US20100298129A1 - selective nickel based hydrogenation catalyst and the preparation thereof - Google Patents
selective nickel based hydrogenation catalyst and the preparation thereof Download PDFInfo
- Publication number
- US20100298129A1 US20100298129A1 US12/741,017 US74101708A US2010298129A1 US 20100298129 A1 US20100298129 A1 US 20100298129A1 US 74101708 A US74101708 A US 74101708A US 2010298129 A1 US2010298129 A1 US 2010298129A1
- Authority
- US
- United States
- Prior art keywords
- catalyst
- carrier
- oxide
- nickel
- hours
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
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- 239000003054 catalyst Substances 0.000 title claims abstract description 82
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 52
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 47
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims abstract description 9
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 5
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 5
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011148 porous material Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- 238000004898 kneading Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 5
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims 1
- 150000001993 dienes Chemical class 0.000 abstract description 17
- 238000000197 pyrolysis Methods 0.000 abstract description 15
- 239000000084 colloidal system Substances 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 29
- 238000003756 stirring Methods 0.000 description 16
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 229910052593 corundum Inorganic materials 0.000 description 12
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 12
- 229910001845 yogo sapphire Inorganic materials 0.000 description 12
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 9
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 8
- 239000011630 iodine Substances 0.000 description 8
- 229910052740 iodine Inorganic materials 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052785 arsenic Inorganic materials 0.000 description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 5
- 229910052684 Cerium Chemical class 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical class [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 4
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 3
- 229940010552 ammonium molybdate Drugs 0.000 description 3
- 235000018660 ammonium molybdate Nutrition 0.000 description 3
- 239000011609 ammonium molybdate Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical class [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- MVDSFVJLJCMBEZ-UHFFFAOYSA-N [I].[S].[As] Chemical compound [I].[S].[As] MVDSFVJLJCMBEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 2
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- PACGUUNWTMTWCF-UHFFFAOYSA-N [Sr].[La] Chemical compound [Sr].[La] PACGUUNWTMTWCF-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000005673 monoalkenes Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004230 steam cracking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- B01J23/83—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 rare earths or actinides
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- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/84—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
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- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
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- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- B01J23/85—Chromium, molybdenum or tungsten
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- B01J37/024—Multiple impregnation or coating
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- C—CHEMISTRY; METALLURGY
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
- C10G45/06—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
-
- 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
- B01J23/70—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
- B01J23/78—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 alkali- or alkaline earth metals
-
- 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
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/02—Gasoline
Definitions
- the present invention relates to a selective nickel-based hydrogenation catalyst and the preparation thereof.
- the catalyst is useful in selective hydrogenation of medium or low distillate oil, in particular, in the first-stage selective hydrogenation process of pyrolysis gasoline distillate.
- Pyrolysis gasoline is the by-product of steam cracking to make ethylene, which approximately comprises more than 50% of the production capacity of ethylene.
- Pyrolysis gasoline contains highly unsaturated hydrocarbons, such as diolefin, styrene and the like, which can be converted into corresponding monoolefin by selective hydrogenation.
- the hydrogenation of pyrolysis gasoline has developed toward the hydrogenation of full distillate using nickel-based catalyst.
- the pyrolysis gasoline raw materials Due to the variability of the pyrolysis gasoline raw materials and the differences in pyrolysis apparatus and pyrolysis modes, the pyrolysis gasoline raw materials are deteriorated, and the hydrogenation load and the content of impurity such as arsenic are increased, thereby causing the inferior performance of palladium-based catalyst for first-stage hydrogenation.
- the pyrolysis gasoline raw materials are deteriorated, and the hydrogenation load and the content of impurity such as arsenic are increased, thereby causing the inferior performance of palladium-based catalyst for first-stage hydrogenation.
- For noble metal catalyst its arsenic and colloid resistance as well as water resistance is low, since the impurity arsenic tends to occupy the empty orbital of Pd, and Pd is located on the surface layer of the catalyst with a content of only parts per thousand.
