TWI455759B - 使用於流通固定床反應器的具形狀催化劑體 - Google Patents
使用於流通固定床反應器的具形狀催化劑體 Download PDFInfo
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- TWI455759B TWI455759B TW100141786A TW100141786A TWI455759B TW I455759 B TWI455759 B TW I455759B TW 100141786 A TW100141786 A TW 100141786A TW 100141786 A TW100141786 A TW 100141786A TW I455759 B TWI455759 B TW I455759B
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- catalyst body
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- 239000003054 catalyst Substances 0.000 title claims 36
- 230000005484 gravity Effects 0.000 claims 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 claims 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 2
- 229930195733 hydrocarbon Natural products 0.000 claims 2
- 150000002430 hydrocarbons Chemical class 0.000 claims 2
- 229910052751 metal Inorganic materials 0.000 claims 2
- 239000002184 metal Substances 0.000 claims 2
- 238000007254 oxidation reaction Methods 0.000 claims 2
- 230000001590 oxidative effect Effects 0.000 claims 2
- 230000000737 periodic effect Effects 0.000 claims 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims 1
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 150000008064 anhydrides Chemical class 0.000 claims 1
- 239000001273 butane Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 claims 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- 150000002484 inorganic compounds Chemical class 0.000 claims 1
- 229910010272 inorganic material Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910044991 metal oxide Inorganic materials 0.000 claims 1
- 150000004706 metal oxides Chemical class 0.000 claims 1
- 150000002739 metals Chemical class 0.000 claims 1
- 229910003455 mixed metal oxide Inorganic materials 0.000 claims 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims 1
- 150000002894 organic compounds Chemical class 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 239000010970 precious metal Substances 0.000 claims 1
- 239000001294 propane Substances 0.000 claims 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 claims 1
Classifications
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- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/195—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium or tantalum
- B01J27/198—Vanadium
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
- C07C45/34—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds
- C07C45/35—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds in propene or isobutene
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/215—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of saturated hydrocarbyl groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/25—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of unsaturated compounds containing no six-membered aromatic ring
- C07C51/252—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of unsaturated compounds containing no six-membered aromatic ring of propene, butenes, acrolein or methacrolein
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/60—Two oxygen atoms, e.g. succinic anhydride
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/13—Hollow or container type article [e.g., tube, vase, etc.]
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Claims (17)
- 一種具形狀催化劑體,其係使用於有機化合物及無機化合物於固定床反應器中之催化轉化,其中該具形狀催化劑體(100;200;300;400)形成為具有底部(150)、圓柱體表面(152)、圓柱體軸(154)及至少一個與該圓柱體軸平行延伸之連續開口(160)的圓柱體,且該圓柱體之該底部具有至少4個轉角(110、120、130、140;210、220、230、240;310、320、330、340;410、420、430、440),且封閉該具形狀催化劑體之幾何底部體為稜柱(10),其具有存在長度及寬度之稜柱底部,其中該長度大於該寬度。
