JP2006517172A - ジルコニア押出し品 - Google Patents
ジルコニア押出し品 Download PDFInfo
- Publication number
- JP2006517172A JP2006517172A JP2006500115A JP2006500115A JP2006517172A JP 2006517172 A JP2006517172 A JP 2006517172A JP 2006500115 A JP2006500115 A JP 2006500115A JP 2006500115 A JP2006500115 A JP 2006500115A JP 2006517172 A JP2006517172 A JP 2006517172A
- Authority
- JP
- Japan
- Prior art keywords
- zirconia
- extrudate
- cobalt
- calcined
- weight
- 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.)
- Granted
Links
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 372
- 235000012438 extruded product Nutrition 0.000 title description 3
- 239000000203 mixture Substances 0.000 claims abstract description 69
- 239000003054 catalyst Substances 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 56
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000004898 kneading Methods 0.000 claims abstract description 9
- 229910017052 cobalt Inorganic materials 0.000 claims description 50
- 239000010941 cobalt Substances 0.000 claims description 50
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 50
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 12
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 12
- 150000001336 alkenes Chemical class 0.000 claims description 11
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims description 7
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical group [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 6
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 5
- 229940011182 cobalt acetate Drugs 0.000 claims description 4
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 4
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 3
- 239000010419 fine particle Substances 0.000 claims 4
- 150000001868 cobalt Chemical class 0.000 claims 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 abstract description 5
- 238000001311 chemical methods and process Methods 0.000 abstract description 2
- 229930195733 hydrocarbon Natural products 0.000 description 31
- 150000002430 hydrocarbons Chemical class 0.000 description 31
- 239000002245 particle Substances 0.000 description 26
- 239000000843 powder Substances 0.000 description 22
- 239000000047 product Substances 0.000 description 22
- 239000004215 Carbon black (E152) Substances 0.000 description 18
- 150000001875 compounds Chemical class 0.000 description 18
- 238000001125 extrusion Methods 0.000 description 15
- -1 for example Chemical compound 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 14
- 239000002253 acid Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 11
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000005470 impregnation Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- 150000007514 bases Chemical class 0.000 description 7
- 238000007655 standard test method Methods 0.000 description 7
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 101100078144 Mus musculus Msrb1 gene Proteins 0.000 description 5
