EP1172478A1 - Process for loading fibers with calcium carbonate - Google Patents
Process for loading fibers with calcium carbonate Download PDFInfo
- Publication number
- EP1172478A1 EP1172478A1 EP01114534A EP01114534A EP1172478A1 EP 1172478 A1 EP1172478 A1 EP 1172478A1 EP 01114534 A EP01114534 A EP 01114534A EP 01114534 A EP01114534 A EP 01114534A EP 1172478 A1 EP1172478 A1 EP 1172478A1
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- European Patent Office
- Prior art keywords
- carbon dioxide
- fiber
- fiber suspension
- suspension
- chemical reaction
- Prior art date
- 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.)
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Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
- D21C9/004—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives inorganic compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
- D21H11/20—Chemically or biochemically modified fibres
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/70—Inorganic compounds forming new compounds in situ, e.g. within the pulp or paper, by chemical reaction with other substances added separately
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
Definitions
- the invention relates to a method for loading in a fiber suspension contained fibers with calcium carbonate through a chemical reaction.
- Fibrous suspensions of the type mentioned serve in particular the Paper and / or cardboard manufacturing.
- the strength that optical properties and the processability of the end product are crucial Role.
- the aim of the invention is in particular the method of the type mentioned with regard to the highest possible economy and the highest possible To further optimize the quality of the fiber suspension.
- this object is achieved by the fiber suspension a medium containing calcium oxide and / or calcium hydroxide is added, that the fibrous suspension treated in this way in particular in at least one Reactor with another, pure carbon dioxide or containing carbon dioxide Medium is applied and that in the course of the chemical reaction for a at least essentially complete conversion of the starting materials mentioned Calcium oxide or calcium hydroxide and carbon dioxide in the reaction products Calcium carbonate and water are taken care of by the pH of the pulp suspension is regulated accordingly. Thereby the measurement of the pH value at one or more points in the process flow.
- the fiber suspension (Pulp) has a consistency of greater than 5%, preferably between 15% to about 40%, which also in this area is adjustable.
- the calcium hydroxide preferably in liquid Form (milk of lime) is added. This means that not necessarily that possibly in or on the fibers of the fiber suspension Accumulated water is necessary for the start and completion of the chemical reaction is.
- calcium carbonate is deposited on the wetted fiber surfaces by adding calcium oxide and / or calcium hydroxide to the moist fiber material, at least some of which can be associated with the water of the fiber amount.
- the fiber material treated in this way is then charged with the pure carbon dioxide or with the medium containing carbon dioxide.
- the resulting CaCO 3 can form a suspension around the fibers.
- dry fiber surfaces can mean all wetted surfaces of the individual fibers. In particular, this also includes the case where the fibers both on their outer surface and inside (lumen) be loaded with calcium carbonate.
- the fibers are loaded with the filler calcium carbonate, the attachment to the wetted fiber surfaces being carried out by a so-called “Fiber Loading TM” process as described as such in US Pat. No. 5,223,090.
- the CO 2 reacts with the calcium hydroxide to form water and calcium carbonate.
- the pH of the fiber suspension is advantageously in a range of adjustable from about 5.5 to about 10.5.
- the ash content of the fiber suspension is in one Range is adjustable from about 1% to about 70%.
- the carbon dioxide is preferably supplied in gaseous form.
- the temperature of the supplied carbon dioxide can range from about - 10 ° to about 250 ° C adjustable or adjustable.
- optical properties for example whiteness, brightness, opacity, color locus, light scattering coefficient, used as an indicator of the course of the chemical reaction become.
- the pH is preferably at the end of the chemical reaction or after enlarging the specific surface by means of at least one Fluffers measured.
- pressure regulation is in the range from approximately 0.1 to approximately 20 bar intended.
- the fiber suspension becomes shear, preferably in at least a fluffer, exposed to to enlarge their specific surface.
- FIG. 1 shows a schematic representation of a purely exemplary embodiment of a device 10 for loading fibers contained in a fiber suspension with calcium carbonate (CaCO 3 ). Accordingly, this device 10 is used to store calcium carbonate on the wetted fiber surfaces of the fiber material. In principle, this loading of the fibers can take place in particular in accordance with the "Fiber Loading TM" process mentioned above.
- the device 10 can comprise one or more reactors R i , in which the fibrous suspension mixed with calcium oxide (CaO) and / or calcium hydroxide (Ca (OH) 2 ) contains pure carbon dioxide (CO 2 ) or a medium containing carbon dioxide (CO 2 ) is acted upon.
- reactors R i in which the fibrous suspension mixed with calcium oxide (CaO) and / or calcium hydroxide (Ca (OH) 2 ) contains pure carbon dioxide (CO 2 ) or a medium containing carbon dioxide (CO 2 ) is acted upon.
- a fluffer 14 can be provided before and / or after and / or in the reactor (s) R i , in which the fiber material of the fiber suspension is split with the aim of increasing the specific surface area of the fiber material in such a way that the accessibility for the Educts to the fiber material surface is optimized. This results in a further improvement of the homogenization and the "Fiber Loading TM" process is optimized accordingly.
- This can be done by subjecting the fiber suspension to shear forces, for example in a fluffer.
- the pH value measurement is preferably carried out at the end of the reaction, after the increase in the specific surface.
- the first fluffer 14 is provided between a refiner 16 and the reactor or reactors 12 i .
- a refiner 20 follows the tank 18, after which it goes to the paper machine PM.
- FIG. 1 The further details still contained in FIG. 1 are also purely exemplary and can be used individually or in any combination.
- the medium containing calcium oxide and / or calcium hydroxide can be added to the fiber material in such a way that at least some of it can associate with the water present in the fiber material, ie between the fibers, in the hollow fibers and in their walls.
