EP1414753A2 - Verfahren zur regenerierung verbrauchter halogenidhaltiger flüssigkeiten - Google Patents

Verfahren zur regenerierung verbrauchter halogenidhaltiger flüssigkeiten

Info

Publication number
EP1414753A2
EP1414753A2 EP02721386A EP02721386A EP1414753A2 EP 1414753 A2 EP1414753 A2 EP 1414753A2 EP 02721386 A EP02721386 A EP 02721386A EP 02721386 A EP02721386 A EP 02721386A EP 1414753 A2 EP1414753 A2 EP 1414753A2
Authority
EP
European Patent Office
Prior art keywords
fluid
acid
halide
alkali
used halide
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.)
Granted
Application number
EP02721386A
Other languages
English (en)
French (fr)
Other versions
EP1414753B9 (de
EP1414753B1 (de
Inventor
Raymond D. Symens
Lyle H. Howard
Thomas William Polkinghorn
Surendra Kumar Mishra
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.)
Tetra Technologies Inc
Tetra Tech Inc
Original Assignee
Tetra Technologies Inc
Tetra Tech Inc
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 Tetra Technologies Inc, Tetra Tech Inc filed Critical Tetra Technologies Inc
Publication of EP1414753A2 publication Critical patent/EP1414753A2/de
Application granted granted Critical
Publication of EP1414753B1 publication Critical patent/EP1414753B1/de
Publication of EP1414753B9 publication Critical patent/EP1414753B9/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • E—FIXED CONSTRUCTIONS
    • E21—EARTH OR ROCK DRILLING; MINING
    • E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B21/00—Methods or apparatus for flushing boreholes, e.g. by use of exhaust air from motor
    • E21B21/06—Arrangements for treating drilling fluids outside the borehole
    • E21B21/068—Arrangements for treating drilling fluids outside the borehole using chemical treatment

