JP2022521509A - モレキュラーシーブssz-115、その合成及び使用 - Google Patents
モレキュラーシーブssz-115、その合成及び使用 Download PDFInfo
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- JP2022521509A JP2022521509A JP2021548622A JP2021548622A JP2022521509A JP 2022521509 A JP2022521509 A JP 2022521509A JP 2021548622 A JP2021548622 A JP 2021548622A JP 2021548622 A JP2021548622 A JP 2021548622A JP 2022521509 A JP2022521509 A JP 2022521509A
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- molecular sieve
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- ssz
- reaction mixture
- trimethylammonio
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- 230000015572 biosynthetic process Effects 0.000 title description 8
- 238000003786 synthesis reaction Methods 0.000 title description 8
- 239000002808 molecular sieve Substances 0.000 claims abstract description 47
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 24
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 8
- -1 trimethylammonio Chemical group 0.000 claims abstract description 7
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 239000011541 reaction mixture Substances 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000002425 crystallisation Methods 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000013078 crystal Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 150000002739 metals Chemical class 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 6
- JQDLGOBFUBDWRV-UHFFFAOYSA-N trimethyl-[5-(1-methylpyrrolidin-1-ium-1-yl)pentyl]azanium Chemical group C[N+](C)(C)CCCCC[N+]1(C)CCCC1 JQDLGOBFUBDWRV-UHFFFAOYSA-N 0.000 claims description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 239000012084 conversion product Substances 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 238000005119 centrifugation Methods 0.000 description 6
- 239000012265 solid product Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000010457 zeolite Substances 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000004809 Teflon Substances 0.000 description 5
- 229920006362 Teflon® Polymers 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 150000001768 cations Chemical class 0.000 description 5
- 238000000921 elemental analysis Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000009616 inductively coupled plasma 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
- 238000001144 powder X-ray diffraction data Methods 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- DDCQHDMZVOKMCI-UHFFFAOYSA-L trimethyl-[5-(1-methylpyrrolidin-1-ium-1-yl)pentyl]azanium dihydroxide Chemical compound [OH-].C[N+]1(CCCC1)CCCCC[N+](C)(C)C.[OH-] DDCQHDMZVOKMCI-UHFFFAOYSA-L 0.000 description 5
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 235000012211 aluminium silicate Nutrition 0.000 description 4
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 239000008119 colloidal silica Substances 0.000 description 4
- 239000005995 Aluminium silicate Substances 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
- 239000011230 binding agent Substances 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 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
