EP1252388B1 - Use of a compound for reducing and/or avoiding the build up of wood components - Google Patents
Use of a compound for reducing and/or avoiding the build up of wood components Download PDFInfo
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- EP1252388B1 EP1252388B1 EP00993298A EP00993298A EP1252388B1 EP 1252388 B1 EP1252388 B1 EP 1252388B1 EP 00993298 A EP00993298 A EP 00993298A EP 00993298 A EP00993298 A EP 00993298A EP 1252388 B1 EP1252388 B1 EP 1252388B1
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- Prior art keywords
- wood
- acid ester
- volatile
- use according
- compound
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
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- 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/22—Other features of pulping processes
- D21C3/226—Use of compounds avoiding scale formation
Definitions
- the present invention relates to the avoidance and / or reduction of deposits of volatile and non-volatile wood constituents in gas-carrying systems, the volatile wood constituents at least partially condensing in the gas-carrying systems.
- the present invention further relates to the reduction and / or avoidance of deposits of wood constituents on machines and / or system parts for the production of wood fibers from wood chips.
- EP-A-0 334 098 describes a method for reducing deposits in Equipment for the evaporation of waste liquors from wood pulp production by Sulfite waste liquor low molecular weight polyacrylic acid is added.
- the deposits are gypsum or silicate deposits that fail during the process.
- US-A-5 762 757 describes a method of preventing deposits organic pulp ingredients such as pitch and sticky Contamination in pulp or paper making systems by a anionic surfactant from the group of Dinonyl sulfosuccinates or a mixture of Dioctyl sulfosuccinate and didecyl sulfosuccinate are either added to the pulp or is applied to the surface of the system.
- DE-A-27 35 300 A describes a method for the aftertreatment of vapor condensate for the distillative removal and burning of steam-volatile oxygen-consuming substances, from liquids and wet combustion non-volatile components. Part of the substances present in the wood are volatile in water and are present in the vapor condensate. In the process the substances are burned at over 1000 ° C.
- WO-A-98/33970 describes a process for the production of fibrous materials for the Production of pulp, paper or wood-based panels, in which the Pretreatment for impregnating dicarboxylic acid dialkyl esters and / or one or several fatty acid polyol mono, di, tri and / or higher polyesters and / or Polyester-polyether copolymers are added. These components clean the Primary fibers from resin components and other wood constituents and cause one higher yield and better optics.
- the present invention is therefore based on the object of a method for To provide with the deposition of volatile and / or non-volatile Wood ingredients in gas-carrying systems is at least reduced.
- Volatile wood constituents in the sense of the invention are all wood constituents that Temperatures above 20 ° C have a vapor pressure.
- reaction products within the meaning of the invention are any products that contain the volatile wood constituents after the condensation, e.g. B. by polymerization.
- the deposits usually have non-volatile wood constituents, e.g. B. fine Wood particles, which separate from the gas stream and sticky films adhere.
- connection has a similar condensation behavior like the wood ingredients; d. H. the connection and the wood constituents condense preferably at the same point in the gas-carrying system and preferably form there a movie.
- the compound is preferably a dicarboxylic acid ester.
- the dicarboxylic acid ester is a dicarboxylic acid dialkyl and / or diisoalkyl ester of C2-C12 Dicarboxylic acids with C1-C13 n- and / or iso-alkanols such as di-n-butyl oxalate, di-n-butyl malonate, Di-n-butyl succinate, di-n-butyl glutarate, di-n-butyl adipate, di-n-butyl suberate, Di-n-butyisebacate, dimethyl adipate, di-n-propyl adipate, diisopropyl adipate, Diisobutyl adipate, di-tert-butyl adipate, di-isoamyl adipate, di-n-hexyl adipate, di- (2-ethylbutyl
- the compound is very particularly preferably a di-n-alkyladipic acid ester and / or a di-iso-alkyl adipic acid ester.
- the most preferred is the compound n-dibutyl adipate.
- the gas-carrying system is very particularly preferably part of a plant for the production from Thermo-Mechanical-Pulp (TMP) or a wood chip refiner system, as described in WO-A-96/41914, which is hereby introduced as a reference becomes.
- TMP Thermo-Mechanical-Pulp
- WO-A-96/41914 WO-A-96/41914
- the gas that flows through the gas-carrying lines can be any gas be, but preferably has water vapor.
- the compound is preferably metered into the gas in gaseous form.
- the specialist realizes that the compound can also be metered into the gas in the liquid state can and then there is converted into a gaseous state.
- the dosage is preferably carried out continuously.
- the dosage of the compound depends on the concentration of the volatile wood constituents in the gas and the gas volume flow.
- The is preferably Concentration 100-5000 ppm, particularly preferably 200-2000 ppm and very particularly preferably 300-1000 ppm.
- the compound is preferably metered into the gas in such an amount that there are no deposits of volatile or non-volatile compounds and / or form their reaction products on the surfaces of the gas-carrying systems or that deposits already formed detach and / or dissolve again. Accordingly the dosage of the compound is preferably regulated automatically.
- the pressure loss in the pipelines is preferably used as the control parameter the gas-carrying system and / or the degree of separation of cyclones, which are in the gas-carrying system. Are also preferred as Control parameters also the gas volume flow and the concentration of volatile Wood ingredients used in the gas or the area coverage.
- connection also be steam-volatile.
- the present invention has the advantage that the gas-carrying systems are less common must be cleaned and the systems therefore have a longer operating time. There z. B. Cyclones are no longer added by deposits, their separability remains receive. Existing deposits are reduced.
- Another object of the present invention is to provide a method to reduce and / or avoid deposits of wood constituents on machines and / or system parts for the production of wood fibers Wood chips (wood chips).
- Deposits in the sense of the invention are any deposits of wood constituents in gas-carrying systems and / or on other systems or Machine parts that are used for the production of wood fiber materials.
- the compound is preferably a dicarboxylic acid ester.
