DK2635527T3 - Fremgangsmåde til fremstilling af lille krystal SSZ-32 - Google Patents
Fremgangsmåde til fremstilling af lille krystal SSZ-32 Download PDFInfo
- Publication number
- DK2635527T3 DK2635527T3 DK11838459.3T DK11838459T DK2635527T3 DK 2635527 T3 DK2635527 T3 DK 2635527T3 DK 11838459 T DK11838459 T DK 11838459T DK 2635527 T3 DK2635527 T3 DK 2635527T3
- Authority
- DK
- Denmark
- Prior art keywords
- reaction mixture
- zeolite
- ssz
- reaction
- crystals
- Prior art date
Links
- 239000013078 crystal Substances 0.000 title claims description 45
- 238000000034 method Methods 0.000 title claims description 44
- 230000008569 process Effects 0.000 title claims description 21
- 238000002360 preparation method Methods 0.000 title description 11
- 239000011541 reaction mixture Substances 0.000 claims description 88
- 239000010457 zeolite Substances 0.000 claims description 76
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 63
- 229910021536 Zeolite Inorganic materials 0.000 claims description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 49
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 238000002425 crystallisation Methods 0.000 claims description 16
- 230000008025 crystallization Effects 0.000 claims description 16
- -1 hydroxide ions Chemical class 0.000 claims description 16
- 229910052681 coesite Inorganic materials 0.000 claims description 14
- 229910052906 cristobalite Inorganic materials 0.000 claims description 14
- 229910052682 stishovite Inorganic materials 0.000 claims description 14
- 229910052905 tridymite Inorganic materials 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052783 alkali metal Inorganic materials 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 238000002441 X-ray diffraction Methods 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 230000001627 detrimental effect Effects 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- HXGZXUVDQQOSAR-UHFFFAOYSA-M 1,3-di(propan-2-yl)imidazol-1-ium;hydroxide Chemical group [OH-].CC(C)N1C=C[N+](C(C)C)=C1 HXGZXUVDQQOSAR-UHFFFAOYSA-M 0.000 claims description 2
- 238000000196 viscometry Methods 0.000 claims 2
- LBRNWTDZIUYYAT-UHFFFAOYSA-M 1-methyl-3-propan-2-ylimidazol-1-ium;hydroxide Chemical group [OH-].CC(C)[N+]=1C=CN(C)C=1 LBRNWTDZIUYYAT-UHFFFAOYSA-M 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 33
- 230000015572 biosynthetic process Effects 0.000 description 28
- 238000003786 synthesis reaction Methods 0.000 description 26
- 239000000047 product Substances 0.000 description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 15
- 239000002184 metal Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 11
- 238000000634 powder X-ray diffraction Methods 0.000 description 10
- 230000035484 reaction time Effects 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 230000000875 corresponding effect Effects 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- 238000001354 calcination Methods 0.000 description 5
- 238000005342 ion exchange Methods 0.000 description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000004627 transmission electron microscopy Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 235000012211 aluminium silicate Nutrition 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 239000005995 Aluminium silicate Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 238000005216 hydrothermal crystallization Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 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 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 235000011128 aluminium sulphate Nutrition 0.000 description 1
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical group O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940077464 ammonium ion Drugs 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 229910001649 dickite Inorganic materials 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910001657 ferrierite group Inorganic materials 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910052621 halloysite Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000001889 high-resolution electron micrograph Methods 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052680 mordenite Inorganic materials 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910052605 nesosilicate Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004762 orthosilicates Chemical class 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 238000001139 pH measurement Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000000153 supplemental effect Effects 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000005406 washing Methods 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
- C01B39/50—Zeolites wherein inorganic bases or salts occlude channels in the lattice framework, e.g. sodalite, cancrinite, nosean, hauynite
-
- 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
- C01B39/48—Other types characterised by their X-ray diffraction pattern and their defined composition using at least one organic template directing agent
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Catalysts (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Claims (11)
1. Fremgangsmåde til fremstilling afen lille krystal SSZ-32-zeolit, omfattende (a) at fremstille en reaktionsblanding omfattende: (i) mindst en aktiv kilde til en oxid af silicium; (ii) mindst en aktiv kilde til en oxid af aluminium; (iii) mindst en aktiv kilde til et alkalimetal; (iv) hydroxidioner; og (v) et organisk templating-middel med strukturen:
hvor R er en Ci- til Cs-alkylgruppe, og A- er en anion, som ikke er skadelig for krystallisering af zeolitten; og (b) at holde reaktionsblandingen under betingelser, der er tilstrækkelige til dannelse af krystaller af zeolitten, hvor zeolitten fremstilles i fravær af en amin-bestanddel; hvor zeolitten har en krystallitstørrelse på 10 til 40 nanometer; hvor reaktionsblandingen har en sammensætning med hensyn til molforhold, der falder inden for nedenstående intervaller:
hvor M er en alkalimetalkation; og Q er det organiske templating-middel; og hvor betingelserne er tilstrækkelige til dannelse af krystaller af zeolitten og omfatter opvarmning af reaktionsblandingen ved en første temperatur på fra 175 °C til 190 °C i et tidsrum på fra 12 til 48 timer; og reduktion af den første temperatur af reaktionsblandingen til en anden temperatur på fra 140 °C til 170 °C i et tidsrum, der er egnet til dannelse af krystaller af zeolitten.
