JP2022130445A - フッ化物源を用いる新規ゼオライト合成法 - Google Patents
フッ化物源を用いる新規ゼオライト合成法 Download PDFInfo
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- JP2022130445A JP2022130445A JP2022093385A JP2022093385A JP2022130445A JP 2022130445 A JP2022130445 A JP 2022130445A JP 2022093385 A JP2022093385 A JP 2022093385A JP 2022093385 A JP2022093385 A JP 2022093385A JP 2022130445 A JP2022130445 A JP 2022130445A
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- Japan
- Prior art keywords
- zeolite
- aluminosilicate zeolite
- catalyst
- aluminosilicate
- crystals
- 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.)
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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 abstract description 244
- 239000010457 zeolite Substances 0.000 title claims abstract description 236
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 169
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 8
- 238000001308 synthesis method Methods 0.000 title 1
- 239000003054 catalyst Substances 0.000 claims abstract description 119
- 239000013078 crystal Substances 0.000 claims abstract description 76
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229910000323 aluminium silicate Inorganic materials 0.000 claims abstract description 74
- 238000000034 method Methods 0.000 claims abstract description 68
- 229910052751 metal Inorganic materials 0.000 claims abstract description 47
- 239000002184 metal Substances 0.000 claims abstract description 47
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 35
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 23
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000011148 porous material Substances 0.000 claims description 61
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 50
- 239000000203 mixture Substances 0.000 claims description 44
- 239000007789 gas Substances 0.000 claims description 42
- 229910052763 palladium Inorganic materials 0.000 claims description 22
- 229910052783 alkali metal Inorganic materials 0.000 claims description 19
- 150000001340 alkali metals Chemical class 0.000 claims description 19
- 229910052802 copper Inorganic materials 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 16
- 229910052697 platinum Inorganic materials 0.000 claims description 15
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 229910052703 rhodium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 238000001157 Fourier transform infrared spectrum Methods 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 229910052707 ruthenium Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 150000001768 cations Chemical class 0.000 claims description 5
