CN1294089A - 制备氨和氨合成气的方法 - Google Patents
制备氨和氨合成气的方法 Download PDFInfo
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- CN1294089A CN1294089A CN00134418A CN00134418A CN1294089A CN 1294089 A CN1294089 A CN 1294089A CN 00134418 A CN00134418 A CN 00134418A CN 00134418 A CN00134418 A CN 00134418A CN 1294089 A CN1294089 A CN 1294089A
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- Prior art keywords
- ammonia
- catalyzer
- ruthenium
- synthesis gas
- carrier
- Prior art date
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 10
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 13
- 229910052582 BN Inorganic materials 0.000 claims abstract description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 150000004767 nitrides Chemical class 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 2
- NLSCHDZTHVNDCP-UHFFFAOYSA-N caesium nitrate Chemical compound [Cs+].[O-][N+]([O-])=O NLSCHDZTHVNDCP-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- YLPJWCDYYXQCIP-UHFFFAOYSA-N nitroso nitrate;ruthenium Chemical compound [Ru].[O-][N+](=O)ON=O YLPJWCDYYXQCIP-UHFFFAOYSA-N 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 101100232929 Caenorhabditis elegans pat-4 gene Proteins 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003304 ruthenium compounds Chemical class 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
- C01C1/0411—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Industrial Gases (AREA)
Abstract
一种从氨合成气体中制备氨的方法,该方法包括在氨合成条件下将氨合成气体与一种含有钌作为活性催化材料载于氮化硼和/或氮化硅载体上的氨催化剂进行接触。
Description
本发明涉及一种通过将氨合成气体与一种用钌作为催化剂活性催化材料承载于金属氮化物载体上的氨催化剂进行接触而合成氨的方法。
钌基催化剂用于从氨合成气合成氨是现有技术(美国专利US4 600 571，日本专利公开NO．9168739和英国专利GB2 033 766)。
为了使昂贵的钌所需的用量最小化，这类催化剂通常承载在一种载体材料上以使活性钌颗粒的可利用的表面积最大化。
已经提出几种载体适合用于催化合成氨，它们是MgO、Al2O3、MgAL2O4。目前，大多数活性钌催化剂是承载于石墨化碳上作为载体材料。
然而，在使用碳基载体中的一个严重缺陷是在工业条件下易于氢化。碳载体慢慢转变成甲烷，结果载体逐渐损耗、最终操作产生困难。
本发明的一般目的是提供一种用改进的氮化硼和／或氮化硅载体作为承载材料的钌基氨合成催化剂。氮化物与碳是等电子的。氮化硼和氮化硅象碳一样作为同素异形体而存在。这些同素异形体是一种石墨形式，通常称之为白石墨。与碳相反，氮化硼和氮化硅在工业氨合成条件下是热力学稳定的。
BN和Si3N4都能够以高表面积材料形式获得，而且使用本领域常规的方法压制成适宜的载体。
所提出的承载于BN或Si3N4上的钌催化剂，在催化合成氨期间完全稳定。
因此，本发明在氨合成中采用氮化硼和／或氮化硅作为催化剂载体、作为氨催化剂用钌作为活性催化材料。
BN或Si3N4既可以商购或根据本领域常规方法制备。氮化物载体的表面积优选高于25m2／g。另外，氮化物载体从Si和B的前体获得，接着在用氨处理期间转变为氮化物。
钌采用常规方法引入到载体上，如用合适的含钌化合物比如氯化钌或醋酸钉浸泡载体。
在助催化之前，该催化剂用还原气体如氢或合成气体进行处理来还原。
通过用助催化剂的盐类浸泡可以提高效果。这些助催化剂选自已知的氨合成催化剂促进剂如碱金属或碱土金属，或者是稀土金属。
这些促进剂可以依次引入或者一起引入。
实施例
实施例1
制备催化剂
