JP5501483B2 - 水素化精製触媒の製造方法 - Google Patents
水素化精製触媒の製造方法 Download PDFInfo
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- JP5501483B2 JP5501483B2 JP2012554184A JP2012554184A JP5501483B2 JP 5501483 B2 JP5501483 B2 JP 5501483B2 JP 2012554184 A JP2012554184 A JP 2012554184A JP 2012554184 A JP2012554184 A JP 2012554184A JP 5501483 B2 JP5501483 B2 JP 5501483B2
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- Prior art keywords
- catalyst
- producing
- cobalt
- salt
- hydrorefining catalyst
- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims description 117
- 238000004519 manufacturing process Methods 0.000 title claims description 34
- 238000000034 method Methods 0.000 claims description 33
- 239000004480 active ingredient Substances 0.000 claims description 31
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 26
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 25
- 238000005470 impregnation Methods 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 20
- 229910017052 cobalt Inorganic materials 0.000 claims description 16
- 239000010941 cobalt Substances 0.000 claims description 16
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 15
- 239000002738 chelating agent Substances 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 12
- 229910052750 molybdenum Inorganic materials 0.000 claims description 12
- 229920000768 polyamine Polymers 0.000 claims description 11
- 150000001868 cobalt Chemical class 0.000 claims description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 9
- 239000002131 composite material Substances 0.000 claims description 9
- 239000011733 molybdenum Substances 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- -1 carbonate compound Chemical class 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 150000002751 molybdenum Chemical class 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical group [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- VIJYFGMFEVJQHU-UHFFFAOYSA-N aluminum oxosilicon(2+) oxygen(2-) Chemical compound [O-2].[Al+3].[Si+2]=O VIJYFGMFEVJQHU-UHFFFAOYSA-N 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 150000003657 tungsten Chemical class 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical group [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 21
- 238000005984 hydrogenation reaction Methods 0.000 description 17
- 230000000694 effects Effects 0.000 description 16
- 238000003756 stirring Methods 0.000 description 16
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 14
- 238000011156 evaluation Methods 0.000 description 13
- 239000003921 oil Substances 0.000 description 12
- 239000002994 raw material Substances 0.000 description 11
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 10
- 239000011609 ammonium molybdate Substances 0.000 description 10
- 235000018660 ammonium molybdate Nutrition 0.000 description 10
- 229940010552 ammonium molybdate Drugs 0.000 description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 9
- 229910052717 sulfur Inorganic materials 0.000 description 9
- 239000011593 sulfur Substances 0.000 description 9
- 229940011182 cobalt acetate Drugs 0.000 description 8
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 4
