CN106669706A - Preparation method of hydrotreating catalyst - Google Patents
Preparation method of hydrotreating catalyst Download PDFInfo
- Publication number
- CN106669706A CN106669706A CN201510750630.5A CN201510750630A CN106669706A CN 106669706 A CN106669706 A CN 106669706A CN 201510750630 A CN201510750630 A CN 201510750630A CN 106669706 A CN106669706 A CN 106669706A
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- China
- Prior art keywords
- catalyst
- oxide
- content
- preparation
- methods according
- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000005470 impregnation Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 55
- 238000002803 maceration Methods 0.000 claims description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 18
- GOJUJUVQIVIZAV-UHFFFAOYSA-N 2-amino-4,6-dichloropyrimidine-5-carbaldehyde Chemical group NC1=NC(Cl)=C(C=O)C(Cl)=N1 GOJUJUVQIVIZAV-UHFFFAOYSA-N 0.000 claims description 13
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 13
- 238000007598 dipping method Methods 0.000 claims description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000012752 auxiliary agent Substances 0.000 claims description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000004898 kneading Methods 0.000 claims description 6
- 239000011574 phosphorus Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 claims description 3
- 239000000806 elastomer Substances 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- HIYNGBUQYVBFLA-UHFFFAOYSA-D cobalt(2+);dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Co+2].[Co+2].[Co+2].[Co+2].[Co+2].[O-]C([O-])=O.[O-]C([O-])=O HIYNGBUQYVBFLA-UHFFFAOYSA-D 0.000 claims description 2
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 claims description 2
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 claims description 2
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 2
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims 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 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- -1 thio ammonium molybdate Chemical compound 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 2
- 239000000460 chlorine Substances 0.000 claims 2
- 229910052801 chlorine Inorganic materials 0.000 claims 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- 238000001935 peptisation Methods 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 4
- KJJPLEZQSCZCKE-UHFFFAOYSA-N 2-aminopropane-1,3-diol Chemical compound OCC(N)CO KJJPLEZQSCZCKE-UHFFFAOYSA-N 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 12
- 238000005984 hydrogenation reaction Methods 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000010779 crude oil Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-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
- 239000005864 Sulphur Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- VLXBWPOEOIIREY-UHFFFAOYSA-N dimethyl diselenide Natural products C[Se][Se]C VLXBWPOEOIIREY-UHFFFAOYSA-N 0.000 description 2
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical group S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 240000005702 Galium aparine Species 0.000 description 1
- 235000014820 Galium aparine Nutrition 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 241000612118 Samolus valerandi Species 0.000 description 1
- 244000275012 Sesbania cannabina Species 0.000 description 1
- 241000219793 Trifolium Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- IQYVXTLKMOTJKI-UHFFFAOYSA-L cobalt(ii) chlorate Chemical compound [Co+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O IQYVXTLKMOTJKI-UHFFFAOYSA-L 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical group 0.000 description 1
- 238000010327 methods by industry Methods 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
- 238000000465 moulding Methods 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052815 sulfur oxide Inorganic materials 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/883—Molybdenum and nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/882—Molybdenum and cobalt
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- 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
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- 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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Abstract
The invention discloses a preparation method of a hydrotreating catalyst. The preparation method comprises the following steps: (1) preparing an impregnating solution containing group-VIII metals, group-VIB metals and 2-amino-1,3 propylene glycol, wherein the molar ratio of 2-amino-1,3 propylene glycol in the impregnating solution to group-VIII metal atoms contained in a final catalyst is 0.1:1 to 2:1; (2) impregnating an aluminum oxide carrier by adopting the impregnating solution prepared in the step (1) and firstly treating for 2-60 minutes under the condition that the microwave power is 2-20 W/g after the end of impregnation; then drying to prepare the hydrotreating catalyst. The catalyst prepared by the preparation method disclosed by the invention is easy to fully vulcanize; more Class-II active centers are generated, so that the effective utilization rate of active components is increased, and the activity of the catalyst is improved.
Description
Technical field
The present invention relates to a kind of preparation method of hydrotreating catalyst, is especially suitable for heavy distillate hydrogenation de-
The preparation method of nitrogen, the hydrotreating catalyst of sweetening process.
