JP5403843B2 - 複合金属酸化物触媒の製造方法、不飽和アルデヒド及び/又はカルボン酸の製造方法及びベルト式か焼装置 - Google Patents
複合金属酸化物触媒の製造方法、不飽和アルデヒド及び/又はカルボン酸の製造方法及びベルト式か焼装置 Download PDFInfo
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- JP5403843B2 JP5403843B2 JP2002528635A JP2002528635A JP5403843B2 JP 5403843 B2 JP5403843 B2 JP 5403843B2 JP 2002528635 A JP2002528635 A JP 2002528635A JP 2002528635 A JP2002528635 A JP 2002528635A JP 5403843 B2 JP5403843 B2 JP 5403843B2
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- catalyst
- calcination
- temperature
- metal oxide
- composite metal
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- 239000003054 catalyst Substances 0.000 title claims description 98
- 238000001354 calcination Methods 0.000 title claims description 73
- 229910044991 metal oxide Inorganic materials 0.000 title claims description 33
- 150000004706 metal oxides Chemical class 0.000 title claims description 33
- 239000002131 composite material Substances 0.000 title claims description 30
- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 150000001732 carboxylic acid derivatives Chemical class 0.000 title claims description 4
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 title 1
- 239000000463 material Substances 0.000 claims description 46
- 239000007789 gas Substances 0.000 claims description 40
- 239000012018 catalyst precursor Substances 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 33
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 30
- QQONPFPTGQHPMA-UHFFFAOYSA-N Propene Chemical compound CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 23
- 239000001301 oxygen Substances 0.000 claims description 23
- 229910052760 oxygen Inorganic materials 0.000 claims description 23
- 230000000694 effects Effects 0.000 claims description 20
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 150000001299 aldehydes Chemical class 0.000 claims description 13
- -1 alkanols Chemical class 0.000 claims description 13
- 239000010941 cobalt Substances 0.000 claims description 13
- 229910017052 cobalt Inorganic materials 0.000 claims description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 11
- 150000001336 alkenes Chemical class 0.000 claims description 10
- 229910052797 bismuth Inorganic materials 0.000 claims description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 9
- 150000001735 carboxylic acids Chemical class 0.000 claims description 9
- 230000002123 temporal effect Effects 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
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- 239000011733 molybdenum Substances 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052718 tin Inorganic materials 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
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- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 4
