JP2017532282A5 - - Google Patents
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- JP2017532282A5 JP2017532282A5 JP2017520902A JP2017520902A JP2017532282A5 JP 2017532282 A5 JP2017532282 A5 JP 2017532282A5 JP 2017520902 A JP2017520902 A JP 2017520902A JP 2017520902 A JP2017520902 A JP 2017520902A JP 2017532282 A5 JP2017532282 A5 JP 2017532282A5
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- JP
- Japan
- Prior art keywords
- mass
- mixture
- fluoride
- salt
- less
- 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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- 239000000463 material Substances 0.000 claims description 149
- 238000000034 method Methods 0.000 claims description 141
- 239000000203 mixture Substances 0.000 claims description 136
- 239000010457 zeolite Substances 0.000 claims description 44
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 34
- 238000002425 crystallisation Methods 0.000 claims description 33
- 230000008025 crystallization Effects 0.000 claims description 33
- 239000003795 chemical substances by application Substances 0.000 claims description 32
- 150000001875 compounds Chemical class 0.000 claims description 28
- 239000013078 crystal Substances 0.000 claims description 28
- 238000004400 29Si cross polarisation magic angle spinning Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 150000002894 organic compounds Chemical class 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- 150000004673 fluoride salts Chemical class 0.000 claims description 9
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000003463 adsorbent Substances 0.000 claims description 4
- 238000005342 ion exchange Methods 0.000 claims description 4
- 239000002808 molecular sieve Substances 0.000 claims description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 111
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 61
- -1 (C 1 -C 3 ) alkyl ammonium fluoride Chemical compound 0.000 description 50
- 229910004298 SiO 2 Inorganic materials 0.000 description 47
- 238000003786 synthesis reaction Methods 0.000 description 29
- 230000015572 biosynthetic process Effects 0.000 description 28
- 150000003839 salts Chemical class 0.000 description 28
- 239000011734 sodium Substances 0.000 description 26
- 239000007787 solid Substances 0.000 description 25
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 19
- 239000000377 silicon dioxide Substances 0.000 description 18
- 238000002441 X-ray diffraction Methods 0.000 description 17
- 229910052783 alkali metal Inorganic materials 0.000 description 16
- 150000001340 alkali metals Chemical class 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 14
- 150000001342 alkaline earth metals Chemical class 0.000 description 14
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 14
- 229910021485 fumed silica Inorganic materials 0.000 description 14
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 14
- 229910021536 Zeolite Inorganic materials 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 229910002027 silica gel Inorganic materials 0.000 description 13
- 239000000741 silica gel Substances 0.000 description 13
- 238000001228 spectrum Methods 0.000 description 13
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 12
