CN1571826A - Sealing composition and its use - Google Patents

Sealing composition and its use Download PDF

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Publication number
CN1571826A
CN1571826A CNA028204824A CN02820482A CN1571826A CN 1571826 A CN1571826 A CN 1571826A CN A028204824 A CNA028204824 A CN A028204824A CN 02820482 A CN02820482 A CN 02820482A CN 1571826 A CN1571826 A CN 1571826A
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China
Prior art keywords
sealing compositions
silicon sol
purposes
composition
jelling agent
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Granted
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CNA028204824A
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Chinese (zh)
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CN1264950C (en
Inventor
P·格林伍德
I·简森
U·斯卡普
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Nouryon Chemicals International BV
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Akzo Nobel NV
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Publication of CN1571826A publication Critical patent/CN1571826A/en
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Publication of CN1264950C publication Critical patent/CN1264950C/en
Anticipated expiration legal-status Critical
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    • 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
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/12—Materials for stopping leaks, e.g. in radiators, in tanks
    • 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
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
    • 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
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00732—Uses not provided for elsewhere in C04B2111/00 for soil stabilisation
    • 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
    • C04B2111/70—Grouts, e.g. injection mixtures for cables for prestressed concrete

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Soil Conditioners And Soil-Stabilizing Materials (AREA)
  • Sealing Material Composition (AREA)
  • Consolidation Of Soil By Introduction Of Solidifying Substances Into Soil (AREA)

Abstract

The present invention relates to the use of a sealing composition for sealing rock or soil, wherein the sealing composition is obtainable by mixing a silica sol and at least one gelling agent, wherein the silica sol has an S-value higher than about 72%. The invention also relates to a method for cutting off a liquid flow in a leaking part or cavity by inserting the sealing composition. The invention also relates to a method for preparing the sealing composition and a composition obtainable from the method.

