EP1789363A1 - Method for preparing a carbon siccative for producing electrodes - Google Patents

Method for preparing a carbon siccative for producing electrodes

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Publication number
EP1789363A1
EP1789363A1 EP04764756A EP04764756A EP1789363A1 EP 1789363 A1 EP1789363 A1 EP 1789363A1 EP 04764756 A EP04764756 A EP 04764756A EP 04764756 A EP04764756 A EP 04764756A EP 1789363 A1 EP1789363 A1 EP 1789363A1
Authority
EP
European Patent Office
Prior art keywords
mill
classifier
adjusted
grain size
sifter
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.)
Granted
Application number
EP04764756A
Other languages
German (de)
French (fr)
Other versions
EP1789363B1 (en
Inventor
Jens-Peter Thiel
Thore MÖLLER
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.)
Claudius Peters Projects GmbH
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Claudius Peters Technologies GmbH
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C15/00—Disintegrating by milling members in the form of rollers or balls co-operating with rings or discs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B11/00—Arrangement of accessories in apparatus for separating solids from solids using gas currents
    • B07B11/04—Control arrangements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B7/00—Selective separation of solid materials carried by, or dispersed in, gas currents
    • B07B7/08—Selective separation of solid materials carried by, or dispersed in, gas currents using centrifugal force
    • B07B7/083—Selective separation of solid materials carried by, or dispersed in, gas currents using centrifugal force generated by rotating vanes, discs, drums, or brushes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C15/00—Disintegrating by milling members in the form of rollers or balls co-operating with rings or discs
    • B02C2015/002—Disintegrating by milling members in the form of rollers or balls co-operating with rings or discs combined with a classifier

Definitions

  • Electrodes which are primarily used for electro-metallurgical processes are produced by compressing körni ⁇ gene carbon masses (dry matter) with the addition of pitch as a binder.
  • the electrode quality depends crucially on the fact that a predetermined grain size spectrum is maintained in the dry matter.
  • Coarse grain, middle grain and fine grain must be selected according to the type of electrode and the fine grain
  • the mean grain size is usually at 30 to 60 microns corresponding to a specific surface of 5000 to 2000 cm 2 / g.
  • the invention is therefore based on the object of providing a method which is easier to influence with regard to the achievement of certain properties of the dust-like or fine-grained target fraction.
  • the solution according to the invention consists in that a mill-sifter combination with grain size that is continuously adjustable during operation is used for grinding the dust fraction.
  • a roller mill with integrated sifter has proven particularly useful, in which the grinding pressure and preferably the rotational speed of the mill and the throughput of air through the mill and the sifter are adjustable.
  • a classifier preferably a dynamic classifier is used, in which the speed should be adjustable for the purpose of adjusting the grain boundaries.
  • the grinding pressure can be adjusted. Since petroleum coke, which is mostly used as a raw material, is unusually hard, the grinding pressure is set two to three times as high as conventional coal grinding.
  • the amount of system air that is, the amount of air flow that carries the refined fines from the refining zone to the sifter, can be reduced if lower maximum grain size is desired, and vice versa.
  • the maximum grain size can also be influenced by the speed of the dynamic classifier. Depending on the type of classifier, further parameters can be added to influence the particle size.
  • the sifter is preferably a known dynamic type, in which the airflow of the mill laden with ground material is guided from the outside to the inside through a ring of tangentially arranged guide vanes and is thereby set in circular motion. Farther inside, it reaches a rotating basket on a spiral track, which is operated at an adjustable speed. The fine particles penetrate the columns of the rotating cage with the flow of air, while the coarser ones are thrown outward again to flow in the space between vanes and
  • the fines thus obtained and continuously removed from the air flow in a known manner no longer require any subsequent homogenization. It can be continuously fed directly to a silo, from which it is taken directly or indirectly, preferably continuously borrowed for use.
  • This silo can also be dimensioned smaller than previously customary, because no mill changeover takes into account quality change Need to become. Even if parameters of the grinding or visual process have to be adapted due to quality changes of the raw material or changes in the formulation, the mill-sifter combination can be continuously operated. If a fundamental formulation change becomes necessary, the conversion can take place in a few minutes.
  • the product which may be obtained in the conversion phase and does not correspond to the target quality can be briefly subjected to intermediate silicidation and then returned to the mill. The continuous operation is thereby practically not interrupted.
  • the Umsehaltvorgang vorzugswei ⁇ se computer controlled, with programmed overrides are used to avoid the accumulation of intermediate product (Abmahlmann) or minimize.
  • the product for example, which is obtained as a loss from grinding, is collected in an intermediate silo and preferably added to the feed material in a computer-controlled manner so that no environmentally harmful product waste is produced.
  • roller mills ball ring mills, roller mills, roller mills and single-roller mills
  • All grindable carbon carriers up to the hardest petroleum cokes can be processed.
  • the driers can be prepared for all types of electrodes with different hardness and fineness requirements.
  • the bandwidth of the producible grains is very large. It is preferably in the range of 1,000 to 10,000 cmVg.
  • the essential advantage of the invention is that the grinding process can be switched on continuously and at the same time into the production process. Since the ensiling is partly avoided, partly facilitated and in particular large silos are avoided, the hitherto often extremely disturbing problem of segregation of different grain within the silos is avoided.

