JP2013049857A - モリブデンおよび第viii族金属を含む触媒ならびに水素化脱硫水素蒸留物のためのその使用 - Google Patents
モリブデンおよび第viii族金属を含む触媒ならびに水素化脱硫水素蒸留物のためのその使用 Download PDFInfo
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- JP2013049857A JP2013049857A JP2012220062A JP2012220062A JP2013049857A JP 2013049857 A JP2013049857 A JP 2013049857A JP 2012220062 A JP2012220062 A JP 2012220062A JP 2012220062 A JP2012220062 A JP 2012220062A JP 2013049857 A JP2013049857 A JP 2013049857A
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- mixture
- catalyst
- weight
- molybdenum
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- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims abstract description 146
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 60
- 239000002184 metal Substances 0.000 title claims abstract description 60
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000011733 molybdenum Substances 0.000 title claims abstract description 39
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 39
- 229910052739 hydrogen Inorganic materials 0.000 title description 12
- 239000001257 hydrogen Substances 0.000 title description 12
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title 1
- 239000000203 mixture Substances 0.000 claims abstract description 123
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 94
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 61
- 239000011593 sulfur Substances 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 49
- 230000008569 process Effects 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 23
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 18
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 150000002816 nickel compounds Chemical class 0.000 claims abstract description 9
- 150000001869 cobalt compounds Chemical class 0.000 claims abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 63
- 239000002245 particle Substances 0.000 claims description 42
- 239000011148 porous material Substances 0.000 claims description 29
- 238000004821 distillation Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000010304 firing Methods 0.000 claims description 13
- 238000004898 kneading Methods 0.000 claims description 13
- 238000009826 distribution Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- -1 molybdenum salt compound Chemical class 0.000 claims description 6
- 238000006477 desulfuration reaction Methods 0.000 claims description 3
- 230000023556 desulfurization Effects 0.000 claims description 3
- 229910010272 inorganic material Inorganic materials 0.000 claims description 2
- 239000011147 inorganic material Substances 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 36
- 229910052759 nickel Inorganic materials 0.000 description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 238000005984 hydrogenation reaction Methods 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 11
- 239000005078 molybdenum compound Substances 0.000 description 11
- 150000002752 molybdenum compounds Chemical class 0.000 description 11
- 239000010941 cobalt Substances 0.000 description 10
- 229910017052 cobalt Inorganic materials 0.000 description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 10
- 238000002156 mixing Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 238000007598 dipping method Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 239000007858 starting material Substances 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 8
- 238000009835 boiling Methods 0.000 description 7
- 239000004215 Carbon black (E152) Substances 0.000 description 6
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- 229930195733 hydrocarbon Natural products 0.000 description 6
- 150000002430 hydrocarbons Chemical class 0.000 description 6
- 150000003464 sulfur compounds Chemical class 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 229910052987 metal hydride Inorganic materials 0.000 description 4
