JP2017029979A - フィッシャー・トロプシュ反応における使用を意図した触媒の調製方法 - Google Patents
フィッシャー・トロプシュ反応における使用を意図した触媒の調製方法 Download PDFInfo
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- JP2017029979A JP2017029979A JP2016147915A JP2016147915A JP2017029979A JP 2017029979 A JP2017029979 A JP 2017029979A JP 2016147915 A JP2016147915 A JP 2016147915A JP 2016147915 A JP2016147915 A JP 2016147915A JP 2017029979 A JP2017029979 A JP 2017029979A
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- Prior art keywords
- reducing gas
- catalyst
- cobalt
- catalyst precursor
- comprised
- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 92
- 239000012018 catalyst precursor Substances 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910001868 water Inorganic materials 0.000 claims abstract description 45
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 40
- 239000001257 hydrogen Substances 0.000 claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000001354 calcination Methods 0.000 claims abstract description 23
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical class [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 15
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 38
- 229910017052 cobalt Inorganic materials 0.000 claims description 36
- 239000010941 cobalt Substances 0.000 claims description 36
- 150000002430 hydrocarbons Chemical class 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- 239000002808 molecular sieve Substances 0.000 claims description 9
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 6
- 229910052753 mercury Inorganic materials 0.000 claims description 6
- 238000002459 porosimetry Methods 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008246 gaseous mixture Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000000969 carrier Substances 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 description 56
- 230000015572 biosynthetic process Effects 0.000 description 21
- 238000003786 synthesis reaction Methods 0.000 description 21
- 229930195733 hydrocarbon Natural products 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000004215 Carbon black (E152) Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 238000005470 impregnation Methods 0.000 description 7
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- -1 Co 3 O 4 Chemical compound 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 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 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000002453 autothermal reforming Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000013529 heat transfer fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
- C07C1/04—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon monoxide with hydrogen
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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- C10G2/32—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts
- C10G2/33—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts characterised by the catalyst used
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- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
【解決手段】 反応器Iにおいて、硝酸コバルトの溶液で含浸された触媒担体を400°Cと450°Cの間に含まれる焼成温度で酸化し、酸化コバルトを含む触媒前駆体を製造する。次いで還元反応器Aにおいて、還元性ガスを流通させることによって、水素に富みかつ水分含有量の低い還元性ガスに該触媒前駆体を接触させ、該酸化コバルトをCoへ還元し、水を生成させる。次いで、反応器Aの出口で回収した水分含有還元性ガスの流れの水分含有量を200容量ppmに低下させ、該還元性ガスの少なくとも一部を反応器Aへリサイクルする。この方法において、該還元性ガスは反応器Aにおいて10,000容量ppm未満の水分含有量で維持される。
【選択図】図1
Description
b) 硝酸コバルトの溶液で含浸された該担体を400°Cと450°Cの間に含まれる焼成温度で酸化し、酸化コバルトを含む触媒前駆体を製造すること、
c) 少なくとも99容量%の水素と200容量ppm未満の水分を含む還元性ガスを準備すること、
d) 該触媒前駆体の床の上に該還元性ガスの流れを流通させることによって該触媒前駆体を該還元性ガスと接触させ、該酸化コバルトを金属コバルトへ還元し、還元された触媒と、水分を含む(laden with water)還元性ガスの流れとを生成すること、
e) 段階d)において回収された、水分を含む還元性ガスの流れの水分含有量を減少させ、200容量ppm未満の水分を含む還元性ガスの流れを形成すること、次いで、
f) 該還元性ガスの流れの少なくとも一部を段階d)へリサイクルこと、
段階d)において該還元性ガスは10,000容量ppm未満の水分含有量で維持される、方法。
おける
本発明方法は、コバルトで含浸された担体を用いることを提案する。
・ 該反応器Aにおける圧力.
・ 該反応器Aにおける温度、特に少なくとも1つの下記パラメータによって定義される温度、すなわち該温度勾配(gradient temperature)、該温度プラトー(temperature plateau)および該還元温度.
・ 該還元段階における期間.
・ 該反応器Aの内容量.
・ 該反応器A内の触媒前駆体の量.
