JP6842428B2 - 高hdn選択性水素化処理触媒 - Google Patents
高hdn選択性水素化処理触媒 Download PDFInfo
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- JP6842428B2 JP6842428B2 JP2017561845A JP2017561845A JP6842428B2 JP 6842428 B2 JP6842428 B2 JP 6842428B2 JP 2017561845 A JP2017561845 A JP 2017561845A JP 2017561845 A JP2017561845 A JP 2017561845A JP 6842428 B2 JP6842428 B2 JP 6842428B2
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- 239000003054 catalyst Substances 0.000 title claims description 150
- 238000005984 hydrogenation reaction Methods 0.000 title claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 162
- 239000002184 metal Substances 0.000 claims description 162
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 53
- 229910052739 hydrogen Inorganic materials 0.000 claims description 53
- 239000001257 hydrogen Substances 0.000 claims description 53
- 238000000034 method Methods 0.000 claims description 46
- 229910052698 phosphorus Inorganic materials 0.000 claims description 45
- 239000011574 phosphorus Substances 0.000 claims description 41
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 40
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 39
- 239000000203 mixture Substances 0.000 claims description 38
- 239000011148 porous material Substances 0.000 claims description 33
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 32
- 230000000737 periodic effect Effects 0.000 claims description 22
- 229910052759 nickel Inorganic materials 0.000 claims description 18
- 229910052750 molybdenum Inorganic materials 0.000 claims description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 12
- 239000011733 molybdenum Substances 0.000 claims description 12
- 239000010941 cobalt Substances 0.000 claims description 10
- 229910017052 cobalt Inorganic materials 0.000 claims description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 9
- 239000010937 tungsten Substances 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 239000011651 chromium Substances 0.000 claims description 6
- 230000000977 initiatory effect Effects 0.000 claims description 3
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- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 150000004678 hydrides Chemical class 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 59
- 239000003921 oil Substances 0.000 description 33
- 229910052757 nitrogen Inorganic materials 0.000 description 29
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 27
- 229910052717 sulfur Inorganic materials 0.000 description 27
- 239000011593 sulfur Substances 0.000 description 27