- 150000001298 alcohols Chemical class 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000006757 chemical reactions by type Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000006835 compression Effects 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 5
- 230000000737 periodic effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- WWUVJRULCWHUSA-UHFFFAOYSA-N 2-methyl-1-pentene Chemical compound CCCC(C)=C WWUVJRULCWHUSA-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical class CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000003868 ammonium compounds Chemical class 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 150000003973 alkyl amines Chemical class 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000010987 cubic zirconia Substances 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000867 polyelectrolyte Polymers 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011973 solid acid Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- YHQXBTXEYZIYOV-UHFFFAOYSA-N 3-methylbut-1-ene Chemical compound CC(C)C=C YHQXBTXEYZIYOV-UHFFFAOYSA-N 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical class OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-N Propionic acid Chemical class CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000005441 aurora Substances 0.000 description 1
- 150000001558 benzoic acid derivatives Chemical class 0.000 description 1
- 150000003842 bromide salts Chemical class 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000003102 growth factor Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical class I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000004694 iodide salts Chemical class 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 235000020030 perry Nutrition 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920002717 polyvinylpyridine Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 1
- 125000005537 sulfoxonium group Chemical group 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/066—Zirconium or hafnium; Oxides or hydroxides 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
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides 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
- 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
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—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
- 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
-
- 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
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
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- C01—INORGANIC CHEMISTRY
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Abstract
e.付形性ドウを押し出して、ジルコニア押出し品を形成するステップ、および
f.ジルコニア押出し品を乾燥および焼成するステップ
を含み、微粒子ジルコニアが、単斜晶ジルコニア以外のジルコニアを15重量%以下含むことを特徴とする、焼成ジルコニア押出し品を調製する方法。本発明により調製された焼成ジルコニウム押出し品は著しく改善された破砕強度を示し、広範囲の化学プロセスにおいて触媒または支持体として適する。