一种氮化硼载体(六角形，表面积85m2／g，由X-射线粉末衍射确定的晶体尺寸为7．5nm)用亚硝基硝酸钌(ruthenium nitroso nitrate)浸泡，得到5wt％的钌浓度。将浸泡试样在80℃干燥，接着在氢气流于450℃下还原。此试样标记为5RuBN。
另一个试样用类似的方法制备，不同的是含7wt％的钌。此试样标记为7RuBN。此催化剂的密度约1．5g／ml。
实施例2
铯促进的催化剂
5RuBN和7RuBN用硝酸铯水溶液浸泡以获得3wt％的铯浓度。此试样分别标记为3Cs5RuBN和3Cs7RuBN。
实施例3
钡促进的催化剂
5RuBN和7RuBN用硝酸钡水溶液浸泡以获得3wt％的钡浓度。此试样分别标记为3Ba5RuBN和3Ba7RuBN。
实施例4
测试催化剂
这些催化剂在等温栓式流动反应器中，于100和400℃操作条件下进行测试。入口气体在氢气／氮气的3∶1混合物中含有4．5％氨。流速调节到在出口处含有12％的氨。在这些条件下这些催化剂在不同速率下生产的氨，以每小时每克催化剂生产氨的ml量表示：
催化剂 ml NH3／(g．h)
5RuBN 140
7RuBN 190
3Cs5RuBN 1150
3Cs7RuRN 1320
3Ba5RuBN 4600
3Ba7RuBN 4930
实施例5
催化剂的热力学稳定性
为确定这些催化剂的稳定性，将3Ba5RuBN和3Ba7RuBN在反应器中于550℃下加热1000小时。在这些条件下氨出口处的浓度是7．0％左右。经过这种处理后，再次测试此催化剂：
催化剂 ml NH3／(g．h)
3Ba5RuBN 4580
3Ba7RuBN 4960
实施例5
催化剂的钝化和再生
为确定此催化剂在钝化后是否能够再生。将实施例5的催化剂(3Ba5RuBN)在室温下用N2中有1000ppm的O2的气体处理10小时，接着暴露在环境气氛下。然后再将其装入此反应器中，于等同条件下测试：
催化剂 ml NH3／(g．h)
3Ba5RuBN 4610。
Claims (2)
1、一种从氨合成气体中制备氨的方法，该方法包括在氨合成条件下将氨合成气体与一种含有钌作为活性催化材料载于氮化硼和／或氮化硅载体上的氨催化剂进行接触。
2、催化剂，该催化剂在从氨合成气体合成氨中是活性的，该催化剂含有承载于氮化硼和／或氮化硅载体上的钌。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US16215199P | 1999-10-29 | 1999-10-29 | |
| US60/162151 | 1999-10-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1294089A true CN1294089A (zh) | 2001-05-09 |
| CN1170770C CN1170770C (zh) | 2004-10-13 |
Family
ID=22584376
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001344188A Expired - Lifetime CN1170770C (zh) | 1999-10-29 | 2000-10-28 | 从氨合成气体中制备氨的方法和催化剂 |
Country Status (13)
| Country | Link |
|---|---|
| US (2) | US6479027B1 (zh) |
| EP (1) | EP1095906B1 (zh) |
| JP (1) | JP2001149780A (zh) |
| KR (1) | KR20010051302A (zh) |
| CN (1) | CN1170770C (zh) |
| AT (1) | ATE285992T1 (zh) |
| AU (1) | AU779326B2 (zh) |
| CA (1) | CA2324328C (zh) |
| DE (1) | DE60017055T2 (zh) |
| MX (1) | MXPA00010606A (zh) |
| RU (1) | RU2247600C2 (zh) |
| TW (1) | TWI225035B (zh) |
| ZA (1) | ZA200006022B (zh) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100448530C (zh) * | 2007-05-23 | 2009-01-07 | 浙江工业大学 | 一种复合氧化物负载钌基氨合成催化剂及其制备方法 |
| CN102300812A (zh) * | 2009-01-29 | 2011-12-28 | 格特·翁加尔 | 用于合成氨的设备和方法 |
| CN102580779A (zh) * | 2012-02-06 | 2012-07-18 | 福州大学 | 以亚硝酰基硝酸钌为前驱体的氨合成催化剂及其制备方法 |
| CN109701586A (zh) * | 2019-03-11 | 2019-05-03 | 刘志刚 | 一种可再生氨（绿氨）合成催化剂 |
| CN111182966A (zh) * | 2017-05-15 | 2020-05-19 | 星火能源 | 用于nh3催化的金属修饰的钡钙铝氧化物及相关材料 |
