JP2012531306A - 最適化されたサイト近接度を有する多金属触媒の調製方法 - Google Patents
最適化されたサイト近接度を有する多金属触媒の調製方法 Download PDFInfo
- Publication number
- JP2012531306A JP2012531306A JP2012518103A JP2012518103A JP2012531306A JP 2012531306 A JP2012531306 A JP 2012531306A JP 2012518103 A JP2012518103 A JP 2012518103A JP 2012518103 A JP2012518103 A JP 2012518103A JP 2012531306 A JP2012531306 A JP 2012531306A
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- Prior art keywords
- catalyst
- range
- tin
- preparing
- metal
- Prior art date
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- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 44
- 230000008569 process Effects 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 77
- 229910052718 tin Inorganic materials 0.000 claims abstract description 52
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 39
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011574 phosphorus Substances 0.000 claims abstract description 35
- 229910052738 indium Inorganic materials 0.000 claims abstract description 26
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 8
- 238000001833 catalytic reforming Methods 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 229910052716 thallium Inorganic materials 0.000 claims abstract description 8
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 claims abstract description 8
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 6
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000465 moulding Methods 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 239000011135 tin Substances 0.000 claims description 58
- 239000000460 chlorine Substances 0.000 claims description 32
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 31
- 229910052801 chlorine Inorganic materials 0.000 claims description 31
- 229910052697 platinum Inorganic materials 0.000 claims description 31
- 150000001875 compounds Chemical class 0.000 claims description 17
- 238000001354 calcination Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 9
- 150000002430 hydrocarbons Chemical class 0.000 claims description 9
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 8
- 239000004215 Carbon black (E152) Substances 0.000 claims description 8
- 229930195733 hydrocarbon Natural products 0.000 claims description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical group [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 5
- 229910052740 iodine Inorganic materials 0.000 claims description 3
- 229910052763 palladium Chemical group 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 3
- 230000000153 supplemental effect Effects 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 150000001491 aromatic compounds Chemical class 0.000 abstract description 3
- 150000002366 halogen compounds Chemical class 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 17
- 238000005004 MAS NMR spectroscopy Methods 0.000 description 16
- 239000011324 bead Substances 0.000 description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000013256 coordination polymer Substances 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 238000002407 reforming Methods 0.000 description 8
- 238000005481 NMR spectroscopy Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 7
- -1 extrudates Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 150000004679 hydroxides Chemical class 0.000 description 4
