US20060054513A1 - Polymer for fuel tanks - Google Patents

Polymer for fuel tanks Download PDF

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Publication number
US20060054513A1
US20060054513A1 US10/512,583 US51258304A US2006054513A1 US 20060054513 A1 US20060054513 A1 US 20060054513A1 US 51258304 A US51258304 A US 51258304A US 2006054513 A1 US2006054513 A1 US 2006054513A1
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United States
Prior art keywords
fuel tank
tank according
polyethylene resin
molecular weight
weight block
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Abandoned
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US10/512,583
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English (en)
Inventor
Michel Walter Lequeux
Francois Neuray
Fabian Siberdt
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.)
Ineos Manufacturing Belgium NV
Original Assignee
Solvay Polyolefins Europe Belgium SA
Innovene Manufacturing Belgium NV
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Application filed by Solvay Polyolefins Europe Belgium SA, Innovene Manufacturing Belgium NV filed Critical Solvay Polyolefins Europe Belgium SA
Assigned to O & D BELGIUM NV reassignment O & D BELGIUM NV MERGER (SEE DOCUMENT FOR DETAILS). Assignors: BP HIGH DENSITY POLYETHYLENE BELGIUM NV
Assigned to INNOVENE MANUFACTURING BELGIUM NV reassignment INNOVENE MANUFACTURING BELGIUM NV CHANGE OF NAME WITH ENGLISH TRANSLATION Assignors: O & D BELGIUM NV
Assigned to BP HIGH DENSITY POLYETHYLENE BELGIUM NV reassignment BP HIGH DENSITY POLYETHYLENE BELGIUM NV CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: SOLVAY POLYOFINS EUROPE-BELGIUM SA
Publication of US20060054513A1 publication Critical patent/US20060054513A1/en
Assigned to INEOS MANUFACTURING BELGIUM NV reassignment INEOS MANUFACTURING BELGIUM NV CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: INNOVENE MANUFACTURING BELGIUM NV
Assigned to SOLVAY POLYOLEFINS EUROPE-BELGIUM (S.A.) reassignment SOLVAY POLYOLEFINS EUROPE-BELGIUM (S.A.) ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LEQUEUX, MICHEL WALTER GHISLAIN, NEURAY, FRANCOIS, SIBERDT, FABIAN
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F10/02—Ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F297/00—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer
    • C08F297/06—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type
    • C08F297/08—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins
    • C08F297/083—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins the monomers being ethylene or propylene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing four or more carbon atoms
    • C08L23/0815—Copolymers of ethene with unsaturated hydrocarbons only containing four or more carbon atoms with aliphatic 1-olefins containing one carbon-to-carbon double bond
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60K—ARRANGEMENT OR MOUNTING OF PROPULSION UNITS OR OF TRANSMISSIONS IN VEHICLES; ARRANGEMENT OR MOUNTING OF PLURAL DIVERSE PRIME-MOVERS IN VEHICLES; AUXILIARY DRIVES FOR VEHICLES; INSTRUMENTATION OR DASHBOARDS FOR VEHICLES; ARRANGEMENTS IN CONNECTION WITH COOLING, AIR INTAKE, GAS EXHAUST OR FUEL SUPPLY OF PROPULSION UNITS IN VEHICLES
    • B60K15/00—Arrangement in connection with fuel supply of combustion engines or other fuel consuming energy converters, e.g. fuel cells; Mounting or construction of fuel tanks
    • B60K15/03—Fuel tanks
    • B60K15/03177—Fuel tanks made of non-metallic material, e.g. plastics, or of a combination of non-metallic and metallic material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F110/02—Ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers

Definitions

  • the present invention relates to an automobile fuel tank comprising polyethylene and to the manufacture of such a tank.
  • Automobile fuel tanks comprising high density polyethylene are known. Such fuel tanks are required to exhibit high safety performance, particularly with regard to fire resistance and impact resistance. They are required to meet minimum statutory industry specified performance criteria both with respect to creep resistance when the tank is subjected to a fire, and crash test resistance when the tank is subjected to an impact. An automobile fuel tank for use in Europe is required to have a fire resistance and an impact resistance both complying with the respective standards defined in ECE34, Annex 5. In order to meet these standards, known blow moulded automobile fuel tanks are required to have a minimum wall thickness of at least 3 mm so as to provide sufficient impact strength and creep resistance for the fuel tank as a whole. An automobile fuel tank composed of polyethylene typically has a volume of up to about 100 litres, or even greater.
  • a fuel tank is required to have a good environmental stress crack resistance, good creep resistance and also good impact resistance.
  • JP 06172594 discloses a polyethylene composition suitable for blow-moulding into a gasoline tank, which comprises a blend of a high molecular weight polymer and a low molecular weight polymer made using a Ziegler catalyst.
  • Ziegler catalysts have a variable comonomer content with molecular weight, and a usually have a broad molecular weight distribution, generally significantly greater than 4.
  • WO 97/02294 and WO 95/11264 both discloses a bimodal HDPE resin in which the low molecular weight component is produced using a metallocene catalyst, and the high molecular weight component produced using a non-metallocene catalyst.
  • the resins a re intended for use as films, they are said to be suitable for blow-moulding into containers a fuel tank is given as one example of a container.
  • the non-metallocene part of the catalyst can be expected to produce a high molecular weight component having a variable comonomer content with molecular weight, and also a broad molecular weight distribution, probably greater than 4. This would be expected to result in a resin having poor impact properties.
  • the present invention provides a fuel tank for a vehicle comprising at least one component which is blow-moulded multimodal polyethylene having a polydispersity M w /M n of at least 4, formed of at least two blocks, each having a polydispersity M w /M n of less than 4.
  • the blow-moulded component forms one or more of the walls of the tank.
  • multimodal polyethylene is meant polyethylene having at least two components of different molecular weights and compositions (ie comonomer content).
  • the polydispersity of the injection-moulded multimodal polyethylene is preferably no greater than 35, more preferably no greater than 20. The most preferred range is 4-20.
  • the invention provides a fuel tank for a vehicle comprising at least one component which is blow-moulded multimodal polyethylene, wherein the polyethylene has a creep deformation at 80° C. of no more than 2.4%, and a Charpy impact at ⁇ 40° C. of at least 15 kJ/m 2 .
  • the polyethylene has a creep resistance at 80° C. of no more than 2.3%; preferably it has a Charpy impact at ⁇ 40° C. of at least 20 kJ/m 2 .
  • Charpy impact is defined as the impact as assessed by notched Charpy tests performed at ⁇ 40° C. on specimens taken from 4 mm compressed plates according to ISO179/1EA.
  • Creep resistance is defined as that assessed by tensile strength measurements preformed at 80° C. under 2.5 Mpa on ISOB1A specimens machined from 2 mm thick compressed plates.
  • the polyethylene is preferably bimodal: by “bimodal” is meant two components of different molecular weights, one having a higher relative molecular weight than the other of the two components and compositions (ie comonomer content).
  • the unformulated polyethylene resin before the incorporation of any additives, preferably has a density of from 930 to 965 kg/m 3 . If following injection moulding the density is lower than 930 kg/m 3 , then the creep resistance of the component may be insufficient for use in an automobile fuel tank. If the density is higher than 965 kg/m 3 , then the walls of the tank may be too brittle, resulting in insufficient impact resistance and toughness. In this specification, the density of the polyethylene is measured according to ISO 1183. Resins used in fuel tanks typically contain about 0.5wt % of carbon black, which increases the density compared with unformulated resin by less than 1 kg/m 3 .