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 229940024546 aluminum hydroxide gel Drugs 0.000 description 2
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 102000034530 Channels/pores Human genes 0.000 description 1
- 108091006155 Channels/pores Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- RWRDLPDLKQPQOW-UHFFFAOYSA-O Pyrrolidinium ion Chemical compound C1CC[NH2+]C1 RWRDLPDLKQPQOW-UHFFFAOYSA-O 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 229940024545 aluminum hydroxide Drugs 0.000 description 1
- 150000003868 ammonium compounds Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 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
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000739 chaotic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000354 decomposition reaction 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
- 239000003085 diluting agent Substances 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000011738 major mineral Substances 0.000 description 1
- 235000011963 major mineral Nutrition 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052605 nesosilicate Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000006384 oligomerization reaction Methods 0.000 description 1
- 150000004762 orthosilicates Chemical class 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
-
- 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
- C01B39/026—After-treatment
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- 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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/02—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils characterised by the catalyst used
- C10G11/04—Oxides
- C10G11/05—Crystalline alumino-silicates, e.g. molecular sieves
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G29/00—Refining of hydrocarbon oils, in the absence of hydrogen, with other chemicals
- C10G29/20—Organic compounds not containing metal atoms
- C10G29/205—Organic compounds not containing metal atoms by reaction with hydrocarbons added to the hydrocarbon oil
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
- C10G47/02—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions characterised by the catalyst used
- C10G47/10—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions characterised by the catalyst used with catalysts deposited on a carrier
- C10G47/12—Inorganic carriers
- C10G47/16—Crystalline alumino-silicate carriers
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G50/00—Production of liquid hydrocarbon mixtures from lower carbon number hydrocarbons, e.g. by oligomerisation
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- Crystallography & Structural Chemistry (AREA)
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- Silicates, Zeolites, And Molecular Sieves (AREA)
- Catalysts (AREA)
Abstract
Description
本出願は、2019年2月27日提出の米国特許仮出願第62/811,225号の優先権及び利益を主張する。
式中、Qは1-メチル-1-[5-(トリメチルアンモニオ)ペンチル]ピロリジニウムジカチオンであり、Mは、第1族または第2族の金属(M)である。
Al2O3:(n)SiO2
式中、nは、5~100の範囲である。
用語「合成されたままの」は、本明細書中では、結晶化後、構造指向剤を除去する前のその形態のモレキュラーシーブを指すために使用される。
モレキュラーシーブSSZ-115は、(a)(1)酸化ケイ素供給源、(2)酸化アルミニウム供給源、(3)第1族または第2族の金属(M)供給源、(4)1-メチル-1-[5-(トリメチルアンモニオ)ペンチル]ピロリジニウムジカチオンを含む構造指向剤(Q)、(5)水酸化物イオン供給源、及び(6)水を含む反応混合物を提供し、(b)反応混合物をモレキュラーシーブの結晶を形成するのに十分な結晶化条件に供することにより合成することができる。