Definitions

  • the present invention relates to a method for regenerating used halide fluids. More specifically the invention relates to enhancing used halide fluids by removing impurities, increasing the density of the halide fluid, and increasing the concentration of electrolytes and adjusting the true crystallization temperature of the fluid.
  • Brine fluids are expensive to produce. Due to the high amounts of chlorides, bromides and, in some brines, zinc that are present in the used fluids, the disposal of used clear brine fluids is also very costly. It is highly desirable that a used halide fluid.
  • the zinc ions from a brine containing zinc bromide or zinc chloride will start precipitating as zinc hydroxide at a slightly acidic or alkaline pH.
  • the density of the solution that is being regenerated will drop substantially.
  • the changes in the density also changes the TCT of the fluid, so that the fluid is unable to meet the specification set by the needs of the oil field for TCT value of the fluid.
  • Using the methods of evaporation or blending to increase density or to adjust the TCT is time consuming, expensive and difficult to control.
  • the present invention relates to an innovative method for regeneration of used halide fluids that have been recuperated from industrial processes such as oil and gas drilling, agricultural chemical processes, metal plating or water treatment facilities.
  • Used halide fluids, bromide or chloride brines for example are usually contaminated with soluble and insoluble impurities.
  • these recuperated, used fluids typically have a density greater than 9.0 lbs/gal but less than the required density of a desired drilling fluid.
  • one preferred method of regeneration of a used halide fluid comprising soluble and insoluble impurities and having a density greater than 9.0 lbs/gal comprises adding an acid to the used halide fluid.
  • the used halide fluid is then contacted with a halogen, bromine for example, to increase fluid density and oxidize impurities.
  • a halogen- generating species such as oxyhalogen salts, hypochloride, hypobromide and the like can be used to increase density, adjust TCT and oxidize impurities.
  • the used halide fluid if comprising a high solid content, should be filtered to remove the solids prior to acidification. .
  • a reducing agent can be added to convert halogen to halide ion while maintaining the temperature at a minimum of 10°C.
  • the fluid is then contacted with an alkali to neutralize any excess acid. Any suspended solid impurities remaining can be separated from the fluid.
  • the pH can be maintained within a range of approximately 0.0 to 5.5.
  • the alkali and alkali earth metal cations this range can be from 0.0 to 10.0.
  • the acid used for acidification can comprise hydrobromic acid.
  • the acid can comprise hydrochloric acid or an organic acid.
  • the reducing agent is preferably selected from a group consisting of anhydrous ammonia, sulfur, hydrogen sulfide, sodium bisulfide, metallic zinc, metallic iron, metallic copper, metallic nickel, metallic cadmium, metallic cobalt, metallic aluminum, metallic chromium, metallic manganese, organic acids, alcohols and aldehydes.
  • the electrolyte to be enhanced in the used fluid is an alkali metal, an alkali earth metal or a base metal. If the alkali earth metal is calcium, the alkali used to neutralize excess acid can be calcium hydroxide or calcium oxide. Alternatively, if the alkali earth metal in the used fluid is strontium, the alkali used to neutralize excess acid is preferably strontium hydroxide or strontium oxide.
  • the alkali used to neutralize excess acid is an alkali metal hydroxide, sodium hydroxide or potassium hydroxide for example.
  • Anhydrous ammonia can also be used to neutralize excess acid.
  • the alkali used to neutralize excess acid is a base metal hydroxide or base metal oxide, such as zinc hydroxide, zinc oxide, copper hydroxide or copper oxide.
  • the alkali used to neutralize excess acid is aluminum hydroxide or aluminum oxide, manganese hydroxide or manganese oxide, chromium hydroxide or chromium oxide.
  • One embodiment of the method for regeneration of used halide fluids comprising soluble and insoluble impurities comprises the steps of: a) determining density of the used halide fluid; b) analyzing chemical composition, the suspended solids content and the oil and grease content of the used halide fluid; c) separating the suspended solids and oil and grease; d) adding acid to the used halide fluid; e) contacting the used halide fluid with halogen or halogen- generating species to increase fluid density and oxidize impurities; f) adding a reducing agent while maintaining the temperature at a minimum of 10°C; g) contacting the fluid with an alkali to neutralize excess acid; h) separating any suspended solid impurities from the fluid.
  • the recuperated used halide fluid is piped into a reactor after density and chemical composition have been determined according to steps (a) and (b).
  • the acid, halogen, reducing agent and alkali can be piped into reactor along with the fluid.
  • the acid, halogen, reducing agent and alkali can be transported separately to the reactor. Bromine is one preferred halogen used in regeneration.
  • Another preferred method regenerates a used halide fluid comprising a blend of a group of halide salts, such as calcium chloride, calcium bromide, zinc bromide or a combination thereof.
  • the starting brine fluid will typically have a density greater than 9.0 lbs/gal.
