JP6152121B2 - 残油脱金属用回転楕円形触媒 - Google Patents
残油脱金属用回転楕円形触媒 Download PDFInfo
- Publication number
- JP6152121B2 JP6152121B2 JP2014557811A JP2014557811A JP6152121B2 JP 6152121 B2 JP6152121 B2 JP 6152121B2 JP 2014557811 A JP2014557811 A JP 2014557811A JP 2014557811 A JP2014557811 A JP 2014557811A JP 6152121 B2 JP6152121 B2 JP 6152121B2
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- Prior art keywords
- titania
- alumina
- pore volume
- metal
- catalyst
- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims description 90
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 95
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 92
- 239000011148 porous material Substances 0.000 claims description 70
- 229910052751 metal Inorganic materials 0.000 claims description 66
- 239000002184 metal Substances 0.000 claims description 66
- 238000000034 method Methods 0.000 claims description 44
- 229930195733 hydrocarbon Natural products 0.000 claims description 41
- 150000002430 hydrocarbons Chemical class 0.000 claims description 41
- 239000004215 Carbon black (E152) Substances 0.000 claims description 35
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 24
- 230000008569 process Effects 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 20
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 15
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 15
- 150000002739 metals Chemical class 0.000 claims description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 12
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000011593 sulfur Substances 0.000 claims description 12
- 238000002441 X-ray diffraction Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 230000000737 periodic effect Effects 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 230000003197 catalytic effect Effects 0.000 claims description 10
- 238000009826 distribution Methods 0.000 claims description 9
- 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 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000000975 co-precipitation Methods 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000001747 exhibiting effect Effects 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims 2
- 229910044991 metal oxide Inorganic materials 0.000 claims 1
- 150000004706 metal oxides Chemical class 0.000 claims 1
- 238000001935 peptisation Methods 0.000 claims 1
- 239000000758 substrate Substances 0.000 claims 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 description 48
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- 239000000843 powder Substances 0.000 description 15
- 239000003921 oil Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- JEGSVFUREJDEAP-UHFFFAOYSA-L aluminum;titanium(4+);sulfate Chemical compound [Al+3].[Ti+4].[O-]S([O-])(=O)=O JEGSVFUREJDEAP-UHFFFAOYSA-L 0.000 description 12