Abstract

The invention relates to a method for preparing a carbon siccative for producing electrodes. The dust fraction is continuously produced by means of a grinder/sifter combination with a particle size or specific surface that can be adjusted during the operation, preferably by means of a roller grinding mill comprising an integrated sifter.

Description

Claudius Peters Technologies GmbH CLAT034PWOClaudius Peters Technologies GmbH CLAT034PWO
Verfahren zum Aufbereiten von Kohle-Trockenstoff für dieProcess for treating coal dry matter for the
Herstellung von ElektrodenProduction of electrodes
Elektroden, die vornehmlich für elektro-metallurgische Pro- zesse verwendet werden, werden durch Verpressen von körni¬ gen Kohlenstoffmassen (Trockenstoff) unter Zusatz von Pech als Bindemittel hergestellt. Die Elektrodenqualität hängt entscheidend davon ab, daß im Trockenstoff ein vorbestimm¬ tes Korngrößenspektrum eingehalten wird. Grobkorn, Mittel- körn und Feinkorn müssen je nach Art der Elektrode und desElectrodes which are primarily used for electro-metallurgical processes are produced by compressing körni¬ gene carbon masses (dry matter) with the addition of pitch as a binder. The electrode quality depends crucially on the fact that a predetermined grain size spectrum is maintained in the dry matter. Coarse grain, middle grain and fine grain must be selected according to the type of electrode and the fine grain
Rohstoffs in bestimmten Verhältnismengen darin vertreten sein. Von besonderer Bedeutung ist dabei die Einhaltung ei¬ ner vorgegebenen Qualität des Feinguts. Darunter fällt im Zusammenhang der Erfindung hauptsächlich der sogenannte Staubanteil, dessen mittlere Korngröße in der Regel bei 30 bis 60 μm entsprechend einer spezifischen Oberfläche von 5000 bis 2000 cm2/g liegt.Raw material in certain proportions. Of particular importance is the observance of a given quality of the fine material. Including in the context of the invention mainly the so-called dust content, the mean grain size is usually at 30 to 60 microns corresponding to a specific surface of 5000 to 2000 cm 2 / g.
Bei bekannten Herstellungsverfahren (DE-A-4122062) werden die einzelnen Fraktionen gebrochen bzw. gemahlen und schließlich klassiert und in gesonderten Dosiersilos abge¬ legt, um daraus nach der jeweiligen Rezeptur in einem ge¬ wünschtem Verhältnis abgezogen zu werden. Die Staubfraktion wird gesondert in einer Rohrmühle (Kugelmühle) gemahlen und homogenisiert, bevor sie gleichfalls in Dosiersilos abge¬ legt wird. Dieses Verfahren hat den Nachteil, daß es nur sehr schwerfällig verändert werden kann, wenn eine Rezep¬ turänderung oder Schwankungen in der Qualität des Rohmate¬ rials eine Anpassung verlangen. Bei der Einstellung der Staubeigenschaften in Abhängigkeit von der Mahlbarkeit des Kokses und den jeweiligen wechselnden Anforderungen wird das bekannte Verfahren im Start/Stop-Betrieb durchgeführt, was zu unregelmäßiger Staubqualität hinsichtlich des Durch¬ satzes, der Feinheit und der spezifischen Oberfläche führt. Dies hat unterschiedlichen Pechbedarf und unerwünscht schwankende physikalische Eigenschaften der Elektroden zur Folge.In known production processes (DE-A-4122062), the individual fractions are crushed or ground and finally classified and deposited in separate metering silos, in order to be withdrawn therefrom according to the respective recipe in a desired ratio. The dust fraction is separately ground and homogenized in a tube mill (ball mill) before it is likewise deposited in dosing silos. This method has the disadvantage that it can only be changed very cumbersome if a recipe change or fluctuations in the quality of the raw material require adaptation. When adjusting the dust properties depending on the grindability of the coke and the respective changing requirements the known method is carried out in start / stop operation, which leads to irregular dust quality in terms of Durch¬ rate, the fineness and the specific surface. This results in different pitch requirements and undesirably fluctuating physical properties of the electrodes.
Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfah¬ ren zu schaffen, das im Hinblick auf die Erreichung be- stimmter Eigenschaften der staubförmigen bzw. feinkörnigen Zielfraktion leichter beeinflußbar ist.The invention is therefore based on the object of providing a method which is easier to influence with regard to the achievement of certain properties of the dust-like or fine-grained target fraction.
Die erfindungsgemäße Lösung besteht darin, daß zum Mahlen der Staubfraktion eine Mühle-Sichter-Kombination mit wäh- rend des Betriebs kontinuierlich verstellbarer Korngröße verwendet wird. Besonders bewährt hat sich die Verwendung einer Wälzmühle mit integriertem Sichter, bei der der Mahl¬ druck und vorzugsweise die Mühlendrehzahl und der Luft¬ durchsatz durch die Mühle und den Sichter verstellbar sind. Als Sichter wird vorzugsweise ein dynamischer Sichter ver¬ wendet, bei dem zum Zwecke der Verstellung der Korngrenzen die Drehzahl verstellbar sein sollte.The solution according to the invention consists in that a mill-sifter combination with grain size that is continuously adjustable during operation is used for grinding the dust fraction. The use of a roller mill with integrated sifter has proven particularly useful, in which the grinding pressure and preferably the rotational speed of the mill and the throughput of air through the mill and the sifter are adjustable. As a classifier, preferably a dynamic classifier is used, in which the speed should be adjustable for the purpose of adjusting the grain boundaries.
Unter einer Mühle-Sichter-Kombination wird eine solche FunktionsVerbindung einer Mühle mit einem Sichter verstan¬ den, bei der das vom Sichter ausgesonderte Überkorn in die Mühle zurückgeführt wird. Diese Kombination erlaubt eine besonders feine Einstellung ohne wesentliche Totzeichen, weil sowohl auf die Eigenschaften des Sichters als auch auf diejenigen der Mühle Einfluß genommen werden kann. Man er¬ reicht damit die kontinuierliche Herstellung vorgegebener Staubmengen beliebiger Feinheiten bei unterschiedlicher Mahlbarkeit durch Anpassung der Drehzahl, des Anpreßdrucks, der Systemluftmenge und/oder der Sichterdrehzahl.Under a mill-sifter combination, such a functional connection of a mill with a sifter is understood, in which the oversized grain separated from the sifter is returned to the mill. This combination allows a particularly fine setting without significant dead-mark, because both the properties of the classifier and those of the mill can be influenced. It thus achieves the continuous production of predetermined amounts of dust of arbitrary fineness with different grindability by adjusting the speed, the contact pressure, the system air quantity and / or the classifier speed.
Zur Berücksichtigung unterschiedlicher Härten des Rohguts kann der Mahldruck verstellt werden. Da der als Rohmaterial größtenteils verwendete Petrolkoks ungewöhnlich hart ist, wird der Mahldruck zwei- bis dreimal so hoch eingestellt wie bei üblicher Kohlemahlung. Die Systemluftmenge, d.h. die Stärke des Luftstroms, der das ermahlene Feingut aus der Mahlzone emporträgt zum Sichter, kann geringer einge- stellt werden, wenn geringere maximale Korngröße gewünscht wird, und umgekehrt. Die maximale Korngröße kann auch durch die Drehzahl des dynamischen Sichters beeinflußt werden. Je nach Typ des Sichters können