  • This method comprises the steps of (1) adding acid to the used halide fluid so that the pH is within a range of approximately 0.0 to 5.5 for a base metal or 0 to 10.0 for alkali and alkali earth metal systems; (2) contacting the used halide fluid with bromine to increase the density to at least 10.0 Ibs./gal. and oxidize soluble impurities; (3) adding a reducing agent while maintaining the temperature at a minimum of 10°C; (4) contacting the fluid with an alkali to neutralize excess acid; and (5) separating any suspended solid impurities from the fluid.
  • the Figure is a schematic of one embodiment of the method of the invention.
  • the present invention relates to an innovative method for regeneration of used halide fluids.
  • the used halide fluids calcium or zinc brine for example, have been recuperated from industrial processes such as oil and gas drilling, agricultural chemical processes, metal plating or water treatment facilities.
  • the recuperated halides often contain soluble and insoluble impurities and can be so diluted that the density of the halides and concentrations of the electrolytes are not acceptable for continued industrial operations.
  • 17. for the purpose of illustration, reference hereafter is made, for convenience, to brine fluids used in oil and gas drilling without limiting the scope of the invention. Clear brine fluids used in deep oil and gas wells become diluted due to the increased concentration of water in the operations system.
  • a used halide fluid 60 such as a drilling fluid
  • a halide fluid has a specific density targeted to the type of drilling operation and/or pressure of the well.
  • Clear brines used as completion, workover and drilling fluids comprise a density higher than the density of water, 8.3 lbs/gal, typically within a range of approximately 11.4 lbs/gal to 16 lbs/gal, and even possibly as high as 23.0 lbs/gal depending on the targeted use of the brine.
  • Electrolytes of alkali metals, alkali earth metals and base metals are commonly used in the composition of these brine fluids and are often selected according to their ability to increase the density of the drilling fluid.
  • the density of the used drilling fluids is restored to a density that is necessary for well operations thereby regenerating the fluid to its useful state.
  • the practice of this invention also allows for the adjustment of the true crystallization temperature (TCT) of the fluid.
  • TCT true crystallization temperature
  • the operator of the production wells checks the specifications for the TCT of the electrolytes within the fluids being used. These precipitates adversely affect the properties of the fluid that are desirable for the oil and gas industries.
  • the Figure illustrates used fluid 60 piped into a reactor 10.
  • the composition and density of the used halide fluid 60 determines the parameters of the method of the reaction. Knowledge of this composition and the properties of the fluid, i.e., electrolytes present, initial pH, density, and impurities present, is critical to determine the procedure and chemicals used during the method.
  • the electrolytes present in the recuperated, used halide fluid 60 can comprise an alkali, alkali earth metal or a base metal salt. These salts can be selected from a group of salts comprising sodium chloride, calcium chloride, zinc chloride, sodium bromide, calcium bromide, zinc bromide or blends of thereof can be employed. Strontium chloride, strontium bromide, copper chloride, copper bromide, nickel chloride, nickel bromide, aluminum chloride or aluminum bromide can also be considered.
  • a used brine fluid 60 often comprises a blend of any of these metal salts, calcium chloride, calcium bromide and/or zinc bromide for example.
  • metal present in the recuperated used halide can comprise zinc, copper cobalt, cadmium, nickel, potassium, cesium, lithium, barium, magnesium, aluminum, manganese, chromium or combinations thereof.
  • the halide ions present can comprise bromide or chloride as illustrated above, but iodide ions are also within the scope of this invention.
  • the manner in which these various electrolytes are blended depends largely on the density and crystallization temperature requirements for the particular brine fluid needed. A double or triple electrolyte blend can be used to obtain a higher density clear brine fluid.
  • bromide electrolytes When blending a relatively high- density clear brine fluid, bromide electrolytes provide higher flexibility than the relatively low-density chloride electrolytes. In addition, the stability and TCT of the blended finished product also depends on the proportion of the individual electrolytes in the composition. For example, brine fluids with a high concentration of calcium chloride may precipitate carbonates or sulfates, which are often present in formation waters of oil or gas wells.
  • Zinc bromide brines can be used to provide high density, calcium-free brine fluids which do not precipitate anions such as carbonates and sulfates due to the acidic nature of the zinc ion. Such zinc bromide brines can also be used to adjust the TCT of the fluid.
  • the density and TCT of the brine fluid can be adjusted by altering the concentration of the electrolyte or electrolytes in the solution.
  • the parameters, acidity, temperature etc., of the method must be adjusted during the regeneration to encompass the blend of electrolytes present.
  • the used halide fluids should be analyzed and evaluated for their solids content.
  • the solids are removed by a solid-liquid separation method know in the art prior to the treatment of the fluids within the reactor 10. High solid content in the feed to the reactor 10 can result in increased undesirable impurities in the finished product and will also affect other properties of the fluids.
  • the initial used halide fluid 60 piped into the reactor 10 is a fluid that was diluted during well operations and can comprise soluble and insoluble impurities such as metallic cations, hydrocarbons, polymers, suspended solids, drill cuttings and sand or grit. Because of dilution by contact with waters found in wells, these used fluids typically have less than the desired density of the required drilling fluid, but a density greater than 9.0lbs/gal.