- the dicarboxylic acid ester is a dicarboxylic acid dialkyl and / or diisoalkyl ester of C2-C12 Dicarboxylic acids with C1-C13 n- and / or iso-alkanols such as di-n-butyl oxalate, di-n-butyl malonate, Di-n-butyl succinate, di-n-butyl glutarate, di-n-butyl adipate, di-n-butyl suberate, Di-n-butyl sebacate, dimethyl adipate, di-n-propyl adipate, diisopropyl adipate, Diisobutyl adipate, di-tert-butyl adipate, di-isoamyl adipate, di-n-hexyl adipate, di- (2-ethylbutyl
- the compound is very particularly preferably a di-n-alkyladipic acid ester and / or a di-iso-alkyl adipic acid ester.
- the most preferred is the compound Di-n-butyl adipate.
- esters can be used alone or in combination with water-soluble or water-insoluble ones
- Solvents as water-free or water-containing solution or as water-containing Dispersion, preferably emulsion, are used.
- Suitable solvents are n- and iso-alkanols, liquid hydrocarbons, acetone and others known solvents, in particular natural oils or modified natural oils, such as beet oil methyl ester.
- Nonionic, ionic and Amphoteric, especially nonionic, surfactants are used as emulsifiers.
- Suitable nonionic emulsifiers are, for example, oxalkyl ethers, preferably Oxethylates and / or terminally blocked oxethylates of fatty alcohols and Fatty acids or oils.
- anionic emulsifiers are alkyl and / or Aryl sulfonates, ⁇ -olefin sulfonates, ⁇ -sulfofatty acid esters, sulfosuccinic acid esters and Alkyl sulfates and ether sulfates as well as carboxymethylated oxethylates and soaps suitable.
- the preparation of the preferably stable emulsions is known. For example, the hydrophobic phase in the aqueous emulsifier-containing phase registered and dispersed with stirring and pumping.
- the plant for producing wood fiber materials preferably has at least a refiner on how he z. B. from WO-A-96/41914 or from WO-A-96/35016 is. These patent applications are hereby introduced for reference.
- the diacid carboxylic ester is preferably used together with the clear filtrate dosed into the refiner.
- the metering is preferably carried out continuously.
- the dicarboxylic acid ester concentration is in the first refiner 100-5000 ppm, particularly preferably 200-2000 ppm and whole particularly preferably 300-1000 ppm.
- the use according to the invention is suitable for machines and systems for Wood fiberization of any kind.
- the machines and / or systems are preferred however part of the TMP process or a process as described in WO-A-96/41914 is described.
- the runtimes of machines and systems succeed extend considerably to the production of wood fiber materials.
- the plants are easier to regulate and the service life of the refiner's grinding set can be extended become.
- the method according to the invention can be integrated into existing systems become. Deposits already present are removed by the inventive Use reduced.
- FIG. 1 shows a process flow diagram for the production of thermo-mechanical pulp (TMP).
- TMP thermo-mechanical pulp
- Cleaned wood chips are conveyed to the 1st refiner stage and mechanically broken down there in the presence of clear filtrate and 330 ppm TALLOFIN® TMP.
- TALLOFIN® TMP is a product of Stockhausen GmbH & Co. KG, which contains 40% by weight di-n-butyl adipate and 60% by weight of a nonionic emulsifier.
- the TALLOFIN® TMP is dosed into the clear filtrate before it flows into the refiner.
- the very high energy input creates temperatures of up to 200 ° C and pressures of 2-3 bar in the refiner (up to 22 MW), so that a considerable part of the water evaporates in the refiner.
- the steam is removed from the refiner through steam lines and fed to heat recovery.
- the steam also contains a certain proportion of di-n-butyl adipate, so that the steam lines, the cyclones and the regulating elements in the steam lines have no or only slight deposits. But even in the refiner itself, no or to a much reduced extent deposits of wood constituents form, so that it has to be cleaned less frequently and the service life of the grinding set is increased.
- the wood fibers are mechanically comminuted again in the second refiner stage before they are then subjected to the further treatment known to the person skilled in the art.
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- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Mechanical Engineering (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
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Abstract
Description
Die vorliegende Erfindung betrifft die Vermeidung und/oder Verminderung
von Ablagerungen von flüchtigen und nicht flüchtigen Holzinhaltsstoffen in gasführenden
Systemen, wobei die flüchtigen Holzinhaltsstoffe zumindest teilweise in
den gasführenden Systemen kondensieren.
Die vorliegende Erfindung betrifft ferner die Verminderung und/oder
Vermeidung von Ablagerungen von Holzinhaltsstoffen an Maschinen und/oder Anlagenteilen
zur Herstellung von Holzfasern aus Holzschnitzeln.The present invention relates to the avoidance and / or reduction of deposits of volatile and non-volatile wood constituents in gas-carrying systems, the volatile wood constituents at least partially condensing in the gas-carrying systems.
The present invention further relates to the reduction and / or avoidance of deposits of wood constituents on machines and / or system parts for the production of wood fibers from wood chips.
Bei der Bearbeitung von Holz, der Produktion und Verarbeitung von Zellstoff und/oder der Papier-, Karton- oder Formfaserherstellung werden oftmals flüchtige Holzinhaltsstoffe frei, die dann in gasführenden System kondensieren und dort feste Ablagerungen bilden. Durch diese Ablagerungen erhöht sich z. B. der Druckverlust der Rohrleitungen, reduziert sich die Trennleistung von gegebenenfalls vorhandenen Zyklonen und werden Regeleinrichtungen blockiert, so daß die Gasleitungen geöffnet und beispielsweise mit Hochdruckaggregaten gereinigt werden müssen. Diese Reinigung ist sehr kostenintensiv und stört den jeweiligen Herstellungsvorgang. When processing wood, producing and processing pulp and / or the manufacture of paper, cardboard or molded fiber often become volatile Free wood constituents, which then condense in gas-carrying systems and solid there Form deposits. These deposits increase z. B. the pressure loss of the pipelines, the separation performance of any existing ones is reduced Cyclones and control devices are blocked so that the gas lines are opened and have to be cleaned with high-pressure units, for example. This cleaning is very expensive and disrupts the respective manufacturing process.
Die EP-A-0 334 098 beschreibt ein Verfahren zur Verminderung von Ablagerungen in Anlagen zur Eindampfung von Sulfitablaugen der Holz-Zellstoffgewinnung, indem der Sulfitablauge niedermolekulare Polyacrylsäure zugegeben wird. Die Ablagerungen sind Gips oder Silikatablagerungen, die während des Prozesses ausfällen.EP-A-0 334 098 describes a method for reducing deposits in Equipment for the evaporation of waste liquors from wood pulp production by Sulfite waste liquor low molecular weight polyacrylic acid is added. The deposits are gypsum or silicate deposits that fail during the process.
