WO1999065823A1 - Method of procucing potassium sulfate - Google Patents
Method of procucing potassium sulfate Download PDFInfo
- Publication number
- WO1999065823A1 WO1999065823A1 PCT/CA1999/000564 CA9900564W WO9965823A1 WO 1999065823 A1 WO1999065823 A1 WO 1999065823A1 CA 9900564 W CA9900564 W CA 9900564W WO 9965823 A1 WO9965823 A1 WO 9965823A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- filtrate
- precipitate
- chloride
- sulfate
- potassium
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/026—Preparation of ammonia from inorganic compounds
- C01C1/028—Preparation of ammonia from inorganic compounds from ammonium sulfate or sulfite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/06—Preparation of sulfates by double decomposition
- C01D5/08—Preparation of sulfates by double decomposition with each other or with ammonium sulfate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- the present invention relates to a method of producing potassium sulfate and more particularly, the invention relates to a method of synthesizing pure potassium sulfate from brines of ammonium sulfate with up to 12% Na 2 S0 4 impurities.
- Potassium chloride and sulfuric acid are reacted and the resulting mixture kneaded to produce potassium sulfate, as disclosed by Iwashita et al., in United States Patent No.
- the present invention has applicability in the fertilizer art.
- One object of the present invention is to provide an improvement in potassium sulfate preparation.
- the process results in the formulation of useful products during the synthesis of the potassium sulfate with recovery of sulfate and potassium in excess of 95% completely in the absence of evaporation. This significant feature has particular importance in terms of energy efficiency and thus the costs of the process.
- a further object of one embodiment of the present invention is to provide a method of producing potassium sulfate from a source containing ammonium sulfate, characterized in that the method comprises the steps of: contacting potassium chloride and ammonium sulfate in a mixer at a temperature of between 20°C and 40°C; precipitating a first precipitate of double salt in a filtrate; mixing, in a second mixing step, the filtrate with potassium chloride; generating a second filtrate containing ammonium and potassium chloride and a second precipitate of double salt; mixing the second double salt precipitate with the first precipitate in a solution of potassium chloride; precipitating a third precipitate of potassium sulfate and a third filtrate; recirculating the third filtrate into the second mixing step; mixing the second filtrate in a mixing tank at a temperature of less than 70°C in a solution of less than 10% by weight sodium chloride, calcium chloride and sodium sulfate; and generating a syngenite precipitate and a
- Another object of one embodiment of the present invention is to provide a method of producing potassium sulfate from a source containing ammonium sulfate, characterized in that the method comprises the steps of: contacting potassium chloride and ammonium sulfate in a mixer at a temperature of less than 30°C; precipitating a first precipitate of double salt in a filtrate; mixing, in a second mixing step, said filtrate with potassium chloride; generating a second filtrate containing ammonium and potassium chloride and a second precipitate of double salt; mixing said second double salt precipitate with said first precipitate in a solution of potassium chloride; precipitating a third precipitate of potassium sulfate and a third filtrate; recirculating said third filtrate into said second mixing step; mixing said second filtrate in a mixing tank at a temperature of less than 70°C in a solution of less than 10% by weight sodium chloride, calcium chloride and sodium sulfate; generating a syngenite precipitate and a fourth filtrate; mixing
- Figure 1 is a schematic illustration of the process flow diagram according to one embodiment of the present invention.
- Figure 2 is a schematic illustration of the process flow diagram according to another embodiment of the present invention.
- Potassium sulfate is a valuable chemical commodity, typically employed in analytical chemistry, cement mixes and fertilizer for chloride sensitive crops such citrus and tobacco crops.
- the compound is also used in the manufacture of glass, alum and is used as a food additive.
- the feedstock material 12 includes solid potassium chloride and ammonium sulfate in an amount less than about 40% by weight (NH 4 ) 2 S0 4 .
- the compounds are mixed in a mixing tank 14, which tank 14 is heated to between 25°C and 30°C in order for the conversion of the compounds to double salt.
- the solution is passed into a separator 16, an example of which is a cyclone.
- the resulting solid is K 2 S0 4 • (NH 4 ) • 2S0 4 , double salt.
- the first filtrate is subsequently passed into a second mixing container 18 into which is added additional potassium chloride brine.
- the container is heated similarly to container 14 and once mixed, the solution is separated by separator 20.
- the resulting second filtrate is subjected to further unit operations to be discussed hereinafter.
- the second precipitate from mixing tank 18 as well as the first precipitate from tank 14 are combined in a third heated container 22 together with saturated potassium chloride brine.