- 150000002736 metal compounds Chemical class 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 229910052698 phosphorus Inorganic materials 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 229910018104 Ni-P Inorganic materials 0.000 description 7
- 229910018536 Ni—P Inorganic materials 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000005470 impregnation Methods 0.000 description 6
- 229910017604 nitric acid Inorganic materials 0.000 description 6
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 229910000348 titanium sulfate Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 4
- 230000023556 desulfurization Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- 239000011275 tar sand Substances 0.000 description 4
- 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 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 239000010779 crude oil Substances 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 238000004231 fluid catalytic cracking Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- -1 phosphorus compound Chemical class 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000002459 porosimetry Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000005662 Paraffin oil Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000005260 alpha ray Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide 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
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000012438 extruded product Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01J21/04—Alumina
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
- B01J27/19—Molybdenum
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- B01J35/51—Spheres
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- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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- B01J35/615—100-500 m2/g
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- B01J35/635—0.5-1.0 ml/g
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- B01J35/638—Pore volume more than 1.0 ml/g
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- B01J35/647—2-50 nm
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- B01J37/0201—Impregnation
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- B01J37/08—Heat treatment
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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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
-
- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
- C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
- C10G45/08—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
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Description
方法も提供する。
ナ含有量は好適には少なくとも95重量%であり、最も好適には99重量%より大きく、前記重量パーセントは本担体の総重量パーセントを基準にしたパーセントである。このように、本担体材料は本明細書に記述する如きチタニア・アルミナ“から本質的に成って”いてもよい。本担体材料の組成に関して本明細書で用いる如き語句“から本質的に成る”は、本明細書では、当該担体材料がチタニア・アルミナおよび他の成分を含有していてもよいことを示す目的で用いるものであるが、但しそのような他の成分が最終的水素化変換用組成物が示す触媒特性に実質的な効果も影響も示さないことを条件とする。
第4,270,779号(この文献は引用することによって全体が本明細書に組み入れられる)に開示および記述されている如き外部ゲル化油滴方法を用いて実施する。このチタニア・アルミナ共沈方法では、共沈チタニア・アルミナ中のチタニア量が5重量%以下のチタニア・アルミナが沈澱するに充分な量の硫酸アルミニウムと硫酸チタン混合物の水溶液を温度が約50℃から約80℃の水ヒール(water heel)にアルミン酸ナトリウムと同時に加える。この沈澱段階中のスラリーのpHを約7.2から約9.0に維持しかつ温度を約50℃から約80℃に維持する。この沈澱段階が終了した時点で前記スラリーのpHを約8.6から約9.3に調整することで、残存する不純物、例えばナトリウムおよび硫酸塩などが最大限に除去され得るようにする。その後、共沈してきたチタニア・アルミナを濾過で取り出し、水で洗浄した後、乾燥させることで、水分含有量が水分分析器を用いて955℃で測定した時に約22重量%から約40重量%、好適には約25重量%から約32重量%のチタニア・アルミナを得る。
性金属もしくは前駆体化合物が入っている水溶液と接触させて所望金属を本担体上に均一に分布させることで実施する。好適には、その金属を本担体の孔の中全体に渡って均一に分布させる。本発明の1つの態様では、本触媒の調製を本触媒担体に所望の触媒活性金属もしくは前駆体化合物が入っている水溶液を湿り開始まで含浸させることで実施する。
可能である。含浸、浸漬などを複数回用いる場合、乾燥および/または焼成を段階と段階の間で実施することも可能である。
合により硫黄の濃度が低下した炭化水素含有生成物をもたらすような水素化処理工程条件下の装置内で実施可能である。本発明に従い、水素化処理工程を好適にはOnstream Catalyst Replacement(OCR)技術を用いて実施する。本発明で用いるに有用な典型的な水素化処理工程条件には、これらに限定するものでないが、約300°から約450℃の範囲の反応温度、約25から約200バールの水素圧、約150から約1500N1/1の範囲のH2:油比および約0.1から約5の空間速度(時-1)が含まれる。本発明の1つの態様における金属含有炭化水素原料の脱硫工程に適した操作条件には、約370℃から約400℃の反応ゾーン温度、約100から約200バールの圧力および油供給材料1リットル当たり約200から約500Nl/1の水素供給速度が含まれる。
に硫酸アルミニウム−チタン混合物を5ガロン加えた。その後、前記硫酸アルミニウムと硫酸チタンの混合物およびアルミン酸ナトリウムを前記ストライクタンクに同時に加えた。前記硫酸アルミニウムと硫酸チタンの混合物を一定流量で加えそして前記アルミン酸ナトリウムの流量を前記ストライクタンク内のpHが一定に8.4に維持されるように変えた。前記硫酸アルミニウム−チタン混合物の流れを前記硫酸アルミニウム−チタン混合物とアルミン酸ナトリウムの同時流入を開始してから50分後に止めた。この時点で沈澱してきたチタニア・アルミナ固体の濃度は約6重量%であった。アルミン酸ナトリウムの流量を1分当たり0.7ガロンにまで低下させそしてストライクタンク内のpHが9.2になった時点で止めた。次に、沈澱してきたチタニア・アルミナ混合物を濾過で取り出した後、フィルターベルト上で洗浄することで残存する硫酸ナトリウムを除去した。次に、その結果として得たフィルターケーキに噴霧乾燥を受けさせた。次に、乾燥させたチタニア・アルミナ粉末を触媒担体の調製で用いた。
せた。完成触媒(触媒Cと識別)の名目上の活性金属含有量は3重量%のMo、1重量%のNiおよび1重量%のPであった。触媒の特性は以下の表1に示す如くであった。
以下に記述するようにして受けさせた。触媒のペレットを栓流反応槽に充填した。供給材料を大気残油と水素で構成させた。前記残油の金属含有量は362ppmのV、71ppmのNiおよび4.6重量%の硫黄含有量であった。前記反応槽の温度を395−375℃の間の様々な温度に維持しかつ1時間当たりの平均空間速度を0.8L/(L.h)にした。金属および硫黄変換を比較した結果を以下の表3に示す。異なる3稼働時間値(210、402および738時間)の時の結果および相当する反応槽温度を示す。
たせた触媒B、CおよびDは触媒A(アルミナのみ)が示した性能に比べて金属、硫黄およびMCR変換に関して向上した性能を示した。触媒Eが示した初期性能は触媒Aのそれに匹敵していたが、触媒Eが金属、硫黄およびMCR変換に関して示した性能は予想外に経時的に低下し、このことは安定性が不足していることを明らかに示している。
Claims (15)
- 金属含有重質炭化水素溜分に水素化脱金属を水素化処理条件下で受けさせる時に用いるに適した触媒活性金属を担持するための回転楕円形担体材料の製造方法であって、
a)チタニア含有量がチタニア・アルミナの総重量を基準にして5重量%以下の共沈チタニア・アルミナを生じさせ、
b)前記チタニア・アルミナに解膠を受けさせることで滴を生じるに充分な粘度を有する固体含有量が20%から35%の水性スラリーを生じさせ、
c)前記スラリーを滴下カラム内で落下させることで回転楕円形粒子を生じさせ、
d)前記回転楕円形粒子に焼成を960℃から1100℃の範囲の温度で受けさせることで、0.7から1.2cc/gの範囲の総細孔容積を有しかつ前記総細孔容積の40%より大きい量で直径が200Åより大きい孔を有し、前記総細孔容積の30%以上が200Åから500Åの範囲の孔を有しかつ前記総細孔容積の10%より大きい量で直径が1000Åより大きい孔を有するような細孔容積分布を示す回転楕円形チタニア・アルミナ担体を得る、