weitere Parameter zur Beein¬ flussung der Korngröße hinzutreten.To take account of different hardnesses of the raw material, the grinding pressure can be adjusted. Since petroleum coke, which is mostly used as a raw material, is unusually hard, the grinding pressure is set two to three times as high as conventional coal grinding. The amount of system air, that is, the amount of air flow that carries the refined fines from the refining zone to the sifter, can be reduced if lower maximum grain size is desired, and vice versa. The maximum grain size can also be influenced by the speed of the dynamic classifier. Depending on the type of classifier, further parameters can be added to influence the particle size.
Bei dem Sichter handelt es sich vorzugsweise um einen be¬ kannten dynamischen Typ, bei welchem der mit vermählenem Gut beladene Luftstrom der Mühle von außen nach innen durch einen Ring von tangential angeordneten Leitschaufeln ge- führt und dadurch in Kreisbewegung versetzt wird. Weiter innen erreicht er auf einer Spiralbahn einen Drehkorb, der mit einer einstellbaren Drehzahl betrieben wird. Die feinen Partikeln durchdringen die Spalten des Drehkorbs mit dem Luftstrom, während die gröberen wieder nach außen geschleu- dert werden, um in dem Raum zwischen Leitschaufeln undThe sifter is preferably a known dynamic type, in which the airflow of the mill laden with ground material is guided from the outside to the inside through a ring of tangentially arranged guide vanes and is thereby set in circular motion. Farther inside, it reaches a rotating basket on a spiral track, which is operated at an adjustable speed. The fine particles penetrate the columns of the rotating cage with the flow of air, while the coarser ones are thrown outward again to flow in the space between vanes and
Drehkorb nach unten zu sinken und von dort dem Mahlprozeß wieder zugeführt zu werden. Das Feingut verläßt den Sichter mit dem Luftstrom, wobei sich seine Feinheit über die Ein¬ stellung der Drehkorb-Drehzahl und die Stärke des Luft- Stroms bestimmen läßt.Rotating basket to sink down and from there to be fed back to the grinding process. The fine material leaves the separator with the air flow, whereby its fineness can be determined by setting the rotary basket speed and the strength of the air flow.
Da auf Schwankungen in der Qualität des Rohmaterials rasch und kontinuierlich während des Betriebs reagiert werden kann und da der gewünschte Korngrößenbereich kontinuierlich genau eingehalten werden kann, bedarf das so gewonnene und dem Luftstrom in bekannter Weise kontinuierlich entnommene Feingut keiner nachträglichen Homogenisierung mehr. Es kann kontinuierlich unmittelbar einem Silo zugeführt werden, aus dem es unmittelbar oder mittelbar vorzugsweise kontinuier- lieh zur Verwendung entnommen wird. Dieses Silo kann auch kleiner als bisher üblich dimensioniert werden, weil keine Mühlenumstellzeiten bei Qualitätsänderung berücksichtigt werden müssen. Auch wenn Parameter des Mahl- oder Sichtvor¬ gangs aufgrund von Qualitätsänderungen des Rohmaterials oder Änderungen der Rezeptur angepaßt werden müssen, kann die Mühle-Sichter-Kombination kontinuierlich weiterbetrie- ben werden. Falls eine grundlegende Rezepturänderung not¬ wendig wird, kann die Umstellung in wenigen Minuten erfol¬ gen. Das in der Umstellungsphase ggf. anfallende, der Ziel¬ qualität nicht entsprechende Produkt kann kurzzeitig zwi¬ schensiliert und anschließend der Mühle wieder zugeführt werden. Der kontinuierliche Betrieb wird dadurch praktisch nicht unterbrochen. Der Umsehaltvorgang erfolgt vorzugswei¬ se rechnergesteuert, wobei programmierte Übersteuerungen eingesetzt werden, um den Anfall an Zwischenprodukt (Abmahlverlust) zu vermeiden