- 238000006243 chemical reaction Methods 0.000 description 22
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- 229910001868 water Inorganic materials 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
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- -1 VIB metals Chemical class 0.000 description 6
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
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- IYYZUPMFVPLQIF-UHFFFAOYSA-N dibenzothiophene Chemical compound C1=CC=C2C3=CC=CC=C3SC2=C1 IYYZUPMFVPLQIF-UHFFFAOYSA-N 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000010763 heavy fuel oil Substances 0.000 description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000012876 carrier material Substances 0.000 description 3
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- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
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- 239000002245 particle Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000011949 solid catalyst Substances 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
- FCEHBMOGCRZNNI-UHFFFAOYSA-N 1-benzothiophene Chemical compound C1=CC=C2SC=CC2=C1 FCEHBMOGCRZNNI-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- 238000004438 BET method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 150000002391 heterocyclic compounds Chemical class 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- 239000002904 solvent Substances 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- UCRCDTHCRQNEPN-UHFFFAOYSA-N 4,6-dimethyldibenzothiophene Chemical compound CC1=CC=CC2=C1SC1=C2C=CC=C1C.CC1=CC=CC2=C1SC1=C2C=CC=C1C UCRCDTHCRQNEPN-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- MYAQZIAVOLKEGW-UHFFFAOYSA-N DMDBT Natural products S1C2=C(C)C=CC=C2C2=C1C(C)=CC=C2 MYAQZIAVOLKEGW-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 description 1
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 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
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical group [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 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
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000012736 aqueous medium Substances 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
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 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
- 239000000356 contaminant Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