- 150000003863 ammonium salts Chemical class 0.000 description 11
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 11
- 238000005004 MAS NMR spectroscopy Methods 0.000 description 10
- 229910017855 NH 4 F Inorganic materials 0.000 description 10
- 125000005263 alkylenediamine group Chemical group 0.000 description 10
- 238000000227 grinding Methods 0.000 description 10
- 239000004570 mortar (masonry) Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 9
- 125000000217 alkyl group Chemical group 0.000 description 9
- 230000005855 radiation Effects 0.000 description 9
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical class CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 9
- OSBSFAARYOCBHB-UHFFFAOYSA-N tetrapropylammonium Chemical class CCC[N+](CCC)(CCC)CCC OSBSFAARYOCBHB-UHFFFAOYSA-N 0.000 description 9
- 125000006526 (C1-C2) alkyl group Chemical group 0.000 description 8
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 8
- 235000012239 silicon dioxide Nutrition 0.000 description 8
- 150000001335 aliphatic alkanes Chemical class 0.000 description 7
- 125000005210 alkyl ammonium group Chemical group 0.000 description 7
- 125000002947 alkylene group Chemical group 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 7
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 229910052708 sodium Inorganic materials 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 description 6
- 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 6
- LNIYNESXCOYFPW-UHFFFAOYSA-N dibenzyl(dimethyl)azanium Chemical class C=1C=CC=CC=1C[N+](C)(C)CC1=CC=CC=C1 LNIYNESXCOYFPW-UHFFFAOYSA-N 0.000 description 6
- ZJHQDSMOYNLVLX-UHFFFAOYSA-N diethyl(dimethyl)azanium Chemical class CC[N+](C)(C)CC ZJHQDSMOYNLVLX-UHFFFAOYSA-N 0.000 description 6
- BUWDPPUOSGERNF-UHFFFAOYSA-N prop-2-enyl(tripropyl)azanium Chemical class CCC[N+](CCC)(CCC)CC=C BUWDPPUOSGERNF-UHFFFAOYSA-N 0.000 description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 6
- 239000011775 sodium fluoride Substances 0.000 description 6
- 235000013024 sodium fluoride Nutrition 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 241000894007 species Species 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 150000003973 alkyl amines Chemical class 0.000 description 5
- 150000001450 anions Chemical class 0.000 description 5
- 239000011698 potassium fluoride Substances 0.000 description 5
- 235000003270 potassium fluoride Nutrition 0.000 description 5
- 239000011541 reaction mixture Substances 0.000 description 5
- PYIHTIJNCRKDBV-UHFFFAOYSA-L trimethyl-[6-(trimethylazaniumyl)hexyl]azanium;dichloride Chemical class [Cl-].[Cl-].C[N+](C)(C)CCCCCC[N+](C)(C)C PYIHTIJNCRKDBV-UHFFFAOYSA-L 0.000 description 5
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 description 4
- IVLICPVPXWEGCA-UHFFFAOYSA-N 3-quinuclidinol Chemical compound C1C[C@@H]2C(O)C[N@]1CC2 IVLICPVPXWEGCA-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 229910052785 arsenic Inorganic materials 0.000 description 4
- YOUGRGFIHBUKRS-UHFFFAOYSA-N benzyl(trimethyl)azanium Chemical class C[N+](C)(C)CC1=CC=CC=C1 YOUGRGFIHBUKRS-UHFFFAOYSA-N 0.000 description 4
- VUFQYRAKSQTZEB-UHFFFAOYSA-N bicyclo[2.2.1]heptan-4-amine Chemical compound C1CC2CCC1(N)C2 VUFQYRAKSQTZEB-UHFFFAOYSA-N 0.000 description 4
