JP2020506800A - 低価格の金属酸化物からのMoVTeNb触媒の合成 - Google Patents
低価格の金属酸化物からのMoVTeNb触媒の合成 Download PDFInfo
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- JP2020506800A JP2020506800A JP2019540662A JP2019540662A JP2020506800A JP 2020506800 A JP2020506800 A JP 2020506800A JP 2019540662 A JP2019540662 A JP 2019540662A JP 2019540662 A JP2019540662 A JP 2019540662A JP 2020506800 A JP2020506800 A JP 2020506800A
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- Prior art keywords
- tellurium
- science
- mixed oxide
- mixture
- niobium
- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims description 31
- 238000003786 synthesis reaction Methods 0.000 title description 11
- 230000015572 biosynthetic process Effects 0.000 title description 10
- 229910044991 metal oxide Inorganic materials 0.000 title description 2
- 150000004706 metal oxides Chemical class 0.000 title description 2
- 239000007858 starting material Substances 0.000 claims abstract description 38
- 239000010955 niobium Substances 0.000 claims abstract description 28
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 27
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 17
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 17
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 16
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011733 molybdenum Substances 0.000 claims abstract description 15
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 13
- 239000003446 ligand Substances 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims abstract 4
- 239000002245 particle Substances 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 15
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- 230000003647 oxidation Effects 0.000 claims description 11
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 11
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 10
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 6
- 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 claims description 6
- 238000005839 oxidative dehydrogenation reaction Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 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
- 239000001294 propane Substances 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
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 239000012153 distilled water Substances 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 9
- 238000009826 distribution Methods 0.000 description 9
- 239000011148 porous material Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000001027 hydrothermal synthesis Methods 0.000 description 7
- FXADMRZICBQPQY-UHFFFAOYSA-N orthotelluric acid Chemical compound O[Te](O)(O)(O)(O)O FXADMRZICBQPQY-UHFFFAOYSA-N 0.000 description 7
- 239000005977 Ethylene Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910000484 niobium oxide Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- 238000004438 BET method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 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
- 238000005516 engineering process Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910003455 mixed metal oxide Inorganic materials 0.000 description 3
- 150000002825 nitriles Chemical class 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Natural products OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- -1 ammonium ions Chemical class 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000012154 double-distilled water Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 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
- 239000012494 Quartz wool Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect 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
- 239000007900 aqueous suspension Substances 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
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 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
- 239000000706 filtrate Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000002808 molecular sieve Substances 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
- 238000002429 nitrogen sorption measurement Methods 0.000 description 1
- GEVPUGOOGXGPIO-UHFFFAOYSA-N oxalic acid;dihydrate Chemical compound O.O.OC(=O)C(O)=O GEVPUGOOGXGPIO-UHFFFAOYSA-N 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
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000012495 reaction gas Substances 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
- 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
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 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
- 238000012546 transfer Methods 0.000 description 1
- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 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
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- 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
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
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- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- C07C5/32—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with formation of free hydrogen
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- C07C5/3332—Catalytic processes with metal oxides or metal sulfides
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- C07C5/42—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor
- C07C5/48—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor with oxygen as an acceptor
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- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/215—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of saturated hydrocarbyl groups
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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を含む出発化合物ならびに2つのキレート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)から生じた生成物懸濁液中に含有される固体を分離して乾燥するステップ、
d)ステップc)から得られた固体を不活性ガス中で活性化するステップ、
を含む混合酸化物材料の製造方法によって解決される。
電荷を平衡にする大きさとする。
Mo1VaNbbTecOx
(式中、
0.27<a<0.31;0.08<b<0.12;0.08<c<0.12)
を有し、
XRDにおいて、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、混合酸化物材料が得られる。
R1=Ph/(Ph+Pi)>0.3、好ましくは>0.35および特に好ましくは>0.4;ならびに/または
R2=Pi/(Pi+Pl)>0.5、好ましくは>0.6および特に好ましくは>0.63;ならびに/または
R3=Pi/(Pi+Pk)<0.8、好ましくは<0.75、特に好ましくは<0.7。
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。
X線回折図は、Medipix PIXcel 3D検出器を搭載したPANalytical Empyreanで、2θ=5〜70°という角度範囲のθ−θ幾何(θ−θGeometrie)で記録した。X線管は、Cu−K線を生成した。Cu−Kβ線は、入射X線の光線路におけるNiフィルターの使用により抑制したため、試料では、15.4nmの波長を有するCu−Kα線(E=8.04778keV)のみが回折された。ソース側光線路の高さは、自動発散スリット(programmable divergence slit−PDS)を用いて、角度範囲全体にわたって、試料が12mmの長さで照射されるように調整した。検出器側のX線の幅は、固定絞りにより、10mmに限定した。水平発散は、0.4radのソーラースリットを使用して最小限に抑えた。検出器側光線路の高さは、ソース側の光線路と類似に、自動散乱防止スリット(programmable anti−scatter slit−PASS)を用いて、角度範囲全体にわたって、試料上の12mmの長さで反射されたX線が検出されるように調整した。
細孔サイズ分布は、窒素吸着測定により、Sorptomatic装置またはTriStar3000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。吸着だけでなく脱着等温線も決定し、Barrett−Joyner−Halenda法(BJH)による評価に用いた。
例示的実施形態:
例1:
例2:
比較例1:
例3:
Claims (13)
- a)モリブデン、バナジウム、ニオブおよびテルル含有出発化合物ならびに2つのキレート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)から生じた生成物懸濁液中に含有される固体を分離して乾燥するステップ、
d)ステップc)から得られた固体を不活性ガス中で活性化するステップ、
を含む、混合酸化物材料の製造方法。 - ステップd)における活性化が450℃〜700℃の間、好ましくは550℃〜650℃の間の温度で行われることを特徴とする、請求項1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1または2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1〜3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ニオブを含むことを特徴とする、請求項1〜4のいずれか一つに記載の方法。
- 五酸化ニオブが100μm未満の粒径D90を有することを特徴とする、請求項5に記載の方法。
- 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1〜6のいずれか一つに記載の方法。
- 二酸化テルルが100μm未満の粒径D90を有することを特徴とする、請求項7に記載の方法。
- キレートオキソ配位子のうちの一つがエチレングリコールであることを特徴とする、請求項1〜8のいずれか一つに記載の方法。
- キレートオキソ配位子のうちの一つがクエン酸であることを特徴とする、請求項1〜9のいずれか一つに記載の方法。
- 元素モリブデン、バナジウム、ニオブおよびテルルを含む、エタンを酸化するための混合酸化物材料であって、以下の化学量論:
Mo1VaNbbTecOx
(式中、0.27<a<0.31;0.08<b<0.12;0.08<c<0.12)
を有し、
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、請求項1に記載の方法によって製造することができる、混合酸化物材料。 - エタンからエテンへの酸化的脱水素化のための、請求項10に記載の触媒の使用。
- プロパンの酸化のための、請求項11に記載の触媒の使用。
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DE102017000861A1 (de) | 2018-08-02 |
US20200290026A1 (en) | 2020-09-17 |
WO2018141654A1 (de) | 2018-08-09 |
KR20190115455A (ko) | 2019-10-11 |
EP3576875A1 (de) | 2019-12-11 |
KR102322199B1 (ko) | 2021-11-08 |
JP6872027B2 (ja) | 2021-05-19 |
US11014075B2 (en) | 2021-05-25 |
CN110461472A (zh) | 2019-11-15 |
WO2018141654A4 (de) | 2018-10-04 |
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