- the product is then separated by separator 24 into a third filtrate for recycle into container 18 and a third solid comprising potassium sulfate crystals in a size distribution of approximately 20 mesh to about 150 mesh. In this portion of the circuit, the yield is approximately 95% S0 4 and 80% potassium.
- the second filtrate from the separator 20 contains ammonium chloride, sodium chloride (approximately 10%) and potassium chloride. This is passed into a fourth mixing container 26 together with calcium chloride and sodium sulfate.
- the container 26 is kept at a temperature of between 25°C and 70°C.
- the resulting mixture is separated with separator into a solid, namely syngenite (CaS0 4 • K 2 S0 4 • xH 2 0) which washed with water and retained for additional unit operations.
- the liquid is passed into a fifth sealed mixing container 30 containing lime or hydrated lime.
- the container is maintained at a temperature of about 80°C in order to liberate ammonia (approximately 98% by volume).
- Residual ammonium is passed into air scrubber 32 resulting in the generation of calcium chloride/sodium chloride brine. This may be subjected to further processing to produce CaCI 2 or NaCI, disposed of in deep well injection or returned to the ocean.
- Further processing includes additional scrubbing of the ammonium in scrubber 34 to which may be added sulfuric acid to result in the generation of ammonium sulfate, a useful fertilizer.
- the same is passed into a sixth mixer 36 maintained at 70°C to which ammonium bicarbonate has been added.
- the mixture is passed into a separator 38 to generate calcium carbonate precipitate with a +95 brightness and a filtrate containing potassium sulfate and ammonium sulfate. The filtrate may be recycled to the initial steps of the process.
- Figure 2 illustrates a flow chart where potassium sulfate is formulated from ammonium sulfate contaminated with sodium sulfate.
- contaminated ammonium sulfate is not useful as a vendible high quality fertilizer.
- Numeral 40 denotes the overall process for Figure 2.
- Ammonium sulfate and potassium chloride are mixed together in mixing tank 42 at a temperature of between 30° and 40° such that there is only enough water to saturate either the ammonium sulfate or potassium chloride.
- the mixture is passed into a separator 44 to produce 80% to 90% potassium sulfate crystal containing approximately 10% to 20% ammonium sulfate.
- the crystal product is filtered and/or washed (not shown) added to a solution of saturated potassium chloride brine in mixing vessel 46 at a temperature of 30°C.
- the solution is filtered with filter 48 with the solid fraction containing in excess 98% pure ammonium sulfate.
- the crystals, once centrifuged and washed have been found to have a purity in excess of 99.5 %.
- the potassium chloride brine from vessel 46 is recycled to mixing vessel 42; the brine from vessel 42 contains between 20% and 30% ammonium chloride and preferably between 22% and 25%, 10% or less sodium chloride and 15 % or less potassium chloride.
- the heated brine is reacted with calcium chloride and ammonium sulfate or sodium sulfate anhydrite from feed in vessel 50 at approximately 30°C to precipitate the soluble potassium chloride as syngenite, CaS0 4 «K 2 S0 4 (x)H 2 0 at separator 52.
- the syngenite salt is then filtered and washed (not shown) to remove the residual chloride brine.
- the salt is then heated in vessel 54 at a temperature of between 70°C and 90°C together with water and a source of ammonia and carbon dioxide or ammonium bicarbonate to convert the calcium sulfate to calcium carbonate.
- the calcium carbonate is separated in separator 56. Since the ammonium sulfate and the SOP are soluble, the calcium carbonate precipitate is filtered and washed with water to remove entrained ammonium sulfate etc.
- the calcium carbonate precipitate is of a sufficiently high quality and size to provide utility as a bulk paper filler of + 95 brightness on blue light.
- the filtrate is recycled to vessel 42 as indicated by A in Figure 2.
- the filtrate from separator 52 is heated in vessel at a temperature of between 60°C and 100°C and reacted with lime to yield a brine of calcium chloride, sodium chloride and ammonia gas.
- the ammonia gas is recovered for further purposes.
- CaCI 2 can be recycled to Step 3 but if that Cl builds up in the circuit; then one has to precipitate the CaCI 2 as CaS0 4 • 2H 2 0 and send the solid gypsum as the recycle.
- Recycle of G increases the circuit efficiency and one can adjust the material balance to the desired recycle and recovery.
- Discharge brine is deep well injected or evaporated to produce CaCI 2 brine for sales.