Description

Sealing compositions and its purposes
The present invention relates to be used to seal the application of the composition of rock and soil.The invention still further relates to a kind of mobile method of liquid that be used for cutting off in leakage part or chamber.The invention still further relates to a kind of method that is used to prepare sealing compositions and a kind of sealing compositions that can obtain by this method.
Background of invention
The requirement and the performance that are used to seal the composition of rock and soil increase as time passes.These requirements relate to improved environment and technical elements.In the past, comprised that the various plastics of toxicant and polymkeric substance be used to sealing as concrete works, the tunnel, or the water in the chamber that forms on the back side of concrete works leaks.These sealing chemical cause phreatic pollution in many cases and are for example used their arrangement works person to bring health problem.But attempted substituting disporduct with the material that is more suitable for environment.Also seek product innovation to satisfy the limit leakage of regulation recently.In some cases, be lower than the 1 liter/water levels of leakage of (100 meters of minute *) and become the upper-level threshold of tunnel structure position.This forces supplier that technical improved sealing prod is provided.US 5,396, and 749 have described and a kind ofly are used to cut off the method for current by grouting, prevent from like this to be leaked and ground caves in and makes troubles by water.Cut off agent by mixing, inorganic salt and water soluble amino ethyl formate polymkeric substance and make as colloidal silica.
But the intensity of these reagent especially shows deficiency when this reagent is exposed to high hydraulic pressure in injection and gelatinization process in several occasions.Especially unsettled reagent causes quite low later strength in the aging step process.Sealing agent is used in addition seal soil in case subterranean zone such as buried source, and the pollution of junk pile etc. is leaked.US 5,836, and 390 have described a kind of method that forms subsurface barrier, and wherein injection comprises as polybutene the thick liquid of polysiloxane and colloidal silica.
Need provide a kind of liquid that especially in the occasion of sealing rock, has the suitable environment of high later strength to cut off agent, wherein cut off agent and can stand from phreatic high hydraulic pressure.Also need to provide the tolerance scouring force and have low-permeability, promptly to water and the impermeable dutiable goods of other liquid.
An object of the present invention is to provide these products that solve above-mentioned prior art defective.
Summary of the invention
The present invention relates to be used to seal the application of the sealing compositions of rock or soil, described sealing compositions can mix and obtains by the S-value being higher than about 72% silicon sol and at least a jelling agent.
The invention still further relates to a kind of method that is used for cutting off the liquid-flow of revealing part or chamber, wherein can mix the sealing compositions that obtains and be injected into and reveal partly or the chamber by S-value being higher than about 72% silicon sol and at least a jelling agent.
The invention still further relates to a kind of method that is used to prepare sealing compositions, comprise the S-value being higher than about 72% silicon sol and at least a jelling agent mixes.The invention still further relates to a kind of sealing compositions that can obtain by this method.
Unexpectedly find to have high S-value, promptly the S-value is higher than about 72% silicon sol and can gives high later stage gel-strength to sealing compositions.Term used herein " gel-strength " is shearing that the gelling sealing compositions was produced along with the time and a kind of tolerance of compressive strength.High later strength provides durable sealing.Find that in addition sealing compositions according to the present invention has low-permeability, this means good sealing characteristics.
" S-value " characterizes silica granule accumulative degree in silicon sol, i.e. the degree of aggregate or microgel formation.The S-value of silicon sol is according to ller, R.K.﹠amp; Dalton, R.L. are in J.Phys.Chem.60 (1956), and the formula that provides among the 955-957 is measured and calculated.
The S-value depends on the silica content of silicon sol, viscosity, and density.The humble gel content of high S-value representation.The S-value representation is present in the SiO in the disperse phase of silicon sol 2Amount, % weight.The microgel degree can be controlled in the production process of silicon sol, for example is further described in as US5368833.
According to a preferred embodiment of the invention, it is about 73% that the S-value is higher than, and preferably is higher than approximately 74%, even more preferably is higher than about 75%.Preferably, the S-value is lower than about 90% and most preferably be lower than about 85%.
Silicon sol comprises and has the about 150nm of the about 3-of average particulate diameter suitably, about 50nm of preferably about 12-and the silica granule of the about 40nm of 12-most preferably from about.Suitably, it is about 900 that silica granule has an about 20-of specific surface area, preferably about 40-about 230 and the about 220m of 60-most preferably from about 2/ g.The about suitably 1-of the density of silicon sol is about 1.6, preferably about 1.1-about 1.5 and the about 1.4kg/m of 1.2-most preferably from about 3
Silicon sol is monodispersed basically suitably, promptly has narrow as far as possible particle size distribution.Suitably, silica granule has and is lower than about 15% number, preferably is lower than 10% number and most preferably is lower than the relative standard deviation of the particle size distribution of about 8% number.The relative standard deviation of particle size distribution is the ratio between the standard deviation of number average particle size particle size and particle size distribution.The silica granule of silicon sol is suitably at stabilization positively charged ion such as K +, Na +, Li +, NH 4 +Or be dispersed in the water under the existence of analogue or its mixture.But also can use other dispersion such as organic solvent, as lower alcohol, acetone or its mixture.The about suitably 1-of the pH of dispersion is about 12, preferably about 7-about 11.As long as it is stable that silicon sol keeps, promptly basically without any assembling or gelling, high silica content is preferred in silicon sol.Consider the technical feature of highly spissated silicon sol excellence and the transmission cost of its reduction, this is useful.According to an embodiment, these compositions, promptly silicon sol and jelling agent separately add the point of application that will seal.This can carry out as utilizing so-called jet grouting, and each composition scene wherein is as mixing in soil.
