JP2020507451A - ニオブおよびテルルの低下した含有量ならびにエタンの酸化的脱水素化に対するより高い活性を有するMoVNbTe触媒の合成 - Google Patents
ニオブおよびテルルの低下した含有量ならびにエタンの酸化的脱水素化に対するより高い活性を有するMoVNbTe触媒の合成 Download PDFInfo
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- JP2020507451A JP2020507451A JP2019540546A JP2019540546A JP2020507451A JP 2020507451 A JP2020507451 A JP 2020507451A JP 2019540546 A JP2019540546 A JP 2019540546A JP 2019540546 A JP2019540546 A JP 2019540546A JP 2020507451 A JP2020507451 A JP 2020507451A
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- Prior art keywords
- tellurium
- mixture
- mixed oxide
- oxide material
- starting compounds
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- 239000010955 niobium Substances 0.000 title claims abstract description 55
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 38
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 26
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 22
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 title claims description 16
- 238000005839 oxidative dehydrogenation reaction Methods 0.000 title claims description 14
- 239000003054 catalyst Substances 0.000 title description 71
- 238000003786 synthesis reaction Methods 0.000 title description 13
- 230000015572 biosynthetic process Effects 0.000 title description 12
- 230000000694 effects Effects 0.000 title description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 25
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011733 molybdenum Substances 0.000 claims abstract description 21
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 230000005855 radiation Effects 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 31
- 239000007858 starting material Substances 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 29
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000007254 oxidation reaction Methods 0.000 claims description 19
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 230000003647 oxidation Effects 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000003446 ligand Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 9
- 235000006408 oxalic acid Nutrition 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 239000001294 propane Substances 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 4
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 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
- 239000007900 aqueous suspension Substances 0.000 claims description 2
- 150000002009 diols Chemical class 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims 1
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 16
- 239000000047 product Substances 0.000 description 20
- 238000002441 X-ray diffraction Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 229910052706 scandium Inorganic materials 0.000 description 11
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 11
- 238000012937 correction Methods 0.000 description 10
- 239000011148 porous material Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 8
- 229930195733 hydrocarbon Natural products 0.000 description 8
- 150000002430 hydrocarbons Chemical class 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000012154 double-distilled water Substances 0.000 description 7
- 238000001027 hydrothermal synthesis Methods 0.000 description 7