- Estimated K recovery can be calculated to be:
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Fertilizers (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims
Priority Applications (14)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EA200001194A EA002758B1 (en) | 1998-06-16 | 1999-06-15 | Method of producing potassium sulfate |
EP99957051A EP1094985A1 (en) | 1998-06-16 | 1999-06-15 | Method of procucing potassium sulfate |
SK1545-2000A SK15452000A3 (en) | 1998-06-16 | 1999-06-15 | Method of procucing potassium sulfate |
MXPA00010125A MXPA00010125A (en) | 1998-06-16 | 1999-06-15 | Method of procucing potassium sulfate. |
JP2000554656A JP2002518281A (en) | 1998-06-16 | 1999-06-15 | Production method of potassium sulfate |
BR9910403-2A BR9910403A (en) | 1998-06-16 | 1999-06-15 | Method for the production of potassium sulphate |
PL99344486A PL344486A1 (en) | 1998-06-16 | 1999-06-15 | Method of procucing potassium sulfate |
HU0101399A HUP0101399A3 (en) | 1998-06-16 | 1999-06-15 | Method of producing potassium sulfate |
SI9920037A SI20525A (en) | 1998-06-16 | 1999-06-15 | Method of producing potassium sulfate |
AU42545/99A AU4254599A (en) | 1998-06-16 | 1999-06-15 | Method of producing potassium sulfate |
KR1020007012544A KR20010034850A (en) | 1998-06-16 | 1999-06-15 | Method of producing potassium sulfate |
IL13909999A IL139099A0 (en) | 1998-06-16 | 1999-06-15 | Method of producing potassium sulfate |
NO20005121A NO20005121L (en) | 1998-06-16 | 2000-10-11 | Process for the preparation of potassium sulphate |
BG104860A BG63775B1 (en) | 1998-06-16 | 2000-10-16 | Method for potassium sulphate production |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US8963098P | 1998-06-16 | 1998-06-16 | |
US60/089,630 | 1998-06-16 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1999065823A1 true WO1999065823A1 (en) | 1999-12-23 |
Family
ID=22218710
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/CA1999/000564 WO1999065823A1 (en) | 1998-06-16 | 1999-06-15 | Method of procucing potassium sulfate |
Country Status (21)
Country | Link |
---|---|
US (1) | US6315976B1 (en) |
EP (1) | EP1094985A1 (en) |
JP (1) | JP2002518281A (en) |
KR (1) | KR20010034850A (en) |
CN (1) | CN1202008C (en) |
AU (1) | AU4254599A (en) |
BG (1) | BG63775B1 (en) |
BR (1) | BR9910403A (en) |
EA (1) | EA002758B1 (en) |
HR (1) | HRP990360A2 (en) |
HU (1) | HUP0101399A3 (en) |
ID (1) | ID28245A (en) |
IL (1) | IL139099A0 (en) |
MX (1) | MXPA00010125A (en) |
NO (1) | NO20005121L (en) |
PL (1) | PL344486A1 (en) |
SI (1) | SI20525A (en) |
SK (1) | SK15452000A3 (en) |
TR (1) | TR200003226T2 (en) |
WO (1) | WO1999065823A1 (en) |
YU (1) | YU76200A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001028925A1 (en) * | 1999-10-21 | 2001-04-26 | Airborne Industrial Minerals Inc. | Formulation of potassium sulfate, sodium carbonate and sodium bicarbonate from potash brine |
CN109911919A (en) * | 2017-12-13 | 2019-06-21 | 北京恩泽佳立科技有限公司 | Potassium sulfate preparation system and method |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7041268B2 (en) * | 2004-03-30 | 2006-05-09 | Council Of Scientific And Industrial Research | Process for recovery of sulphate of potash |
CN1803615B (en) * | 2006-01-04 | 2010-04-14 | 四川安县银河建化集团有限公司 | Method for preparing potassium sulphate by chromium contained Glauber salt |
CN101687141B (en) * | 2007-04-12 | 2012-09-05 | Cefco有限责任公司 | Process and apparatus for carbon capture and elimination of multi-pollutants in flue gas from hydrocarbon fuel sources and recovery of multiple by-products |
CA2737825A1 (en) * | 2011-04-20 | 2012-10-20 | Carbon Solutions Incorporated | Conversion of acid gas to sulphate or phosphate-based fertilizers |
US8409542B2 (en) * | 2011-06-14 | 2013-04-02 | Nichromet Extraction Inc. | Method and system for the production of potassium sulfate from potassium chloride |
CA2854103C (en) | 2011-11-17 | 2019-01-08 | Gc Technology Limited | Interconnected system and method for the purification and recovery of potash |
