JP5823295B2 - Uzm−35アルミノシリケートゼオライト、uzm−35の製造方法及びそれを用いる方法 - Google Patents
Uzm−35アルミノシリケートゼオライト、uzm−35の製造方法及びそれを用いる方法 Download PDFInfo
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- JP5823295B2 JP5823295B2 JP2011530097A JP2011530097A JP5823295B2 JP 5823295 B2 JP5823295 B2 JP 5823295B2 JP 2011530097 A JP2011530097 A JP 2011530097A JP 2011530097 A JP2011530097 A JP 2011530097A JP 5823295 B2 JP5823295 B2 JP 5823295B2
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- zeolite
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims description 60
- 239000010457 zeolite Substances 0.000 title claims description 38
- 229910021536 Zeolite Inorganic materials 0.000 title claims description 33
- 238000000034 method Methods 0.000 title claims description 25
- 229910000323 aluminium silicate Inorganic materials 0.000 title description 24
- 239000000203 mixture Substances 0.000 claims description 25
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- 239000011541 reaction mixture Substances 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 150000001768 cations Chemical class 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 239000004215 Carbon black (E152) Substances 0.000 claims description 9
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 9
- 238000002441 X-ray diffraction Methods 0.000 claims description 9
- 229910052733 gallium Inorganic materials 0.000 claims description 9
- 229930195733 hydrocarbon Natural products 0.000 claims description 9
- 150000002430 hydrocarbons Chemical class 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- -1 dimethyldipropylammonium cation Chemical class 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910017090 AlO 2 Inorganic materials 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 150000004679 hydroxides Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 claims description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 239000008119 colloidal silica Substances 0.000 claims description 2
- 229910000373 gallium sulfate Inorganic materials 0.000 claims description 2
- SBDRYJMIQMDXRH-UHFFFAOYSA-N gallium;sulfuric acid Chemical compound [Ga].OS(O)(=O)=O SBDRYJMIQMDXRH-UHFFFAOYSA-N 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims 1
- FYKIGFSMRYURSB-UHFFFAOYSA-N CCC[N+](C)(C)CCC.N Chemical compound CCC[N+](C)(C)CCC.N FYKIGFSMRYURSB-UHFFFAOYSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims 1
- 239000012084 conversion product Substances 0.000 claims 1
- 229910021485 fumed silica Inorganic materials 0.000 claims 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims 1
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- 239000000047 product Substances 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 14
- 238000005119 centrifugation Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 239000012265 solid product Substances 0.000 description 11