Description
a.50重量%から85重量%の総固形分を有する混合物を得るために、微粒子ジルコニアを溶媒と混合および混練することを含む付形性ドウを調製するステップ、
b.付形性ドウを押し出して、ジルコニア押出し品を形成するステップ、および
c.ジルコニア押出し品を乾燥および焼成するステップ
を含み、微粒子ジルコニアが、単斜晶ジルコニア以外のジルコニアを15重量%以下含むことを特徴とする、焼成ジルコニア押出し品を製造する方法が提供される。
a.50重量%から85重量%の総固形分を有する混合物を得るために、微粒子ジルコニアおよびコバルト前駆物質を溶媒と混合および混練することを含む付形性ドウを調製するステップ、
b.付形性ドウを押し出して、ジルコニア/コバルト押出し品を形成するステップ、および
c.ジルコニア/コバルト押出し品を乾燥および焼成するステップ
を含み、微粒子ジルコニアが、単斜晶ジルコニア以外のジルコニアを15重量%以下含むことを特徴とする、焼成コバルト/ジルコニアを調製する方法が提供される。
a.50重量%から85重量%の総固形分を有する混合物を得るために、微粒子ジルコニアを溶媒と混合および混練することを含む付形性ドウを調製するステップ、
b.付形性ドウを押し出して、ジルコニア押出し品を形成するステップ、
c.ジルコニア押出し品を液体コバルト前駆物質に含浸させて、コバルト含浸ジルコニア押出し品を形成するステップ、および
d.コバルト含侵ジルコニア押出し品を乾燥および焼成するステップ
を含み、微粒子ジルコニアが、単斜晶ジルコニア以外のジルコニアを15重量%以下含むことを特徴とする、焼成コバルト含浸ジルコニア押出し品を調製する方法が提供される。
(a)0.3ml/g以上の細孔体積、
(b)100N/cm以上のラジアル破砕強度、および
(c)50m2/g以上の表面積。
以下の実施例において、用語、強熱損失(または「LOI」)は、炉において550℃で2時間処理した後の、その試料の重量損失によって測定された試料において存在する水分の量である。
本発明による焼成ジルコニア押出し品を以下のように調製する。商標DAIICHI RC−100(DKK Daiichi Kigenso Kagaku Kogyo Co.Ltd.から市販されている)を有し、1.9%の強熱損失を有する酸化ジルコニウム粉末7060グラムを、水2654グラム、アンモニア溶液416グラム(水酸化アンモニウム25重量%を含む)、SUPERFLOC N100(Cytec Industries B.V.、Botlekweg 175、3197 KA、Botlek−Rotterdam、The Netherlandsから市販されているポリ電解質)69グラム、およびポリビニルアルコール(Kuraray Specialties Europea、GmbH、c/o Clariant Benelux N.V.、Diemerhof 36、1112 XN Diemen、The Netherlandsから市販されているMOWIOL 8−88)139グラムと混合する。
実施例1において使用されたジルコニア粉体を、Daiichi HC−100 80%および商標SEPR HC15を有するジルコニア粉体(Societe Europeenne des Produits Refractaires、Les Miroires、18 Rue D’Alsace、92400 Courbevoie、Franceから市販されている)20%の混合物によって置き換える以外は、実施例1の手順を繰り返す。SEPR HC15は、正方晶ジルコニア98.3重量%および単斜晶ジルコニア(上記実施例1において記載されているものと同様のX線回折装置および同様な設定を使用して、X線回折によって解析された)1.7重量%を含み、LOI24.4%を含む。実施例1におけるものと同様の、押出しドウのLOIを実現するためには、添加する水の量を減少させる。得られたドウは、測定されたLOI32.87%およびpH10.2を有する。押出し、乾燥および焼成は、実施例1に対するものと同様の方法において実施する。最終押出し品のラジアル破砕強度を標準試験法ASTM D6175−98を使用して、測定した。結果を以下の表1に示す。
実施例1において使用されたジルコニア粉体を、Daiichi RC−100 50%および商標SEPR HC15(実施例2において使用されているものと同様の)を有するジルコニア粉体50%の混合物によって置き換える以外は、実施例1の手順を繰り返す。実施例1におけるものと同様の押出しドウのLOIを実現するためには、水の量を減少させる。得られたドウは、測定されたLOI31.89%およびpH9.8を有する。押出し、乾燥および焼成は、実施例1に対するものと同様の方法において実施する。最終押出し品のラジアル破砕強度を標準試験法ASTM D6175−98を使用して、測定した。結果を以下の表1に示す。
実施例1において使用されているジルコニア粉体を、ジルコニア粉体SEPR HC15(実施例2において使用されているものと同様の)によって置き換える以外は、実施例1の手順を繰り返す。実施例1におけるものと同様の押出しドウのLOIを実現するためには、添加する水の量を減少させる。得られたドウは、測定されたLOI31.89%およびpH9.8を有する。押出し、乾燥および焼成は、実施例1に対するものと同様の方法において実施する。最終押出し品のラジアル破砕強度を標準試験法ASTM D6175−98を使用して測定した。結果を以下の表1に示す。
実施例1において使用されているジルコニア粉体を、押出し混合物に添加する前に400℃で、焼成されたジルコニア粉体SEPR HC15(実施例2において使用されているものと同様の)によって置き換える以外は、実施例1の手順を繰り返す。粉体は、X線回折(上記実施例1において記載されているものと同様のX線回折装置および同様な設定を使用して)によって解析された正方晶(98.3%)および単斜晶(1.7%)ジルコニアの混合物からなり、LOI3.2%を有する。実施例1におけるものと同様の押出しドウのLOIを実現するためには、添加する水の量を減少させる。得られたドウは、測定されたLOI33.75%およびpH9.8を有する。押出し、乾燥および焼成は、実施例1に対するものと同様の方法において実施する。最終押出し品のラジアル破砕強度を標準試験法ASTM D6175−98を使用して測定する。結果を以下の表1に示す。