2. Fremgangsmåde ifølge krav 1, hvor molforholdet H2O/S1O2 er 15 til 20.
3. Fremgangsmåde ifølge krav 1, hvor den mindst ene aktive kilde til en oxid af silicium og den mindst ene aktive kilde til en oxid af aluminium er afledt af en fælles kilde.
4. Fremgangsmåde ifølge krav 1, hvor det organiske templating-middel er N-methyl-N'-isopropylimidazoliumhydroxid.
5. Fremgangsmåde ifølge krav 1, hvor det organiske templating-middel er N,N'-diisopropylimidazoliumhydroxid.
6. Fremgangsmåde ifølge krav 1, hvor zeolitten, i sin form som syntetiseret, har et molforhold mellem silica og alumina på 20 til mindre end 40.
7. Fremgangsmåde ifølge krav 1, hvor zeolitten har en krystal I itstørrelse på 12 til 20 nanometer.
8. Fremgangsmåde ifølge krav 1, hvor zeolitten, i sin kalcinerede form, har et røntgendiffraktionsmønster i det væsentlige som vist i følgende tabel:
9. Fremgangsmåde ifølge krav 1, yderligere omfattende at overvåge mindst en viskometri-parameter for reaktionsblandingen; og at bestemme et endepunkt.
10. Fremgangsmåde ifølge krav 9, hvor den mindst ene viskometri-parameter for reaktionsblandingen er udvalgt fra gruppen bestående af viskositet-forskydningshastighedsindeks, målt viskositet eller en kombination deraf.
11. Fremgangsmåde ifølge krav 9, hvor endepunktet bestemmes på basis af en ændring i målt viskositet af reaktionsblandingen, en ændring i pH-værdien af reaktionsblandingen eller en kombination deraf.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US12/940,776 US8545805B2 (en) | 2010-11-05 | 2010-11-05 | Method for preparing small crystal SSZ-32 |
| PCT/US2011/057225 WO2012061037A2 (en) | 2010-11-05 | 2011-10-21 | Method for preparing small crystal ssz-32 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DK2635527T3 true DK2635527T3 (da) | 2019-03-04 |
Family
ID=46019822
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DK11838459.3T DK2635527T3 (da) | 2010-11-05 | 2011-10-21 | Fremgangsmåde til fremstilling af lille krystal SSZ-32 |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US8545805B2 (da) |
| EP (1) | EP2635527B1 (da) |
| JP (1) | JP5822408B2 (da) |
| KR (1) | KR101886296B1 (da) |
| CN (1) | CN103153860A (da) |
| BR (1) | BR112013005114B1 (da) |
| CA (1) | CA2810594C (da) |
| DK (1) | DK2635527T3 (da) |
| ES (1) | ES2712742T3 (da) |
| MY (1) | MY159186A (da) |
| SG (1) | SG189466A1 (da) |
| WO (1) | WO2012061037A2 (da) |
| ZA (1) | ZA201301712B (da) |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8734758B2 (en) * | 2010-11-05 | 2014-05-27 | Chevron U.S.A. Inc. | Method for preparing molecular sieves |
| CN103420391B (zh) * | 2012-05-16 | 2015-08-12 | 中国石油化工股份有限公司 | 小晶粒sapo-34分子筛的制备方法 |
| JP6228013B2 (ja) * | 2013-02-13 | 2017-11-08 | Ｊｘｔｇエネルギー株式会社 | 潤滑油基油の製造方法 |
| US8999288B1 (en) * | 2013-09-16 | 2015-04-07 | Chevron U.S.A. Inc. | Method for preparing zeolite SSZ-35 |
| US9056779B2 (en) * | 2013-09-18 | 2015-06-16 | Chevron U.S.A. Inc. | Method for preparing MWW-type molecular sieves |
| US9573124B2 (en) | 2014-05-21 | 2017-02-21 | Chevron U.S.A. Inc. | Method for making molecular sieve SSZ-95 |