- 239000002923 metal particle Substances 0.000 description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 4
- 235000011150 stannous chloride Nutrition 0.000 description 4
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000000571 coke Substances 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 150000002823 nitrates Chemical class 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 125000002524 organometallic group Chemical group 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 229910002846 Pt–Sn Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910009038 Sn—P Inorganic materials 0.000 description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Chemical compound [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- VBWYZPGRKYRKNV-UHFFFAOYSA-N 3-propanoyl-1,3-benzoxazol-2-one Chemical compound C1=CC=C2OC(=O)N(C(=O)CC)C2=C1 VBWYZPGRKYRKNV-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 238000005727 Friedel-Crafts reaction Methods 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910018956 Sn—In Inorganic materials 0.000 description 1
- 229910052767 actinium Inorganic materials 0.000 description 1
- QQINRWTZWGJFDB-UHFFFAOYSA-N actinium atom Chemical compound [Ac] QQINRWTZWGJFDB-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- JRLDUDBQNVFTCA-UHFFFAOYSA-N antimony(3+);trinitrate Chemical class [Sb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JRLDUDBQNVFTCA-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000007233 catalytic pyrolysis Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000012050 conventional carrier Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005388 cross polarization Methods 0.000 description 1
- 238000005384 cross polarization magic-angle spinning Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229940044658 gallium nitrate Drugs 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000000449 magic angle spinning nuclear magnetic resonance spectrum Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 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 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- FYWSTUCDSVYLPV-UHFFFAOYSA-N nitrooxythallium Chemical compound [Tl+].[O-][N+]([O-])=O FYWSTUCDSVYLPV-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical class OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- 238000004525 petroleum distillation Methods 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 238000002002 phosphorus-31 magic angle spinning nuclear magnetic resonance spectrum Methods 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000006057 reforming reaction Methods 0.000 description 1
- 230000004044 response Effects 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
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical class [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010996 solid-state NMR spectroscopy Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- PUGUQINMNYINPK-UHFFFAOYSA-N tert-butyl 4-(2-chloroacetyl)piperazine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCN(C(=O)CCl)CC1 PUGUQINMNYINPK-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
- B01J27/13—Platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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Abstract
Description
・COのp軌道と金属の空d軌道との間のσ結合;
・充填d軌道とCOの空(empty)反結合性軌道との間のπバックボンディング。