- SAYJSSIMFYICKR-UHFFFAOYSA-N 1,3-bis(1-adamantyl)imidazol-1-ium Chemical compound C1C(C2)CC(C3)CC2CC13[N+](C=C1)=CN1C(C1)(C2)CC3CC2CC1C3 SAYJSSIMFYICKR-UHFFFAOYSA-N 0.000 claims description 4
- DFLRGRAIPLYIIM-UHFFFAOYSA-N 2-ethyl-1,3,4-trimethylimidazol-1-ium Chemical compound CCC=1N(C)C(C)=C[N+]=1C DFLRGRAIPLYIIM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- ZSIQJIWKELUFRJ-UHFFFAOYSA-N azepane Chemical compound C1CCCNCC1 ZSIQJIWKELUFRJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 229950002932 hexamethonium Drugs 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 claims description 3
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical group CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 claims description 3
- OSBSFAARYOCBHB-UHFFFAOYSA-N tetrapropylammonium Chemical compound CCC[N+](CCC)(CCC)CCC OSBSFAARYOCBHB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- LSLKRGFUTWJIJJ-UHFFFAOYSA-N 1,1,2,2,3-pentamethylimidazol-1-ium Chemical compound CN1C([N+](C=C1)(C)C)(C)C LSLKRGFUTWJIJJ-UHFFFAOYSA-N 0.000 claims description 2
- KCUGPPHNMASOTE-UHFFFAOYSA-N 1,2,3-trimethylimidazol-1-ium Chemical compound CC=1N(C)C=C[N+]=1C KCUGPPHNMASOTE-UHFFFAOYSA-N 0.000 claims description 2
- AFXCFLUNQLKEKT-UHFFFAOYSA-N 1,2-dimethyl-3-[(4-methylphenyl)methyl]imidazol-1-ium Chemical compound CC1=[N+](C=CN1C)CC1=CC=C(C=C1)C AFXCFLUNQLKEKT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052762 osmium Inorganic materials 0.000 claims description 2
- 229910052702 rhenium Inorganic materials 0.000 claims description 2
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 claims description 2
- VZJFGSRCJCXDSG-UHFFFAOYSA-N Hexamethonium Chemical compound C[N+](C)(C)CCCCCC[N+](C)(C)C VZJFGSRCJCXDSG-UHFFFAOYSA-N 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 59
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 48
- 239000000047 product Substances 0.000 description 48
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 33
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 30
- 229910002089 NOx Inorganic materials 0.000 description 24
- -1 SDA cation Chemical class 0.000 description 24
- 239000000499 gel Substances 0.000 description 24
- 239000000463 material Substances 0.000 description 21
- 150000001342 alkaline earth metals Chemical class 0.000 description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 229910021529 ammonia Inorganic materials 0.000 description 17
- 239000010949 copper Substances 0.000 description 17
- 239000003638 chemical reducing agent Substances 0.000 description 14
- 229910000510 noble metal Inorganic materials 0.000 description 14
- 239000003513 alkali Substances 0.000 description 13
- 150000002739 metals Chemical class 0.000 description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 12