| RU2760897C2 (ru) * | 2014-05-21 | 2021-12-01 | Шеврон Ю.Эс.Эй. Инк. | Молекулярное сито ssz-95 |
| DK3145865T3 (da) * | 2014-05-21 | 2021-03-08 | Chevron Usa Inc | Fremgangsmåder under anvendelse af molekylsigte SSZ-95 |
| US9192924B1 (en) * | 2014-06-04 | 2015-11-24 | Chevron U.S.A. Inc. | Molecular sieve SSZ-99 |
| MY179311A (en) * | 2015-02-05 | 2020-11-04 | Tosoh Corp | Novel zeolite |
| CN107683256B (zh) * | 2015-05-21 | 2020-02-21 | 雪佛龙美国公司 | 分子筛ssz-27及其合成 |
| CN105645428B (zh) * | 2016-02-29 | 2018-03-02 | 中国科学院山西煤炭化学研究所 | 具有介孔‑微孔分等级结构的ssz‑32分子筛的制备方法 |
| CN109890758B (zh) | 2016-11-17 | 2022-04-29 | 雪佛龙美国公司 | 高硅ssz-32x沸石 |
| KR20230019438A (ko) * | 2020-06-03 | 2023-02-08 | 셰브런 유.에스.에이.인크. | Szr 프레임워크 유형 분자체의 합성 |
| CN113979444B (zh) * | 2020-07-27 | 2023-11-24 | 中国石油化工股份有限公司 | 一种具有fer结构的分子筛的制备方法和fer结构的分子筛 |
| US11180376B1 (en) * | 2021-03-19 | 2021-11-23 | Chevron U.S.A. Inc. | Synthesis of zeolites having the ferrierite structure |
| KR20230160340A (ko) | 2021-03-26 | 2023-11-23 | 셰브런 유.에스.에이.인크. | 분자체 ssz-93, 촉매 및 이의 사용 방법 |
| US12558676B2 (en) * | 2023-03-02 | 2026-02-24 | Chevron U.S.A. Inc. | Method for preparing small crystal SSZ-81 zeolite |
Family Cites Families (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3140249A (en) | 1960-07-12 | 1964-07-07 | Socony Mobil Oil Co Inc | Catalytic cracking of hydrocarbons with a crystalline zeolite catalyst composite |
| NL132193C (da) | 1961-12-21 | |||
| US3140253A (en) | 1964-05-01 | 1964-07-07 | Socony Mobil Oil Co Inc | Catalytic hydrocarbon conversion with a crystalline zeolite composite catalyst |
| CA1072525A (en) | 1975-05-22 | 1980-02-26 | Exxon Research And Engineering Company | Catalysts, method of making said catalysts and uses thereof |
| JPS5962349A (ja) * | 1982-10-04 | 1984-04-09 | Showa Shell Sekiyu Kk | 高シリカゼオライト触媒の製法 |
| US4818507A (en) * | 1986-07-14 | 1989-04-04 | Shell Oil Company | Novel process for the preparation of ZSM-5 aluminosilicate zeolite |
| US4935215A (en) | 1987-05-26 | 1990-06-19 | Mobil Oil Corporation | Measurement and control of zeolite synthesis |
| US4849194A (en) * | 1987-05-26 | 1989-07-18 | Mobil Oil Corporation | Measurement and control of zeolite synthesis |
| US5053373A (en) | 1988-03-23 | 1991-10-01 | Chevron Research Company | Zeolite SSZ-32 |
| US5252527A (en) | 1988-03-23 | 1993-10-12 | Chevron Research And Technology Company | Zeolite SSZ-32 |
| JPH02129015A (ja) * | 1988-11-07 | 1990-05-17 | Tosoh Corp | 多孔質結晶性珪酸塩の製造方法 |
| AU647147B2 (en) | 1991-07-05 | 1994-03-17 | Chevron Research And Technology Company | Zeolite SSZ-32 |
| DE69525860T2 (de) * | 1995-03-17 | 2002-06-27 | Chevron U.S.A. Inc., San Ramon | Herstellung von zeolithen unter verwendung von organischem templat und amin |
| US5707601A (en) * | 1995-03-17 | 1998-01-13 | Chevron U.S.A. Inc. | Process for preparing zeolites having MTT crystal structure using small, neutral amines |
| US7390763B2 (en) | 2003-10-31 | 2008-06-24 | Chevron U.S.A. Inc. | Preparing small crystal SSZ-32 and its use in a hydrocarbon conversion process |