- non-noble metal catalyst For non-noble metal catalyst, it has certain arsenic tolerance and colloid and water resistance due to the structural difference and high metal content; moreover, it has relatively remarkable price advantage. Thus, there is need of the market and technical competition to develop a new nickel-based catalyst for first-stage hydrogenation of full distillate pyrolysis gasoline.
- U.S. Pat. No. 3,472,763 reports a Ni/Al 2 O 3 catalyst for the selective hydrogenation of diolefin, comprising 1-20% nickel as active component, 1-5% MoO 3 as aids, 1-5% alkali metal and alkaline earth metal as aids, and having a pore volume of more than 0.4 ml/g and a specific surface area of more than 30 m 2 /g.
- This catalyst is prepared by impregnating the Al 2 O 3 carrier with the aqueous solution of above-mentioned active component and aids.
- CN1218822A reports a Ni/Al 2 O 3 catalyst suitable for the selective hydrogenation of pyrolysis gasoline distillates. This catalyst is prepared by loading nickel on alumina carrier comprising lithium or alkaline earth metal. However, this catalyst is not good at withstanding the hydrogenation load and its hydrogenation stability is to be improved.
- An excellent selective hydrogenation catalyst should have higher hydrogenation activity and better selectivity. More importantly, it should have good stability. That is to say, it is necessary for such catalyst to have capability to resist impurity and colloid, thereby prolonging its lifetime.
- the aim of the present invention is to develop a nickel-based Al 2 O 3 supported catalyst for selective hydrogenation of diolefin.
- the catalyst has good hydrogenation performance, especially has good hydrogenation stability, and can be applied to the selective hydrogenation of full distillate pyrolysis gasoline.
- the selective nickel-based hydrogenation catalyst of the present invention is characterized in that based on the total weight of the catalyst, it comprises:
- said catalyst has a specific surface area of 60-150 m 2 /g and a pore volume of 0.4-0.6 ml/g.
- This catalyst is especially useful in the diolefin selective hydrogenation of medium or low distillate oil, in particular, in the diolefin selective hydrogenation of full distillate pyrolysis gasoline.
- the present invention also provides a method for preparing such catalyst, comprising:
- the present invention preferably recommends that the modified alumina carrier is prepared by:
- the catalyst according to the present invention comprises 2-8% silica, which may increase the stability of the catalyst, especially the carrier during calcination.
- the content of silica is 3-4%.
- the content of nickel oxide is 15-19%.
- the catalyst according to the present invention comprises alkaline earth metal, which may adjust the acidity of the catalyst after calcination and improve the colloid resistance during hydrogenation reaction.
- the alkaline earth metal is magnesium and/or strontium.
- the content of alkaline earth metal oxide is preferably 2-5%.
- the lanthanum and/or cerium are added in the form of nitrate dissolved in the impregnating solution so as to improve the hydrogenation activity and stability of the catalyst.
- the content of lanthanum oxide and/or cerium oxide is 3-5%.
- the VIB group element is added to improve the hydrogenation activity and impurity (for example, sulfur) resistance of the catalyst.
- the VIB group element is one or more of Cr, Mo and W.
- the content of VIB group element oxide is preferably 3-6%.
- the solution of the active component and aids are impregnated onto the resultant catalyst carrier in twice to increase the dispersity of the active component of the catalyst and improve the activity and stability of catalyst.
- the compounds of nickel (as active component), magnesium, strontium lanthanum and cerium (as aids) in above-mentioned preparation process may be in the form of sulfate, nitrate and halide and so on. Preferably, they are in the form of nitrate, since nitrate is easily soluble in water to be fully dissolved and form stable solution.
- the alumina hydrate as the starting material for preparing the catalyst according to the present invention, may be alumina hydrates prepared by carbon dioxide method, ammonia method, and nitric acid method and so on.
- the alumina hydrate prepared by nitric acid method is preferable due to its better hydrogenation performance.
- the catalyst according to the present invention should be reduced under hydrogen at the temperature of 350-400° C. for 5-6 hours prior to use. During the reduction, the volume ratio of hydrogen to catalyst is 150:1 to 500:1.
