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EP2121541A1 - Accélérateur de prise et de durcissement pour des liants hydrauliques et procédé de fabrication - Google Patents

Accélérateur de prise et de durcissement pour des liants hydrauliques et procédé de fabrication

Info

Publication number
EP2121541A1
EP2121541A1 EP08716832A EP08716832A EP2121541A1 EP 2121541 A1 EP2121541 A1 EP 2121541A1 EP 08716832 A EP08716832 A EP 08716832A EP 08716832 A EP08716832 A EP 08716832A EP 2121541 A1 EP2121541 A1 EP 2121541A1
Authority
EP
European Patent Office
Prior art keywords
accelerator
aluminum
sulfate
weight
solidification
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.)
Withdrawn
Application number
EP08716832A
Other languages
German (de)
English (en)
Inventor
Heinz Schürch
Franz Wombacher
Benedikt Lindlar
Didier Lootens
Robert Flatt
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.)
Sika Technology AG
Original Assignee
Sika Technology AG
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
Application filed by Sika Technology AG filed Critical Sika Technology AG
Priority to EP08716832A priority Critical patent/EP2121541A1/fr
Publication of EP2121541A1 publication Critical patent/EP2121541A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/10—Accelerators; Activators
    • C04B2103/12—Set accelerators
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/10—Accelerators; Activators
    • C04B2103/14—Hardening accelerators
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00034—Physico-chemical characteristics of the mixtures
    • C04B2111/00146—Sprayable or pumpable mixtures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/10—Compositions or ingredients thereof characterised by the absence or the very low content of a specific material
    • C04B2111/1062—Halogen free or very low halogen-content materials
    • C04B2111/1068—Halogens other than chlorine
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

