JP2016523789A - スズ酸ケイ酸チタン、その製造法及びその使用 - Google Patents
スズ酸ケイ酸チタン、その製造法及びその使用 Download PDFInfo
- Publication number
- JP2016523789A JP2016523789A JP2016507098A JP2016507098A JP2016523789A JP 2016523789 A JP2016523789 A JP 2016523789A JP 2016507098 A JP2016507098 A JP 2016507098A JP 2016507098 A JP2016507098 A JP 2016507098A JP 2016523789 A JP2016523789 A JP 2016523789A
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- JP
- Japan
- Prior art keywords
- silicate
- titanium
- stannate
- solution
- present
- 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.)
- Granted
Links
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000010936 titanium Substances 0.000 title claims description 52
- 229910052719 titanium Inorganic materials 0.000 title claims description 38
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 36
- 229940071182 stannate Drugs 0.000 title claims description 35
- 125000005402 stannate group Chemical group 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- GNKTZDSRQHMHLZ-UHFFFAOYSA-N [Si].[Si].[Si].[Ti].[Ti].[Ti].[Ti].[Ti] Chemical compound [Si].[Si].[Si].[Ti].[Ti].[Ti].[Ti].[Ti] GNKTZDSRQHMHLZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 8
- 239000003463 adsorbent Substances 0.000 claims abstract description 6
- 150000002739 metals Chemical class 0.000 claims abstract description 6
- 239000011148 porous material Substances 0.000 claims description 37
- 229910052708 sodium Inorganic materials 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 150000001768 cations Chemical class 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000001179 sorption measurement Methods 0.000 claims description 12
- 238000005342 ion exchange Methods 0.000 claims description 11
- 230000032050 esterification Effects 0.000 claims description 10
- 238000005886 esterification reaction Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 9
- 229910052700 potassium Inorganic materials 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000005809 transesterification reaction Methods 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052788 barium Inorganic materials 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052758 niobium Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 229910052712 strontium Inorganic materials 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012736 aqueous medium Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000003826 tablet Substances 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 238000006845 Michael addition reaction Methods 0.000 claims description 2
- 229910052768 actinide Inorganic materials 0.000 claims description 2