oder zu minimieren. Das etwa als Abmahlverlust anfallende Produkt wird in einem Zwi¬ schensilo aufgefangen und dem Aufgabegut vorzugsweise rech¬ nergesteuert so beigemischt, daß keine umweltbelastenden Produktabfälle entstehen.Since fluctuations in the quality of the raw material can be reacted rapidly and continuously during operation, and since the desired particle size range can be continuously maintained precisely, the fines thus obtained and continuously removed from the air flow in a known manner no longer require any subsequent homogenization. It can be continuously fed directly to a silo, from which it is taken directly or indirectly, preferably continuously borrowed for use. This silo can also be dimensioned smaller than previously customary, because no mill changeover takes into account quality change Need to become. Even if parameters of the grinding or visual process have to be adapted due to quality changes of the raw material or changes in the formulation, the mill-sifter combination can be continuously operated. If a fundamental formulation change becomes necessary, the conversion can take place in a few minutes. The product which may be obtained in the conversion phase and does not correspond to the target quality can be briefly subjected to intermediate silicidation and then returned to the mill. The continuous operation is thereby practically not interrupted. The Umsehaltvorgang vorzugswei¬ se computer controlled, with programmed overrides are used to avoid the accumulation of intermediate product (Abmahlverlust) or minimize. The product, for example, which is obtained as a loss from grinding, is collected in an intermediate silo and preferably added to the feed material in a computer-controlled manner so that no environmentally harmful product waste is produced.
Alle Typen von Wälzmühlen (Kugelringmühlen, Walzenteller¬ mühlen, Walzenschüsselmühlen bis hin zu Einwalzenmühlen) können zum Einsatz kommen. Alle mahlbaren Kohlenstoffträger bis hin zu den härtesten Petrolkoksen können verarbeitet werden. Es können die Trockenstoffe für alle Typen von Elektroden mit unterschiedlichsten Anforderungen an Härte und Feinheit zubereitet werden. Die Bandbreite der erzeug¬ baren Körnungen ist sehr groß. Sie liegt vorzugsweise im Bereich von 1.000 bis 10.000 cmVg.All types of roller mills (ball ring mills, roller mills, roller mills and single-roller mills) can be used. All grindable carbon carriers up to the hardest petroleum cokes can be processed. The driers can be prepared for all types of electrodes with different hardness and fineness requirements. The bandwidth of the producible grains is very large. It is preferably in the range of 1,000 to 10,000 cmVg.
Während es bislang erforderlich war, verschiedene Fraktio¬ nen zeitversetzt zu erzeugen und das Produkt in gesonderten Silos zwischen zu lagern, besteht der wesentliche Vorteil der Erfindung darin, daß der Mahlvorgang kontinuierlich und zeitgleich in den Produktionsvorgang eingeschaltet werden kann. Da die Silierung teils vermieden, teils erleichtert wird und insbesondere große Silos vermieden werden, wird das bisher häufig äußerst störende Problem der Segregation unterschiedlicher Körnung innerhalb der Silos vermieden. While it has hitherto been necessary to generate different fractions with a time delay and to store the product in separate silos, the essential advantage of the invention is that the grinding process can be switched on continuously and at the same time into the production process. Since the ensiling is partly avoided, partly facilitated and in particular large silos are avoided, the hitherto often extremely disturbing problem of segregation of different grain within the silos is avoided.