  • the invention relates to a solidification and hardening accelerator for hydraulic binders, to a process for preparing a solidification and hardening accelerator for hydraulic binders, and to the use of the setting and hardening accelerator in a shotcrete or sprayed mortar.
  • EP 0 076 927 B1 discloses alkali-free solidification accelerators for hydraulic binders which are intended to avoid these disadvantages.
  • a hydraulic binder such as cement, lime, hydraulic lime and gypsum and mortar and concrete made therefrom
  • the mixture containing said binder is from 0.5 to 10% by weight based on the weight of this binder
  • an alkali-free solidification and hardening accelerator this accelerator containing aluminum hydroxide.
  • Such mortars and concretes are due to the accelerated solidification and hardening particularly well suited as sprayed mortar and concrete.
  • EP 0 946 451 B1 discloses solidification and hardening accelerators in dissolved form for hydraulic binders, which can be mixed more easily with the concrete when spraying the concrete.
  • Such a solidification and hardening accelerator consists, inter alia, of aluminum hydroxide, aluminum salts and organic carboxylic acids. From WO 03/106375 A1, solidification and hardening accelerators are known which contain at least aluminum sulfate, alkanolamine and hydrofluoric acid.
  • WO 2005/075381 A1 describes a solidification
  • a hardening accelerator comprising aluminum hydroxide, aluminum sulfate and organic acid, wherein the accelerator has a molar ratio of aluminum to organic acid of less than 0.65 and a molar ratio of
  • Aluminum to sulfate of greater than 0.83 has.
  • Shotcrete known wherein the additive comprises the reaction product of aluminum hydroxide and an organic acid, and aluminum sulfate and at least one alkanolamine.
  • the additive preferably contains 16-18
  • Hardening accelerators are also a relatively low early strength in the first few hours and days and the insufficient stability of the solution. Presentation of the invention
  • the invention has for its object to achieve the best possible accelerator with the highest possible stability with the longest possible stability of the accelerator at a solidification and hardening accelerator for hydraulic binders of the type mentioned.
  • Inventive solidification and hardening accelerators for hydraulic binders are fluoride-free and include sulfate, aluminum and and 1 to 16% by weight of organic acid, based on the total weight of the accelerator, with the molar ratio of aluminum to sulfate being less than 0.83.
  • Such accelerators can be produced in various ways.
  • the accelerator is preferably a water-based accelerator which may occur as a solution, with partially finely dispersed particles or as a dispersion.
  • the accelerator according to the invention is alkali and chloride-free. Under an alkali and chloride-free accelerator is used in construction chemistry Usually understood as an accelerator which has less than 1 wt .-% alkali, or alkali metal or chloride ions, based on the weight of the accelerator. In addition, a preferred accelerator according to the invention preferably contains no mineral acid.
  • the abovementioned substances are advantageously to be found as ions in solution, but may also occur in complexed form or undissolved in the accelerator. This is particularly the case when the accelerator occurs as a solution with partially finely dispersed particles or as a dispersion.
  • the accelerator according to the invention comprises from 17 to 35% by weight of sulphate, from 3.2 to 9.5% by weight of aluminum and from 1 to 10% by weight of organic acid. Even more preferred is an accelerator comprising 24 to 29% by weight, preferably 24.5 to 27% by weight, more preferably 24.95 to 27% by weight of sulfate, 4 to 6.5% by weight of aluminum and 2 to 8% by weight. % organic acid, based on the total weight of the accelerator.
  • a particularly suitable accelerator comprises magnesium, preferably in an amount of 0.01 to 6 wt .-%, in particular 0.4 to 3.1 wt .-%, based on the total weight of the accelerator.
  • the accelerator according to the invention may additionally comprise glycehn, preferably in an amount of from 0.1 to 8% by weight, in particular from 2 to 4% by weight, based on the total weight of the accelerator.
  • An inventive fluoride-free solidification and hardening accelerator for hydraulic binders can be prepared, for example, from at least 40 to 60 wt .-% aluminum sulfate (Al 2 (SO 4 ) 3 * 14H 2 O) and 1 to 16 wt .-% of organic acid, based on the total weight of the accelerator, wherein the molar ratio of aluminum to sulfate is less than 0.83.
  • the aluminum sulfate used for the preparation may contain a different amount of water of crystallization.
  • the aluminum sulfate is typically used is aluminum sulfate tetradecahydrate (AI 2 (SO 4) 3 * 14H 2 O). It is also commonly referred to as 17% aluminum sulfate because it contains 17% Al 2 O 3 .
  • the amounts of aluminum sulphate mentioned in this document refer to Al 2 (SO 4 ) 3 .14H 2 O. If the aluminum sulphate contains other amounts of water of crystallization, the amounts of aluminum sulphate required for the present invention are easily calculated. Thus, 40 to 60% by weight of Al 2 (SO 4 ) 3 * 14H 2 O would correspond to an amount of a water-free Al 2 (SO 4 ) 3 of from 23 to 35% by weight.
  • the aluminum sulfate can also be produced by a reaction of aluminum hydroxide with sulfuric acid in the preparation of the accelerator, forming corresponding sulfate ions in the aqueous solution.
  • aluminum sulfate can be produced by a reaction of a basic aluminum compound with sulfuric acid.
  • at least 45 to 55 wt .-% aluminum sulfate (Al 2 (SO 4 ) 3 * 14H 2 O) is used in the preparation of the inventive accelerator. Even more preferred is an amount of over 50% by weight.
