JP2007520337A - 構造的に強化された分解触媒 - Google Patents
構造的に強化された分解触媒 Download PDFInfo
- Publication number
- JP2007520337A JP2007520337A JP2006551280A JP2006551280A JP2007520337A JP 2007520337 A JP2007520337 A JP 2007520337A JP 2006551280 A JP2006551280 A JP 2006551280A JP 2006551280 A JP2006551280 A JP 2006551280A JP 2007520337 A JP2007520337 A JP 2007520337A
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- JP
- Japan
- Prior art keywords
- catalyst
- zeolite
- kaolin
- microspheres
- matrix
- 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
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 243
- 238000005336 cracking Methods 0.000 title claims description 21
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 210
- 239000004005 microsphere Substances 0.000 claims abstract description 159
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 155
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 153
- 239000010457 zeolite Substances 0.000 claims abstract description 150
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 145
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 143
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 104
- 239000011159 matrix material Substances 0.000 claims abstract description 101
- 239000011148 porous material Substances 0.000 claims abstract description 86
- 238000000034 method Methods 0.000 claims description 72
- 230000008569 process Effects 0.000 claims description 34
- 239000013078 crystal Substances 0.000 claims description 23
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 19
- 229910052753 mercury Inorganic materials 0.000 claims description 19
- 238000011065 in-situ storage Methods 0.000 claims description 18
- 239000012013 faujasite Substances 0.000 claims description 17
- 229930195733 hydrocarbon Natural products 0.000 claims description 15
- 150000002430 hydrocarbons Chemical class 0.000 claims description 15
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- 238000004231 fluid catalytic cracking Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 4
- 230000001747 exhibiting effect Effects 0.000 claims description 3
- RREGISFBPQOLTM-UHFFFAOYSA-N alumane;trihydrate Chemical compound O.O.O.[AlH3] RREGISFBPQOLTM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002002 slurry Substances 0.000 description 59
- 239000000463 material Substances 0.000 description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 52
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 45
- 229910052863 mullite Inorganic materials 0.000 description 45
- 239000000203 mixture Substances 0.000 description 44
- 239000000047 product Substances 0.000 description 44
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 35
- 238000002425 crystallisation Methods 0.000 description 32
- 230000008025 crystallization Effects 0.000 description 32
- 239000007787 solid Substances 0.000 description 32
- 239000011734 sodium Substances 0.000 description 29
- 230000000694 effects Effects 0.000 description 27
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 26
- 239000004115 Sodium Silicate Substances 0.000 description 25
- 229910052911 sodium silicate Inorganic materials 0.000 description 25
- 238000001354 calcination Methods 0.000 description 24
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- 239000002245 particle Substances 0.000 description 23
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 18
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000000227 grinding Methods 0.000 description 9