- Nickel nitrate available from Xi′ an Chemical Reagent Factory
- Magnesium nitrate and strontium nitrate available from Shanghai Colloid Chemical Plant;
- Cerium nitrate and lanthanum nitrate available from Shensheng Reagent Factory, Fufeng, Yixing, Jiangsu;
- Alumina powder available from Lanhua Xiangxin Additives Factory.
- alumina carrier 140 ml water, 5 ml nitric acid (the content of which is 60%) and 16 ml silica sol (comprising 40% silica) are added to 300 g pseudo-boehmite alumina powder. After kneading and extruding, the formed alumina carrier is dried in air at 120° C., and then calcinated at 560° C. for 4 hours. 100 g calcinated carrier is impregnated with a solution form by dissolving 26 g magnesium nitrate into water, dried in air at 120° C., and calcinated at 1050° C. for 4 hours, thereby obtaining the modified Al 2 O 3 carrier.
- 10 g nickel nitrate is added to 20 ml water with stirring. While stirring, 2.1 g cerium nitrate and 0.3 g ammonium molybdate are added. The pH of the solution is adjusted to 4. Then 10 g carrier is impregnated with the solution, aged for 12 hours, dried at 120° C., and calcinated at 400° C. for 4 hours, thereby obtaining the catalyst.
- alumina carrier 140 ml water and 5 ml nitric acid (the content of which is 60%) are added to 300 g pseudo-boehmite alumina powder. After kneading and extruding, the formed alumina carrier is dried in air at 120° C., and then calcinated at 560° C. for 4 hours. 100 g calcinated carrier is impregnated with a solution formed by dissolving 16.7 g magnesium nitrate and 3 g strontium nitrate into water, dried in air at 120° C., and calcinated at 1050° C. for 4 hours, thereby obtaining the Al 2 O 3 carrier.
- 10 g nickel nitrate is added to 20 ml water with stirring. While stirring, 2.1 g cerium nitrate and 0.3 g ammonium molybdate are added. The pH of the solution is adjusted to 4. Then 10 g carrier is impregnated with the solution, aged for 12 hours, dried at 120° C., and calcinated at 400° C. for 4 hours, thereby obtaining the catalyst.
- alumina carrier 140 ml water, 5 ml nitric acid (the content of which is 60%) and 14 ml silica sol (comprising 40% silica) are added to 300 g pseudo-boehmite alumina powder. After kneading and extruding, the formed alumina carrier is dried in air at 120° C., and then calcinated at 460° C. for 4 hours. 100 g calcinated carrier is impregnated with a solution formed by dissolving 20 g magnesium nitrate and 3.5 g strontium nitrate into water, dried in air at 120° C., and calcinated at 1000° C. for 4 hours, thereby obtaining the Al 2 O 3 carrier.
- nickel nitrate 8.6 g nickel nitrate is added to 20 ml water with stirring. While stirring, 1.5 g lanthanum nitrate and 0.6 g ammonium tungstate are added. The pH of the solution is adjusted to 4. Then 10 g carrier is impregnated with the solution, aged for 12 hours, dried at 120° C., and calcinated at 350° C. for 4 hours, thereby obtaining the catalyst.
- alumina carrier 140 ml water, 5 ml nitric acid (the content of which is 60%) and 14 ml silica sol (comprising 40% silica) are added to 300 g pseudo-boehmite alumina powder. After kneading and extruding, the formed alumina carrier is dried in air at 120° C., and calcinated at 1000° C. for 4 hours, thereby obtaining the Al 2 O 3 carrier.
- nickel nitrate 8.6 g nickel nitrate is added to 20 ml water with stirring. While stirring, 1.5 g lanthanum nitrate and 0.6 g ammonium tungstate are added. The pH of the solution is adjusted to 4. Then 10 g carrier is impregnated with the solution, aged for 12 hours, dried at 120° C., and calcinated at 350° C. for 4 hours, thereby obtaining the catalyst.
