EP1369521B1 - Procédé pour le mercerisage en continu des fils textiles - Google Patents

Procédé pour le mercerisage en continu des fils textiles Download PDF

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Publication number
EP1369521B1
EP1369521B1 EP03076705A EP03076705A EP1369521B1 EP 1369521 B1 EP1369521 B1 EP 1369521B1 EP 03076705 A EP03076705 A EP 03076705A EP 03076705 A EP03076705 A EP 03076705A EP 1369521 B1 EP1369521 B1 EP 1369521B1
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EP
European Patent Office
Prior art keywords
yarns
bundle
mercerization
yarn
treatment
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP03076705A
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German (de)
English (en)
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EP1369521A3 (fr
EP1369521A2 (fr
Inventor
Roberto Badiali
Mario Minuti
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Savio Macchine Tessili SpA
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Savio Macchine Tessili SpA
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Publication of EP1369521A3 publication Critical patent/EP1369521A3/fr
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/04—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of yarns, threads or filaments
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B7/00—Mercerising, e.g. lustring by mercerising
    • D06B7/04—Mercerising, e.g. lustring by mercerising of yarns, threads or filaments
    • D—TEXTILES; PAPER
    • D07—ROPES; CABLES OTHER THAN ELECTRIC
    • D07B—ROPES OR CABLES IN GENERAL
    • D07B7/00—Details of, or auxiliary devices incorporated in, rope- or cable-making machines; Auxiliary apparatus associated with such machines
    • D07B7/02—Machine details; Auxiliary devices
    • D07B7/04—Devices for imparting reverse rotation to bobbin- or reel cages