- 238000007254 oxidation reaction Methods 0.000 description 12
- 239000010948 rhodium Substances 0.000 description 12
- 239000010953 base metal Substances 0.000 description 11
- 239000011230 binding agent Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- 238000001878 scanning electron micrograph Methods 0.000 description 11
- 238000011144 upstream manufacturing Methods 0.000 description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 229930195733 hydrocarbon Natural products 0.000 description 10
- 238000010189 synthetic method Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 9
- 239000000835 fiber Substances 0.000 description 9
- 150000002430 hydrocarbons Chemical class 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 8
- 239000011541 reaction mixture Substances 0.000 description 8
- 239000011449 brick Substances 0.000 description 7
- 239000011651 chromium Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 239000002808 molecular sieve Substances 0.000 description 7
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 7
- 230000009467 reduction Effects 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 239000012013 faujasite Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 238000000634 powder X-ray diffraction Methods 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- JCXJVPUVTGWSNB-UHFFFAOYSA-N Nitrogen dioxide Chemical compound O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 229910052788 barium Inorganic materials 0.000 description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 239000011572 manganese Substances 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 238000004626 scanning electron microscopy Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910001868 water Inorganic materials 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 229910008051 Si-OH Inorganic materials 0.000 description 4
- 229910006358 Si—OH Inorganic materials 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- YWZGBJRUJMCHLS-PHIMTYICSA-N (2r,6s)-1,1-diethyl-2,6-dimethylpiperidin-1-ium Chemical compound CC[N+]1(CC)[C@@H](C)CCC[C@H]1C YWZGBJRUJMCHLS-PHIMTYICSA-N 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000003502 gasoline Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008719 thickening Effects 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- 241000408939 Atalopedes campestris Species 0.000 description 2
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 238000010531 catalytic reduction reaction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000012784 inorganic fiber Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000006259 organic additive Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 125000005372 silanol group Chemical group 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 2