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- 229910052782 aluminium Inorganic materials 0.000 description 8
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- 238000009792 diffusion process Methods 0.000 description 7
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 7
- 239000012452 mother liquor Substances 0.000 description 7
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910002796 Si–Al Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 6
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- 230000007062 hydrolysis Effects 0.000 description 6
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- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 230000002829 reductive effect Effects 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
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- 239000008186 active pharmaceutical agent Substances 0.000 description 4
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
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- 229910052742 iron Inorganic materials 0.000 description 4
- 235000015097 nutrients Nutrition 0.000 description 4
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
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- 238000006386 neutralization reaction Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920003091 Methocel™ Polymers 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- XFBXDGLHUSUNMG-UHFFFAOYSA-N alumane;hydrate Chemical class O.[AlH3] XFBXDGLHUSUNMG-UHFFFAOYSA-N 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
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- PMYUVOOOQDGQNW-UHFFFAOYSA-N hexasodium;trioxido(trioxidosilyloxy)silane Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] PMYUVOOOQDGQNW-UHFFFAOYSA-N 0.000 description 2
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
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- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 1
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
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- 241001330988 Palmyra Species 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
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- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
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Classifications
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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Abstract
Description
「マトリックスはシーブの中に存在するナトリウムの吸込みとして働くことでマトリックス触媒の中のゼオライト粒子に安定性を加えると言われている。前記マトリックスは下記の追加的機能を果たす:ゼオライトを希釈する機能;それを熱および蒸気および機械的摩滅に対して安定にする機能;ゼオライトを最大能力で使用することができかつ再生を容易に行うことができるように高い間隙率を与える機能;そして最後に、再生および分解中の伝熱そして大規模な接触分解中の熱貯蔵にとって重要であるバルク特性(bulk properties)を与える機能。」
従来技術の流動接触分解触媒では、下記の2つの一般的技術の中の1つを用いて活性ゼオライト系成分を当該触媒の微小球の中に取り込ませている。1つの技術では、ゼオライト系成分を結晶化させた後に個別の段階で微小球の中に取り込ませる。2番目の技術、即ちインサイチュ技術では、最初に微小球を生じさせた後にゼオライト系成分を前記微小球自身の中で結晶化させることでゼオライト系成分と非ゼオライト系成分の両方を含有する微小球を生じさせる。
発明の詳細な説明
本発明の触媒微小球は、共通譲渡の特許文献1に開示されている如き一般的方法を用いて製造したものである。重要なことは、本発明の触媒のアルミナが豊富な非ゼオライト系マトリックスを好適には粒子の少なくとも90重量%が2.0ミクロン未満、好適には少なくとも90重量%が1ミクロン未満の超微細粉末形態の含水カオリン源から生じさせることにある。その超微細含水カオリンに粉砕そして発熱を経る焼成を受けさせる。典型的なゼオライト微小球は、大きさが本発明で用いるそれよりも大きなカオリンから生じさせたアルミナが豊富なマトリックスを用いて生じさせた微小球であり、これの特徴的な発熱により少なくとも実質的に焼成されている。Satintone(商標)No.1(ムライトが実質的に全く生じないような特徴的な発熱を経る焼成を受けた市販カオリン)がアルミナが豊富なマトリックスを生じさせる目的で商業ベースで最初に用いた材料である。Satintone(商標)No.1は、粒子の70%が2ミクロン未満の含水カオリンを用いて作られたものである。アルミナが豊富なマトリックスを生じさせる目的で用いる他の源には、特徴的な発熱により少なくとも実質的焼成を受けた微細な含水カオリン[例えばASP(商標)600、即ち表題が「Aluminum Silicate Pigments」(EC−1167)のEngelhard Technical Bulletin No.TI−1004に記述されている市販含水カオリン]が含まれる。ブックレットカオリン(Booklet kaolin)が最も普及して商業的に用いられていて世界規模で多大な効果を満たしている。本発明以前では、そのようなより大きなカオリン粒子が触媒微小球のアルミナが豊富なマトリックスを生じさせる時の最新技術に相当しておりかつ欠点を持たないと考えられていた。