Die US-A-5 762 757 beschreibt eine Methode zum Verhindern von Ablagerungen organischer Inhaltsstoffe von Zellstoff wie beispielsweise Pech und klebrige Verunreinigungen in zellstoff- oder papierherstellenden Systemen, indem ein anionischer Tensid der Gruppe der Dinonyl Sulfosuccinate oder ein Gemisch aus Dioctyl Sulfosuccinat und Didecyl Sulfosuccinat entweder dem Zellstoff zugeführt oder auf die Oberfläche des Systems aufgebracht wird.US-A-5 762 757 describes a method of preventing deposits organic pulp ingredients such as pitch and sticky Contamination in pulp or paper making systems by a anionic surfactant from the group of Dinonyl sulfosuccinates or a mixture of Dioctyl sulfosuccinate and didecyl sulfosuccinate are either added to the pulp or is applied to the surface of the system.
Die DE-A-27 35 300 A beschreibt ein Verfahren zur Brüdenkondensatnachbehandlung und zwar zum destillativen Entfernen und Verbrennen von wasserdampfflüchtigen, sauerstoffverzehrenden Substanzen, aus Flüssigkeiten sowie der Nassverbrennung nicht wasserdampfflüchtiger Anteile. Ein Teil der im Holz vorhandenen Substanzen sind wasserdampfflüchtig und im Brüdenkondensat vorhanden. In dem Verfahren werden die Substanzen bei über 1000°C verbrannt.DE-A-27 35 300 A describes a method for the aftertreatment of vapor condensate for the distillative removal and burning of steam-volatile oxygen-consuming substances, from liquids and wet combustion non-volatile components. Part of the substances present in the wood are volatile in water and are present in the vapor condensate. In the process the substances are burned at over 1000 ° C.
Die WO-A-98/33970 beschreibt ein Verfahren zur Herstellung von Faserstoffen für die Erzeugung von Zellstoff, Papier oder Holzwerkstoffplatten, bei dem bei der Vorbehandlung zum Imprägnieren Dicarbonsäuredialkylester und/oder ein oder mehrere Fettsäurepolyol- mono, -di, tri- und/oder höhere Polyester und/oder Polyester- Polyether- Copolymere zugesetzt werden. Diese Bestandteile reinigen die Primärfasern von Harzanteilen und anderen Holzinhaltsstoffen und bewirken eine höhere Ausbeute und eine bessere Optik. WO-A-98/33970 describes a process for the production of fibrous materials for the Production of pulp, paper or wood-based panels, in which the Pretreatment for impregnating dicarboxylic acid dialkyl esters and / or one or several fatty acid polyol mono, di, tri and / or higher polyesters and / or Polyester-polyether copolymers are added. These components clean the Primary fibers from resin components and other wood constituents and cause one higher yield and better optics.
Der vorliegenden Erfindung liegt deshalb die Aufgabe zugrunde, ein Verfahren zur Verfügung zu stellen, mit dem die Ablagerung von flüchtigen und/oder nicht flüchtigen Holzinhaltsstoffen in gasführenden Systemen zumindest vermindert wird.The present invention is therefore based on the object of a method for To provide with the deposition of volatile and / or non-volatile Wood ingredients in gas-carrying systems is at least reduced.
Die Aufgabe wird erfindungsgemäß mit einer Verwendung einer Verbindung zur Vermeidung und/oder Verminderung von Ablagerungen von flüchtigen und nicht flüchtigen Holzinhaltsstoffen in gasführenden Systemen gemäß Anspruch 1 gelöst, wobei zumindest einige der flüchtigen Holzinhaltsstoffen zumindest teilweise in den gasführenden Systemen kondensieren und das Gas mindestens die Verbindung enthält, die
- ein ähnliches Kondensationsverhalten aufweist wie die flüchtigen Holzinhaltsstoffe,
- Ablagerungen von flüchtigen Holzinhaltsstoffen und/oder deren Reaktionsprodukten zumindest vermindert.
- has a condensation behavior similar to that of the volatile wood constituents,
- Deposits of volatile wood constituents and / or their reaction products are at least reduced.
Flüchtige Holzinhaltsstoffe im Sinne der Erfindung sind alle Holzinhaltsstoffe, die bei Temperaturen oberhalb von 20°C einen Dampfdruck aufweisen. Reaktionsprodukte im Sinne der Erfindung sind jegliche Produkte, die die flüchtigen Holzinhaltsstoffe nach der Kondensation, z. B. durch Polymerisation, bilden.Volatile wood constituents in the sense of the invention are all wood constituents that Temperatures above 20 ° C have a vapor pressure. reaction products Within the meaning of the invention are any products that contain the volatile wood constituents after the condensation, e.g. B. by polymerization.
Da die kondensierten flüchtigen Holzinhaltsstoffe und deren Reaktionsprodukte auf den Oberflächen der gasführenden Systeme oftmals einen klebrigen Film ausbilden, weisen die Ablagerungen meist noch nicht flüchtige Holzinhaltsstoffe, z. B. feine Holzpartikel, auf, die sich aus dem Gasstrom abscheiden und an den klebrigen Filmen anhaften.Because the condensed volatile wood components and their reaction products often form a sticky film on the surfaces of the gas-carrying systems, the deposits usually have non-volatile wood constituents, e.g. B. fine Wood particles, which separate from the gas stream and sticky films adhere.
Erfindungsgemäß weist die Verbindung ein ähnliches Kondensationsverhalten auf wie die Holzinhaltsstoffe; d. h. die Verbindung und die Holzinhaltsstoffe kondensieren vorzugsweise an derselben Stelle in dem gasführenden System und bilden dort vorzugsweise einen Film.According to the invention, the connection has a similar condensation behavior like the wood ingredients; d. H. the connection and the wood constituents condense preferably at the same point in the gas-carrying system and preferably form there a movie.
