US20040168782A1 - Fibrous web and process for the preparation thereof - Google Patents

Fibrous web and process for the preparation thereof Download PDF

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Publication number
US20040168782A1
US20040168782A1 US10/475,771 US47577104A US2004168782A1 US 20040168782 A1 US20040168782 A1 US 20040168782A1 US 47577104 A US47577104 A US 47577104A US 2004168782 A1 US2004168782 A1 US 2004168782A1
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United States
Prior art keywords
filler
fibrils
fiber
fiber web
web
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
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US10/475,771
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English (en)
Inventor
Petri Silenius
Jari Meuronen
Markku Leskela
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Metsa Board Oyj
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Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
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Assigned to M-REAL OYJ reassignment M-REAL OYJ ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LESKELA, MARKKU, MEURONEN, JARI, SILENIUS, PETRI
Publication of US20040168782A1 publication Critical patent/US20040168782A1/en
Priority to US11/808,273 priority Critical patent/US20080073049A1/en
Priority to US12/588,594 priority patent/US20100218908A1/en
Priority to US13/676,418 priority patent/US20130139987A1/en
Abandoned legal-status Critical Current

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Classifications

    • 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
    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
    • D21H17/24—Polysaccharides
    • D21H17/28—Starch
    • 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
    • D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
    • 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
    • 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