Definitions

  • the present invention relates to the treatment of yarns with process fluids to give them the desired characteristics for their final use for producing fabrics or other end-products.
  • the treatment of yarn with reagent liquids is adopted for a wide variety of processings, for different types of fibres such as cotton, wool, silk, linen, etc., which give the yarn the desired characteristics or remove undesired components that reduce their value and the possibility of use.
  • this type of treatment can relate to dyeing, mercerizing, bleaching, washing, sizing and so forth.
  • Batch processing on yarn is generally extremely onerous due to the considerable labour involved, the low performance of the process fluids, the high plant investments and finally as a result of the environmental implications caused by the reagents discharged with the waste water which consequently require further costs to bring the drain water within specification.
  • Batch treatment also has the additional problem of the constancy of the product quality for each processing batch, depending on the variability of the parameters of each single batch processing such as temperatures, times, concentrations, etc.
  • mercerizing consists in the treatment of yarn with alkaline solutions - typically caustic soda, but possibly also with other basic compounds - at a high concentration, followed by drawing.
  • alkaline solutions typically caustic soda, but possibly also with other basic compounds - at a high concentration, followed by drawing.
  • the mercerizing treatment of cellulose yarn improves its mechanical properties, it enhances its gloss and also its adsorption capacity and reactivity towards the finishing products and the affinity to dyes. This enhancements takes place on the single fibers of the yarn in a state of semi-plasticity induced by the concentrated alkalis with which they are soaked.
  • mercerizing is typically carried out on skeins of yarn, suitably prepared by means of a reeling step, which are subjected to batch mercerizing and are then washed, neutralized, dried, unwound and reformed in bobbins.
  • Proposals have also been made in the known art to treat yarns with mercerizing solutions by first preparing the single yarn with winding onto beams, each having hundreds of yarn.
  • the yarns are unwound from the beams in parallel, passed individually in a sequence of tanks at atmospheric pressure containing soda baths and other treatment fluids, drawn by pairs of rolls and rewound onto other beams or onto single spools.
  • the objective of the present invention is to provide a continuous treatment system of yarns with process fluids and, specifically mercerizing fluids, which allows the drawbacks of the systems available in the known art, to be overcome.
  • Figure 1 illustrates the general scheme of the treatment system of yarns with process fluids.
  • Figure 2 shows an embodiment variation of the mercerizing tubular reactor.
  • the yarn 1 to be treated is fed starting from a series of bobbins 2 arranged in parallel on specific unwinding creels, not shown in the figure for the sake of simplicity, which release a series of parallel yarns which are concentrated in a cable laying funnel 3 forming a bundle 4 of yarns 1 adhering to each other.
  • the process and the device according to the invention can also operate on a single yarn 1, but their industrial application is more interesting - for its productivity and efficiency - with numerous yarns, preferably collected in a bundle 4 consisting of from 20 to 200 yarns or more, depending on their number and characteristics.
  • At least one auxiliary thread 5 with long coils, indicatively having a shed of 200 to 1500 mm, is wound around them, accompanying the bundle during its processing, and is subsequently separated and recovered at the end of the processing line.
  • This expedient in the case of the breakage of one or more single yarns 1, prevents them from not continuing their run through the overall machinery but, with continuous feeding, they accumulate in one of the continuous processing machines.
  • said winding is effected with one or more auxiliary threads 5 with a high chemical and mechanical resistance - for example made of Kevlar - which are released from one or more bobbins 8 held by a rotating reel, not shown in the figure for the sake of simplicity, around the bundle 4 and rotating according to the arrow A.
  • An alternative for increasing the adherence between the yarns 1 of the bundle 4 can be to apply a slight twisting to the bundle itself, a few twists per meter, assembling the creel of the bobbins 2 on a rotating support, according to the rope-making technique.
  • the pulling of the yarns 1 to form the bundle 4 is effected with the pair of guiding rolls 10, which rotate at a controlled rate and which determine the linear pulling-rate of the bundle 4 of yarns 1 being processed, generally at a rate in the order of hundreds of m/min, sending it to the mercerizing reactors.
  • An important characteristic of the present invention consists in the treatment operation and structure of the reactor in which the treatment of the bundle 4 of yarns 1 is effected with the process fluid which, in the illustrative present description, consists of an alkaline solution of sodium hydrate at a high concentration.
  • This operation is carried out in a tubular reactor 15 with a vertical axis and equipped at the beginning with an ejector cr a Venturi tube 16.
  • the ejector or Venturi tube 16 is fed with a pressurized driving fluid consisting of the mercerizing alkaline solution, for example sodium hydrate at 30° Be, which corresponds to about 297 g/l, the bundle 4 of yarns 1 is guided by a deviator roll 9 and introduced into the reactor 15, with an inlet hole in correspondence with the depression of the contracted vein of the Venturi 16 fluid.
  • the fluid sucks and pulls the bundle 4 of yarns 1 from the bobbins 2 released at a controlled rate by the initial guiding rolls 10.
  • the bundle 4 of yarns 1 passes through the tubular reactor 15, along its axial direction, and exits with the mercerizing fluid from its lower output 17.
  • the inlet pressure of the treatment fluid is regulated so as to obtain, in correspondence with the contracted vein of the ejector 16, a driving fluid rate ranging from 12 to 40 m/sec, preferably from 15 to 20 m/sec.
  • a collection tank 18 of the mercerizing solution is situated in correspondence with the lower output 17 of the tubular reactor 15 of the ejector type.