- the following chemical reaction occurs:
- the "Fiber Loading "process is now preferably carried out so that the fiber suspension a medium containing calcium oxide and / or calcium hydroxide is added is that the fiber suspension treated in this way in particular in at least a reactor with another, pure carbon dioxide or containing carbon dioxide Medium is applied and that in the course of the chemical reaction for an at least substantially complete implementation of the above Starting materials calcium oxide or calcium hydroxide and carbon dioxide in the reaction products Calcium carbonate and water is taken care of by the pH of the Fibrous suspension is regulated accordingly.
- FIGS. 1a-c each show the pH for different exemplary embodiments displayed over the respective reaction time.
- Such a pH control is, for example, also the one shown in FIG. 2 Embodiment possible.
- the present fibrous raw material 22 in a pulper 24 processed into a fiber material 26, in which the fibers are then at least essentially already isolated, i.e. are separated from each other.
- the Fiber material 26 at least partially contains water. This can be both between the fibers as well as in the interior (lumens) and in the walls of the hollow fibers are present.
- the fiber material 26 can, for example, in Form of a so-called "dewatered crump pulp" (see. US-A-5,223,090) provided his.
- the fiber material 26 is then fed to a collecting container 28 or the like, in which an agent 30 containing calcium oxide and / or calcium hydroxide (slaked lime) is added in such a way that at least a part thereof coincides with that in the fiber material, ie between the fibers, in the hollow fibers and associated in their walls, existing water.
- an agent 30 containing calcium oxide and / or calcium hydroxide (slaked lime) is added in such a way that at least a part thereof coincides with that in the fiber material, ie between the fibers, in the hollow fibers and associated in their walls, existing water.
- the dry content of the fiber material can then be increased, for example, by feeding to a press 32, the press water 34 again is returned to the cycle.
- the fiber material 26 with the pure carbon dioxide or carbon dioxide-containing medium which in the figure 2 is indicated by the arrow pointing into the reactor 36.
- the pH of the fiber suspension can be measured to monitor and / or regulate the chemical reaction.
- the pH is preferably adjustable in a range from about 5.5 to about 10.5.
- the ash content of the fiber suspension can be regulated, for example, in a range from about 1% to about 70%.
- the carbon dioxide can in particular be supplied in gaseous form.
- the temperature of the carbon dioxide supplied is advantageously in a range of adjustable from about -10 ° to about 250 ° C.
- optical properties for example whiteness, brightness, opacity, Color locus, light scattering coefficient can be used.
- a dilution (H 2 O) is also possible in the areas designated "VD" in FIG. 1.
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Biochemistry (AREA)
- Paper (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zum Beladen von in einer Faserstoffsuspension enthaltenen Fasern mit Calciumcarbonat durch eine chemische Reaktion.The invention relates to a method for loading in a fiber suspension contained fibers with calcium carbonate through a chemical reaction.
Faserstoffsuspensionen der eingangs genannten Art dienen insbesondere der Papier- und/oder Kartonherstellung. Der insbesondere auch aus ökonomischen und ökologischen Gründen erforderliche schonende Umgang mit Rohstoffresourcen äußert sich bei der Papierherstellung in zunehmend niedrigeren Flächengewichten der Papierbahn sowie im teilweisen Ersatz des Faserstoffes durch Füllstoffe. Werden kostengünstigere Rohstoffe eingesetzt, so soll die Papierqualität zumindest beibehalten werden. Hierbei spielen unter anderem die Festigkeit, die optischen Eigenschaften sowie die Verarbeitbarkeit des Endproduktes eine entscheidende Rolle.Fibrous suspensions of the type mentioned serve in particular the Paper and / or cardboard manufacturing. The particularly from economic and ecological reasons necessary careful handling of raw material resources manifests itself in paper making in increasingly lower basis weights the paper web and in the partial replacement of the fibrous material with fillers. If cheaper raw materials are used, the paper quality should at least be maintained. Here, among other things, the strength that optical properties and the processability of the end product are crucial Role.
Ziel der Erfindung ist es, das Verfahren der eingangs genannten Art insbesondere im Hinblick auf eine möglichst hohe Wirtschaftlichkeit und eine möglichst hohe Qualität der Faserstoffsuspension weiter zu optimieren.The aim of the invention is in particular the method of the type mentioned with regard to the highest possible economy and the highest possible To further optimize the quality of the fiber suspension.
Diese Aufgabe wird nach der Erfindung dadurch gelöst, der Faserstoffsuspension ein Calciumoxid und/oder Calciumhydroxid enthaltendes Medium zugesetzt wird, daß die so behandelte Faserstoffsuspension insbesondere in wenigstens einem Reaktor mit einem weiteren, reines Kohlendioxid oder Kohlendioxid enthaltenden Medium beaufschlagt wird und daß im Verlauf der chemischen Reaktion für eine zumindest im wesentlichen vollständige Umsetzung der genannten Ausgangsstoffe Calciumoxid bzw. Calciumhydroxid und Kohlendioxid in die Reaktionsprodukte Calciumcarbonat und Wasser gesorgt wird, indem der pH-Wert der Faserstoffsuspension entsprechend geregelt wird. Dabei kann die Messung des pH-Wertes an einer oder mehreren Stellen im Prozeßablauf erfolgen. Die Faserstoffsuspension (Pulp) weist dabei eine Stoffdichte (Konsistenz) von größer 5%, vorzugsweise zwischen 15% bis etwa 40%, auf, die zudem in diesem Bereich noch regelbar ist.According to the invention, this object is achieved by the fiber suspension a medium containing calcium oxide and / or calcium hydroxide is added, that the fibrous suspension treated in this way in particular in at least one Reactor with another, pure carbon dioxide or containing carbon dioxide Medium is applied and that in the course of the chemical reaction for a at least essentially complete conversion of the starting materials mentioned Calcium oxide or calcium hydroxide and carbon dioxide in the reaction products Calcium carbonate and water are taken care of by the pH of the pulp suspension is regulated accordingly. Thereby the measurement of the pH value at one or more points in the process flow. The fiber suspension (Pulp) has a consistency of greater than 5%, preferably between 15% to about 40%, which also in this area is adjustable.
