JP2010149114A - 水素化脱金属および水素化脱硫用触媒、ならびに連結方法における単一調合の使用 - Google Patents
水素化脱金属および水素化脱硫用触媒、ならびに連結方法における単一調合の使用 Download PDFInfo
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- JP2010149114A JP2010149114A JP2009287005A JP2009287005A JP2010149114A JP 2010149114 A JP2010149114 A JP 2010149114A JP 2009287005 A JP2009287005 A JP 2009287005A JP 2009287005 A JP2009287005 A JP 2009287005A JP 2010149114 A JP2010149114 A JP 2010149114A
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- 238000009472 formulation Methods 0.000 title description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 135
- 239000002184 metal Substances 0.000 claims abstract description 135
- 150000002739 metals Chemical class 0.000 claims abstract description 82
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 20
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 20
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 77
- 239000011148 porous material Substances 0.000 claims description 41
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 35
- 229910052750 molybdenum Inorganic materials 0.000 claims description 35
- 239000011733 molybdenum Substances 0.000 claims description 35
- 229910052759 nickel Inorganic materials 0.000 claims description 27
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 26
- 239000011574 phosphorus Substances 0.000 claims description 26
- 229910052698 phosphorus Inorganic materials 0.000 claims description 26
- 239000010941 cobalt Substances 0.000 claims description 22
- 229910017052 cobalt Inorganic materials 0.000 claims description 22
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 22
- 239000003245 coal Substances 0.000 claims description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 11
- 229910052796 boron Inorganic materials 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
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- 101100132433 Arabidopsis thaliana VIII-1 gene Proteins 0.000 abstract 3
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- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 16
- 238000005470 impregnation Methods 0.000 description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 12
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- 229910052717 sulfur Inorganic materials 0.000 description 12
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- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 8
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- 229910000147 aluminium phosphate Inorganic materials 0.000 description 7
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- 150000001868 cobalt Chemical class 0.000 description 6
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- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 6
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000003125 aqueous solvent Substances 0.000 description 2
- 229910001593 boehmite Inorganic materials 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 229960002645 boric acid Drugs 0.000 description 2
