DK2860158T3 - Metalholdig silicoaluminophosphat-molekylsigte med rho-skeletstruktur og fremgangsmåde til fremstilling heraf - Google Patents
Metalholdig silicoaluminophosphat-molekylsigte med rho-skeletstruktur og fremgangsmåde til fremstilling heraf Download PDFInfo
- Publication number
- DK2860158T3 DK2860158T3 DK12878414.7T DK12878414T DK2860158T3 DK 2860158 T3 DK2860158 T3 DK 2860158T3 DK 12878414 T DK12878414 T DK 12878414T DK 2860158 T3 DK2860158 T3 DK 2860158T3
- Authority
- DK
- Denmark
- Prior art keywords
- metal
- mixture
- diethylamine
- source
- molecular sieve
- Prior art date
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- 229910052751 metal Inorganic materials 0.000 title claims description 51
- 239000002184 metal Substances 0.000 title claims description 51
- 238000000034 method Methods 0.000 title claims description 28
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 85
- 239000002808 molecular sieve Substances 0.000 claims description 84
- 239000000203 mixture Substances 0.000 claims description 76
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 33
- 238000002425 crystallisation Methods 0.000 claims description 31
- 230000008025 crystallization Effects 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000000499 gel Substances 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 25
- 229910021641 deionized water Inorganic materials 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 24
- 230000008569 process Effects 0.000 claims description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 150000003839 salts Chemical class 0.000 claims description 16
- 229910052710 silicon Inorganic materials 0.000 claims description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 15
- 229910052725 zinc Inorganic materials 0.000 claims description 15
- 239000011701 zinc Substances 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910017052 cobalt Inorganic materials 0.000 claims description 14
- 239000010941 cobalt Substances 0.000 claims description 14
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- 229910052749 magnesium Inorganic materials 0.000 claims description 14
- 239000011777 magnesium Substances 0.000 claims description 14
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- 239000004094 surface-active agent Substances 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 239000011574 phosphorus Substances 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 7
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 7
- 229910001868 water Inorganic materials 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- -1 aluminum alkoxide Chemical class 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 125000001664 diethylamino group Chemical group [H]C([H])([H])C([H])([H])N(*)C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical class [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 3
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 claims description 3
- CXRFDZFCGOPDTD-UHFFFAOYSA-M Cetrimide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)C CXRFDZFCGOPDTD-UHFFFAOYSA-M 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- LQQFSMCMZMSDQQ-UHFFFAOYSA-M dimethyl-octadecyl-(3-trimethylsilylpropyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCC[Si](C)(C)C LQQFSMCMZMSDQQ-UHFFFAOYSA-M 0.000 claims description 2
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 2
- GVMSPQSHPILRIP-UHFFFAOYSA-M hexadecyl-dimethyl-(3-trimethylsilylpropyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)CCC[Si](C)(C)C GVMSPQSHPILRIP-UHFFFAOYSA-M 0.000 claims description 2
- 229910052605 nesosilicate Inorganic materials 0.000 claims description 2
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 2
- 150000004762 orthosilicates Chemical class 0.000 claims description 2
- 229910001392 phosphorus oxide Inorganic materials 0.000 claims description 2
- LFGREXWGYUGZLY-UHFFFAOYSA-N phosphoryl Chemical class [P]=O LFGREXWGYUGZLY-UHFFFAOYSA-N 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- IKRRMNBUMJLUOL-UHFFFAOYSA-M trimethyl(pentadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCC[N+](C)(C)C IKRRMNBUMJLUOL-UHFFFAOYSA-M 0.000 claims description 2