- PYIHTIJNCRKDBV-UHFFFAOYSA-L trimethyl-[6-(trimethylazaniumyl)hexyl]azanium;dichloride Chemical compound [Cl-].[Cl-].C[N+](C)(C)CCCCCC[N+](C)(C)C PYIHTIJNCRKDBV-UHFFFAOYSA-L 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- ZLFGJBCVGPLYNI-UHFFFAOYSA-M 1,2,3-trimethylimidazol-1-ium;hydroxide Chemical compound [OH-].CC=1N(C)C=C[N+]=1C ZLFGJBCVGPLYNI-UHFFFAOYSA-M 0.000 description 1
- GNUJKXOGRSTACR-UHFFFAOYSA-M 1-adamantyl(trimethyl)azanium;hydroxide Chemical compound [OH-].C1C(C2)CC3CC2CC1([N+](C)(C)C)C3 GNUJKXOGRSTACR-UHFFFAOYSA-M 0.000 description 1
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910017119 AlPO Inorganic materials 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000269350 Anura Species 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000197727 Euscorpius alpha Species 0.000 description 1
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- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
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Images
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Abstract
Description
本出願は、2016年9月30日に出願された米国仮出願第62/402698号の優先権を主張する。
結晶化度パーセント=I結晶質/(I結晶質+I非晶質)(I=強度)
を意味する。
約12から約500のSiO2/Al2O3、
約3から約125のSDA2O/Al2O3、
約30から約7500のH2O/Al2O3、
約0.4から約0.6のOH-/SiO2及び/又は
約0.4から約0.6のF-/SiO2
のうちの一又は複数を有し得る。
TMAda-OH、25wt%11.6gを、~30-32のSARを有するゼオライトY(CBV720、Zeolyst)1.65gと混合した。次いで混合物を約70℃まで加熱し、~7.5gのH2Oを蒸発させた。最終的に、HF(48%)0.57gを濃縮ゲル混合物に滴下し、スパチュラによって均質になるまで混合物を攪拌した。次いで、攪拌下(45rpm)、155℃で4日間混合物を加熱した。反応混合物のpH範囲は、約6から約8であった。
TMAda-OH、25wt%11.6gを、~60のSARを有するゼオライトY(CBV760、Zeolyst)1.65gと混合した。次いで混合物を約70℃まで加熱し、~7.5gのH2Oを蒸発させた。最終的に、HF(48%)0.57gを濃縮ゲル混合物に滴下し、スパチュラによって均質になるまで混合物を攪拌した。次いで、攪拌下(45rpm)、155℃で4日間混合物を加熱した。反応混合物のpH範囲は、約6から約8であった。
Al(i-OPr)3をTMAdaOH、25wt%及びTEOSと混合した。攪拌条件下、室温で6-8時間混合物を加水分解し、続いて約60-70℃で加熱してエタノール及びH2Oを蒸発させた。その後、HFを添加し、H2O/SiO2/Al2O3/TMAda-OH/HFのモル比が3/1/0.0167/0.5/0.5の最終的なゲル組成物がもたらされた。結果として得られた乾燥ゲルを手で均質化し、23mLのテフロン加工鋼製オートクレーブに移し、40rpmで回転する炉内で、150℃で5日間ゲルを加熱した。生成されたままの状態の生成物を、空気中、昇温速度3℃/分、580℃で8時間焼成した。図2bは、生成されたままの状態の生成物のSEM画像である。
TMAda-OH、25wt%11.6gを、~100のSARを有するゼオライトY(HSZ-HUA385、Tosoh)1.65gと混合した。次いで混合物を約70℃まで加熱し、~7.5gのH2Oを蒸発させた。最終的に、HF(48%)0.57gを濃縮ゲルに滴下し、スパチュラを用いて均質になるまで混合物を攪拌した。次いで、攪拌下(45rpm)、155℃で4日間混合物を加熱した。反応混合物のpH範囲は、約6から約8であった。
TPA-OH、40wt%10.5gを、~60のSARを有するゼオライトY(CBV760、Zeolyst)2.5gと混合した。次いで混合物を約70℃まで加熱し、~3gのH2Oを蒸発させた。最終的に、HF(48%)0.86gを濃縮ゲルに滴下し、スパチュラを用いて均質になるまで混合物を攪拌した。次いで、静止条件で、175℃で5日間混合物を加熱した。反応混合物のpH範囲は、約6から約8であった。
TEA-OH、35wt%11.2gを、~60のSARを有するゼオライトY(CBV760、Zeolyst)2.95gと混合した。次いで混合物を約70℃まで加熱し、~1.2gのH2Oを蒸発させた。最終的に、HF(48%)1.2gを濃縮ゲル混合物に滴下し、スパチュラによって均質になるまで混合物を攪拌した。次いで、攪拌下(45rpm)、155℃で7日間混合物を加熱した。反応混合物のpH範囲は、約6から約8であった。