Bei Zusetzung eines Calciumoxid und/oder Calciumhydroxid enthaltenen Mediums an die Faserstoffsuspension läuft eine chemische Reaktion mit exothermer Eigenschaft ab, wobei das Calciumhydroxid vorzugsweise in flüssiger Form (Kalkmilch) zugesetzt wird. Dies bedeutet, daß nicht unbedingt das möglicherweise in bzw. an den Faserstoffen der Faserstoffsuspension ein- bzw. angelagerte Wasser zum Start und Ablauf der chemischen Reaktion notwendig ist.If calcium oxide and / or calcium hydroxide are added Medium to the fiber suspension runs a chemical reaction exothermic property, the calcium hydroxide preferably in liquid Form (milk of lime) is added. This means that not necessarily that possibly in or on the fibers of the fiber suspension Accumulated water is necessary for the start and completion of the chemical reaction is.
Aufgrund dieser Ausbildung wird eine deutlich höhere Wirtschaftlichkeit sowie eine höhere Qualität der Faserstoffsuspension erreicht.Due to this training, a significantly higher economy and a achieved higher quality of the fiber suspension.
Bei dem Beladen der Fasern wird Calciumcarbonat an die benetzten Faseroberflächen eingelagert, indem dem feuchten Fasermaterial Calciumoxid und/oder Calciumhydroxid zugesetzt wird, wobei zumindest ein Teil davon sich mit dem Wasser der Faserstoffmenge assoziieren kann. Das so behandelte Fasermaterial wird dann mit dem reinen Kohlendioxid oder mit dem Kohlendioxid enthaltenden Medium beaufschlagt. Überdies kann das entstandene CaCO3 um die Fasern eine Suspension bilden. When the fibers are loaded, calcium carbonate is deposited on the wetted fiber surfaces by adding calcium oxide and / or calcium hydroxide to the moist fiber material, at least some of which can be associated with the water of the fiber amount. The fiber material treated in this way is then charged with the pure carbon dioxide or with the medium containing carbon dioxide. In addition, the resulting CaCO 3 can form a suspension around the fibers.
Dabei kann der Begriff "benetzte Faseroberflächen" alle benetzten Oberflächen der einzelnen Fasern umfassen. Damit ist insbesondere auch der Fall mit erfaßt, bei dem die Fasern sowohl an ihrer Außenfläche als auch in ihrem Innern (Lumen) mit Calciumcarbonat beladen werden.The term "wetted fiber surfaces" can mean all wetted surfaces of the individual fibers. In particular, this also includes the case where the fibers both on their outer surface and inside (lumen) be loaded with calcium carbonate.
Demnach werden die Fasern mit dem Füllstoff Calciumcarbonat beladen, wobei die Anlagerung an die benetzten Faseroberflächen durch einen sog. "Fiber Loading ™" -Prozeß erfolgt, wie er als solcher in der US-A-5,223,090 beschrieben ist. In diesem "Fiber Loading™"-Prozeß reagiert das CO2 mit dem Calciumhydroxid zu Wasser und Calciumcarbonat.Accordingly, the fibers are loaded with the filler calcium carbonate, the attachment to the wetted fiber surfaces being carried out by a so-called "Fiber Loading ™" process as described as such in US Pat. No. 5,223,090. In this "Fiber Loading ™" process, the CO 2 reacts with the calcium hydroxide to form water and calcium carbonate.
Bei einer bevorzugten Ausgestaltung des erfindungsgemäßen Verfahrens wird der jeweilige pH-Istwert mit einem entsprechend vorgebbaren Sollwert verglichen und die Regelabweichung über wenigstens eine der folgenden Prozeßstellgrößen vermindert oder beseitigt:
- Verweilzeit der Faserstoffsuspension im Reaktor;
- Zuflußgeschwindigkeit der Faserstoffsuspension;
- Druck des Kohlendioxids;
- Temperatur der Faserstoffsuspension und/oder des Calciumhydroxids;
- Druck im Reaktor;
- Temperatur des CO2;
- Druck des CO2;
- Konzentration des CO2 im Medium;
- Konzentration des CaO, des Ca(OH)2 und der Fasern;
- spezifische Faseroberfläche.
- Residence time of the fiber suspension in the reactor;
- Flow rate of the pulp suspension;
- Pressure of carbon dioxide;
- Temperature of the fiber suspension and / or calcium hydroxide;
- Pressure in the reactor;
- Temperature of CO 2 ;
- Pressure of CO 2 ;
- Concentration of CO 2 in the medium;
- Concentration of CaO, Ca (OH) 2 and fibers;
- specific fiber surface.
Vorteilhafterweise ist der pH-Wert der Faserstoffsuspension in einem Bereich von etwa 5,5 bis etwa 10,5 regelbar. The pH of the fiber suspension is advantageously in a range of adjustable from about 5.5 to about 10.5.
Von Vorteil ist auch, wenn der Aschegehalt der Faserstoffsuspension in einem Bereich von etwa 1 % bis etwa 70 % regelbar ist.It is also advantageous if the ash content of the fiber suspension is in one Range is adjustable from about 1% to about 70%.
Das Kohlendioxid wird vorzugsweise gasförmig zugeführt.The carbon dioxide is preferably supplied in gaseous form.
Die Temperatur des zugeführten Kohlendioxids kann in einem Bereich von etwa - 10° bis etwa 250°C einstellbar oder regelbar sein.The temperature of the supplied carbon dioxide can range from about - 10 ° to about 250 ° C adjustable or adjustable.
In bestimmten Fällen ist es von Vorteil, wenn zusätzlich optische Eigenschaften, beispielsweise Weisse (Brightness), Helligkeit, Opazität, Farbort, Lichtstreuungskoeffizient, als Indikator für den Ablauf der chemischen Reaktion herangezogen werden.In certain cases it is advantageous if additional optical properties, for example whiteness, brightness, opacity, color locus, light scattering coefficient, used as an indicator of the course of the chemical reaction become.