- OHCYZUDVCRJREC-UHFFFAOYSA-M trimethyl(pentadecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCC[N+](C)(C)C OHCYZUDVCRJREC-UHFFFAOYSA-M 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 3
- 238000001354 calcination Methods 0.000 claims 3
- 239000007809 chemical reaction catalyst Substances 0.000 claims 2
- 150000004767 nitrides Chemical class 0.000 claims 2
- 229910018404 Al2 O3 Inorganic materials 0.000 claims 1
- 239000006096 absorbing agent Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000149 penetrating effect Effects 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 description 21
- 230000015572 biosynthetic process Effects 0.000 description 19
- 238000003786 synthesis reaction Methods 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 11
- 239000007789 gas Substances 0.000 description 11
- 238000000926 separation method Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 10
- 238000009472 formulation Methods 0.000 description 9
- 230000007935 neutral effect Effects 0.000 description 9
- 239000012265 solid product Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000003463 adsorbent Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 241000269350 Anura Species 0.000 description 6
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 6
- 239000010457 zeolite Substances 0.000 description 6
- 229910021536 Zeolite Inorganic materials 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 4
- 235000011007 phosphoric acid Nutrition 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000008240 homogeneous mixture Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- ONWIUHATKXRGRY-UADPMFFRSA-N (2r)-6-amino-2-[[(2r)-2-[[(2r)-2-[[(2r)-2-[[(2r)-2-[[(2r)-2-[[(2r,3s)-2-amino-3-hydroxybutanoyl]amino]propanoyl]amino]-3-(4-hydroxyphenyl)propanoyl]amino]-3-phenylpropanoyl]amino]-4-methylpentanoyl]amino]-4-methylpentanoyl]amino]-n-[(2r)-1-[[(2r)-1-[[2-[[ Chemical compound C([C@H](C(=O)N[C@H](CC(C)C)C(=O)N[C@H](CC(C)C)C(=O)N[C@H](CCCCN)C(=O)N[C@H](CC(C)C)C(=O)N[C@H](C)C(=O)NCC(=O)N[C@H](CCCN=C(N)N)C(=O)N[C@H](CC=1C2=CC=CC=C2NC=1)C(N)=O)NC(=O)[C@@H](CC=1C=CC(O)=CC=1)NC(=O)[C@@H](C)NC(=O)[C@H](N)[C@H](C)O)C1=CC=CC=C1 ONWIUHATKXRGRY-UADPMFFRSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229940058344 antitrematodals organophosphorous compound Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- OAVPQXXPJZPXTA-UHFFFAOYSA-N n,n'-di(propan-2-yl)propane-1,3-diamine Chemical compound CC(C)NCCCNC(C)C OAVPQXXPJZPXTA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- AICNZRYBCUSVMO-UHFFFAOYSA-M trimethyl(tridecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCC[N+](C)(C)C AICNZRYBCUSVMO-UHFFFAOYSA-M 0.000 description 1
- VCOYQLVGJRYNFY-UHFFFAOYSA-M trimethyl(tridecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCC[N+](C)(C)C VCOYQLVGJRYNFY-UHFFFAOYSA-M 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
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/54—Phosphates, e.g. APO or SAPO compounds
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates [SAPO compounds]
-
- 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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Catalysts (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Claims (18)
1. Metal-silicoaluminophosphat-molekylsigte med RHO-skeletstruktur, hvis kemiske sammensætning i den vandfrie tilstand udtrykkes som: mR-nMe-(SixAlyPz)02, hvor R repræsenterer en template, der eksisterer i mikroporer af metal-silicoaluminophosphat-molekylsigten; R er diethylamin, en blanding af diethylamin og triethylamin, en blanding af diethylamin og morpholin eller en blanding af diethylamin og tetraethylammoniumhydroxid; m er moltallet for templaten pr. én mol af (SixAlyPz)02, m=0,l~0,5; Me repræsenterer et metalatom, der trænger ind i metal-silicoaluminophosphat-molekylsigtens skelet; Me er ét eller flere metalatomer udvalgt fra gmppen bestående af vanadium, kobber, molybden, zirconium, cobalt, mangan, magnesium, jern, nikkel og zink; n er moltallet for Me pr. én mol af (SixAlyPzjCk, n=0,001~ 0,30; x, y, z henholdsvis repræsenterer moltallet for Si, Al, P, hvor x = 0,01-0,60, y = 0,2-0,60, z = 0,2-0,60 og x + y + z =1.