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- 239000006260 foam Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- ZLTPDFXIESTBQG-UHFFFAOYSA-N isothiazole Chemical compound C=1C=NSC=1 ZLTPDFXIESTBQG-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 235000012245 magnesium oxide Nutrition 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002897 organic nitrogen compounds Chemical class 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 150000004032 porphyrins Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
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- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 238000005507 spraying Methods 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 239000011275 tar sand Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000002699 waste material Substances 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
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
-
- 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
- B01J21/04—Alumina
-
- 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
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
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Description
[0003] 本発明は、JX日鉱日石エネルギー株式会社(100−8162 東京都千代田区大手町二丁目6番3号)と、Advanced Refining Technologies L.L.C.(7500 Grace Drive,Columbia,MD)との間の共同研究契約により開発された。
(a)0.60:1未満の第VIII族金属成分対リン成分のモル比、
(b)0.45:1未満の第VIII族金属成分対第VIB族金属成分のモル比、
(c)0.23:1超のリン成分対第VIB族金属成分のモル比、及び
(d)75Å超かつ95Å未満のメディアン孔径、を有することを特徴とする。
[0012] 本明細書で用いられるとき、以下の用語又は語句は指定の意味を有する。
[0013] 「窒素」への言及は、元素窒素自体、並びに、窒素を含有する化合物の例示としてである。同様に、「イオウ」への言及は、元素イオウ、並びに、イオウを含有する化合物の例示としてである。
[0016] 本発明の触媒を含むプロセスを用いて典型的に処理される「供給原料」、つまり石油供給原料は、「重質」又は「軽質」という用語で説明されることが多い。石油留分に対する用語である「軽質」及び「重質」は、精製業における一般的な意味で本明細書で使用され、それぞれ比較的低沸点及び高沸点範囲を指す。重質燃料油(HFO)は、最終生成物(残渣燃料)と、これらが配合される一次精製流の両方を含む。重質燃料油類のメンバーは、様々な分子量、炭素数(典型的には、約C7〜約C50)、及び約121℃〜600℃(約250°F〜約1112°F)の沸点を有する炭化水素を含む多様な物質群である。これらは、石油炭化水素に加え、イオウ、窒素、及び酸素を含有する1つ又は2つ以上の複素環式化合物、及び有機金属性又は金属性化合物を含有する。完成した重質燃料(残渣燃料)は、原油供給原料から、より質の高い炭化水素全てを事実上蒸留し、クラッキングし、又は触媒的に除去した後に、精製プロセスの残渣油を主に含む生成物である。実質的に全て(少なくとも90体積%)の炭化水素の供給流、つまり供給原料は、典型的には、約300°F〜1050°F、好ましくは約600°F〜1000°Fの範囲の沸点に含まれる。供給原料は、常圧軽油及び減圧軽油(AGO及びVGO)などの石油留分の混合物を含み得る。好適な供給原料として、重質炭化水素系鉱物若しくは合成油、又はこれらの1つ若しくは2つ以上の留分の組み合わせが挙げられる。したがって、直留軽油、減圧軽油、脱金属油、常圧残渣油、減圧残渣油、脱アスファルト減圧残渣油、脱アスファルト溶剤、コーカー蒸留物、接触分解蒸留物、シェール油、タールサンド油、液化石炭などとして既知の供給原料、及びこれらの混合物が意図される。好ましい供給原料は、約500℃超(約932°F超)以上の温度から始まる沸点範囲を有するであろう。好適な供給原料は、典型的には、通常は有機窒素化合物として、1ppmから4.0重量%未満の量で存在する窒素を含む。供給原料は、通常は、5重量%未満、好ましくは4重量%未満のイオウ含量をもたらすのに十分な、イオウ含有化合物も含むであろう。任意の特定の製油所から回収した様々な生成物留分の沸点範囲は、原油源の特性、製油所の地方の市場、製品価格などといった因子により変化し得る。
[0020] 「表面積」は、本明細書では、BET表面積測定法により決定される比表面積を指す。表面積を測定するBET法は、参照することによって本明細書に組み込まれるBrunauer、Emmett及びTellerのJ.Am.Chem.Soc.60(1938)309〜319に詳述されている。