- 229910052794 bromium Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000004939 coking Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- 150000007530 organic bases Chemical class 0.000 description 4
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 239000012041 precatalyst Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 239000002841 Lewis acid Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910017318 Mo—Ni Inorganic materials 0.000 description 2
- 229910003294 NiMo Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000001994 activation Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- WHDPTDWLEKQKKX-UHFFFAOYSA-N cobalt molybdenum Chemical compound [Co].[Co].[Mo] WHDPTDWLEKQKKX-UHFFFAOYSA-N 0.000 description 2
- 238000003869 coulometry Methods 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 150000007517 lewis acids Chemical class 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- 229910052701 rubidium Inorganic materials 0.000 description 2
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000005486 sulfidation Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 239000007848 Bronsted acid Substances 0.000 description 1
- 229910020515 Co—W Inorganic materials 0.000 description 1
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 1
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 150000005673 monoalkenes Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 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
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
- B01J23/8885—Tungsten containing also molybdenum
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- B01J37/0203—Impregnation the impregnation liquid containing organic compounds
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/20—Sulfiding
-
- 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
-
- 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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Description
▲し▼博万霖化工科技有限公司により提供され、孔容積が0.90〜0.95ml/g、比表面積が300〜320m2/gである。
▲し▼博万霖化工科技有限公司により提供され、二酸化ケイ素の含有量が3.5%、孔容積が0.90〜0.95ml/g、比表面積が300〜320m2/gである。
▲し▼博万霖化工科技有限公司により提供され、孔容積が0.85〜0.90ml/g、比表面積が280〜300m2/gである。
白銀良友化学試剤有限公司により提供され、濃度が25〜30wt%である。
触媒の金属含有量の測定方法:原子吸収法を用いて触媒中の金属含有量を測定した。
30℃で、14.21gの酢酸コバルトを60mlのアンモニア水及び5mlのエチレンジアミンの混合溶液に添加し、撹拌して溶解させた。そして、モリブデン酸アンモニウム31.97g、硝酸ニッケル9.32gを更に添加し、撹拌して溶解させた後、水酸化カリウム3.49gを添加し、溶液の体積が80mlとなるようにアンモニア水を入れて調整した。100gのγ−Al2O3担体を含浸させ、12時間エイジング化し、120℃で4時間乾燥させ、580℃で4時間焼成し、触媒Aが得られた。
25℃で、28.01gの酢酸コバルトを50mlのアンモニア水及び7mlエチレンジアミンの混合溶液中に添加し、撹拌して溶解させた。そして、モリブテンモリブデン酸アンモニウム14.21g、メタタングステン酸アンモニウム18.8gを添加し、撹拌して溶解させた後、水酸化リチウム2.38gを添加し、溶液の体積が100mlとなるようにアンモニア水を加えて調整した。100gのα−Al2O3担体を含浸させ、12時間エイジング化し、100℃で5時間乾燥させ、350℃で5時間焼成し、触媒Bが得られた。
20℃で、7.1gの硝酸コバルトを55mlのアンモニア水及び5mlのエチレンジアミン四酢酸の混合溶液中に添加し、撹拌して溶解させた。そして、モリブデン酸アンモニウム42.67g、酢酸ニッケル7.8g、硝酸ストロンチウム6.60gを添加し、撹拌して溶解させた後、炭酸リチウム6.84gを添加し、溶液の体積が110mlとなるようにアンモニア水を加えて調整した。100gの改質γ−Al2O3担体を含浸させ、12時間エイジング化し、200℃で4時間乾燥させ、400℃で3.5時間焼成し、触媒Cが得られた。
改質γ−Al2O3粉末300gに、リン酸8.4mlを添加し、水140mlを加え、混練押出成形を行い、空気中120℃で乾燥させ、560℃で6時間焼成して、リン素含有の改質γ−Al2O3担体が得られた。
30℃で、14.21gの酢酸コバルトを60mlのアンモニア水に添加し、大半の酢酸コバルトが溶解するまでに撹拌し、5mlのエチレンジアミンを更に添加し、酢酸コバルトが完全溶解するまで撹拌し続けた。モリブデン酸アンモニウム31.97g、硝酸ニッケル9.32gを更に添加して、撹拌して溶解させた後、水酸化カリウム3.49gを添加し、溶液の体積が80mlとなるようにアンモニア水を加えて調整した。100gのγ−Al2O3担体を含浸させ、12時間エイジング化し、120℃で4時間乾燥させ、580℃で4時間焼成し、触媒Eが得られた。