Term " silicon sol " and " silica granule " also mean at this and comprise as the silica granule of aluminium modification and the silica granule and the colloidal sol of colloidal sol and boron modification.The silicon sol of boron modification is described in as US2, and 630,410.Sometimes the silicon sol of aluminium modification that also is called the silicon sol of aluminate modification can be by with the aluminate ion Al (OH) of appropriate amount 4 -Stir and heating under add in the conventional non-modified silicasol and make.Suitably, use corresponding to about 0.05-about 2, the about 2Al atom/nm of preferably about 0.1- 2The rare sodium aluminate or the potassium aluminate solution of the aluminium modification value of silica granule surface-area.The silica granule of aluminium modification comprises aluminate ion insertion or exchange, produces to have the fixedly silico-aluminate position of negative surface charge.The pH of the silicon sol of aluminium modification can preferably utilize ion exchange resin to regulate, and it is about 11 to be adjusted to the about 3-of pH suitably, preferably about 4-about 10.The silica granule of aluminium modification has Al suitably 2O 3The about 3wt% of the about 0.05-of content, the about 2wt% of preferably about 0.1-.The step of the silicon sol of preparation aluminium modification is further as being described in " silica chemistry ", lIer, K.Ralph, number of pages 407-409, JohnWiley﹠amp; Sons (1979) and US 5 368 833.
Jelling agent is inorganic salt or acid suitably, organic salt such as sodium acetate, or acid is as acetate, but preferred inorganic salt such as Repone K, calcium chloride, sodium-chlor, magnesium chloride, sal epsom, potassiumiodide, magnesium nitrate, SODIUMNITRATE, saltpetre, nitrocalcite and water glass or its mixture, preferably calcium chloride, sodium-chlor or Repone K and sodium-chlor most preferably, sodium aluminate.
Gel time conditioning agent such as acid triactin (triacetin), glyceryl diacetate, Glauber ' s salt (NaSO 4* 10H 2O), sulfuric acid, phosphoric acid or its mixture also can be added into sealing compositions to control its gelling.
Term used herein " gel time " be meant when the composition that constitutes sealing compositions mixes, begin until the sealing composition become too thickness and can not move or time that is inserted into the leak point institute's elapsed time value.Viscosity is controlled the even matter that make to form said composition suitably and is moved front end, moves to the direction of the point that will seal.Suitably, the initial viscosity of sealing compositions is that about 3-is about 100, the about 30mPas of preferably about 4-.Gel time can be controlled by the amount of regulating jelling agent easily.Sometimes, gelling immediately and need not obviously dilute said composition obtains agglomerative pressure-resistant seal composition.Short gel time is in when underground relatively and is optimal under the situation that sealing compositions might be diluted rapidly in the crack.In some cases, the particularly important is for the crack, gelling does not begin before preferably should not infiltrating this crack fully at the front end of the composition that is inserted.Usually, the gel time when rock seals is that about 1-is about 120, and preferably about 2-is about 60, more preferably from about 5-about 40 and most preferably from about about 20 minutes of 5-.When soil seals, gel time normally about 5 minutes-Yue 24 hours, preferred about 10 minutes-Yue 6 hours and most preferably from about 15 minutes-Yue 3 hours.
Each composition can mix at ambient temperature.Jelling agent is suitably with the about 30wt% of the about 1-of concentration, and the aqueous solution of the about 15wt% of preferably about 2-adds in the silicon sol.Wherein adding the silicon sol that jelling agent is arranged suitably, to have the about 1-of silica content suitably about 70, preferably about 20-about 60 and the about 50wt% of 35-most preferably from about.High silica content in the silicon sol is favourable owing to the transmission cost that reduces silicon sol in many cases.
The about suitably 1-of silica content in the sealing compositions is about 60, preferably about 15-about 50 and the about 45wt% of 30-most preferably from about.But high silica content minimize retraction rate and maximization later strength.The weight ratio of silica and jelling agent depends on that the applied field merging can change along with the application scenario.Suitably, silica granule: the jelling agent weight ratio is about 400: about 10: 1 of 1-, preferred about 200: about 20: 1 of 1-.
Gelatinization agents content in the sealing compositions can change according to the kind of used jelling agent.But gelatinization agents content about 0.1-of composition suitably is about 10, the about 5wt% of preferably about 0.2-.If sodium-chlor is as jelling agent, this content about 0.2-of composition suitably is about 5, preferably about 1-about 3 and the about 2wt% of 1.5-most preferably from about.If calcium chloride is as jelling agent, this content about 0.1-of composition suitably is about 2, preferably about 0.2-about 1 and the about 0.5wt% of 0.25-most preferably from about.
According to preferred embodiment, sealing compositions is revealed part or the chamber is inserted by silicon sol is injected separately, and sealing compositions scene like this is as forming in the crack of rock or in the chamber of soil.Therefore jelling agent also can be injected into separately and reveal part or chamber.This can for example be undertaken by injecting the sealing composition simultaneously, for example makes jelling agent and silicon sol to be injected into simultaneously by the parallel placement of injection nozzle that will be used for silicon sol and jelling agent and need not premix.But reveal part or chamber at some, as in soil, for example Already in the soil, its amount makes and need not to add further jelling agent to form sealing compositions the jelling agent of salt form.Therefore, in a preferred embodiment of the invention, only silicon sol is injected into separately and is revealed part or chamber.This method is generally cut off as the water and the aqueous solution, any liquid-flow of organic solution etc., but this method mainly is fit to cut off flowing of the water and the aqueous solution.