上記の反応混合物からのモレキュラーシーブの結晶化は、ポリプロピレンジャーまたはテフロンで裏打ちされたもしくはステンレス鋼のオートクレーブなどの適切な反応容器内で、静置、転倒または撹拌条件下のいずれかで、結晶化が起こるのに十分な時間(例えば、約2~40日、または5~30日)の間、125℃~200℃(例えば、140℃~170℃)で実施することができる。結晶化は通常オートクレーブ内で行われるため、反応混合物は自生圧力を受ける。
合成されたままの無水形態では、モレキュラーシーブSSZ-115は、表2に記載のように、以下のモル濃度関係を有する化学組成を有し得る:
式中、組成変数Q及びMは、本明細書において上記したとおりである。
Al2O3:(n)SiO2
式中、nは、5~100の範囲(例えば、5~75、5~60、5~50、10~100、10~75、または10~60)である。
モレキュラーシーブSSZ-115は、現在の商業的/工業的重要性の多くを含む様々な有機化合物変換プロセスを触媒するための吸着剤または触媒として使用し得る。SSZ-115によって、それ自体で、または他の結晶性触媒を含む1つ以上の他の触媒活性物質と組み合わせて効果的に触媒される化学変換プロセスの例には、酸活性を有する触媒を必要とするプロセスが含まれる。SSZ-115によって触媒され得る有機変換プロセスの例として、分解、水素化分解、不均化、アルキル化、オリゴマー化、及び異性化が挙げられる。
10.20gの脱イオン水、0.64gの50%NaOH水溶液、4.79gの16.72% 1-メチル-1-[5-(トリメチルアンモニオ)ペンチル]ピロリジニウム水酸化物溶液及び2.00gのCBV720 Y-ゼオライト粉末(Zeolyst International、SiO2/Al2O3 モル比=30)を、テフロンライナー内で一緒に混合した。得られたゲルを均一になるまで撹拌した。次いで、ライナーに蓋をして、Parr steelオートクレーブ反応器内に配置した。次いでオートクレーブをオーブンに入れ、静置条件下、150℃で10日間加熱した。固体生成物を遠心分離によって回収し、脱イオン水で洗浄し、95℃で乾燥させた。
10.27gの脱イオン水、0.52gの50%NaOH水溶液、4.79gの16.72% 1-メチル-1-[5-(トリメチルアンモニオ)ペンチル]ピロリジニウム水酸化物溶液及び2.00gのCBV760 Y-ゼオライト粉末(Zeolyst International、SiO2/Al2O3 モル比=60)を、テフロンライナー内で一緒に混合した。得られたゲルを均一になるまで撹拌した。次いで、ライナーに蓋をして、Parr steelオートクレーブ反応器内に配置した。次いでオートクレーブをオーブンに入れ、静置条件下、150℃で8日間加熱した。固体生成物を遠心分離によって回収し、脱イオン水で洗浄し、95℃で乾燥させた。
5.23gの脱イオン水、0.30gの50%NaOH水溶液、5.56gの16.72% 1-メチル-1-[5-(トリメチルアンモニオ)ペンチル]ピロリジニウム水酸化物溶液、0.25gの50%Reheis F-2000水酸化アルミニウム乾燥ゲル及び5.00gのLUDOX(登録商標)AS-30コロイド状シリカ(水中の30重量%懸濁液)をテフロンライナー内で一緒に混合した。得られたゲルを均一になるまで撹拌した。次いで、ライナーに蓋をして、Parr steelオートクレーブ反応器内に配置した。次いで、オートクレーブをオーブンに入れ、43rpmでタンブリングしながら160℃で18日間加熱した。固体生成物を遠心分離によって回収し、脱イオン水で洗浄し、95℃で乾燥させた。
3.14gの脱イオン水、0.28gの45%KOH水溶液、3.34gの16.72% 1-メチル-1-[5-(トリメチルアンモニオ)ペンチル]ピロリジニウム水酸化物溶液、0.15gの50%Reheis F-2000水酸化アルミニウム乾燥ゲル及び3.00gのLUDOX(登録商標)AS-30コロイド状シリカをテフロンライナー内で一緒に混合した。得られたゲルを均一になるまで撹拌した。次いで、ライナーに蓋をして、Parr steelオートクレーブ反応器内に配置した。次いで、オートクレーブをオーブンに入れ、43rpmでタンブリングしながら160℃で30日間加熱した。固体生成物を遠心分離によって回収し、脱イオン水で洗浄し、95℃で乾燥させた。
0.24gの50%NaOH水溶液、2.23gの16.72% 1-メチル-1-[5-(トリメチルアンモニオ)ペンチル]ピロリジニウム水酸化物溶液、0.20gの50%Reheis F-2000水酸化アルミニウム乾燥ゲル及び3.00gのLUDOX(登録商標)AS-30コロイド状シリカをテフロンライナー内で一緒に混合した。得られたゲルを均一になるまで撹拌した。次いで、ライナーに蓋をして、Parr steelオートクレーブ反応器内に配置した。次いで、オートクレーブをオーブンに入れ、43rpmでタンブリングしながら160℃で11日間加熱した。固体生成物を遠心分離によって回収し、脱イオン水で洗浄し、95℃で乾燥させた。
実施例1の合成されたままのモレキュラーシーブを、540℃に加熱した空気の流通下、1℃/分の速度で、マッフル炉内で焼成し、540℃で5時間保持し、冷却し、次いで粉末XRDで分析した。
焼成した実施例4のモレキュラーシーブ物質を、10mL(モレキュラーシーブ1gあたり)の1N硝酸アンモニウム溶液で95℃、2時間処理した。混合物を冷却し、溶媒をデカントして取り除き、同じプロセスを繰り返した。
Claims (11)
- 焼成されたままの形態で、図3に示すパターンと実質的に同じ粉末X線回折パターンを有するモレキュラーシーブ。
- モル濃度関係:
Al2O3:(n)SiO2
を有する組成を有し、式中、nが、5~100の範囲である、請求項1に記載のモレキュラーシーブ。 - モル濃度関係:
Al2O3:(n)SiO2
を有する組成を有し、式中、nが、10~60の範囲である、請求項1に記載のモレキュラーシーブ。 - 合成されたままの形態で、図1に示すパターンと実質的に同じ粉末X線回折パターンを有するモレキュラーシーブ。
- 請求項4に記載のモレキュラーシーブの合成方法であって、
(a)
(1)酸化ケイ素の供給源、
(2)酸化アルミニウムの供給源、
(3)第1族または第2族の金属(M)の供給源、
(4)1-メチル-1-[5-(トリメチルアンモニオ)ペンチル]ピロリジニウムジカチオンを含む構造指向剤(Q)、
(5)水酸化物イオン供給源、及び
(6)水
を含む反応混合物を提供し、ならびに
(b)前記反応混合物を、前記モレキュラーシーブの結晶を形成するのに十分な結晶化条件に供することを含む、前記合成方法。 - 前記結晶化条件が、125℃~200℃の温度を含む、請求項7に記載の方法。
- 有機化合物を含む原料から変換生成物への変換プロセスであって、前記原料を、請求項1に記載のモレキュラーシーブを含む触媒に、有機化合物変換条件で接触させることを含む、前記変換プロセス。
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