[実施例1]
[実施例2]
[実施例3]
[実施例4−6]
実施例1−3の微小球に通常手順(特許文献1および米国特許5,395,809)による結晶化を23時間受けさせることでゼオライトYを生じさせ、下記の結果を得た。その種晶は米国特許4,631,262に記述されている種晶である。
[実施例7]
[実施例8]
[実施例9]
[実施例10]
米国特許第6,069,012号に実質的に記述されているようにインジェクターの位置が2.125”のACE(商標)微小規模固定式流動床装置を用いて、これを表面WHSVを8にして980度Fで操作し、触媒を9グラムおよびガスオイルA供給材料(表5)を用いることで、触媒性能を測定した。前記特許には前記インジェクターの位置はライザー滞留時間が2−2.5秒であることに相当すると示唆されている。触媒ストリップ時間を575秒に一定に保った。実施例8および9の触媒をBrownが特許文献1で開示した如き活性調節用微小球で希釈した。しかしながら、米国特許第6,069,012号の教示および通常の反応工学への忠実さが保たれたままであるようにする目的で、いろいろな触媒に評価を床容積を一定にして受けさせるべきであることは明らかである。それによって、比較を行う時の蒸気滞留時間が一定であることが確保される。それを行う目的で前記触媒配合物をABDが等しくなるように混合して、それらに試験を一定の重量で受けさせた。Brownが示した活性調節用微小球(ABDが約0.98)および実施例3の微小球(ABDが0.53)を適切な量で用いることでそれを実施した。
[実施例12]
[実施例14]
[実施例15]
[実施例16]
[実施例17]
発泡アルミナホスト材料の調製:
General(商標)ミキサーのボウルの中にCatapal(商標)プソイドベーマイトを1152g入れた。水中1.5%のMethocel(商標)溶液を1188g調製した後、これに酢酸を72g添加した。その一緒にした溶液を前記Catapal(商標)アルミナに混合しながらゆっくり添加した後、それを高速で20分間混合した。次に、水を更に150g用いて前記混合物をDenverミキサーに移した後、高速で更に15分間混合した。次に、1.5%のMethocel(商標)溶液を更に840g、酢酸を10gおよび水を150ml加えた後、混合を更に10分間継続した。次に、この材料を前記ミキサーから取り出した後、600gのCabot発泡アルミナをゆっくり加え、そして前記混合物をスープ状に保持するに充分な量の水と一緒にして手で混合した。高せん断機械的混合も低せん断機械的混合も実施しなかった。次に、そのベーマイトで発泡したアルミナ混合物に乾燥をケーキとし受けさせた後、焼成を500℃で3時間受けさせた。次に、その焼成を受けさせたケーキをJaw Crusherおよび粉砕機でメッシュサイズが−40/+230の画分がふるいで保持されるように粉砕することでFCCの粒子サイズになるまで小さくした。総水銀細孔容積は0.96cc/gであった。
発泡アルミナホストの中のゼオライトYの結晶化:
1リットルの樹脂製ケトルに脱イオン水を480部、44重量%の二ケイ酸ナトリウム溶液を220部、開始剤(種晶)(名目上、ケイ酸ナトリウム中0.5%のAl2O3)を56部、この上に示したようにして生じさせた発泡アルミナを80部およびシリカゲルを19部加えた。次に、この反応槽に撹拌機、還流冷却器および熱電対を取り付けた後、それを205度Fに30分間加熱した。その温度に到達した時点でメタカオリン微小球を34.3部添加した後、温度を205度Fに16から20時間、即ち分離した固体のゼオライトY含有量がX線回折で最大限に到達するまで維持した。次に、その反応混合物を濾過し、反応混合物の体積の2倍の量の脱イオン水で洗浄した後、空気の温度が120℃のオーブンの中で乾燥させた。その乾燥させた生成物の一部を保持し、そしてその残りを200メッシュのスクリーンでふるい分けすることで2画分に分けた。各々をX線回折で分析した。
Claims (10)
- ゼオライトの結晶が多孔質のアルミナ含有マトリックスの表面を覆う層として含まれているが、前記ゼオライトで被覆されているマトリックスが孔を形成する形態で配置していて、前記ゼオライトの層が前記孔の壁の上に形成されているゼオライト系FCC触媒であって、直径が40−20,000Åの孔に関して0.27cc/gより高い水銀間隙率を示しかつ結晶化したゼオライトを少なくとも40重量%含有するゼオライト系FC触媒。
- ゼオライトの結晶がカオリン以外のアルミナ源に本質的に由来する多孔質のアルミナ含有マトリックスの表面を覆う層として含まれているが、前記ゼオライトで被覆されているマトリックスが孔を形成する形態で配置していて、前記ゼオライトの層が前記孔の壁の上に形成されているゼオライト系FCC触媒であって、直径が40−20,000Åの孔に関して0.20cc/gより高い水銀間隙率を示すゼオライト系FCC触媒。
- 前記ゼオライトがゼオライトYである請求項2記載の触媒。
- 直径が40−20,000Åの孔に関して少なくとも0.30cc/gの水銀間隙率を示す請求項2記載の触媒。
- 前記ゼオライトを前記マトリックスの表面の上でインサイチュで結晶化させたものである請求項2記載の触媒。
- 前記多孔質マトリックスが直径が少なくとも600Åの所にピークを有するとして特徴づけられるモード分布を示す孔を含有する請求項2記載の触媒。
- 直径が600−20,000Åの孔に関して少なくとも0.10cc/gの水銀間隙率を示す請求項2記載の触媒。
- 前記アルミナ源が三水化アルミニウムに由来する請求項2記載の触媒。
- インサイチュで結晶化したY−ホージャサイトを含有しかつ直径が40−20,000Åの範囲内の孔に関して約0.20cc/gより高い水銀間隙率を示す微小球を含んで成る流動接触分解触媒であって、前記微小球がカオリン以外のアルミナ源に本質的に由来するアルミナ−マトリックスを含んで成る触媒。
- 炭化水素原料をFCC条件下で分解する方法であって、前記炭化水素原料を請求項1、2、または9記載の触媒に接触させることを含んで成る方法。
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Also Published As
Publication number | Publication date |
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KR101121608B1 (ko) | 2012-03-13 |
KR20070001987A (ko) | 2007-01-04 |
EP1711261A1 (en) | 2006-10-18 |
JP5469294B2 (ja) | 2014-04-16 |
TW200538539A (en) | 2005-12-01 |
CN1913965A (zh) | 2007-02-14 |
WO2005077530A1 (en) | 2005-08-25 |
AU2005212160A1 (en) | 2005-08-25 |
US6942784B2 (en) | 2005-09-13 |
BRPI0507405A (pt) | 2007-06-26 |
US20040220046A1 (en) | 2004-11-04 |
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