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 description 4
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 4
- RBUJTRYJXATERJ-UHFFFAOYSA-N dibenzyl(diethyl)azanium Chemical class C=1C=CC=CC=1C[N+](CC)(CC)CC1=CC=CC=C1 RBUJTRYJXATERJ-UHFFFAOYSA-N 0.000 description 4
- PJABQHODPAEOFU-UHFFFAOYSA-N diethyl(dipropyl)azanium Chemical class CCC[N+](CC)(CC)CCC PJABQHODPAEOFU-UHFFFAOYSA-N 0.000 description 4
- WQHRRUZRGXLCGL-UHFFFAOYSA-N dimethyl(dipropyl)azanium Chemical class CCC[N+](C)(C)CCC WQHRRUZRGXLCGL-UHFFFAOYSA-N 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- UMRZSTCPUPJPOJ-KNVOCYPGSA-N norbornane Chemical compound C1C[C@H]2CC[C@@H]1C2 UMRZSTCPUPJPOJ-KNVOCYPGSA-N 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- VJGWNHDROCRKKK-UHFFFAOYSA-N prop-1-enyl(tripropyl)azanium Chemical class CCC[N+](CCC)(CCC)C=CC VJGWNHDROCRKKK-UHFFFAOYSA-N 0.000 description 4
- SBYHFKPVCBCYGV-UHFFFAOYSA-N quinuclidine Chemical compound C1CC2CCN1CC2 SBYHFKPVCBCYGV-UHFFFAOYSA-N 0.000 description 4
- AHLATJUETSFVIM-UHFFFAOYSA-M rubidium fluoride Chemical compound [F-].[Rb+] AHLATJUETSFVIM-UHFFFAOYSA-M 0.000 description 4
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical class C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 4
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910001512 metal fluoride Inorganic materials 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- BGQMOFGZRJUORO-UHFFFAOYSA-M tetrapropylammonium bromide Chemical compound [Br-].CCC[N+](CCC)(CCC)CCC BGQMOFGZRJUORO-UHFFFAOYSA-M 0.000 description 3
- WYMOJXIRERFNHS-UHFFFAOYSA-N 1,1,2-trimethylpiperidin-1-ium Chemical class CC1CCCC[N+]1(C)C WYMOJXIRERFNHS-UHFFFAOYSA-N 0.000 description 2
- FFZBKYWLYLHWGP-UHFFFAOYSA-N 1,1,3,3-tetramethylpiperidin-1-ium Chemical class CC1(C)CCC[N+](C)(C)C1 FFZBKYWLYLHWGP-UHFFFAOYSA-N 0.000 description 2
- QDRFNXRYFUFFLV-UHFFFAOYSA-N 1,2,3-trimethylimidazolidine Chemical class CC1N(C)CCN1C QDRFNXRYFUFFLV-UHFFFAOYSA-N 0.000 description 2
- QDBSMKFBIMHREN-UHFFFAOYSA-N 1,4-dibenzyl-1,4-diazoniabicyclo[2.2.2]octane Chemical compound C1C[N+](CC=2C=CC=CC=2)(CC2)CC[N+]12CC1=CC=CC=C1 QDBSMKFBIMHREN-UHFFFAOYSA-N 0.000 description 2
- KKXBPUAYFJQMLN-UHFFFAOYSA-N 1-adamantyl(trimethyl)azanium Chemical class C1C(C2)CC3CC2CC1([N+](C)(C)C)C3 KKXBPUAYFJQMLN-UHFFFAOYSA-N 0.000 description 2
- GZAPDEOMGLZCAF-UHFFFAOYSA-N 1-ethyl-1,3,3-trimethylpiperidin-1-ium Chemical class CC[N+]1(C)CCCC(C)(C)C1 GZAPDEOMGLZCAF-UHFFFAOYSA-N 0.000 description 2
- MFQQHFRKVCFEBQ-UHFFFAOYSA-N 1-methyl-1-azoniabicyclo[2.2.2]octane Chemical class C1CC2CC[N+]1(C)CC2 MFQQHFRKVCFEBQ-UHFFFAOYSA-N 0.000 description 2
- DMBILWVUAAPKHW-UHFFFAOYSA-N 2-adamantyl(trimethyl)azanium Chemical class C1C(C2)CC3CC1C([N+](C)(C)C)C2C3 DMBILWVUAAPKHW-UHFFFAOYSA-N 0.000 description 2
- 241001432959 Chernes Species 0.000 description 2
- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 description 2
- GSBKRFGXEJLVMI-UHFFFAOYSA-N Nervonyl carnitine Chemical class CCC[N+](C)(C)C GSBKRFGXEJLVMI-UHFFFAOYSA-N 0.000 description 2
- 239000004111 Potassium silicate Substances 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 2