  • the molar ratio of aluminum to sulphate must always be less than 0.83.
  • the molar ratio of aluminum to sulfate is less than 0.80, more preferably less than 0.7.
  • the molar ratio of aluminum to the organic acid is preferably greater than 0.67. Particularly preferred is a molar ratio of aluminum to organic acid of more than 1.
  • the organic acid it is preferable to use a carboxylic acid, more preferably a monocarboxylic acid. Particularly preferred is the formic acid, but other equivalent organic acids such as e.g. Acetic acid can be used.
  • the acid is used in an amount of from 1 to 16% by weight, preferably from 1 to 10% by weight, more preferably from 2 to 7% by weight, based on the total weight of the accelerator.
  • the accelerator according to the invention can be produced particularly favorably, since in a particularly preferred embodiment it can be produced without the expensive aluminum hydroxide Al (OH) 3 and is thus free of aluminum hydroxide.
  • Al (OH) 3 the expensive aluminum hydroxide
  • the aluminum hydroxide can be in amorphous or crystalline form can be used.
  • amorphous aluminum hydroxide is used.
  • the aluminum hydroxide may also be used in the form of aluminum hydroxide carbonate, aluminum hydroxysulfate or the like.
  • magnesium hydroxide Mg (OH) 2 preferably in an amount of from 0.1 to 10% by weight, in particular from 1 to 5% by weight, based on the total weight of the accelerator, is additionally used for the preparation .
  • magnesium hydroxide it is also possible to use the corresponding amount of another magnesium compound, in particular a magnesium salt or oxide, for example magnesium oxide MgO, magnesium oxyhydroxide or magnesium carbonate.
  • the accelerator according to the invention may additionally contain alkanolamine during the preparation, preferably in an amount of 0.1-10% by weight, based on the total weight of the accelerator.
  • alkanolamine diethanolamine DEA is advantageously used.
  • At least one further divalent or higher metal sulfate may be used, preferably in an amount of 0.1-5% by weight, based on the total weight of the accelerator.
  • Particularly preferred as another metal sulfate is the manganese (II) sulfate.
  • iron sulfate is also suitable.
  • silica throughout the present specification is understood to mean a silica, in addition to the ortho-silicic acid all Forms of silica, so the anhydride of ortho-silica, the actual silicon dioxide, as well as colloidal, precipitated or fumed silica or silica, counted.
  • the silica used in the accelerator according to the invention is or preferably therefore contains colloidal, precipitated, fumed silica or microsilicic acid (silica fume) or a mixture thereof.
  • particularly suitable silicas are colloidal silica, silica, Aerosil® or Sipernat®.
  • the silica particularly suitable for the present invention has compact or porous particles, typically with a specific surface area of 50-1000 m 2 / g, in particular from 80 to 500 m 2 / g and a particle size in the range of 4 to 1000 nm, in particular from 7 to 500 nm. Particular preference is given to colloidal silica particles, so-called nanoparticles.
  • the silica particles used in the accelerator according to the invention may have a different size distribution. Thus, for example, small and large silica particles can be present together in the accelerator.
  • the silica particles suitable for the present invention may also be waste products obtained, for example, by chemical mechanical polishing (CMP) of silica products.
  • CMP chemical mechanical polishing
  • the surface of the silica particles can also be chemically modified.
  • the content of silicon dioxide, or the solids content of the silica, based on the total weight of the accelerator, is preferably 0.1 to 40% by weight, preferably 1 to 30% by weight, more preferably 3 to 20% by weight, in particular 6 to 15% by weight.
  • the silica is present as a silica dispersion and contains silica particles.
  • water is used as the liquid medium.
  • Silica sol is particularly preferred as the silica dispersion.
  • the silica sol preferably contains colloidal silica, in particular amorphous colloidal silica, having a particle size in the range from 4 to 1000 nm, in particular from 7 to 500 nm.
  • the silica sol has a specific surface area of 50-700 m 2 / g, in particular from 80 to 500 m 2 / g.
  • a silica dispersion is a dispersion with silica.
  • the accelerator of the invention preferably comprises a silica sol having a silica content, based on the total weight of the silica sol, of from 1 to 60% by weight, in particular from 5 to 50% by weight, more preferably from 10 to 40% by weight.
  • the proportion of the silica dispersion, in particular of silica sol, in the accelerator is preferably from 0.1 to 60% by weight, in particular from 5 to 55% by weight, based on the total weight of the accelerator.
  • accelerators which have a proportion of silica sol or of a silica foam dispersion of more than 20% by weight, in particular in a proportion of from 23 to 55% by weight, more preferably in a proportion of from 25 to 40 wt .-%.
  • the accelerator according to the invention may additionally comprise flow agents, in particular polycarboxylates, or stabilizers.
  • the accelerator according to the invention may comprise further suitable additives known to the person skilled in the art.
  • it contains no further thickening agents or thixotropic agents.
  • Hardening accelerator can be prepared from (in% by weight, in each case based on the total weight of the accelerator):
  • magnesium hydroxide 0.1 to 10% by weight of magnesium hydroxide
  • Al 2 (SO 4 ) 3 * 14H 2 O aluminum sulfate (Al 2 (SO 4 ) 3 * 14H 2 O), preferably 51 - 55 wt .-%