- 如申請專利範圍第1項之具形狀催化劑體,其中在兩個相鄰轉角之間的該圓柱體表面中設置凹區(172),及/或在兩個相鄰轉角之間的該圓柱體表面中設置突起(170)。
- 如申請專利範圍第1項之具形狀催化劑體,其中該具形狀催化劑體具有與該圓柱體軸及/或4個轉角平行延伸之開口(160);及/或其中該具形狀催化劑體具有兩個彼此相對排列之凹區及/或兩個彼此相對排列之突起。
- 如申請專利範圍第2項之具形狀催化劑體,其中該具形狀催化劑體具有與該圓柱體軸及/或4個轉角平行延伸之開口(160);及/或其中該具形狀催化劑體具有兩個彼此相對排列之凹區及/或兩個彼此相對排列之突起。
- 如申請專利範圍第1項之具形狀催化劑體, 其中該具形狀催化劑體具有1mm-1 至1.8mm-1 之該具形狀催化劑體之幾何表面積與該具形狀催化劑體之體積的比率;及/或其中至少一個選自該等轉角、該凹區、該等凹區、該突起及該等突起之元件為圓形。
- 如申請專利範圍第2項之具形狀催化劑體,其中該具形狀催化劑體具有1mm-1 至1.8mm-1 之該具形狀催化劑體之幾何表面積與該具形狀催化劑體之體積的比率;及/或其中至少一個選自該等轉角、該凹區、該等凹區、該突起及該等突起之元件為圓形。
- 如申請專利範圍第4項之具形狀催化劑體,其中該具形狀催化劑體具有1mm-1 至1.8mm-1 之該具形狀催化劑體之幾何表面積與該具形狀催化劑體之體積的比率;及/或其中至少一個選自該等轉角、該凹區、該等凹區、該突起及該等突起之元件為圓形。
- 如申請專利範圍第1項之具形狀催化劑體,其中該稜柱(10)為立方體;及/或其中該具形狀催化劑體之體積與該周圍立方體之體積的比率在不考慮該至少一個開口時大於80%且在考慮該至少一個開口時大於70%;及/或其中該等轉角由該稜柱底部之稜柱轉角封閉;及/或其中兩個轉角界定該稜柱底部之長度及/或兩個轉角界 定該稜柱底部之寬度。
- 如申請專利範圍第2項之具形狀催化劑體,其中該突起或該等突起設置在界定該長度之轉角之間,及/或該凹區或該等凹區設置在界定該寬度之轉角之間。
- 如申請專利範圍第7項之具形狀催化劑體,其中該等轉角為圓形,各自具有重心(180),及/或該等轉角中之至少兩者彼此不同;及/或其中該重心在各情況下距該圓柱體軸1.5mm至5mm,較佳2.5mm至4mm;及/或其中該等圓形轉角具有在1mm至2mm範圍內的制圓直徑;及/或其中由該等圓形轉角所形成之各別圓弧之半徑在0.5mm至2.5mm範圍內;及/或其中由該等圓形突起所形成之各別圓弧之半徑在2mm至3.5mm範圍內;及/或其中由該等圓形凹區所形成之各別圓弧之半徑在1mm至9mm範圍內。
- 如申請專利範圍第10項之具形狀催化劑體,其中該等轉角排列於該底部中以使得通過界定該稜柱底部之該寬度之兩個轉角之該等重心的直線上的垂線與通過此等轉角之該重心且通過該圓柱體軸之直線之間的角度為10°至75°,較佳為25°至60°。
- 如申請專利範圍第1項之具形狀催化劑體,其中該具形狀催化劑體之平行於該圓柱體軸之尺寸或高度為2mm 至20mm,較佳為3mm至6mm;及/或其中該稜柱底部之該長度為2mm至10mm,較佳為4mm至8mm。
- 如申請專利範圍第3項之具形狀催化劑體,其中該圓柱體之外徑或兩個相對凹區之間的距離為3mm至10mm,較佳為5mm至8mm;及/或其中該開口之直徑為0.5mm至4mm,較佳為1mm至3mm。
- 如申請專利範圍第1項之具形狀催化劑體,其中該具形狀催化劑體之容積密度小於0.75kg/l;及/或其中平均單向側向抗壓強度大於28N及/或不同平均單向側向抗壓強度大於70N。
- 如申請專利範圍第1項之具形狀催化劑體,其包含:至少一種選自釩與磷之混合氧化物、一或多種週期表副族金屬、週期表副族金屬之金屬氧化物或混合金屬氧化物及一或多種貴金屬的元素。
- 如申請專利範圍第1項之具形狀催化劑體,其包含至少一種選自氧化鋁、二氧化矽、矽酸鋁、二氧化鋯及二氧化鈦的元素。
- 一種如申請專利範圍第1項至第16項中任一項之具形狀催化劑體之用途,其係用於部分氧化反應、一或多種烴之部分氧化反應、由烴或正丁烷製造順丁烯二酸酐、藉由在乙酸存在下對乙烯進行氧化來製造乙酸乙烯酯單體、或將丙烯或丙烷氧化成丙烯醛及/或丙烯酸。
Applications Claiming Priority (1)
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DE102010052126A DE102010052126A1 (de) | 2010-11-22 | 2010-11-22 | Katalysatorformkörper für durchströmte Festbettreaktoren |
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TW201223641A TW201223641A (en) | 2012-06-16 |
TWI455759B true TWI455759B (zh) | 2014-10-11 |
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TW100141786A TWI455759B (zh) | 2010-11-22 | 2011-11-16 | 使用於流通固定床反應器的具形狀催化劑體 |
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US (1) | US9409160B2 (zh) |
EP (1) | EP2643086B1 (zh) |
CN (1) | CN103269798B (zh) |
DE (1) | DE102010052126A1 (zh) |
ES (1) | ES2737431T3 (zh) |
HU (1) | HUE046812T2 (zh) |
TW (1) | TWI455759B (zh) |
WO (1) | WO2012069481A1 (zh) |
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DE102014004786B4 (de) | 2014-04-02 | 2021-09-30 | Clariant International Ltd. | Alkalimetall-modifizierter Vanadium-Phosphor-Oxid (VPO)-Katalysator |
EP2985075A1 (en) | 2014-08-15 | 2016-02-17 | Basf Se | Shaped body made of a porous material |
CN104741110A (zh) * | 2015-03-25 | 2015-07-01 | 襄阳市精信催化剂有限责任公司 | 二氧化硫氧化制备硫酸催化剂的工艺 |
RU2722157C1 (ru) * | 2015-07-22 | 2020-05-27 | Басф Корпорейшн | Катализаторы с высокой геометрической площадью поверхности для получения винилацетатного мономера |
EP3320971A1 (de) * | 2016-11-15 | 2018-05-16 | Basf Se | Mechanisch stabiler katalysator zur hydrierung von carbonylverbindungen und verfahren zu dessen herstellung |
CN110461468B (zh) | 2017-03-27 | 2022-10-14 | 三菱化学株式会社 | 催化剂以及催化剂组 |