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910001882 dioxygen Inorganic materials 0.000 claims description 3
- 239000011135 tin Substances 0.000 claims description 3
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- 229910052725 zinc Inorganic materials 0.000 claims description 3
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- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052776 Thorium Inorganic materials 0.000 claims description 2
- 229910052770 Uranium Inorganic materials 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
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- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 239000010955 niobium Substances 0.000 claims description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 2
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- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 229910052702 rhenium Inorganic materials 0.000 claims description 2
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
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- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 claims description 2
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 239000012071 phase Substances 0.000 description 31
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 10
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 9
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- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 3
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- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 3
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- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 description 1
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- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
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- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 150000004675 formic acid derivatives Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 150000004715 keto acids Chemical class 0.000 description 1
- 239000000314 lubricant Substances 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
- 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
- 238000005259 measurement Methods 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 239000005078 molybdenum compound Substances 0.000 description 1
- 150000002752 molybdenum compounds Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000005839 oxidative dehydrogenation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 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
- 239000004033 plastic Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000005029 sieve analysis Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Images
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Description
[X1 aX2 bOx]p[X3 cX4 dX5 eX6 fX7 gX2 hOy]q (I)
Mo12BiiX8 kFelX9 mX10 nOz (II)
を有し、前記式中
X1は、ビスマス、テルル、アンチモン、スズ及び/又は銅;有利にビスマスを表し、
X2は、モリブデン及び/又はタングステンを表し、
X3は、アルカリ金属、タリウム及び/又はサマリウム;有利にカリウムを表し、
X4は、アルカリ土類金属、ニッケル、コバルト、銅、マンガン、亜鉛、スズ、カドミウム及び/又は水銀;有利にニッケル及び/又はコバルトを表し、
X5は、鉄、クロム、セリウム及び/又はバナジウム;有利に鉄を表し、
X6は、リン、ヒ素、ホウ素及び/又はアンチモンを表し、
X7は、希土類金属、チタン、ジルコニウム、ニオブ、タンタル、レニウム、ルテニウム、ロジウム、銀、金、アルミニウム、ガリウム、インジウム、ケイ素、ゲルマニウム、鉛、トリウム及び/又はウラン;有利にケイ素、アルミニウム、チタン及び/又はジルコニウムを表し、
aは、0.01〜8であり、
bは、0.1〜30であり、
cは、0〜4であり、
dは、0〜20であり、
eは、0〜20であり、
fは、0〜6であり、
gは、0〜15であり、
hは、8〜16であり、
x、yは、式I中の酸素以外の元素の原子価及び頻度により決定される数であり、
p、qは、p/qの割合が0.1〜10となるような数であり、
X8は、コバルト及び/又はニッケル;有利にコバルトを表し、
X9は、ケイ素及び/又はアルミニウム;有利にケイ素を表し、
X10は、アルカリ金属、例えばカリウム、ナトリウム、セシウム及び/又はルビジウム;特にカリウムを表し、
iは、0.1〜2であり、
kは、2〜10であり、
lは、0.5〜10であり、
mは、0〜10であり、
nは、0〜0.5であり、
zは、式II中の酸素以外の元素の原子価及び頻度により決定される数である。
1:100〜200℃; 2:150〜250℃; 3:200〜300℃; 4:250〜350℃; 5:350〜400℃; 6:400〜550℃; 7:400〜550℃; 8:400〜550℃。
1:100〜400℃; 2:250〜550℃; 3:400〜550℃。
1:100〜250℃; 2:200〜350℃; 3:350〜550℃; 4: 400〜550℃。
1:100〜200℃; 2:150〜300℃; 3:200〜350℃; 4:300〜400℃; 5:400〜500℃; 6:400〜600℃。
1:100〜200℃; 2:150〜250℃; 3:200〜300℃; 4:250〜350℃; 5:350〜400℃; 6:400〜500℃; 7:400〜550℃; 8:400〜550℃; 9:400〜600℃; 10:400〜600℃; 11:400〜700℃; 12:400〜700℃。
15mmの内径及び20mmの外径を有する鋼管中に、まず直径2〜3mmのステアタイト球からなる15cmの長さの充填物を充填した。引き続き、試験すべき触媒100gを充填し、この場合に60〜70cmの平均充填高さであった。この鋼管を窒素で十分に洗浄した塩浴を用いて触媒及びステアタイト球を有する充填物の全体の高さにわたり熱処理した。プロペン5体積%、酸素9.5体積%及び窒素85.5体積%の組成の100Nl/h(標準状態での体積)の一定の供給ガス量で、鋼管の出口で測定したプロペン転化率が95%になるように塩浴の温度を変えた。このプロペン転化率は次のように定義される:
SWP[%] = SACS + SACR
例1
まず主相の出発材料を製造した。このために、60℃でヘプタモリブデン酸アンモニウム244kgを少しずつ水660l中に溶かし、撹拌しながら20℃の47.5質量%の水酸化カリウム溶液1.12kgを添加して、第1の溶液を得た。硝酸コバルト溶液288.7kg(コバルト12.5質量%)に硝酸鉄溶液133.8kg(鉄13.8質量%)を添加し、その際に温度を60℃に保持することにより第2の溶液を製造した。この第2の溶液を30分内で60℃でモリブデン酸溶液に添加した。添加の終了から15分後に、シリカゾル19.16kg(密度1.36〜1.42g/ml、pH8.5〜9.5、アルカリ含有量最大0.5質量%;SiO2 46.80質量%)を仕込み原料中に添加した。その後15分間撹拌した。得られた仕込み原料を引き続き噴霧乾燥し、その際に、約30質量%の強熱減量(600℃で3h)を有する粉末が得られた。
例1からの触媒前駆体を、500gの量で常用の実験室マッフル炉(この場合、時間的及び局所的温度変動は約±3℃)中で、多様な設定温度で6hにわたりか焼した。か焼温度に依存する触媒特性を、第2表に記載した。
例1からの触媒前駆体300kgを、1車両の相互に9段重ねて配置された棚上に分配した。この車両を炉内へ搬入し、空気流中で加熱した。185℃で1時間内で加熱し、このこの値の温度を1時間保持し、次いで2℃/minの速度で210℃に加熱し、この値の温度で2時間保持し、2℃/minの速度で250℃に加熱し、この値の温度で1時間保持し、5℃/minの速度で465℃に加熱し、この値の温度で6時間保持した。記載した温度は、炉に設定された設定温度である。車両の個々の棚上では、この温度から変動する異なる温度となる。この各部分から、個々の棚の全ての平均試料を取り出し、引き続き試験した。
まず主相の出発材料を製造した。このために、60℃でヘプタモリブデン酸アンモニウム213kgを少しずつ水600l中に溶かし、撹拌しながら20℃の46.8質量%の水酸化カリウム溶液0.97kgを添加した。硝酸コバルト溶液262.9kg(コバルト12.4質量%)に硝酸鉄溶液80.2kg(鉄14.2質量%)を添加し、その際に温度を60℃に保持することにより第2の溶液を製造した。この第2の溶液を30分内で60℃でモリブデン酸溶液に添加した。添加の終了から15分後に、シリカゾル19.16kg(密度1.36〜1.42g/ml、pH8.5〜9.5、アルカリ含有量最大0.5質量%;SiO2 46.80質量%)を仕込み原料中に添加した。その後15分間撹拌した。得られた仕込み原料を引き続き噴霧乾燥し、その際に、約30質量%の強熱減量(600℃で3h)を有する粉末が得られた。
例2からの触媒前駆体を、500gの量で常用の実験室マッフル炉(この場合、時間的及び局所的温度変動は約±3℃)中で、多様な設定温度で6hにわたりか焼した。か焼温度に依存する触媒特性を、第5表に示した。