- 230000001590 oxidative effect Effects 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000005977 Ethylene Substances 0.000 description 5
- 238000001354 calcination Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- FXADMRZICBQPQY-UHFFFAOYSA-N orthotelluric acid Chemical compound O[Te](O)(O)(O)(O)O FXADMRZICBQPQY-UHFFFAOYSA-N 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 229910003455 mixed metal oxide Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 238000004438 BET method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- XFHGGMBZPXFEOU-UHFFFAOYSA-I azanium;niobium(5+);oxalate Chemical compound [NH4+].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XFHGGMBZPXFEOU-UHFFFAOYSA-I 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 150000002825 nitriles Chemical class 0.000 description 3
- -1 oxyacids Chemical class 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 239000012494 Quartz wool Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 229910000484 niobium oxide Inorganic materials 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 238000005063 solubilization Methods 0.000 description 2
- 230000007928 solubilization Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 241001061225 Arcos Species 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910017488 Cu K Inorganic materials 0.000 description 1
- 229910017541 Cu-K Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Natural products OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 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 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000012438 extruded product Nutrition 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- DKCWBFMZNUOFEM-UHFFFAOYSA-L oxovanadium(2+);sulfate;hydrate Chemical compound O.[V+2]=O.[O-]S([O-])(=O)=O DKCWBFMZNUOFEM-UHFFFAOYSA-L 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 1
- 238000001350 scanning transmission electron microscopy Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000000153 supplemental effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 150000003498 tellurium compounds Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 description 1
- 229940041260 vanadyl sulfate Drugs 0.000 description 1
- 229910000352 vanadyl sulfate Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- 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
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
Description
M1:Mo1V0.15Te0.12Nb0.128O3.7またはMo7.8V1.2Te0.937Nb1O28.9
M2:*Mo1V0.32Te0.42Nb0.08O4.6またはMo4.31V1.36Te1.81Nb0.33O19.81
で記載できる。
a)モリブデン、バナジウム、ニオブ、およびテルルが酸化状態+4で存在する含テルル出発化合物、ならびにシュウ酸および少なくとも1つのさらに別のオキソ配位子を含有する、出発化合物の混合物を製造するステップ、
b)100〜300℃の温度において、出発化合物の混合物を水熱処理して、生成物懸濁液を得るステップ、
c)ステップb)から生じた懸濁液中に含有される混合酸化物材料を分離して乾燥するステップ、
を含むモリブデン、バナジウム、テルルおよびニオブを含有する混合酸化物材料の製造方法によって解決される。
Mo1VaNbbTecOn (I)
(式中、
a=0.2〜0.35、
b=0超0.08まで、好ましくは0.01超0.08まで
c=0超0.08まで、好ましくは0.01超0.08まで
n=(I)中の酸素ではない元素の原子価および存在量によって定まる数)
を有することを特徴とする、混合酸化物材料によって解決される。
本発明による触媒のパラメータを決定するために、以下の方法を使用する:
DIN 66131に準拠するBET法により決定する。BET法に関する出版物は、J. Am. Chem. Soc. 60、309(1938)にも見出される。測定は、Sorptomatic 1990装置を用いて、77Kにおいて行った。測定前に、試料を2h、523Kにおいて真空化した。BET法による、等温線の線形回帰は、p/p0=0.01〜0.3(p0=730トル)の圧力範囲で行った。
使用した装置:
電子レンジMultiwave GO
反応容器PTFE
プラスチックチューブ50ml
ICP Spectro Arcos
分析用40%HF
分析用37%HCl
分析用98%硫酸
硫酸1:1
ステップ1 100℃へと10分、1分間維持
ステップ2 180℃へと5分、20分間維持。
プラズマ性能:1400ワット
冷却ガス流量:14l/分
補助ガス流量:1.4l/分
噴霧ガス流量:0.8l/分
標準液はすべて、酸を加えて調整し、スカンジウムの質量濃度は2mg/lである。
