JP5973460B2 - 酸化物材料 - Google Patents
酸化物材料 Download PDFInfo
- Publication number
- JP5973460B2 JP5973460B2 JP2013543350A JP2013543350A JP5973460B2 JP 5973460 B2 JP5973460 B2 JP 5973460B2 JP 2013543350 A JP2013543350 A JP 2013543350A JP 2013543350 A JP2013543350 A JP 2013543350A JP 5973460 B2 JP5973460 B2 JP 5973460B2
- Authority
- JP
- Japan
- Prior art keywords
- ucb
- oxide material
- delamination
- zeolite
- mcm
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000000463 material Substances 0.000 title claims description 94
- 230000032798 delamination Effects 0.000 claims description 69
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 47
- 239000000203 mixture Chemical group 0.000 claims description 46
- 239000010457 zeolite Substances 0.000 claims description 44
- 239000012690 zeolite precursor Substances 0.000 claims description 38
- 229910021536 Zeolite Inorganic materials 0.000 claims description 36
- 239000011148 porous material Substances 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 7
- 238000002441 X-ray diffraction Methods 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000010936 titanium Chemical group 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical group [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical group [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 60
- 238000000034 method Methods 0.000 description 52
- 230000015572 biosynthetic process Effects 0.000 description 45
- 239000000047 product Substances 0.000 description 40
- 238000003786 synthesis reaction Methods 0.000 description 39
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 description 36
- FPGGTKZVZWFYPV-UHFFFAOYSA-M tetrabutylammonium fluoride Chemical compound [F-].CCCC[N+](CCCC)(CCCC)CCCC FPGGTKZVZWFYPV-UHFFFAOYSA-M 0.000 description 34
- -1 fluoride anions Chemical class 0.000 description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 25
- 230000008569 process Effects 0.000 description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 24
- 238000000634 powder X-ray diffraction Methods 0.000 description 24
- 239000007787 solid Substances 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 16
- 239000010410 layer Substances 0.000 description 16
- 238000001179 sorption measurement Methods 0.000 description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 14
- 238000000527 sonication Methods 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
- 238000001914 filtration Methods 0.000 description 13
- 239000007864 aqueous solution Substances 0.000 description 12
- 238000012512 characterization method Methods 0.000 description 12
- 239000000523 sample Substances 0.000 description 12
- 239000007789 gas Substances 0.000 description 11
- 230000020477 pH reduction Effects 0.000 description 11
- 238000001144 powder X-ray diffraction data Methods 0.000 description 11
- 239000002002 slurry Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000003960 organic solvent Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 8
- 238000005119 centrifugation Methods 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000002243 precursor Substances 0.000 description 8
- 238000003917 TEM image Methods 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 7
- 238000005096 rolling process Methods 0.000 description 7
- 230000008961 swelling Effects 0.000 description 7