  • the bundle 4 of yarns 1, on the other hand, is resent upwards by means of a diverting pulley 19 immersed in the liquid collected in the tank 18, it passes, through a loose squeezing group 20 consisting of one or more couples of loose rolls 21 pressed against each other, which squeeze the solution in excess held by the yarn bundle 4.
  • the tank 18 has an overflow mouth 22 which maintains the liquid level inside; the alkaline mercerizing solution is collected from said tank, filtered, reconditioned with respect to concentration and temperature, and then recycled to mercerizing section according to known techniques.
  • the ascending bundle 4 of yarns 1 is subjected to the control and regulation of its tension value by means of the compensator 25, which is illustrated with reference to the subsequent figure 2, and is therefore pulled upwards by the drawing device 30, comprising the discharge rolls 31, which operates at a linear rate corresponding to the shortening induced in the treatment in the reactor 15, for example at 60-70% of the arrival rate of the bundle 4 at the Venturi 16.
  • the discharge rolls 31 also act as gripping rolls for the drawing of the bundle 4 due to the effect of the drawing rolls 32, situated downstream of the gripping rolls and are rotated with a higher rate than the rolls 31, for example at 90% of the arrival rate of the bundle 4 at the Venturi 16, thus recovering most of the shortening induced in the yarns 1 and providing the tension necessary for fully receiving the benefits obtained from the mercerization.
  • the yarn is then discharged from the mercerization unit by means of the directional deviator rolls 33.
  • figure 1 shows a second mercerizing reactor 15', completely analogous to the previous one.
  • the same numerical references refer to similar components and having the same function.
  • the alkaline mercerizing solution again induces an enlargement and shortening of the yarns 1 which form the bundle 4, so that it is pulled with the discharge rolls 31' at a linear rate which corresponds to the new shortening obtained in the treatment in the reactor 15'.
  • the discharge rolls 31' and the drawing rolls 32' operate completely analogously to the previous ones and at a linear rate which obtains a tension and induces a drawing with the recovery of length of the bundle of up to 90% of the initial arrival value of the bundle 4 at the-Venturi 16.
  • the yarn is then discharged by means of directional deviator rolls 33'.
  • the treatment is perfected and a new shortening of the yarn is obtained, which is again drawn in the intermediate section between the rolls 31' and 32' and, for example, brought back to the value of 90% of the initial length which it had in correspondence with the initial guiding rolls 10.
  • the bundle 4 of yarns 1 is fed to the washing with water.
  • the washing is effected in several steps, with water in countercurrent and at a decreasing temperature, so that the last washing is carried out with the purest and coldest water and thus using the resulting water, containing the removed soda, for the next-to-last washing, and so on.
  • the water coming from the first washing, containing the soda removed in the series of countercurrent washings can then be used to prepare the concentrated mercerizing solution for being reintegrated in the plant.
  • the illustrative scheme of figure 1 shows, to simplify the drawing, two washing steps in countercurrent.
  • the mercerized bundle 4 of yarns 1, guided by the directional rolls 33', is introduced in the first washing step into the unit 40, by means of the Venturi nozzle 41 fed with a pressurized stream of washing water coming from the subsequent step.
  • the bundle 4 enters the Venturi 41 in correspondence with one of its side holes in correspondence with the depression of the contracted vein of the fluid which sucks the bundle 4 of yarns 1, creating close contact between the mercerized yarns forming the bundle and the washing water.
  • the bundle 4 of yarns 1 leaves the Venturi 41 together with the washing water which is collected in the collection tank 42 of the mercerization solution.
  • the bundle 4 of yarns 1 is, on the contrary, resent upwards by means of a loose diverting roll 44, immersed in the water collected in the tank 42, it passes through a squeezing group 45 consisting of one or more pairs of loose rolls 46 pressed against each other, which squeeze the solution in excess held by the bundle 4 of yarns 1.
  • the tank 42 is provided with a overflow mouth 47, from which the washing water is recovered and re-used.
  • the bundle 4 of yarns 1, rising from the washing unit, is subjected to the control and regulation of its tension value by means of the compensator 50, analogous to the compensator 25, which is illustrated with reference to the following figure 2, and is therefore pulled upwards by the final drawing device 51, completely analogous to the drawing devices 30 and 30'.
  • the final drawing unit 51 situated between the two washing steps, consists of a pair of gripping rolls 52, and a subsequent pair of drawing rolls 53, which operate so as to restore, for example, the initial length of the bundle 4 of yarns 1.
  • the gripping rolls 52 operate at the linear rate with which the bundle 4 leaves the lower part of the Venturi 41.
  • the subsequent drawing rolls 39 are activated, on the other hand, at the same linear rate as that of the arrival of the bundle 4 at the first Venturi 16, thus completely recovering the entire shortening induced in the yarns 1 and providing the definite mercerizing tension.
  • the yarn is then discharged with the directional deviator rolls 55.
  • figure 1 shows a second washing unit 40', completely analogous to the previous unit 40.
  • the same reference numbers refer to similar components and having the same function.
  • the Venturi nozzle 41' is fed with a pressurized stream of the purest washing water, whereas the water coming from the second unit 40' is used as feeding in the first unit 40.
  • the neutralization unit 40" is completely analogous to the washing unit 40' and operates again with a Venturi nozzle 41", this time fed with a pressurized stream of a diluted solution of acetic acid to remove the alkaline residue from the yarns of the bundle 4.
  • the same reference numbers in unit 40" refer to similar components and having the same function as unit 41'.
  • the neutralization solution is collected in the underlying tank 42" and is recycled; the pH of the resulting acetic solution is checked in the tank 42", and its composition is controlled, before being recycled, for any possible corrections to be made to its number and to verify the neutralization trend.