Vorzugsweise ist die Verbindung ein Dicarbonsäureester. Besonders bevorzugt ist der Dicarbonsäureester ein Dicarbonsäuredialkyl- und/oder diisoalkylester von C2-C12 Dicarbonsäuren mit C1-C13 n- und/oder iso-Alkanolen wie Di-n-butyloxalat, Di-n-butylmalonat, Di-n-butylsuccinat, Di-n-butylglutarat, Di-n-butyladipat, Di-n-butylsuberat, Di-n-butyisebacat, Dimethyladipat, Di-n-propyladipat, Diisopropyladipat, Diisobutyladipat, Di-tert-butyladipat, Di-isoamyladipat, Di-n-hexyladipat, Di-(2-ethylbutyl)adipat, Di-(2-ethylhexyl)adipat, Diisodecyladipat sowie Dimethylphthalat, Diethylphthalat, Di-n-butylphthalat, Diisobutylphthalat, Di-(2-ethylhexyl)phthalat und Diisodecylphthalat sowie die entsprechenden Terephthalsäureester und die Diester der C9-Dicarbonsäure (Trimethyladipinsäure) und der Dodecandicarbonsäure.The compound is preferably a dicarboxylic acid ester. Is particularly preferred the dicarboxylic acid ester is a dicarboxylic acid dialkyl and / or diisoalkyl ester of C2-C12 Dicarboxylic acids with C1-C13 n- and / or iso-alkanols such as di-n-butyl oxalate, di-n-butyl malonate, Di-n-butyl succinate, di-n-butyl glutarate, di-n-butyl adipate, di-n-butyl suberate, Di-n-butyisebacate, dimethyl adipate, di-n-propyl adipate, diisopropyl adipate, Diisobutyl adipate, di-tert-butyl adipate, di-isoamyl adipate, di-n-hexyl adipate, di- (2-ethylbutyl) adipate, Di- (2-ethylhexyl) adipate, diisodecyl adipate and dimethyl phthalate, Diethyl phthalate, di-n-butyl phthalate, diisobutyl phthalate, di (2-ethylhexyl) phthalate and Diisodecyl phthalate and the corresponding terephthalic acid esters and diesters C9 dicarboxylic acid (trimethyladipic acid) and dodecanedicarboxylic acid.
Ganz besonders bevorzugt ist jedoch die Verbindung ein Di-n-Alkyladipinsäureester und/oder ein Di-iso-Alkyladipinsäureester. Am meisten bevorzugt ist die Verbindung n-Dibutyladipat.However, the compound is very particularly preferably a di-n-alkyladipic acid ester and / or a di-iso-alkyl adipic acid ester. The most preferred is the compound n-dibutyl adipate.
Die erfindungsgemäße Verwendung eignet sich zur Vermeidung und Verminderung von Ablagerungen von flüchtigen oder nicht flüchtigen Holzinhaltsstoffen in gasführenden Systemen beliebiger Art. Vorzugsweise sind die gasführenden Systeme jedoch Teil einer:
- Holzverarbeitungsanlage, insbesondere einer Anlage zur Herstellung von Holzfaserstoff und/oder Holzfaserplatten,
- Anlage zu Herstellung von Zellstoff,
- Zellstoffverarbeitungsanlage,
- Papier- oder Kartonherstellungsanlage und/oder
- Anlage zur Herstellung von Teilen oder Gegenständen aus Formfasem.
- Wood processing plant, in particular a plant for the production of wood pulp and / or wood fiber boards,
- Plant for the production of pulp,
- Pulp processing plant,
- Paper or cardboard manufacturing plant and / or
- Plant for the production of parts or objects from shaped fibers.
Ganz besonders bevorzugt ist das gasführende System Teil einer Anlage zur Herstellung von Thermo-Mechanical-Pulp (TMP) oder einer Hackschnitzel-Refineranlage, wie sie in der WO-A-96/41914 beschrieben ist, die hiermit als Referenz eingeführt wird.The gas-carrying system is very particularly preferably part of a plant for the production from Thermo-Mechanical-Pulp (TMP) or a wood chip refiner system, as described in WO-A-96/41914, which is hereby introduced as a reference becomes.
Das Gas, das durch die gasführenden Leitungen strömt, kann jedes beliebige Gas sein, das jedoch vorzugsweise Wasserdampf aufweist.The gas that flows through the gas-carrying lines can be any gas be, but preferably has water vapor.
Vorzugsweise wird die Verbindung gasförmig in das Gas dosiert. Der Fachmann erkennt, daß die Verbindung jedoch auch im flüssigen Zustand in das Gas dosiert werden kann und dann dort in einen gasförmigen Zustand überführt wird. Die Dosierung erfolgt vorzugsweise kontinuierlich.The compound is preferably metered into the gas in gaseous form. The specialist realizes that the compound can also be metered into the gas in the liquid state can and then there is converted into a gaseous state. The dosage is preferably carried out continuously.
Die Dosiermenge der Verbindung hängt von der Konzentration der flüchtigen Holzinhaltsstoffe in dem Gas und dem Gasvolumenstrom ab. Vorzugsweise beträgt die Konzentration 100-5000 ppm, besonders bevorzugt 200-2000 ppm und ganz besonders bevorzugt 300-1000 ppm.The dosage of the compound depends on the concentration of the volatile wood constituents in the gas and the gas volume flow. The is preferably Concentration 100-5000 ppm, particularly preferably 200-2000 ppm and very particularly preferably 300-1000 ppm.
Vorzugsweise wird die Verbindung in einer solchen Menge in das Gas dosiert, daß sich keine Ablagerungen an flüchtigen oder nicht flüchtigen Verbindungen und/oder deren Reaktionsprodukten auf den Oberflächen der gasführenden Systeme bilden bzw. daß sich bereits gebildete Ablagerungen wieder ab- und/oder auflösen. Dementsprechend wird die Dosierung der Verbindung vorzugsweise automatisch geregelt. Als Regelparameter wird vorzugsweise der Druckverlust in den Rohrleitungen des gasführenden Systems und/oder der Abscheidegrad von Zyklonen, die sich in dem gasführenden System befinden, genommen. Ebenfalls bevorzugt werden als Regelparameter auch der Gasvolumenstrom und die Konzentration an flüchtigen Holzinhaltsstoffen im Gas oder die Flächenbelegung eingesetzt.The compound is preferably metered into the gas in such an amount that there are no deposits of volatile or non-volatile compounds and / or form their reaction products on the surfaces of the gas-carrying systems or that deposits already formed detach and / or dissolve again. Accordingly the dosage of the compound is preferably regulated automatically. The pressure loss in the pipelines is preferably used as the control parameter the gas-carrying system and / or the degree of separation of cyclones, which are in the gas-carrying system. Are also preferred as Control parameters also the gas volume flow and the concentration of volatile Wood ingredients used in the gas or the area coverage.