Definitions

  • the present invention relates to the fiber web according to the preamble of claim 1 .
  • a fiber web such as this in general comprises a filler-containing base web possibly coated with a pigment-containing coating layer.
  • the invention also relates to the method according to the preamble of claim 17 for the preparation of a fiber web.
  • the slush in papermaking is made up of cellulose fibers or lignocellulose fibers, fines and fillers. Many of these components, in particular fillers, are so small in size that they will not adhere mechanically to the wire and they have to be bound to larger fibers or to each other by flocculation.
  • retention chemicals which are added to the slush before the forming of the web. Retention chemicals to be mentioned include polymeric products such as polyethylene imine, low molar mass polyacrylamide and polyamine, as well as cationic starch, guar or polyacrylamine combined with colloidal silica, alumina or montmorillonite.
  • the amount of retention chemicals is in general at least 0.5% of the dry matter of the fiber, typically approx. 0.6-1% of the dry matter of the fiber.
  • the invention is based on the observation that the amount of conventional retention agents can be reduced significantly by replacing at least a portion of the conventional mineral fillers, i.e. pulverous mineral pigments, with a composite pigment containing light-scattering material particles deposited on the surface of the fines.
  • a filler product of this type is known from FI patent publication 100729.
  • the product comprises strings of pearls made up of calcium carbonate particles deposited on the fines and of fine fibrils.
  • this filler of a novel type that calcium carbonate is deposited on fine fibrils prepared from cellulose fibers and/or mechanical pulp fibers by beating.
  • the size distribution of the fines fraction mainly corresponds to wire screen fraction P100.
  • 10-100% of the filler in the base web is made up of cellulose fibrils or lignocellulose fibrils on which there are deposited light-scattering material particles, and these coated cellulose or lignocellulose fibrils constitute at maximum approx. 70% of the weight of the base web.
  • the fiber web according to the invention is characterized in what is stated in the characterizing part of claim 1 .
  • the method according to the invention for the preparation of a fiber web is for its part characterized in what is stated in the characterizing part of claim 17 .
  • the invention provides considerable advantages.
  • paper of uniform quality as well as a high level of formation and high retention can be produced; additionally the circulation waters are substantially cleaner and the retention agent requirement is reduced.
  • the invention does not require any flocculation of the filler, contrary to the commercially available retention systems; this has a fundamental effect on formation and the optical effect of the filler.
  • the base web does not contain any conventional retention agents, or their amount is over 20% smaller, preferably up to 50% smaller, than that of a web that has the same level of formation and contains conventional particulate fillers.
  • the option according to the invention therefore decreases the chemicals costs in the preparation of a fiber web and facilitates the recycling of waters in a paper or board machine.
  • the said reduction of 20% can thus be calculated separately from one of the components or from both components in total.
  • Example 3 the amount of the polymer component has been reduced by slightly less than 30% by weight while the quantity of nanoparticles has remained unchanged.
  • FIG. 1 shows, of the results of Example 2, the web formation as a function of the total retention
  • FIG. 2 shows the formation as a function of the wire water consistency.
  • the filler used contains a fines fraction comprising fibrils obtained from a chemical pulp.
  • chemical pulp is meant in this context a pulp that has been treated with digestion chemicals for the delignification of cellulose fibers.
  • the fibrils used in the invention are fibrils obtained by beating from pulps prepared by the sulfate process and by other alkaline processes.
  • the invention is also suited for fillers produced from fibrils obtained from chemimechanical and mechanical pulps.
  • the average thickness of cellulose or lignocellulose fibrils is smaller than 1 ⁇ m.
  • the fibrils are characterized by one or both of the following criteria:
  • the source material for the fibrils i.e. the fines based on cellulose or other fibers, is fibrillated by beating in a pulp refiner.
  • the desired fraction may, when necessary, be separated using a screen, but the fines need not always be screened.
  • Suitable fibril fractions include wire screen fractions P50-P400.
  • refiners with grooved blades are used.
  • the light-scattering material particles in the filler are inorganic or organic salts which can be formed from their source materials by precipitation in an aqueous medium.
  • Such compounds include calcium carbonate, calcium oxalate, calcium sulfate, barium sulfate, and mixtures thereof.
  • the material particles are precipitated on the fibrils in order to produce an aggregate resembling a string-of-pearls.
  • the amount of the inorganic salt compound is approx. 0.0001-95% by weight, preferably approx. 0.1-90% by weight, most suitably approx. 60-80% by weight, calculated from the amount of filler, and approx. 0.1-60% by weight, preferably approx. 0.5-50% by weight of the paper.
  • the filler is prepared by depositing the mineral pigment on the surface of fine fibrils prepared from cellulose fibers and/or mechanical pulp fibers.
  • the precipitation of calcium carbonate can be carried out by feeding into an aqueous slush of fibrils an aqueous calcium hydroxide mixture, which possibly contains solid calcium hydroxide, and a compound that contains carbonate ions and is at least partly dissolved in water. It is also possible to introduce carbon dioxide gas into the aqueous phase, which gas in the presence of calcium hydroxide produces calcium carbonate. There form string-of-pearls-like calcium carbonate crystal aggregates which are held together by fibrils, i.e.
  • the diameter of the calcium carbonate particles in the aggregates is approx. 0.1-5.1 ⁇ m, typically approx. 0.2-3 ⁇ m.
  • fibrils corresponding in the main (at least more than 55%) to wire screen fractions P50-P400 are used.
  • the paper pulp is slushed in a manner known per se to a suitable consistency (typically a solids content of approx. 0.1-1%) and is spread onto the wire.
  • a suitable consistency typically a solids content of approx. 0.1-1%) and is spread onto the wire.