US9737827B2 (en) * | 2012-08-13 | 2017-08-22 | Enviro Water Minerals Company, Inc. | System for removing high purity salt from a brine |
EP2932030B1 (en) * | 2012-12-13 | 2016-06-01 | Solvay SA | Process for recovering soda values from underground soda deposits |
CN104261433B (en) * | 2014-09-24 | 2016-06-29 | 湘潭市天志科技有限公司 | A kind of method that solid waste utilized containing potassium, chloride ion produces potassium sulfate |
CN106629781B (en) * | 2015-10-28 | 2017-12-05 | 绥芬河市石英经贸有限公司 | A kind of preparation method of potassium sulfate |
CN106315627A (en) * | 2016-08-12 | 2017-01-11 | 宜昌富升化工有限公司 | Production technology of potassium sulfate |
CN106335910B (en) * | 2016-08-25 | 2017-11-24 | 辽宁津大肥业有限公司 | A kind of preparation method of potassium sulfate and ammonium chloride |
CA2968257C (en) | 2017-05-24 | 2022-05-24 | Inotel Inc. | Potassium magnesium fertilizer |
WO2019082207A1 (en) * | 2017-10-25 | 2019-05-02 | Fertis India Pvt. Ltd. | Energy efficient synthesis of sulphate of potash using ammonia as a catalyst |
IT202000018238A1 (en) | 2020-07-28 | 2022-01-28 | Edale S R L | PRODUCTION PROCESS OF FERTILIZER BASED ON POTASSIUM SULPHATE |
KR102454672B1 (en) | 2020-12-28 | 2022-10-14 | 한국세라믹기술원 | Optimized Manufacturing Method Of Potassium Sulfate Using Sodium Sulfate And Potassium Chloride |
EP4299553A1 (en) * | 2022-06-30 | 2024-01-03 | SABIC Global Technologies B.V. | Production of nitrogen, potassium, sulfur nutrient through de-carbonization and utilization of calcium sulfate |
Citations (3)
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GB411820A (en) * | 1932-12-08 | 1934-06-08 | Albert Eric Cashmore | Improvements in or relating to the production of potassium sulphate or mixed crystals of potassium sulphate and ammonium sulphate |
CA1197663A (en) * | 1983-03-21 | 1985-12-10 | Jean-Marc Lalancette | Potassium sulfate from magnesium sulfate |
CN1091112A (en) * | 1993-02-20 | 1994-08-24 | 湖南省化肥工业公司 | Preparation of potassium sulfate by circulating double decomposition of ammonium sulfate and potassium chloride |
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US1824361A (en) | 1929-04-29 | 1931-09-22 | Morse Harry Wheeler | Manufacture of sulphate of potash |
US1936070A (en) | 1931-03-11 | 1933-11-21 | American Potash & Chem Corp | Process for the manufacture of potassium sulphate |
US1922682A (en) | 1931-08-15 | 1933-08-15 | Holz August | Method of converting potassium chloride into potassium sulphate |
US1990896A (en) | 1932-07-30 | 1935-02-12 | Pacific Coast Borax Co | Method of making potassium sulphate |
US2882128A (en) * | 1954-09-16 | 1959-04-14 | Chimiques Pour L Andustrie Et | Preparation of potassium sulphate from calcium sulphate and potassium chloride |
US3369867A (en) | 1964-05-14 | 1968-02-20 | American Potash & Chem Corp | Method of producing potassium sulfate |
US3436175A (en) | 1964-06-19 | 1969-04-01 | Duval Corp | Method of producing ammonium sulfate,potassium sulfate and magnesium oxide from langbeinite |
US3528767A (en) | 1966-03-16 | 1970-09-15 | Donald E Garrett | Production of potassium chloride,potassium sulfate and sodium sulfate from brines and the like containing potassium,chloride and sulfate |
US3423171A (en) | 1966-06-14 | 1969-01-21 | Kali Forschungs Inst | Method for making alkali metal sulfate |
US3429657A (en) | 1966-09-02 | 1969-02-25 | Us Interior | Method for recovering and producing potassium salts |
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DE1902738B2 (en) * | 1969-01-21 | 1977-02-10 | Kali Und Salz Ag, 3500 Kassel | PROCESS FOR THE PRODUCTION OF POTASSIUM SULPHATE AND / OR SYNGENITE |
US3687639A (en) | 1970-05-25 | 1972-08-29 | Int Minerals & Chem Corp | Production of finely divided potassium sulfate crystals |
US3656891A (en) | 1970-08-05 | 1972-04-18 | Occidental Petroleum Corp | Process for the production of potassium sulfate and borax |
