CN1575201A - 适于作为氢化催化剂前体的含铁氧化性物质 - Google Patents
适于作为氢化催化剂前体的含铁氧化性物质 Download PDFInfo
- Publication number
- CN1575201A CN1575201A CNA02821157XA CN02821157A CN1575201A CN 1575201 A CN1575201 A CN 1575201A CN A02821157X A CNA02821157X A CN A02821157XA CN 02821157 A CN02821157 A CN 02821157A CN 1575201 A CN1575201 A CN 1575201A
- Authority
- CN
- China
- Prior art keywords
- iron
- composition
- weight
- ferric
- precursor
- 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 19
- 239000012018 catalyst precursor Substances 0.000 title claims description 6
- 238000005984 hydrogenation reaction Methods 0.000 title abstract description 17
- 239000000463 material Substances 0.000 title abstract 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims description 42
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052728 basic metal Inorganic materials 0.000 claims description 6
- 150000003818 basic metals Chemical class 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000002829 reductive effect Effects 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 150000001341 alkaline earth metal compounds Chemical class 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical group 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 9
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 20
- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- KBMSFJFLSXLIDJ-UHFFFAOYSA-N 6-aminohexanenitrile Chemical compound NCCCCCC#N KBMSFJFLSXLIDJ-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 150000001412 amines Chemical class 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000009466 transformation Effects 0.000 description 5
- -1 2-amino methyl cyclopentyl Chemical group 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 125000005219 aminonitrile group Chemical group 0.000 description 4
- 239000003085 diluting agent Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 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 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 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
- 150000001721 carbon Chemical group 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 235000014413 iron hydroxide Nutrition 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052701 rubidium Inorganic materials 0.000 description 2
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 2
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 2
- RPMBPYXLPIWSFJ-UHFFFAOYSA-N 2-aminopentanenitrile Chemical compound CCCC(N)C#N RPMBPYXLPIWSFJ-UHFFFAOYSA-N 0.000 description 1
- XGYKKVTZDQDYJQ-UHFFFAOYSA-N 4-aminobutanenitrile Chemical compound NCCCC#N XGYKKVTZDQDYJQ-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- ZTOMUSMDRMJOTH-UHFFFAOYSA-N glutaronitrile Chemical compound N#CCCCC#N ZTOMUSMDRMJOTH-UHFFFAOYSA-N 0.000 description 1
- LLEVMYXEJUDBTA-UHFFFAOYSA-N heptanedinitrile Chemical compound N#CCCCCCC#N LLEVMYXEJUDBTA-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- BTNXBLUGMAMSSH-UHFFFAOYSA-N octanedinitrile Chemical compound N#CCCCCCCC#N BTNXBLUGMAMSSH-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical group [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- IAHFWCOBPZCAEA-UHFFFAOYSA-N succinonitrile Chemical compound N#CCCC#N IAHFWCOBPZCAEA-UHFFFAOYSA-N 0.000 description 1
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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
Abstract
Description
温度[℃] | ADN转化率[%] | ACN选择性[%] | HMD选择性[%] | ACN+HMD选择性[%] |
80 | 57.9 | 79.58 | 19.37 | 99.0 |
90 | 73.0 | 71.0 | 28.0 | 99.0 |
107 | 100.0 | 0.9 | 98.9 | 99.8 |
温度[℃] | ADN转化率[%] | ACN选择性[%] | HMD选择性[%] | ACN+HMD选择性[%] |
80 | 47.3 | 80.48 | 18.57 | 98.9 |
90 | 72.1 | 67.3 | 31.7 | 99.0 |
107 | 99.9 | 0.6 | 98.6 | 99.2 |
Claims (9)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10151558.8 | 2001-10-23 | ||
DE10151558A DE10151558A1 (de) | 2001-10-23 | 2001-10-23 | Als Katalysatorvorstufe geeignete oxidische Masse |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1575201A true CN1575201A (zh) | 2005-02-02 |
CN100494161C CN100494161C (zh) | 2009-06-03 |
Family
ID=7702989