| CN114733551A (zh) * | 2022-05-06 | 2022-07-12 | 福州大学 | 一种高性能Ru基合成氨催化剂及其制备方法和应用 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7723258B2 (en) * | 2000-06-21 | 2010-05-25 | Green Hydrotec Corp. | Method and substance for reactive catalytic combustion |
| US20040058809A1 (en) * | 2000-06-21 | 2004-03-25 | Green Hydrotec, Corp. | Method and substance for reactive catalytic combustion |
| ITMI20020214A1 (it) * | 2002-02-06 | 2003-08-06 | Snam Progetti | Sistema catalitico per la produzione di olefine |
| ATE321736T1 (de) * | 2002-07-11 | 2006-04-15 | Haldor Topsoe As | Verfahren zur herstellung von ammoniak sowie katalysator hierzu |
| WO2008154613A1 (en) * | 2007-06-12 | 2008-12-18 | Hsm Systems, Inc. | Improved procedures for ammonia production |
| CN103977828B (zh) * | 2013-12-10 | 2016-02-10 | 中国科学院大连化学物理研究所 | 用于氨合成及氨分解的催化剂 |
| EP3156126A4 (en) * | 2014-02-27 | 2017-11-22 | Japan Science and Technology Agency | Support metal catalyst and method for synthesizing ammonia using same catalyst |
| CN104785255A (zh) * | 2015-04-21 | 2015-07-22 | 福州大学 | 一种氮掺杂活性炭为载体的钌系氨合成催化剂及其制备 |
| CN107847860A (zh) * | 2015-07-09 | 2018-03-27 | 优美科股份公司及两合公司 | 具有nh3‑scr活性、氨氧化活性和对挥发性钒和钨化合物的吸附能力的三效催化剂 |
| WO2017151769A1 (en) | 2016-03-01 | 2017-09-08 | Beach Joseph | Electrically enhanced haber-bosch (eehb) anhydrous ammonia synthesis |
| JP6675619B2 (ja) * | 2016-08-08 | 2020-04-01 | 国立大学法人東京工業大学 | アンモニア合成用触媒の製造方法及びアンモニアの製造方法 |
| WO2019156029A1 (ja) * | 2018-02-07 | 2019-08-15 | 国立大学法人東京工業大学 | 複合物、触媒及びアンモニアの製造方法 |
| WO2019156028A1 (ja) * | 2018-02-07 | 2019-08-15 | 国立大学法人東京工業大学 | 複合物、複合物の製造方法、触媒及びアンモニアの製造方法 |
| US11772979B2 (en) | 2019-01-31 | 2023-10-03 | Starfire Energy | Metal-decorated barium calcium aluminum oxide catalyst for NH3 synthesis and cracking and methods of forming the same |
| CN111841317B (zh) * | 2019-12-12 | 2022-08-05 | 万华化学集团股份有限公司 | 一种光气分解规整填料催化剂和制备方法及一种含光气尾气处理装置和处理方法 |
| CN111185164A (zh) * | 2020-03-06 | 2020-05-22 | 福州大学 | 一种以乙酸钌为前驱体的氨合成催化剂及其制备方法 |
| KR102426142B1 (ko) | 2020-05-07 | 2022-07-28 | 한국과학기술연구원 | 육방정 구조의 지지체에 촉매금속이 담지된 촉매 및 이의 제조방법 |
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-
2000
- 2000-10-16 AT AT00122537T patent/ATE285992T1/de not_active IP Right Cessation
- 2000-10-16 DE DE60017055T patent/DE60017055T2/de not_active Expired - Fee Related
- 2000-10-16 EP EP00122537A patent/EP1095906B1/en not_active Expired - Lifetime
- 2000-10-18 TW TW089121752A patent/TWI225035B/zh not_active IP Right Cessation