実施例1において使用されているジルコニア粉体を、ジルコニア粉体、MEL XZO 880/1(MEL Chemicals、Clifton Junction、P.O.BOX 6、Swinton、M27 8LS、Manchester、UKから市販されている)によって置き換える以外は、実施例1の手順を繰り返す。粉体は、X線回折(上記実施例1において記載されているものと同様のX線回折装置および同様な設定を使用して)、X線回折によって解析された正方晶ジルコニア100%からなり、LOI1.9%を有する。実施例1におけるものと同様の押出しドウのLOIを実現するためには、添加する水の量を減少させる。得られたドウは、測定されたLOI48.5%およびpH9.3を有する。押出し、乾燥および焼成は、実施例1に対するものと同様の方法において実施する(2.5mm円筒型板だけを使用した以外)。最終押出し品のラジアル破砕強度を標準試験法ASTM D6175−98を使用して測定する。結果を以下の表1に示す。
LOI5.3%で、商標DAIICHI RC−100(実施例1において使用されているものと同様の)を有する酸化ジルコニウム粉264グラムを、5重量%ポリビニルアルコール水溶液(商標MOWIOL 18−88)90グラムと混合する。この混合物を、Werner & Pfleiderer、Stuttgart、Germanyによって供給されるSigma(Z−blade)混練機タイプLUK0.5において、2分間混練する。混合物にSUPERFLOC N100、2.5グラムを添加し、混合を5分間続ける。次いで、水8グラムを混合物に添加し、混合を30分間続ける。それによって得られたドウは、測定されたLOI31.5%およびpH8.4を有する。このドウを、1インチ単軸スクリュウピン押出機(The Bonnot社によって供給される)を使用して、1.6mm三葉形型板を使用して押し出す。押出し品を120℃で1時間乾燥し、次いで、固定炉において生成物温度550℃で2時間焼成する。最終押出し品の細孔体積は0.312ml/g、表面積は55m2/gである。最終押出し品のラジアル破砕強度は、233N/cmである。この実施例は、本発明の調製方法において、酸または塩基を使用する必要はないことを示している。したがって、酸または塩基が、触媒に有害な影響を及ぼす場合には、押出し品の調製において、酸または塩基の使用を避けることができる。
ドウを、1.0mm三葉形型板を使用して押し出す以外は、実施例1の手順を繰り返す。押出し品を120℃で1時間乾燥し、次いで、回転炉において生成物温度550℃で2時間焼成する。この手順を繰り返し、2つの生成物を混合した。最終生成物は、J.Amer.Chem.Soc.、60(1938)309において記載されている窒素吸着BET法によって表面積60.5m2/g、H.L.RitterおよびL.C.Drake、In.Eng.Chem.、Anal.Ed.、17(1945)782において記載されている水銀貫入法によって測定した細孔体積0.352ml/g、および実施例1において使用したのと同様の試験法によって測定したラジアル破砕強度154N/cmを有する。
酸化ジルコニウムDAIICHI RC−100粉末18749グラムを、水酸化コバルト8091グラムと混合する。乾燥粉末をSimpson混合物混和機においてブレンドする。このブレンドに、ポリビニルアルコール5重量%水溶液(MOWIOL 18−88)5729グラム、固体ポリビニルアルコール(MOWIOL 18−88)210.5グラム、クエン酸255グラム、および水2802グラムを添加する。と混合する。この混合物をSIMPSON混合物混和機において、36分混練する。次いで、SUPERFLOC N100、505グラムを添加し、混合をさらに5分間続ける。それによって得られたドウは、測定されたLOI31.8%を有し、pHは、7.8である。このドウを、2.25インチBONNOT押出機を使用して、1.0mm三葉形型板を使用して押し出す。押出し品を120℃で4時間乾燥し、次いで、固定炉において生成物温度550℃で1時間焼成する。この手順を繰り返し、2つの生成物を混合する。最終生成物は強度113N/cmを有する。
Claims (10)
- a.50重量%から85重量%の総固形分を有する混合物を得るために、微粒子ジルコニアを溶媒と混合および混練することを含む付形性ドウを調製するステップ、
b.付形性ドウを押し出して、ジルコニア押出し品を形成するステップ、および
c.ジルコニア押出し品を乾燥および焼成するステップ
を含み、
微粒子ジルコニアが、単斜晶ジルコニア以外のジルコニアを15重量%以下含むことを特徴とする、焼成ジルコニア押出し品を調製する方法。 - d.50重量%から85重量%の固形分を有する混合物を得るために、微粒子ジルコニアおよびコバルト前駆物質を溶媒と混合および混練することを含む付形性ドウを調製するステップ、
e.付形性ドウを押し出して、ジルコニア/コバルト押出し品を形成するステップ、および
f.ジルコニア/コバルト押出し品を乾燥および焼成するステップ
を含み、
微粒子ジルコニアが、単斜晶ジルコニア以外のジルコニアを15重量%以下含むことを特徴とする、焼成コバルト/ジルコニア押出し品を調製する方法。 - コバルト前駆物質が、水酸化コバルト、酢酸コバルト、硝酸コバルト、酸化コバルト、およびその混合物から選択される請求項2に記載の方法。
- 微粒子ジルコニアが、単斜晶ジルコニア以外のジルコニアを10重量%以下含む請求項1から3のいずれかに記載の方法。
- 請求項1または4に記載の方法によって調製された焼成ジルコニア押出し品。
- 請求項2から4のいずれかに記載の方法によって調製された焼成ジルコニア/コバルト押出し品。
- a.50重量%から85重量%の総固形分を有する混合物を得るために、微粒子ジルコニアを溶媒と混合および混練することを含む付形性ドウを調製するステップ、
b.付形性ドウを押し出して、ジルコニア押出し品を形成するステップ、
c.液体コバルト前駆物質にジルコニア押出し品を含浸させて、コバルト含浸ジルコニア押出し品を形成するステップ、および
d.コバルト含浸ジルコニア押出し品を乾燥および焼成するステップ
を含み、
微粒子ジルコニアが、単斜晶ジルコニア以外のジルコニアを15重量%以下含むことを特徴とする、焼成コバルト含浸ジルコニア押出し品を調製する方法。 - 液体コバルト前駆物質が、硝酸コバルト、酢酸コバルト、水酸化コバルト、およびその混合物から選択されるコバルト塩の水溶液から選択される請求項7に記載の方法。
- 請求項7または8に従って調製された焼成コバルト含浸ジルコニア押出し品。
- 請求項6に記載の焼成ジルコニア/コバルト押出し品または請求項9に記載の焼成コバルト含浸ジルコニア押出し品の触媒としての存在下において、フィッシャー−トロプシュ反応条件で水素と一酸化炭素とを接触させることを含む11から14個の炭素原子を有する高級オレフィンを調製する方法。
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