- alumina carrier 140 ml water, 5 ml nitric acid (the content of which is 60%) and 9 ml silica sol (comprising 40% silica) are added to 300 g pseudo-boehmite alumina powder. After kneading and extruding, the formed alumina carrier is dried in air at 120° C., and then calcinated at 460° C. for 4 hours. 100 g calcinated carrier is impregnated with a solution formed by dissolving 15.5 g magnesium nitrate into water, dried in air at 120° C., and calcinated at 1030° C. for 4 hours, thereby obtaining the Al 2 O 3 carrier.
- nickel nitrate is added to 20 ml water with stirring. While stirring, 0.63 g cerium nitrate, 0.62 g lanthanum nitrate and 0.5 g ammonium tungstate are added. The pH of the solution is adjusted to 4. Then 10 g carrier is impregnated with the solution, aged for 12 hours, dried at 120° C., and calcinated at 400° C. for 4 hours, thereby obtaining the catalyst.
- the formed alumina carrier is dried in air at 120° C., and calcinated at 1030° C. for 4 hours, thereby obtaining the Al 2 O 3 carrier.
- nickel nitrate 7.9 g nickel nitrate is added to 20 ml water with stirring. While stirring, 0.6 g ammonium molybdate is added. The pH of the solution is adjusted to 4. Then 10 g carrier is impregnated with the solution, aged for 12 hours, dried at 120° C., and calcinated at 400° C. for 4 hours, thereby obtaining the catalyst.
- alumina carrier 140 ml water, 5 ml nitric acid (the content of which is 60%) and 12 ml silica sol (comprising 40% silica) are added to 300 g pseudo-boehmite alumina powder. After kneading and extruding, the formed alumina carrier is dried in air at 120° C., and then calcinated at 460° C. for 4 hours. 100 g calcinated carrier is impregnated with a solution formed by dissolving 5.8 g strontium nitrate into water, dried in air at 120° C., and calcinated at 1020° C. for 4 hours, thereby obtaining the Al 2 O 3 carrier.
- nickel nitrate is added to 20 ml water with stirring. While stirring, 1.1 g cerium nitrate, 1.1 g lanthanum nitrate and 0.6 g potassium chromate are added. The pH of the solution is adjusted to 4. Then 10 g carrier is impregnated with the solution, aged for 12 hours, dried at 120° C., and calcinated at 350° C. for 4 hours, thereby obtaining the catalyst.
- alumina carrier 140 ml water, 5 ml nitric acid (the content of which is 60%) and 12 ml silica sol (comprising 40% silica) are added to 300 g pseudo-boehmite alumina powder. After kneading and extruding, the formed alumina carrier is dried in air at 120° C., and then calcinated at 460° C. for 4 hours. 100 g calcinated carrier is impregnated with a solution formed by dissolving 21.6 g magnesium nitrate into wate, dried in air at 120° C., and calcinated at 1020° C. for 4 hours, thereby obtaining the Al 2 O 3 carrier.
- nickel nitrate is added to 20 ml water with stirring. While stirring, 1.1 g cerium nitrate is added. The pH of the solution is adjusted to 4. Then 10 g carrier is impregnated with the solution, aged for 12 hours, dried at 120° C., and calcinated at 350° C. for 4 hours, thereby obtaining the catalyst.
- Iodine value measured according to IC1 method, expressed in g I 2 /100 g oil;
- Diolefin measured according to maleic anhydride method, expressed in g I 2 /100 g oil;
- Arsenic content measured by DV-4300 atomic emission spectroscopy
- Sulfur content measured by WK-2B microcoulometric detector
- Colloid measured according to Petroleum Product Testing Method SYB-2103-60.
- the full distillate pyrolysis gasoline is used as the starting materials, the properties of which are shown in Table 1.
- the catalysts of Examples 1, 2, 3 and 4 as well as Comparative Examples 1, 2, 3 and 4 are evaluated on 100 ml adiabatic bed hydrogenation apparatus. Firstly, the catalyst is reduced under hydrogen at the temperature of 350-400° C. for 10 hours. The temperature is lowered to 60° C. After the catalyst is inactivated by cyclohexane containing 1000 ppm dimethyl disulfide for 2 hours, the raw oil is added.