- 150000001255 actinides Chemical class 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 238000003795 desorption Methods 0.000 claims description 2
- 238000006735 epoxidation reaction Methods 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 230000033444 hydroxylation Effects 0.000 claims description 2
- 238000005805 hydroxylation reaction Methods 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 230000004962 physiological condition Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 description 48
- 239000000243 solution Substances 0.000 description 42
- 239000011135 tin Substances 0.000 description 41
- 239000011734 sodium Substances 0.000 description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 11
- 229910052718 tin Inorganic materials 0.000 description 11
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 8
- 238000010304 firing Methods 0.000 description 6
- 125000004429 atom Chemical group 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 150000004760 silicates Chemical class 0.000 description 5
- -1 zirconium silicates Chemical class 0.000 description 5
- 235000019484 Rapeseed oil Nutrition 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 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 3
- 229910008484 TiSi Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000017 hydrogel Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 150000004702 methyl esters Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 150000003608 titanium Chemical class 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 2
- 101100065719 Drosophila melanogaster Ets98B gene Proteins 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229910008487 TiSn Inorganic materials 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical class [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 229940079864 sodium stannate Drugs 0.000 description 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- UBZYKBZMAMTNKW-UHFFFAOYSA-J titanium tetrabromide Chemical compound Br[Ti](Br)(Br)Br UBZYKBZMAMTNKW-UHFFFAOYSA-J 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 1
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
Classifications
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
-
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
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- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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- B01J35/615—100-500 m2/g
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- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B01J35/635—0.5-1.0 ml/g
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Abstract
Description
Mv+ wTixSiySnzO2x+2y+2z+0.5vw