  • the high load melt index (HLMI) of the resin is preferably between 1 and 10, more preferably between 2 and 7 g/10 min. HLMI is measured using the procedures of ASTM D 1238 at 190° C. using a load of 21.6 kg.
  • an important parameter of the resin is its viscosity at low shear rate. Accordingly it is preferred that the value of ⁇ 0 , the viscosity at a shear rate of 1 s ⁇ 1 , with a conical die having a ratio of length to internal diameter of 0.3:1, is at least 2.5 ⁇ 10 6 dPa.s, preferably at least 3 ⁇ 10 6 dPa.s.
  • the bimodal polyethylene preferably comprises 20-80% of a high molecular weight block, and 70-30% of a low molecular weight block. Most preferred is 35-65% of the high molecular weight block, and 65-35% of the low molecular weight block.
  • the low molecular weight block is preferably a homopolymer of ethylene, but may also be a copolymer.
  • the high molecular weight block is preferably a copolymer of ethylene and one or more of butene, pentene, hexene and octene.
  • the Melt Index (MI 2 ) of the low molecular weight block is preferably less than 500, more preferably less than 100 g/10 min. MI 2 is measured using the procedures of ASTM D 1238 at 190° C. using a load of 21.6 kg.
  • the HLMI of high molecular weight block is preferably between 0.001 and 2, more preferably between 0.01 and 0.7; its density is preferably less than 950, more preferably less than
  • the polyethylene resin utilised in the present invention may be made using a Ziegler-Natta catalyst.
  • the Ziegler-Natta catalyst should be one capable of producing individual blocks having polydispersities of less than 4.
  • the polydispersity of overall resin in such a case is preferably between 10 and 18.
  • Ziegler-Natta catalysts typically consist of two main components. One component is an alkyl or hydride of a Group I to III metal, most commonly Al(Et) 3 or Al(iBu) 3 or Al(Et) 2 Cl but also encompassing Grignard reagents, n-butyllithium, or dialkylzinc compounds.
  • the second component is a salt of a Group IV to VIII transition metal, most commonly halides of titanium or vanadium such as TiCl 4 , TiCl 3 , VCl 4 , or VOCl 3 .
  • the catalyst components when mixed, usually in a hydrocarbon solvent, may form a homogeneous or heterogeneous product. Such catalysts may be impregnated on a support, if desired, by means known to those skilled in the art and so used in any any of the major processes known for co-ordination catalysis of polyolefins such as solution, slurry, and gas-phase. In addition to the two major components described above, minor amounts of other compounds (typically electron donors) may be added to further modify the polymerisation behaviour or activity of the catalyst.
  • At least the high molecular weight block, and preferably both blocks, of the polyethylene resin are made using a metallocene catalyst, in which case the polydispersity of the resin is preferably between 5 and 9. It is believed that the improved properties of the fuel tanks are due to the fact that metallocene catalysts have a generally constant comonomer content as molecular weight varies.
  • Metallocenes may typically be represented by the general formula: (C 5 R n ) y Z x (C 5 R m )ML (4-y-l)
  • the most preferred complexes are those wherein y is 1 and L is halide or alkyl.
  • Typical examples of such complexes are bis (cyclopentadienyl) zirconium dichloride and bis(cyclopentadieniyl zirconium dimethyl.
  • the cyclopentadienyl ligands may suitably be substituted by alkyl groups such as methyl, n-butyl or vinyl. Alternatively the R groups may be joined together to form a ring substituent, for example indenyl or fluorenyl.
  • the cyclopentadienyl ligands may be the same or different.
  • Typical examples of such complexes are bis(n-butylcyclopentadienyl)zirconium dichloride or his (methylcyclopentadienyl)zirconium dichloride.
  • metallocene complex is constrained geometry complexes in which the metal is in the highest oxidation state.
  • constrained geometry complexes in which the metal is in the highest oxidation state.
  • the complexes have the general formula: wherein:
  • Cp* is a single ⁇ 5-cyclopentadienyl or ⁇ 5-substituted cyclopentadienyl group optionally covalently bonded to M through -Z-Y— and corresponding to the formula: wherein each R is independently hydrogen or a moiety selected from halogen, alkyl, aryl, haloalkyl, alkoxy, aryloxy, silyl groups, and combinations thereof of up to 20 non-hydrogen atoms, or two or more R groups together form a fused ring system;
  • Y is a nitrogen or phosphorus containing group corresponding to the formula (—NR 1 ) or (—P R 1 ) wherein R 1 is C 1 -C 10 alkyl or C 6 -C 10 aryl and wherein Z is SiR′′ 2 , CR′′ 2 , SiR′′ 2 SiR′′ 2 , CR′′ ⁇ CR′′ or GeR′′ 2 in which R′′ is hydrogen or hydrocarbyl.
  • M is titanium or zirconium.
  • metallocene complexes are those wherein the anionic ligand represented in the above formulae is replaced with a diene moiety.
  • the transition metal may be in the +2 or +4 oxidation state and a typical example of this type of complex is ethylene bis indenyl zirconium (II) 1,4-diphenyl butadiene.
  • II ethylene bis indenyl zirconium
  • Examples of such complexes may be found in EP 775148A and WO 95/00526 the disclosures of which are incorporated herein by reference.
  • complexes may have the general formula: wherein:
  • the polymerisation was then started by flushing the solid catalyst A, ethylene bis (4,5,6,7-tetrahydro-1-indenyl) zirconium dichloride (prepared in accordance with the method of Brintzinger as published in the Journal of Organometallic Chemistry 288 (1995) pages 63 to 67), into the autoclave with 200 ml of isobutane.
  • the temperature, partial pressure of ethylene, and the H 2 /C 2 ratio were kept constant over the polymerisation period.
  • the reaction was stopped by cooling and then venting the reactor.
  • the low molecular weight polyethylene was then collected from the reactor.
  • the high molecular weight ethylene-hexene copolymer obtained was collected from the reactor.
  • the desired quantity of the low molecular weight polyethylene fraction obtained in Example A above was blended with the desired quantity of the high molecular weight ethylene-hexene copolymer obtained in Example B together with Irganox B225 antioxidant commercially available from CIBA Speciality Chemicals.
  • the resulting blend was pelletised in an extruder (APV Baker under the trade name MP19TC25).
  • the details of the blending recipes are specified in Table 2. TABLE 1 polymerisation conditions LMW block HMW block H 2 /C2 C2 1- gas partial hexene phase pressure content Ex.
  • ratio (bar) (g) 1 3290 16 24 2 1960 18 20 3 1790 6 6 4 3290 18 50 5 1960 14 27 6 1570 14 20 7 1580 4 6 8 1830 10 18 9 1020 18 20 10 1790 6 10 11 1030 16 24 12 1030 4 6 13 1830 12 18.7 14 1690 12 26.8 15 1190 6 10 16 1330 18 50 17 1020 14 27 18 1190 12 18.7 19 1330 12 27
  • compressed plates of varying thicknesses were formed as follows. Polymer flake was loaded into a picture-frame mould and brought in contact with the plates of a hot press, which were rapidly heated up to 190° C. at a pressure of 20 bar. The sample was held at those conditions for approximately 5 minutes. The pressure was increased to 80 bar in order to force the polymer to flow out through the shape of the frame. After 5 minutes, pressure was released and the temperature was decreased at a rate of 15° C./min down to 35° C. The plates thus obtained were stored at room temperature for at least 7 days before being submitted to any mechanical tests.
  • Creep resistance was assessed by tensile strength measurements performed at 80° C. under 2.5 Mpa on ISOB1A specimens machined from 2 mm thick compressed plates.
  • Environmental stress crack resistance was determined by FNCT performed at 50° C. under 7 Mpa stress on 6 ⁇ 6 mm specimens taken from compressed plates.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Cooling, Air Intake And Gas Exhaust, And Fuel Tank Arrangements In Propulsion Units (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Blow-Moulding Or Thermoforming Of Plastics Or The Like (AREA)
  • Containers Having Bodies Formed In One Piece (AREA)
US10/512,583 2002-04-26 2003-04-10 Polymer for fuel tanks Abandoned US20060054513A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP02077189A EP1357152A1 (en) 2002-04-26 2002-04-26 Polymer for fuel tanks
EP02077189.5 2002-04-26
PCT/EP2003/003791 WO2003091329A1 (en) 2002-04-26 2003-04-10 Polymer for fuel tanks