2. Metal-silicoaluminophosphat-molekylsigte ifølge krav 1, kendetegnet ved, at templaten R er en blanding af diethylamin og triethylamin, en blanding af diethylamin og morpholin eller en blanding af diethylamin og tetraethylammoniumhydroxid; hvor molforholdet af diethylamin i blandingen er mere end 70 %.
3. Metal-silicoaluminophosphat-molekylsigte ifølge krav 1, kendetegnet ved, at metalatomet Me er ét eller flere metalatomer udvalgt fra gruppen bestående af kobber, cobalt, mangan, magnesium, jem, nikkel og zink.
4. Metal-silicoaluminophosphat-molekylsigte ifølge krav 1, kendetegnet ved, at metalatomet Me, der trænger ind i metal-silicoaluminophosphat-molekylsigtens skelet, er ét eller flere metalatomer udvalgt fra gruppen bestående af kobber, cobalt, mangan, magnesium og zink.
5. Fremgangsmåde til fremstilling af metal-silicoaluminophosphat-molekylsigten ifølge krav 1, der indbefatter følgende trin: (1) en metalkilde, en siliciumkilde, en aluminiumkilde, en phosphorkilde, et overfladeaktivt middel, en template og deioniseret vand blandes ensartet ved omrøring, og en udgangsgelblanding med følgende molforhold opnås: Me/Al203 = 0,01-1,0; S1O2/AI2O3 = 0,01-2,0; P2O5/AI2O3 = 0,5-2,0; H2O/AI2O3 = 21-200; S/AI2O3 = 0,01-0,5; S repræsenterer mindst ét overfladeaktivt middel; R/ AI2O3, = 0,5-5,5; R er diethylamin, en blanding af diethylamin og triethylamin, en blanding af diethylamin og morpholin eller en blanding af diethylamin og tetraethylammoniumhydroxid; hvor i trinnet (1) udgangsgelblandingen opnås ved følgende trin: blanding af 2/3 af det deioniserede vand med phosphorsyre; tilsætning af metalkilden og omrøring for ensartet blanding; tilsætning af aluminiumkilde og omrøring for ensartet blanding; tilsætning af siliciumkilden; tilsætning af opløsningen af det overfladeaktive middel i den resterende 1/3 af det deioniserede vand og omrøring i mindst 1 time; tilsætning af organisk amin-template og omrøring i mindst 1 time for at opnå udgangsgelblandingen; (2) udgangsgelblandingen overføres i en syntetisk kedel, forsegles og opvarmes derefter til krystalliseringstemperatur, og krystalliseres i rotationstilstande; hvor krystalliseringstemperaturen er 155-230 °C, og krystalliseringstiden er 1-72 timer; (3) efter afslutning af krystalliseringen vaskes og tørres det faste krystalprodukt for at opnå metal-silicoaluminophosphat-molekylsigten med RHO-skeletstruktur.
6. Fremgangsmåde ifølge krav 5, kendetegnet ved, at siliciumkildcn er en eller flere siliciumkilder udvalgt ffa gruppen bestående af siliciumdioxidopløsning, silieagel, aktiv siliciumdioxid og orthosilicater; aluminiumkilden er én eller flere aluminiumkilder udvalgt fra gruppen bestående af aluminiumsalte, aktiveret aluminiumdioxid, aluminiumalkoxid og pseudobøhmit; phosphorkilden er én eller flere phosphorkilder udvalgt fra gruppen bestående af phosphorsyre, phosphat, organiske phosphorforbindelser og phosphoroxider; det overfladeaktive middel er ét eller flere overfladeaktive midler udvalgt fra gruppen bestående af dodecyltrimethylammoniumchlorid, dodecyltrimethylamminiumbromid, trid ecyltrimethylammoniumchlorid, trid ecyltrimethylammoniumbromid, tetradecyltrimethylammoniumchlorid, tetradecyltrimethylammoniumbromid, pentadecyltrimethylammoniumchlorid, pentadecyltrimethylammoniumbromid, hexadecyltrimethylammoniumbromid, hexadecyltrimethylammoniumchlorid, dimethylhexadecyl [3-trimethylsilylpropyl]ammoniumchlorid, dimethyloctadecyl [3-trimethylsilylpropyl] ammoniumchlorid og hexadecyl(trimethoxy)silan.