  • the above-mentioned filler usually in an amount of approx. 1-100% by weight of the weight of the fibers in the fiber pulp, in other words the amount of filler may be up to equal to the amount of the actual fiber pulp.
  • the disclosed filler constitutes at least 5% by weight, most suitably 10-100% by weight, of the filler in the base web, and respectively 10-50% by weight of the fiber material in the base web.
  • a base web in which the fiber material in its entirety is made up of filler fibrils, and thus in general the present filler may constitute 1-100% by weight of the fiber material in the base web.
  • coated cellulose fibrils or lignocellulose fibrils constitute at maximum approx. 70%, e.g. approx. 10-65%, of the weight of the base web, in which case the rest of the web comprises conventional mechanical and/or chemical pulp used in papermaking and/or conventional fillers and/or other additives.
  • a portion (at maximum 95%, usually 90-10% by weight, of the total amount of filler) of the filler used in the slush may consist of conventional fillers, such as calcium carbonate (natural or precipitated), kaolin, talc, hydrogenated aluminum oxides (aluminum trihydroxides), calcium sulfate, barium sulfate, calcium oxalate, or titanium dioxide.
  • conventional fillers such as calcium carbonate (natural or precipitated), kaolin, talc, hydrogenated aluminum oxides (aluminum trihydroxides), calcium sulfate, barium sulfate, calcium oxalate, or titanium dioxide.
  • at least 80%, especially preferably at least 90%, of the precipitated light-scattering pigment particles are attached to fibrils.
  • the filler used is mainly a product in which the particles are not loose but attached to fibrils.
  • the formation and retention of paper are improved by using a portion of the filler in a form bound to fibrils.
  • the filler used is at least partly for example calcium carbonate, calcium oxalate, calcium sulfate or barium sulfate, of which a portion is in a pulverous form and a portion in a form attached to fibrils.
  • a portion (at least approx. 5% by weight, preferably at least 10% by weight, most suitably at least 20% by weight) of the pulverous filler is replaced with a product attached to fibrils.
  • the fiber pulp is formed into a paper or board web.
  • the fiber web is dried and most suitably coated, and optionally after-treated by for example calendering.
  • the web can be coated with, for example, calcium carbonate, gypsum, aluminum silicate, kaolin, aluminum hydroxide, magnesium silicate, talc, titanium dioxide, barium sulfate, zinc oxide, synthetic pigment, or mixtures thereof.
  • the light-scattering material particles of the filler in the web are present in the fiber web in a substantially unflocculated form. This means that the formation of the web is quite good.
  • the web contains conventional retention agents, such as cationic starch and/or silica, in total at maximum 0.40% by weight of the mass of the fiber.
  • the web is substantially or entirely free of ionic retention agents.
  • Conventional retention agents in particular include those used together with conventional fillers.
  • cellulose-containing material is meant here generally paper or board or a corresponding cellulose-containing material derived from a lignocellulose-containing raw material, in particular wood or annual or perennial plants.
  • the said material may be wood-containing or woodfree, and it may be prepared from mechanical, semimechanical (chemimechanical) or chemical pulp.
  • the chemical pulp and the mechanical pulp may be bleached or unbleached.
  • the material may also contain recycled fibers, in particular recycled paper or recycled board.
  • the grammage of the material web varies typically within the range 35-500 g/m 2 , in particular it is approx. 50-450 g/m 2 .
  • the grammage of base paper is 20-250 g/m 2 , preferably 30-80 g/m 2 .
  • a base paper of this type having a grammage of approx. 50-70 g/m 2
  • 10-20 g of coating/m 2 /side and by calendering the paper
  • An especially preferred product is a coated offset paper in which high gloss and high opacity and bulk are combined.
  • the invention is also suited for the production of coated fine papers, possibly also containing mechanical pulp, as well as writing and printing papers.
  • Birch sulfate pulp was beaten in Valmet's JC-01 refiner in order to produce a pulp suitable for the preparation of filler.
  • the consistency during the beating was approx. 4%, its total energy consumption 343 kWh/t and its specific edge load 0.5 J/m.
  • Example 1 The product described in Example 1 was used as filler in coated fine papers.
  • the following table depicts the results of a fine paper test run carried out in Sweden with STFI's pilot machine (FEX): TABLE 2 Results of fine paper runs Filler Wire water concentration, consistency, Total % g/l retention, % Formation, % PCC 18.8 2.03 72.9 10.6 PCC 21.0 2.68 66.9 11.1 SuperFill 17.8 0.48 91.1 10.4 SuperFill 22.4 0.67 88.3 9.5
  • the PCC used in the tests was Albacar LO product supplied by Specialty Minerals.
  • the method is provided special value by the fact that the above-mentioned combinations of properties are achieved simultaneously with better optical properties and strengths.
  • base paper having a grammage of 56 g/m 2 was prepared in mill conditions.
  • the slush consisted of a mixture of birch pulp (74%) and pine pulp (24%). After beating, the SR number of the pine pulp was 32-34° and that of the birch pulp was 22-25°. The SR number of the pulp in the head box was 35-40°.
  • the wire section of the paper machine was Valmet's hybride wire (Sym-former), and the wet press end comprised Valmet's Sym-Press II having a triple press and a conventional drying section.
  • the retention chemicals used were nanoparticles and cationic starch (Compozil Plus: EKA NP 780 nanoparticle and EKA PL 1510 C-Pam, supplier: EKA Chemicals).
  • talc and PCC the doses were as follows: nanoparticle 280 g/t, polymer 70 g/t, and those for SuperFill were: nanoparticle 280 g/t, polymer 50 g/t.
  • the amounts of cationic starch and resin size used were 8 kg/t and 5.2 kg/t.
  • Alum was dosed for talc in an amount of 13 kg/t and for PCC and SuperFill in an amount of 19 kg/t.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)
US10/475,771 2001-04-24 2002-04-24 Fibrous web and process for the preparation thereof Abandoned US20040168782A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US11/808,273 US20080073049A1 (en) 2001-04-24 2007-06-07 Fibrous web and process for the preparation thereof
US12/588,594 US20100218908A1 (en) 2001-04-24 2009-10-20 Fibrous web and process for the preparation thereof
US13/676,418 US20130139987A1 (en) 2001-04-24 2012-11-14 Fibrous web and process for the preparation thereof