  • Al (OH) 3 aluminum hydroxide
  • the silica is present, for example, as a silica dispersion, in particular as silica sol, the water can be completely introduced into the silica dispersion and no additional water must be used in the preparation of the accelerator.
  • an accelerator which contains a small amount of aluminum hydroxide, in particular less than 1% by weight.
  • up to 10% of magnesium hydroxide and / or a corresponding amount of magnesium oxide are used in the preparation of the accelerator.
  • the pure Mg Amount based on the total amount of accelerator is 0 to 6 wt .-%, preferably 0.4 to 4.2 wt .-%, more preferably 0.8 to 2.9 wt .-%, in particular 1, 3 to 2 , 1% by weight.
  • the ratio of aluminum to sulfate is increased by the
  • Sulfate content and lower aluminum content to a value less than 0.83, preferably less than 0.8, in particular set less than 0.7.
  • the aluminum content given as Al 2 O 3 is therefore preferably chosen to be less than 14%, more preferably less than 13% and in particular less than 12% Al 2 O 3 .
  • magnesium hydroxide and / or oxide is used in the preparation of the accelerator, the temperature of the mixture increases so much due to the strong reaction of the magnesium hydroxide and / or oxide with the organic acid that the water does not have to be heated for these mixtures.
  • the other components are then added to this heated mixture.
  • the components can also be added in any other order. This simplifies the process and requires less energy.
  • An additional advantage of the use of magnesium is the significantly higher storage stability of the accelerators caused by the magnesium ions. Even at a content of 1 wt .-% of magnesium hydroxide in the production is a good Shelf life achieved. At higher levels, storage stability is at least three months.
  • the stability of the accelerators is positively influenced by the reduced amount of aluminum. Due to the reduced amount of aluminum or the reduced ratio of aluminum to sulfate and the sulfate resistance is increased.
  • the accelerators according to the invention can be present, for example, as a solution, dispersion or in powder form, it being preferred that an accelerator present as a powder is dissolved or dispersed in water before use.
  • the present invention relates to a method for accelerating the solidification and hardening of hydraulic binders and mortar or concrete produced therefrom, characterized in that the mixture containing hydraulic binder, a fluoride-free solidification and hardening accelerator according to the invention in an amount of 0.1 to 15 wt .-%, in particular from 1 to 10 wt .-%, based on the weight of the hydraulic binder, is added.
  • the inventive accelerator can accelerate the setting and hardening of hydraulic binders, hydraulic
  • Fillers mortar or concrete can be used. A preferred type of fillers, mortar or concrete can be used.
  • binders their hardening and setting by the accelerator according to the invention, respectively. the process can be accelerated are cement such as blended cements, lime, hydraulic lime and gypsum, each alone or in admixture with latent hydraulic binders or inert fillers, and examples of blends containing these binders are mortar and concrete, especially sprayed mortar and shotcrete ,
  • Another object of the present invention is also a curable resp. hardened binder-containing mixture containing the accelerator according to the invention, in particular sprayed mortar and shotcrete containing the inventive accelerator.
  • solidification and hardening accelerators By using the solidification and hardening accelerators according to the invention, an extremely rapid setting of the corresponding binders or of the mixtures containing such binders is effected, and high initial and final strengths are achieved.
  • the setting and hardening accelerators are not corrosive or toxic to the processor or the environment.
  • Table 2 shows the molar ratios of aluminum to sulfate and of aluminum to the organic acid, here formic acid, of the samples measured.
  • the values of the molar ratios of aluminum to organic acid are above 0.67, the values of the molar ratios of aluminum to sulfate below 0.83. Further, the aluminum content of the various examples is given.
  • Table 3 Strengths in MPa and storage stability in days; in Examples A1 to A8 and B1 and B2, the storage stability was not measured. In Comparative Example B3, the strength could not be measured because the accelerator precipitated in the production.
  • accelerators with magnesium hydroxide are especially suitable.
  • This accelerator could be obtained with a particularly good storage stability, while accelerators without magnesium hydroxide, although good
  • a suitable accelerator contains less than 16% by weight, in particular less than 10% by weight, of formic acid, based on the total weight of the accelerator.
  • Comparative Example B3 which contains 17 wt .-% of formic acid (or 20 wt .-% of an 85% formic acid) more than 16 wt .-% formic acid, precipitated in the preparation and could not be used as an accelerator.
  • Comparative Example B1 without acid shows in particular less good early strength after 6 hours or 1 day compared with the accelerators according to the invention.
  • Example A18 with 11.9 wt .-% formic acid (or 14 wt .-% of an 85% formic acid) shows good strength values, but was stable only about 1 week.
  • examples A16 and A17 with 1.7% by weight (or 2% by weight of an 85% formic acid) or 6.8% by weight of formic acid (or 8% by weight of an 85% formic acid) show good strength values
  • silica sol in the accelerator causes the accelerator to have both good strength values (Example A27) and, in addition, a better storage stability (see in particular Example A28 compared to A17)