標準液:
Mo 300/400/500 mg/l
Nb 100/50/20 mg/l
Te 150/100/50 mg/l
V 100/50/20 mg/l
Mo 287.151nm 補正用スカンジウム(korr. Sc) 424.683nm
202.095nm 補正用スカンジウム 424.683nm
204.664nm 補正用スカンジウム 424.683nm
202.095nm
Nb 269.706nm 補正用スカンジウム 424.683nm
316.240nm 補正用スカンジウム 424.683nm
316.340nm
Te 225.902nm 補正用スカンジウム 335.373nm
170.000nm 補正用スカンジウム 335.373nm
170.000nm
V 292.402nm 補正用スカンジウム 424.683nm
292.402nm
311.071nm 補正用スカンジウム 424.683nm
X線回折図を、粉末X線回折法(XRD)およびシェラー式による評価により作成した。
FEI Titan 80/300 TEM/STEM電子顕微鏡上で、300keVの加速電圧を用いて走査型透過電子顕微鏡検査を行った。球面収差は、照度補正(Illuminationskorrektur)を用いて補正した。すべての高角環状暗視野写真(HAADF)は、17.4mradの収束半角および70〜200mradの環状暗視野検出器半角で撮影した。結晶試料は、ミクロトーム技術を用いて調製した。
二次電子検出器を装備したJEOL JSM−7500F上で、走査型電子顕微鏡検査を記録した。加速電圧は、2.0kVおよび放出電流は10μAだった。作動距離はおよそ8mmだった。
例1:MoV0.3Nb0.05Te0.05
100mLのPTFEビーカーに2回蒸留水75mLを入れて、モノエチレングリコール175.8mgを滴加してから、MoO35397.5mg、V2O51023.3mg、TeO2299.2mg、Nb2O5・xH2O(Nb=63.45重量%)274.4mg、クエン酸540.3mgおよびシュウ酸168.5mgを懸濁させた。テフロンビーカーに栓をして、特殊鋼製オートクレーブボンベ(Edelstahlautoklavenbombe)内に移した。このボンベを圧密に閉め、190℃へと予熱した炉の中の水平回転軸上に固定した。48時間後に、オートクレーブボンベを、炉から取り出し、直ちに流水下で急冷し、続いて氷浴で45分間冷却した。
例2:
比較例1:(可溶性前駆体に由来するMoV0.3Nb0.1Te0.1)
比較例2:
例3:
例4:MoV0.30Nb0.03Te0.03
例5:MoV0.30Nb0.06Te0.03
例6:
Claims (16)
- 元素モリブデン、バナジウム、ニオブおよびテルルを含み、XRDにおいて、Cu−Kα線を使用した際、回折反射h、i、kおよびlを有し、それらのピークがおよそ回折角(2θ)26.2°±0.5°(h)、27.0°±0.5°(i)、7.8°±0.5°(k)および28.0°±0.5°(l)に位置する混合酸化物材料であって、以下の化学量論:
Mo1VaNbbTecOn (I)
(式中、
a=0.2〜0.35、
b=0超0.08まで、
c=0超0.08まで、
n=(I)中の酸素ではない元素の原子価および存在量によって定まる数)
を有することを特徴とする、混合酸化物材料。 - 15m2/g超であるBET表面積を有することを特徴とする、請求項1に記載の混合酸化物材料。
- a)モリブデン、バナジウム、ニオブ、およびテルルが酸化状態+4で存在するテルル含有出発化合物、ならびにシュウ酸および少なくとも1つのさらに別のオキソ配位子を含む、出発化合物の混合物を製造するステップ、
b)100℃〜300℃の温度において、出発化合物の混合物を水熱処理して、生成物懸濁液を得るステップ、
c)ステップb)から生じた懸濁液中に含有される混合酸化物材料を分離して乾燥するステップ、
を含む、請求項1または2に記載の混合酸化物材料の製造方法。 - テルル含有出発化合物が、二酸化テルルまたは式Mx n+TeO3(式中、n=1または2およびx=2/nであり、Mは、アルカリ金属またはアルカリ土類金属である)の化合物であることを特徴とする、請求項3に記載の方法。
- 出発化合物の混合物が、水性懸濁液として存在することを特徴とする、請求項3または4に記載の方法。
- 出発化合物の混合物が、さらに別のオキソ配位子としてジカルボン酸、ジオールまたは隣接位に2つのヒドロキシ基を有する別の化合物を含むことを特徴とする、請求項3〜5のいずれか一つに記載の方法。
- 出発化合物の混合物が、三酸化モリブデンを含むことを特徴とする、請求項3〜6のいずれか一つに記載の方法。
- 出発化合物の混合物が、五酸化バナジウムを含むことを特徴とする、請求項3〜7のいずれか一つに記載の方法。
- 出発化合物の混合物が、さらに別のオキソ配位子としてクエン酸を含むことを特徴とする、請求項3〜8のいずれか一つに記載の方法。
- 出発化合物の混合物が、さらに別のオキソ配位子としてクエン酸とグリコールとを含むことを特徴とする、請求項3〜9のいずれか一つに記載の方法。
- ステップc)での乾燥を、50℃〜400℃において行うことを特徴とする、請求項3〜10のいずれか一つに記載の方法。
- ステップc)での乾燥を、2ステップにおいて、まず50℃〜150℃において、次いで350℃〜400℃において行うことを特徴とする、請求項3〜11のいずれか一つに記載の方法。
- 乾燥に、不活性ガス中での500℃〜650℃における活性化がさらに続くことを特徴とする、請求項3〜12のいずれか一つに記載の方法。
- エタンのエテンへの酸化的脱水素化のための、請求項1または2に記載の混合酸化物材料の使用。
- プロパンのアクリル酸への酸化のための、請求項1または2に記載の混合酸化物材料の使用。
- アンモニアを用いたプロパンのアクリルニトリルのアンモ酸化のための、請求項1または2に記載の混合酸化物材料の使用。
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DE102017000861A1 (de) * | 2017-01-31 | 2018-08-02 | Clariant Produkte (Deutschland) Gmbh | Synthese eines MoVTeNb-Katalysators aus preisgünstigen Metalloxiden |
DE102017000862A1 (de) * | 2017-01-31 | 2018-08-02 | Clariant Produkte (Deutschland) Gmbh | Synthese eines MoVNbTe-Katalysators mit reduziertem Gehalt an Niob und Tellur und höherer Aktivität für die oxidative Dehydrierung von Ethan |
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CN110494221B (zh) | 2023-03-28 |
US20200061583A1 (en) | 2020-02-27 |
EP3576873A1 (de) | 2019-12-11 |
KR102316006B1 (ko) | 2021-10-26 |
KR20190112791A (ko) | 2019-10-07 |
DE102017000862A1 (de) | 2018-08-02 |
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