limit for example, for copper ions may lie below the stability limit for iron ions due to their stronger destabilising effect.
  • the stability limit can be found experimentally in that for samples of cellulose solutions with different metal ion contents, different temperatures and different times of exposure, the percentage of samples producing exothermic reactions is found.
  • the stability limit can be defined based on a probability value of an exothermic reaction which is realistic for the plant operation. For example, such a probability value may be below 0.01% or below 1 ⁇ 10 ⁇ 6 % so that with the set stability limit an exothermic reaction is only to be expected with a probability of 0.01% or 1 ⁇ 10 ⁇ 6 %.
  • the method according to the invention and the device according to the invention can be further improved in a series of advantageous embodiments which can be combined with one another as required.
  • the quantity of the treatment medium added to the cellulose, cellulose suspension and/or cellulose solution is adjusted in dependence of the content of the at least one type of metal ion.
  • the content of the at least one type of metal ion introduced by the cellulose in the cellulose suspension and/or cellulose solution is suppressed below the stability limit.
  • a particularly high level of environmental compatibility and economy of the method can be achieved in that, in a further development, the added treatment medium is recovered in a following processing step in the Lyocell method.
  • the water added to a cellulose suspension in the course of the pretreatment of the cellulose can be returned as press water from the expressing stage of the cellulose suspension and be reused when pulping the cellulose.
  • this press water can be purified before it is added to the cellulose and in particular it can be freed at least partially of metal ions.
  • recovered amine oxide can be used, which for example can be regenerated from a spinning bath through which the freshly extruded spinning threads are passed and in which the cellulose precipitates.
  • the recirculated tertiary amine oxide can be purified and in particular be freed at least partially of the metal ions it contains before it is added to the cellulose, cellulose suspension and/or cellulose solution.
  • a commercially available ion exchanger can be used to remove the metal ions.
  • a fresh, non-recycled treatment medium of the same kind is added to the cellulose, cellulose suspension and/or cellulose solution.
  • fresh water in particular fully desalinated or partially desalinated fresh water can be fed into the recirculated press water and/or fresh tertiary amine oxide can be fed into the recycled tertiary amine oxide.
  • part of the treatment medium is discharged from the production process and is therefore no longer available for return within the process, then, destabilising metal ions are also removed from the process with the drained off treatment medium.
  • the content of the destabilising metal ions in the cellulose suspension and/or cellulose solution can also be controlled via the quantity of the discharge of treatment medium which can no longer be returned to the process.
  • the discharged treatment medium is preferably replaced by fresh treatment medium.
  • the quantity of discharged treatment medium depends preferably on the content of destabilising metal ions in the cellulose, cellulose suspension and/or cellulose solution so that as much of the treatment medium as possible can be recycled.
  • the metal ion content can be particularly effectively controlled if the respective proportions of recycled and fresh treatment medium are adjusted in dependence of the content of the at least one type of metal ion. If, for example, the content of the metal ions increases, then the proportion of the recycled and returned treatment medium and thus the introduction of metal ions into the cellulose suspension and/or cellulose solution is reduced. If the metal ion content decreases, then the proportion of the recycled treatment medium can be increased with respect to the proportion of the fresh treatment medium.
  • the metal ions can be determined by inline sensors, i.e. sensors, which are arranged in the plant volume through which the cellulose suspension and/or cellulose solution flows during the Lyocell production, and/or in an automatic laboratory analysis device after a manual sampling.
  • the signal from the sensors can be used by a control device for the automatic dosing of the relative proportion of the recovered treatment medium and the fresh treatment medium.
  • This type of automatic dosing can, for example, be implemented by valves operated by actuators.
  • the metal ion content can either be passed to a control device automatically by the automatic laboratory analysis device or the content of the metal ions can be entered manually using an input device.
  • mass spectrometers For the acquisition of metal ions, mass spectrometers, devices for the measurement of atomic absorption, sensors based on Raman scattering and devices with graphite tube technology can be employed.
  • the metal ion content is in each case adjusted below the stability limit.