The sealing composition also can utilize other method such as jet grouting and be inserted into and reveal part or chamber, and wherein at least a portion material of constituting this leakages part or chamber is removed to add sealing compositions and to be reset to than removed same point morning with the sealing compositions that adds wherein subsequently.This method preferably is applicable to sealing soil.
According to a preferred embodiment, silicon sol and jelling agent mixed before injection immediately.In this article, word " immediately " was meant about 0-about 30 seconds, about 15 seconds of preferably about 0-.The so-called on-line mixing of the mode of each composition of this blend compositions.
According to a preferred embodiment, sealing compositions also can prepared beforehand also use in 60 minutes and preferred 30 minutes before inserting composition in batch technology suitably.But the mode of this preparation sealing compositions needs a kind of sufficiently stable sealing compositions, makes it can be stored before inserting and does not have remarkable gelling.About suitably 1 minute-Yue 1 hour inject time of sealing compositions, preferred about 5 minutes-Yue 30 minutes.Injection/depth of penetration changes along with the leak that will seal certainly.But about 50 meters of methods of the present invention for about 0.5-, the degree of depth particularly advantageous that preferably about 5-is about 30 meters.About 50 crust of the about suitably 1-of injection pressure, about 25 crust of preferably about 2-.
The sealing composition is applicable to that mainly providing impermeable bed to be used for anti-sealing leaks under the face of land.The sealing of rock comprises inserts for example chamber such as microfracture with sealing compositions, and the underground water that is particularly useful in control example such as the tunnel leaks.The diameter that typically refers to the chamber by term " microfracture " is lower than 20 μ m.Because the diameter of the silica granule in the silicon sol is the about 100nm of about 10-, the sealing compositions that comprises these silica granules is applicable to certainly and is injected in the microfracture.
The present invention now describes, but it obviously can change according to many modes.These variations are not considered to deviate from the spirit and scope of the invention, and all these changes that it will be apparent to those skilled in the art mean in the scope that is included in claims.Following examples further specify how the present invention can carry out rather than to the qualification of its scope.
Embodiment 1
Sealing compositions is by the preparation of the salts solution of 1.7M sodium-chlor, and the latter under agitation adds in the different silicon sol product that 200g defines in following table.The add-on of the salts solution in all compositions is a 40g solution.Composition is worn out the highest 672 hours with assessment later stage shearing resistance.In table 1, one group of composition is exposed to 55 ℃ increase temperature and another group is exposed to pH12 to quicken the aging of sealing compositions.The calculating of the particle diameter of silica granule is undertaken by the Sear ' s method that is used for calculated specific surface area.Shear strength test uses awl experimental evidence Svensk Standard SS 02 71 25 to carry out.
In addition, measure the compressive strength of sealing compositions.This can be undertaken by compression testing, and usage load frame wherein has the pressure head of the diameter identical with sample, load cell (wherein sample is placed between load cell and the pressure head) with plane surface, displacement transducer, battery power data recorder, signal processing software.The load frame orders about pressure head and moves in vertical direction.The type of frame with in machine works, be used to control the identical of vertical drilling machine.Load is controlled by weight, and weight bears a heavy burden load head and without any transmitting (deadweight).Pressure head is made up of the rigidity steel cylinder with 50mm diameter.Load cell has the capacity of 300kg.Load cell forms a plane surface.Sample is between load cell and pressure head.The tolerance range of load cell is within 0.1kg.Displacement transducer has stroke capacity 5mm.The error of actual transmodulator is tested to maximum 0.4% by manufactory.Develop and be used for the test for data register to monitor the vibration and the distortion of conditioning process at the scene.Register is monitoring continuously in process of the test.Compression testing is only carried out at solidified sample in 28 days.Mould cylinder size is 50mm diameter and 25mm height.The mould cylinder is arranged in and has flat jar.Pour the upper end of sealing compositions subsequently into to cylinder.All samples solidify under pH10 in 20 ℃ of water-baths.Only cross section is exposed to water.Before test, sample is separated from the mould cylinder.
Table 1
The composition that uses following colloidal sol to make: Particle diameter (nm) The S-value Surface-area (m based on product 2/g) Shearing resistance (kPa), 55 ℃, pH 10,672h Shearing resistance (kPa), 20 ℃, pH12,672h
Colloidal sol 1 ????17 ????77 ????68 ????326 ????-
Colloidal sol 2 ????12 ????76 ????88 ????640 ????475
Colloidal sol 3 ????11 ????70 ????100 ????218 ????-
Colloidal sol 4 ????7 ????70 ????108 ????250 ????70
Colloidal sol 5 ????5 ????45 ????75 ????48 ????39
In table 1 as can be seen, envrionment temperature and at pH12 (expedite product aging) down and under pH10 and temperature 55 ℃ (also causing weathering process faster), by having the sealing compositions made according to the silicon sol of S-value of the present invention and comparing after 672 hours and cause than high-gel strength by contrasting composition that silicon sol 3-5 makes.
Table 2
The composition that uses following colloidal sol to make: Particle diameter (nm) The S-value Surface-area (m based on product 2/g) Compressive strength (kPa)/maximum load
Colloidal sol 6 ????35 ????90 ????40 ????48
Colloidal sol 1 ????17 ????77 ????68 ????50
Colloidal sol 2 ????12 ????76 ????88 ????45
Colloidal sol 3 ????11 ????70 ????100 ????11
Colloidal sol 5 ????5 ????45 ????75 ????11
In table 2, as can be seen, be higher than compressive strength by the sealing compositions made of contrast silicon sol 3 and 5 by having the seal combination deposits yields of making according to the silicon sol of S-value of the present invention.