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- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
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- 239000002283 diesel fuel Substances 0.000 description 3
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- 238000010438 heat treatment Methods 0.000 description 3
- 150000002751 molybdenum Chemical class 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
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- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
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- 125000004434 sulfur atom Chemical group 0.000 description 2
- 239000003039 volatile agent Substances 0.000 description 2
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 1
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 229910039444 MoC Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 235000019169 all-trans-retinol Nutrition 0.000 description 1
- 239000011717 all-trans-retinol Substances 0.000 description 1
- 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 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
- 239000012736 aqueous medium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- XUFUCDNVOXXQQC-UHFFFAOYSA-L azane;hydroxy-(hydroxy(dioxo)molybdenio)oxy-dioxomolybdenum Chemical compound N.N.O[Mo](=O)(=O)O[Mo](O)(=O)=O XUFUCDNVOXXQQC-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- TXCOQXKFOPSCPZ-UHFFFAOYSA-J molybdenum(4+);tetraacetate Chemical compound [Mo+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O TXCOQXKFOPSCPZ-UHFFFAOYSA-J 0.000 description 1
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- YPFBRNLUIFQCQL-UHFFFAOYSA-K tribromomolybdenum Chemical compound Br[Mo](Br)Br YPFBRNLUIFQCQL-UHFFFAOYSA-K 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
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Classifications
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- 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
- C10G45/12—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 crystalline alumino-silicates, e.g. molecular sieves
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- 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
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- 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
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- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
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- 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
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- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B01J35/615—100-500 m2/g
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/08—Nitrates
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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
- 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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- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
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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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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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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- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4018—Spatial velocity, e.g. LHSV, WHSV
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
【解決手段】該蒸留物水素化脱硫触媒は、無機酸化物材料、三酸化モリブデンならびに第VIII族金属化合物(この第VIII族金属化合物は、ニッケル化合物およびコバルト化合物からなる群から選択される。)を含む混合物を焼成して作製される焼成混合物を含み、前記焼成混合物は、金属換算のモリブデンと焼成混合物の全重量とに基づく重量%を用いると7重量%から22重量%の範囲内のモリブデン含有量ならびにその元素形態での第VIII族金属と焼成混合物の全重量とに基づく重量%を用いると3重量%から12重量%の範囲内の第VIII族金属含有量を有する。
【選択図】なし
Description
この実施例は、触媒Aおよび比較触媒Bの調製を説明する。
触媒Aは、初めに、316.4重量部の脱イオン水に、724.71重量部の硝酸コバルト(Co(NO3)2・6H2O)を溶解して水性コバルト溶液を形成し、加熱し、その後水性コバルト溶液を冷却することにより調製した。水性コバルト溶液をミュラーミキサー内で、3134.8重量部の2%シリカ−アルミナ、新しいCo/Mo/P/Ni水素化触媒(2.9重量%のCo、12.0重量%のMo、0.09重量%のP、および0.02重量%のNi)の粉砕微粉680.3重量部、301.1重量部の三酸化モリブデン粉末、30重量部の市販の押出し助剤、3465.7重量部の脱イオン水および硝酸と一緒に混合した。この混合物を、1.3mm三分割ダイスを使用して押出した。押出物を100℃で乾燥した。