Da die oben genannten Herstellungsverfahren in der Regel in der Gegenwart von Wasser durchgeführt werden und das Wasser zumindest teilweise verdampft, wird die Verbindung in einer anderen bevorzugten Ausführungsform des erfindungsgemäßen Verfahrens direkt in das Wasser dosiert. In diesem Fall muß die Verbindung ebenfalls wasserdampfflüchtig sein.Because the above manufacturing process is usually in the presence of Water are carried out and the water is at least partially evaporated the compound in another preferred embodiment of the invention Process dosed directly into the water. In this case, the connection also be steam-volatile.
Die vorliegende Erfindung hat den Vorteil, daß die gasführenden Systeme seltener gereinigt werden müssen und die Anlagen deshalb eine längere Laufzeit haben. Da z. B. Zyklone nicht mehr von Ablagerungen zugesetzt werden, bleibt deren Trennfähigkeit erhalten. Bereits bestehende Ablagerungen werden vermindert.The present invention has the advantage that the gas-carrying systems are less common must be cleaned and the systems therefore have a longer operating time. There z. B. Cyclones are no longer added by deposits, their separability remains receive. Existing deposits are reduced.
Eine weitere Aufgabe der vorliegenden Erfindung ist die Bereitstellung eines Verfahrens zur Verminderung und/oder Vermeidung von Ablagerungen von Holzinhaltsstoffen an Maschinen und/oder Anlagenteilen zur Herstellung von Holzfasern aus Holzschnitzeln (Hackschnitzeln).Another object of the present invention is to provide a method to reduce and / or avoid deposits of wood constituents on machines and / or system parts for the production of wood fibers Wood chips (wood chips).
Diese Aufgabe wird erfindungsgemäß mit einer Verwendung einer Verbindung zur Verminderung und/oder Vermeidung von Ablagerungen von Holzinhaltsstoffen an Maschinen und/oder Anlagenteilen zur Herstellung von Holzfaserstoffen aus Holzschnitzeln gelöst, bei dem die Zerfaserung des Holzes in Gegenwart mindestens einer Verbindung erfolgt, die:
- auf den Oberflächen der Maschinen und/oder Anlagenteile einen Film bildet und
- Ablagerungen von flüchtigen Holzinhaltsstoffen und/oder deren Reaktionsprodukten zumindest vermindert.
- forms a film on the surfaces of the machines and / or system parts and
- Deposits of volatile wood constituents and / or their reaction products are at least reduced.
Ablagerungen im Sinne der Erfindung sind jegliche Ablagerungen von Holzinhaltsstoffen in gasführenden Systemen und/oder an sonstigen Anlagen- oder Maschinenteilen, die zur Herstellung von Holzfaserstoffen eingesetzt werden. Deposits in the sense of the invention are any deposits of wood constituents in gas-carrying systems and / or on other systems or Machine parts that are used for the production of wood fiber materials.
Vorzugsweise ist die Verbindung ein Dicarbonsäureester. Besonders bevorzugt ist der Dicarbonsäureester ein Dicarbonsäuredialkyl- und/oder diisoalkylester von C2-C12 Dicarbonsäuren mit C1-C13 n- und/oder iso-Alkanolen wie Di-n-butyloxalat, Di-n-butylmalonat, Di-n-butylsuccinat, Di-n-butylglutarat, Di-n-butyladipat, Di-n-butylsuberat, Di-n-butylsebacat, Dimethyladipat, Di-n-propyladipat, Diisopropyladipat, Diisobutyladipat, Di-tert-butyladipat, Di-isoamyladipat, Di-n-hexyladipat, Di-(2-ethylbutyl)adipat, Di-(2-ethylhexyl)adipat, Diisodecyladipat sowie Dimethylphthalat, Diethylphthalat, Di-n-butylphthalat, Diisobutylphthalat, Di-(2-ethylhexyl)phthalat und Diisodecylphthalat sowie die entsprechenden Terephthalsäureester und die Diester der C9-Dicarbonsäure (Trimethyladipinsäure) und der Dodecandicarbonsäure.The compound is preferably a dicarboxylic acid ester. Is particularly preferred the dicarboxylic acid ester is a dicarboxylic acid dialkyl and / or diisoalkyl ester of C2-C12 Dicarboxylic acids with C1-C13 n- and / or iso-alkanols such as di-n-butyl oxalate, di-n-butyl malonate, Di-n-butyl succinate, di-n-butyl glutarate, di-n-butyl adipate, di-n-butyl suberate, Di-n-butyl sebacate, dimethyl adipate, di-n-propyl adipate, diisopropyl adipate, Diisobutyl adipate, di-tert-butyl adipate, di-isoamyl adipate, di-n-hexyl adipate, di- (2-ethylbutyl) adipate, Di- (2-ethylhexyl) adipate, diisodecyl adipate and dimethyl phthalate, Diethyl phthalate, di-n-butyl phthalate, diisobutyl phthalate, di (2-ethylhexyl) phthalate and Diisodecyl phthalate and the corresponding terephthalic acid esters and diesters C9 dicarboxylic acid (trimethyladipic acid) and dodecanedicarboxylic acid.
Ganz besonders bevorzugt ist die Verbindung jedoch ein Di-n-Alkyladipinsäureester und/oder ein Di-iso-Alkyladipinsäureester. Am meisten bevorzugt ist die Verbindung Di-n-Butyladipat.However, the compound is very particularly preferably a di-n-alkyladipic acid ester and / or a di-iso-alkyl adipic acid ester. The most preferred is the compound Di-n-butyl adipate.
