EP1250487B1 - Paper making processes using enzyme and polymer combinations - Google Patents

Paper making processes using enzyme and polymer combinations Download PDF

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Publication number
EP1250487B1
EP1250487B1 EP00991473A EP00991473A EP1250487B1 EP 1250487 B1 EP1250487 B1 EP 1250487B1 EP 00991473 A EP00991473 A EP 00991473A EP 00991473 A EP00991473 A EP 00991473A EP 1250487 B1 EP1250487 B1 EP 1250487B1
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EP
European Patent Office
Prior art keywords
pulp
cationic polymer
cationic
enzyme
polymer composition
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.)
Expired - Lifetime
Application number
EP00991473A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1250487A2 (en
Inventor
Walter B. Hill, Jr.
Richard L. Barclay
James A. O'malley
Randall W. Conrod
John Desjardins
Roger M. Plourde
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.)
Buckman Laboratories International Inc
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Buckman Laboratories International Inc
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Filing date
Publication date
Application filed by Buckman Laboratories International Inc filed Critical Buckman Laboratories International Inc
Publication of EP1250487A2 publication Critical patent/EP1250487A2/en
Application granted granted Critical
Publication of EP1250487B1 publication Critical patent/EP1250487B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • D21H17/005—Microorganisms or enzymes
    • 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
    • D21H11/02—Chemical or chemomechanical or chemothermomechanical pulp
    • D21H11/06—Sulfite or bisulfite pulp
    • 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
    • D21H17/29—Starch cationic
    • 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
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
    • D21H17/375—Poly(meth)acrylamide
    • 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
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/41—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups
    • D21H17/44—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups cationic
    • D21H17/45—Nitrogen-containing groups
    • D21H17/455—Nitrogen-containing groups comprising tertiary amine or being at least partially quaternised
    • 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
    • D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
    • D21H23/76—Processes or apparatus for adding material to the pulp or to the paper characterised by choice of auxiliary compounds which are added separately from at least one other compound, e.g. to improve the incorporation of the latter or to obtain an enhanced combined effect
    • D21H23/765—Addition of all compounds to the pulp