(式中、Mはプロトン,アンモニウム、金属又は金属の混合物の少なくとも1つであり、vは、正の整数であるMの原子価であり、x、y、z及びwはモル比であり:
xは1であり、
yは0.01〜99であり、
zは0.01〜99であり、
wは0.01〜50である)を有する、非晶質スズ酸ケイ酸チタン(titanium stannate silicate)を提供する。
0.29:1:1.02:0.06のモル比を有するNa:Ti:Si:Snの製造
95gの脱塩水を含む容器内で、27.6mLの30% NaOH溶液、10mLの27% Na2SiO3溶液、及び6.8mLの13.5重量%のNa2SnO3溶液を溶解させた。この容器内の溶液を溶液Aと呼ぶ。112gの脱塩水を含む他の容器内に、16mLの35% TiOCl2溶液を加えた。この容器内の溶液を溶液Bと呼ぶ。次いで、溶液Aを、激しく撹拌しながら、溶液Bに5分間で加える。添加が完了した後、混合物を更に10分間混合し続ける。溶液のpHは7.5〜7.9の範囲にあるべきであり、必要であれば、希HCl又は希NaOHを用いてpHを調整する。次いで、試料を4時間以上(4日以内)、熟成させる。スラリーをろ過し、残留した物質を110℃で一晩、オーブンで乾燥させた。得られた白色固体を顆粒状にし、425μmのふるいでふるいにかけ、水で再スラリー化し、1時間撹拌した。次いで、スラリーをろ過し、脱塩水で、洗浄水の伝導率が200μS/cm以下になるまで洗浄した。得られた白色の物質を110℃で一晩、オーブンで乾燥させた。方法により、約12.5gの白色固体が生成された。
0.23:1:0.34:0.18のモル比を有するNa:Ti:Si:Snの製造
異なる量の出発材料を使用し、実施例1に記載されたのと同様の工程を使用した。溶液Aは、95gの脱塩水、26.7mLの30% NaOH溶液、3.4mLの27% Na2SiO3溶液、及び20mLの13.5重量%のNa2SnO3溶液を含んでいた。溶液Bは実施例1と同様であった。約10.8gの白色固体が生成された。
材料は非晶質であり(XRD)、0.23:1:0.34:0.18のNa:Ti:Si:Snモル比、0.48mL/gの細孔容積を有し、BET比表面積=431m2/g、平均孔径=51Åであった。
H + で交換された材料
異なる量の出発材料を用い、実施例1に記載されたのと同様の方法を使用した。溶液Aは、380gの脱塩水、105mLの30% NaOH溶液、13.7mLの27% Na2SiO3溶液、及び80.8mLの13.5重量%のNa2SnO3溶液を含んでいた。溶液Bは、64.5mLの35% TiOCl2溶液を450gの脱塩水に加えることにより調製した。次いで、溶液Aを、激しく撹拌しながら、溶液Bに10分間で加える。添加が完了した後、混合物を更に10分間混合し続ける。溶液のpHは7.5〜7.9の範囲にあるべきであり、必要であれば、希HCl又は希NaOHを用いてpHを調整する。混合物に40gのNaClを加えた(任意)。次いで、試料を4時間以上熟成させる。スラリーをろ過し、残留した物質を110℃で一晩、オーブンで乾燥させた。乾燥後、白色固体を顆粒状にし、425μmのふるいでふるいにかけ、水で再スラリー化し、pH2.0(10% HClを用いてpHを調整)で1時間撹拌した。次いで、スラリーをろ過し、脱塩水で、洗浄水の伝導率が200μS/cm以下になるまで洗浄した。得られた白色の物質を110℃で一晩、オーブンで乾燥させた。方法により、約40.7gの白色固体が生成された。
Siを用いない製造
異なる量の出発材料を用い、実施例1に記載されたのと同様の方法を使用した。溶液Aは、90gの脱塩水、24.3mLの30% NaOH溶液、及び25mLの13.5重量%のNa2SnO3水溶液を含んでいた。溶液Bは、100gの脱塩水、及び15mLの35% TiOCl2溶液を含んでいた。溶液Aを、激しく撹拌しながら、溶液Bに5分間で加える。添加が完了した後、混合物を更に10分間混合し続ける。溶液のpHは7.5〜7.9の範囲にあるべきであり、そうでない場合、希HCl又は希NaOHを用いてpHを調整する。混合物に10gのNaClを加えた(任意)。次いで、試料を4時間以上(4日以下)熟成させる。スラリーをろ過し、残留した物質を110℃で一晩、オーブンで乾燥させた。得られた白色固体を顆粒状にし、425μmのふるいでふるいにかけ、水で再スラリー化し、pH2.0(10% HClを用いてpHを調整)で1時間撹拌した。次いで、スラリーをろ過し、脱塩水で、洗浄水の伝導率が200μS/cm以下になるまで洗浄した。得られた白色の物質を110℃で一晩、オーブンで乾燥させた。方法により、約8.2gの白色固体が生成された。
実施例1、2、3及び4により製造した試料を、450℃で2時間、空気中で焼成した。焼成後、実施例4が結晶性のままであったのを除き、全ての試料は非晶質のままであった。
従来のTiSi合成
米国特許第5053139A号の実施例9に従い、ケイ酸チタン粉末を製造した:569.11gのTiCl4を、2リットルを製造するために十分な脱イオン水に加えることにより、2リットルの1.5M塩化チタン溶液(溶液A)を製造した。638.2gのNa2SiO3.5H2Oを、2リットルを製造するために十分な3M NaOHに加えることにより、2リットルの1.5Mケイ酸ナトリウム溶液(溶液B)を製造する。溶液Bを、激しく撹拌しながら、16cc/分の速度で溶液Aに加える。添加が完了した後、混合物を更に15分間混合し続ける。溶液のpHは7.5〜7.9の範囲にあるべきであり、そうでない場合、希HCl又は希NaOHを用いてpHを調整する。次いで、試料を2〜4日間熟成させる。熟成後、物質上のあらゆる水を捨てる。次いで、試料をろ過し、物質1リットルあたり1リットルの脱イオン水で洗浄し、4〜6リットルの脱イオン水で再スラリー化し、ろ過し、最後に物質1リットルあたり2リットルの水で再度洗浄した。
SnCl 2 を用いた、TiSi修飾による陽イオン交換