  • the stability limit is preferably below 10 mg/kg for iron ions and below 0.5 mg/kg for copper ions.
  • FIG. 1 shows an embodiment of a device according to the invention for the production of a cellulose solution in a schematic representation, whereby the method according to the invention can be implemented by the embodiment;
  • FIG. 2 shows a schematic representation of the processing steps for the production of the cellulose suspension
  • FIG. 3 shows a schematic representation of the variation of the amount of the removed iron ions against time
  • FIG. 4 shows a schematic representation of the chemical oxygen demand in the press water against time
  • FIG. 5 shows a schematic representation of a first method for controlling the metal ion content.
  • FIG. 1 shows a plant 1 for the production of endless molded bodies 2 , for example strands, out of a spinnable cellulose solution containing water, cellulose and tertiary amine oxide.
  • cellulose in the form of leaves or plates 3 and/or rolls 4 is fed in batches to a pulper 5 .
  • the cellulose 3 , 4 is disintegrated with water as treatment medium, symbolically represented by the arrow 6 , and a cellulose suspension is formed, preferably still without solvent or amine oxide.
  • Enzymes or enzyme solutions can be added for the homogenisation and Stabilisation of the cellulose suspension.
  • the quantity of the added water 6 is determined in dependence of the water content of the cellulose. Typically the water content of the cellulose used is between 5 and 15 percent by mass. This span of variation is compensated by changing the addition of water appropriately, so that the water content of the cellulose suspension or the slurry ratio of solids/liquid remains approximately constant or attains a freely selected value.
  • the cellulose suspension is passed through a thick matter pump 7 via a pipe system 8 to a press device 9 , whereby the cellulose suspension of water and cellulose is preferably maintained in a temperature range from 60 to 100° C.
  • the cellulose suspension produced by the pulper 5 is expressed, for example, by rotating rolls 10 .
  • the expressed water or press water 11 is collected by a collecting device 11 ′ and passed back at least in part as water 6 serving as treatment medium to the pulper 5 by a conveying means 12 , through an optional filter device 13 and through a mixing device 14 .
  • the press device 9 can also be provided with a suction device (not shown) for sucking off excess water from the cellulose suspension.
  • the drawn-off water is, with this embodiment, passed back, as the press water, at least in part to the pulper 5 .
  • sucked-off water or water removed from the cellulose suspension by other means is also press water which can be reused for the disintegration of the cellulose.
  • the filter 13 can comprise one or more surface filters, deep-bed filters, membrane filters, plate filters, edge filters, separators, centrifuges, hydrocyclones, belt filters and vacuum belt filters, tube filters, filter presses, rotating filters, reversible-flow filters and multilayer filters.
  • the press water 11 can be osmotically treated in the filter 13 ; alternatively or additionally, metal ions and particles can be filtered out of the press water 11 or metal-binding additives can be fed to the press water 11 .
  • the respective proportions of the returned treatment medium 11 and of fresh treatment medium 15 fed from another fresh source, for example fresh water, in the water passed to the pulper are set by the mixing device 14 .
  • the proportion of the treatment medium 11 which is passed out of the plant 1 through a waste water pipe 16 , is set by the mixing device 14 .
  • the mixing device 14 can for example comprise a selector valve or a number of valves.
  • the mixing device 14 is controlled by a control device 17 such that the proportions of the press water 11 and the fresh water 15 in the water 6 fed to the pulper 5 can be set to variably specifiable values by an output signal from the control device via at least one control line 18 .
  • the cellulose suspension is transported further through the pipe system 8 to a stirring and conveying means 19 in which a shear stress acting on the cellulose suspension is generated by a stirring or conveying tool 20 , such as a screw, paddle or blade.
  • a stirring or conveying tool 20 such as a screw, paddle or blade.
  • no annular layer mixers can be employed, such as originating from DRAIS Misch- and Christssysteme and sold under the designation CoriMix®.
  • the annular layer mixers are only used for moistening or impregnating dry cellulose materials which are not used in the method described here.