Background technology
Content containing nitrogen, sulphur, oxygen and metal impurities in crude oil is continuously increased, and crude oil degree of heaviness is constantly deepened,
Pendulum is come true in face of people, and the presence of these impurity not only makes catalyst poisoning in subsequent processes, but also meeting
The pernicious gases such as substantial amounts of sulfur and nitrogen oxides are given off, the health of the mankind and the protection of environment is injured.Using work
Property the high, catalyst of good stability relax can not only process conditions, moreover it is possible to reduce hydrogen consumption, reach energy-saving effect.
Hydroprocessing processes be exactly with containing the VIIIth race in periodic table and group VIB it is metal oxide supported to refractory without
In machine porous material, typically using aluminum oxide, silica, titanium dioxide, carborundum, boron oxide, zirconium oxide and their combinations
Composite carrier together.By dipping process, catalyst precarsor is prepared, then through the drying and roasting of some steps
Operation prepares finished catalyst.Finished catalyst is containing hydrogen sulfide, sulfur-bearing organic compound using presulfurization is front carried out
In the presence of thing or elemental sulfur, oxidized catalyst is set to change into sulphided state catalyst.
The purpose of weighted BMO spaces is to remove the impurity such as nitrogen, sulphur, oxygen in feedstock oil, the quality and quantity of intermediate oil
All increased.For example, it is hydrocracked and is required for pre-processing feedstock oil with hydroforming reaction, prevents miscellaneous in crude oil
Matter makes catalyst poisoning, and catalyst is once be poisoned, and the loss for causing is inestimable.So, hydroprocessing processes are oil refining process
In one of indispensable and particularly significant step.It is known in the art, without the activearm of calcined catalyst
Divide dispersiveness high, weaker model ylid bloom action power is only existed between active metal and carrier, therefore it is anti-to effectively improve catalyst
Should activity.High activity, the development of the catalyst of high stability are always the bottleneck of this area institute Gonna breakthrough, industrial using high living
Property, high stability catalyst not only can voluminous target product, and reaction can also be made to carry out under conditions of relatively relaxing, transport
Turn cycle stretch-out, reduce production cost.
This area is done a lot of work in terms of activity of hydrocatalyst is improved, and many documents have been reported, and are achieved
Great success, is that later research and development are laid a good foundation.CN 85103891 describes the preparation method of hydrogenation conversion catalyst.Should
Method is that phosphorus containg substances and soluble amine compound are separately added into maceration extract, and two kinds of solution is admixed together to be impregnated,
And need to adjust the pH value of maceration extract and the temperature of dipping solution in dipping process.The method prepares catalyst process condition and answers
Miscellaneous, ammonium hydroxide has ammonia to release in course of dissolution, and harmful to environment, denitrification effect is not obvious, is difficult industrialized production.
Chinese patent CN 101590416A describe the preparation method of molybdenum-nickel hydrogenation catalyst, the method be using kneading ~
Two steps of dipping are prepared catalyst, first under conditions of nitric acid presence, by molybdenum oxide, titanium-containing compound, containing phosphatization
Compound and aluminum oxide Jing kneadings, extruded moulding, dry, roasting obtains the aluminum oxide article shaped of titaniferous, phosphorus, molybdenum, then impregnates nickeliferous
Phosphoric acid solution, obtain molybdenum-nickel hydrogenation catalyst after drying, roasting.Chinese patent CN 1052501A disclose hydrogenation and urge
The preparation method of agent.The method is added in the maceration extract containing the metals of Co-W-Mo tri- and helped to improve the activity of catalyst
Agent P, F, B, using segmentation impregnation, after drying, roasting finished catalyst are obtained.Said method is lived in dip loading
Property metal after through high-temperature roasting, active metal component is stronger with the active force of carrier, affect catalyst cure efficiency, and
And also assemble can amount of activated metal component, the decentralization of active metal is affected, and then affect the activity of catalyst.
In Japan Patent JP11033412, a kind of method for preparing load type metal catalyst is disclosed.The method is by gold
The aqueous solution of category salt and surfactant is added in porous media material, and room temperature lower section is put more than 1 hour, and ultrasonic wave is used afterwards
Process the maceration extract 2 hours, it is ultrasonically treated after, the porous media material after this is impregnated was in 120 DEG C of dryings 12 hours
Roasting 2 hours, obtains finished catalyst under 500 DEG C of air atmospheres.The method preparation catalyst process engineering is loaded down with trivial details, and activity is low,
It is unsuitable for industrial mass production.