Definitions

  • the present invention relates to paper making processes and products made from these processes. More particularly, the present invention relates to treating paper making pulp with a cellulytic enzyme and one or more polymers.
  • the present invention provides a method of making paper or paperboard as set out in claim 1 that includes introducing at least one cellulytic enzyme composition and at least one cationic polymer composition to a paper making pulp within 5 minutes of each other, to form a treated pulp.
  • the enzyme composition and polymer composition can be added to the pulp separately, or they can be pre-combined and then added.
  • the pulp may also be further treated with at least one cationic starch.
  • the resulting pulp is then formed into a sheet of pulp, preferably having improved drainage and/or retention properties compared to conventional treatments. After drainage and drying, the resulting paper or paperboard preferably exhibits excellent opaqueness and other physical properties.
  • the present invention further relates to a method of making paper or paperboard that includes treating pulp in a blend chest with a cationic polymer composition and then passing the treated pulp to a machine chest wherein an enzyme composition is added to the treated pulp.
  • the enzyme-treated pulp is then refined and passed to a stuff box. From the stuff box, the pulp is then passed through a white water silo where a second cationic polymer composition is added to the pulp and then the pulp is formed into paper or paperboard.
  • the present invention also provides a paper making system for carrying out the above-described methods, and paper and paperboard made according to the methods.
  • the present invention provides methods of making paper or paperboard.
  • at least one cellulytic enzyme composition and at least one cationic polymer composition are introduced to a paper making pulp within 5 minutes of each other.
  • the enzyme composition and polymer composition can be added to the pulp separately, or they can be pre-combined and then added.
  • the resulting pulp is then formed into a paper or paperboard.
  • a cationic starch can also be added to the pulp or treated pulp either at about the same time as the cationic polymer composition and enzyme composition are added, or at a later time.
  • the cationic starch can be the same as or different from the cationic polymer added earlier.
  • Paper and paperboard products made according to the method preferably exhibit excellent opaqueness and/or other physical properties. Sheets of pulp from which the paper and paperboard products are made preferably exhibit excellent drainage and/or excellent retention of pulp fines.
  • the method of the present invention can be practiced on conventional paper making machines with modifications that can be easily made in view of the present invention.
  • the method can employ many different types of paper making pulp or combinations thereof.
  • the pulp may comprise virgin and/or recycled pulp, such as virgin sulfite pulp, broke pulp, a hardwood kraft pulp, a softwood kraft pulp, mixtures of such pulps, and the like.
  • the enzyme composition and the cationic polymer composition are added at about the same time. Adding these two components at about the same time means that the two components are added within 5 minutes of each other and more preferably are added within 2 minutes or within 1 minute of each other and most preferably are added essentially simultaneously to the pulp.
  • the enzyme composition and the polymer composition can generally be added at any location of the paper making process but preferably are added prior to the whitewater silo in a paper making process and more preferably are added prior to the machine chest and even more preferably are added prior to the blend chest. Most preferably, the enzyme composition and cationic polymer composition are added prior to the first refiner in a paper making process, which is generally located before the blend chest.
  • the enzyme composition used for treating the pulp may contain any conventional paper making pulp-treating enzyme that has cellulytic activity. Other components can be present as long as these other components do not negatively affect the cellulytic activity of the enzyme composition. Preferably, the enzyme composition also exhibits hemicellulytic activity. Suitable enzymes and enzyme-containing compositions include those described in U.S. Patent No. 5,356,800 to Jaquess , U.S. Patent No. 6,342,381 and International Publication No. WO 99/43780 . Other exemplary paper making pulp-treating enzymes are BUZYME TM 2523 and BUZYME TM 2524, both available from Buckman Laboratories International, Inc., Memphis, Tennessee.
  • the cellulytic enzyme composition preferably contains from about 5% to about 20% by weight enzyme.
  • the preferred enzyme composition can further contain polyethylene glycol, hexylene glycol, polyvinylpyrrolidone, tetrahydrofuryl alcohol, glycerine, water, and other conventional enzyme composition additives, as for example, described in U.S. Patent No. 5,356,800 .
  • the enzyme may be added to the pulp in an amount of from about 0.001 to about 0.100% by weight enzyme based on the dry weight of the pulp, for example, from about 0.005 to about 0.05% by weight.
  • the enzyme composition contains at least one polyamide oligomer and at least one enzyme.
  • the polyamide is present in an effective amount to stabilize the enzyme.
  • Exemplary enzyme compositions containing polyamide oligomers and enzymes are described in International Published Application No. WO 99/43780 .
  • the enzyme composition can include a combination of two or more different enzymes.