60℃でヘプタモリブデン酸アンモニウム213kgを少しずつ水600lに溶かし、撹拌しながら20℃の46.8質量%の水酸化カリウム溶液0.97kgを添加した。硝酸コバルト溶液333.7kg(コバルト12.4質量%)に硝酸鉄溶液116.25kg(鉄14.2質量%)を添加し、その際に温度を30℃に保持し、添加の終了後になお30分間撹拌することにより第2の溶液を製造した。60℃で硝酸ビスマス溶液112.3kg(ビスマス11.2%)をこの鉄−コバルト溶液に混入した。この第2の溶液を30分の時間内で60℃でモリブデン酸溶液に添加した。添加の終了から15分後に、シリカゾル19.16kg(SiO2 46.80質量%)を得られた仕込み原料中に添加した。その後15分間撹拌した。得られた仕込み原料を引き続き噴霧乾燥し、その際に、約30質量%の強熱減量(600℃で3h)を有する粉末が得られた。
例3からの触媒前駆体を、500gの量で常用の実験室マッフル炉(この場合、時間的及び局所的温度変動は約±3℃)中で、多様な設定温度で6hにわたりか焼した。か焼温度に依存する触媒特性を、第7表に示した。
例1を繰り返すが、この場合に12の区域を有するベルト式か焼装置を使用した。最初の8つの区域の温度及び滞留時間は例1に記載したと同様であった。区域9〜12は統一的に500℃にサーモスタット制御し、滞留時間はそれぞれ2hであった。室9〜12中の雰囲気はほとんど酸素からなっていた。このようにして触媒3.5tを製造した。100kgの充填重量を有する容器からそれぞれ1kgの量の試料を取り出し、前記したと同様に特性決定した。得られた結果は第8表に記載した。
混合機中で、相互に続けてMoO3 191.5kg、CoO 45.6kg、Fe2O3 27.2kg、SiO2 10.4kg、K2O 0.4kgを均質に混合し;引き続き例1で製造した助触媒相を、化学量論[Bi2W2O9×2WO3]0.5[Mo12Co5.5Fe3.0Si1.6K0.08Oy]の材料が得られるような割合で添加し、これを外径5mm、高さ2mm及び孔径2mmの円筒状のリングに成形した。この成形したリングを、3つの室を有するベルト式か焼装置中でか焼し、これらの室はそれぞれ270℃、465℃、465℃にサーモスタット制御された。室毎の滞留時間は3hであった。このように触媒2.5tを製造した。100kgの充填容量の各容器から、それぞれ1kgの量の試料を取り出し、前記したように特性決定した。得られた結果を第9表に記載した。
例3を繰り返すが、この場合に化学組成Mo12Co7Fe3Bi1.0Si1.6K0.08Ozが得られるように成分の量を選択した。か焼は8の区域を有するベルト式か焼装置中で行い、これらの区域はそれぞれ160℃、210℃、240℃、290℃、380℃、515℃、515℃、400℃にサーモスタット制御した。100kgの充填容量の各容器から、それぞれ1kgの量の試料を取り出し、前記したように特性決定した。得られた結果を第10表に記載した。
混合機中で、相互に続けてMoO3 114.4kg、CoO 34.5kg、Fe2O3 15.8kg、SiO2 6.3kg、Bi2O3 9.2kg及びK2O 0.2kgを均質に混合した。この混合物を外径5mm、高さ3mm及び孔径2mmの円筒状のリングに成形した。この成形したリングを、3つの室を有するベルト式か焼装置中でか焼し、これらの室はそれぞれ350℃、510℃、510℃にサーモスタット制御された。室毎の滞留時間は2.5hであった。このように触媒2.5tを製造した。100kgの充填容量の各容器から、それぞれ1kgの量の試料を取り出し、前記したように特性決定した。得られた結果を第11表に記載した。
Claims (13)
- 酸素以外の複合金属酸化物材料を構成する元素の酸化物及び/又は酸化物に移行可能な化合物を含有する粒子状の触媒前駆体を製造し、この触媒前駆体をか焼により触媒活性形に移行させる、有機化合物をα,β−不飽和アルデヒド及び/又はカルボン酸に気相酸化するために適した、複合金属酸化物材料からなる活性相を有する触媒の製造方法において、か焼のために粒子状の触媒前駆体の供給流をほぼ一定の速度で少なくとも1つのか焼区域を通過するように案内し、かつか焼区域内で触媒前駆体の進行方向に対して垂直に、触媒前駆体の供給流を通過するようにガス流を導通させ、その際、か焼区域内での温度の時間的な最大変動及び局所的な最大温度差はそれぞれ≦5℃であることを特徴とする、複合金属酸化物触媒の製造方法。
- 複合金属酸化物材料が、モリブデン及びタングステンから選択される少なくとも1種の第1の金属と、ビスマス、テルル、アンチモン、スズ、銅、鉄、コバルト及び/又はニッケルから選択される少なくとも1種の第2の金属とを含有する、請求項1記載の方法。
- 複合金属酸化物材料が式I又はII:
[X1 aX2 bOx]p[X3 cX4 dX5 eX6 fX7 gX2 hOy]q (I)
Mo12BiiX8 kFelX9 mX10 nOz (II)
を有し、前記式中
X1は、ビスマス、テルル、アンチモン、スズ及び/又は銅を表し、
X2は、モリブデン及び/又はタングステンを表し、
X3は、アルカリ金属、タリウム及び/又はサマリウムを表し、
X4は、アルカリ土類金属、ニッケル、コバルト、銅、マンガン、亜鉛、スズ、カドミウム及び/又は水銀を表し、
X5は、鉄、クロム、セリウム及び/又はバナジウムを表し、
X6は、リン、ヒ素、ホウ素及び/又はアンチモンを表し、
X7は、希土類金属、チタン、ジルコニウム、ニオブ、タンタル、レニウム、ルテニウム、ロジウム、銀、金、アルミニウム、ガリウム、インジウム、ケイ素、ゲルマニウム、鉛、トリウム及び/又はウランを表し、
aは、0.01〜8であり、
bは、0.1〜30であり、
cは、0〜4であり、
dは、0〜20であり、
eは、0〜20であり、
fは、0〜6であり、
gは、0〜15であり、
hは、8〜16であり、
x、yは、式I中の酸素以外の元素の原子価及び頻度により決定される数であり、
p、qは、p/qの割合が0.1〜10となるような数であり、
X8は、コバルト及び/又はニッケルを表し、
X9は、ケイ素及び/又はアルミニウムを表し、
X10は、アルカリ金属を表し、
iは、0.1〜2であり、
kは、2〜10であり、
lは、0.5〜10であり、
mは、0〜10であり、
nは、0〜0.5であり、
zは、式II中の酸素以外の元素の原子価及び頻度により決定される数である、