Japan Patent JP 04 ~ 166231 describes a kind of hydrogenation catalyst preparation method.The method is soaked using substep
Stain, carrier first with phosphorous active metal component solution impregnation after, be dried at room temperature ~ 200 DEG C, impregnated carrier after being dried
Contact with polyol solution, passing below 200 DEG C of dryings, obtain finished catalyst.United States Patent (USP) US 6281333
Disclose a kind of preparation method of hydrotreating catalyst.The carrier loaded active metal maceration extract containing volatile organic components, no
Catalyst is obtained through roasting, in above-mentioned catalyst preparation process, organic additive is added in maceration extract, the catalyst Jing rooms after dipping
Temperature ageing is some as a child, is dried process.There is metal precipitating, color blackening phenomena in dried catalyst surface, and
And have a large amount of dust to occur in catalyst surface.So both have impact on high degree of dispersion of the active component in carrier surface, and to urging
Agent brings adverse effect during later stage filling, directly affects the reactivity of catalyst.
The content of the invention
For the deficiencies in the prior art, the present invention provides a kind of preparation method of hydrotreating catalyst.The method is obtained
Catalyst be easy to full cure, generate more II classes activated centres, increased the effective rate of utilization of active component, improve
The activity of catalyst.
A kind of preparation method of hydrotreating catalyst, comprises the steps：
（1）Prepare and contain group VIII metal, group VIB metal and 2- amino -1, the maceration extract of 3 propane diols, 2- ammonia in maceration extract
The content of propylene glycol of base -1,3 is 0.1 with the mol ratio of contained group VIII metal atom in final catalyst:1~2:1, preferably
0.5:1-1:1；
（2）Using step（1）The maceration extract oxide impregnation alumina supporter of preparation, dipping terminate after first microwave power be 2 ~ 20W/
2 ~ 60min, most preferably preferably 5 ~ 30min, 10 ~ 15min are processed under conditions of g, preferably 6 ~ 18W/g, most preferably 8-10 W/g,
Wherein microwave power presses the Mass Calculation of final catalyst；Then drying is obtained hydrotreating catalyst.
The inventive method step（1）In, group VIII metal is Co and/or Ni, and group VIB metal is W and/or Mo, with most
On the basis of the weight of whole catalyst, the content that group VIII metal is counted with oxide is as 1 wt % ~ 15 wt %, preferred 4wt % ~ 10
Wt %, the content that group VIB metal is counted with oxide is as 10 wt % ~ 30 wt %.It is preferred that 15wt % ~ 25 wt %.Above-mentioned tungsten master
Will be from one or two in ammonium metatungstate, tetrathio ammonium tungstate, molybdenum is essentially from molybdenum oxide, ammonium molybdate, tetrathio molybdic acid
One or more in ammonium, ammonium paramolybdate, nickel mostlys come from nickel nitrate, basic nickel carbonate, nickel oxalate, nickel chloride, nickel acetate
One or more, cobalt mostlys come from one or more of cobalt nitrate, cobalt oxalate, basic cobaltous carbonate, cobaltous chlorate.
The inventive method step（1）In, described maceration extract can as needed contain auxiliary agent, and described auxiliary agent is selected from
One or more in phosphorus, titanium, silicon, zinc, copper, zirconium, boron, fluorine, lanthanum, cerium, vanadium, preferred phosphorus.Auxiliary agent is in terms of oxide in catalyst
In weight content be 0.01% ~ 10%, preferably 0.01% ~ 2%.
The inventive method step（2）In, described alumina support can using commercial goods or self-control, preferably after
Person.Self-control process is as follows：Aluminum hydroxide solid elastomer powder and SB powder are made into catalyst load through kneading, shaping, then drying roasting
Body.The routine shaping assistant such as extrusion aid, binding agent, peptizing agent can be added as needed in kneading process.Described oxidation
Adjuvant component can be contained in alumina supporter.Described drying condition is as follows：Baking temperature be 50 DEG C ~ 300 DEG C, preferably 100 DEG C ~
150 DEG C, drying time 0.5h ~ 22h, preferred 8h ~ 15h.Be dried atmosphere can be air atmosphere, vacuum atmosphere, steam atmosphere,
Inert gas atmosphere etc., is dried under preferred air atmosphere.Described roasting condition is as follows：Sintering temperature is 350 DEG C ~ 650 DEG C, excellent
Select 450 DEG C ~ 550 DEG C, roasting time 0.5h ~ 22h, preferred 8h ~ 15h, most preferably 6 ~ 10h.Forming method mainly has compressing tablet, mould
Plate, powder spin, extrusion, forming oil column etc., the shape of carrier can be spherical, piece shape, bar shaped（Clover or bunge bedstraw herb
Irregular strip）Deng.The shape of carrier can be selected according to specific needs, preferably bar shaped, and carrier dimensions may be selected on request difference.