- 235000010338 boric acid Nutrition 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 238000007324 demetalation reaction Methods 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
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- 239000002019 doping agent Substances 0.000 description 2
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- 239000000446 fuel Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 description 2
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
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- 238000007670 refining Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 241001070941 Castanea Species 0.000 description 1
- 235000014036 Castanea Nutrition 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 241000640882 Condea Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-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
- 229910003294 NiMo Inorganic materials 0.000 description 1
- HOGKWLXRMABQDU-UHFFFAOYSA-N OB(O)OB(O)O.N.N.N.N Chemical compound OB(O)OB(O)O.N.N.N.N HOGKWLXRMABQDU-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 241000071415 Vibone Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical class [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 150000001649 bromium compounds Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- NKCVNYJQLIWBHK-UHFFFAOYSA-N carbonodiperoxoic acid Chemical compound OOC(=O)OO NKCVNYJQLIWBHK-UHFFFAOYSA-N 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- VLXBWPOEOIIREY-UHFFFAOYSA-N dimethyl diselenide Natural products C[Se][Se]C VLXBWPOEOIIREY-UHFFFAOYSA-N 0.000 description 1
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000004231 fluid catalytic cracking Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- JCCNYMKQOSZNPW-UHFFFAOYSA-N loratadine Chemical compound C1CN(C(=O)OCC)CCC1=C1C2=NC=CC=C2CCC2=CC(Cl)=CC=C21 JCCNYMKQOSZNPW-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003791 organic solvent mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
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- 238000001812 pycnometry Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000003476 subbituminous coal Substances 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000009736 wetting Methods 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/883—Molybdenum and nickel
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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Abstract
【解決手段】第VIB族からの少なくとも1種の金属と、主要プロモータVIII-1および共プロモータVIII-i(iは2〜5の範囲である)と称される第VIII族からの少なくとも2種の金属と、多孔性の耐火性酸化物によって構成された少なくとも1種の担体とを含み、第VIII族からの元素は、原子比[VIII-1/(VIII-1+・・・+VIII-i)]によって規定される比で存在し、該比は、0.5〜0.85の範囲である、触媒、並びに、重質炭化水素仕込原料の水素化処理方法であって、少なくとも1回の水素化脱金属工程と少なくとも1回の水素化脱硫工程とを包含し、水素化脱金属および水素化脱硫の工程のそれぞれにおいて同一の原子比を有する本発明による触媒を使用する。
【選択図】なし
Description
「d」は細孔径(nm)を表し、
tは表面張力(48.5Pa)であり、
θは接触角(θ=140゜)であり、
Pは圧力(MPa)である。