Der pH-Meßort wird vorzugsweise wenigstens einer der folgenden Schritte gewählt wird:
- mindestens vor/nach Reaktion;
- auch während der Reaktion;
- ggf. mehrere Messungen.
- at least before / after reaction;
- also during the reaction;
- possibly several measurements.
Der pH-Wert wird dabei vorzugsweise am Ende der chemischen Reaktion oder nach der Vergrößerung der spezifischen Oberfläche mittels mindestens eines Fluffers gemessen.The pH is preferably at the end of the chemical reaction or after enlarging the specific surface by means of at least one Fluffers measured.
Erfindungsgemäß ist eine Druckregelung im Bereich von etwa 0,1 bis etwa 20 bar vorgesehen.According to the invention, pressure regulation is in the range from approximately 0.1 to approximately 20 bar intended.
Weiters wird die Faserstoffsuspension Scherkräften, vorzugsweise in mindestens einem Fluffer, ausgesetzt, um dadurch u.a. deren spezifische Oberfläche zu vergrößern. Furthermore, the fiber suspension becomes shear, preferably in at least a fluffer, exposed to to enlarge their specific surface.
Im übrigen kann bei dem Beladen der Fasern mit Calciumcarbonat insbesondere so vorgegangen werden, wie dies in der US-A-5,223,090 beschrieben ist. Der Inhalt dieser Druckschrift wird hiermit durch Bezugnahme in die vorliegende Anmeldung mit aufgenommen.Otherwise, in particular when loading the fibers with calcium carbonate proceed as described in US-A-5,223,090. The content this document is hereby incorporated by reference into the present application recorded with.
Weitere Merkmale und Vorteile der Erfindung ergeben sich aus der folgenden Beschreibung von Ausführungsbeispielen, bei der auf die Zeichnung Bezug genommen wird; in dieser zeigen:
- Figur 1:
- in schematischer Darstellung eine mögliche Ausführungsform einer Vorrichtung zum Beladen von in einer Faserstoffsuspension enthaltenen Fasern mit Calciumcarbonat;
- Figuren 1a - 1c:
- verschiedene pH-Wert-Verläufe über der Reaktionszeit; und
- Figur 2:
- eine schematische Darstellung einer weiteren Ausführungsform zum Beladen von Fasern.
- Figure 1:
- a schematic representation of a possible embodiment of a device for loading fibers contained in a fiber suspension with calcium carbonate;
- Figures 1a - 1c:
- different pH values over the reaction time; and
- Figure 2:
- is a schematic representation of another embodiment for loading fibers.
Figur 1 zeigt in schematischer Darstellung eine rein beispielhafte Ausführungsform
einer Vorrichtung 10 zum Beladen von in einer Faserstoffsuspension enthaltenen
Fasern mit Calciumcarbonat (CaCO3). Entsprechend dient diese Vorrichtung
10 der Einlagerung von Calciumcarbonat an die benetzten Faseroberflächen
des Fasermaterials. Dabei kann dieses Beladen der Fasern dem Prinzip
nach insbesondere entsprechend dem zuvor genannten "Fiber Loading™"-Prozeß
erfolgen.FIG. 1 shows a schematic representation of a purely exemplary embodiment of a
Die Vorrichtung 10 kann einen oder mehrere Reaktoren Ri umfassen, in der die
mit Calciumoxid (CaO) und/oder Calciumhydroxid (Ca(OH)2) versetzte Faserstoffsuspension
mit reinem Kohlendioxid (CO2) oder mit einem Kohlendioxid (CO2)
enthaltenden Medium beaufschlagbar ist.The
pH-Meßort:
- mindestens vor/nach Reaktion;
- auch während der Reaktion;
- ggf. mehrere Messungen.
- at least before / after reaction;
- also during the reaction;
- possibly several measurements.
Vor und/oder nach und/oder in dem bzw. den Reaktoren Ri kann jeweils ein Fluffer
14 vorgesehen sein, in dem das Fasermaterial der Fasersuspension mit dem
Ziel gespalten wird, die spezifische Oberfläche des Fasermaterials derart zu vergrößern,
daß die Zugänglichkeit für die Edukte an die Fasermaterialoberfläche
optimiert wird. Dadurch ergibt sich eine weitergehende Verbesserung der Homogenisierung
und der "Fiber Loading ™"-Prozeß wird entsprechend optimiert.
Dies kann dadurch geschehen, daß die Fasderstoffsuspension Scerkräften ausgesetzt
wird., z.B. in einem Fluffer. Die pH-Wert-Messung erfolgt vorzugsweise
am Ende der Reaktion, nach der Vergrößerung der spezifischen Oberfläche.
Bei dem vorliegenden Ausführungsbeispiel ist der erste Fluffer 14 zwischen einem
Refiner 16 und dem bzw. den Reaktoren 12i vorgesehen. Alternativ oder zusätzlich
ist es beispielsweise auch möglich, einen solchen Fluffer 14 zwischen dem
wenigstens einen Reaktor 12i und einem Tank 18 vorzusehen. Beim vorliegenden
Ausführungsbeispiel folgt auf den Tank 18 wieder ein Refiner 20, wonach es zur
Papiermaschine PM geht.A
This can be done by subjecting the fiber suspension to shear forces, for example in a fluffer. The pH value measurement is preferably carried out at the end of the reaction, after the increase in the specific surface.
In the present exemplary embodiment, the
Auch die weiteren in Figur 1 noch enthaltenen Angaben sind rein beispielhaft und einzeln oder in beliebiger Kombination verwendbar.The further details still contained in FIG. 1 are also purely exemplary and can be used individually or in any combination.