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FI20010847 2001-04-24
FI20010847A FI117873B (fi) 2001-04-24 2001-04-24 Kuiturata ja menetelmä sen valmistamiseksi
PCT/FI2002/000344 WO2002090652A1 (en) 2001-04-24 2002-04-24 Fibrous web and process for the preparation thereof

Related Child Applications (1)

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US11/808,273 Continuation US20080073049A1 (en) 2001-04-24 2007-06-07 Fibrous web and process for the preparation thereof

Publications (1)

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US20040168782A1 true US20040168782A1 (en) 2004-09-02

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US10/475,771 Abandoned US20040168782A1 (en) 2001-04-24 2002-04-24 Fibrous web and process for the preparation thereof
US11/808,273 Abandoned US20080073049A1 (en) 2001-04-24 2007-06-07 Fibrous web and process for the preparation thereof
US12/588,594 Abandoned US20100218908A1 (en) 2001-04-24 2009-10-20 Fibrous web and process for the preparation thereof
US13/676,418 Abandoned US20130139987A1 (en) 2001-04-24 2012-11-14 Fibrous web and process for the preparation thereof

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US11/808,273 Abandoned US20080073049A1 (en) 2001-04-24 2007-06-07 Fibrous web and process for the preparation thereof
US12/588,594 Abandoned US20100218908A1 (en) 2001-04-24 2009-10-20 Fibrous web and process for the preparation thereof
US13/676,418 Abandoned US20130139987A1 (en) 2001-04-24 2012-11-14 Fibrous web and process for the preparation thereof

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US (4) US20040168782A1 (zh)
EP (1) EP1392922A1 (zh)
JP (1) JP5064644B2 (zh)
CN (1) CN1279243C (zh)
AU (1) AU2002247795B2 (zh)
CA (1) CA2444795C (zh)
FI (1) FI117873B (zh)
NZ (1) NZ541156A (zh)
WO (1) WO2002090652A1 (zh)

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US20060060318A1 (en) * 2002-10-24 2006-03-23 Petri Silenius Method for manufacturing paper and board
US20090211720A1 (en) * 2005-03-18 2009-08-27 Myllymaeki Vesa Composite Materials, Method for Their Preparation, and Use in Paper and Board Manufacturing
US20120080156A1 (en) * 2010-10-01 2012-04-05 Fpinnovations Cellulose-reinforced high mineral content products and methods of making the same
US8231764B2 (en) 2009-05-15 2012-07-31 Imerys Minerals, Limited Paper filler method
US10053817B2 (en) 2010-04-27 2018-08-21 Fiberlean Technologies Limited Process for the manufacture of structured materials using nano-fibrillar cellulose gels
US10214859B2 (en) 2016-04-05 2019-02-26 Fiberlean Technologies Limited Paper and paperboard products
US10253457B2 (en) 2010-11-15 2019-04-09 Fiberlean Technologies Limited Compositions
US10294371B2 (en) 2009-03-30 2019-05-21 Fiberlean Technologies Limited Process for the production of nano-fibrillar cellulose gels
US10301774B2 (en) 2009-03-30 2019-05-28 Fiberlean Technologies Limited Process for the production of nano-fibrillar cellulose suspensions
US10577469B2 (en) 2015-10-14 2020-03-03 Fiberlean Technologies Limited 3D-formable sheet material
US10794006B2 (en) 2016-04-22 2020-10-06 Fiberlean Technologies Limited Compositions comprising microfibrilated cellulose and polymers and methods of manufacturing fibres and nonwoven materials therefrom
US11155697B2 (en) 2010-04-27 2021-10-26 Fiberlean Technologies Limited Process for the production of gel-based composite materials
US11846072B2 (en) 2016-04-05 2023-12-19 Fiberlean Technologies Limited Process of making paper and paperboard products