- OSSXLTCIVXOQNK-UHFFFAOYSA-M dimethyl(dipropyl)azanium;hydroxide Chemical compound [OH-].CCC[N+](C)(C)CCC OSSXLTCIVXOQNK-UHFFFAOYSA-M 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000000921 elemental analysis Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- 230000029936 alkylation Effects 0.000 description 4
- 238000005804 alkylation reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000004517 catalytic hydrocracking Methods 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- GSBKRFGXEJLVMI-UHFFFAOYSA-N Nervonyl carnitine Chemical compound CCC[N+](C)(C)C GSBKRFGXEJLVMI-UHFFFAOYSA-N 0.000 description 3
- 150000001342 alkaline earth metals Chemical class 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- FIVJMCNNMIGYRO-UHFFFAOYSA-N bis(2-hydroxyethyl)-dimethylazanium Chemical compound OCC[N+](C)(C)CCO FIVJMCNNMIGYRO-UHFFFAOYSA-N 0.000 description 3
- IUNCEDRRUNZACO-UHFFFAOYSA-N butyl(trimethyl)azanium Chemical compound CCCC[N+](C)(C)C IUNCEDRRUNZACO-UHFFFAOYSA-N 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 3
- 229960001231 choline Drugs 0.000 description 3
- WQHRRUZRGXLCGL-UHFFFAOYSA-N dimethyl(dipropyl)azanium Chemical compound CCC[N+](C)(C)CCC WQHRRUZRGXLCGL-UHFFFAOYSA-N 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- MXTMXRYBYWOAGX-UHFFFAOYSA-N dimethyl(diphenyl)azanium Chemical compound C=1C=CC=CC=1[N+](C)(C)C1=CC=CC=C1 MXTMXRYBYWOAGX-UHFFFAOYSA-N 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 150000002892 organic cations Chemical class 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000010555 transalkylation reaction Methods 0.000 description 2
- WKBPZYKAUNRMKP-UHFFFAOYSA-N 1-[2-(2,4-dichlorophenyl)pentyl]1,2,4-triazole Chemical compound C=1C=C(Cl)C=C(Cl)C=1C(CCC)CN1C=NC=N1 WKBPZYKAUNRMKP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical class [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 150000003842 bromide salts Chemical class 0.000 description 1
- WRMFBHHNOHZECA-UHFFFAOYSA-N butan-2-olate Chemical compound CCC(C)[O-] WRMFBHHNOHZECA-UHFFFAOYSA-N 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000020335 dealkylation Effects 0.000 description 1
- 238000006900 dealkylation reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- ZJHQDSMOYNLVLX-UHFFFAOYSA-N diethyl(dimethyl)azanium Chemical compound CC[N+](C)(C)CC ZJHQDSMOYNLVLX-UHFFFAOYSA-N 0.000 description 1
- JQDCIBMGKCMHQV-UHFFFAOYSA-M diethyl(dimethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(C)CC JQDCIBMGKCMHQV-UHFFFAOYSA-M 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- KHBDINVATPZDSQ-UHFFFAOYSA-M dimethyl(dipropyl)azanium;bromide Chemical compound [Br-].CCC[N+](C)(C)CCC KHBDINVATPZDSQ-UHFFFAOYSA-M 0.000 description 1