実施例1-5の記載と同様の方法によってITW(SAR~80)を調製した。当該方法において、1,2,3TMI-OHが有機構造指向剤であり、CBV780のみがSi及びAlの供給源であった。H2O:SiO2:Al2O3:1,2,3TMI-OH:HF=7:1:0.0125:0.5:0.5のモル組成を有する最終的なゲルを、150℃の炉内で7日間回転させた。生成されたままの状態の生成物の粉末XRD(図6)による分析は、生成物がITW構造を有したことを示し、試料は、棒様の形態を有する(図7に示されるSEM画像)。
実施例1-5の記載と同様の方法によってSTW(SAR~80)を調製した。当該方法において、2E134TMI-OHが有機構造指向剤であり、CBV780のみがSi及びAlの供給源であった。H2O:SiO2:Al2O3:2E134TMI-OH:HF=4:1:0.0125:0.5:0.5のモル組成(5%wtのSTW種結晶を添加した)を有する最終的なゲルを、160℃の炉内で7日間回転させた。生成されたままの状態の生成物の粉末XRD(図8)による分析は、生成物がSTW構造を有したことを示し、試料は、六角両錐棒状形態を有する(図9に示されるSEM画像)。
Claims (60)
- 少なくとも1つのゼオライト、フッ化物源、構造指向剤(SDA)、及び任意選択的な追加のシリカ源を含む合成ゲルを、少なくとも100℃の温度で、所望されるゼオライト形態の結晶が形成するまで反応させることを含む、アルミノケイ酸塩ゼオライトを製造する方法。
- 前記結晶は、少なくとも約90%純相である、請求項1に記載の方法。
- 前記結晶は、少なくとも約20のシリカ対アルミナモル比(SAR)を有する、請求項1又は2に記載の方法。
- 前記所望されるゼオライトは、小細孔ゼオライト、中細孔ゼオライト及び大細孔ゼオライトからなる群から選択される、請求項1から3の何れか一項に記載の方法。
- 前記所望されるゼオライトは、小細孔ゼオライトである、請求項4に記載の方法。
- 前記小細孔ゼオライトは、AFX、AEI、CHA、LTA、ITW、RTH、LEV、STT、SFW又はIHWである、請求項5に記載の方法。
- 前記小細孔ゼオライトは、CHAである、請求項6に記載の方法。
- SDAカチオンは、トリメチルアダマントアンモニウム、N,N,N-ジメチルエチルシクロヘキシルアンモニウム、ペンタメチルイミダゾリウム、1,2-ジメチル-3-(4-メチルベンジル)イミダゾリウム、1,2,3-トリメチルイミダゾリウム、1,3-ビス(1-アダマンチル)イミダゾリウム、2,6-N,N-ジエチル-cis-2,6-ジメチルピペリジウム又はそれらの組合せである、請求項5に記載の方法。
- 前記結晶は、約5μm未満の平均結晶サイズを有する、請求項5から8の何れか一項に記載の方法。
- CHAの結晶は、約1μm未満の平均結晶サイズを有する、請求項7に記載の方法。
- 前記結晶は、約20から約500のSARを有する、請求項5から10の何れか一項に記載の方法。
- 前記所望されるゼオライトは、中細孔ゼオライトである、請求項4に記載の方法。
- SDAカチオンは、テトラプロピルアンモニウム、2-エチル-1,3,4-トリメチルイミダゾリウム、トリメチルアダマントアンモニウム、ヘキサメチレンイミン、ヘキサメトニウム、テトラブチルアンモニウム又はそれらの組合せである、請求項12に記載の方法。
- 前記中細孔ゼオライトは、MFI、STW、MWW、ITH又はMELである、請求項12又は13に記載の方法。
- 前記結晶は、約5μm未満の平均結晶サイズを有する、請求項12から14の何れか一項に記載の方法。
- 前記結晶は、約20から約500のSARを有する、請求項12から15の何れか一項に記載の方法。
- 前記所望されるゼオライトは、大細孔ゼオライトである、請求項4に記載の方法。
- 前記構造指向剤は、テトラエチルアンモニウム、1,3,3-トリメチル-6-アゾニウムトリシクロ[3.2.1.46,6]ドデカン又はそれらの組合せである、請求項17に記載の方法。
- 前記大細孔ゼオライトは、BEA又はISVである、請求項17又は18に記載の方法。
- 前記結晶は、約5μm未満の平均結晶サイズを有する、請求項17から19の何れか一項に記載の方法。
- 前記結晶は、約20から約500のSARを有する、請求項17から20の何れか一項に記載の方法。
- 前記少なくとも1つのゼオライトのみが、アルミノケイ酸塩ゼオライトを形成するシリカ及びアルミニウムの供給源である、請求項1から21の何れか一項に記載の方法。
- 前記ゼオライトは、ゼオライトYである、請求項1から22の何れか一項に記載の方法。
- 前記ゼオライトYは、約12から約500のシリカ対アルミナ比を有する、請求項23に記載の方法。
- 前記少なくとも1つのゼオライトは、2以上のゼオライトを含む、請求項1から24の何れか一項に記載の方法。
- 前記少なくとも1つのゼオライトは、2以上のゼオライトYを含む、請求項25に記載の方法。
- 前記合成ゲルは、実質的にアルカリ金属を含まない、請求項1から26の何れか一項に記載の方法。
- 前記アルカリ金属は、Naである、請求項27に記載の方法。
- 前記合成ゲルは、以下のモル組成比:
約12から約500のSiO2/Al2O3、
約3から約125のSDA2O/Al2O3、
約30から約7500のH2O/Al2O3、
約0.4から約0.6のOH-/SiO2及び/又は
約0.4から約0.6のF-/SiO2
のうちの一又は複数を有する、請求項1から28の何れか一項に記載の方法。 - 合成は、シーディングされたアルミノケイ酸塩ゼオライト結晶の非存在下で行われる、請求項1から29の何れか一項に記載の方法。
- 前記合成ゲルは、第二のSDAをさらに含む、請求項1から30の何れか一項に記載の方法。
- 第二のSDAカチオンは、テトラメチルアンモニウムである、請求項31に記載の方法。
- 反応工程は、約120から約180℃の温度で、約1から約15日間行われる、請求項1から32の何れか一項に記載の方法。
- 反応工程は、約11未満のpHで行われる、請求項1から33の何れか一項に記載の方法。