  • the used halide fluid if comprising a high solid content, should be filtered to remove the solids prior to acidification. The method operates more efficiently if oil and grease residues and other solids are removed prior to the process. A separation process prior to acidification can remove oil and grease.
  • the separation process can include destabilization of the emulsified oil followed by physical separation of the oily phase by a suitable process known in the art.
  • One primary purpose of regenerating used halide fluids according to the method of this invention is to enhance the electrolytes lost during well operations or industrial use of the fluid.
  • the initial density of the recuperated halide fluid is calculated and the chemical composition analyzed. After analysis, the selection and amount of the proper alkali used to neutralize excess acid and restore lost electrolytes can be made. If the recuperated halide fluid is a calcium chloride, for example, a calcium oxide can be used to neutralize excess acid thereby restoring calcium ions.
  • adding acid 50 to the used halide fluid 60 acidifies the fluid.
  • the composition of the initial used halide fluid 60 can comprise aqueous zinc bromide or aqueous calcium bromide.
  • a blend of chlorides and bromides of calcium and zinc in various proportions can be used.
  • Acidification is required to avoid precipitation of the metallic salts, particularly where zinc and calcium are present.
  • the used halide comprises base metals, a pH within a range of 0 to 6, preferably 0 to 5.5, is therefore preferred.
  • the used halide comprises alkali or alkali earth metals, a pH within a range of 0 to 10, is preferred.
  • the acid 50 used for acidification can comprise hydrobromic acid.
  • the acid can comprise hydrochloric acid or an organic acid.
  • the used halide fluid is then contacted with bromine.
  • Bromine is effective to increase fluid density, adjust true crystallization temperature and removes or destroys impurities.
  • Impurities can comprise metals, hydrocarbons or polymers.
  • the used halide fluid can be contacted with a bromine-generating species.
  • bromine enhances the bromide ions available in the fluid so as to return the used halide fluid to the desired density for it's specific use. Bromine also functions to oxidize impurities such as metallic cations, and the polymers and hydrocarbons found in the used fluid. If polymers are present, which is usually the case since various polymers are used as viscosifiers, then oxidation is necessary to destroy these polymers. If the used brine is not viscosified, however, acidification is not necessary to oxidize the polymer. That step can be eliminated so that the process next comprises the addition of a halogen.
  • bromine does not increase the pH of the fluids that can promote unwanted precipitation of the metals. Compared to peroxides, bromine increases the density of the fluid rather than reducing it. Preferably the bromine is added while maintaining the temperature at a minimum of 10°C, especially when adding bromine to a blend of used halides.
  • a cooler 100 can be used to contol the rate of the reaction by maintaining the desired reaction temperature.
  • the temperature is maintained at a minimum of 20°C.
  • the resulting TCT can be adjusted to avoid the precipitation of electrolytes, which can reduce the density of the fluid.
  • a reducing agent 30 can be added in a controlled manner to combine with and remove excess bromine. Preferably the addition of the reducing agent is controlled by maintaining the temperature at a minimum of approximately 10°C.
  • the reducing agent is preferably selected from a group consisting of anhydrous ammonia, sulfur, hydrogen sulfide, sodium bisulfide, metallic zinc, metallic iron, metallic copper, metallic nickel, metallic cadmium, metallic cobalt, metallic aluminum, metallic manganese, metallic chromium, organic acids, alcohols and aldehydes.
  • the fluid is preferably contacted with an alkali 20 to neutralize any excess acid.
  • a base metal, an alkali metal and an alkali earth metal can be present in the used fluid.
  • the composition and density of the base metal is determined prior to the halide fluid 60 entering the reactor 10.
  • the metal ions must be restored to the original density required for the useful function of the halide brine in the well.
  • the alkali earth metal in the recuperated halide fluid is calcium
  • the alkali used to neutralize excess acid can be calcium hydroxide or calcium oxide.
  • the alkali used to neutralize excess acid is preferably strontium hydroxide or strontium oxide.
  • the electrolyte to be restored is an alkali metal
  • the alkali used to neutralize excess acid can be an alkali metal hydroxide.
  • sodium is the alkali metal
  • the alkali used to neutralize excess acid is sodium hydroxide.
  • the electrolyte that is to be restored is a base metal or base metal
  • the alkali used to neutralize excess acid can be a base metal oxide. In this case, when a base metal is used to neutralize excess acid, measures should be taken to vent the hydrogen gas that is emitted from the process.
  • the base metal oxide is selected from a group consisting of zinc oxide, copper oxide, cobalt oxide, cadmium oxide or nickel oxide.
  • the alkali used to neutralize excess acid is a base metal hydroxide.
  • the base metal hydroxide can be selected from a group of base metal oxides consisting of zinc, copper, cobalt, cadmium or nickel.
  • the alkali used to neutralize excess acid is anhydrous ammonia