ガラスビーカー中で、実施例5により製造したケイ酸シリカ50.0gを、450mLの脱塩水中でスラリー化した。このスラリーに、29.34gのSnCl2.2H2Oを固体として加えた。混合物の色は白色から黄色に変化する。スラリーのpHは8.80から1.60に変化した。混合物を、室温で更に2時間撹拌した。2時間後、スラリーをろ過し、脱塩水で、ろ液の伝導率が20マイクロジーメンス/cm以下になるまで洗浄した。黄色がかったろ過ケーキを110℃で、オーブン中で乾燥し、48.2gの黄色の粉末を得た。得られた材料は、XRDにより非晶質であった。
錠剤の製造
実施例3の材料を、グラファイトと混合し、1.5×1.5mmの大きさの錠剤にした。得られた錠剤を、500℃で2時間焼成した。
同時のエステル化及びエステル交換におけるTiSiの使用
pH2.00におけるHCl処理によりNa含有量を低下させた以外は、実施例5により製造された材料から10mLのケイ酸チタン錠剤を製造した。ろ過した後、0.8重量%のNaを含有する材料を洗浄及び乾燥した。この材料を1.5×1.5mmの錠剤に打錠した。錠剤を固定層反応器に装填した。反応器に、5重量%のドデカン酸を加えたMeOH(1.73mL/h)及びなたね油(3.47mL/h)を連続的に供給した。反応条件は、180℃、28バールのN2背圧、LHSVなたね油0.347h−1(3.47mL/h)、LHSV MeOH 0.173h−1(1.73mL/h)であった。
同時のエステル化及びエステル交換におけるTiSiSnの使用
実施例3により製造した材料から、10mLのスズ酸ケイ酸チタン錠剤を製造した。錠剤を固定層反応器に装填した。反応器に、5重量%のドデカン酸を加えたMeOH(1.73mL/h)及びなたね油(3.47mL/h)を連続的に供給した。反応条件は、180℃、28バールのN2背圧、LHSVなたね油0.347h−1(3.47mL/h)、LHSV MeOH 0.173h−1(1.73mL/h)であった。
Claims (15)
- 一般式:
Mv+ wTixSiySnzO2x+2y+2z+0.5vw
(式中、Mはプロトン,アンモニウム、金属又は金属の混合物の少なくとも1つであり、vは、正の整数であるMの原子価であり、x、y、z及びwはモル比であり:
xは1であり、
yは0.01〜99であり、
zは0.01〜99であり、
wは0.01〜50である)を有する、非晶質スズ酸ケイ酸チタン。 - Mが、プロトン、アンモニウム、Na、Li、K、Cs、Ca、Mg、Sr、Ba、Fe(II)、Fe(III)、Sn(II)、Ce、La、Nb、Ni、V、W、Mo、Al、Zn、Cu、Mnの少なくとも1つである、請求項1に記載のスズ酸ケイ酸チタン。
- yが0.1〜10の範囲であり、好ましくは0.2〜5である、請求項1又は2に記載のスズ酸ケイ酸チタン。
- zが0.03〜5の範囲であり、好ましくは0.05〜1である、請求項1〜3のいずれか1項に記載のスズ酸ケイ酸チタン。
- wが0.1〜10の範囲である、請求項1〜4のいずれか1項に記載のスズ酸ケイ酸チタン。
- 前記スズ酸ケイ酸チタンが、液体窒素吸着により測定し、少なくとも0.3mL/gの細孔容積を有する、請求項1〜5のいずれか1項に記載のスズ酸ケイ酸チタン。
- 前記スズ酸ケイ酸チタンが、液体窒素吸着により測定し、少なくとも40Åの平均孔径を有する、請求項1〜6のいずれか1項に記載のスズ酸ケイ酸チタン。
- 粉末、錠剤、顆粒又は押出物の形状である、請求項1〜7のいずれか1項に記載のスズ酸ケイ酸チタン。
- 可溶性ケイ酸塩原料、可溶性スズ酸塩原料、及び可溶性チタン原料間の水性媒体中での沈殿反応を含み、それによってスズ酸ケイ酸チタンを沈殿させ、分離させることを含む、請求項1〜8のいずれか1項に記載のスズ酸ケイ酸チタンの製造方法。
- プロトン、アンモニウム、Na、Li、K、Cs、Ca、Mg、Sr、Ba、Fe(II)、Fe(III)、Sn(II)、Ce、La、Nb、Ni、V、W、Mo、Al、Zn、Cu、Mnイオン、及びそれらの組合せから選択される陽イオンによるイオン交換工程を更に含む、請求項9に記載の方法。
- 前記スズ酸ケイ酸チタンを、200℃を超える温度で更に焼成することを含む、請求項9〜10のいずれか1項に記載の方法。
- 化学反応における触媒若しくは触媒担体として、又は吸着剤としての、請求項1〜8のいずれか1項に記載のスズ酸ケイ酸チタンの使用。
- 前記化学反応が、エステル化、マイケル付加、エステル交換、酸化、エポキシ化、又はヒドロキシル化である、請求項12に記載の使用。
- 水溶液からの、放射性核種、好ましくは90Sr又はアクチニドの吸着及び除去のための、請求項12に記載の使用。
- 生理的条件下における、金属、好ましくは、Pt(II)、Pt(IV)、Pd、Gd、Hg、Cd、Au又はHoの選択的吸着又は脱離のための、請求項12に記載の使用。
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CA2909405A1 (en) | 2014-10-16 |
CA2909405C (en) | 2018-11-20 |
CN105339304B (zh) | 2018-02-13 |
AR095849A1 (es) | 2015-11-18 |
TWI637909B (zh) | 2018-10-11 |
KR20160006679A (ko) | 2016-01-19 |
WO2014167524A1 (en) | 2014-10-16 |
BR112015025752A2 (pt) | 2017-07-18 |
CN105339304A (zh) | 2016-02-17 |
EP2984036B1 (en) | 2020-03-11 |
US20160067677A1 (en) | 2016-03-10 |
US10814310B2 (en) | 2020-10-27 |
EP2984036A1 (en) | 2016-02-17 |
KR101773694B1 (ko) | 2017-08-31 |
TW201446651A (zh) | 2014-12-16 |
MY194298A (en) | 2022-11-27 |
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