Die Ester können allein oder in Kombination mit wasserlöslichen oder wasserunlöslichen Lösungsmitteln als wasserfreie oder wasserhaltige Lösung oder als wasserhaltige Dispersion, vorzugsweise Emulsion, zum Einsatz gelangen. Geeignete Lösungsmittel sind n- und iso-Alkanole, flüssige Kohlenwasserstoffe, Aceton und andere bekannte Lösungsmittel, insbesondere werden natürliche Öle oder modifizierte natürliche Öle, wie Rübölmethylester eingesetzt.The esters can be used alone or in combination with water-soluble or water-insoluble ones Solvents as water-free or water-containing solution or as water-containing Dispersion, preferably emulsion, are used. Suitable solvents are n- and iso-alkanols, liquid hydrocarbons, acetone and others known solvents, in particular natural oils or modified natural oils, such as beet oil methyl ester.
Bei der Herstellung der Dispersionen werden nichtionogene, ionische und amphotere, insbesondere nichtionische Tenside als Emulgatoren verwendet.Nonionic, ionic and Amphoteric, especially nonionic, surfactants are used as emulsifiers.
Geeignete nichtionische Emulgatoren sind beispielsweise Oxalkylether, vorzugsweise Oxethylate und/oder endständig blockierte Oxethylate von Fettalkoholen und Fettsäuren bzw. Ölen. Als anionische Emulgatoren sind Alkyl- und/oder Arylsulfonate, α-Olefinsulfonate, α-Sulfofettsäureester, Sulfobernsteinsäureester sowie Alkylsulfate und Ethersulfate sowie carboxymethylierte Oxethylate und Seifen geeignet. Die Herstellung der vorzugsweise stabilen Emulsionen ist bekannt. Beispielsweise wird die hydrophobe Phase in die wäßrige emulgatorhaltige Phase eingetragen und unter Rühren und Umpumpen dispergiert. Suitable nonionic emulsifiers are, for example, oxalkyl ethers, preferably Oxethylates and / or terminally blocked oxethylates of fatty alcohols and Fatty acids or oils. As anionic emulsifiers are alkyl and / or Aryl sulfonates, α-olefin sulfonates, α-sulfofatty acid esters, sulfosuccinic acid esters and Alkyl sulfates and ether sulfates as well as carboxymethylated oxethylates and soaps suitable. The preparation of the preferably stable emulsions is known. For example, the hydrophobic phase in the aqueous emulsifier-containing phase registered and dispersed with stirring and pumping.
Vorzugsweise weist die Anlage zur Herstellung von Holzfaserstoffen mindestens einen Refiner auf, wie er z. B. aus der WO-A-96/41914 oder aus der WO-A-96/35016 bekannt ist. Diese Patentanmeldungen werden hiermit als Referenz eingeführt.The plant for producing wood fiber materials preferably has at least a refiner on how he z. B. from WO-A-96/41914 or from WO-A-96/35016 is. These patent applications are hereby introduced for reference.
Vorzugsweise wird der Disäurecarbonester vorzugsweise zusammen mit dem Klarfiltrat in den Refiner dosiert. Die Dosierung erfolgt vorzugsweise kontinuierlich.The diacid carboxylic ester is preferably used together with the clear filtrate dosed into the refiner. The metering is preferably carried out continuously.
In einer bevorzugten Ausführungsform beträgt die Dicarbonsäureester-Konzentration in dem ersten Refiner 100-5000 ppm, besonders bevorzugt 200-2000 ppm und ganz besonders bevorzugt 300-1000 ppm.In a preferred embodiment, the dicarboxylic acid ester concentration is in the first refiner 100-5000 ppm, particularly preferably 200-2000 ppm and whole particularly preferably 300-1000 ppm.
Die erfindungsgemäße Verwendung eignet sich für Maschinen und Anlagen zur Holzzerfaserung jeglicher Art. Vorzugsweise sind die Maschinen und/oder Anlagen jedoch Teil des TMP-Verfahrens oder eines Verfahrens, wie es in der WO-A-96/41914 beschrieben ist.The use according to the invention is suitable for machines and systems for Wood fiberization of any kind. The machines and / or systems are preferred however part of the TMP process or a process as described in WO-A-96/41914 is described.
Mit der vorliegenden Erfindung gelingt es, die Laufzeiten von Maschinen und Anlagen zur Herstellung von Holzfaserstoffen erheblich zu verlängern. Die Anlagen sind besser regelbar, und die Standzeit der Mahlgarnitur des Refiners kann verlängert werden. Das erfindungsgemäße Verfahren kann in bereits bestehende Anlagen integriert werden. Bereits vorhandene Ablagerungen werden durch die erfindungsgemäße Verwendung vermindert.With the present invention, the runtimes of machines and systems succeed extend considerably to the production of wood fiber materials. The plants are easier to regulate and the service life of the refiner's grinding set can be extended become. The method according to the invention can be integrated into existing systems become. Deposits already present are removed by the inventive Use reduced.
Im folgenden wird die Erfindung anhand der Figur 1 erläutert. Die Erläuterungen sind lediglich beispielhaft und schränken den allgemeinen Erfindungsgedanken nicht ein.The invention is explained below with reference to FIG. 1 . The explanations are only examples and do not restrict the general idea of the invention.
Figur 1 zeigt ein Verfahrensfließbild zur Herstellung von Thermo-Mechanical-Pulp
(TMP). Gereinigte Hackschnitzel werden in die 1. Refinerstufe gefördert und dort in
der Gegenwart von Klarfiltrat und 330 ppm TALLOFIN® TMP mechanisch zerlegt.
TALLOFIN® TMP ist ein Produkt der Stockhausen GmbH & Co. KG, das 40 Gew.-%
Di-n-butyladipat und 60 Gew.-% eines nichtionogenen Emulgators enthält. Das
TALLOFIN® TMP wird in das Klarfiltrat dosiert bevor dieses in den Refiner strömt.
Durch den sehr hohen Energieeintrag entstehen im Refiner (bis zu 22 MW) Temperaturen
von oberhalb 200°C und Drucke von 2-3 bar, so daß ein erheblicher Teil des
Wassers im Refiner verdampft. Der Dampf wird durch Dampfleitungen aus dem Refiner
ab- und einer Wärmerückgewinnung zugeführt. Der Dampf enthält neben flüchtigen
und nicht flüchtigen Holzinhaltsstoffen auch einen gewissen Anteil an Di-n-butyladipat,
so daß die Dampfleitungen, die Zyklone und die Regelorgane in den
Dampfleitungen keine oder nur geringe Beläge aufweisen. Aber auch im Refiner
selbst bilden sich keine bzw. in stark reduziertem Maß Ablagerungen von Holzinhaltsstoffen,
so daß dieser seltener gereinigt werden muß und die Standzeit der
Mahlgamitur erhöht wird.