  • a treatment medium such as tertiary amine oxide, in particular N-methylmorpholine-N-oxide, is passed in aqueous form via a pipe 21 to the cellulose suspension with a molar ratio NMMNO/H 2 O of between 1:1 and 1:2.5 as solvent for the cellulose.
  • additives such as stabilizers and enzymes, organic additives, delustering substances, alkalis, solid or liquid alkaline earth, zeolites, finely pulverised metals such as zinc, silver, gold, platinum for the production of anti-microbial and/or electrically or thermally conducting fibers during and after the spinning process and/or dyes can be added to the cellulose suspension.
  • concentration of the additives can be controlled in the range from 100 to 100,000 ppm referred to the fibre product.
  • the concentration of the fed NMMNO depends on the water content of the celluloses 3 , 4 currently in the cellulose suspension.
  • the stirring and conveying means 19 acts as a mixer in that the tertiary amine oxide is mixed with the cellulose suspension and the cellulose solution is produced. Then, the cellulose solution to which NMMNO has been added is transported via the pipe system 8 to a second stirring and conveying means 22 .
  • the stirring and conveying means 22 can comprise a vaporization stage. From the stirring and conveying means 22 the pipe system can be heated. In contrast to the unheated pipe system 8 , the heated pipe system in FIG. 1 is given the reference symbol 8 ′.
  • a pipe system can be used, as described in WO 01/88232 A1, WO 01/88419 A1 and WO 03/69200 A1.
  • the metal ion content of the cellulose solution, in particular copper and iron ions, in the pipe 8 ′ and/or in at least one of the shear zones 19 , 22 , or before and/or after one of the shear zones is measured using the sensors 23 , 23 ′ and a signal representing the metal content or the content of individual destabilising metal ions, such as iron, chrome, copper and/or molybdenum is output to the control device 17 .
  • the metal ion content can, in a further embodiment, be determined using wet-chemical methods after manual sampling in an automatic laboratory analysis device and passed on from there to the control device 17 automatically or manually.
  • the feedback to the controller for the metal ion content contains a manual process stage and cannot therefore be automated.
  • the control device 17 compares the metal ion content measured by the sensors 23 , 23 ′ with predetermined limits and outputs a signal depending on this metal ion content to the mixing device 14 . Due to the control signal to the mixing device 14 , the composition of the water 6 passed as treatment medium to the pulper 5 is set in dependence of the content of the destabilising metal ions in the cellulose solution and the metal content or the content of individual metal ions in the cellulose solution to which tertiary amine oxide has been added is regulated under closed-loop control to a predetermined value. Since the concentration of reactions in the cellulose solution increases after the vaporization stage, preferably a sensor is provided which monitors the metal content of the cellulose solution after the addition of all ingredients and after all the vaporization stages.
  • the content of destabilising metal ions in the cellulose solution is too high, then the proportion of fresh water in the water 6 fed to the pulper 5 is increased. Thereby, the metal content is adjusted by the control device 17 such that it remains below a stability limit of 10 mg/kg.
  • the metal content can also be determined before the formation of the cellulose solution, i.e. still in the cellulose suspension, whereby this measurement is more appropriate than the measurement of the metal content directly in the cellulose solution.
  • sensors 23 , 23 ′ devices for atomic absorption measurement, mass spectrometers, optical detectors for the acquisition of fluorescence spectra, emission spectra or Raman scattering can be used. These types of sensors are known and are produced by various manufacturers, e.g. Perkin Elmer.
  • the control device 17 takes into account the previously determined metal content of the cellulose 3 , 4 passed to the pulper 5 .
  • the analyzed metal content of individual metal ions or the complete content of metal in the cellulose 3 , 4 just used can be entered into the control device 17 via an input device 24 .
  • This preadjustment is taken into account in the determination of the proportions of the press water and fresh water in the water fed to the pulper 5 . For example, with cellulose containing a high metal content, a higher proportion of fresh water 15 is passed to the pulper 5 at the start or certain metal-binding additives are mixed into the cellulose suspension.