Beispielsweise mittels dieser Vorrichtung 10 kann somit eine Anlagerung von Calciumcarbonat
an die benetzten Faseroberflächen des Fasermaterials erfolgen,
wobei dieses Beladen der Fasern vom Prinzip her insbesondere wieder entsprechend
dem zuvor genannten "Fiber Loading™"-Prozeß erfolgen kann.By means of this
Dabei kann dem Fasermaterial das Calciumoxid und/oder Calciumhydroxid (gelöschter Kalk) enthaltende Medium insbesondere so zugesetzt werden, daß zumindest ein Teil davon sich mit dem im Fasermaterial, d.h. zwischen den Fasern, in den Hohlfasern und in deren Wänden, vorhandenen Wasser assoziieren kann, wobei sich die folgende chemische Reaktion einstellt: The medium containing calcium oxide and / or calcium hydroxide (slaked lime) can be added to the fiber material in such a way that at least some of it can associate with the water present in the fiber material, ie between the fibers, in the hollow fibers and in their walls. the following chemical reaction occurs:
In einem jeweiligen Reaktor wird das Fasermaterial dann derart mit Kohlendioxid
(CO2) beaufschlagt, daß Calciumcarbonat (CaCO3) an die benetzten Faseroberflächen
weitestgehend angelagert wird. Dabei stellt sich die folgende chemische
Reaktion ein:
(Calciumcarbonat + Wasser)
(Calcium carbonate + water)
Beispielsweise mittels der zuvor beschriebenen Vorrichtung wird bei dem "Fiber Loading"-Prozeß nun vorzugsweise so vorgegangen, daß der Faserstoffsuspension ein Calciumoxid und/oder Calciumhydroxid enthaltendes Medium zugesetzt wird, daß die so behandelte Faserstoffsuspension insbesondere in wenigstens einem Reaktor mit einem weiteren, reines Kohlendioxid oder Kohlendioxid enthaltenden Medium beaufschlagt wird und daß im Verlauf der chemischen Reaktion für eine zumindest im wesentlichen vollständige Umsetzung der genannten Ausgangsstoffe Calciumoxid bzw. Calciumhydroxid und Kohlendioxid in die Reaktionsprodukte Calciumcarbonat und Wasser gesorgt wird, indem der pH-Wert der Faserstoffsuspension entsprechend geregelt wird.For example, by means of the device described above, the "Fiber Loading "process is now preferably carried out so that the fiber suspension a medium containing calcium oxide and / or calcium hydroxide is added is that the fiber suspension treated in this way in particular in at least a reactor with another, pure carbon dioxide or containing carbon dioxide Medium is applied and that in the course of the chemical reaction for an at least substantially complete implementation of the above Starting materials calcium oxide or calcium hydroxide and carbon dioxide in the reaction products Calcium carbonate and water is taken care of by the pH of the Fibrous suspension is regulated accordingly.
Dabei ist es von Vorteil, wenn der jeweilige pH-Istwert mit einem entsprechend vorgebbaren Sollwert verglichen und die Regelabweichung über wenigstens eine der folgenden Prozeßstellgrößen vermindert oder beseitigt wird:
- Verweilzeit der Faserstoffsuspension im Reaktor;
- Zuflußgeschwindigkeit der Faserstoffsuspension;
- Druck des Kohlendioxids;
- Temperatur der Faserstoffsuspension und/oder des Calciumhydroxids;
- Druck im Reaktor;
- Temperatur des CO2;
- Druck des CO2;
- Konzentration des CO2 im Medium;
- Konzentration des CaO, des Ca(OH)2 und der Fasern;
- spezifische Faseroberfläche.
- Residence time of the fiber suspension in the reactor;
- Flow rate of the pulp suspension;
- Pressure of carbon dioxide;
- Temperature of the fiber suspension and / or calcium hydroxide;
- Pressure in the reactor;
- Temperature of CO 2 ;
- Pressure of CO 2 ;
- Concentration of CO 2 in the medium;
- Concentration of CaO, Ca (OH) 2 and fibers;
- specific fiber surface.
In den Figuren 1a - c sind für verschiedene Ausführungsbeispiele jeweils der pH-Wert über der jeweiligen Reaktionszeit dargestellt.FIGS. 1a-c each show the pH for different exemplary embodiments displayed over the respective reaction time.
Eine solche pH-Regelung ist beispielsweise auch bei der in der Figur 2 dargestellten Ausführungsform möglich.Such a pH control is, for example, also the one shown in FIG. 2 Embodiment possible.
Gemäß dieser Figur 2 wird das vorliegende Faserstoff-Ausgangsmaterial 22 in
einem Pulper 24 zu einem Fasermaterial 26 aufbereitet, in dem die Fasern dann
zumindest im wesentlichen bereits vereinzelt, d.h. voneinander getrennt sind. Das
Fasermaterial 26 enthält zumindest teilweise Wasser. Dieses kann sowohl
zwischen den Fasern als auch in den Innenräumen (Lumen) und in den Wänden
der Hohlfasern vorhanden sein. Das Fasermaterial 26 kann beispielsweise in
Form eines sogenannten "dewatered crump pulp" (vgl. die US-A-5,223,090) vorgesehen
sein.According to this FIG. 2, the present fibrous
Das Fasermaterial 26 wird anschließend einem Sammelbehälter 28 oder dergleichen
zugeführt, in dem ein Calciumoxid und/oder Calciumhydroxid (gelöschter
Kalk) enthaltendes Mittel 30 so zugesetzt wird, daß zumindest ein Teil davon sich
mit dem im Fasermaterial, d.h. zwischen den Fasern, in den Hohlfasern und in
deren Wänden, vorhandenen Wasser assoziiert. Dabei stellt sich wieder die folgende,
oben bereits erwähnte chemische Reaktion ein:
The
Im Anschluß daran kann der Trockengehalt des Fasermaterials erhöht werden,
beispielsweise durch Zuführung zu einer Presse 32, deren Preßwasser 34 wieder
in den Kreislauf zurückgeführt wird. In diesem beispielsweise durch zwei Fluffer
14 abgeschlossenen Reaktor 36 wird das Fasermaterial 26 mit dem reines Kohlendioxid
oder Kohlendioxid enthaltenden Medium beaufschlagt, was in der Figur
2 durch den in den Reaktor 36 weisenden Pfeil angedeutet ist.The dry content of the fiber material can then be increased,
for example, by feeding to a
Durch die Beaufschlagung des in der beschriebenen Weise bereits vorbehandelten
Fasermaterials mit dem reines Kohlendioxid oder Kohlendioxid enthaltenden
Medium stellt sich die folgende, zuvor ebenfalls bereits erwähnte chemische
Reaktion ein:
(Calciumcarbonat + Wasser)
(Calcium carbonate + water)
Unabhängig von der jeweiligen Art der verwendeten Vorrichtung sind hinsichtlich einer weiteren Optimierung des "Fiber Loading™"-Prozesses einzeln oder in beliebiger Kombination auch die folgenden Maßnahmen oder Merkmale von Vorteil:Regardless of the particular type of device used are regarding a further optimization of the "Fiber Loading ™" process individually or in any Combination also the following measures or features are advantageous:
Zur Überwachung und/oder Regelung der chemischen Reaktion kann der pH-Wert
der Faserstoffsuspension gemessen werden. Dabei ist der pH-Wert vorzugsweise
in einem Bereich von etwa 5,5 bis etwa 10,5 einstellbar.