  • the enzyme composition can include, for example, a combination of a lipase and a cellulase, and optionally can include a stabilizing agent.
  • the stabilizing agent may be a polyamide oligomer as described herein.
  • the cationic polymer composition added to the pulp at about the same time as the enzyme composition, is added in an amount effective to preferably improve the drainage or retention of the pulp compared to no cationic polymer being present.
  • the cationic polymer is added in an amount of at least about 0.227 (0.5 pound) cationic polymer per 907.18 kg (ton) of paperstock, based on dried solids of the pulp, and preferably in an amount of at least about 0.454 kg per 907.18 kg (1 pound per ton) of paperstock.
  • the cationic polymer is added in an amount of from about 0.907 kg per 907.18 kg (2 pounds per ton) of paperstock to about 2.722 kg per 907.18 kg (6 pounds per ton) of paperstock, based on dried solids.
  • the cationic polymer may preferably be added in an amount of from about 0.0001 % to about 0.0100% by weight based on the dried solids weight of the pulp.
  • cationic polymers include, but are not limited to, cationic starches, cationic polyacrylamide polymers, for example, copolymers of an acrylamide with a cationic monomer, wherein the cationic monomer may be in a neutralized or quatemized form. Nitrogen-containing cationic polymers are preferred.
  • Exemplary cationic monomers which may be copolymerized with acrylamide to form preferred cationic polymers according to the present invention include amino alkyl esters of acrylic or methacrylic acid, and diallylamines in either neutralized or quatemized form.
  • Exemplary cationic monomers and cationic polyacrylamide polymers are described in U.S. Patent No. 4,894,119 to Baron, Jr., et al.
  • the cationic polymer may also be a polyacrylamide formed from comonomers that include, for example, 1-trimethylammonium-2-hydroxypropylmethacrylate methosulphate.
  • Other examples of cationic polymers include, but are not limited to, homopolymers of diallylamine monomers, homopolymers of aminoalkylesters of acrylic acids, and polyamines, as described in U.S. Patent No. 4,894,119 . Co-polymers, ter-polymers or high forms of polymers may also be used. Further, for purposes of the present invention, a mixture of two or more cationic polymers may be used.
  • nonionic acrylamide units are preferably present in the copolymer, and preferably present in an amount of at least about 30 mol% and generally in an amount of no greater than 95 mol%. At least about 5 mol%, and generally no greater than about 70 mol%, of the polymer is preferably formed from a cationic comonomer.
  • the weight average molecular weight of the cationic polymer is preferably over 1,000, for example, from about 10,000 to about 15,000,000, or from about 100,000 to about 10,000,000.
  • the cationic polymer present has a weight average molecular weight of at least about 10,000 and is pre-combined with the enzyme composition before the cationic polymer composition and enzyme composition are added together to the pulp.
  • the resulting treated pulp may then be processed by a conventional paper making machine and techniques.
  • the treated pulp may be additionally treated with one or more components, including other polymers such as anionic and non-ionic polymers, clays, other fillers, dyes, pigments, defoamers, biocides, pH adjusting agents such as alum, and other conventional paper making or processing additives.
  • One particularly preferred additive for use according to the methods of the present invention is a cationic starch.
  • Cationic starch may be added to the pulp or treated pulp of the present invention to form a starch treated pulp.
  • Starch may be added at one or more points along the flow of paper making pulp through the paper making apparatus or system of the present invention.
  • cationic starch can be added to a pulp at about the same time that the enzyme and cationic polymer are added to the pulp.
  • the cationic starch can alternatively or additionally be added to the treated pulp after the pulp is first treated with both the enzyme and cationic polymer.
  • Preferred cationic starches include, but are not limited to, potato starches, corn starches, and other wet-end starches, or combinations thereof.
  • starch Conventional amounts of starch can be added to the pulp.
  • An exemplary amount of starch that can be used according to the present invention is from about 2.27 to about 11.34 kg per 907.18 kg (5 to about 25 pounds per ton) based on the dried solids weight of the pulp.
  • a microparticle additive may be added to the pulp at any time during the process.
  • the microparticle additive can modify the charge of the pulp or the charge of a component of the pulp.
  • the microparticle additive can be, for example, a charging or modifying agent, a filler, a coagulating agent, and/or a retention aid.
  • the microparticle additive can be a natural or synthetic hectorite, bentonite, zeolite, alumina sol, or any of conventional particulate additives as are known to those skilled in the art.
  • a biocide may be added to the pulp or treated pulp in accordance with conventional uses of biocides in paper making processes.
  • a biocide may be added to the treated pulp in a blend chest after the pulp has been treated with the enzyme and cationic polymer.
  • Biocides useful in the paper making pulps according to the present invention include biocides well known to those skilled in the art, for example, BUSAN TM 1130, available from Buckman Laboratories International, Inc., Memphis, Tennessee.
  • FIG. 1 A flow chart of a paper making system for carrying out the method of the present invention is set forth in Figure 1 . It is to be understood that the system shown is exemplary of the present invention and is in no way intended to restrict the scope of the invention.