ことを含んで成る方法。 - 前記担体のチタニア・アルミナがR値が0.4から1.7のアルミナを少なくとも90重量%含有して成る、ただしR値は2θ=32°の所のX線回折ピークの積分強度と2θ=46°の所のX線回折ピークの積分強度の間の比率である、請求項1記載の方法。
- 段階(a)の前記共沈チタニア・アルミナが共沈チタニア・アルミナ中のチタニア量が5重量%以下になるほどの量の硫酸チタニルと硫酸アルミニウムとアルミン酸ナトリウムの水溶液から共沈を起こさせることで生じさせたものである請求項1記載の方法。
- 前記回転楕円形粒子に焼成を980℃から1060℃の範囲の温度で1時間から3時間受けさせる請求項1記載の方法。
- 段階(a)の前記共沈チタニア・アルミナのチタニア量がチタニア・アルミナの総重量を基準にして2.5から4.0重量%のチタニアである請求項1記載の方法。
- チタニア量がチタニア・アルミナ全体を基準にして5重量%以下の共沈チタニア・アルミナを含有して成る回転楕円形触媒担体であって、0.7から1.2cc/gの範囲
の総細孔容積を有しかつ前記総細孔容積の40%より大きい量で直径が200Åより大きい孔を有し、前記総細孔容積の30%以上が200Åから500Åの範囲の孔を有しかつ前記総細孔容積の10%より大きい量で直径が1000Åより大きい孔を有するような細孔容積分布を示す担体。 - チタニアが前記共沈チタニア・アルミナ中に存在する量がチタニア・アルミナの総重量を基準にして2.5から4.0重量%のチタニアの範囲の量である請求項6記載の担体。
- アルミナR値が0.4から1.7のチタニア・アルミナを少なくとも90重量%含有して成る、ただしR値は2θ=32°の所のX線回折ピークの積分強度と2θ=46°の所のX線回折ピークの積分強度の間の比率である、請求項6記載の担体。
- 前記担体の細孔容積の分布が、前記総細孔容積の50%から90%が直径が200Åより大きい孔を有するか、或いは、前記総細孔容積の30%から80%が直径が200から500Åの孔を有するか、或いは、前記総細孔容積の15%以上が直径が1000Åより大きい孔を有するか、或いは、これらの組み合わせである、請求項6または8記載の担体。
- 重質炭化水素の水素化脱金属用触媒であって、
a)チタニア量がチタニア・アルミナの総重量を基準にして5重量%以下のチタニア・アルミナを含有して成る回転楕円形担体、および
b)周期律表の6族の金属、周期律表の9族の金属、周期律表の10族の金属およびこれらの組み合わせから成る群より選択される金属(i)、および任意に燐(ii)、を含有して成る少なくとも1種の触媒作用剤、
を含有して成っていて
前記担体が1グラム当たり0.7から1.2立方センチメートルの範囲の総細孔容積を有することに加えて前記総細孔容積の40%より大きい量で直径が200Åより大きい孔を有し、前記総細孔容積の30%以上が200Åから500Åの範囲の孔を有しかつ前記総細孔容積の10%より大きい量で直径が1000Åより大きい孔を有する、
触媒。 - 前記担体がチタニア・アルミナを含有して成っていて前記チタニア・アルミナがR値が0.4から1.7のアルミナを少なくとも90重量%有する、ただしR値は2θ=32°の所のX線回折ピークの積分強度と2θ=46°の所のX線回折ピークの積分強度の間の比率である、請求項10記載の触媒。
- 前記少なくとも1種の触媒作用剤がコバルト、ニッケル、モリブデンまたはこれらの組み合わせから成る群より選択される請求項10記載の触媒。
- 水素化処理工程中に高い活性と安定性を示す金属含有重質炭化水素溜分の水素化脱金属用触媒の製造方法であって、回転楕円形の多孔質担体に周期律表の6族の金属、周期律表の9族の金属、周期律表の10族の金属およびこれらの組み合わせから成る群より選択した少なくとも1種の金属(i)、および任意に燐(ii)、を含有して成っていて熱で分解して金属酸化物になり得る少なくとも1種の触媒作用剤もしくは前駆体が入っている水溶液を含浸させた後、その結果として得た含浸担体に乾燥そして焼成を受けさせることで担持された触媒を生じさせることを含んで成っていて、前記担体が請求項1記載の方法で生じさせておいたものである方法。
- 金属、硫黄およびミクロカーボン残渣の少なくとも1つを含有する重質炭化水素溜分に
水素化処理を受けさせて該金属、硫黄およびミクロカーボン残渣の少なくとも1つを除去するか或いはその含有量を減少させるための方法であって、前記重質炭化水素溜分と請求項10記載の触媒を300°から450℃の範囲の反応温度、25から200バールの水素圧、150から1500N1/1の範囲のH2:油比および約0.1から
5時-1の空間速度から成る水素化処理工程条件下で接触させることを含んで成る方法。 - 前記重質炭化水素溜分がニッケル、バナジウムおよびこれらの組み合わせから成る群より選択される金属を含有する請求項14記載の方法。
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US10279335B2 (en) | 2019-05-07 |
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WO2013123315A1 (en) | 2013-08-22 |
US20150224476A1 (en) | 2015-08-13 |
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EP2814603A4 (en) | 2015-09-30 |
CN104411400A (zh) | 2015-03-11 |
US20190184376A1 (en) | 2019-06-20 |
CA2864815A1 (en) | 2013-08-22 |
TWI579043B (zh) | 2017-04-21 |
EP2814603A1 (en) | 2014-12-24 |
SG11201404833VA (en) | 2014-09-26 |
EP2814603B1 (en) | 2020-09-09 |
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US10589254B2 (en) | 2020-03-17 |
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