  • the bundle 4 of yarns 1 washed in units 40, 40' and neutralized in unit 40" is then subjected to a complete drying step, for example in the drying unit 60 with a winding path around the cylindrical surfaces of a series of squeezing cylinders 61 and drying cylinders 62 heated with diathermic oiL.
  • drying with hot air can be effected at about 100°C, after a passage through a Venturi with a depression of around 200 mbar to remove the liquid particles still separated.
  • the yarns forming the bundle 4 of yarns 1 thus mercerized are then separated in the separation unit 70 of the bundle 4, according to an inverse process with respect to that previously effected.
  • the first step consists in unwinding one or more auxiliary threads 5 initially wound, which are rewound onto one or more bobbins 71 held by a rotating reel, not shown in the figure for the sake of simplicity, around the bundle 4 and rotating according to the arrow B, in the opposite direction to the arrow A and with the same winding shed.
  • the yarns 1 become parallel again and are no longer constrained in the bundle and can be separated by passing them in their guide yarns 72 to be rewound onto separate bobbins of mercerized yarn.
  • An important characteristic of the present invention is the way in which the yarn is impregnated with the process fluid, and essentially in the specific case of the mercerization of cellulose fibers.
  • the impregnation and reaction step is effected in very short times in the reactor 15, starting in the Venturi 16.
  • a high flow-rate is established with respect to the bundle 4 of yarn 1, and there is a vortical motion and brusque involvement also of the yarns inside the bundle 4.
  • the mercerization treatment can be repeated once or several times in subsequent reaction steps, to graduate its effect and then complete the drawing action after the washing, until the desired result is obtained.
  • FIG. 2 shows an embodiment variation of the reactor with the ejector 16 forming the first part of the tubular mercerization reactor 15.
  • the single Venturi nozzle 16 described above, in the mercerization reactor 85 is substituted by several, i.e. two or more Venturi tubes in series along the reactor, in which the bundle 4 of yarns 1 passes in sequence, from the first Venturi 86' to the subsequent Venturi tubes 86" , 86''', and so on.
  • the Venturi driving fluid consists again of the treatment solution: in this particular case the mercerization alkaline solution.
  • the inlet 87 of the pressurized driving fluid in the Venturi 86 are situated at the side, whereas the bundle 4 of yarns 1 follows, in a straight path, the axis of the sequence of the Venturi nozzles in the reactor 85.
  • the stream of driving fluid under pressure can thus be subdivided and distributed among the inlets 87', 87'', . . . so as to gradually increase the volumetric ratio between the volume fed of mercerizing solution and the amount of yarn operating in the axial direction, from the beginning to the end of the sequence.
  • the bundle 4 of yarns 1 being processed enters in an axial direction from the first Venturi 86' and axially follows the whole sequence receiving, in correspondence with each narrowing and depression of the contracted vein of the fluid, the arrival of the partialized stream of driving fluid from their entrances 87.
  • a second further embodiment variation of the invention contemplates, in correspondence with the first entrance 87 for the process fluid, an entrance 83 for service connection with compressed air, both for maintenance operations and for the activation of the reaction unit with the insertion of the bundle 4 in the sequence of Venturi tubes 86.
  • This embodiment variation of the reactor 85 with several Venturi nozzles 86 in series allows a more effective contact and sealing for the fluids and can be adopted both for mercerizing reactors and for the subsequent washing and neutralization operations of the yarn 4 after the treatment with alkaline solutions.
  • FIG. 2 shows an illustrative structure of the compensator 25, with which the tension of the bundle 4 of yarns 1 rising towards the drawing system, is regulated and controlled.
  • the compensator comprises two end pulleys 91, 91' situated at the ends of a telescopic rod 92 whose extremes are maintained in extension by an internal spring 93 set under compression.
  • the higher tension of the bundle 4 of yarns 1 tends to draw the end pulleys 91, 91' closer and compress the spring 93.
  • the telescopic rod 92 for example, has the lower end fixed to the structure and the upper end free to be extended: the pulley 91 is therefore free to move away from the pulley 91', which remains still.
  • Two reference points 94 and 94' are situated on the telescopic rod 92, which represent fixed and adjustable limits of the approaching and distancing run end, respectively, of the two pulleys, detected by two proximity sensors 95 and 95', connected to the driving unit of the device
  • the tension increases to the maximum value allowed and the driving unit of the treatment device operates an increase in the feeding rate of the yarn bundle 4.
  • the sensor 95' detects that the reference point 94' has reached the allowed extension limit of the telescopic rod and that the tension has been reduced to the minimum value allowed
  • the driving unit of the treatment device causes a decrease in the feeding rate of the yarn bundle 4 until the telescopic rod has been extended to an intermediate value.
  • the driving unit of the device remains inactive in the regulation of the feeding rate of the bundle.
  • the treatment operations with process fluids are effected with continuous operations, and not on lots of yarn, without requiring previous preparation on bobbins or skeins followed by their unwinding and re-preparation.
  • continuous yarn processing is more economical, due to the lesser amount of labour used, the high performance of the process fluids and washing water, the lower overall plant investments and, finally, fewer environmental implications as a result of the reduced quantity of reagents discharged with the waste water.
  • the constancy of the product quality which is obtained with the continuous treatment system according to the present invention is considerably improved, due to the constancy of the parameters of each processing step which can be maintained at the desired temperature, time, concentration values.
  • the amounts of treatment solutions are extremely limited and, as far as the mercerizing alkaline solutions are concerned, their carbonation is very moderate.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Claims (7)