25℃で、28.01gの酢酸コバルトを20mlのエチレンジアミン及び80mlの水の混合溶液中に添加し、撹拌して溶解させた。モリブデン酸アンモニウム14.21g、メタタングステン酸アンモニウム18.8gを更に添加し、撹拌して溶解させた後、水酸化リチウム2.38gを添加し、100gのα−Al2O3担体に含浸させ、12時間エイジング化し、100℃で5時間乾燥させ、350℃で5時間焼成し、触媒Fが作られた。
20℃で、7.1gの硝酸コバルトを110mlのアンモニア水に添加し、撹拌して溶解させ、100gの改質γ−Al2O3担体に含浸させ、12時間エイジング化し、200℃で4時間干燥させ、400℃で3.5時間焼成した。モリブデン酸アンモニウム42.67g、醋酸ニッケル7.8g、硝酸ストロンチウム6.60gを110mlのアンモニア水に添加し、撹拌して溶解させた後、炭酸リチウム6.84gを添加した。100gの改質γ−Al2O3担体を含浸させ、12時間エイジング化し、200℃で4時間乾燥させ、400℃で3.5時間焼成し、触媒Gが得られた。
上記の方法で得られた触媒A及びEに対して、それぞれ200時間の評価を行った。分解ガソリンの一段階水素化製品を原料として用い、原料の性質は表1に示した。触媒の評価は、100mlの断熱床水素化反応装置において行われた。6時間ごとにサンプリングし、製品のヨウ素価、硫黄含有量を分析した。触媒の200時間評価の平均値データを、表4に示す。
触媒B、D及びFに対して1000時間評価を行った。評価原料、触媒前硫化条件、評価条件及び原料は、実施例4と同様とした。触媒評価における製品のヨウ素価、硫黄含有量の平均値データを、表5に示す。
上記の方法で得られた触媒C及びGに対して、それぞれ1000時間の水素化評価を行った。ディーゼルオイルを原料として用いた。原料の性質は表1に示した。触媒の評価は、100mlの断熱床水素化反応装置において行われた。6時間ごとにサンプリングして、製品の窒素、硫黄の含有量を分析した。触媒の1000時間評価の平均値のデータを、表6に示す。
Claims (9)
- 担体に活性成分が担持され、活性成分には、コバルト、モリブデンが含まれる水素化精製触媒の製造方法において、
アンモニア水とポリアミンキレート剤とを混合させ、複合溶剤に調製し、
前記複合溶剤に活性成分であるコバルトを含有する塩を添加し、コバルト塩を溶解させ、
前記コバルト塩を溶解させた複合溶剤に、モリブデン塩、又はモリブデン塩と、その他の活性成分、添加剤である塩類を添加すると共に溶解させて、含浸液を調製し、
前記含浸液に担体を含浸させた後、エイジング(aging)、乾燥、活性化を行い、触媒を生成することを特徴とする、水素化精製触媒の製造方法。 - 前記含浸液を調製する過程において、ニッケル塩、タングステン塩及び/又はIA族の可溶性塩基又は炭酸塩化合物を添加することを特徴とする、請求項1に記載の水素化精製触媒の製造方法。
- 前記含浸液のpH値が10以上であることを特徴とする、請求項1に記載の水素化精製触媒の製造方法。
- 前記ポリアミンキレート剤は、エチレンジアミン四酢酸、トリエチレンテトラアミン、エチレンジアミンのうちの1種類又は多種類であることを特徴とする、請求項1に記載の水素化精製触媒の製造方法。
- 前記ポリアミンキレート剤の添加量は、前記含浸液量の5〜10体積%であることを特徴とする、請求項1に記載の水素化精製触媒の製造方法。
- 前記コバルト塩は、コバルトの硫酸塩、ハロゲン化物、硝酸塩又は酢酸塩から選択されることを特徴とする、請求項1に記載の水素化精製触媒の製造方法。
- 前記コバルト塩は、コバルトの硝酸塩又は酢酸塩であることを特徴とする、請求項6に記載の水素化精製触媒の製造方法。
- 前記担体は、耐高温無機酸化物であることを特徴とする、請求項1に記載の水素化精製触媒の製造方法。
- 前記担体は、酸化アルミニウム、酸化ケイ素、酸化アルミニウム―酸化ケイ素、又は、上述物質から改質したものであることを特徴とする、請求項8に記載の水素化精製触媒の製造方法。
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PCT/CN2010/000418 WO2011103699A1 (zh) | 2010-02-25 | 2010-03-31 | 一种加氢精制催化剂制备方法 |
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CN104941654B (zh) * | 2015-05-21 | 2017-07-21 | 中国石油大学(北京) | 一种氧化铝基加氢精制催化剂及其制备方法与应用 |
CN105214728A (zh) * | 2015-10-14 | 2016-01-06 | 中国石油大学(华东) | 一种非负载型镍钼配合物加氢催化剂的制备方法 |
CN106635135B (zh) * | 2016-12-23 | 2018-08-14 | 兰州石化职业技术学院 | 一种催化裂化汽油的加氢脱硫方法 |
US11788017B2 (en) | 2017-02-12 | 2023-10-17 | Magëmã Technology LLC | Multi-stage process and device for reducing environmental contaminants in heavy marine fuel oil |
US12025435B2 (en) | 2017-02-12 | 2024-07-02 | Magēmã Technology LLC | Multi-stage device and process for production of a low sulfur heavy marine fuel oil |
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JP7080693B2 (ja) * | 2018-03-28 | 2022-06-06 | 日揮触媒化成株式会社 | 炭化水素油の水素化処理触媒、その製造方法、および水素化処理方法 |
CN111151269B (zh) * | 2018-11-08 | 2023-02-03 | 中国石油化工股份有限公司 | 加氢脱硫催化剂的制备方法 |
CN111250103B (zh) * | 2018-11-30 | 2023-04-07 | 中国石油天然气股份有限公司 | 负载型加氢催化剂及其制备方法 |
CN112973737B (zh) * | 2019-12-13 | 2022-04-05 | 中国石油化工股份有限公司 | 一种液相加氢催化剂及其制备方法 |
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CN115845866A (zh) * | 2021-09-23 | 2023-03-28 | 中国石油天然气股份有限公司 | 一种加氢精制催化剂制备方法 |
CN116212887A (zh) * | 2021-12-06 | 2023-06-06 | 中国石油天然气股份有限公司 | 一种加氢精制催化剂及其制备方法 |
CN114950474B (zh) * | 2022-04-26 | 2024-03-22 | 陕西延长石油(集团)有限责任公司 | 一种使用配合物前驱体调控金属负载催化剂金属活性中心分散度的方法 |
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