本発明者らは、アルミナをベースとする担体Aを調製し、同一の形成された担体から下記実施例において記載されるような触媒を調製することができるようにした。この目的で、本発明者らは、ベーマイトまたはLa Roche ChemicalsによってVersal(登録商標) 250の商標名で市販されているアルミナゲルから構成された基質を使用した。このゲルは、52.7%の硝酸(乾燥ゲルの重量(g)当たり酸1重量%)を含有する水溶液と混練され、Z形アーム付き混練機(Aoustin MX2)中で20分間混練された。次いで、ペースト状物は、20.3%のアンモニアを含有する水溶液(酸のモル当たりアンモニア40モル%)と5分間にわたって同一の混練機において混練された。この混練の終了時に、ペースト状物は、ピストン式押出機(Retma)を用いて、内径2.0mmの三葉形オリフィスを有するダイ中を通された。次いで、押出物は、120℃で終夜乾燥させられ、乾燥空気の重量(kg)当たり200gの水を含有する湿潤空気の流れの中で700℃で2時間にわたって焼成された。
本発明者らは、アルミナをベースとする担体Bを調製して、形成された同担体から以下の実施例に記載されるようにして触媒を調製することができるようにした。この目的で、Condea Chemie GmbHによって商標名SB3で販売されている平板状ベーマイトから構成された基質が、66%硝酸を含有する溶液と混合され(乾燥ゲルの重量(グラム)当たり酸7重量%)、次いで15分間にわたって混練された。この混練の後、得られたペースト状物は、1.5mmの内径を有する三葉形オリフィスを有するダイ中を通された。次いで、押出物は、120℃で終夜乾燥させられ、7.5容積%の水を含有する湿潤空気の流れの中550℃で2時間にわたって焼成された。1.3mmの径を有する三葉形押出物がこうして得られ、このものは、比表面積245m2/g、全細孔容積0.65ml/g、11nmを中心としたメソ孔分布を有していた。それ故に、担体Bは、全細孔容積の0%のマクロ孔容積を有していた。
本発明者らは、実施例1からのバイモーダル担体Aの乾式含浸を行った。含浸用水溶液は、モリブデン、ニッケルおよびコバルトの塩のほかリン酸(H3PO4)および過酸化水素(H2O2)を含んでいた。モリブデン塩は七モリブデン酸アンモニウムMo7O24(NH4)6・4H2Oであり、ニッケル(コバルト)塩は硝酸ニッケル(コバルト)Ni(NO3)2・6H2O(Co(NO3)2・6H2O)であった。溶液中のこれらの塩のそれぞれの量は、所望量の各元素を担体表面に固定するように決定された。
本発明者らは、表1に示される特徴を有する上記担体Aに乾式含浸させた。含浸用水溶液は、モリブデン、ニッケルおよびコバルトの塩のほかリン酸(H3PO4)および過酸化水素(H2O2)を含んでいた。モリブデン塩は七モリブデン酸アンモニウムMo7O24(NH4)6・4H2Oであり、ニッケル(コバルト)塩は硝酸ニッケル(コバルト)Ni(NO3)2・6H2O(Co(NO3)2・6H2O)であった。溶液中のこれらの塩のそれぞれの量は、所望量の各元素を担体表面に固定するように決定された。
本発明者らは、表1に示される特徴を有する上記担体Aに乾式含浸させた。含浸用水溶液は、モリブデンおよびニッケルの塩のほかリン酸(H3PO4)および過酸化水素(H2O2)を含んでいた。モリブデン塩は七モリブデン酸アンモニウムMo7O24(NH4)6・4H2Oであり、ニッケル塩は硝酸ニッケルNi(NO3)2・6H2Oであった。溶液中のこれらの塩のそれぞれの量は、所望量の各元素を担体表面に固定するように決定された。
本発明者らは、マクロ多孔度を有しておらず且つ表1に示される特徴を有していた担体Bに乾式含浸させた。含浸用水溶液は、モリブデン、ニッケルおよびコバルトの塩のほかリン酸(H3PO4)および過酸化水素(H2O2)を含んでいた。モリブデン塩は七モリブデン酸アンモニウムMo7O24(NH4)6・4H2Oであり、ニッケル(コバルト)塩は硝酸ニッケル(コバルト)Ni(NO3)2・6H2O(Co(NO3)2・6H2O)であった。溶液中のこれらの塩のそれぞれの量は、所望量の各元素を担体表面に固定するように決定された。
本発明者らは、マクロ多孔度を有しておらず且つ表1に示される特徴を有していた担体Bに乾式含浸させた。含浸用水溶液は、モリブデン、ニッケルおよびコバルトの塩のほかリン酸(H3PO4)および過酸化水素(H2O2)を含んでいた。モリブデン塩は七モリブデン酸アンモニウムMo7O24(NH4)6・4H2Oであり、ニッケル(コバルト)塩は硝酸ニッケル(コバルト)Ni(NO3)2・6H2O(Co(NO3)2・6H2O)であった。溶液中のこれらの塩のそれぞれの量は、所望量の各元素を担体表面に固定するように決定された。
本発明者らは、表1に示される特徴を有していた同担体Bに乾式含浸させた。含浸用水溶液は、モリブデンおよびコバルトの塩のほかリン酸(H3PO4)および過酸化水素(H2O2)を含んでいた。モリブデン塩は七モリブデン酸アンモニウムMo7O24(NH4)6・4H2Oであり、コバルト塩は硝酸コバルトCo(NO3)2・6H2Oであった。溶液中のこれらの塩のそれぞれの量は、所望量の各元素を担体表面に固定するように決定された。
実施例1〜4に記載された触媒C、D、E、F、G、Hが、本発明の方法における石油残渣の水素化処理試験において比較された。仕込原料は、中東原産(Arabian Light)の常圧残渣(atmospheric residue:AR)によって構成されていた。これらの残渣の特徴は、高い粘度(45mm2/s)、高いコンラドソン炭素残留(Conradson Carbon Residue)(10.2重量%)、高いアスファルテン含有量(3.2重量%)、高いニッケル含有量(10.6重量ppm)、バナジウム含有量(41重量ppm)及び硫黄含有量(3.38重量%)にある。該仕込原料の完全な特徴を表7に示す。
HDS(重量%)=((重量%S)仕込原料−(重量%S)試験)/(重量%S)仕込原料×100
HDM収率は次のように定義される:
HDM(重量%)=((重量ppm Ni+V)仕込原料−(重量ppm Ni+V)試験)/(重量ppm Ni+V)仕込原料×100
それ故に、本発明による触媒の組み合わせによって、同一のモリブデン含有量をやはり有しない比較の従来技術の触媒によるより良好なHDS活性だけでなくより良好なHDM活性ももたらされるように思われる。
このように、本発明による触媒を組み合わせることよって、それにもかかわらず同じモリブデン含有量を有する対照の先行技術の触媒よりも、HDS活性だけでなくHDM活性も良くなることがわかる。HDSおよびHDM転化の程度は、実際に、本発明の触媒調合を用いることによって、HDM区間におけるNiMoとHDM区間CoMoとの連結(触媒は両方の状況において同量のモリブデンを含有する)によるより良好である。
Claims (16)
- 第VIB族からの少なくとも1種の金属と、第VIII族からの少なくとも2種の金属と、多孔性の耐火性酸化物によって構成される少なくとも1種の担体とを含み、第VIII族からの少なくとも2種の金属のうちの1種は主要プロモータVIII-1と呼ばれ、1種または複数種の他のものは共プロモータVIII-iと呼ばれ、ここで、iは2〜5の範囲であり、第VIII族からの元素は、原子比[VIII-1/(VIII-1+…+VIII-i)]により定義される比で存在し、前記原子比は0.5〜0.85の範囲である、触媒。