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FI124859B (fi) 2011-06-21 2015-02-27 Upm Kymmene Corp Painopaperituote sekä menetelmä ja järjestelmä painopaperituotteen valmistamiseksi
US9879361B2 (en) 2012-08-24 2018-01-30 Domtar Paper Company, Llc Surface enhanced pulp fibers, methods of making surface enhanced pulp fibers, products incorporating surface enhanced pulp fibers, and methods of making products incorporating surface enhanced pulp fibers
FI125836B (fi) * 2013-04-26 2016-03-15 Wetend Tech Oy Menetelmä täyteaineen järjestämiseksi paperi- tai kartonkimassaan ja paperi tai kartonki
JP6403788B2 (ja) 2014-02-21 2018-10-10 ドムター ペーパー カンパニー， エルエルシー 紙製品及びその製造方法
CN106458751B (zh) 2014-02-21 2019-11-15 同拓纸业有限责任公司 纤维水泥中的表面增强纸浆纤维
US11473245B2 (en) 2016-08-01 2022-10-18 Domtar Paper Company Llc Surface enhanced pulp fibers at a substrate surface
WO2018075627A1 (en) 2016-10-18 2018-04-26 Domtar Paper Company, Llc Method for production of filler loaded surface enhanced pulp fibers
CA3088962A1 (en) 2018-02-05 2019-08-08 Harshad PANDE Paper products and pulps with surface enhanced pulp fibers and increased absorbency, and methods of making same
CA3134990A1 (en) 2019-03-26 2020-10-01 Domtar Paper Company, Llc Paper products subjected to a surface treatment comprising enzyme-treated surface enhanced pulp fibers and methods of making the same

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US8491755B2 (en) * 2002-10-24 2013-07-23 M-Real Oyj Method for manufacturing paper and board
US20060060318A1 (en) * 2002-10-24 2006-03-23 Petri Silenius Method for manufacturing paper and board
US20090211720A1 (en) * 2005-03-18 2009-08-27 Myllymaeki Vesa Composite Materials, Method for Their Preparation, and Use in Paper and Board Manufacturing
US10982387B2 (en) 2009-03-30 2021-04-20 Fiberlean Technologies Limited Process for the production of nano-fibrillar cellulose suspensions
US10294371B2 (en) 2009-03-30 2019-05-21 Fiberlean Technologies Limited Process for the production of nano-fibrillar cellulose gels
US10301774B2 (en) 2009-03-30 2019-05-28 Fiberlean Technologies Limited Process for the production of nano-fibrillar cellulose suspensions
US10975242B2 (en) 2009-03-30 2021-04-13 Fiberlean Technologies Limited Process for the production of nano-fibrillar cellulose gels
US8231764B2 (en) 2009-05-15 2012-07-31 Imerys Minerals, Limited Paper filler method
US11162219B2 (en) 2009-05-15 2021-11-02 Fiberlean Technologies Limited Paper filler composition
US9127405B2 (en) 2009-05-15 2015-09-08 Imerys Minerals, Limited Paper filler composition
US10100464B2 (en) 2009-05-15 2018-10-16 Fiberlean Technologies Limited Paper filler composition
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US11732411B2 (en) 2009-05-15 2023-08-22 Fiberlean Technologies Limited Paper filler composition
US11970817B2 (en) 2009-05-15 2024-04-30 Fiberlean Technologies Limited Paper filler composition
US10633796B2 (en) 2010-04-27 2020-04-28 Fiberlean Technologies Limited Process for the manufacture of structured materials using nano-fibrillar cellulose gels
US10100467B2 (en) 2010-04-27 2018-10-16 Fiberlean Technologies Limited Process for the manufacture of structured materials using nano-fibrillar cellulose gels
US11155697B2 (en) 2010-04-27 2021-10-26 Fiberlean Technologies Limited Process for the production of gel-based composite materials
US10053817B2 (en) 2010-04-27 2018-08-21 Fiberlean Technologies Limited Process for the manufacture of structured materials using nano-fibrillar cellulose gels
US20120080156A1 (en) * 2010-10-01 2012-04-05 Fpinnovations Cellulose-reinforced high mineral content products and methods of making the same
US8608906B2 (en) * 2010-10-01 2013-12-17 Fpinnovations Cellulose-reinforced high mineral content products and methods of making the same
AU2011308039B2 (en) * 2010-10-01 2015-01-22 Fpinnovations Cellulose-reinforced high mineral content products and methods of making the same
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WO2002090652A1 (en) 2002-11-14
US20100218908A1 (en) 2010-09-02
CN1279243C (zh) 2006-10-11
CA2444795A1 (en) 2002-11-14
EP1392922A1 (en) 2004-03-03
NZ541156A (en) 2007-02-23
FI20010847A (fi) 2002-10-25
CA2444795C (en) 2013-07-16
US20080073049A1 (en) 2008-03-27
FI20010847A0 (fi) 2001-04-24
US20130139987A1 (en) 2013-06-06
JP2004525280A (ja) 2004-08-19
AU2002247795B2 (en) 2007-09-06
FI117873B (fi) 2007-03-30
CN1516768A (zh) 2004-07-28

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