Claims

Patentansprüche claims
1. Verfahren zum Aufbereiten von Kohle-Trockenstoff für die Herstellung von Elektroden, bei dem Fraktionen un¬ terschiedlicher Körnung hergestellt und in einem vorbe¬ stimmten Verhältnis gemischt werden und bei dem die Fraktionen mindestens eine staubförmige bis feinkörnige Fraktion umfassen, die auf eine vorbestimmte, einstell¬ bare Korngröße gemahlen wird, dadurch gekennzeichnet, daß zum Mahlen der staubförmigen bis feinkörnigen Frak¬ tion eine Mühle-Sichter-Kombination mit während des Be¬ triebs kontinuierlich verstellbarer Korngröße verwendet wird.1. A process for preparing coal dry matter for the production of electrodes, in which fractions of different grain size are produced and mixed in a predetermined ratio and in which the fractions comprise at least one dust-like to fine-grained fraction which corresponds to a predetermined, adjustable grain size is ground, characterized in that for grinding the dust-like to fine-grained Frak¬ tion, a mill-sifter combination is used with continuously variable grain size during Be¬ operation.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Mühle-Sichter-Kombination eine Wälzmühle mit inte¬ griertem Sichter verwendet wird.2. The method according to claim 1, characterized in that a roller mill with inte¬ grated classifier is used as a mill-sifter combination.
3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß der Mahldruck der Mühle verstellt wird.3. The method according to claim 2, characterized in that the grinding pressure of the mill is adjusted.
4. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß die Drehzahl des Mühlenantriebs verstellt wird.4. The method according to claim 2, characterized in that the rotational speed of the mill drive is adjusted.
5. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß der Luftdurchsatz der Mühle und des Sichters verstellt wird.5. The method according to claim 2, characterized in that the air flow rate of the mill and the classifier is adjusted.
6. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeich¬ net, daß ein dynamischer Sichter verwendet wird.6. The method according to claim 1 or 2, characterized gekennzeich¬ net, that a dynamic separator is used.
7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß die Drehzahl des Sichters verstellt wird.7. The method according to claim 6, characterized in that the rotational speed of the classifier is adjusted.
8. Verfahren nach einem der Ansprüche 1 bis 7, dadurch ge¬ kennzeichnet, daß die Mühle-Sichter-Kombination während des kontinuierlichen Betriebs etwaigen QualitatsSchwan¬ kungen des Rohmaterials oder Rezepturänderungen ange¬ paßt wird. 8. The method according to any one of claims 1 to 7, characterized ge indicates that the mill-classifier combination during of the continuous operation, any quality fluctuations in the raw material or changes in formulation are adapted.
EP04764756A 2004-09-02 2004-09-02 Method for preparing a carbon siccative for producing electrodes Revoked EP1789363B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2004/009798 WO2006024315A1 (en) 2004-09-02 2004-09-02 Method for preparing a carbon siccative for producing electrodes

Publications (2)

Publication Number Publication Date
EP1789363A1 true EP1789363A1 (en) 2007-05-30
EP1789363B1 EP1789363B1 (en) 2009-02-11

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US (1) US8052077B2 (en)
EP (1) EP1789363B1 (en)
JP (1) JP4857271B2 (en)
CN (1) CN100548876C (en)
DE (1) DE502004008991D1 (en)
WO (1) WO2006024315A1 (en)

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WO2006024315A1 (en) 2006-03-09
US20070284463A1 (en) 2007-12-13
CN101010258A (en) 2007-08-01
JP4857271B2 (en) 2012-01-18
US8052077B2 (en) 2011-11-08
DE502004008991D1 (en) 2009-03-26
CN100548876C (en) 2009-10-14
JP2008511525A (en) 2008-04-17
EP1789363B1 (en) 2009-02-11

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