請求項2記載の方法。
- 触媒前駆体を少なくとも2つのか焼区域を通過するように案内し、前記の少なくとも2つのか焼区域は異なる温度にサーモスタット制御されている、請求項1から3までのいずれか1項記載の方法。
- か焼区域内の温度の時間的な最大変動が≦3℃である、請求項1から4までのいずれか1項記載の方法。
- か焼区域内の温度の時間的な最大変動が≦2℃である、請求項5記載の方法。
- か焼区域内の局所的な最大温度差が≦3℃である、請求項1から6までのいずれか1項記載の方法。
- か焼区域内の局所的な最大温度差が≦2℃である、請求項7記載の方法。
- 活性相として式I又はII:
[X 1 a W b O x ] p [X 3 c X 4 d X 5 e X 7 g Mo h O y ] q (I)
Mo 12 Bi i X 8 k Fe l X 9 m X 10 n O z (II)
[前記式中
X 1 は、ビスマスを表し、
X 3 は、カリウムを表し、
X 4 は、コバルトを表し、
X 5 は、鉄を表し、
X 7 は、ケイ素を表し、
aは、0.01〜8であり、
bは、0.1〜30であり、
cは、0〜4であり、
dは、0〜20であり、
eは、0〜20であり、
gは、0〜15であり、
hは、8〜16であり、
x、yは、式I中の酸素以外の元素の原子価及び頻度により決定される数であり、
p、qは、p/qの割合が0.1〜10となるような数であり、
X 8 は、コバルトを表し、
X 9 は、ケイ素を表し、
X 10 は、カリウムを表し、
iは、0.1〜2であり、
kは、2〜10であり、
lは、0.5〜10であり、
mは、0〜10であり、
nは、0〜0.5であり、
zは、式II中の酸素以外の元素の原子価及び頻度により決定される数である]の複合金属酸化物材料を有する少なくとも1tの触媒バッチにおいて、その際、任意に採取されるバッチの抜き取り試料の活性度の標準偏差は、95%のプロペン転化率が得られる温度として表して、プロペン5体積%、酸素9.5体積%及び窒素85.5体積%からなる混合物が触媒100gを通過して100Nl/hで導入される場合に、7℃より低く、その際、抜き取り試料の数は、100kg当たり少なくとも1つの抜き取り試料である、触媒バッチ。 - 3〜6個の炭素原子を有するアルカン、アルカノール、アルケン及び/又はアルケナールのガス状の供給流を高めた温度で分子酸素の存在で、請求項9記載の少なくとも1つの触媒バッチを有する少なくとも1つの反応区域を通過させる、α,β−モノエチレン性不飽和アルデヒド及び/又はカルボン酸の製造方法。
- アルカン、アルカノール、アルケン及び/又はアルケナールによる触媒の負荷は、毎時で少なくとも160Nl/触媒lである、請求項10記載の方法。
- アルケンはプロペンでありかつアクロレインが得られる、請求項10又は11記載の方法。
- ガス状の供給流を第1の反応区域及び第2の反応区域に続けて導通し、その際に、第1の反応区域の温度は300〜330℃であり、第2の反応区域の温度は300〜365℃でありかつ第1の反応区域の温度を少なくとも5℃上回り、第1の反応区域は40〜80モル%のアルカン、アルカノール、アルケン及び/又はアルケナールの転化率まで延在している、請求項10から12までのいずれか1項記載の方法。
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-
2000
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2001
- 2001-09-20 US US10/363,856 patent/US6881702B2/en not_active Expired - Lifetime
- 2001-09-20 EP EP07021039.8A patent/EP1889657B1/de not_active Expired - Lifetime
- 2001-09-20 CN CNB2005101141898A patent/CN100551528C/zh not_active Expired - Lifetime
- 2001-09-20 EP EP01969749A patent/EP1322585B1/de not_active Expired - Lifetime
- 2001-09-20 DE DE50113515T patent/DE50113515D1/de not_active Expired - Lifetime
- 2001-09-20 CN CNB018160662A patent/CN1231293C/zh not_active Expired - Lifetime
- 2001-09-20 WO PCT/EP2001/010911 patent/WO2002024620A2/de active IP Right Grant
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WO2002024620A2 (de) | 2002-03-28 |
CN1768933A (zh) | 2006-05-10 |
DE10046957A1 (de) | 2002-04-11 |
EP1889657A2 (de) | 2008-02-20 |
CN100551528C (zh) | 2009-10-21 |
EP1889657B1 (de) | 2019-11-06 |
US20090171117A1 (en) | 2009-07-02 |
US6881702B2 (en) | 2005-04-19 |
EP1889657A3 (de) | 2012-08-29 |
CN1462210A (zh) | 2003-12-17 |
DE50113515D1 (de) | 2008-03-06 |
EP1322585A2 (de) | 2003-07-02 |
WO2002024620A3 (de) | 2002-12-12 |
US20040034249A1 (en) | 2004-02-19 |
JP2004508931A (ja) | 2004-03-25 |
CN1231293C (zh) | 2005-12-14 |
EP1322585B1 (de) | 2008-01-16 |
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