  1. Procédé pour le mercerisage de fils comprenant une ou plusieurs étapes de traitement du fil avec une solution alcaline, une ou plusieurs étapes d'étirage du fil après le traitement alcalin, une ou plusieurs étapes de lavage aqueux et de neutralisation du résidu alcalin encore présent dans le fil, caractérisé en ce que le procédé est mis en oeuvre, en continu, selon les étapes successives suivantes :
    - les fils (1) sont rassemblés dans un faisceau (4) préparé dans une section (6) dans laquelle une solidarité est conférée entre les fils et sont ensuite amenés avec un dispositif d'alimentation (10),
    - le faisceau (4) de fils (1) est introduit pour le traitement de mercerisage dans le réacteur tubulaire (15, 85) par aspiration avec un ajutage Venturi (16, 86') dans lequel la solution de mercerisage alcaline est amenée comme un fluide d'entraînement sous pression, entraînant avec elle le faisceau (4) de fils (1) et réagit dans un ou plusieurs réacteurs (15, 85) à partir duquel/desquels elle sort depuis la partie inférieure, tirée par des rouleaux de décharge (31, 31'),
    - le faisceau (4) est subséquemment étiré en continu dans une ou plusieurs unités d'étirage comprenant des rouleaux de saisie et de décharge (31, 31') et des rouleaux d'étirage (32, 32') situés en aval, qui sont amenés à tourner à une vitesse supérieure à celle des rouleaux (31, 31').
  2. Procédé pour le mercerisage de fils selon la revendication 1, caractérisé en ce que les étapes de traitement ultérieur de fils mercerisés après l'étirage avec les fluides de traitement sont mises en oeuvre en continu en mettant en contact le faisceau (4) avec lesdits fluides de traitement dans des ajutages Venturi (41, 41', 41"), chacun alimenté avec le fluide de traitement, comme fluide d'entraînement, entraînant avec lui le faisceau (4) de fils (1) .
  3. Procédé pour le mercerisage de fils selon la revendication 1, caractérisé en ce que, en correspondance avec la veine contractée de l'ajutage Venturi (16), le débit du fluide d'entraînement est maintenu entre 12 et 40 m/s.
  4. Procédé pour le mercerisage de fils selon la revendication 3, caractérisé en ce que, en correspondance avec la veine contractée de l'ajutage Venturi (16), le débit du fluide d'entraînement est maintenu entre 15 et 20 m/s.
  5. Procédé pour le mercerisage de fils selon la revendication 1, caractérisé en ce que, dans le réacteur de mercerisage (85), le faisceau (4) de fils (1) traverse séquentiellement un ou plusieurs tubes Venturi (86', 86", 86''') disposés en séries le long du réacteur lui-même.
  6. Procédé pour le mercerisage de fils selon la revendication 5, caractérisé en ce que, dans le réacteur de mercerisage (85), le courant de fluide d'entraînement sous pression est subdivisé et réparti parmi les entrées (87', 87") des ajutages Venturi (86', 86", ...) pour augmenter graduellement le rapport volumétrique entre le volume du fluide de traitement amené et la quantité de fil traitée dans la direction axiale.
  7. Procédé pour le mercerisage de fils selon la revendication 1, caractérisé en ce que le faisceau (4) est constitué de 20 à 200 fils (1).
EP03076705A 2002-06-05 2003-06-02 Procédé pour le mercerisage en continu des fils textiles Expired - Lifetime EP1369521B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ITMI20021220 2002-06-05
IT2002MI001220A ITMI20021220A1 (it) 2002-06-05 2002-06-05 Procedimento e dispositivo per il mercerizzo in continuo dei filati tessili