本発明は、白金族からの少なくとも1種の金属Mと、スズと、リンプロモータと、ハロゲン化化合物と、多孔質担体と、ガリウム、インジウム、タリウム、ヒ素、アンチモン、およびビスマスによって構成される群より選択される少なくとも1種のプロモータX1とを含む触媒に関する。触媒は、H3PO4のシグナルに対して−30〜−50ppmの範囲に、31Pマジック角スピニングNMRシグナルを有する。それはまた、オーバーラップのゼロ度における一酸化炭素結合についての波数:2077cm−1超を有する。本発明は、また、前記触媒の調製、および接触改質または芳香族生成反応におけるその使用に関する。
本発明は、白金族からの少なくとも1種の金属Mと、スズと、リンプロモータと、ハロゲン化化合物と、多孔質担体と、少なくとも1種のプロモータX1とを含む触媒であって、該プロモータX1は、ガリウム、インジウム、タリウム、ヒ素、およびアンチモンによって構成される群より選択され、好ましくはガリウム、タリウム、およびインジウムによって構成される群より選択され、一層好ましくはガリウムおよびインジウムによって構成される群より選択され、かつ、前記触媒は、31Pマジック角スピニングNMRシグナルをH3PO4のシグナルに対して−30〜−50ppmの範囲に有する、触媒に関する。
a) サブ工程a1)またはa2)の一方の間に、単数または複数のプロモータX1およびリンを導入する工程、ここで、前記サブ工程a1)は、主要酸化物の前駆体の合成に相当し、前記サブ工程a2)は担体の成形に相当する;
b) サブ工程a1)およびa2)のうち少なくとも一方の間にスズを導入する工程、ここで、工程a)およびb)は場合により連続的にあるいは同時に行われる;
c) 工程b)の終わりに得られた生成物を乾燥させる工程;
d) 工程c)で得られた生成物を、350〜650℃の範囲の温度で焼成する工程;
e) 白金族からの少なくとも1種の金属Mを沈着させる工程;
f) 中性ガス流または酸素含有ガス流中、150℃を越えない中程度の温度で乾燥させる工程;
g) 工程f)で得られた生成物を、350〜650℃の範囲の温度で焼成する工程。
以下の実施例は本発明を例証するものである。
0.3重量%のスズを含有しかつ平均径が1.2mmであるアルミナビーズの形態の担体の調製を、二塩化スズと、塩化アルミニウムの加水分解により得られたアルミナヒドロゾルとを接触させることにより行った。これにより得られたアルミナヒドロゾルを、次いで、添加油(additive oil)で満たされた垂直カラム中に通過させた。このようにして得られた球体を600℃までの温度で熱処理し、良好な機械的強度を有するビーズを得た。これにより得られた担体のBET比表面積は205m2/gであった。
0.3重量%のスズおよび0.3重量%のインジウムを含有しかつ平均径が1.2mmであるアルミナビーズの形態の担体の調製を、二塩化スズおよび硝酸インジウムと、塩化アルミニウムの加水分解により得られたアルミナヒドロゾルとを接触させることにより行った。これにより得られたアルミナヒドロゾルを、次いで、添加油で満たされた垂直カラム中に通過させた。このようにして得られた球体を600℃までの温度で熱処理し、良好な機械的強度を有するビーズを得た。これにより得られた担体は、201m2/gのBET比表面積を有していた。
0.3重量%のスズおよび0.4重量%のリンを含有しかつ平均径が1.2mmであるアルミナビーズの形態の担体を、実施例1に記載された方法と同様の方法で、二塩化スズおよびリン酸と、アルミナヒドロゾルとを接触させることにより得た。これにより得られた担体のBET比表面積は198m2/gであった。
0.3重量%のスズ、0.3重量%のインジウムおよび0.4重量%のリンを含有しかつ平均径が1.2mmであるアルミナビーズの形態の担体を、実施例1に記載された方法と同様の方法で、二塩化スズ、硝酸インジウムおよびリン酸と、アルミナヒドロゾルとを接触させることにより得た。これにより得られた担体のBET比表面積は196m2/gであった。
実施例4と同様の方法で、アルミナビーズの形態の担体を調製した。但し、本実施例においては、スズとリンは実施例4と同量であるが、インジウムは0.2重量%しか導入しなかった。これにより得られた担体のBET比表面積は210m2/gであった。
担体を調製し、実施例3と同量のスズとリンを目標とした。これにより得られた担体のBET比表面積は180m2/gであった。
担体を調製し、実施例1と同量のスズを目標とした。
担体を調製し、実施例4と同量のインジウムおよびリン、ならびに0.2重量%のスズを目標とした。このようにして得られた担体のBET比表面積は182m2/gであった。
0.1重量%のスズ、0.4重量%のアンチモン、および0.4重量%のリンを含有し、かつ平均径が1.2mmであるアルミナビーズ担体を、二塩化スズ、硝酸ガリウム、およびリン酸を用いる実施例4に記載の方法と類似の方法で調製した。このようにして得られた担体のBET比表面積は191m2/gであった。
本明細書に提示される方法を用いて測定される、触媒C〜Iの31P NMRシグナルの値、並びに、{1H−31P}CP MASシリーズにおける種々のシグナルの面積の増加が、表1に詳細に記載されている。増加は、交差分極(CP MAS)において得られるシグナルの面積と、直接分極(MAS)において同様のケミカルシフトを有するシグナルの面積との比として計算した。
実施例1〜9に記載したように調製された触媒のサンプルを、石油の蒸留に由来するナフサタイプの炭化水素供給原料の転化に適応した反応床中に置いた。
・パラフィン化合物:52.6%;
・ナフテン:31.6%;
・芳香族分子:15.8%;
の組成(重量による)を有し、全体密度は0.759g/cm3であった。
・反応器の圧力は、8bar g(0.8Mpa g)に維持された;
・供給原料の流量:触媒の重量(kg)当たり2.0kg/時間;
・供給原料の水素/炭化水素モル比:4
供給原料の接触転化に由来する液体流出物(リフォメートとも称される)のリサーチオクタン価の等質(iso-quality)比較を行った。104のリサーチオクタン価に対して比較を行った。
Claims (12)
- 白金族からの少なくとも1種の金属Mと、スズと、リンプロモータと、ハロゲン化化合物と、多孔質担体と、ガリウム、インジウム、タリウム、ヒ素、アンチモン、およびビスマスによって構成される群より選択される少なくとも1種のプロモータX1とを含む触媒の調製方法であって、以下の工程を含む方法:
a) サブ工程a1)またはa2)の一方の間に、単数または複数のプロモータX1およびリンを導入する工程、ここで、前記サブ工程a1)は、主要酸化物の前駆体の合成に相当し、前記サブ工程a2)は担体の成形に相当する;
b) サブ工程a1)およびa2)のうち少なくとも一方の間にスズを導入する工程、ここで、工程a)およびb)は場合により連続的にあるいは同時に行われる;
c) 工程b)の終わりに得られた生成物を乾燥させる工程;
d) 工程c)で得られた生成物を、350〜650℃の範囲の温度で焼成する工程;
e) 白金族からの少なくとも1種の金属Mを沈着させる工程;
f) 中性ガスの流れまたは酸素を含有するガスの流れ中、150℃を越えない中程度の温度で乾燥させる工程;
g) 工程f)で得られた生成物を、350〜650℃の範囲の温度で焼成する工程。 - 原子比Sn/Mは0.5〜4.0の範囲である、請求項1に記載の触媒の調製方法。
- 比X1/Mは0.1〜5.0の範囲である、請求項1または2に記載の触媒の調製方法。
- 比P/Mは0.2〜30.0の範囲である、請求項1〜3のいずれか1つに記載の触媒の調製方法。
- 金属Mの量は0.01〜5重量%の範囲である、請求項1〜4のいずれか1つに記載の触媒の調製方法。
- 金属Mは白金またはパラジウムである、請求項1〜5のいずれか1つに記載の触媒の調製方法。
- ハロゲン化化合物はフッ素、塩素、臭素、およびヨウ素によって構成される群より選択される、請求項1〜6のいずれか1つに記載の触媒の調製方法。
- ハロゲン化化合物の量は0.1〜15.0重量%の範囲である、請求項1〜7のいずれか1つに記載の触媒の調製方法。