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- ZSIQJIWKELUFRJ-UHFFFAOYSA-N azepane Chemical compound C1CCCNCC1 ZSIQJIWKELUFRJ-UHFFFAOYSA-N 0.000 description 2
- VBQDSLGFSUGBBE-UHFFFAOYSA-N benzyl(triethyl)azanium Chemical class CC[N+](CC)(CC)CC1=CC=CC=C1 VBQDSLGFSUGBBE-UHFFFAOYSA-N 0.000 description 2
- IVFSNAWJLNNRKU-UHFFFAOYSA-N benzyl-diethyl-methylazanium Chemical class CC[N+](C)(CC)CC1=CC=CC=C1 IVFSNAWJLNNRKU-UHFFFAOYSA-N 0.000 description 2
- ODRZUUBZEIXMOS-UHFFFAOYSA-N benzyl-ethyl-dimethylazanium Chemical class CC[N+](C)(C)CC1=CC=CC=C1 ODRZUUBZEIXMOS-UHFFFAOYSA-N 0.000 description 2
- 150000001649 bromium compounds Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000008119 colloidal silica Substances 0.000 description 2
- HCKMSHYCAFVSGW-UHFFFAOYSA-N cyclohexyl(trimethyl)azanium Chemical class C[N+](C)(C)C1CCCCC1 HCKMSHYCAFVSGW-UHFFFAOYSA-N 0.000 description 2
- 125000005131 dialkylammonium group Chemical group 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- WDSYOBJACYKNAS-UHFFFAOYSA-N dibenzyl(dipropyl)azanium Chemical class C=1C=CC=CC=1C[N+](CCC)(CCC)CC1=CC=CC=C1 WDSYOBJACYKNAS-UHFFFAOYSA-N 0.000 description 2
- FIBFAXJLKAVKML-UHFFFAOYSA-N dibenzyl-ethyl-propylazanium Chemical class C(C)[N+](CC1=CC=CC=C1)(CC1=CC=CC=C1)CCC FIBFAXJLKAVKML-UHFFFAOYSA-N 0.000 description 2
- GFHKUCHXCVOEAT-UHFFFAOYSA-N dibenzyl-methyl-propylazanium Chemical class C[N+](CC1=CC=CC=C1)(CC1=CC=CC=C1)CCC GFHKUCHXCVOEAT-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- FRNYKUYJIUPPPW-UHFFFAOYSA-N ethyl(tripropyl)azanium Chemical class CCC[N+](CC)(CCC)CCC FRNYKUYJIUPPPW-UHFFFAOYSA-N 0.000 description 2
- YOMFVLRTMZWACQ-UHFFFAOYSA-N ethyltrimethylammonium Chemical class CC[N+](C)(C)C YOMFVLRTMZWACQ-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 150000004694 iodide salts Chemical class 0.000 description 2
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 2
- 229910052912 lithium silicate Inorganic materials 0.000 description 2
- VFOJFWOVDZGATC-UHFFFAOYSA-N methyl(tripropyl)azanium Chemical class CCC[N+](C)(CCC)CCC VFOJFWOVDZGATC-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 2
- 229910052913 potassium silicate Inorganic materials 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- UHVNJQHZIBLGSF-UHFFFAOYSA-N prop-1-en-2-yl(tripropyl)azanium Chemical class CCC[N+](CCC)(CCC)C(C)=C UHVNJQHZIBLGSF-UHFFFAOYSA-N 0.000 description 2
- 125000005624 silicic acid group Chemical class 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 235000019794 sodium silicate Nutrition 0.000 description 2
- 230000007847 structural defect Effects 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 150000005621 tetraalkylammonium salts Chemical class 0.000 description 2
- SEACXNRNJAXIBM-UHFFFAOYSA-N triethyl(methyl)azanium Chemical class CC[N+](C)(CC)CC SEACXNRNJAXIBM-UHFFFAOYSA-N 0.000 description 2