  • the metal content decreases, as it is acquired by the sensors 23 , 23 ′ in the cellulose solution to which tertiary amine oxide has been added, below a certain limit which is taken as sufficient for protection against exothermic reactions, for example 10 mg/kg, then the proportion of press water in the water passed to the pulper 5 is increased. Consequently, with sufficient protection against exothermic reactions, less fresh water is consumed and less press water is discharged to the environment.
  • the now extrudable cellulose solution is passed to an extrusion head 25 which is provided with a large number of extrusion openings (not shown).
  • the highly viscous cellulose solution is extruded into an air gap 26 through each of these extrusion openings to give in each case an endless molded body 2 .
  • An orientation of the cellulose molecules occurs due to a drawing of the cellulose solution which is still viscous after the extrusion.
  • the extruded cellulose solution is drawn away from the extrusion openings by a drawing device 27 with a speed which is greater than the extrusion speed.
  • the endless molded bodies 2 pass through a precipitation bath 28 containing a liquid such as water which is a non-solvent, whereby the cellulose in the endless molded bodies 2 is precipitated.
  • the endless moulded bodies 2 are cooled by a cooling gas flow 29 .
  • the cooling gas flow should be turbulent and exhibit a velocity component in the extrusion direction, as described in WO 03/57951 A1 and in WO 03/57952 A1.
  • the precipitation bath 28 becomes increasingly enriched with tertiary amine oxide so that it must be continually regenerated by means of a recovery device 30 .
  • the liquid from the precipitation bath is fed during operation to the recovery device 30 via a pipe 31 , which for example is connected to an overflow of the precipitation bath.
  • the recovery device 30 extracts the tertiary amine oxide from the liquid and returns pure water via a pipe 32 . Non-reusable waste substances are discarded from the device 1 via a pipe 33 for disposal.
  • the amine oxide is separated from the water and fed via a pipe 34 to a further mixing device 35 to which fresh amine oxide is also fed by a pipe 36 .
  • the regenerated amine oxide from the pipe 34 is mixed with the fresh amine oxide 36 and fed to the shear zone 19 via the pipe 21 .
  • Metal ions can be removed from the regenerated amine oxide via an ion exchanger, for example from Rohm and Haas, Amberlite GT 73, or via a filter 37 .
  • an ion exchanger for example from Rohm and Haas, Amberlite GT 73, or via a filter 37 .
  • the mixing device 35 and the purification device 37 can be controlled by the control device 17 in dependence of the metal ion content measured by the sensors 23 , 23 ′.
  • the endless moulded bodies are treated further, for example washed, brightened, chemically treated in a device 38 to influence the cross-linking properties, and/or dried and pressed out further in a device 39 .
  • the endless moulded bodies can also be processed by a cutting device, which is not shown, to form staple fibers and passed out of the device 1 in fleece form.
  • the overall conveyance of the cellulose solution in the pipe system 8 ′ occurs continuously, whereby buffer containers 40 can be provided in the pipe system 8 ′ to compensate variations in the conveyed amount and/or of the conveying pressure and to facilitate continuous processing without dead water regions arising.
  • the pipe system 8 ′ is equipped with a heating system (not shown) to maintain the cellulose solution during conveyance at a temperature at which the viscosity is sufficiently low for an economical transport without decomposition of the tertiary amine oxide.
  • the temperature of the cellulose solution in the pipe section 8 ′ is here between 75 and 110° C.
  • the homogenisation and uniform mixing which can be increased by static or rotating mixers, is promoted by the high temperature.
  • the residence time of the cellulose suspension or solution in the pipe system 8 , 8 ′ from the thick matter pump 7 to the extrusion head 25 is between 5 minutes and 2 hours, preferably about 30 to 60 minutes.
  • a first series of experiments deals with the cellulose pretreatment for the production of the cellulose suspension and the examination of the press water.
  • reference is made to the schematic representation of the pretreatment in FIG. 2 , and furthermore the reference symbols of FIG. 1 are used.
  • cellulose 3 , 4 (cf. FIG. 1 ) of the type MoDo Dissolving Wood Pulp, pine sulphite wood pulp, was placed in a pulper 5 from the company Grubbens with a net filling volume of 2 m 3 with water 6 in a mixing ratio of 1:17 (solids density 5.5%).