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US20060054513A1 true US20060054513A1 (en) 2006-03-16

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US10/512,583 Abandoned US20060054513A1 (en) 2002-04-26 2003-04-10 Polymer for fuel tanks

Country Status (9)

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US (1) US20060054513A1 (enExample)
EP (2) EP1357152A1 (enExample)
JP (1) JP2005523968A (enExample)
CN (1) CN1649953A (enExample)
AU (1) AU2003226803A1 (enExample)
BR (1) BR0309571A (enExample)
CA (1) CA2483458A1 (enExample)
MX (1) MXPA04010571A (enExample)
WO (1) WO2003091329A1 (enExample)

Cited By (7)

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US20070299213A1 (en) * 2006-06-22 2007-12-27 General Electric Company Process For Making Polysiloxane/Polyimide Copolymer Blends
US20070298255A1 (en) * 2006-06-22 2007-12-27 General Electric Company Conductive Wire Comprising A Polysiloxane/Polyimide Copolymer Blend
US20070299215A1 (en) * 2006-06-22 2007-12-27 General Electric Company Polysiloxane/Polyimide Copolymers and Blends Thereof
US20080223602A1 (en) * 2007-03-12 2008-09-18 General Electric Company Polysiloxane/polyimide copolymer blends
US20080236864A1 (en) * 2007-03-28 2008-10-02 General Electric Company Cross linked polysiloxane/polyimide copolymers, methods of making, blends thereof, and articles derived therefrom
US20100028578A1 (en) * 2007-01-16 2010-02-04 Prime Polymer Co., Ltd. Blow molding ethylene resin composition and blow molded article therefrom
US10377886B2 (en) * 2015-03-31 2019-08-13 Japan Polyethylene Corporation Polyethylene for pipe and joint, and molded body thereof

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EP1605014A1 (en) * 2004-06-09 2005-12-14 SOLVAY POLYOLEFINS EUROPE - BELGIUM (Société Anonyme) Polyethylene pipe fitting resins
GB0423555D0 (en) * 2004-10-22 2004-11-24 Borealis Tech Oy Process
WO2007094383A1 (ja) * 2006-02-15 2007-08-23 Mitsui Chemicals, Inc. 耐環境応力破壊改良剤及びこれを含んで成る耐環境応力破壊性改良樹脂組成物
JP2010242057A (ja) * 2009-03-19 2010-10-28 Asahi Kasei Chemicals Corp ガラス基板合紙
BR112015004929B1 (pt) 2012-09-13 2021-05-18 Dow Global Technologies Llc composição e artigo
JP2017179305A (ja) * 2016-03-31 2017-10-05 日本ポリエチレン株式会社 ポリエチレン樹脂用改質材、ポリエチレン樹脂組成物の製造方法、及び成形体の製造方法
JP2017179304A (ja) * 2016-03-31 2017-10-05 日本ポリエチレン株式会社 ポリエチレン樹脂用改質材、並びに、それを用いたポリエチレン樹脂組成物の製造方法、及び、成形体の製造方法

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US8491997B2 (en) 2006-06-22 2013-07-23 Sabic Innovative Plastics Ip B.V. Conductive wire comprising a polysiloxane/polyimide copolymer blend
US20070298255A1 (en) * 2006-06-22 2007-12-27 General Electric Company Conductive Wire Comprising A Polysiloxane/Polyimide Copolymer Blend
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EP1357152A1 (en) 2003-10-29
EP1499674A1 (en) 2005-01-26
CA2483458A1 (en) 2003-11-06
CN1649953A (zh) 2005-08-03
MXPA04010571A (es) 2005-08-15
AU2003226803A1 (en) 2003-11-10
WO2003091329A1 (en) 2003-11-06
JP2005523968A (ja) 2005-08-11
BR0309571A (pt) 2005-02-09

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