The inventive method step（2）, described baking temperature is 100 DEG C ~ 250 DEG C, preferably 120 DEG C ~ 200 DEG C, when being dried
Between 0.5h ~ 5h, preferred 1h ~ 3h.
Result of study shows that 2- amino -1 in maceration extract of the present invention, 3 propane diols have with group VIII metal atom Ni or Co
Stronger interaction, can form stable comple.Particularly above-mentioned complex compound 2- ammonia under suitable microwave treatment conditions
Base -1, the active force of the chelate bonds that 3 propane diols are formed with group VIII metal atom Ni or Co is further strengthened, and makes Ni or Co
Curing temperature significantly improve than the curing temperature of Mo or W, postpone Ni or Co sulfuration, increase molybdenum or the sulphidity of tungsten, hold
Class Ni (Co)-Mo (the W)-S of high activity II activated centres are easily formed, and can at short notice make active component be dispersed in load
Body surface face, specific surface area of catalyst is big, and active bit quantity increases, and substantially increases active component effective rate of utilization, reduces catalysis
The cost of agent.
Specific embodiment
The present invention is further elaborated below by embodiment, but following examples do not constitute the limit to the inventive method
System.In the present invention, wt% is mass fraction.
Embodiment 1（It is prepared by alumina support）
200 grams of aluminum hydroxide solid elastomer powder is weighed, 100 grams of SB powder adds sesbania powder and citric acid each 4 grams, adds after mixing acid
Solution, the concentration of nitric acid is 2wt% in acid solution, and remaining is distilled water.Roll 15 ~ 25 minutes, with the three of a diameter of 1.7mm
Leaf grass orifice plate carries out extrusion, 120 DEG C of Jing dryings 12 hours, 550 DEG C of roastings 3 hours, obtains alumina support, i.e. Z-1, its property
It is as follows：Pore volume is 0.72ml/g, and specific surface area is 342m2/g。
Embodiment 2
Appropriate carrier Z-1 is weighed, with Mo, Ni, P, 2- amino -1 is contained, the maceration extract of 3 propane diols carries out waiting body to carrier Z-1
Product dipping, maceration extract consists of MoO3Content be 88.5g/100ml, NiO contents are 15 g/100ml, and the content of P is
2.3g/100ml, 2- amino -1, the consumption of 3 propane diols is 0.5 with the mol ratio of Ni atoms in final catalyst:1.Dipping terminates
After carry out microwave treatment, the power of microwave is 8 W/g, and process time is 15min, and the sample after microwave treatment is in 180 DEG C of air
Drying under atmosphere obtains catalyst C-1 in 3 hours, and catalyst consists of 23%MoO3, 3.6%NiO, 1.5% p.
Embodiment 3
Appropriate catalyst carrier Z-1 is weighed, with Mo, Ni, P, 2- amino -1 is contained, the maceration extract of 3 propane diols is to carrier Z-1
Carry out incipient impregnation, maceration extract consists of MoO3Content be 89.5g/100ml, NiO contents be 15 g/100ml, P's
Content is 2.5g/100ml, and 2- amino -1, the consumption of 3 propane diols is 1 with the mol ratio of Ni contents in final catalyst:1.Leaching
Sample after stain carries out microwave treatment, and the power of microwave is 10 W/g, and process time is 15min, and the sample after microwave treatment exists
Drying under 150 DEG C of air atmospheres obtains catalyst C-2 in 1 hour, and catalyst consists of 23%MoO3, 3.6%NiO, 1.63% p.