[0038] 「前含浸」触媒は、有孔性の触媒キャリアが形成される前に、金属含有液が添加される触媒を指す。「後含浸」触媒は、有孔性の触媒キャリアが形成された後に、金属含有液が添加される触媒を指す。触媒粒子の形成前又は後に、有孔性触媒キャリアを焼成できる。焼成され成形されたキャリアが含浸され、その後再度焼成される、後含浸が好ましい。
[0044] 成形された触媒の表面積は、一実施形態では、約150〜約350m2/gの範囲であってよい。本発明の別の実施形態では、担体の表面積は、約200〜約320m2/gの範囲であってよい。
[0049] リン含有酸性成分の量は、第VIII族金属成分対リン含有酸性成分のモル比が約0.60:1未満、別の実施形態では約0.55:1未満、別の実施形態では約0.53:1未満であるのに十分であり、一実施形態では、かかる比は、典型的には、約0.05:1〜約0.59:1、別の実施形態では約0.10:1〜約0.53:1、別の実施形態では約0.25:1〜約0.50:1の範囲であってよい。
[0052] 焼成は、少なくとも一部、好ましくは全ての金属成分又は前駆体を酸化物形態に変換するのに十分な温度及び時間で実施され、これらの条件は、一実施形態では約300℃〜約900℃、別の実施形態では約450℃〜約650℃で、一実施形態では約0.5〜約3時間、別の実施形態では約0.5〜約2時間の範囲であってよい。
一連の4種類の触媒を調製し、それらの水素処理活性について試験した。触媒は、表1にまとめたMo、Ni、Co、及びPから選択される金属を、様々な量でアルミナ担体上に含んでおり(実験1〜4)、一連の参照触媒と比較する(実験5〜8)。触媒を、パートEに記載するように試験した。供給原料は、パートDに記載されるものとした。反応条件は、パートEに示されるものであった。表3は各触媒の特性を示し、表4は各触媒の反応成績を示す。各反応(HDS、HDN及び水素化脱金属(HDM))の速度定数は、360、380及び400℃での結果に基づき、一次反応速度論と仮定する。HDN選択性は、kHDN/kHDSとして計算する。塩基性窒素除去は、原料と生成物の塩基性窒素含量の測定値から計算する。金属耐性は、HDS活性が、初期活性の20%まで低下するのに要した時間を計算する。実験1〜4の触媒は本発明の触媒であるが、実験5〜8の触媒は比較対象として提供される。結果は、対照実験8の成績に対する割合として示される。実験4は、一番高いHDN選択性を示す。
[0077] 水素/油比:1000L/L
[0078] LHSV:0.44時−1
[0079] 水素分圧:14.4MPa
[0080] HDM及びHDS両段階の反応温度:68、45、及び45時間それぞれの反応時間において、360、380及び400℃の各温度。
[0084] 以下に列挙した段落は、本発明の様々な、かつ別の実施形態を示す。
[0085] 少なくとも1種の金属含有触媒成分と、少なくとも1種のリン含有触媒成分と、を含む、担持された触媒であって、金属含有触媒成分中の金属は、元素周期表の第VIB族から選択される少なくとも1種、元素周期表の第VIII族から選択される少なくとも1種の別の金属であり、そしてかかる触媒成分は有孔担体上に担持されており、かかる触媒は、
(a)0.60:1未満の第VIII族金属成分対リン成分のモル比、
(b)0.45:1未満の第VIII族金属成分対第VIB族金属成分のモル比、
(c)0.23:1超のリン成分対第VIB族金属成分のモル比、及び
(d)75Å超かつ95Å未満のメディアン孔径、を有することを特徴とする、触媒。
(b)第VIII族金属成分対第VIB族金属成分のモル比が、約0.05:1〜約0.44:1であり、
(c)リン成分対第VIB族金属成分のモル比が、約0.24:1〜約0.95:1であり、
(d)メディアン孔径が、約78〜約92Åであり、そして
(e)担体がアルミナを含む、段落[0084]の実施形態に記載の触媒。
(b)第VIB族金属が、クロム、タングステン及びモリブデン、並びにこれらの混合物から選択される、段落[0085]の実施形態に記載の触媒。
[0089] 供給原料の水素処理中に高HDN選択性を有する触媒の調製方法であって、有孔担体を、少なくとも1種の金属含有触媒成分と、少なくとも1種のリン含有触媒成分と、を含有する水溶液で含浸することであって、金属含有触媒成分中の金属は、元素周期表の第VIB族から選択される少なくとも1種であり、金属含有触媒成分中の少なくとも1種の別の金属は、元素周期表の第VIII族から選択され、かかる成分は金属酸化物に熱分解可能である、ことと、その後、得られる含浸した担体を乾燥して焼成し、担持された触媒をもたらすことと、を含み、かかる担持された触媒が、
(a)0.60未満の第VIII族金属成分対リン成分のモル比、
(b)0.45未満の第VIII族金属成分対第VIB族金属成分のモル比、
(c)0.23超のリン成分対第VIB族金属成分のモル比、及び
(d)75Å超かつ95Å未満のメディアン孔径、を有することを特徴とする、方法。
(b)第VIII族金属成分対第VIB族金属成分のモル比が、約0.05:1〜約0.44:1であり、
(c)リン成分対第VIB族金属成分のモル比が、約0.24:1〜約0.95:1であり、
(d)メディアン孔径が、約78〜約92Åであり、そして
(e)担体がアルミナを含む、段落[0088]の実施形態に記載の方法。
(b)第VIB族金属が、クロム、タングステン及びモリブデン、並びにこれらの混合物から選択される、段落[0089]の実施形態に記載の方法。
少なくとも1種の金属含有触媒成分と、少なくとも1種のリン含有触媒成分と、を含む、担持された触媒であって、前記金属含有触媒成分中の少なくとも1種の金属は、クロム、タングステン及びモリブデンから選択される、元素周期表の第VIB族であり、前記金属含有触媒成分中の少なくとも1種の別の金属は、コバルト及びニッケルから選択される元素周期表の第VIII族であり、そして前記触媒成分は小孔担体上に担持されており、前記触媒が、