  • the cellulose exhibited a Cuoxam DP 650 and an ⁇ -cellulose content greater or less than 95%.
  • Commercially available celluloses based on hardwood or softwood can be used. Hemicellulose contents in the cellulose in the range from 2 to 20% can also be treated in the process.
  • celluloses Sappi Eucalyptus, Bacell Eucalyptus, Tembec Temfilm HW, Alicell VLV and Weyerelle ⁇ -cellulose of less than 95%.
  • the fed water 6 consisted of 30 parts of fully desalinated fresh water 15 and 70 parts of press water.
  • a cellulase enzyme complex such as for example Cellupract® AL 70 from Biopract GmbH or Cellusoft from Novo Nordisk, can be used as the enzyme preparation 52 .
  • the pretreatment was terminated in a process step B by the addition of sodium hydroxide solution 52 in the ratio of 1:500 referred to the cellulose content of the cellulose suspension in the pulper 5 .
  • the cellulose suspension was then dewatered in a process step C in a vacuum belt filter acting as press means 9 with following expressing system from the company Pannevis to about 50%, so that the expressed cellulose exhibited a dry content of about 50%. From step C, the expressed cellulose was then passed on via the pipe 8 for production of a cellulose solution containing NMMNO, water and cellulose. These steps are not shown in FIG. 2 for the sake of clarity.
  • the press water was collected in the press means 9 and let off via the pipe 11 (cf. FIG. 1 ). Approximately 75% of the press water was fed back to the pulper 5 and about 25% of the press water was passed via the pipe 16 to a waste water purifier.
  • the degree of polymerisation of the cellulose was always selected such that a DP (degree of polymerisation) of about 450 to about 550 was obtained in the spinning solution.
  • the cellulose concentration was set to about 12% in the spinning solution.
  • the press water remaining in the system 1 was again mixed in a mixing device 14 (cf. FIG. 1 ) in a process step D with the fully desalinated water, as described above.
  • the press water collected during the expressing stage was analyzed for the copper and iron ion content and additionally the chemical oxygen demand was determined.
  • FIG. 3 gives a schematic temporal progression of the iron ion extraction.
  • the chemical oxygen demand was determined in the press water according to DIN 38409 and approximates to a constant value with increasing duration of the press water feedback.
  • the cellulose solution obtained through press water feedback is stable and exhibits an onset temperature of at least 160° C. According to experiments, with this method an onset temperature of at the most 147° C. is actually obtained.
  • the onset temperature according to Table 1 using the method according to the invention with press water feedback also lies above the onset temperature as obtained with the method of WO 95/08010 and which in practice is about 150° C.
  • the onset temperatures still lie above the onset temperatures for the dry processing of cellulose and can be increased by an enzymatic pretreatment of the cellulose. This means that the press water feedback is suitable for industrial use.
  • the iron and copper content as well as the overall metal ion content of the cellulose varied noticeably with the various types of cellulose, as can be seen from Table 2.
  • the metal content of the various types of cellulose was determined by incineration in the platinum crucible according to DIN EN ISO 11885 (E22) and with flame AAS.
  • TABLE 2 Used cellulose Substances contained Cellulose Cellulose Cellulose Cellulose Cellulose Cellulose Cellulose Cellulose Cellulose in cellulose 1 mg/kg 2 mg/kg 3 mg/kg 4 mg/kg 5 mg/kg 6 mg/kg 7 mg/kg 8 mg/kg Fe 1.3 2.0 1.6 5.8 2.2 2.6 14 13 Mn ⁇ 0.3 ⁇ 0.1 0.2 0.33 n.d.
  • FIG. 5 the reference symbols of FIGS. 1 and 2 are used for elements with similar or the same function.
  • the amount of press water returned to the pulper 5 was adjusted to the iron and copper content of the expressed cellulose.
  • the iron ion and copper ion content was measured as representative values for the metal ion content by the sensors 23 , 23 ′ (cf. FIG. 1 ).