一般に、該触媒前駆体の最適還元に要求される水素1の流量は、1 Nm3/h/kg触媒前駆体と6 Nm3/h/kg触媒前駆体の間、好ましくは2 Nm3/h/kg触媒前駆体と5 Nm3/h/kg触媒前駆体の間に含まれていてよい。反応器Aにおける該還元ガスの流量は、該還元ガス中の水を希釈するように、かつ、したがって反応器Aにおける該還元ガス中の水分含有量を10,000容量ppm未満、好ましくは5,000容量ppm未満、さらには4,000 容量ppm未満の含有量に減少させるように、増加されてよい。
参考例
本発明によるフィッシャー・トロプシュ触媒は、下記の段階を実施することによって調製される。
V2: 該還元された触媒のTPRの間に消費された水素の全体積[Nml/g]
V3: 該不動態化コバルト部分によって消費された水素の体積 [Nml/g] (該還元された触媒のTPR の500°Cでの初期値(default value)までの間に消費された水素の体積)
例えばOil & Gas Science and Technology, Rev. IFP, Vol. 64 (2009), No. 1, pp. 11-12に記載されているような昇温還元(TPR)。この技術に従って、触媒を水素の流れの下で加熱する。
実施例1
この実施例において、該参考例の該コバルト・ベース・フィッシャー・トロプシュ触媒前駆体を、水素中に水分含有量2容量%を含む還元性ガスで還元する。実施例1において該還元ガスの組成は変動する:該還元ガスは98容量%の水素と2容量%の水分を含む。
さらなる実施例において、該参考例のコバルト・ベース・フィッシャー・トロプシュ触媒前駆体の還元のために用いられるガスは 純水素ではなく、水素と窒素の混合物である。該還元性ガスは20容量%の窒素と80容量%の水素を含む。該還元性ガス中の窒素含有量の増大は、該触媒の還元率を減少させる作用を有する。フィッシャー・トロプシュ合成に使用された触媒の触媒成績は、本発明に従って調製された参考例触媒に対し、結果として、低下する。
さらなる実施例において、該還元段階の期間を短縮した。実施例3において、該最終還元温度での維持期間を半分、すなわち10時間に短縮し、実施例4において、該プラトーの期間を90%短縮し、すなわち2時間に短縮する。
Claims (15)
- フィッシャー・トロプシュ反応における使用を意図した触媒の調製方法であって、下記の連続する段階が実施される方法:
a) 硝酸コバルトの溶液で含浸された担体を準備すること、
b) 硝酸コバルトの溶液で含浸された該担体を400°Cと450°Cの間に含まれる焼成温度で酸化し、酸化コバルトを含む触媒前駆体を製造すること、
c) 少なくとも99容量%の水素と200容量ppm未満の水分を含む還元性ガスを準備すること、
d) 該触媒前駆体の床の上に該還元性ガスの流れを流通させることによって該触媒前駆体を該還元性ガスと接触させ、該酸化コバルトを金属コバルトへ還元し、還元された触媒と、水分を含む(laden with water)還元性ガスの流れとを生成すること、
e) 段階d)において回収された、水分を含む還元性ガスの流れの水分含有量を減少させ、200容量ppm未満の水分を含む還元性ガスの流れを形成すること、次いで、
f) 該還元性ガスの流れの少なくとも一部を段階d)へリサイクルこと、
段階d)において該還元性ガスは10,000容量ppm未満の水分含有量で維持される、方法。 - 請求項1に記載の方法において、段階d)において、還元性ガスの流量は1 Nm3/h/kg触媒前駆体と6 Nm3/h/kg触媒前駆体の間、好ましくは2 Nm3/h/kg触媒前駆体と5 Nm3/h/kg触媒前駆体の間に含まれている、方法。
- 請求項1または2に記載の方法において、段階d)は、0と1.5 MPa gの間、好ましくは0.3と1 MPa gの間に含まれる圧力で、かつ、350°Cと500°Cの間、好ましくは400°Cと450°Cの間に含まれる最終還元温度で行われる、方法。
- 請求項3に記載の方法において、段階d)は、該焼成温度未満の最終還元温度で行われる、方法。
- 請求項3または4に記載の方法において、段階d)において、還元性ガスの温度は、0.5°C/分と4°C/分の間、好ましくは0.5°C/分と3°C/分の間、さらには0.5°C/分と2°C/分の間に含まれる温度勾配に従って徐々に上昇させられる、方法。
- 請求項1〜5のいずれかに記載の方法において、段階b)において、該含浸された担体は、2時間超、好ましくは2時間と10時間の間に含まれる期間の間、該焼成温度に維持される、方法。
- 請求項1〜6のいずれかに記載の方法において、段階e)において、該還元性ガスは冷却され、該冷却によって凝縮された水分は除去される、方法。
- 請求項7に記載の方法において、段階e)において、さらに該還元性ガスを、水分を捕捉する少なくとも1つのモレキュラ・シーブに接触させる、方法。
- 請求項8に記載の方法において、該モレキュラ・シーブは、段階d)において回収された水分含有(water-laden)還元性ガスの流れの一部に同シーブを接触させることによって再生され、該一部は次いで段階e)の入口において該還元性ガスと一緒に導入される、方法。
- 請求項1〜9のいずれかに記載の方法において、段階d)において、該触媒前駆体は、5時間と24時間の間に含まれる期間の間、最終還元温度に維持される、方法。
- 請求項1〜10のいずれかに記載の方法において、酸化コバルトの少なくとも一部が金属コバルトに還元されるときは、該還元済み触媒は段階d)から取り出される、方法。
- 請求項1〜11いずれかに記載の方法において、該担体は、100m2/gと500m2/gの間、好ましくは150m2/gと300m2/gの間に含まれる比表面積、および、0.4ml/gと1.2ml/gの間に含まれる、水銀ポロシメトリーによって測定された細孔容積を有する多孔担体である、方法。
- 請求項1〜12のいずれかに記載の方法において、該担体は、アルミナ、シリカとアルミナとの混合物、シリカ、酸化チタンおよび酸化亜鉛からなる担体群から選ばれたものである、方法。
- 請求項1〜13のいずれかに記載の方法によって調製された触媒。
- 炭化水素化合物の製造方法であって、請求項14に記載の触媒、または請求項1〜13のいずれかに記載の方法によって調製された触媒が、水素と一酸化炭素とのガス状混合物に接触させられる、方法。
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