Publications (3)

Publication Number Publication Date
EP1369521A2 EP1369521A2 (fr) 2003-12-10
EP1369521A3 EP1369521A3 (fr) 2005-03-23
EP1369521B1 true EP1369521B1 (fr) 2007-08-08

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US (1) US20030226346A1 (fr)
EP (1) EP1369521B1 (fr)
CN (1) CN1311118C (fr)
AT (1) ATE369453T1 (fr)
DE (1) DE60315377D1 (fr)
EG (1) EG24384A (fr)
IT (1) ITMI20021220A1 (fr)

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ITMI20061767A1 (it) 2006-09-15 2008-03-16 Savio Macchine Tessili Spa Procedimento e dispositivo per la mercerizzazione in continuo di filati tessili
DE102007010866A1 (de) 2007-03-02 2008-09-04 Leibniz-Institut für Naturstoff-Forschung und Infektionsbiologie e.V. -Hans-Knöll-Institut- Vorrichtung und Verfahren zur Durchführung von emersen Mikrokultivierungen bei Mikroorganismen und Zellen
CN101525826B (zh) * 2009-03-10 2012-05-09 东华大学 一种纱线束状连续回流丝光的方法
DE102009052953A1 (de) * 2009-11-12 2011-05-19 Fleissner Gmbh Vorrichtung zum Waschen von gesponnenen Filamenten
CN102809499B (zh) * 2012-08-15 2015-01-14 中国科学院宁波材料技术与工程研究所 一种碳纤维拉伸性能测试的制样方法
CN102926149B (zh) * 2012-11-12 2013-12-18 无锡市天然绿色纤维科技有限公司 一种辫子连续丝光机及其加工方法
CN104452144A (zh) * 2014-12-11 2015-03-25 区有辉 一种经轴纱线丝光上浆的生产设备及制作工艺
EP3494254B1 (fr) 2016-08-04 2021-09-29 PVH Corp. Tissus et vêtements sans repassage, et leur procédé de finition
KR101878786B1 (ko) * 2016-12-30 2018-07-17 주식회사 효성 파라 아라미드 필라멘트의 수세 및 중화 장치

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DE60315377D1 (de) 2007-09-20
ITMI20021220A1 (it) 2003-12-05
CN1469001A (zh) 2004-01-21
EP1369521A3 (fr) 2005-03-23
ATE369453T1 (de) 2007-08-15
US20030226346A1 (en) 2003-12-11
CN1311118C (zh) 2007-04-18
EG24384A (en) 2009-04-07
EP1369521A2 (fr) 2003-12-10

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