Embodiment 4
Appropriate catalyst carrier Z-1 is weighed, with Mo, Ni, P, 2- amino -1 is contained, the maceration extract of 3 propane diols enters to carrier Z-1
Went volume impregnation, maceration extract consists of MoO3Content be 89.5g/100ml, NiO contents be 15 g/100ml, P's contains
Measure as 2.5g/100ml, 2- amino -1, the consumption of 3 propane diols is 1 with the mol ratio of Ni contents in final catalyst:1.After filtration
Sample carry out microwave treatment, the power of microwave is 10W/g, and process time is 25min, and the sample after microwave treatment is at 180 DEG C
Drying under air atmosphere obtains catalyst C-3 in 1 hour, and catalyst consists of 23%MoO3, 3.6%NiO, 1.63% p.
Embodiment 5
Appropriate catalyst carrier Z-1 is weighed, with Mo, Co, P, 2- amino -1 is contained, the maceration extract of 3 propane diols enters to carrier Z-1
Went volume impregnation, maceration extract consists of MoO3Content be 89.5g/100ml, CoO contents be 13.5 g/100ml, P's
Content is 2.2g/100ml, and the consumption of the propane diols of 2- amino -1,3 is 0.8 with the mol ratio of Ni contents in final catalyst:1.
Sample after filtration carries out microwave treatment, and the power of microwave is 15W/g, and process time is 20min, and the sample after microwave treatment exists
Drying under 130 DEG C of air atmospheres obtains catalyst C-4 in 3 hours, and catalyst consists of 23%MoO3, 3.6%CoO, 1.48% p.
Comparative example 1
It is added without 2- amino -1,3 propane diols, remaining obtains catalyst C-5 with embodiment 1.
Comparative example 2
Microwave treatment is not carried out, remaining obtains catalyst C-6 with embodiment 1.
Comparative example 3
Using citric acid replacement 2- amino -1 of same molar, 3 propane diols, remaining obtains catalyst C-7 with embodiment 1.
The catalyst of above-described embodiment and comparative example carries out active evaluation test, institute in the small-sized hydrogenation reaction devices of 50ml
It is atmosphere 3rd side cut diesel oil with raw material, property is shown in Table 1.Catalyst will carry out presulfurization using before, and sulfurized oil is virgin kerosene, wherein
Add the DMDS of 5wt%（DMDS）, feedstock oil is introduced directly into after presulfurization carries out test reaction.Presulfurization and test bar
Part is shown in Table 2, and evaluation result is shown in Table 3.
Table 1
Table 2
Table 3
From data in table 3, prepared apparently higher than comparative example method using the activity of the catalyst of the inventive method preparation
Catalyst.
Table 4
| Catalyst is numbered | C-1 | C-2 | C-3 | C-4 | C-5 | C-6 | C-7 |
| With respect to denitrification activity, % | 139 | 155 | 140 | 142 | 100 | 118 | 121 |
| It is relatively desulphurizing activated, % | 132 | 145 | 128 | 121 | 98 | 102 | 110 |
C-1 ~ C-7 catalyst 1200h Activity evaluations are shown in Table 4, and by data in table 4 the inventive method preparation is can be seen that
Catalyst stability is good, is conducive to long-term operation.
Claims (18)
1. a kind of preparation method of hydrotreating catalyst, it is characterised in that：Comprise the steps：
（1）Prepare and contain group VIII metal, group VIB metal and 2- amino -1, the maceration extract of 3 propane diols, 2- ammonia in maceration extract
The content of propylene glycol of base -1,3 is 0.1 with the mol ratio of contained group VIII metal atom in final catalyst:1~2:1；
（2）Using step（1）The maceration extract oxide impregnation alumina supporter of preparation, dipping terminate after first microwave power be 2 ~ 20W/
2 ~ 60min is processed under conditions of g, then drying is obtained hydrotreating catalyst.
2. method according to claim 1, it is characterised in that：Step（1）The content of propylene glycol of 2- amino -1,3 in maceration extract
It is 0.5 with the mol ratio of contained group VIII metal atom in final catalyst:1-1:1.
3. method according to claim 1, it is characterised in that：Step（2）Dipping terminate after first microwave power be 6 ~
5 ~ 30min is processed under conditions of 18W/g.
4. method according to claim 3, it is characterised in that：Step（2）Dipping terminate after first microwave power be 8-
10 ~ 15min is processed under conditions of 10 W/g.