- 229920006362 Teflon® Polymers 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910021485 fumed silica Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000011541 reaction mixture Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000004627 transmission electron microscopy Methods 0.000 description 5
- 238000004400 29Si cross polarisation magic angle spinning Methods 0.000 description 4
- 238000005004 MAS NMR spectroscopy Methods 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000004299 exfoliation Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- 239000004809 Teflon Substances 0.000 description 3
- 125000005210 alkyl ammonium group Chemical group 0.000 description 3
- HOPRXXXSABQWAV-UHFFFAOYSA-N anhydrous collidine Natural products CC1=CC=NC(C)=C1C HOPRXXXSABQWAV-UHFFFAOYSA-N 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- ZSIQJIWKELUFRJ-UHFFFAOYSA-N azepane Chemical compound C1CCCNCC1 ZSIQJIWKELUFRJ-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- UTBIMNXEDGNJFE-UHFFFAOYSA-N collidine Natural products CC1=CC=C(C)C(C)=N1 UTBIMNXEDGNJFE-UHFFFAOYSA-N 0.000 description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 3
- 239000012969 di-tertiary-butyl peroxide Substances 0.000 description 3
- 230000008034 disappearance Effects 0.000 description 3
- 229910001657 ferrierite group Inorganic materials 0.000 description 3
- 239000003517 fume Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 238000004375 physisorption Methods 0.000 description 3
- 238000002459 porosimetry Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- GFYHSKONPJXCDE-UHFFFAOYSA-N sym-collidine Natural products CC1=CN=C(C)C(C)=C1 GFYHSKONPJXCDE-UHFFFAOYSA-N 0.000 description 3
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 3
- DICGYDRHQMUZEA-UHFFFAOYSA-N 2,3-bis(2-methylpropyl)-1h-imidazol-3-ium;hydroxide Chemical compound [OH-].CC(C)CC=1NC=C[N+]=1CC(C)C DICGYDRHQMUZEA-UHFFFAOYSA-N 0.000 description 2
- 229910002483 Cu Ka Inorganic materials 0.000 description 2
- 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 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
- 238000007171 acid catalysis Methods 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 238000001116 aluminium-27 magic angle spinning nuclear magnetic resonance spectrum Methods 0.000 description 2
- 238000005280 amorphization Methods 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- DMEGYFMYUHOHGS-UHFFFAOYSA-N cycloheptane Chemical compound C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000010414 supernatant solution Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- FQUYSHZXSKYCSY-UHFFFAOYSA-N 1,4-diazepane Chemical compound C1CNCCNC1 FQUYSHZXSKYCSY-UHFFFAOYSA-N 0.000 description 1
- FTVFPPFZRRKJIH-UHFFFAOYSA-N 2,2,6,6-tetramethylpiperidin-4-amine Chemical compound CC1(C)CC(N)CC(C)(C)N1 FTVFPPFZRRKJIH-UHFFFAOYSA-N 0.000 description 1
- UWKQJZCTQGMHKD-UHFFFAOYSA-N 2,6-di-tert-butylpyridine Chemical compound CC(C)(C)C1=CC=CC(C(C)(C)C)=N1 UWKQJZCTQGMHKD-UHFFFAOYSA-N 0.000 description 1
- ORILYTVJVMAKLC-UHFFFAOYSA-N Adamantane Natural products C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 229910017855 NH 4 F Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- QXNDZONIWRINJR-UHFFFAOYSA-N azocane Chemical compound C1CCCNCCC1 QXNDZONIWRINJR-UHFFFAOYSA-N 0.000 description 1
- 238000003442 catalytic alkylation reaction Methods 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- NISGSNTVMOOSJQ-UHFFFAOYSA-N cyclopentanamine Chemical compound NC1CCCC1 NISGSNTVMOOSJQ-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000806 fluorine-19 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000000449 magic angle spinning nuclear magnetic resonance spectrum Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003791 organic solvent mixture Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 239000011135 tin Chemical group 0.000 description 1