Claims (14)

1. be used to seal the purposes of the sealing compositions of rock or soil, wherein said sealing compositions can mix and obtains by the S-value being higher than about 72% silicon sol and at least a jelling agent.
2. by sealing compositions insert being revealed the method that part or chamber are used for cutting off the liquid-flow of revealing part or chamber, described sealing compositions can obtain by S-value being higher than about 72% silicon sol and the mixing of at least a jelling agent.
3. mix the method that is used to prepare sealing compositions by the S-value being higher than about 72% silicon sol and at least a jelling agent.
4. according to the method for claim 3, wherein silicon sol and jelling agent are on-the-spot by separately silicon sol being injected described leakage part or chamber mixes in leakage part or chamber.
5. can mix the sealing compositions that obtains by the S-value being higher than about 72% silicon sol and at least a jelling agent.
6. according to the purposes of claim 1, according to the method for claim 2-4, according to the sealing compositions of claim 5, wherein the S-value is higher than about 75%.
7. according to the purposes of claim 1 or 6, according to claim 2-4,6 each methods, according to the sealing compositions of claim 5-6, wherein silicon sol is the silicon sol of aluminium modification.
8. according to any claim 1, the purposes of 6-7, according to claim 2-4, each method of 6-7, according to each sealing compositions of claim 5-7, wherein composition has the about 50wt% of the about 35-of silica content.
9. according to claim 1, each purposes of 6-8, according to claim 2-4, each method of 6-8, according to each sealing compositions of claim 5-8, wherein jelling agent is selected from Repone K, sodium-chlor, calcium chloride, magnesium chloride, magnesium nitrate, sal epsom or its mixture.
10. according to any claim 1, each purposes of 6-9, according to claim 2-4, each method of 6-9, according to each sealing compositions of claim 5-9, wherein composition has the relative standard deviation of the particle size distribution that is lower than about 15% number.
11. according to any claim 1, each purposes of 6-10, according to claim 2-4, each method of 6-10, according to each sealing compositions of claim 5-10, wherein composition has the about 5wt% of the about 0.2-of gelatinization agents content.
12. according to claim 1, each purposes of 6-11, according to claim 2-4, each method of 6-11, according to each sealing compositions of claim 5-11, wherein silicon sol comprises and has the about 230m of the about 40-of specific surface area 2The silica granule of/g.
13. according to claim 1, each purposes of 6-12, according to claim 2-4, each method of 6-12, according to each sealing compositions of claim 5-12, wherein composition has the weight ratio about 400 of silica granule and jelling agent: about 10: 1 of 1-.
14. according to claim 1, each purposes of 6-13, according to claim 2-4, each method of 6-13, according to each sealing compositions of claim 5-13, wherein composition comprises the silica granule with size Yue-Yue 12-50nm.
CNB028204824A 2001-10-18 2002-09-23 Sealing composition and its use Expired - Fee Related CN1264950C (en)

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JP4243337B2 (en) 2009-03-25
AU2002337551B2 (en) 2005-07-28
CA2463638C (en) 2009-02-03
MY131479A (en) 2007-08-30
CN1264950C (en) 2006-07-19
NZ532133A (en) 2005-09-30
CA2463638A1 (en) 2003-04-24
BR0213278B1 (en) 2012-09-18
KR100543613B1 (en) 2006-01-20
KR20030032847A (en) 2003-04-26
BR0213278A (en) 2004-10-26
ZA200402800B (en) 2005-06-29
NO20042047L (en) 2004-07-13
WO2003033618A1 (en) 2003-04-24
EP1436357A1 (en) 2004-07-14
JP2005505680A (en) 2005-02-24
HK1071394A1 (en) 2005-07-15
AR036828A1 (en) 2004-10-06

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