- 第VIB族からの金属は、モリブデンおよびタングステンから選択される、請求項1に記載の触媒。
- 第VIII族からの金属は、鉄、ニッケルおよびコバルトから選択され、主要プロモータ(VIII-1)は、コバルトまたはニッケルである、請求項1または2に記載の触媒。
- 前記触媒は、第VIB族からの1種の金属と第VIII族からの2種の金属とを含み、第VIB族からの1種の金属はモリブデンであり、第VIII族からの2種の金属がニッケルおよびコバルトである、請求項1〜3のいずれか1つに記載の触媒。
- 前記触媒は、リンおよびホウ素から選択される少なくとも1種のドーピング元素を含む、請求項3に記載の触媒。
- 前記触媒は、第VIB族からの1種以上の金属を、全触媒質量に対する第VIB族からの1種以上の金属の三酸化物の重量で2〜9%の範囲の量で含み、第VIII族からの複数種の金属の合計量は、全触媒質量に対する第VIII族からの複数種の金属の酸化物の重量で0.3〜2%の範囲である、請求項1〜5のいずれか1つに記載の触媒。
- 前記触媒は、第VIB族からの1種以上の金属を、全触媒質量に対する第VIB族からの1種以上の金属の三酸化物の重量で厳密に9%超且つ17%未満の範囲の量で含み、第VIII族からの複数種の金属の合計量は、全触媒質量に対する第VIII族からの複数種の金属の酸化物の重量で厳密に2%超且つ5%未満である、請求項1〜5のいずれか1つに記載の触媒。
- 請求項1〜7のいずれか1つによる少なくとも2種の触媒を含む触媒系であって、第一触媒は、第VIB族からの1種以上の金属を、全触媒質量に対する第VIB族からの1種以上の金属の三酸化物の重量で2〜9%の範囲の量で含み、第VIII族からの複数種の金属の合計量が、全触媒質量に対する第VIII族からの複数種の金属の酸化物の重量で0.3〜2%であり、第二触媒は、第VIB族からの1種以上の金属を、全触媒質量に対する第VIB族からの1種以上の金属の三酸化物の重量で厳密に9%超且つ17%未満の範囲の量で含み、第VIII族からの複数種の金属の合計量が、全触媒質量に対する第VIII族からの複数種の金属の酸化物の重量で厳密に2%超且つ5%未満であり、前記第一および第二の触媒は、同じ原子比を有する、触媒系。
- 前記第一触媒のマクロ孔容積が、全細孔容積(TPV)の5%超である、請求項8に記載の触媒系。
- 前記第二触媒のマクロ孔容積が、全細孔容積(TPV)の10%未満である、請求項8または9に記載の触媒系。
- 重質炭化水素仕込原料の水素化処理方法であって、少なくとも1回の水素化脱金属工程と少なくとも1回の水素化脱硫工程とを包含し、水素化脱金属および水素化脱硫の工程のそれぞれにおいて同一の原子比を有する少なくとも1種の触媒を使用し、前記触媒は、請求項1〜7のいずれか1つによる触媒である、方法。
- 水素化脱金属工程は、第VIB族からの1種以上の金属を、全触媒質量に対する第VIB族からの1種以上の金属の三酸化物の重量で2〜9%の範囲の量で含み、第VIII族からの複数種の金属の合計量が、全触媒質量に対する第VIII族からの複数種の金属の酸化物の重量で0.3〜2%の範囲である、触媒を使用し、水素化脱硫工程は、第VIB族からの1種以上の金属を、全触媒質量に対する第VIB族からの1種以上の金属の三酸化物の重量で厳密に9%超且つ17%未満の範囲の量で含み、第VIII族からの複数種の金属の合計量が、全触媒質量に対する第VIII族からの複数種の金属の酸化物の重量で厳密に2%超且つ5%未満である、触媒を使用する、請求項11に記載の方法。
- 仕込原料は、1重量%超の沸点500℃超の分子を有し、金属(Ni+V)含有量が1重量ppm超であり、ヘプタン中に沈殿するアスファルテン含有量が0.05重量%超である、請求項11または12に記載の方法。
- 重質仕込原料は、粉末状の石炭と混合され、前記仕込原料は場合によっては、石炭の転化に由来し、新石炭と再混合される副生成物である、請求項13に記載の方法。
- 前記方法は、固定床において、320〜450℃の範囲の温度、3〜30MPaの範囲の水素分圧、毎時の触媒の容積当たりの仕込原料容積0.05〜5の範囲の毎時空間速度、および立方メートル当たり200〜5000標準立方メートルの範囲の気体水素対液体炭化水素仕込原料の比で行われる、請求項11〜14のいずれか1つに記載の方法。
- 前記方法は、沸騰床において、320〜450℃の範囲の温度、3〜30MPaの範囲の水素分圧、毎時の触媒容積当たりの仕込原料容積0.1〜10の範囲の毎時空間速度、立方メートル当たり100〜3000標準立方メートルの範囲の気体水素対液体炭化水素仕込原料の比で行われる、請求項11〜14のいずれか1つに記載の方法。
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JP2015536823A (ja) * | 2012-11-29 | 2015-12-24 | イエフペ エネルジ ヌヴェルIfp Energies Nouvelles | アルミナゲルからの水素化処理触媒、および該触媒の調製方法 |
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TW201034751A (en) | 2010-10-01 |
FR2940143B1 (fr) | 2015-12-11 |
US20100155301A1 (en) | 2010-06-24 |
EP2255873A2 (fr) | 2010-12-01 |
CN105562020A (zh) | 2016-05-11 |
CA2688820A1 (fr) | 2010-06-18 |
ES2819254T3 (es) | 2021-04-15 |
CN101822994A (zh) | 2010-09-08 |
RU2444406C2 (ru) | 2012-03-10 |
FR2940143A1 (fr) | 2010-06-25 |
JP5548437B2 (ja) | 2014-07-16 |
TWI558455B (zh) | 2016-11-21 |
KR20100071016A (ko) | 2010-06-28 |
US8394262B2 (en) | 2013-03-12 |
KR101645726B1 (ko) | 2016-08-04 |
CA2688820C (fr) | 2017-01-24 |
EP2255873A3 (fr) | 2011-03-30 |
EP2255873B1 (fr) | 2020-06-24 |
RU2009146970A (ru) | 2011-06-27 |
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