- ハロゲン化化合物は塩素であり、塩素含有量は0.1〜5.0重量%の範囲である、請求項1〜8のいずれか1つに記載の触媒の調製方法。
- 担体は、マグネシウム、チタン、ジルコニウム、アルミニウム、およびケイ素の酸化物によって構成される群より選択される少なくとも1種の酸化物を含む、請求項1〜9のいずれか1つに記載の触媒の調製方法。
- 請求項1〜10のいずれか1つに記載の触媒の調製方法であって、スズは、担体の合成又は成形の間に一部のみ導入され、該方法は、スズの補完部分を担体上に沈着させる補足工程を、工程d)と工程e)の間か、工程e)と工程f)の間か、または、工程g)の後のいずれかに含み、該補足工程を工程d)と工程e)の間に含む場合、該補足工程の後に乾燥および焼成を行う場合と行わない場合があり、該補足工程を工程e)と工程f)の間または工程g)の後に含む場合、該補足工程の後に乾燥および焼成を行う、方法。
- 前記触媒を炭化水素供給原料と接触させるにことよる接触改質または芳香族生成のための反応において、請求項1〜11のいずれか1つに従って調製された触媒を用いる方法。
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FR3039082B1 (fr) * | 2015-07-24 | 2017-07-21 | Ifp Energies Now | Catalyseur multi-metallique dope par du phosphore et un lanthanide |
FR3074063B1 (fr) * | 2017-11-30 | 2019-11-01 | IFP Energies Nouvelles | Catalyseur multi-metallique dope par du phosphore et de l'ytterbium |
FR3120076A1 (fr) | 2021-02-22 | 2022-08-26 | IFP Energies Nouvelles | Procédé de production de composés aromatiques et/ou d’essences à partir d’une charge hydrocarbonée de type naphta |
FR3123230A1 (fr) | 2021-05-28 | 2022-12-02 | IFP Energies Nouvelles | Procédé de traitement à régénération continue de catalyseur d’une charge hydrocarbonée |
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WO2008087273A2 (fr) * | 2006-12-22 | 2008-07-24 | Ifp | Catalyseur bimetallique ou multi-metallique presentant un indice de bimetallicite et une capacite d'adsorption d'hydrogene optimises |
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2009
- 2009-07-01 FR FR0903226A patent/FR2947465B1/fr active Active
-
2010
- 2010-06-15 US US13/381,281 patent/US20120178979A1/en not_active Abandoned
- 2010-06-15 DK DK10734170.3T patent/DK2448670T3/en active
- 2010-06-15 CN CN2010800301225A patent/CN102665897A/zh active Pending
- 2010-06-15 CN CN201610819884.2A patent/CN106423226B/zh active Active
- 2010-06-15 EP EP10734170.3A patent/EP2448670B1/fr active Active
- 2010-06-15 JP JP2012518103A patent/JP5615917B2/ja active Active
- 2010-06-15 RU RU2012103328/04A patent/RU2535206C2/ru active
- 2010-06-15 WO PCT/FR2010/000443 patent/WO2011012776A2/fr active Application Filing
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2017
- 2017-03-23 US US15/467,677 patent/US20170252726A1/en not_active Abandoned
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US4522935A (en) * | 1983-06-02 | 1985-06-11 | Uop Inc. | Platinum and indium-containing catalyst for reforming hydrocarbons |
JP2005525933A (ja) * | 2002-05-22 | 2005-09-02 | シエル・インターナシヨナル・リサーチ・マートスハツペイ・ベー・ヴエー | ビスマスおよびリン含有改質触媒、作製方法、およびナフサ改質方法 |
WO2008087273A2 (fr) * | 2006-12-22 | 2008-07-24 | Ifp | Catalyseur bimetallique ou multi-metallique presentant un indice de bimetallicite et une capacite d'adsorption d'hydrogene optimises |
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Also Published As
Publication number | Publication date |
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CN106423226A (zh) | 2017-02-22 |
DK2448670T3 (en) | 2016-01-11 |
FR2947465B1 (fr) | 2012-05-11 |
WO2011012776A2 (fr) | 2011-02-03 |
RU2012103328A (ru) | 2013-08-10 |
WO2011012776A3 (fr) | 2011-11-17 |
JP5615917B2 (ja) | 2014-10-29 |
US20170252726A1 (en) | 2017-09-07 |
CN106423226B (zh) | 2022-09-27 |
US20120178979A1 (en) | 2012-07-12 |
FR2947465A1 (fr) | 2011-01-07 |
CN102665897A (zh) | 2012-09-12 |
EP2448670B1 (fr) | 2015-09-23 |
EP2448670A2 (fr) | 2012-05-09 |
RU2535206C2 (ru) | 2014-12-10 |
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