  • the alkali in one specific embodiment of the method of this invention, the alkali
  • the reducing agent (30) is p-formaldehyde
  • the halogen (40) is bromine
  • the acid (50) used during the method is hydrobromic acid.
  • the alkali is lime
  • the reducing agent is ammonia
  • the halogen is bromine
  • the acid is hydrobromic acid.
  • Ammonia is one preferred reducing agent in an alkali and alkali earth metal systems and p-formaldehyde is the preferred reducing agent in a base metal system.
  • the equipment used to perform the method of this invention can be straightforward and quite simple. Basically, a reaction tank or pipe, one or more pumps and storage tanks are required. In one aspect of the method of this invention, the steps performed during the method are performed in a mixed reactor, preferably a stirred reactor or a tube reactor 10. In one embodiment, the recuperated used halide fluid is piped into the reactor 10 along with the bromine, acid 50, reducing agent 30 and alkali 20 so that the various chemical solutions are combined in the influent pipe and then mixed within in the reactor 10.
  • the influent chemical solutions can be piped in separately.
  • the base metals used to enhance the electrolytes can be placed in a reactor along with used halide fluid. Bromine, acid, a reducing agent and alkali can then be piped into the reactor either separately or together in one pipeline.
  • Meters can be strategically placed along the influent pipeline and effluent pipeline to monitor the properties of the solutions: oxidation- reduction potential (ORP), pH and density. Alternatively, the properties can be measured manually.
  • the meters comprise an ORP meter, a pH meter and a density meter.
  • the chemical reaction is continued and the effluent product returned to the reactor until the desired levels of density, oxidation-reduction potential and pH are achieved.
  • the reaction process can be carried on as a batch process or a continuous process.
  • a cooler 100 is used to maintain the lower temperatures. Separation of the resulting fluid from any suspended solid can be performed by several known methods.
  • a gravity settler
  • separation of the resulting fluid from any suspended solid is performed in a clarifer.
  • a centrifuge or pressure filter or vacuum filter can also be used to separate solids from the resulting product, independently or as a subsequent process to a clarifier.
  • Example 1 35. A 500 ml sample of a recovered completion fluid from an oil well with density of 15.98 lb/gallon and iron content of 540 mg/kg was placed in a glass beaker and kept stirred using an electrically driven stirrer. To this 10 ml of liquid bromine was introduced. Using a hot plate the temperature of the reaction fluid was raised to 148°F (64.4°C). The solution was kept stirred at this temperature for 1 hour, which followed by addition of 2.9 g of p-formaldehyde as 1 the reducing agent. Zinc oxide was added on as required basis to neutralize the excess acid of the fluid. The final fluid was filtered and analyzed for density and iron content, which respectively were determined to be 17.91 lb/gallon and
  • a 500 ml sample of a recovered completion fluid from an oil well of Example 1 was placed in a glass beaker and kept stirred using a electrically driven stirrer. To this 20 ml of liquid bromine was introduced, while using a hot plate the temperature of the reaction solution was raised to 102°F (38.9°C). The reaction fluid was kept stirred at this temperature for 1 hour, which was followed by addition of 5.9 g of p-formaldehyde as the reducing agent. Zinc oxide was added on as required basis to neutralize the excess acidity of the reaction fluid. The final fluid was filtered and analyzed. The iron content of the final fluid was determined to be 40 mg/kg.
  • Example 3 37. This test was conducted on a 500 ml sample of the same fluid as described in Example 1. In this case, 10 ml of liquid bromine was introduced to the fluid, while it was kept stirred and using a hot plate the temperature of the reaction solution was raised to 80°F (26.7°C).
  • the reaction fluid was kept stirred at this temperature for 1 hour, which was followed by addition of 13 g of metallic zinc as the reducing agent. In this test no basic material was added for the neutralization of excess acid.
  • the final fluid was filtered and analyzed. The density and iron content of the final product was determined to be 19.95 lb/gallon and 32 mg/kg, respectively.
  • Example 39 On a 500 ml sample of the same fluid that was used in Example 4 test was conducted. In this case, while the liquid bromine addition was maintained at 20 ml, the reaction suspension was heated to about 180°F (82.2°C) for 1.7 hrs. 5.9 g of p-formaldehyde was used as the reducing agent. Similar to Example 4, lime was used for the neutralization of excess acid content. The final reaction fluid was filtered and analyzed. The density and iron content were determined to be 13.4 lb/gallon and 10 mg/kg, respectively.
  • Example 7 41 On a 500 ml of the same fluid that was used in Example 6, the addition of liquid bromine in this test was increased to 30 ml. The temperature of the reaction fluid was maintained at 150°F (65.6°C) for 0.5 hour. In this case, 8.8 g of p-formaldehyde was added as the reducing agent, while lime was used for the neutralization of excess acid content of the reaction. The density and iron content of the final filtered fluid were measured to be 16.13 lb/gallon and 42 mg/kg, respectively.
  • Example 8 Example 8:
  • Example 7 Test described in Example 7 was repeated, while in this case zinc oxide was used for the neutralization of excess acid, replacing lime of Example 7.
  • the density and iron content of the final filtered fluid were measured to be 16.08 lb/gallon and 44 mg/kg, respectively.