(a)約0.05:1〜約0.59:1の第VIII族金属成分対リン成分のモル比、
(b)約0.05:1〜約0.44:1の第VIII族金属成分対第VIB族金属成分のモル比、
(c)約0.24:1〜約0.95:1のリン成分対第VIB族金属成分のモル比、
(d)約78〜約92Åのメディアン孔径、及び、
(e)アルミナを含む担体、を有することを特徴とし、そして
(1)前記触媒の表面積が、約150〜約350m2/gであり、かつ
(2)前記担体の総細孔容積が、約0.5〜約1.1cc/gである、触媒。
Claims (10)
- 少なくとも1種の金属含有触媒成分と、少なくとも1種のリン含有触媒成分と、を含む、担持された水素処理触媒であって、前記金属含有触媒成分中の金属は、元素周期表の第VIB族から選択される少なくとも1種、元素周期表の第VIII族から選択される少なくとも1種の別の金属であり、そして前記触媒成分は有孔担体上に担持されており、前記触媒が、
(a)0.60:1未満の第VIII族金属成分対リン成分のモル比、
(b)0.45:1未満の第VIII族金属成分対第VIB族金属成分のモル比、
(c)約0.65:1〜約0.90:1のリン成分対第VIB族金属成分のモル比、及び
(d)約80Å〜約90Åのメディアン孔径、を有することを特徴とし、
前記担体の総細孔容積は約0.65〜約0.9cc/gである、
水素処理触媒。 - (a)前記第VIII族金属成分対リン成分のモル比が、約0.05:1〜約0.59:1であり、
(b)前記第VIII族金属成分対第VIB族金属成分のモル比が、約0.05〜約0.44:1であり、
(c)前記リン成分対第VIB族金属成分のモル比が、約0.65:1〜約0.90:1であり、
(d)前記担体がアルミナを含む、請求項1に記載の触媒。 - (a)前記第VIII族金属が、コバルト、ニッケル及びこれらの混合物から選択され、そして
(b)前記第VIB族金属が、クロム、タングステン及びモリブデン、並びにこれらの混合物から選択される、請求項2に記載の触媒。 - 前記触媒の表面積が、約150〜約350m2/gである、請求項1に記載の触媒。
- 152%以上の水素化脱窒素(HDN)選択性と50%以上の相対金属耐性との組合せを示し、ここでHDN選択性は、水素化脱窒素の速度定数の水素化脱硫(HDS)の速度定数に対する比(kHDN/kHDS)として計算され、そして相対金属耐性は、HDS活性が、初期活性の20%まで低下するのに要した時間として計算される、請求項1に記載の触媒。
- 供給原料の水素処理中に高い水素化脱窒素(HDN)選択性を有する触媒の調製方法であって、有孔担体を、少なくとも1種の金属含有触媒成分と、少なくとも1種のリン含有触媒成分と、を含有する水溶液で含浸することであって、前記金属含有触媒成分中の金属は、元素周期表の第VIB族から選択される少なくとも1種であり、前記金属含有触媒成分中の少なくとも1種の別の金属は、元素周期表の第VIII族から選択され、前記成分は金属酸化物に熱分解可能である、ことと、その後、得られた前記含浸した担体を乾燥して焼成し、担持された触媒をもたらすことと、を含み、前記担持された触媒が、
(a)0.60未満の第VIII族金属成分対リン成分のモル比、
(b)0.45未満の第VIII族金属成分対第VIB族金属成分のモル比、
(c)約0.65:1〜約0.90:1のリン成分対第VIB族金属成分のモル比、及び
(d)約80Å〜約90Åのメディアン孔径、を有することを特徴とし、
前記担体の総細孔容積は約0.65〜約0.9cc/gである、
方法。 - (a)前記第VIII族金属成分対リン成分のモル比が、約0.05:1〜約0.59:1であり、
(b)前記第VIII族金属成分対第VIB族金属成分のモル比が、約0.05〜約0.44:1であり、
(c)前記リン成分対第VIB族金属成分のモル比が、約0.65:1〜約0.90:1であり、そして
(d)前記担体がアルミナを含む、請求項6に記載の方法。 - (a)前記第VIII族金属が、コバルト、ニッケル及びこれらの混合物から選択され、そして
(b)前記第VIB族金属が、クロム、タングステン及びモリブデン、並びにこれらの混合物から選択される、請求項7に記載の方法。 - 前記供給原料の水素処理中に高い水素化脱窒素(HDN)選択性を有する触媒が152%以上の水素化脱窒素(HDN)選択性と50%以上の相対金属耐性との組合せを示し、ここでHDN選択性は、水素化脱窒素の速度定数の水素化脱硫(HDS)の速度定数に対する比(kHDN/kHDS)として計算され、そして相対金属耐性は、HDS活性が、初期活性の20%まで低下するのに要した時間として計算される、請求項6に記載の方法。
- 少なくとも1種の金属含有触媒成分と、少なくとも1種のリン含有触媒成分と、を含む、担持された水素処理触媒であって、前記金属含有触媒成分中の少なくとも1種の金属は、クロム、タングステン及びモリブデンから選択される、元素周期表の第VIB族であり、前記金属含有触媒成分中の少なくとも1種の別の金属は、コバルト及びニッケルから選択される元素周期表の第VIII族であり、そして前記触媒成分は有孔担体上に担持されており、
前記触媒が、
(a)約0.05:1〜約0.59:1の第VIII族金属成分対リン成分のモル比、
(b)約0.05:1〜約0.44:1の第VIII族金属成分対第VIB族金属成分のモル比、
(c)約0.65:1〜約0.90:1のリン成分対第VIB族金属成分のモル比、
(d)約80Å〜約90Åのメディアン孔径、及び、
(e)アルミナを含む担体、を有することを特徴とし、そして
(1)前記触媒の表面積が、約150〜約350m2/gであり、かつ
(2)前記担体の総細孔容積が、約0.65〜約0.9cc/gである、水素処理触媒。
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