7. Fremgangsmåde ifølge krav 5, kendetegnet ved, at metalkilden er én eller flere metalkilder udvalgt fra gruppen bestående af oxider, uorganiske salte og organiske salte af vanadium, kobber, molybden, zirconium, cobalt, mangan, magnesium, jern, nikkel eller zink; og metalkilden er fortrinsvis én eller flere metalkilder udvalgt fra gruppen bestående af oxider, uorganiske salte og organiske salte af kobber, cobalt, mangan, magnesium, jern, nikkel eller zink; og metalkilden er endvidere fortrinsvis én eller flere metalkilder udvalgt fra gruppen bestående af oxider, uorganiske salte og organiske salte af kobber, cobalt, mangan, magnesium eller zink.
8. Fremgangsmåde ifølge krav 5, kendetegnet ved, at metalkilden er én eller flere metalkilder udvalgt fra gruppen bestående af oxider, uorganiske salte og organiske salte af kobber, cobalt, mangan, magnesium, jern, nikkel eller zink;
9. Fremgangsmåde ifølge krav 5, kendetegnet ved, at metalkilden er én eller flere metalkilder udvalgt fra gruppen bestående af oxider, uorganiske salte og organiske salte af kobber, cobalt, mangan, magnesium eller zink.
10. Fremgangsmåde ifølge krav 5, kendetegnet ved, at molforholdet mellem Me og AI2O3 i trinnet (1) cr 0,01-0,5.
11. Fremgangsmåde ifølge krav 5, kendetegnet ved, at molforholdet mellem Me og AI2O3 i trinnet (1) er 0,01-0,35.
12. Fremgangsmåde ifølge krav 5, kendetegnet ved, at molforholdet mellem S og AI2O3 i trinnet (1) er 0,05-0,35.
13. Fremgangsmåde ifølge krav 5, kendetegnet ved, at molforholdet mellem R og AI2O3 i trinnet (1) er 1,0-4,0.
14. Fremgangsmåde ifølge krav 5, kendetegnet ved, at R i trinnet (1) er en blanding af diethylamin og triethylamin, en blanding af diethylamin og morpholin eller en blanding af diethylamin og tetraethylammoniumhydroxid; hvor molforholdet af diethylamin i blandingen er mere end 70 %.
15. Fremgangsmåde ifølge krav 5, kendetegnet ved, at krystalliseringstemperaturen i trin (2) er 170-215 °C, og krystalliseringstiden er 2-48 timer.
16. Katalysator til syrekatalyseret reaktion, der opnås ved kalcinering af mindst én af metal-silicoaluminophosphat-molekylsigtene ifølge kravene 1-4 ved 400-700 °C i luften.
17. Gasabsorber, der opnås ved kalcinering af mindst én af metal-silicoaluminophosphat-molekylsigtene ifølge kravene 1-4 ved 400-700 °C i luften.
18. Katalysator til selektiv oxideringsreaktion, der opnås ved kalcinering af mindst én af metal-silicoaluminophosphat-molekylsigtene ifølge kravene 1-4 ved 400-700 °C i luften.