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mining & Mineral Resources (AREA)
  • Geology (AREA)
  • Fluid Mechanics (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Removal Of Specific Substances (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Treating Waste Gases (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
EP02721386A 2001-03-15 2002-03-14 Verfahren zur regenerierung verbrauchter halogenidhaltiger flüssigkeiten Expired - Lifetime EP1414753B9 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US27617201P 2001-03-15 2001-03-15
US276172P 2001-03-15
PCT/US2002/007622 WO2002074699A2 (en) 2001-03-15 2002-03-14 Method for regeneration of used halide fluids

Publications (3)

Publication Number Publication Date
EP1414753A2 true EP1414753A2 (de) 2004-05-06
EP1414753B1 EP1414753B1 (de) 2006-03-01
EP1414753B9 EP1414753B9 (de) 2006-08-23

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP02721386A Expired - Lifetime EP1414753B9 (de) 2001-03-15 2002-03-14 Verfahren zur regenerierung verbrauchter halogenidhaltiger flüssigkeiten

Country Status (7)

Country Link
EP (1) EP1414753B9 (de)
CN (1) CN1278949C (de)
AU (1) AU2002252321A1 (de)
GB (1) GB2388592B (de)
IL (2) IL157852A0 (de)
NO (1) NO324398B1 (de)
WO (1) WO2002074699A2 (de)

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Publication number Priority date Publication date Assignee Title
CN109020001A (zh) * 2018-09-10 2018-12-18 青海瑞能新型燃料科技有限公司 一种锂电池生产过程中含醇废液综合回收方法

Family Cites Families (2)

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Publication number Priority date Publication date Assignee Title
US4895665A (en) * 1989-04-26 1990-01-23 George D. Smith Method for treating and reclaiming oil and gas well working fluids and drilling pits
US5254257A (en) * 1993-01-19 1993-10-19 Culligan International Company Reclaiming of spent brine

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO02074699A3 *

Also Published As

Publication number Publication date
CN1278949C (zh) 2006-10-11
GB2388592A (en) 2003-11-19
IL157852A0 (en) 2004-03-28
WO2002074699A2 (en) 2002-09-26
GB0321133D0 (en) 2003-10-08
CN1630618A (zh) 2005-06-22
GB2388592B (en) 2004-11-24
WO2002074699A3 (en) 2004-02-19
NO20034061L (no) 2003-11-14
AU2002252321A1 (en) 2002-10-03
NO20034061D0 (no) 2003-09-12
NO324398B1 (no) 2007-10-01
EP1414753B9 (de) 2006-08-23
EP1414753B1 (de) 2006-03-01
IL157852A (en) 2006-07-05

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