Nach der Zerfaserung im ersten Refiner werden die Holzfasern in der 2. Refinerstufe
noch einmal mechanisch zerkleinert, bevor sie dann der dem Fachmann bekannten
weiteren Behandlung unterzogen werden. Auch in der 2. Refinerstufe entstehen
große Mengen Dampf, die der Wärmerückgewinnung zugeführt werden. Der Dampf
enthält wiederum neben flüchtigen und nicht flüchtigen Holzinhaltsstoffen auch einen
gewissen Anteil an Di-n-butyladipat, so daß die Dampfleitungen, die Zyklone und die
Regelorgane in den Dampfleitungen keine oder nur geringe Beläge aufweisen. Aber
auch in diesem Refiner selbst bilden sich keine bzw. in stark reduziertem Maß Ablagerungen
von Holzinhaltsstoffen, so daß dieser seltener gereinigt werden muß und
die Standzeit der Mahlgamitur erhöht wird. FIG. 1 shows a process flow diagram for the production of thermo-mechanical pulp (TMP). Cleaned wood chips are conveyed to the 1st refiner stage and mechanically broken down there in the presence of clear filtrate and 330 ppm TALLOFIN® TMP. TALLOFIN® TMP is a product of Stockhausen GmbH & Co. KG, which contains 40% by weight di-n-butyl adipate and 60% by weight of a nonionic emulsifier. The TALLOFIN® TMP is dosed into the clear filtrate before it flows into the refiner. The very high energy input creates temperatures of up to 200 ° C and pressures of 2-3 bar in the refiner (up to 22 MW), so that a considerable part of the water evaporates in the refiner. The steam is removed from the refiner through steam lines and fed to heat recovery. In addition to volatile and non-volatile wood constituents, the steam also contains a certain proportion of di-n-butyl adipate, so that the steam lines, the cyclones and the regulating elements in the steam lines have no or only slight deposits. But even in the refiner itself, no or to a much reduced extent deposits of wood constituents form, so that it has to be cleaned less frequently and the service life of the grinding set is increased.
After defibration in the first refiner, the wood fibers are mechanically comminuted again in the second refiner stage before they are then subjected to the further treatment known to the person skilled in the art. Large quantities of steam are also generated in the second refiner stage, which are then used for heat recovery. In addition to volatile and non-volatile wood constituents, the steam also contains a certain proportion of di-n-butyl adipate, so that the steam lines, the cyclones and the regulating elements in the steam lines have no or only slight deposits. But even in this refiner itself no or to a greatly reduced extent deposits of wood constituents form, so that this has to be cleaned less frequently and the service life of the grinding set is increased.
Claims (14)
- Use of a compound for preventing and/or reducing deposits of volatile and non-volatile wood constituents in gas-conveying systems in the processing of wood, the production and processing of pulp and/or the manufacture of paper, cardboard or moulded fibres, where volatile wood constituents at least partially condense in the gas-conveying systems, characterised in that the compound:has similar condensation characteristics to the volatile wood constituents,at least reduces deposits of volatile wood constituents and/or the reaction products thereof andthe compounds are metered into the gas or into an aqueous phase which is formed during the processing of wood, the production and processing of pulp and/or the manufacture of paper, cardboard or moulded fibre.
- Use according to claim 1, characterised in that the compound is a dicarboxylic acid ester.
- Use according to claim 2, characterised in that the dicarboxylic acid ester is a di-n-alkyladipic acid ester and/or a diisoalkyladipic acid ester.
- Use according to claim 2, characterised in that the dicarboxylic acid ester is dibutyl adipate.
- Use according to one of claims 1 to 4, characterised in that the gas-conveying system is part of a:wood processing plant, particularly a plant for producing wood fibre and/or wood fibre board,plant for producing pulp,pulp processing plant,paper or cardboard manufacturing plant and/orplant for producing parts and/or objects made of moulded fibres.
- Use according to one of claims 1 to 5, characterised in that the gas comprises water vapour.
- Use of a compound for reducing and/or preventing deposits of wood constituents on machines and/or parts of equipment for the manufacture of wood fibre from wood chips, characterised in that the shredding of the wood into fibres takes place in the presence of at least the compound whichforms a film on the surfaces of the machines and/or equipment parts andat least reduces deposits of volatile wood constituents and/or the reaction products thereof.
- Use according to claim 7, characterised in that the compound is a dicarboxylic acid ester.
- Use according to claim 8, characterised in that the dicarboxylic acid ester is a di-n-alkyl adipic acid ester and/or a diisoalkyl adipic acid ester.
- Use according to claim 8, characterised in that the dicarboxylic acid ester is dibutyl adipate.
- Use according to one of claims 7 to 10, characterised in that the machine and/or equipment parts for producing wood fibres from wood chips comprise at least one refiner.
- Use according to claim 11, characterised in that the dicarboxylic acid ester is measured into the first refiner preferably together with the clear filtrate.
- Use according to claim 11 or 12, characterised in that the concentration of the dicarboxylic acid ester is 100-5000, preferably 200-2000 ppm, most preferably 300-1000 ppm.