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| PCT/CN2012/076625 WO2013181833A1 (zh) | 2012-06-08 | 2012-06-08 | 具有rho骨架结构的金属磷酸硅铝分子筛及其制备方法 |
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| US9499409B2 (en) * | 2012-06-08 | 2016-11-22 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Metal silicoaluminophosphate molecular sieve with RHO framework structure, and method for preparing the same |
| GB2540832B (en) * | 2015-02-20 | 2019-04-17 | Johnson Matthey Plc | Bi-metal molecular sieve catalysts |
| CN106276945B (zh) * | 2015-06-10 | 2018-05-18 | 中国科学院大连化学物理研究所 | 一种具有中、微孔复合孔道结构的rho-sapo分子筛 |
| WO2017205023A1 (en) * | 2016-05-25 | 2017-11-30 | Uop Llc | HIGH CHARGE DENSITY METALLOALUMINOPHOSPHOSILICATE MOLECULAR SIEVES MeAPSO-82 |
| CN106745035B (zh) * | 2017-03-17 | 2019-04-05 | 中触媒新材料股份有限公司 | 一种多级孔ssz-13分子筛及其合成方法和应用 |
| CN111013649B (zh) * | 2018-10-10 | 2022-07-12 | 中国石油化工股份有限公司 | Ni-SAPO-34分子筛的制备方法、制备的分子筛及其用途 |
| CN111099607B (zh) * | 2018-10-25 | 2023-04-07 | 中国石油化工股份有限公司 | 掺杂硅的磷铝酸盐和它的合成方法 |
| CN111099637B (zh) * | 2018-10-25 | 2023-03-03 | 中国石油化工股份有限公司 | 硅磷铝分子筛及其制备方法 |
| CN110560146A (zh) * | 2019-09-18 | 2019-12-13 | 广东工业大学 | 一种双金属mel分子筛及其制备方法和应用 |
| CN111592009B (zh) * | 2020-06-04 | 2023-09-12 | 南京工业大学 | 一种沸石分子筛的制备方法及其应用 |
| CN114477222B (zh) * | 2020-10-23 | 2023-04-11 | 中国石油化工股份有限公司 | 硅硼分子筛、分子筛组合物及其制备方法 |
| CN112844445B (zh) * | 2021-02-03 | 2022-05-10 | 中国石油大学(北京) | Silicalite-1分子筛微孔孔道限域的ZnCo基双金属催化剂的制备与应用 |
| CN113318782B (zh) * | 2021-05-28 | 2022-05-17 | 江西农业大学 | 一种富锰的Mn-SAPO-18分子筛催化剂的制备方法及其用途 |
| CN114031092B (zh) * | 2021-12-16 | 2023-03-24 | 中节能万润股份有限公司 | 一种sapo-20分子筛的制备方法 |
| CN115283007B (zh) * | 2022-08-25 | 2024-05-24 | 中山大学 | 铂金属纳米团簇ha分子筛的制备及其在1,2,3,4-四氢喹啉合成中的应用 |
| CN116422289B (zh) * | 2023-04-07 | 2024-01-12 | 东北石油大学 | 一种从炼厂气中脱除n2的分子筛及其制备方法和应用 |
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| US5925586A (en) * | 1996-12-31 | 1999-07-20 | Exxon Chemical Patents, Inc. | Phosphorus modified small pore molecular sieve catalysts, and their use in the production of light olefins |
| JP4174634B2 (ja) * | 1997-12-26 | 2008-11-05 | 三菱瓦斯化学株式会社 | シリカ変性シリコアルミノホスフェート触媒、その製造方法及びそれを用いるメチルアミン類等の製造方法 |
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| CN1108870C (zh) * | 1999-12-29 | 2003-05-21 | 中国科学院大连化学物理研究所 | MeAPSO－56分子筛及其合成方法 |
| CN1108869C (zh) * | 1999-12-29 | 2003-05-21 | 中国科学院大连化学物理研究所 | MeAPSO－35分子筛及其合成方法 |
| CN1108868C (zh) * | 1999-12-29 | 2003-05-21 | 中国科学院大连化学物理研究所 | MeAPSO－18分子筛及其合成方法 |
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| MY179762A (en) * | 2007-03-26 | 2020-11-12 | Pq Corp | Novel microporous crystalline material comprising a molecular sieve or zeolite having an 8-ring pore opening structure and methods of making and using same |
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| US9499409B2 (en) * | 2012-06-08 | 2016-11-22 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Metal silicoaluminophosphate molecular sieve with RHO framework structure, and method for preparing the same |
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| AU2012381962A1 (en) | 2014-12-11 |
| EP2860158B1 (en) | 2017-08-02 |
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| EP2860158A1 (en) | 2015-04-15 |
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