Der Aschegehalt der Faserstoffsuspension ist beispielsweise in einem Bereich
von etwa 1% bis etwa 70% regelbar.The pH of the fiber suspension can be measured to monitor and / or regulate the chemical reaction. The pH is preferably adjustable in a range from about 5.5 to about 10.5.
The ash content of the fiber suspension can be regulated, for example, in a range from about 1% to about 70%.
Das Kohlendioxid kann insbesondere gasförmig zugeführt werden. Die Temperatur des zugeführten Kohlendioxids ist zweckmäßigerweise in einem Bereich von etwa -10° bis etwa 250°C einstellbar.The carbon dioxide can in particular be supplied in gaseous form. The temperature of the carbon dioxide supplied is advantageously in a range of adjustable from about -10 ° to about 250 ° C.
Als Indikatoren für die Regelung der chemischen Reaktion können beispielsweise optische Eigenschaften, beispielsweise Weisse (Brightness), Helligkeit, Opazität, Farbort, Lichtstreuungskoeffizient, herangezogen werden.As indicators for regulating the chemical reaction, for example optical properties, for example whiteness, brightness, opacity, Color locus, light scattering coefficient can be used.
Grundsätzlich ist es auch möglich, bei der Regelung der chemischen Reaktion als Regelgröße den pH-Wert, den Ascheanteil und/oder den Anteil an Calciumcarbonat (CaCO3) heranzuziehen.In principle, it is also possible to use the pH, the ash content and / or the calcium carbonate (CaCO 3 ) content as a controlled variable when regulating the chemical reaction.
In den in der Figur 1 mit "VD" bezeichneten Bereichen ist auch eine Verdünnung (H2O) möglich.A dilution (H 2 O) is also possible in the areas designated "VD" in FIG. 1.
Auch die im folgenden genannten Maßnahmen oder Merkmale können, einzeln
oder in beliebiger Kombination, einer weiteren Optimierung des Faserladeprozesses
dienen:
- Volumen und Massenstrom regelbar;
- Temperatur regelbar in einem Bereich von etwa 5°C bis etwa 95°C;
- Stoffdichte regelbar in einem Bereich von etwa 15% bis etwa 40%; vorzugsweise von etwa 20 % bis etwa 25 %;
- pH-Wert regelbar von etwa 10 bis etwa 13.
- Kristalltypen: rhomboedrisch, skalenoedrisch, rosettenartig, sphärisch, nadelförmig, prismenförmig, aragonitisch, plättförmig, GCC und ähnliche;
- Reaktion unter etwa 0,1
bis etwa 20 bar; - Temperatur von etwa -10° bis etwa 200°C;
- Verweilzeit von etwa 1 Minute bis etwa 1 Stunde.
- dient der Vergrößerung der spezifischen Oberfläche;
- einsetzbar vor und/oder nach und/oder in einem jeweiligen Reaktor bzw. den Reaktoren;
Spaltweite von etwa 0,1 bis etwa 100 mm, vorzugsweise einstellbar;- Energieeintrag in einen Bereich von etwa 5 kWh/t bis etwa 200 kWh/t.
- vor und/oder nach und/oder in einem jeweiligen Reaktor bzw. den Reaktoren bzw. dem "Fiber Loading™"-Prozeß.
- (*) Kristalltypen: romboedrisch, skalenoedrisch, rosettenartig, sphärisch, nadelförmig, prismenförmig, aragonitisch, plättförmig, GCC und ähnliche;
- (*) Reaktion unter etwa 0,1
bis etwa 20 bar; - (**) Temperatur in einem Bereich von etwa -10° bis etwa 250°C;
- (*) pH-Wert von etwa 5,5
bis etwa 10,5 regelbar; - (**)
Stoffdichte etwa 0,1% bis etwa 15%; - (**) CO2-Zugabe;
- (**) Verweilzeit.
- Bei einem zugrundeliegenden Massenanteil von etwa 1 % bis etwa 70 % des Füllstoffs, etwa 1 % bis etwa 60 % an den Fasern angelagerter Füllstoff, der Rest freies FLPCC™ (Fiber Loaded Precipiated Calcium Carbonate) in der Suspension.
- Volume and mass flow adjustable;
- Temperature adjustable in a range from about 5 ° C to about 95 ° C;
- Consistency adjustable in a range from about 15% to about 40%; preferably from about 20% to about 25%;
- pH adjustable from about 10 to about 13.
- Crystal types: rhombohedral, scalenohedral, rosette-like, spherical, needle-shaped, prism-shaped, aragonitic, plate-shaped, GCC and the like;
- Reaction under about 0.1 to about 20 bar;
- Temperature from about -10 ° to about 200 ° C;
- Residence time from about 1 minute to about 1 hour.
- serves to enlarge the specific surface;
- can be used before and / or after and / or in a respective reactor or reactors;
- Gap width from about 0.1 to about 100 mm, preferably adjustable;
- Energy input in a range from about 5 kWh / t to about 200 kWh / t.