- Use according to one of claims 7 to 13, characterised in that the machines and/or equipment parts are components of a plant for producing thermomechanical pulp.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19959826A DE19959826A1 (en) | 1999-12-10 | 1999-12-10 | Process for reducing and / or avoiding deposits of wood constituents |
DE19959826 | 1999-12-10 | ||
PCT/EP2000/011926 WO2001042555A2 (en) | 1999-12-10 | 2000-11-29 | Method for reducing and/or avoiding the build up of wood components |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1252388A2 EP1252388A2 (en) | 2002-10-30 |
EP1252388B1 true EP1252388B1 (en) | 2004-06-02 |
Family
ID=7932319
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00993298A Expired - Lifetime EP1252388B1 (en) | 1999-12-10 | 2000-11-29 | Use of a compound for reducing and/or avoiding the build up of wood components |
Country Status (11)
Country | Link |
---|---|
US (1) | US20040011482A1 (en) |
EP (1) | EP1252388B1 (en) |
CN (1) | CN1409783A (en) |
AT (1) | ATE268406T1 (en) |
AU (1) | AU2837601A (en) |
CA (1) | CA2394173A1 (en) |
DE (2) | DE19959826A1 (en) |
NO (1) | NO322867B1 (en) |
RU (1) | RU2002117417A (en) |
TW (1) | TW541382B (en) |
WO (1) | WO2001042555A2 (en) |
Citations (2)
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DE2735300A1 (en) * | 1977-08-05 | 1979-02-08 | Konrad Mattern | Spray treatment plant for removing and utilising spray condensates - preventing pollution of natural water by waste e.g. from cellulose plant |
WO1998033970A1 (en) * | 1997-02-04 | 1998-08-06 | Stockhausen Gmbh & Co. Kg | Process for producing fibrous materials with improved properties |
Family Cites Families (16)
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DE3809663A1 (en) * | 1988-03-23 | 1989-10-12 | Metallgesellschaft Ag | METHOD FOR REDUCING DEPOSITS IN EQUIPMENT FOR EVAPORATING SULFIT BLUE |
US5080759A (en) * | 1990-09-04 | 1992-01-14 | Quaker Chemical Corporation | Method for controlling stickies in pulp and papermaking processes using recycled paper |
CA2059256A1 (en) * | 1992-01-13 | 1993-07-14 | David Arthur Aston | Pitch control |
US5256252A (en) * | 1992-07-15 | 1993-10-26 | Nalco Chemical Company | Method for controlling pitch deposits using lipase and cationic polymer |
DE4311598A1 (en) * | 1993-04-08 | 1994-10-13 | Henkel Kgaa | Process for controlling the settling of sticky contaminants from pulp suspensions |
US5779858A (en) * | 1995-04-12 | 1998-07-14 | Betzdearborn Inc. | Deposition control in pulp and papermaking systems using a composition comprising of polyvinyl alcohol and gelatin |
US5723021A (en) * | 1995-04-12 | 1998-03-03 | Betzdearborn Inc. | Method for inhibiting deposition in pulp and papermaking systems using a composition comprising of polyvinyl alcohol, gelatin and cationic polymer |
DE19519268C1 (en) * | 1995-05-31 | 1997-01-23 | Stockhausen Chem Fab Gmbh | Use of pulp and paper making agents |
BR9606439A (en) * | 1995-06-12 | 1998-07-14 | Sprout Bauer Inc Andritz | Process of producing pulp from ligno-cellulosic material containing fibers in a refining system equipped with a primary refiner |
NZ331188A (en) * | 1996-02-02 | 1998-11-25 | Hercules Inc | Emulsifier system for rosin sizing agents |
DE19616733C2 (en) * | 1996-04-26 | 2000-07-13 | Stockhausen Chem Fab Gmbh | Process for the thermal-mechanical surface treatment of sheet-like material webs, in particular made of paper and cardboard, using adhesive agents |
US5746888A (en) * | 1996-07-09 | 1998-05-05 | Betzdearborn Inc. | Methods for inhibiting organic contaminant deposition in pulp and papermaking systems |
US5762757A (en) * | 1996-12-05 | 1998-06-09 | Betzdearborn Inc. | Methods for inhibiting organic contaminant deposition in pulp and papermaking systems |
US6113738A (en) * | 1998-03-16 | 2000-09-05 | Nalco Chemical Company | Use of additives to breakdown and stabilize wax during fiber recycle |
US6256387B1 (en) * | 1999-07-06 | 2001-07-03 | Chin-Yang Wang | Device rack |
US6558513B1 (en) * | 2001-05-29 | 2003-05-06 | Hercules Incorporated | Non-aqueous release from paper machine equipment |
-
1999
- 1999-12-10 DE DE19959826A patent/DE19959826A1/en not_active Ceased
-
2000
- 2000-11-29 US US10/148,210 patent/US20040011482A1/en not_active Abandoned
- 2000-11-29 EP EP00993298A patent/EP1252388B1/en not_active Expired - Lifetime
- 2000-11-29 WO PCT/EP2000/011926 patent/WO2001042555A2/en active IP Right Grant
- 2000-11-29 DE DE50006708T patent/DE50006708D1/en not_active Expired - Lifetime
- 2000-11-29 AU AU28376/01A patent/AU2837601A/en not_active Abandoned
- 2000-11-29 AT AT00993298T patent/ATE268406T1/en active
- 2000-11-29 RU RU2002117417/12A patent/RU2002117417A/en unknown
- 2000-11-29 CA CA002394173A patent/CA2394173A1/en not_active Abandoned
- 2000-11-29 CN CN00816924A patent/CN1409783A/en active Pending
- 2000-12-06 TW TW089125951A patent/TW541382B/en active
-
2002
- 2002-06-06 NO NO20022676A patent/NO322867B1/en not_active IP Right Cessation
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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DE2735300A1 (en) * | 1977-08-05 | 1979-02-08 | Konrad Mattern | Spray treatment plant for removing and utilising spray condensates - preventing pollution of natural water by waste e.g. from cellulose plant |
WO1998033970A1 (en) * | 1997-02-04 | 1998-08-06 | Stockhausen Gmbh & Co. Kg | Process for producing fibrous materials with improved properties |
Also Published As
Publication number | Publication date |
---|---|
WO2001042555A3 (en) | 2001-12-06 |
AU2837601A (en) | 2001-06-18 |
RU2002117417A (en) | 2004-01-27 |
DE50006708D1 (en) | 2004-07-08 |
CA2394173A1 (en) | 2001-06-14 |
CN1409783A (en) | 2003-04-09 |
NO322867B1 (en) | 2006-12-18 |
NO20022676L (en) | 2002-06-06 |
EP1252388A2 (en) | 2002-10-30 |
NO20022676D0 (en) | 2002-06-06 |
ATE268406T1 (en) | 2004-06-15 |
DE19959826A1 (en) | 2001-06-28 |
WO2001042555A2 (en) | 2001-06-14 |
TW541382B (en) | 2003-07-11 |
US20040011482A1 (en) | 2004-01-22 |
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