- 238000005406 washing Methods 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
- 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
- B01J29/7038—MWW-type, e.g. MCM-22, ERB-1, ITQ-1, PSH-3 or SSZ-25
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
-
- 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
- B01J29/041—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
-
- 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
- B01J29/65—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38, as exemplified by patent documents US4046859, US4016245 and US4046859, respectively
-
- 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
-
- 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
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Description
材料。ゼオライト合成及び層間剥離で使用したすべての試薬は、試薬グレード品質のものであり、受領したままで使用した。N2ガス物理吸着に使用したUSYゼオライトは、Zeolyst Internationalから受領した(CBV760、60のSi/Al比)。TONゼオライトは、Chevron Energy Technology Companyで合成された。
塩化物を用いないMCM−22(P)の層間剥離。塩化テトラブチルアンモニウムを用いず、2倍のフッ化テトラブチルアンモニウムを用いたことを除いて、上述したものと同じ条件下で、MCM−22(P)の層間剥離を試みた。層間剥離は成功しなかった。図1を参照。
ERB−1の合成。ERB−1を文献の方法によって合成した。(Milliniら、Microporous Materials、(1995)、4巻、221頁)。水酸化ナトリウム(EMD Chemicals、97%、0.653g)及びピペリジン(Sigma Aldrich、99%、6.360g)を、脱イオン水(16.228g)中に溶解させた。ホウ酸(J.T.Baker、4.396g)を混合物に添加し、ホウ酸が完全に溶解するまで323Kで混合物全体を撹拌した。溶液を室温まで冷却した後、ヒュームドシリカ(Sigma Aldrich、3.300g)を1時間にわたって徐々に添加した。混合物全体をさらに5時間撹拌し、半分に分割した。各ゲルをテフロン(登録商標)で裏打ちされたオートクレーブ(Parr instrument、23mL)中に移した。各反応器をしっかりと密閉し、反応器を転がしながら、対流オーブン内で、448Kで7日間加熱した。7日間加熱した後、反応器を室温に冷却し、遠心分離によって生成物を分離した。分離した生成物を脱イオン水で徹底的に洗浄し、最後に313Kで一晩乾燥させた。合成ERB−1を特徴づける粉末X線回折(PXRD)パターン(図12中のパターンA)は、文献データと合致し、それぞれ3.4°及び6.8°で001及び002回折ピークを示す。これらのピークは、ERB−1のラメラ構造を表す。
材料。ゼオライト合成及び層間剥離で使用したすべての試薬は、試薬グレード品質のものであり、受領したままで使用した。
PREFERの層間剥離によるUCB−3の合成及び特徴づけ
N,N−ジメチルホルムアミド(4mL)中のPREFER(0.20g)、臭化セチルトリメチルアンモニウム(CTAB、0.22g)、フッ化テトラブチルアンモニウム(TBAF、0.34g)、塩化テトラブチルアンモニウム(TBACl、0.34g)の混合物を、密閉したPFAチューブ内で、373Kで16時間加熱した。16時間加熱した後、混合物を室温に冷却し、濾過によって固体を分離した。固体を脱イオン水で大規模に洗浄し、323Kで一晩乾燥させた。合成された材料をUCB−3と指定した。やはりPREFER層間剥離から生じる、UCB−2と比べたこの合成手順の利点は、酸性化工程も酸も必要とされないことである。
PREFERの層間剥離によるUCB−4の合成及び特徴づけ
N,N−ジメチルホルムアミド(4mL)中のPREFER(0.20g)、臭化セチルトリメチルアンモニウム(CTAB、0.22g)、フッ化テトラブチルアンモニウム(TBAF、0.34g)、塩化テトラブチルアンモニウム(TBACl、0.34g)の混合物を、密閉したPFAチューブ内で、373Kで16時間加熱した。室温に冷却した後、氷浴中で1時間、スラリーを超音波処理にかけた。次いで、固体を濾過によって分離し、DMF約50mLで洗浄した。濾過によって分離した後、固体を323Kで一晩乾燥させた。合成された材料をUCB−4と指定した。この合成は、UCB−3の合成と同様に、酸性化及び酸の使用の必要性を不要にするが、UCB−3と異なり、これは超音波処理を伴う。
Al−SSZ−70の合成
水酸化アルミニウム(Al2O3として53重量%、0.171g)、蒸留水(6.88g)、水酸化ジイソブチルイミダゾリウム溶液(0.50mmol/g、35.6g)、水酸化ナトリウム溶液(1N、8.89g)、及びヒュームドシリカ(5.50g)からなるゲルを、4つのポーションに分割した。23mLのテフロン(登録商標)で裏打ちされたオートクレーブ内で、423Kで転がしながら11日間、それぞれのゲルを加熱した。反応混合物を室温に冷却した後、固体を濾過によって分離し、その後、蒸留水で洗浄した。固体を353Kで一晩乾燥させた。
N,N−ジメチルホルムアミド(4mL)中のAl−SSZ−70(0.20g)、臭化セチルトリメチルアンモニウム(CTAB、0.22g)、フッ化テトラブチルアンモニウム(TBAF、0.34g)、塩化テトラブチルアンモニウム(TBACl、0.34g)の混合物を、密閉したPFAチューブ内で、373Kで16時間加熱した。室温に冷却した後、氷浴中で1時間、スラリーを超音波処理にかけた。次いで、固体を濾過によって分離し、DMF約50mLで洗浄した。濾過によって分離した後、固体を323Kで一晩乾燥させた。合成された材料をUCB−5と指定した。
B−SSZ−70の合成
ホウ酸(0.172g)、蒸留水(2.52g)、水酸化ジイソブチルイミダゾリウム溶液(0.48mmol/g、17.7g)、水酸化ナトリウム溶液(1N、4.20g)、及びヒュームドシリカ(2.60g)からなるゲルを、2つのポーションに分割した。23mLのテフロン(登録商標)で裏打ちされたオートクレーブ内で、423Kで17日間、転がしながらそれぞれのゲルを加熱した。反応混合物を室温に冷却した後、固体を濾過によって分離し、その後、蒸留水で洗浄した。固体を353Kで一晩乾燥させた。