- before and / or after and / or in a respective reactor or the reactors or the "Fiber Loading ™" process.
- (*) Crystal types: rhombohedral, scalenohedral, rosette-like, spherical, needle-shaped, prism-shaped, aragonitic, plate-shaped, GCC and the like;
- (*) Reaction under about 0.1 to about 20 bar;
- (**) temperature in a range from about -10 ° to about 250 ° C;
- (*) pH adjustable from about 5.5 to about 10.5;
- (**) consistency from about 0.1% to about 15%;
- (**) CO 2 addition;
- (**) dwell time.
- With an underlying mass fraction of about 1% to about 70% of the filler, about 1% to about 60% of the filler attached to the fibers, the rest free FLPCC ™ (Fiber Loaded Precipiated Calcium Carbonate) in the suspension.
- 1010
- Vorrichtung zum Beladen von FasernDevice for loading fibers
- 12i 12 i
- Reaktorreactor
- 1414
- FlufferFluffer
- 1616
- Refinerrefiner
- 1818
- Tanktank
- 2020
- Refinerrefiner
- 2222
- Ausgangsmaterialstarting material
- 2424
- Pulperpulper
- 2626
- Fasermaterialfiber material
- 2828
- SammelbehälterClippings
- 3030
- Calciumoxid und/oder Calciumhydroxid enthaltendes ReaktionsmittelContaining calcium oxide and / or calcium hydroxide reactant
- 3232
- PressePress
- 3434
- Preßwasserpress water
- 3636
- Reaktorreactor
- 3838
- VentilValve
- 4040
- Papiermaschinepaper machine
- VDVD
- Verdünnung (H2O)Dilution (H 2 O)
Claims (12)
dadurch gekennzeichnet,
characterized,
dadurch gekennzeichnet, daß der jeweilige pH-Istwert mit einem entsprechend vorgebbaren Sollwert verglichen und die Regelabweichung über wenigstens eine der folgenden Prozeßstellgrößen vermindert oder beseitigt wird:
characterized in that the respective actual pH value is compared with a correspondingly predeterminable target value and the control deviation is reduced or eliminated via at least one of the following process control variables:
dadurch gekennzeichnet, daß der pH-Wert der Faserstoffsuspension (26) in einem Bereich von etwa 5,5 bis etwa 10,5 regelbar ist.The method of claim 1 or 2,
characterized in that the pH of the fibrous stock suspension (26) can be regulated in a range from about 5.5 to about 10.5.
dadurch gekennzeichnet, daß der Aschegehalt der Faserstoffsuspension (26) in einem Bereich von etwa 1 % bis etwa 70 % regelbar ist.Method according to one of the preceding claims,
characterized in that the ash content of the fiber suspension (26) can be regulated in a range from approximately 1% to approximately 70%.
dadurch gekennzeichnet, daß das Kohlendioxid gasförmig zugeführt wird.Method according to one of the preceding claims,
characterized in that the carbon dioxide is supplied in gaseous form.
dadurch gekennzeichnet, daß die Temperatur des zugeführten Kohlendioxids in einem Bereich von etwa -10° bis etwa 250° C einstellbar oder regelbar ist. Method according to one of the preceding claims,
characterized in that the temperature of the supplied carbon dioxide is adjustable or controllable in a range from approximately -10 ° to approximately 250 ° C.
dadurch gekennzeichnet, daß zusätzlich optische Eigenschaften, beispielsweise Weisse (Brightness), Helligkeit, Opazität, Farbort, Lichtstreuungskoeffizient, als Indikatoren für den Ablauf der chemischen Reaktion herangezogen werden.Method according to one of the preceding claims,
characterized in that additional optical properties, for example whiteness, brightness, opacity, color locus, light scattering coefficient, are used as indicators for the course of the chemical reaction.
dadurch gekennzeichnet, daß bezüglich des pH-Meßortes wenigstens einer der folgenden Schritte gewählt wird:
characterized in that at least one of the following steps is selected with regard to the pH measuring location:
dadurch gekennzeichnet, daß der pH-Wert vorzugsweise am Ende der chemischen Reaktion gemessen wird.Method according to one of the preceding claims,
characterized in that the pH is preferably measured at the end of the chemical reaction.
dadurch gekennzeichnet, daß der pH-Wert vorzugsweise nach der Vergrößerung der spezifischen Oberfläche mittels mindestens eines Fluffers gemessen wird.Method according to one of claims 1 to 8,
characterized in that the pH is preferably measured after increasing the specific surface by means of at least one fluff.
dadurch gekennzeichnet, daß eine Druckregelung im Bereich von etwa 0,1 bis etwa 20 bar vorgesehen ist. Method according to one of the preceding claims,
characterized in that a pressure control in the range of about 0.1 to about 20 bar is provided.