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB02821157XA Ceased CN100494161C (zh) | 2001-10-23 | 2002-10-18 | 将腈氢化成胺的方法 |
Country Status (11)
Country | Link |
---|---|
US (1) | US7115781B2 (zh) |
EP (1) | EP1438130A1 (zh) |
JP (1) | JP2005506186A (zh) |
KR (1) | KR20040045888A (zh) |
CN (1) | CN100494161C (zh) |
AR (1) | AR037112A1 (zh) |
BR (1) | BR0213255A (zh) |
CA (1) | CA2463051A1 (zh) |
DE (1) | DE10151558A1 (zh) |
MX (1) | MXPA04003122A (zh) |
WO (1) | WO2003035249A1 (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108779060A (zh) * | 2016-02-16 | 2018-11-09 | 英威达纺织(英国)有限公司 | 用于选择性腈加氢的促进剂 |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9776175B2 (en) * | 2013-03-19 | 2017-10-03 | Korea Institute Of Energy Research | Iron-based catalyst and method for preparing the same and use thereof |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3125437A (en) * | 1964-03-17 | Method of briquetting iron ores | ||
US2292570A (en) * | 1938-11-12 | 1942-08-11 | Standard Catalytic Co | Process for the production of catalysts |
CA915707A (en) * | 1969-07-11 | 1972-11-28 | J. Kershaw Bernard | Hydrogenation of adiponitrile |
US4064172A (en) * | 1973-09-12 | 1977-12-20 | Imperial Chemical Industries Limited | Hexamethylene diamine by hydrogenation of adiponitrile in presence of an activated iron oxide catalyst |
GB1486890A (en) * | 1973-09-12 | 1977-09-28 | Ici Ltd | Catalysts and their use in hydrogenation |
GB8419851D0 (en) * | 1984-08-03 | 1984-09-05 | Ici Plc | Catalyst production |
US5846507A (en) * | 1994-05-26 | 1998-12-08 | Zhejiang University Of Technology | Fe1-x O-based catalyst for ammonia synthesis |
DE4446893A1 (de) * | 1994-12-27 | 1996-07-04 | Basf Ag | Verfahren zur Herstellung von aliphatischen alpha,omega-Aminonitrilen |
EP0925276B1 (de) * | 1996-09-10 | 2001-12-05 | Basf Aktiengesellschaft | Verfahren zur herstellung von aliphatischen alpha, omega-aminonitrilen |
DE19809687A1 (de) * | 1998-03-06 | 1999-09-09 | Basf Ag | Hydrierkatalysator |
-
2001
- 2001-10-23 DE DE10151558A patent/DE10151558A1/de not_active Withdrawn
-
2002
- 2002-10-18 EP EP02781268A patent/EP1438130A1/de not_active Ceased
- 2002-10-18 JP JP2003537804A patent/JP2005506186A/ja not_active Withdrawn
- 2002-10-18 AR ARP020103930A patent/AR037112A1/es unknown
- 2002-10-18 US US10/493,504 patent/US7115781B2/en not_active Expired - Fee Related
- 2002-10-18 KR KR10-2004-7005879A patent/KR20040045888A/ko not_active Application Discontinuation
- 2002-10-18 MX MXPA04003122A patent/MXPA04003122A/es not_active Application Discontinuation
- 2002-10-18 CN CNB02821157XA patent/CN100494161C/zh not_active Ceased
- 2002-10-18 WO PCT/EP2002/011667 patent/WO2003035249A1/de active Application Filing
- 2002-10-18 CA CA002463051A patent/CA2463051A1/en not_active Abandoned
- 2002-10-18 BR BR0213255-9A patent/BR0213255A/pt not_active IP Right Cessation
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108779060A (zh) * | 2016-02-16 | 2018-11-09 | 英威达纺织(英国)有限公司 | 用于选择性腈加氢的促进剂 |
CN108779060B (zh) * | 2016-02-16 | 2022-01-28 | 英威达纺织(英国)有限公司 | 用于选择性腈加氢的促进剂 |
Also Published As
Publication number | Publication date |
---|---|
JP2005506186A (ja) | 2005-03-03 |
WO2003035249A8 (de) | 2003-07-24 |
EP1438130A1 (de) | 2004-07-21 |
US7115781B2 (en) | 2006-10-03 |
CA2463051A1 (en) | 2003-05-01 |
CN100494161C (zh) | 2009-06-03 |
MXPA04003122A (es) | 2005-01-25 |
KR20040045888A (ko) | 2004-06-02 |
WO2003035249A1 (de) | 2003-05-01 |
BR0213255A (pt) | 2004-09-28 |
US20040254070A1 (en) | 2004-12-16 |
AR037112A1 (es) | 2004-10-20 |
DE10151558A1 (de) | 2003-04-30 |
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Owner name: BASF SE Free format text: FORMER OWNER: BASF AG Effective date: 20121128 |
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Effective date of registration: 20121128 Address after: Ludwigshafen, Germany Patentee after: BASF SE Address before: Ludwigshafen, Germany Patentee before: Basf AG |
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Decision date of declaring invalidation: 20130326 Decision number of declaring invalidation: 20171 Granted publication date: 20090603 |