- WOYQCKODTASHPN-UHFFFAOYSA-M dimethyl(dipropyl)azanium;chloride Chemical compound [Cl-].CCC[N+](C)(C)CCC WOYQCKODTASHPN-UHFFFAOYSA-M 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- KVFVBPYVNUCWJX-UHFFFAOYSA-M ethyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(C)C KVFVBPYVNUCWJX-UHFFFAOYSA-M 0.000 description 1
- YOMFVLRTMZWACQ-UHFFFAOYSA-N ethyltrimethylammonium Chemical compound CC[N+](C)(C)C YOMFVLRTMZWACQ-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000008241 heterogeneous mixture Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 150000004694 iodide salts Chemical class 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VFOJFWOVDZGATC-UHFFFAOYSA-N methyl(tripropyl)azanium Chemical compound CCC[N+](C)(CCC)CCC VFOJFWOVDZGATC-UHFFFAOYSA-N 0.000 description 1
- 150000005673 monoalkenes Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- LXPCOISGJFXEJE-UHFFFAOYSA-N oxifentorex Chemical compound C=1C=CC=CC=1C[N+](C)([O-])C(C)CC1=CC=CC=C1 LXPCOISGJFXEJE-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- OSBSFAARYOCBHB-UHFFFAOYSA-N tetrapropylammonium Chemical compound CCC[N+](CCC)(CCC)CCC OSBSFAARYOCBHB-UHFFFAOYSA-N 0.000 description 1
- FBEVECUEMUUFKM-UHFFFAOYSA-M tetrapropylazanium;chloride Chemical compound [Cl-].CCC[N+](CCC)(CCC)CCC FBEVECUEMUUFKM-UHFFFAOYSA-M 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- 239000011031 topaz Substances 0.000 description 1
- 229910052853 topaz Inorganic materials 0.000 description 1
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 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
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/46—Other types characterised by their X-ray diffraction pattern and their defined composition
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/06—Aluminium compounds
- C07F5/069—Aluminium compounds without C-aluminium linkages
-
- 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
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
-
- 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
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/04—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
-
- 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
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/06—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis
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Description
Mm n+R+ rAl1−xExSiyOz
(式中、Mはカリウム及びナトリウム交換性カチオンの組合せを表し;Rはジメチルジプロピルアンモニウムのような一価有機アンモニウムカチオンであり;Eはガリウムのような骨格元素である)によって表される。
Mm +R+ rAl1−xExSiyOz
(式中、Mはカリウム及びナトリウム交換性カチオンの組合せを表し;mは(Al+E)に対するMのモル比であり、0.05〜3の範囲であり;Rは、ジメチルジプロピルアンモニウム(DMDPA+)、コリン、エチルトリメチルアンモニウム(ETMA+)、ジエチルジメチルアンモニウム(DEDMA+)、トリメチルプロピルアンモニウム、トリメチルブチルアンモニウム、ジメチルジエタノールアンモニウム、テトラエチルアンモニウム(TEA+)、テトラプロピルアンモニウム(TPA+)、メチルトリプロピルアンモニウム、及びこれらの混合物からなる群から選択される一価有機アンモニウムカチオンであり;rは(Al+E)に対するRのモル比であり、0.25〜2.0の値を有し;Eは、ガリウム、鉄、ホウ素、及びこれらの混合物からなる群から選択される元素であり;xはEのモル分率であり、0〜1.0の値を有し;yは(Al+E)に対するSiのモル比であり、2より大きく12までの範囲であり;zは(Al+E)に対するOのモル比であり、等式:
z=(m+r+3+4・y)/2
によって定められる値を有する)
によって表される実験組成を有し、
少なくとも、表A:
aM2O:bR2/pO:1−cAl2O3:cE2O3:dSiO2:eH2O
(ここで、aは0.05〜1.25の値を有し;bは1.5〜40の値を有し;cは0〜1.0の値を有し;dは4〜40の値を有し;eは25〜4000の値を有する)
の組成を有する反応混合物を形成し;反応混合物を、150℃〜200℃又は165℃〜185℃の温度において、ゼオライトを形成するのに十分な時間加熱する;ことを含む。
Mm +R+ rAl1−xExSiyOz
(式中、Mはカリウム及びナトリウム交換性カチオンの組合せを表す)
によって表される実験組成を有する。Rは一価有機アンモニウムカチオンであり、その例としてはジメチルジプロピルアンモニウムカチオン(DMDPA+)、コリン[(CH3)3N(CH2)2OH]+、ETMA+、DEDMA+、トリメチルプロピルアンモニウム、トリメチルブチルアンモニウム、ジメチルジエタノールアンモニウム、メチルトリプロピルアンモニウム、TEA+、TPA+、及びこれらの混合物が挙げられ(しかしながらこれらに限定されない);rは(Al+E)に対するRのモル比であり、0.25〜2.0の範囲であり、一方、mは(Al+E)に対するMのモル比であり、0.05〜3の範囲である。(Al+E)に対するケイ素の比はyによって表され、2〜30の範囲である。Eは、4面体配位の元素であり、骨格内に存在しており、ガリウム、鉄、及びホウ素からなる群から選択される。Eのモル分率はxによって表され、0〜1.0の値を有し;一方、zは(Al+E)に対するOのモル比であり、等式:
z=(m・n+r+3+4・y)/2
によって与えられる。Mが1種類のみの金属である場合には、加重平均価数はその1種類の金属の価数、即ち+1又は+2である。しかしながら、1種類より多いM金属が存在する場合には、全量は
aM2O:bR2/pO:1−cAl2O3:cE2O3:dSiO2:eH2O
(ここで、aは0.05〜1.25の範囲であり;bは1.5〜40の範囲であり;cは0〜1.0の範囲であり;dは4〜40の範囲であり;eは25〜4000の範囲である)
によって示すことができる。アルコキシドを用いる場合には、アルコール加水分解生成物を除去するための蒸留又は蒸発工程を含ませることが好ましい。反応混合物は、密封した反応容器内、自生圧下で、150℃〜200℃、165℃〜185℃、又は170℃〜180℃の温度において、1日間〜3週間の間、好ましくは5日間〜12日間の間反応させる。結晶化が完了した後、濾過又は遠心分離のような手段によって固体生成物を不均一混合物から単離し、次に脱イオン水で洗浄し、空気中、雰囲気温度乃至100℃において乾燥する。場合によっては、ゼオライトの形成を促進するためにUZM−35種晶を反応混合物に加えることができることを指摘しなければならない。
z’=(a・n+3+4・y’)/2
によって定められる値を有する)
によって示される。
[0027]幾つかの場合においては、合成した生成物の純度は、そのX線粉末回折パターンを参照して評価することができる。したがって、例えば試料が純粋であると言及する場合には、試料のX線パターンが結晶質の不純物に起因する線を含まないことのみを意図し、アモルファス材料が存在しないことは意図しない。
[0029]まず16.64gの水酸化アルミニウム(27.78%Al)及び526.79gのジメチルジプロピルアンモニウムヒドロキシド(18.8%溶液)を激しく攪拌しながら混合することによって、アルミノシリケート溶液を調製した。十分に混合した後、252.98gのLudox AS-40(40%SiO2)を加えた。高速メカニカルスターラーを用いて反応混合物を更に1時間均一化し、100℃のオーブン内に一晩配置した。分析によって、得られたアルミノシリケート溶液が6.52重量%のSi及び0.64重量%のAlを含み、9.78のSi/Al比を与えたことが示された。
[0033]まず37.17gの水酸化アルミニウム(27.78%Al)及び1053.58gのジメチルジプロピルアンモニウムヒドロキシド(18.8%溶液)を激しく攪拌しながら混合することによって、アルミノシリケート反応溶液を調製した。十分に混合した後、505.96gのLudox AS-40(SiO2,40%)を加えた。高速メカニカルスターラーを用いて反応混合物を1時間均一化し、テフロン(登録商標)ボトル内に密封し、オーブン内において100℃に一晩配置した。分析によって、アルミノシリケート溶液が6.16重量%のSi及び0.67重量%のAlを含んでいた(Si/Al=8.83)ことが示された。
[0036]まず37.17gの水酸化アルミニウム(27.78%Al)及び1053.58gのジメチルジプロピルアンモニウムヒドロキシド(18.8%溶液)を激しく攪拌しながら混合することによって、アルミノシリケート反応溶液を調製した。十分に混合した後、505.96gのLudox AS-40(SiO2,40%)を加えた。高速メカニカルスターラーを用いて反応混合物を1時間均一化し、テフロン(登録商標)ボトル内に密封し、オーブン内において100℃に一晩配置した。分析によって、アルミノシリケート溶液が6.16重量%のSi及び0.67重量%のAlを含んでいた(Si/Al=8.83)ことが示された。
[0039]本実施例は、UZM−35材料の変性を示す。UZM−35試料(Si/Al=7.57)の10gの部分を、窒素雰囲気中において、3℃/分で540℃に昇温し、その温度で更に1時間保持してか焼し、その後雰囲気を空気に変えて更に9時間か焼を継続した。120gの脱イオン水中に、まず2gのHNO3(69%)を希釈し、次に10gのNH4NO3を溶解することによって溶液を調製した。この溶液を75℃に加熱し、その後、か焼したUZM−35を加えた。スラリーを75℃において1時間攪拌した。濾過によって生成物を単離し、脱イオン水で洗浄し、100℃において12時間乾燥させた。
[0041]本実施例はUZM−35材料の変性を示す。UZM−35試料(Si/Al=7.57)の20gの部分を、窒素雰囲気下において、3℃/分で560℃に昇温し、その温度に1時間保持することによってか焼し、その後雰囲気を空気に変えて更に9時間か焼を継続した。これとは別に、490gの脱イオン水中に20gのNH4NO3を溶解することによって溶液を調製した。溶液を75℃に加熱し、その後、か焼したUZM−35を加えた。スラリーを75℃において1時間攪拌した。濾過によって生成物を単離し、脱イオン水で洗浄し、100℃において12時間乾燥させた。