  • the iron concentration was maintained as closely as possible below 10 mg/kg absolutely dry and the copper concentration just below 0.5 mg/kg absolutely dry.
  • the setting of the metal ion content according to the invention can also be achieved via the tertiary amine oxide recovered from the spinning bath 28 .
  • the degree of purification at the metal ion filter 37 and/or the proportion of the tertiary amine oxide 36 freshly added to the regenerated tertiary amine oxide 34 can be set in dependence of the metal ion content as measured by the sensors 23 and 23 ′, as well as in dependence of the metal ion content previously found in the cellulose 3 , 4 .
  • the control functions similarly as with the press water feedback.
  • water from the spinning bath 28 recovered in the recovery device 30 can be returned to the pulper 5 instead of or together with the press water.
  • the metal ion filter 37 as it is used for the recovery of the tertiary amine oxide from the spinning bath 28 , can of course also be used for the purification of the returned press water.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Biochemistry (AREA)
  • Artificial Filaments (AREA)
  • Paper (AREA)
  • Electrotherapy Devices (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Casting Support Devices, Ladles, And Melt Control Thereby (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
US11/569,056 2004-05-13 2005-03-01 Lyocell Method and Device Involving the Control of the Metal Ion Content Abandoned US20070210481A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102004024029.9 2004-05-13
DE102004024029A DE102004024029A1 (de) 2004-05-13 2004-05-13 Lyocell-Verfahren und -Vorrichtung mit Steuerung des Metallionen-Gehalts
PCT/EP2005/002138 WO2005113870A1 (de) 2004-05-13 2005-03-01 Lyocell-verfahren und -vorrichtung mit steuerung des metallionen-gehalts

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EP (1) EP1745166B1 (de)
KR (1) KR100808288B1 (de)
CN (1) CN1997780A (de)
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DE (2) DE102004024029A1 (de)
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US20090026647A1 (en) * 2006-12-22 2009-01-29 Reifenhauser Gmbh & Co. Kg Maschinenfabrik Making a spunbond fleece from cellulosic filaments
US20110040029A1 (en) * 2007-08-16 2011-02-17 Josef Glaser Mixture, especially spinning solution

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AT512601B1 (de) * 2012-03-05 2014-06-15 Chemiefaser Lenzing Ag Verfahren zur Herstellung einer Cellulosesuspension
CN103173879B (zh) * 2013-04-01 2015-07-08 北京化工大学 单向排列的静电纺纳米初生长纤维的立式流动水浴收集方法及其装置
CN105525376B (zh) * 2015-11-27 2018-03-27 济南圣泉集团股份有限公司 一种再生纤维素纤维及其制备方法
EP3536850A1 (de) * 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Zellstoff und lyocellformkörper mit reduziertem cellulosegehalt
CN116005477B (zh) * 2023-02-23 2024-01-05 武汉虹之彩包装印刷有限公司 一种纸纤维染色前处理方法及芯层浆料比检测方法

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090026647A1 (en) * 2006-12-22 2009-01-29 Reifenhauser Gmbh & Co. Kg Maschinenfabrik Making a spunbond fleece from cellulosic filaments
US20110040029A1 (en) * 2007-08-16 2011-02-17 Josef Glaser Mixture, especially spinning solution
US8709272B2 (en) * 2007-08-16 2014-04-29 Helfenberger Immobilien Llc & Co Textilforschungs- Und Entwicklungs Keg Mixture, especially spinning solution

Also Published As

Publication number Publication date
TWI297743B (en) 2008-06-11
ATE393845T1 (de) 2008-05-15
EP1745166A1 (de) 2007-01-24
WO2005113870A1 (de) 2005-12-01
KR100808288B1 (ko) 2008-03-03
DE502005003909D1 (de) 2008-06-12
DE102004024029A1 (de) 2005-12-08
TW200604398A (en) 2006-02-01
CN1997780A (zh) 2007-07-11
EP1745166B1 (de) 2008-04-30
KR20070020290A (ko) 2007-02-20

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