- Intake temperature room temperature ⁇ 60° C.
- Air speed of fresh raw oil 3.5h ⁇ 1 ,
- the volume ratio of hydrogen to oil 200:1 (based on the fresh oil).
- the evaluation is carried out for 200 hours. And the iodine value and diolefin of the products are analyzed every 6 hours. The average data of the iodine value and diolefin of the product for each catalyst during the 200-hour evaluation are shown in Table 2.
- Example 2 1000-hour long period evaluation is performed on the catalyst of Example 2. The evaluation was carried out on 100 ml adiabatic bed hydrogenation apparatus. Firstly, the catalyst is reduced under hydrogen at the temperature of 400-450° C. for 10 hours. The temperature is lowered to 60° C. After the catalyst is inactivated by cyclohexane containing 1000 ppm dimethyl disulfide for 3 hours, the raw oil is added.
- Intake temperature room temperature ⁇ 70° C.
- Air speed of fresh raw oil 2.8h ⁇ 1 ,
- the volume ratio of hydrogen to oil 200:1 (based on the fresh oil).
- the iodine value and diolefin of the product are analyzed every 12 hours. The average data during every 200 hours are taken.
- the indexes of hydrogenation raw oil (C 5 -C 9 ) are shown in Table 3.
- the hydrogenation catalyst according to the present invention has good hydrogenation performance, especially has impurity and colloid resistance as well as good hydrogenation stability.
- the catalyst can be applied to selective hydrogenation of diolefin unsaturated hydrocarbons, especially the first-stage selective hydrogenation process of full distillate pyrolysis gasoline.
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CN200710176670.9 | 2007-11-01 | ||
PCT/CN2008/001781 WO2009062386A1 (en) | 2007-11-01 | 2008-10-22 | A selective nickle based htdrogenation catalyst and the preparation thereof |
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CN102139218A (zh) * | 2011-03-22 | 2011-08-03 | 中国华能集团清洁能源技术研究院有限公司 | 一种煤制合成气完全甲烷化的催化剂及其制备方法 |
CN102139218B (zh) * | 2011-03-22 | 2012-09-26 | 中国华能集团清洁能源技术研究院有限公司 | 一种煤制合成气完全甲烷化的催化剂及其制备方法 |
CN102259004A (zh) * | 2011-07-06 | 2011-11-30 | 中国华能集团清洁能源技术研究院有限公司 | 用于煤制天然气甲烷化反应器的催化剂及其制备方法 |
CN102259005A (zh) * | 2011-07-06 | 2011-11-30 | 中国华能集团清洁能源技术研究院有限公司 | 用于煤制天然气辅助甲烷化反应器的催化剂及其制备方法 |
US9518229B2 (en) | 2012-07-20 | 2016-12-13 | Inaeris Technologies, Llc | Catalysts for thermo-catalytic conversion of biomass, and methods of making and using |
US9522392B2 (en) | 2013-03-15 | 2016-12-20 | Inaeris Technologies, Llc | Phosphorous promotion of zeolite-containing catalysts |
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CN114289028A (zh) * | 2021-12-01 | 2022-04-08 | 中国海洋石油集团有限公司 | 一种顺酐液相连续加氢制备丁二酸酐的非贵金属催化剂及其制备方法 |
Also Published As
Publication number | Publication date |
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JP5357170B2 (ja) | 2013-12-04 |
GB2467086B8 (en) | 2012-02-15 |
GB201008986D0 (en) | 2010-07-14 |
CN101423775B (zh) | 2010-05-12 |
WO2009062386A1 (en) | 2009-05-22 |
CN101423775A (zh) | 2009-05-06 |
JP2011502050A (ja) | 2011-01-20 |
MY150048A (en) | 2013-11-29 |
US9597668B2 (en) | 2017-03-21 |
GB2467086A (en) | 2010-07-21 |
US20140349844A1 (en) | 2014-11-27 |
KR101469303B1 (ko) | 2014-12-04 |
KR20100075498A (ko) | 2010-07-02 |
GB2467086B (en) | 2012-02-08 |
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