US11547989B2 (en) | 2018-02-12 | 2023-01-10 | Huntsman Petrochemical Llc | Cored round trilobe shaped catalyst for producing maleic anhydride |
DE102019127788A1 (de) * | 2019-10-15 | 2021-04-15 | Clariant International Ltd. | Neues Reaktorsystem für die Herstellung von Maleinsäureanhydrid durch katalytische Oxidation von n-Butan |
DE102019127790A1 (de) * | 2019-10-15 | 2021-04-15 | Clariant International Ltd | Neues Katalysatorsystem für die Herstellung von Maleinsäureanhydrid durch katalytische Oxidation von n-Butan |
JP2022554292A (ja) | 2019-10-31 | 2022-12-28 | 中国石油化工股▲ふん▼有限公司 | 担持触媒、その調製方法およびその適用 |
WO2021239483A1 (en) | 2020-05-26 | 2021-12-02 | Basf Se | Shaped catalyst body with improved properties, its preparation and use |
JP2023531736A (ja) | 2020-06-26 | 2023-07-25 | ビーエーエスエフ ソシエタス・ヨーロピア | 多孔質触媒支持体成形体 |
EP4359123A1 (en) | 2021-06-25 | 2024-05-01 | Basf Se | High purity tableted alpha-alumina catalyst support |
US11731120B1 (en) | 2022-03-11 | 2023-08-22 | Saudi Arabian Oil Company | Lobular catalyst structure and reactor for hydrocarbon conversion by hot and compressed water based processes |
WO2024079247A1 (en) | 2022-10-12 | 2024-04-18 | Basf Se | Epoxidation catalyst |
WO2024084002A1 (en) | 2022-10-21 | 2024-04-25 | Clariant International Ltd | Mechanically stable vpo catalyst and process for the production thereof |
EP4357019A1 (de) | 2022-10-21 | 2024-04-24 | Clariant International Ltd | Vpo-katalysator mit verbesserter selektivität und stabilität sowie verfahren zu dessen herstellung |
DE102022004204A1 (de) | 2022-11-12 | 2024-05-23 | Hans-Jürgen Eberle | Vefahren zur Herstellung von Maleinsäureanhydrid |
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DE3930533C1 (zh) * | 1989-09-13 | 1991-05-08 | Degussa Ag, 6000 Frankfurt, De | |
DE3930534A1 (de) | 1989-09-13 | 1991-03-21 | Degussa | Verfahren zur herstellung von acrolein durch katalytische gasphasenoxidation von propen |
DE3935073A1 (de) * | 1989-10-20 | 1991-04-25 | Sued Chemie Ag | Verfahren zur katalytischen dehydrierung von kohlenwasserstoffen, insbesondere von alkylaromaten |
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2010
- 2010-11-22 DE DE102010052126A patent/DE102010052126A1/de not_active Withdrawn
-
2011
- 2011-11-16 TW TW100141786A patent/TWI455759B/zh active
- 2011-11-22 EP EP11793371.3A patent/EP2643086B1/de active Active
- 2011-11-22 US US13/988,583 patent/US9409160B2/en active Active
- 2011-11-22 ES ES11793371T patent/ES2737431T3/es active Active
- 2011-11-22 HU HUE11793371A patent/HUE046812T2/hu unknown
- 2011-11-22 WO PCT/EP2011/070695 patent/WO2012069481A1/de active Application Filing
- 2011-11-22 CN CN201180055916.1A patent/CN103269798B/zh active Active
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US3966644A (en) * | 1973-08-03 | 1976-06-29 | American Cyanamid Company | Shaped catalyst particles |
US4441990A (en) * | 1982-05-28 | 1984-04-10 | Mobil Oil Corporation | Hollow shaped catalytic extrudates |
Also Published As
Publication number | Publication date |
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CN103269798B (zh) | 2016-08-03 |
DE102010052126A1 (de) | 2012-05-24 |
EP2643086A1 (de) | 2013-10-02 |
CN103269798A (zh) | 2013-08-28 |
HUE046812T2 (hu) | 2020-03-30 |
TW201223641A (en) | 2012-06-16 |
EP2643086B1 (de) | 2019-06-19 |
US20130338378A1 (en) | 2013-12-19 |
US9409160B2 (en) | 2016-08-09 |
ES2737431T3 (es) | 2020-01-14 |
WO2012069481A1 (de) | 2012-05-31 |
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