- 2000-10-20 US US09/692,037 patent/US6479027B1/en not_active Expired - Fee Related
- 2000-10-26 ZA ZA200006022A patent/ZA200006022B/xx unknown
- 2000-10-26 CA CA2324328A patent/CA2324328C/en not_active Expired - Lifetime
- 2000-10-27 RU RU2000126938/04A patent/RU2247600C2/ru active
- 2000-10-27 MX MXPA00010606A patent/MXPA00010606A/es active IP Right Grant
- 2000-10-27 AU AU69599/00A patent/AU779326B2/en not_active Expired
- 2000-10-27 JP JP2000328905A patent/JP2001149780A/ja not_active Withdrawn
- 2000-10-28 KR KR1020000063683A patent/KR20010051302A/ko not_active Application Discontinuation
- 2000-10-28 CN CNB001344188A patent/CN1170770C/zh not_active Expired - Lifetime
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2002
- 2002-09-17 US US10/244,677 patent/US6764668B2/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100448530C (zh) * | 2007-05-23 | 2009-01-07 | 浙江工业大学 | 一种复合氧化物负载钌基氨合成催化剂及其制备方法 |
| CN102300812A (zh) * | 2009-01-29 | 2011-12-28 | 格特·翁加尔 | 用于合成氨的设备和方法 |
| CN102300812B (zh) * | 2009-01-29 | 2015-07-22 | 格特·翁加尔 | 用于合成氨的设备和方法 |
| CN102580779A (zh) * | 2012-02-06 | 2012-07-18 | 福州大学 | 以亚硝酰基硝酸钌为前驱体的氨合成催化剂及其制备方法 |
| CN102580779B (zh) * | 2012-02-06 | 2013-07-03 | 福州大学 | 以亚硝酰基硝酸钌为前驱体的氨合成催化剂及其制备方法 |
| CN111182966A (zh) * | 2017-05-15 | 2020-05-19 | 星火能源 | 用于nh3催化的金属修饰的钡钙铝氧化物及相关材料 |
| CN111182966B (zh) * | 2017-05-15 | 2023-05-30 | 星火能源 | 用于nh3催化的金属修饰的钡钙铝氧化物及相关材料 |
| CN109701586A (zh) * | 2019-03-11 | 2019-05-03 | 刘志刚 | 一种可再生氨（绿氨）合成催化剂 |
| CN114733551A (zh) * | 2022-05-06 | 2022-07-12 | 福州大学 | 一种高性能Ru基合成氨催化剂及其制备方法和应用 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1095906A2 (en) | 2001-05-02 |
| TWI225035B (en) | 2004-12-11 |
| CN1170770C (zh) | 2004-10-13 |
| EP1095906B1 (en) | 2004-12-29 |
| JP2001149780A (ja) | 2001-06-05 |
| AU779326B2 (en) | 2005-01-20 |
| CA2324328A1 (en) | 2001-04-29 |
| US6479027B1 (en) | 2002-11-12 |
| MXPA00010606A (es) | 2002-07-09 |
| US6764668B2 (en) | 2004-07-20 |
| EP1095906A3 (en) | 2002-03-20 |
| RU2247600C2 (ru) | 2005-03-10 |
| DE60017055T2 (de) | 2005-05-25 |
| ATE285992T1 (de) | 2005-01-15 |
| CA2324328C (en) | 2011-01-25 |
| KR20010051302A (ko) | 2001-06-25 |
| AU6959900A (en) | 2001-05-03 |
| ZA200006022B (en) | 2001-08-24 |
| US20030017097A1 (en) | 2003-01-23 |
| DE60017055D1 (de) | 2005-02-03 |
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