dadurch gekennzeichnet, daß die Faserstoffsuspension (26) Scherkräften, vorzugsweise in mindestens einem Fluffer, ausgesetzt wird.Method according to one of the preceding claims,
characterized in that the fiber suspension (26) is subjected to shear forces, preferably in at least one fluffer.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10033979 | 2000-07-13 | ||
DE10033979A DE10033979A1 (en) | 2000-07-13 | 2000-07-13 | Method for loading fibers with calcium carbonate |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1172478A1 true EP1172478A1 (en) | 2002-01-16 |
EP1172478B1 EP1172478B1 (en) | 2004-09-08 |
Family
ID=7648737
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP01114534A Expired - Lifetime EP1172478B1 (en) | 2000-07-13 | 2001-06-16 | Process for loading fibers with calcium carbonate |
Country Status (6)
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---|---|
US (1) | US6537425B2 (en) |
EP (1) | EP1172478B1 (en) |
JP (1) | JP2002030592A (en) |
AT (1) | ATE275661T1 (en) |
CA (1) | CA2352885A1 (en) |
DE (2) | DE10033979A1 (en) |
Cited By (6)
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WO2003006740A1 (en) * | 2001-07-11 | 2003-01-23 | Voith Paper Patent Gmbh | Method of loading a fiber suspension with calcium carbonate |
WO2006048280A1 (en) | 2004-11-03 | 2006-05-11 | J. Rettenmaier & Söhne GmbH & Co. KG | Cellulose-containing filling material for paper, tissue, or cardboard products, method for the production thereof, paper, tissue, or cardboard product containing such a filling material, or dry mixture used therefor |
WO2008110191A1 (en) * | 2007-03-12 | 2008-09-18 | Voith Patent Gmbh | Method for the preparation of saturated fibers |
WO2008131819A1 (en) * | 2007-04-26 | 2008-11-06 | Voith Patent Gmbh | Method for loading fibres in a fibrous suspension with calcium carbonate formed from calcium hydrogen carbonate solution |
WO2008131820A1 (en) * | 2007-04-26 | 2008-11-06 | Voith Patent Gmbh | Method for loading fibres in a fibrous suspension with calcium carbonate formed from (hydrogen)carbonate compounds |
EP3127868B1 (en) | 2014-03-31 | 2021-06-16 | Nippon Paper Industries Co., Ltd. | Calcium-carbonate-microparticle/fiber composite and manufacturing method therefor |
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DE10107448A1 (en) * | 2001-02-16 | 2002-08-22 | Voith Paper Patent Gmbh | Method and device for loading fibers contained in a fiber suspension with a filler |
DE10120635A1 (en) * | 2001-04-27 | 2002-10-31 | Voith Paper Patent Gmbh | Method and device for loading fibers with calcium carbonate |
US7056419B2 (en) * | 2002-09-30 | 2006-06-06 | American Air Liquide, Inc. | Methods for modifying electrical properties of papermaking compositions using carbon dioxide |
US20040108083A1 (en) * | 2002-12-09 | 2004-06-10 | Specialty Minerals (Michigan) Inc. | Filler-fiber composite |
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DE10317719A1 (en) * | 2003-04-17 | 2004-11-11 | Voith Paper Patent Gmbh | Introducing calcium carbonate into cellulosic, fibrous papermaking suspension, adds calcium hydroxide, de-waters and injects carbon dioxide to precipitate carbonate in moist suspension |
DE10325688A1 (en) * | 2003-06-06 | 2004-12-23 | Voith Paper Patent Gmbh | Process to precipitate bulk calcium carbonate in a fibrous suspension by admixture of liquid or solid calcium hydroxide, or calcium oxide |
FI120463B (en) * | 2003-07-15 | 2009-10-30 | Upm Kymmene Corp | Method of making paper and paper |
FI119563B (en) * | 2003-07-15 | 2008-12-31 | Fp Pigments Oy | Process and apparatus for the pre-processing of fibrous materials for the production of paper, paperboard or other equivalent |
DE10347920A1 (en) * | 2003-10-15 | 2005-05-19 | Voith Paper Patent Gmbh | Method and device for loading a pulp suspension |
DE10347919A1 (en) * | 2003-10-15 | 2005-05-19 | Voith Paper Patent Gmbh | Method for adjusting a pH and machine for producing a fibrous web |
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GB0413068D0 (en) * | 2004-06-11 | 2004-07-14 | Imerys Minerals Ltd | Treatment of pulp |
DE102004045089A1 (en) * | 2004-09-17 | 2006-03-23 | Voith Paper Patent Gmbh | Method and device for loading a pulp suspension |
WO2007006369A1 (en) * | 2005-07-14 | 2007-01-18 | Voith Patent Gmbh | Method and device for loading fibres in a fibre suspension with filler |
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FI124831B (en) * | 2010-03-10 | 2015-02-13 | Upm Kymmene Oyj | Process and reactor for in-line production of calcium carbonate in a pulp flow |
FI125826B (en) * | 2010-08-04 | 2016-02-29 | Nordkalk Oy Ab | Process for the production of paper or board |
CN104818641B (en) * | 2015-05-08 | 2017-08-25 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | It is a kind of that the method that fiber discongests mashing is carried out based on flyash desiliconization liquid |
JP6530145B2 (en) | 2017-03-31 | 2019-06-12 | 日本製紙株式会社 | Method of manufacturing inorganic particle composite fiber sheet |
DE102020108071A1 (en) * | 2020-03-24 | 2021-09-30 | Delfortgroup Ag | Wrapping paper for smoking articles with improved ash appearance |
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- 2001-06-16 AT AT01114534T patent/ATE275661T1/en not_active IP Right Cessation
- 2001-06-16 DE DE50103512T patent/DE50103512D1/en not_active Expired - Fee Related
- 2001-07-11 CA CA002352885A patent/CA2352885A1/en not_active Abandoned
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WO2006048280A1 (en) | 2004-11-03 | 2006-05-11 | J. Rettenmaier & Söhne GmbH & Co. KG | Cellulose-containing filling material for paper, tissue, or cardboard products, method for the production thereof, paper, tissue, or cardboard product containing such a filling material, or dry mixture used therefor |
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WO2008131819A1 (en) * | 2007-04-26 | 2008-11-06 | Voith Patent Gmbh | Method for loading fibres in a fibrous suspension with calcium carbonate formed from calcium hydrogen carbonate solution |
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EP3127868B1 (en) | 2014-03-31 | 2021-06-16 | Nippon Paper Industries Co., Ltd. | Calcium-carbonate-microparticle/fiber composite and manufacturing method therefor |
Also Published As
Publication number | Publication date |
---|---|
DE10033979A1 (en) | 2002-01-24 |
JP2002030592A (en) | 2002-01-31 |
DE50103512D1 (en) | 2004-10-14 |
ATE275661T1 (en) | 2004-09-15 |
CA2352885A1 (en) | 2002-01-13 |
US6537425B2 (en) | 2003-03-25 |
US20020026989A1 (en) | 2002-03-07 |
EP1172478B1 (en) | 2004-09-08 |
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