N,N−ジメチルホルムアミド(4mL)中のB−SSZ−70(0.20g)、臭化セチルトリメチルアンモニウム(CTAB、0.22g)、フッ化テトラブチルアンモニウム(TBAF、0.34g)、塩化テトラブチルアンモニウム(TBACl、0.34g)の混合物を、密閉したPFAチューブ内で、373Kで16時間加熱した。室温に冷却した後、氷浴中で1時間、スラリーを超音波処理にかけた。次いで、固体を濾過によって分離し、DMF約50mLで洗浄した。濾過によって分離した後、固体を323Kで一晩乾燥させた。合成された材料をUCB−6と指定した。
Claims (13)
- 層状ゼオライト前駆体の少なくとも部分的な層間剥離を含み、非晶質シリカ相を欠き、式XO2及びY2O3の酸化物を含み、式中、Xは、四価の元素を表し、Yは三価の元素を表し、XとYの原子比が3超である、酸化物材料。
- 非晶質シリカ相を欠き、式XO 2 及びY 2 O 3 の酸化物を含み、式中、Xは、四価の元素を表し、Yは三価の元素を表し、XとYの原子比が3超である、層間剥離酸化物材料。
- 非晶質シリカ相を欠き、式XO 2 及びY 2 O 3 の酸化物を含み、式中、Xは、四価の元素を表し、Yは三価の元素を表し、XとYの原子比が3超である、層間剥離層状ゼオライト酸化物材料。
- Xがケイ素である、請求項1〜3のいずれか一項に記載の酸化物材料。
- XとYの前記原子比が200未満である、請求項4に記載の酸化物材料。
- XとYの前記原子比が100未満である、請求項4に記載の酸化物材料。
- Yがアルミニウムである、請求項4に記載の酸化物材料。
- Xが、ケイ素、ゲルマニウム、バナジウム、チタン、スズ、又はこれらの混合物であり、Yが、アルミニウム、ホウ素、鉄、クロム、チタン、ガリウム、セリウム、ランタン、サマリウム、及びこれらの混合物からなる群から選択される、請求項1〜3のいずれか一項に記載の酸化物材料。
- 骨格内にホスフェートも含有する、請求項8に記載の酸化物材料。
- 6〜10 2θ/度の範囲内のX線回折ピークの極大と、20〜30 2θ/度の範囲内のX線回折ピークの極大との相対強度比が0.50以下である、請求項1〜3のいずれか一項に記載の酸化物材料。
- Yがホウ素である、請求項1〜3のいずれか一項に記載の酸化物材料。
- 層間剥離ゼオライト材料UCB−1;UCB−2;UCB−3;UCB−4;UCB−5;又はUCB−6である、請求項1〜3のいずれか一項に記載の酸化物材料。
- 0.60cm3/g以下の、メソ細孔及びマクロ細孔を含む大細孔の細孔容積を有する、請求項1〜3のいずれか一項に記載の酸化物材料。
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US13/161,091 US9522390B2 (en) | 2010-12-10 | 2011-06-15 | Oxide materials and synthesis by fluoride/chloride anion promoted exfoliation |
PCT/US2011/063990 WO2012078900A1 (en) | 2010-12-10 | 2011-12-08 | Novel oxide material and synthesis by fluoride/chloride anion promoted exfoliation |
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US9296714B2 (en) * | 2012-02-07 | 2016-03-29 | Basf Se | Micropowder and molding containing a zeolitic material containing Ti and Zn |
BR112015008390B1 (pt) * | 2012-10-18 | 2021-11-03 | Basf Se | Processo para o pós-tratamento de um material zeolítico tendo uma estrutura de armação mww, material zeolítico tendo uma estrutura de armação mww e uso de um material zeolítico |
US9636669B2 (en) * | 2013-02-22 | 2017-05-02 | The Regents Of The University Of California | Zeolitic materials with heteroatom substitutions on external surface of lattice framework |
US9126190B2 (en) * | 2013-07-30 | 2015-09-08 | Chevron U.S.A. Inc. | Zeolite SSZ-70 having enhanced external surface area |
WO2015066539A1 (en) | 2013-11-01 | 2015-05-07 | Chevron U.S.A. Inc. | Delaminated zeolite catalyzed aromatic alkylation |
CN106536411B (zh) | 2014-06-06 | 2020-05-12 | 巴斯夫欧洲公司 | 具有mww骨架结构的含硼沸石的合成 |
WO2016040327A1 (en) | 2014-09-08 | 2016-03-17 | The Regents Of The University Of California | Highly active, selective, accessible, and robust zeolitic sn-baeyer-villiger oxidation catalyst |
US9738838B2 (en) * | 2014-10-22 | 2017-08-22 | Chevron U.S.A. Inc. | Hydroprocessing of hydrocarbons using delaminated zeolite supports as catalysts |
WO2016065035A1 (en) | 2014-10-22 | 2016-04-28 | Chevron U.S.A. Inc. | Hydrocarbon reactions using delaminated zeolite supports as catalysts |
US20160115397A1 (en) * | 2014-10-22 | 2016-04-28 | Chevron U.S.A. Inc. | Hydroprocessing of hydrocarbons using delaminated zeolite supports as catalysts |
US9783461B2 (en) * | 2014-11-04 | 2017-10-10 | Chevron U.S.A. Inc. | Olefin oligomerization using delaminated zeolite supports as catalyst |
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AU2011338335A1 (en) | 2013-05-23 |
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TWI542546B (zh) | 2016-07-21 |
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CA2821098A1 (en) | 2012-06-14 |
US9718049B2 (en) | 2017-08-01 |
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