触媒Bは、初めに、200重量部の脱イオン水に、264.9重量部の硝酸コバルト(Co(NO3)2・6H2O)を溶解して水性コバルト溶液を形成することにより調製した。水性コバルト溶液をミュラーミキサー内で、3278.7重量部の広い細孔アルミナ、新しいCo/Mo/P/Ni水素化触媒(2.9重量%のCo、12.0重量%のMo、0.09重量%のP、および0.02重量%のNi)の粉砕微粉680.3重量部、301.1重量部の三酸化モリブデン粉末、30重量部の市販の押出し助剤および28.46.8重量部の脱イオン水と一緒に混合した。この混合物を、1.3mm三分割ダイスを使用して押出した。押出物を100℃で乾燥した。
この実施例は、実施例Iで説明した触媒を試験するのに使用される方法を説明する。この方法は、100ppm未満の硫黄を有する生成物を生成するために蒸留物供給原料の硫黄含有量の除去を与える。
水素ガスを、周囲圧力で、1200SCF/(供給物のB)の速度で反応器へ導入し、供給物を、周囲温度で、1.5/時間のLHSVを与えるための速度で反応器へ導入した。供給物は、およそ2.5重量%の全硫黄水準までTNPSでスパイクされた直留ディーゼルであった(供給物の性質は表2で示される)。供給物が床を通り抜けたら、触媒温度を、65°F/時間の速度で450°Fまで漸進的に上昇させ、次いで、450°Fで4時間保った。次いで、温度を、50°F/時間の速度で450°Fから650°Fまで上げ、次いで、650°Fで2時間保った。その後、システムを冷却させた。その後、スパイクされていない供給物を、1.0/時間のLHSVを与えるための速度で反応器へ導入し、400°Fの温度で維持し、水素を、1200SCF/(供給物のB)の速度および300psigの全圧力で導入した。
水素ガスを、周囲圧力で、203m 3 /m 3 (1200SCF/(供給物のB))の速度で反応器へ導入し、供給物を、周囲温度で、1.5/時間のLHSVを与えるための速度で反応器へ導入した。供給物は、およそ2.5重量%の全硫黄水準までTNPSでスパイクされた直留ディーゼルであった(供給物の性質は表2で示される)。供給物が床を通り抜けたら、触媒温度を、18℃/時間(65°F/時間)の速度で232℃(450°F)まで漸進的に上昇させ、次いで、232℃(450°F)で4時間保った。次いで、温度を、10℃/時間(50°F/時間)の速度で232℃(450°F)から343℃(650°F)まで上げ、次いで、343℃(650°F)で2時間保った。その後、システムを冷却させた。その後、スパイクされていない供給物を、1.0/時間のLHSVを与えるための速度で反応器へ導入し、204℃(400°F)の温度で維持し、水素を、203m 3 /m 3 (1200SCF/(供給物のB))の速度および2.1x10 6 Pa(300psig)の全圧力で導入した。
Claims (11)
- 無機材料、三酸化モリブデンおよびニッケル化合物を共混練して混合物を形成すること、
前記混合物を粒子に成形すること、ならびに
前記粒子を焼成して、焼成混合物を得ること
を含み、前記焼成混合物は、金属換算のモリブデンと焼成混合物の全重量とに基づく重量%を用いると7重量%から22重量%の範囲内のモリブデン含有量ならびにその元素形態での第VIII族金属と焼成混合物の全重量とに基づく重量%を用いると3重量%から12重量%の範囲内の第VIII族金属含有量を有する、
超低硫黄蒸留生成物の製造における蒸留物水素化脱硫触媒として使用するための組成物の製造方法。 - 前記焼成工程が、焼成温度が、約600℃(1112°F)から約760℃(1400°F)の範囲内である、制御された温度条件下で、所望の細孔構造を有する前記焼成混合物を得るのに有効な焼成時間実施される、請求項1に記載の方法。
- 前記所望の細孔構造が、前記焼成混合物の全細孔容積の少なくとも70%が、70オングストロームから150オングストロームの範囲内の径を有する前記焼成混合物の細孔中に存在するような前記焼成混合物についての細孔サイズ分布を含む、請求項2に記載の方法。
- 前記混合物が、三酸化モリブデン、ニッケル化合物および無機酸化物材料から本質的になる、請求項1、2または3に記載の方法。
- 前記混合物が、モリブデン塩化合物を含まない材料を有する、請求項1、2、3または4に記載の方法。
- 前記共混練工程が、前記混合物が3から6の範囲内に維持されるpHを有するように実施される、請求項1、2、3、4または5に記載の方法。
- 無機酸化物材料、三酸化モリブデンならびに第VIII族金属化合物(この第VIII族金属化合物はニッケル化合物およびコバルト化合物からなる群から選択される。)を含む混合物を焼成して作製される焼成混合物を含み、前記焼成混合物は、金属換算のモリブデンと焼成混合物の全重量とに基づく重量%を用いると7重量%から22重量%の範囲内のモリブデン含有量ならびにその元素形態での第VIII族金属と焼成混合物の全重量とに基づく重量%を用いると3重量%から12重量%の範囲内の第VIII族金属含有量を有する、超低硫黄蒸留生成物の製造における蒸留物水素化脱硫触媒として使用するための組成物。
- 前記焼成混合物が、前記焼成混合物の全細孔容積の少なくとも70%が70オングストロームから150オングストロームの範囲内の径を有する前記焼成混合物の細孔中に存在するような細孔サイズ分布を有する、請求項7に記載の組成物。
- 適切な蒸留物脱硫プロセス条件下で、第一硫黄濃度を含む蒸留物供給原料を、請求項1、2、3、4、5または6に記載の方法で作製された蒸留物水素化脱硫触媒組成物についての請求項7または8に記載の組成物と接触させること、および
第二硫黄濃度を有する前記超低硫黄蒸留生成物を生成すること
を含む、超低硫黄蒸留生成物の製造方法。 - 前記第一硫黄濃度が0.01重量%(100ppmw)から2重量%(20,000ppmw)の範囲内であり、前記第二硫黄濃度が50ppmw未満である、請求項9に記載の方法。
- 前記適切な蒸留物脱硫プロセス条件が、200℃から420℃の範囲内の水素化脱硫温度、690kPaから13,800kPaの範囲内の水素化脱硫反応圧力および0.1/時間から10/時間の範囲内の液体毎時空間速度を含む、請求項9または10に記載の方法。
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JP2005169232A (ja) * | 2003-12-10 | 2005-06-30 | Petroleum Energy Center | 炭化水素油の水素化脱硫触媒及びその製造方法 |
JP2005314657A (ja) * | 2004-03-29 | 2005-11-10 | Cosmo Oil Co Ltd | 重質炭化水素油の水素化処理方法 |
JP2006000726A (ja) * | 2004-06-16 | 2006-01-05 | Petroleum Energy Center | 炭化水素油の水素化処理触媒及びその製造方法、並びに炭化水素油の水素化処理方法 |
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CN102698769B (zh) | 2016-08-24 |
US7824541B2 (en) | 2010-11-02 |
RU2009107522A (ru) | 2010-09-10 |
US20080060977A1 (en) | 2008-03-13 |
WO2008016971A2 (en) | 2008-02-07 |
US20110124497A1 (en) | 2011-05-26 |
JP2009545443A (ja) | 2009-12-24 |
BRPI0715357B1 (pt) | 2017-03-28 |
CA2659797C (en) | 2015-02-10 |
EP2049251A2 (en) | 2009-04-22 |
US8530373B2 (en) | 2013-09-10 |
CA2659797A1 (en) | 2008-02-07 |
JP5616937B2 (ja) | 2014-10-29 |
RU2438778C2 (ru) | 2012-01-10 |
BRPI0715357A2 (pt) | 2013-06-18 |
US8883673B2 (en) | 2014-11-11 |
WO2008016971A3 (en) | 2008-04-10 |
US20130296163A1 (en) | 2013-11-07 |
CN102698769A (zh) | 2012-10-03 |
CN101516500A (zh) | 2009-08-26 |
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