[0043]まず37.17gの水酸化アルミニウム(27.78%Al)及び1053.58gのジメチルジプロピルアンモニウムヒドロキシド(18.8%溶液)を激しく攪拌しながら混合することによって、アルミノシリケート溶液を調製した。十分に混合した後、505.96gのLudox AS-40(40%SiO2)を加えた。高速メカニカルスターラーを用いて反応混合物を更に1時間均一化し、100℃のオーブン内に一晩配置した。分析によって、得られたアルミノシリケート溶液が6.16重量%のSi及び0.67重量%のAlを含み、8.83のSi/Al比を与えたことが示された。
[0046]まず、37.17の水酸化アルミニウム(27.78%Al)及び1053.58gのジメチルジプロピルアンモニウムヒドロキシド(18.8%溶液)を激しく攪拌しながら混合することによって、アルミノシリケート溶液を調製した。十分に混合した後、505.96gのLudox AS-40(40%SiO2)を加えた。高速メカニカルスターラーを用いて反応混合物を更に1時間均一化し、100℃のオーブン内に一晩配置した。分析によって、得られたアルミノシリケート溶液が6.16重量%のSi及び0.67重量%のAlを含み、8.83のSi/Al比を与えたことが示された。
Claims (9)
- 少なくともAlO2及びSiO2の4面体単位の三次元骨格、並びに合成したままの形態で且つ無水ベースで実験式:
Mm +RrAl1−xExSiyOz
(式中、Mはカリウム及びナトリウム交換性カチオンの組合せを表し;mは(Al+E)に対するMのモル比であり、0.05〜3の範囲であり;Rは一価ジメチルジプロピルアンモニウムカチオンであり;rは(Al+E)に対するRのモル比であり、0.25〜2.0の値を有し;Eは、ガリウム、鉄、ホウ素、及びこれらの混合物からなる群から選択される元素であり;xはEのモル分率であり、0〜1.0の値を有し;yは(Al+E)に対するSiのモル比であり、2より大きく12までの範囲であり;zは(Al+E)に対するOのモル比であり、等式:
z=(m+r+3+4・y)/2
によって定められる値を有する)
によって表される実験組成を有し、
少なくとも、表A:
- xが0である、請求項1に記載のゼオライト。
- 少なくともAlO2及びSiO2の4面体単位の三次元骨格、並びに合成したままの形態で且つ無水ベースで実験式:
Mm +RrAl1−xExSiyOz
(式中、Mはカリウム及びナトリウム交換性カチオンの組合せを表し;mは(Al+E)に対するMのモル比であり、0.05〜3の範囲であり;Rは一価ジメチルジプロピルアンモニウムカチオンであり;rは(Al+E)に対するRのモル比であり、0.25〜2.0の値を有し;Eは、ガリウム、鉄、ホウ素、及びこれらの混合物からなる群から選択される元素であり;xはEのモル分率であり、0〜1.0の値を有し;yは(Al+E)に対するSiのモル比であり、2より大きく12までの範囲であり;zは(Al+E)に対するOのモル比であり、等式:
z=(m+r+3+4・y)/2
によって定められる値を有する)
によって表される実験組成を有し、
少なくとも、表A:
M、R、Al、Si、及び場合によってはEの反応性源を含み、酸化物のモル比で表して
aM2O:bR2/pO:1−cAl2O3:cE2O3:dSiO2:eH2O
(ここで、aは0.05〜1.25の値を有し;bは1.5〜40の値を有し;cは0〜1.0の値を有し;dは4〜40の値を有し;eは25〜4000の値を有する)
の組成を有する反応混合物を形成し;反応混合物を、150℃〜200℃の温度において、ゼオライトを形成するのに十分な時間加熱する;ことを含む上記方法。 - Mの源が、ハロゲン化物塩、硝酸塩、酢酸塩、水酸化物、硫酸塩、及びこれらの混合物からなる群から選択される、請求項3に記載の方法。
- Eの源が、アルカリホウ酸塩、ホウ酸、沈殿オキシ水酸化ガリウム、硫酸ガリウム、硫酸第2鉄、塩化第2鉄、及びこれらの混合物からなる群から選択される、請求項3に記載の方法。
- アルミニウム源が、アルミニウムイソプロポキシド、アルミニウムsec−ブトキシド、沈殿アルミナ、Al(OH)3、アルミニウム金属、及びアルミニウム塩からなる群から選択され、ケイ素源が、テトラエチルオルトシリケート、ヒュームドシリカ、コロイダルシリカ、及び沈殿シリカからなる群から選択される、請求項3に記載の方法。
- 反応混合物を150℃〜185℃の温度において1日間〜3週間の間反応させる、請求項3に記載の方法。
- UZM−35種晶を反応混合物に加えることを更に含む、請求項3に記載の方法。
- 炭化水素流を、少なくともAlO2及びSiO2の4面体単位の三次元骨格、並びに合成したままの形態で且つ無水ベースで実験式:
Mm +RrAl1−xExSiyOz
(式中、Mはカリウム及びナトリウム交換性カチオンの組合せを表し;mは(Al+E)に対するMのモル比であり、0.05〜3の範囲であり;Rは一価有機アンモニウムジメチルジプロピルアンモニウムカチオンであり;rは(Al+E)に対するRのモル比であり、0.25〜2.0の値を有し;Eは、ガリウム、鉄、ホウ素、及びこれらの混合物からなる群から選択される元素であり;xはEのモル分率であり、0〜1.0の値を有し;yは(Al+E)に対するSiのモル比であり、2より大きく12までの範囲であり;zは(Al+E)に対するOのモル比であり、等式:
z=(m+r+3+4・y)/2
によって定められる値を有する)
によって表される実験組成を有し、
少なくとも、表A:
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PCT/US2009/057062 WO2010039431A2 (en) | 2008-09-30 | 2009-09-16 | Uzm-35 aluminosilicate zeolite, method of preparation and processes using uzm-35 |
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US8247631B2 (en) | 2010-06-21 | 2012-08-21 | Uop Llc | Process for catalytic cracking of hydrocarbons using UZM-35 |