- WGYXSYLSCVXFDU-UHFFFAOYSA-N triethyl(propyl)azanium Chemical class CCC[N+](CC)(CC)CC WGYXSYLSCVXFDU-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- KEVGQBVVYQPYIF-UHFFFAOYSA-N Br.Br.Br.Br.Br.Br.Br Chemical compound Br.Br.Br.Br.Br.Br.Br KEVGQBVVYQPYIF-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- WWXBHTZSYYGCSG-UHFFFAOYSA-N [4-(carbamoylamino)phenyl]arsonic acid Chemical compound NC(=O)NC1=CC=C([As](O)(O)=O)C=C1 WWXBHTZSYYGCSG-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- KVBCYCWRDBDGBG-UHFFFAOYSA-N azane;dihydrofluoride Chemical compound [NH4+].F.[F-] KVBCYCWRDBDGBG-UHFFFAOYSA-N 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-O azanium;hydrofluoride Chemical compound [NH4+].F LDDQLRUQCUTJBB-UHFFFAOYSA-O 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000005388 cross polarization Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- FVFWICRKDMTBSF-UHFFFAOYSA-N dibenzyl-ethyl-methylazanium Chemical class C=1C=CC=CC=1C[N+](C)(CC)CC1=CC=CC=C1 FVFWICRKDMTBSF-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 239000011874 heated mixture Substances 0.000 description 1
- 229950006187 hexamethonium bromide Drugs 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical class C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- CYPPCCJJKNISFK-UHFFFAOYSA-J kaolinite Chemical compound [OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[O-][Si](=O)O[Si]([O-])=O CYPPCCJJKNISFK-UHFFFAOYSA-J 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 150000002826 nitrites Chemical class 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
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- 239000012254 powdered material Substances 0.000 description 1
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- 238000000371 solid-state nuclear magnetic resonance spectroscopy Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
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- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 description 1
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- FAPSXSAPXXJTOU-UHFFFAOYSA-L trimethyl-[6-(trimethylazaniumyl)hexyl]azanium;dibromide Chemical compound [Br-].[Br-].C[N+](C)(C)CCCCCC[N+](C)(C)C FAPSXSAPXXJTOU-UHFFFAOYSA-L 0.000 description 1
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| PCT/CN2015/091979 WO2016058541A1 (en) | 2014-10-15 | 2015-10-15 | Solidothermal synthesis of zeolitic materials and zeolites obtained therefrom |
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| JP2017532282A JP2017532282A (ja) | 2017-11-02 |
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| WO2016058541A1 (en) | 2014-10-15 | 2016-04-21 | Basf Se | Solidothermal synthesis of zeolitic materials and zeolites obtained therefrom |
| KR102558113B1 (ko) | 2015-02-12 | 2023-07-24 | 바스프 에스이 | Bea 골격 구조를 갖는 탈알루미늄화된 제올라이트 물질의 제조 방법 |
| EP3292099B1 (en) | 2015-05-04 | 2020-07-22 | Basf Se | Process for the preparation of melonal |
| EP3322686B1 (en) | 2015-07-15 | 2019-09-11 | Basf Se | Process for preparing an arylpropene |
| JP2018538284A (ja) | 2015-11-27 | 2018-12-27 | ビーエーエスエフ ソシエタス・ヨーロピアＢａｓｆ Ｓｅ | 金属−有機骨格体の超高速高空時収量合成 |
| PL3386919T3 (pl) | 2015-12-08 | 2022-02-21 | Basf Se | Zawierający cynę materiał zeolitowy o strukturze szkieletowej bea |
| EP3178788A1 (en) | 2015-12-08 | 2017-06-14 | Basf Se | A tin-containing zeolitic material having a bea framework structure |
| JP6786876B2 (ja) * | 2016-05-23 | 2020-11-18 | 東ソー株式会社 | Ｃｈａ型ゼオライトの製造方法 |
| KR102470492B1 (ko) * | 2016-09-06 | 2022-11-23 | 바스프 에스이 | Mww 골격 구조를 갖는 붕소 함유 제올라이트의 고체열 합성 |
| EP3519355A4 (en) * | 2016-09-27 | 2020-04-22 | Basf Se | HIGHLY EFFICIENT SOLIDOTHERMAL SYNTHESIS OF ZEOLITHIC MATERIALS |