  • a supply of enzyme composition and a supply of cationic polymer composition are simultaneously combined at desired respective concentrations with a flowing stream of paper making pulp to form a treated pulp.
  • the supply of pulp shown represents a flow of pulp, as for example, supplied from a pulp holding tank or silo.
  • the supply of pulp shown in Figure 1 can be a conduit, holding, or mixing tank, or other container, passageway, or mixing zone for the flow of pulp.
  • the supply of enzyme composition can be, for example, a holding tank having an outlet in communication with an inlet of a treated pulp tank.
  • the supply of cationic polymer composition can be, for example, a holding tank having an outlet in communication with an inlet of the treated pulp tank.
  • the pulp treated with the enzyme composition and cationic polymer composition is passed from the treated pulp tank through a refiner and then through a blend chest where optional additives including a biocide are combined with the treated pulp.
  • the refiner has an inlet in communication with an outlet of the treated pulp tank, and an outlet in communication with an inlet of the blend chest.
  • the pulp treated in the blend chest is passed from an outlet of the blend chest through a communication to an inlet of a machine chest.
  • the blend chest and machine chest can be of any conventional type known to those skilled in the art.
  • the machine chest ensures a level head, that is, a constant pressure on the treated pulp or stock throughout the downstream portion of the system, particularly at the head box.
  • a cationic starch is added to the refined treated pulp at the blend chest, and the system includes a conventional stuff box. Additional cationic starch may be added at the stuff box although not depicted in Figure 2 .
  • the system of Figure 2 has a second refiner between the machine chest and the stuff box.
  • Other additives including pH adjustment agents such as alum, may also be added at the stuff box. pH adjusting agents can be added at other points along the flow of pulp or treated pulp through the apparatus.
  • the apparatus of the present invention can also include metering devices for providing a suitable concentration of enzyme to the flow of pulp, for example, from about 0.001 to about 0.100 percent by weight enzyme, based on the dried solids weight of the pulp.
  • the apparatus can include a metering device for providing a suitable amount of the cationic polymer to the flow of pulp, for example, from about 0.0001 to about 1.000 percent by weight cationic polymer, based on the dried solids weight of the pulp.
  • Other metering or dosing devices are preferably provided for the other additives and ingredients that may be used during the method.
  • Pulp is treated in a blend chest with a cationic polymer composition, such as a nitrogen-containing cationic polymer or a cationic starch.
  • a cationic polymer composition such as a nitrogen-containing cationic polymer or a cationic starch.
  • the treated pulp is passed from the blend chest to a machine chest wherein an enzyme composition is added to the treated pulp to form an enzyme-treated pulp.
  • the enzyme-treated pulp is then refined and passed to a stuff box where optional cationic polymer composition is optionally added to the pulp.
  • the optional cationic polymer composition if used, may be the same or different than the first cationic polymer composition, added to the pulp at the blend chest. Alternatively, no additional cationic polymer is added to the pulp at the stuff box.
  • the pulp is then passed to a white water silo where a nitrogen-containing cationic polymer composition is added to the pulp.
  • the pulp is then passed through a fan pump to a screen and subsequently to a head box.
  • the drained stock resulting from sheet making in the head box is recirculated to the white-water silo.
  • the nitrogen-containing cationic polymer composition can be, for instance, a cationic polymer containing acrylamide units and units of a cationic monomer.
  • the first cationic polymer composition added can be a nitrogen-containing polymer, a cationic starch, or another cationic polymer.
  • the optional cationic polymer composition can also be a nitrogen-containing polymer, a cationic starch, or another cationic polymer.
  • the first cationic polymer composition, the nitrogen-containing cationic polymer composition, and the optional cationic polymer composition can be the same or different.
  • At least one of the cationic polymer compositions and the optional cationic polymer composition comprises a starch.
  • the nitrogen-containing cationic polymer composition contains acrylamide units and units of a cationic monomer.
  • a cleaner for example, a centrifugal force cleaning device, can be disposed between, for instance, the fan pump and the screen, according to any of the embodiments of Figures 1-3 above.
  • the method and apparatus of the present invention provide extended interaction time between the pulp, enzyme, and cationic polymer.
  • Treated pulp reaching the headbox in the system of the present invention can be formed into a paper or paperboard precursor sheet.
  • the sheet exhibits excellent drainage and/or retention of fines.
  • Resulting paper and paperboard made according to the method of the present invention exhibit excellent opaqueness and other physical properties.
EP00991473A 1999-11-19 2000-11-14 Paper making processes using enzyme and polymer combinations Expired - Lifetime EP1250487B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US16633099P 1999-11-19 1999-11-19
US166330P 1999-11-19
PCT/US2000/042119 WO2001036740A2 (en) 1999-11-19 2000-11-14 Paper making processes using enzyme and polymer combinations