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US8597611B2 (en) * | 2010-07-01 | 2013-12-03 | Uop Llc | UZM-45 aluminosilicate zeolite, method of preparation and processes using UZM-45 |
CN103874656B (zh) | 2011-10-12 | 2016-09-07 | 埃克森美孚研究工程公司 | Mse骨架型分子筛的合成 |
EP2766118B1 (en) * | 2011-10-12 | 2017-03-08 | ExxonMobil Research and Engineering Company | Synthesis of mse-framework type molecular sieves |
JP6134335B2 (ja) * | 2011-12-22 | 2017-05-24 | ユーオーピー エルエルシー | Uzm−39アルミケイ酸塩ゼオライト |
JP6106759B2 (ja) | 2012-11-16 | 2017-04-05 | エクソンモービル リサーチ アンド エンジニアリング カンパニーExxon Research And Engineering Company | Mseフレームワーク型モレキュラーシーブの合成 |
US9211530B2 (en) | 2012-12-14 | 2015-12-15 | Uop Llc | Low silicon SAPO-42 and method of making |
US8884056B2 (en) | 2012-12-14 | 2014-11-11 | Uop Llc | Anaerobic conversion of 4-carboxybenzaldehyde in ionic liquids |
US9233856B2 (en) * | 2013-04-20 | 2016-01-12 | Uop Llc | Use of zeolitic materials for removing mercury (+2) ions from liquid streams |
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EP3317227B1 (en) * | 2015-06-30 | 2021-03-24 | Uop Llc | Uzm-53, an mtt zeolite |
JP6734692B2 (ja) | 2016-04-26 | 2020-08-05 | 三井金属鉱業株式会社 | Mse型ゼオライトの製造方法 |
KR101795404B1 (ko) | 2016-05-18 | 2017-11-08 | 현대자동차 주식회사 | 촉매 및 촉매의 제조 방법 |
KR101878547B1 (ko) * | 2016-05-19 | 2018-07-16 | 포항공과대학교 산학협력단 | 제올라이트를 이용한 에틸렌 전환 방법 |
US10272420B2 (en) * | 2016-10-06 | 2019-04-30 | Uop Llc | Composition of matter and structure of zeolite UZM-55 |
JP6749594B2 (ja) * | 2017-03-24 | 2020-09-02 | 国立大学法人横浜国立大学 | チタノシリケートの製造方法 |
CN108929342A (zh) * | 2018-08-20 | 2018-12-04 | 太原理工大学 | 一种介孔沸石模板剂及其制备方法和应用 |
US11897779B2 (en) | 2018-08-24 | 2024-02-13 | East China Normal University | Microporous aluminotitanosilicate crystalline zeolite, method of preparation and applications thereof |
CN111099612B (zh) * | 2018-10-25 | 2021-11-30 | 中国石油化工股份有限公司 | 分子筛scm-23、其合成方法及其用途 |
JP2024510925A (ja) * | 2021-03-02 | 2024-03-12 | ビーエーエスエフ コーポレーション | リン修飾uzm-35ゼオライト、それの調製方法、及び使用方法 |
CN113289673B (zh) * | 2021-06-02 | 2022-10-04 | 润和科华催化剂(上海)有限公司 | 一种异构化催化剂及其制备方法和应用 |
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CA2737615C (en) | 2015-01-06 |
JP2012504105A (ja) | 2012-02-16 |
MY152273A (en) | 2014-09-15 |
RU2011117314A (ru) | 2012-11-10 |
EP2328839A2 (en) | 2011-06-08 |
RU2500619C2 (ru) | 2013-12-10 |
MX2011003386A (es) | 2011-04-21 |
US20100081775A1 (en) | 2010-04-01 |
US7922997B2 (en) | 2011-04-12 |
CN102171146A (zh) | 2011-08-31 |
WO2010039431A3 (en) | 2010-06-10 |
WO2010039431A2 (en) | 2010-04-08 |
EP2328839B1 (en) | 2017-05-10 |
US20110178357A1 (en) | 2011-07-21 |
CA2737615A1 (en) | 2010-04-08 |
BRPI0919492A2 (pt) | 2019-09-24 |
EP2328839A4 (en) | 2012-05-30 |
KR20110081193A (ko) | 2011-07-13 |
CN102171146B (zh) | 2013-09-11 |
ES2629133T3 (es) | 2017-08-07 |
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