| MY201604A (en) * | 2018-07-27 | 2024-03-05 | Basf Mobile Emissions Catalysts Llc | Process for preparing a zeolitic material having a framework type fer |
| US20220339611A1 (en) * | 2019-09-20 | 2022-10-27 | Basf Se | Synthesis and Use of a Zeolitic Material Having the ITH Framework Structure Type |
| CN113979448B (zh) * | 2020-07-27 | 2023-05-02 | 中国石油化工股份有限公司 | 含氟zsm-35分子筛及其制备方法 |
| JP2024508239A (ja) * | 2021-02-03 | 2024-02-26 | ビーエーエスエフ コーポレーション | Ｃｈａ様骨格構造を有するゼオライト材料及びその合成 |
| US11565943B2 (en) * | 2021-02-11 | 2023-01-31 | Chevron U.S.A. Inc. | Synthesis of ton framework type molecular sieves |
| US20220347663A1 (en) * | 2021-04-27 | 2022-11-03 | Chevron U.S.A. Inc. | Ferrosilicate ssz-70 molcular sieve, its synthesis and use |
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| DE4407872C2 (de) | 1994-03-04 | 2003-10-23 | Alsi Penta Zeolithe Gmbh | Verfahren zur Herstellung von hochsiliciumhaltigen Zeolithen |
| CN1214978C (zh) * | 2003-03-20 | 2005-08-17 | 吉林大学 | 具有超高水热稳定的有序介孔分子筛材料及其合成方法 |
| WO2008058398A1 (en) * | 2006-11-16 | 2008-05-22 | UNIVERSITé LAVAL | Nanozeolites and process for preparation thereof |
| JP5278866B2 (ja) * | 2006-12-03 | 2013-09-04 | 独立行政法人産業技術総合研究所 | Ｃｄｏ型高シリカゼオライトの前駆体となる層状ケイ酸塩及びその製造方法 |
| ES2303787B2 (es) | 2007-02-01 | 2009-06-12 | Universidad Politecnica De Valencia | "material cristalino microporoso de naturaleza zeolitica, zeolita itq-39, procedimiento de preparacion y usos". |
| JP5898187B2 (ja) | 2010-06-18 | 2016-04-06 | ビーエーエスエフ ソシエタス・ヨーロピアＢａｓｆ Ｓｅ | Ｌｅｖ型構造ゼオライト系材料とその製造方法 |
| CN102627287B (zh) * | 2012-04-20 | 2014-04-16 | 浙江大学 | 通过固相原料研磨无溶剂条件下合成分子筛的方法 |
| WO2014060261A1 (en) | 2012-10-18 | 2014-04-24 | Basf Se | Post-treatment of deboronated mww zeolite |
| KR102179936B1 (ko) | 2012-10-18 | 2020-11-17 | 바스프 에스이 | 제올라이트 물질의 후처리 |
| WO2014060982A2 (en) | 2012-10-19 | 2014-04-24 | Basf Se | Catalyst for the Conversion of Syngas to Olefins and Preparation Thereof |
| CN102992343A (zh) | 2012-12-09 | 2013-03-27 | 浙江大学 | 无有机模板固相法合成沸石分子筛的方法 |
| CN103121698B (zh) * | 2013-02-01 | 2014-11-05 | 浙江大学 | 一种固相研磨合成sapo-34的方法 |
| US20150090610A1 (en) | 2013-09-27 | 2015-04-02 | Basf Corporation | Processes for filling containers in adsorbed gas systems |
| DE102014222018A1 (de) | 2013-10-29 | 2015-04-30 | China Petroleum & Chemical Corporation | Vollständig aus Si gebildetes Molekularsieb und Syntheseprozess dafür |
| CN104556087B (zh) | 2013-10-29 | 2017-11-28 | 中国石油化工股份有限公司 | 一种全硅分子筛及其合成方法 |
| CN103979574B (zh) * | 2014-06-05 | 2016-03-30 | 郑州大学 | 固相合成分子筛的方法 |
| WO2016058541A1 (en) | 2014-10-15 | 2016-04-21 | Basf Se | Solidothermal synthesis of zeolitic materials and zeolites obtained therefrom |
| CN104891520B (zh) * | 2015-06-02 | 2017-08-29 | 中国科学院上海高等研究院 | 一种固相合成多级孔分子筛的方法 |
-
2015
- 2015-10-15 WO PCT/CN2015/091979 patent/WO2016058541A1/en not_active Ceased
- 2015-10-15 US US15/518,945 patent/US10301185B2/en not_active Expired - Fee Related
- 2015-10-15 CN CN201580055841.5A patent/CN107074566A/zh active Pending
- 2015-10-15 EP EP15850244.3A patent/EP3206991A4/en not_active Withdrawn
- 2015-10-15 JP JP2017520902A patent/JP6656242B2/ja not_active Expired - Fee Related
- 2015-10-15 KR KR1020177009998A patent/KR20170070052A/ko not_active Withdrawn
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