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Catalysts (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

L'invention concerne un accélérateur de prise et de durcissement exempt de fluorure, destiné à des liants hydrauliques, contenant du sulfate, de l'aluminium et de l'acide organique, le rapport molaire de l'aluminium sur le sulfate étant inférieur à 0,83.
EP08716832A 2007-02-13 2008-02-13 Accélérateur de prise et de durcissement pour des liants hydrauliques et procédé de fabrication Withdrawn EP2121541A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP08716832A EP2121541A1 (fr) 2007-02-13 2008-02-13 Accélérateur de prise et de durcissement pour des liants hydrauliques et procédé de fabrication

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP20070102295 EP1964824A1 (fr) 2007-02-13 2007-02-13 Accélérateur de prise et de durcissement pour liant hydraulique et son procédé de fabrication
EP08716832A EP2121541A1 (fr) 2007-02-13 2008-02-13 Accélérateur de prise et de durcissement pour des liants hydrauliques et procédé de fabrication
PCT/EP2008/051742 WO2008098961A1 (fr) 2007-02-13 2008-02-13 Accélérateur de prise et de durcissement pour des liants hydrauliques et procédé de fabrication

Publications (1)

Publication Number Publication Date
EP2121541A1 true EP2121541A1 (fr) 2009-11-25

Family

ID=38091767

Family Applications (2)

Application Number Title Priority Date Filing Date
EP20070102295 Withdrawn EP1964824A1 (fr) 2007-02-13 2007-02-13 Accélérateur de prise et de durcissement pour liant hydraulique et son procédé de fabrication
EP08716832A Withdrawn EP2121541A1 (fr) 2007-02-13 2008-02-13 Accélérateur de prise et de durcissement pour des liants hydrauliques et procédé de fabrication

Family Applications Before (1)

Application Number Title Priority Date Filing Date
EP20070102295 Withdrawn EP1964824A1 (fr) 2007-02-13 2007-02-13 Accélérateur de prise et de durcissement pour liant hydraulique et son procédé de fabrication

Country Status (10)

Country Link
US (1) US8221543B2 (fr)
EP (2) EP1964824A1 (fr)
JP (1) JP2010517923A (fr)
CN (1) CN101605737B (fr)
AU (1) AU2008214598A1 (fr)
BR (1) BRPI0807674A2 (fr)
CA (1) CA2677778C (fr)
CL (1) CL2008000453A1 (fr)
MX (1) MX2009008651A (fr)
WO (1) WO2008098961A1 (fr)

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CN112521123B (zh) * 2020-12-26 2022-04-01 南京航空航天大学 一种碱式硫酸镁水泥泡沫混凝土保温材料的制备方法

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BRPI0807674A2 (pt) 2014-05-20
AU2008214598A1 (en) 2008-08-21
CA2677778C (fr) 2015-03-31
CN101605737B (zh) 2013-04-17
US8221543B2 (en) 2012-07-17
CN101605737A (zh) 2009-12-16
WO2008098961A1 (fr) 2008-08-21
US20100018440A1 (en) 2010-01-28
EP1964824A1 (fr) 2008-09-03
CL2008000453A1 (es) 2008-11-07
CA2677778A1 (fr) 2008-08-21
MX2009008651A (es) 2009-09-11
JP2010517923A (ja) 2010-05-27

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