| US20080083657A1 (en) * | 2006-10-04 | 2008-04-10 | Zones Stacey I | Isomerization process using metal-modified small crystallite mtt molecular sieve |
| US7824658B2 (en) * | 2006-12-28 | 2010-11-02 | Chevron U.S.A., Inc. | Method of making ultrasmall crystal MTT molecular sieves |
| KR20090094028A (ko) * | 2006-12-28 | 2009-09-02 | 셰브런 유.에스.에이.인크. | 초소형 결정 ｍｔｔ분자체의 제조방법 |
| US20100121583A1 (en) | 2008-11-13 | 2010-05-13 | E.I. Dupont De Nemours And Company | Method for measurement of in-situ viscosity |
| US20100116034A1 (en) | 2008-11-13 | 2010-05-13 | E. I. Dupont De Nemours And Company | Apparatus for measurement of in-situ viscosity |
| US8734758B2 (en) * | 2010-11-05 | 2014-05-27 | Chevron U.S.A. Inc. | Method for preparing molecular sieves |
-
2010
- 2010-11-05 US US12/940,776 patent/US8545805B2/en active Active
-
2011
- 2011-10-21 KR KR1020137014584A patent/KR101886296B1/ko active Active
- 2011-10-21 ES ES11838459T patent/ES2712742T3/es active Active
- 2011-10-21 EP EP11838459.3A patent/EP2635527B1/en active Active
- 2011-10-21 CA CA2810594A patent/CA2810594C/en active Active
- 2011-10-21 WO PCT/US2011/057225 patent/WO2012061037A2/en not_active Ceased
- 2011-10-21 BR BR112013005114-0A patent/BR112013005114B1/pt active IP Right Grant
- 2011-10-21 CN CN2011800492903A patent/CN103153860A/zh active Pending
- 2011-10-21 SG SG2013029665A patent/SG189466A1/en unknown
- 2011-10-21 DK DK11838459.3T patent/DK2635527T3/da active
- 2011-10-21 MY MYPI2013001293A patent/MY159186A/en unknown
- 2011-10-21 JP JP2013537690A patent/JP5822408B2/ja active Active
-
2013
- 2013-03-06 ZA ZA2013/01712A patent/ZA201301712B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| BR112013005114A2 (pt) | 2016-04-26 |
| ZA201301712B (en) | 2014-05-28 |
| WO2012061037A2 (en) | 2012-05-10 |
| US20120114553A1 (en) | 2012-05-10 |
| CA2810594C (en) | 2018-09-11 |
| EP2635527A2 (en) | 2013-09-11 |
| EP2635527B1 (en) | 2018-11-21 |
| JP5822408B2 (ja) | 2015-11-24 |
| KR101886296B1 (ko) | 2018-08-07 |
| MY159186A (en) | 2016-12-30 |
| CA2810594A1 (en) | 2012-05-10 |
| CN103153860A (zh) | 2013-06-12 |
| BR112013005114B1 (pt) | 2021-08-17 |
| JP2013541492A (ja) | 2013-11-14 |
| US8545805B2 (en) | 2013-10-01 |
| WO2012061037A3 (en) | 2012-06-28 |
| KR20130108625A (ko) | 2013-10-04 |
| SG189466A1 (en) | 2013-05-31 |
| EP2635527A4 (en) | 2016-09-07 |
| ES2712742T3 (es) | 2019-05-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| DK2635527T3 (da) | Fremgangsmåde til fremstilling af lille krystal SSZ-32 | |
| CA2983038C (en) | Process for preparing a molecular sieve | |
| CN101801848B (zh) | 高活性zsm-48的合成 | |
| CN102216216B (zh) | 分子筛ssz-82组合物及其合成 | |
| CA2891025C (en) | Synthesis of zsm-5 crystals with improved morphology | |
| EP2461907B1 (en) | Synthesis and use of zsm-12 | |
| AU753445B2 (en) | Preparation of zeolite L | |
| EP2836461B1 (en) | Molecular sieve ssz-87 composition of matter and synthesis thereof | |
| EP4673401A1 (en) | Method for preparing small crystal ssz-81 zeolite |