US3895920A (en) | 1970-09-03 | 1975-07-22 | Donald E Garrett | Method of producing coarse potash |
US3843772A (en) | 1972-09-14 | 1974-10-22 | Int Minerals & Chem Corp | Production of white potassium sulfate crystals |
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-
1999
- 1999-06-14 US US09/332,500 patent/US6315976B1/en not_active Expired - Fee Related
- 1999-06-15 ID IDW20010127A patent/ID28245A/en unknown
- 1999-06-15 JP JP2000554656A patent/JP2002518281A/en active Pending
- 1999-06-15 KR KR1020007012544A patent/KR20010034850A/en not_active Application Discontinuation
- 1999-06-15 EP EP99957051A patent/EP1094985A1/en not_active Withdrawn
- 1999-06-15 CN CNB998056839A patent/CN1202008C/en not_active Expired - Fee Related
- 1999-06-15 WO PCT/CA1999/000564 patent/WO1999065823A1/en not_active Application Discontinuation
- 1999-06-15 IL IL13909999A patent/IL139099A0/en unknown
- 1999-06-15 SI SI9920037A patent/SI20525A/en not_active IP Right Cessation
- 1999-06-15 SK SK1545-2000A patent/SK15452000A3/en unknown
- 1999-06-15 BR BR9910403-2A patent/BR9910403A/en not_active Application Discontinuation
- 1999-06-15 TR TR2000/03226T patent/TR200003226T2/en unknown
- 1999-06-15 MX MXPA00010125A patent/MXPA00010125A/en not_active Application Discontinuation
- 1999-06-15 AU AU42545/99A patent/AU4254599A/en not_active Abandoned
- 1999-06-15 HU HU0101399A patent/HUP0101399A3/en unknown
- 1999-06-15 PL PL99344486A patent/PL344486A1/en unknown
- 1999-06-15 YU YU76200A patent/YU76200A/en unknown
- 1999-06-15 EA EA200001194A patent/EA002758B1/en not_active IP Right Cessation
- 1999-11-18 HR HR60/089,630A patent/HRP990360A2/en not_active Application Discontinuation
-
2000
- 2000-10-11 NO NO20005121A patent/NO20005121L/en not_active Application Discontinuation
- 2000-10-16 BG BG104860A patent/BG63775B1/en unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB411820A (en) * | 1932-12-08 | 1934-06-08 | Albert Eric Cashmore | Improvements in or relating to the production of potassium sulphate or mixed crystals of potassium sulphate and ammonium sulphate |
CA1197663A (en) * | 1983-03-21 | 1985-12-10 | Jean-Marc Lalancette | Potassium sulfate from magnesium sulfate |
CN1091112A (en) * | 1993-02-20 | 1994-08-24 | 湖南省化肥工业公司 | Preparation of potassium sulfate by circulating double decomposition of ammonium sulfate and potassium chloride |
Non-Patent Citations (1)
Title |
---|
DATABASE WPI Section Ch Week 9715, Derwent World Patents Index; Class C04, AN 97-154962, XP002116365 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001028925A1 (en) * | 1999-10-21 | 2001-04-26 | Airborne Industrial Minerals Inc. | Formulation of potassium sulfate, sodium carbonate and sodium bicarbonate from potash brine |
US6334990B1 (en) | 1999-10-21 | 2002-01-01 | Airborne Industrial Minerals Inc. | Formulation of potassium sulfate, sodium carbonate and sodium bicarbonate from potash brine |
CN109911919A (en) * | 2017-12-13 | 2019-06-21 | 北京恩泽佳立科技有限公司 | Potassium sulfate preparation system and method |
Also Published As
Publication number | Publication date |
---|---|
IL139099A0 (en) | 2001-11-25 |
HRP990360A2 (en) | 2000-04-30 |
AU4254599A (en) | 2000-01-05 |
MXPA00010125A (en) | 2004-10-14 |
NO20005121D0 (en) | 2000-10-11 |
US6315976B1 (en) | 2001-11-13 |
NO20005121L (en) | 2001-02-15 |
CN1202008C (en) | 2005-05-18 |
TR200003226T2 (en) | 2001-03-21 |
BR9910403A (en) | 2001-01-09 |
SK15452000A3 (en) | 2001-04-09 |
HUP0101399A3 (en) | 2003-04-28 |
JP2002518281A (en) | 2002-06-25 |
BG63775B1 (en) | 2002-12-29 |
PL344486A1 (en) | 2001-11-05 |
YU76200A (en) | 2003-02-28 |
ID28245A (en) | 2001-05-10 |
BG104860A (en) | 2001-07-31 |
EA002758B1 (en) | 2002-08-29 |
KR20010034850A (en) | 2001-04-25 |
HUP0101399A2 (en) | 2001-12-28 |
EP1094985A1 (en) | 2001-05-02 |
SI20525A (en) | 2001-10-31 |
CN1299337A (en) | 2001-06-13 |
EA200001194A1 (en) | 2001-06-25 |
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