Publications (2)

Publication Number Publication Date
EP1250487A2 EP1250487A2 (en) 2002-10-23
EP1250487B1 true EP1250487B1 (en) 2010-09-29

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EP00991473A Expired - Lifetime EP1250487B1 (en) 1999-11-19 2000-11-14 Paper making processes using enzyme and polymer combinations

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EP (1) EP1250487B1 (pt)
JP (1) JP4528478B2 (pt)
CN (1) CN1281818C (pt)
AT (1) ATE483059T1 (pt)
AU (1) AU770908B2 (pt)
BR (1) BR0015768B1 (pt)
CA (1) CA2391576C (pt)
DE (1) DE60045040D1 (pt)
ES (1) ES2350914T3 (pt)
MX (1) MXPA02004886A (pt)
NZ (1) NZ518975A (pt)
PT (1) PT1250487E (pt)
WO (1) WO2001036740A2 (pt)
ZA (1) ZA200203739B (pt)

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EP1859103B1 (en) * 2005-01-05 2015-04-08 Dow Global Technologies LLC Enhanced efficacy of fungicides in paper and paperboard
EP2147149B1 (en) * 2007-05-16 2017-03-22 Buckman Laboratories International, Inc. Methods to control organic contaminants in fibers
US8454798B2 (en) 2010-04-15 2013-06-04 Buckman Laboratories International, Inc. Paper making processes and system using enzyme and cationic coagulant combination
US8758562B2 (en) 2010-08-25 2014-06-24 Hercules Incorporated Method for increasing the advantages of starch in pulped cellulosic material in the production of paper and paperboard
CN103930619B (zh) * 2011-08-25 2016-12-07 索理思科技开曼公司 增加强度助剂在制造纸和纸板中的优势的方法
EP2929087B1 (en) * 2012-12-06 2017-02-08 Kemira OYJ Compositions used in paper and methods of making paper
CN104153243A (zh) * 2013-05-13 2014-11-19 广西南宁碧欧生物科技有限公司 一种新型促进打浆的纤维改性生物酶制剂
CN103541259B (zh) * 2013-10-19 2015-12-02 沅江浣溪沙酶技术有限公司 芦苇、狄苇造纸制浆用复合酶液的生产方法及应用
BR102015032911A2 (pt) * 2015-12-29 2017-07-04 Fibria Celulose S.A Process for the production of pulp pulp, pulp pulp and its use, paper
MX2021000113A (es) * 2018-07-10 2021-03-09 Novozymes As Metodo de fabricacion de papel o carton.
CN110983851A (zh) * 2019-11-20 2020-04-10 山鹰华南纸业有限公司 一种提高纸机烘干部运行效率的方法

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FI85389C (fi) * 1989-12-12 1992-04-10 Enso Gutzeit Oy Foerfarande foer tillverkning av massa.
US5169497A (en) * 1991-10-07 1992-12-08 Nalco Chemical Company Application of enzymes and flocculants for enhancing the freeness of paper making pulp
US5256252A (en) * 1992-07-15 1993-10-26 Nalco Chemical Company Method for controlling pitch deposits using lipase and cationic polymer
US5356800A (en) * 1992-11-30 1994-10-18 Buckman Laboratories International, Inc. Stabilized liquid enzymatic compositions
DK131193D0 (pt) * 1993-11-23 1993-11-23 Novo Nordisk As
US5423946A (en) * 1994-03-07 1995-06-13 Nalco Chemical Company Cationic anionic polyelectrolytes for enhancing the freeness of paper pulp
KR100256636B1 (ko) * 1994-04-12 2000-05-15 김충섭 종이내 충전물의 함량을 높이고 스코트 내부결합강도를 증가시키는 종이의 제조방법
US5501770A (en) * 1994-08-12 1996-03-26 Nalco Chemical Company Enzymes in combination with polyelectrolytes for enhancing the freeness of clarified sludge in papermaking
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FI990444A (fi) * 1998-03-11 1999-09-12 Nalco Chemical Co Kuitumassan jauhautuneisuustilan lisäys

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Publication number Publication date
CA2391576A1 (en) 2001-05-25
WO2001036740A2 (en) 2001-05-25
AU770908B2 (en) 2004-03-04
DE60045040D1 (de) 2010-11-11
PT1250487E (pt) 2010-11-29
JP4528478B2 (ja) 2010-08-18
AU3269601A (en) 2001-05-30
EP1250487A2 (en) 2002-10-23
CN1281818C (zh) 2006-10-25
BR0015768A (pt) 2002-10-22
ATE483059T1 (de) 2010-10-15
CN1423717A (zh) 2003-06-11
BR0015768B1 (pt) 2009-08-11
MXPA02004886A (es) 2003-02-27
NZ518975A (en) 2003-11-28
JP2003515002A (ja) 2003-04-22
ZA200203739B (en) 2003-02-26
WO2001036740A3 (en) 2002-02-07
CA2391576C (en) 2007-04-24
ES2350914T3 (es) 2011-01-28

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