- V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Mo、Ru、Rh、Pd、Ag、W、Re、Os、Ir、Pt及びAuから選択される金属を担持する、請求項1から34の何れか一項に記載の方法によって得られるアルミノケイ酸塩ゼオライトを含む、排気ガスを処理するための触媒。
- 前記金属は、Fe及びCuから選択される、請求項35に記載の触媒。
- 前記金属は、Pt、Ru及びPdから選択される、請求項35に記載の触媒。
- NOxを含有する排気ガス流を、請求項35から37の何れか一項に記載の触媒に接触させることを含む、NOxを貯蔵する方法。
- NOxを含有する排気ガス流を、請求項35から37の何れか一項に記載の触媒に接触させることを含む、NOxを選択的に還元させる方法。
- 排気ガスの成分を酸化させる方法であって、前記成分を含有する排気ガス流を、請求項35から37の何れか一項に記載の触媒に接触させることを含み、前記成分は、CO、炭化水素及びNH3から選択される、方法。
- ウォールフロー型ハニカムフィルタ及びフロースルー型ハニカム基材から選択される基材上に支持されているか、又はウォールフロー型ハニカムフィルタ及びフロースルー型ハニカム基材から選択される基材中に埋め込まれている請求項35から37の何れか一項に記載の触媒を含む触媒製品。
- 少なくとも約90%純相のITW骨格、及び約140未満のシリカ対アルミナ比を含むアルミノケイ酸塩ゼオライト。
- 約60から約140のシリカ対アルミナ比を有する、請求項42に記載のアルミノケイ酸塩ゼオライト。
- 約0.5μmから約5μmの平均結晶サイズを有する、請求項42又は43に記載のアルミノケイ酸塩ゼオライト。
- 少なくとも約95%純相のITW骨格を含む、請求項42から44の何れか一項に記載のアルミノケイ酸塩ゼオライト。
- 少なくとも約97%純相のITW骨格を含む、請求項42から45の何れか一項に記載のアルミノケイ酸塩ゼオライト。
- アルカリ金属を実質的に含まない、請求項42から46の何れか一項に記載のアルミノケイ酸塩ゼオライト。
- 少なくとも約90%純相のSTW骨格、及び約100未満のシリカ対アルミナ比を含むアルミノケイ酸塩ゼオライト。
- 約80から約100のシリカ対アルミナ比を有する、請求項48に記載のアルミノケイ酸塩ゼオライト。
- 約0.5μmから約5μmの平均結晶サイズを有する、請求項48又は49に記載のアルミノケイ酸塩ゼオライト。
- 少なくとも約95%純相のSTW骨格を含む、請求項48から50の何れか一項に記載のアルミノケイ酸塩ゼオライト。
- 少なくとも約97%純相のSTW骨格を含む、請求項48から51の何れか一項に記載のアルミノケイ酸塩ゼオライト。
- アルカリ金属を実質的に含まない、請求項48から52の何れか一項に記載のアルミノケイ酸塩ゼオライト。
- 少なくとも約90%純相のCHA骨格を含むアルミノケイ酸塩ゼオライトであって、図10のFT-IRスペクトルを有する、アルミノケイ酸塩ゼオライト。
- 少なくとも約90%純相のCHA骨格を含むアルミノケイ酸塩ゼオライトであって、前記アルミノケイ酸塩ゼオライトの振動数約3730cm-1と約1870cm-1の間の強度比は、そのFT-IRスペクトルによると、約5未満である、アルミノケイ酸塩ゼオライト。
- 前記アルミノケイ酸塩ゼオライトの振動数約3730cm-1と約1870cm-1の間の強度比の範囲は、約1:10から約5:1である、請求項55に記載のアルミノケイ酸塩ゼオライト。
- 約3μm未満の平均結晶サイズを有する、請求項55又は56に記載のアルミノケイ酸塩ゼオライト。
- 約20から約500のSARを有する、請求項55から57の何れか一項に記載のアルミノケイ酸塩ゼオライト。
- 少なくとも約95%純相のCHA骨格を含む、請求項55から58の何れか一項に記載のアルミノケイ酸塩ゼオライト。
- アルカリ金属を実質的に含まない、請求項55から59の何れか一項に記載のアルミノケイ酸塩ゼオライト。
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US11939901B1 (en) | 2023-06-12 | 2024-03-26 | Edan Prabhu | Oxidizing reactor apparatus |
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GB2597877A (en) | 2022-02-09 |
GB2597877B (en) | 2022-09-14 |
US11007513B2 (en) | 2021-05-18 |
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JP2020502017A (ja) | 2020-01-23 |
RU2021112572A3 (ja) | 2021-12-09 |
GB2569757B (en) | 2022-09-14 |
RU2019113166A3 (ja) | 2021-05-25 |
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DE102017122676A1 (de) | 2018-04-05 |
US10682635B2 (en) | 2020-06-16 |
WO2018064273A1 (en) | 2018-04-05 |
CN109923070A (zh) | 2019-06-21 |
US11452996B2 (en) | 2022-09-27 |
GB202116437D0 (en) | 2021-12-29 |
KR20190056423A (ko) | 2019-05-24 |
US20200353453A1 (en) | 2020-11-12 |
RU2019113166A (ru) | 2020-10-30 |
US20210237043A1 (en) | 2021-08-05 |
GB2569757A (en) | 2019-06-26 |
GB2597878B (en) | 2022-12-07 |
KR102594931B1 (ko) | 2023-10-30 |
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