5. method according to claim 1, it is characterised in that：Step（1）In, group VIII metal be Co and/or Ni, the VIth
B races metal is W and/or Mo, and on the basis of the weight of final catalyst, the content that group VIII metal is counted with oxide is as 1 wt %
~ 15 wt %, the content that group VIB metal is counted with oxide is as 10 wt % ~ 30 wt %.
6. method according to claim 5, it is characterised in that：On the basis of the weight of final catalyst, group VIII metal
, as 4wt % ~ 10 wt %, the content that group VIB metal is counted with oxide is as 15wt % ~ 25 wt % for the content counted with oxide.
7. method according to claim 5, it is characterised in that：The one kind of tungsten in ammonium metatungstate, tetrathio ammonium tungstate
Or two kinds.
8. method according to claim 5, it is characterised in that：Molybdenum is from molybdenum oxide, ammonium molybdate, four thio ammonium molybdate, secondary
One or more in ammonium molybdate.
9. method according to claim 5, it is characterised in that：Nickel comes from nickel nitrate, basic nickel carbonate, nickel oxalate, chlorine
One or more of change nickel, nickel acetate.
10. method according to claim 5, it is characterised in that：Cobalt comes from cobalt nitrate, cobalt oxalate, basic cobaltous carbonate, chlorine
One or more of sour cobalt.
11. methods according to claim 1, it is characterised in that：Step（1）Described in maceration extract contain auxiliary agent, it is described
One or more in phosphorus, titanium, silicon, zinc, copper, zirconium, boron, fluorine, lanthanum, cerium, the vanadium of auxiliary agent.
12. methods according to claim 11, it is characterised in that：Auxiliary agent is phosphorus.
13. methods according to claim 11, it is characterised in that：Weight content of the auxiliary agent in terms of oxide in the catalyst
For 0.01% ~ 10%.
14. methods according to claim 1, it is characterised in that：Step（2）Middle carrying alumina production procedure is as follows：Will
Aluminum hydroxide solid elastomer powder and SB powder kneadings, shaping, then make catalyst carrier after drying, roasting.
15. methods according to claim 14, it is characterised in that：Extrusion aid, binding agent and peptization are added in kneading process
Agent.
16. methods according to claim 14, it is characterised in that：Described drying condition is as follows：Baking temperature be 50 DEG C ~
300 DEG C, drying time 0.5h ~ 22h, described roasting condition is as follows：Sintering temperature is 350 DEG C ~ 650 DEG C, roasting time 0.5h ~
22h。
17. methods according to claim 1, it is characterised in that：Step（2）Described baking temperature is 100 DEG C ~ 250 DEG C,
Drying time 0.5h ~ 5h.
18. methods according to claim 17, it is characterised in that：Step（2）Described baking temperature is 120 DEG C ~ 200
DEG C, drying time 1h ~ 3h.
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| CN110280258A (en) * | 2019-08-02 | 2019-09-27 | 北京高新利华科技股份有限公司 | A kind of diesel oil hydrofining catalyst and preparation method thereof |
| CN111729689A (en) * | 2020-06-19 | 2020-10-02 | 湖北中超化工科技有限公司 | Regeneration method of deactivated hydrogenation catalyst |
| CN111974406A (en) * | 2019-05-22 | 2020-11-24 | 环球油品有限责任公司 | Process for preparing highly reactive metal oxide and metal sulfide materials |
| CN116139884A (en) * | 2022-12-31 | 2023-05-23 | 中国海洋石油集团有限公司 | Preparation method of vulcanized hydrogenation catalyst |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111974406A (en) * | 2019-05-22 | 2020-11-24 | 环球油品有限责任公司 | Process for preparing highly reactive metal oxide and metal sulfide materials |
| CN110280258A (en) * | 2019-08-02 | 2019-09-27 | 北京高新利华科技股份有限公司 | A kind of diesel oil hydrofining catalyst and preparation method thereof |
| CN110280258B (en) * | 2019-08-02 | 2022-05-17 | 北京高新利华科技股份有限公司 | Diesel oil hydrofining catalyst and preparation method thereof |
| CN111729689A (en) * | 2020-06-19 | 2020-10-02 | 湖北中超化工科技有限公司 | Regeneration method of deactivated hydrogenation catalyst |
| CN116139884A (en) * | 2022-12-31 | 2023-05-23 | 中国海洋石油集团有限公司 | Preparation method of vulcanized hydrogenation catalyst |
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