JP5577321B2 - 特定のサイズの球状粒子から作られたメソ構造化アルミノケイ酸塩材料 - Google Patents
特定のサイズの球状粒子から作られたメソ構造化アルミノケイ酸塩材料 Download PDFInfo
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- JP5577321B2 JP5577321B2 JP2011502410A JP2011502410A JP5577321B2 JP 5577321 B2 JP5577321 B2 JP 5577321B2 JP 2011502410 A JP2011502410 A JP 2011502410A JP 2011502410 A JP2011502410 A JP 2011502410A JP 5577321 B2 JP5577321 B2 JP 5577321B2
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- 239000000463 material Substances 0.000 title claims abstract description 109
- 239000012798 spherical particle Substances 0.000 title claims abstract description 40
- 229910000323 aluminium silicate Inorganic materials 0.000 title claims abstract description 30
- 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 30
- 238000000034 method Methods 0.000 claims abstract description 65
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000011159 matrix material Substances 0.000 claims abstract description 33
- 239000011148 porous material Substances 0.000 claims abstract description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims description 54
- 239000004094 surface-active agent Substances 0.000 claims description 39
- 230000008569 process Effects 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 19
- 239000007921 spray Substances 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 17
- 238000005507 spraying Methods 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 13
- 239000012265 solid product Substances 0.000 claims description 13
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- 238000001035 drying Methods 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000003054 catalyst Substances 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 9
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
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- 238000000227 grinding Methods 0.000 claims description 3
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- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 238000007670 refining Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 description 56
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 44
- 239000002245 particle Substances 0.000 description 35
- 229910052757 nitrogen Inorganic materials 0.000 description 22
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- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 17
- 238000004458 analytical method Methods 0.000 description 16
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- 238000001179 sorption measurement Methods 0.000 description 13
- 238000004627 transmission electron microscopy Methods 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 11
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 10
- 238000009826 distribution Methods 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 229910004298 SiO 2 Inorganic materials 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 9
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- 239000012071 phase Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 6
- 238000001338 self-assembly Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 5
- 239000000693 micelle Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 229920001983 poloxamer Polymers 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000002736 nonionic surfactant Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229920001451 polypropylene glycol Polymers 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004876 x-ray fluorescence Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- -1 chloro alkoxide Chemical group 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000006482 condensation reaction Methods 0.000 description 3
- 238000003618 dip coating Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000002563 ionic surfactant Substances 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000008520 organization Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000012800 visualization Methods 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011805 ball Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000000875 corresponding effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 102220500397 Neutral and basic amino acid transport protein rBAT_M41T_mutation Human genes 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 108010039918 Polylysine Proteins 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- 229920002359 Tetronic® Polymers 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229940072056 alginate Drugs 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000005899 aromatization reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- 230000004888 barrier function Effects 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
- 239000011230 binding agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- QMNOIORHZMRPLS-UHFFFAOYSA-N butan-1-ol;ethane-1,2-diol;propane-1,2-diol Chemical compound OCCO.CCCCO.CC(O)CO QMNOIORHZMRPLS-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000020335 dealkylation Effects 0.000 description 1
- 238000006900 dealkylation reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 239000000412 dendrimer Substances 0.000 description 1
- 229920000736 dendritic polymer Polymers 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 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
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-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
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 150000002367 halogens Chemical group 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 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 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000006384 oligomerization reaction Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003791 organic solvent mixture Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920001308 poly(aminoacid) Polymers 0.000 description 1
- 229920000656 polylysine Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 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
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001330 spinodal decomposition reaction Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 description 1
- 238000010555 transalkylation reaction Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—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
- C01B39/04—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 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Description
本発明は、少なくとも2つの基本球状粒子からなるメソ構造化アルミノケイ酸塩材料であって、前記球状粒子はそれぞれ酸化ケイ素および酸化アルミニウムをベースとするマトリクスからなり、前記マトリクスの細孔径は1.5〜30nmの範囲であり、Si/Alモル比は1以上であり、無定形壁の厚さは1〜30nmの範囲であり、前記基本球状粒子の径Dは10<D(μm)≦100である、メソ構造化アルミノケイ酸塩材料に関する。本発明による材料のアルミニウム含有量は多く、Si/Alモル比は好ましくは1〜10にわたる。
本発明によるアルミノケイ酸塩材料は、基本球状粒子からなるメソ構造化材料であり、前記粒子はそれぞれ酸化ケイ素および酸化アルミニウムをベースとするマトリクスからなる。前記マトリクスは、メソ構造化されており、1〜30nmの厚さの無定形壁と、1.5〜30nmの均一な細孔径と、1以上のSi/Alモル比を有する。前記基本球状粒子の径D(ミクロンで表される)は、10<D(μm)≦100であり、好ましくは、11〜70μmの範囲である。出願人によるEISA法の実施および制御によってこれらの粒子のサイズが制御可能となることにより、およびこれらの粒子の形状が完全に球状であることにより、本発明による材料を、精製および石油化学の分野において適用される触媒および吸着剤として用いる際、均質でない、すなわち、不規則な形状の基本粒子の形態の当該技術の状況において知られた材料と比べて、化合物の拡散のより良い制御が可能となる。本発明による材料の前記粒子のそれぞれを構成するマトリクスのSi/Alモル比は、有利には1〜10であり、より有利には1〜5である。本発明による材料のアルミニウム含有量は多く、これが本発明による材料に、触媒用途としては興味深い酸−塩基特性を与える。本発明による材料はまた、メソ細孔スケールで示す、組織化された細孔性において特に興味深い。
本発明の対象は、少なくとも2つの基本球状粒子からなるメソ構造化アルミノケイ酸塩材料であって、前記球状粒子はそれぞれ酸化ケイ素および酸化アルミニウムをベースとするメソ構造化マトリクスからなり、前記メソ構造化マトリクスの細孔径は1.5〜30nmの範囲であり、Si/Alモル比は1以上であり、無定形壁の厚さは1〜30nmの範囲であり、前記基本球状粒子の径Dは10μm超かつ100μm以下(10<D(μm)≦100)である、ものである。
以下、実施例において、用いられるエアロゾル技術は、本発明の明細書において上述した技術である。
1kgの三塩化アルミニウム六水和物をエタノール10kg、水5L、HCl 36mL、および界面活性剤CTAB1.4kgを含む溶液に添加する。集合物を、周囲温度で、アルミナ前駆体が完全に溶解するまで攪拌したままにする。次いで、3.6kgのオルトケイ酸テトラエチル(tetraethylorthosilicate:TEOS)を添加する。周囲温度で10分間攪拌した後、集合物を、乾燥空気/窒素混合物であるキャリアガスが送られる室内に「一流体型」スプレーノズルによって噴霧する。噴霧により得られた小滴を、本発明の明細書に上記された手順によって、本発明の主要な方法の段階c)に従い、100〜120℃で乾燥させる。粒子をバッグフィルター中に集める。前記粒子を、ジェットミルを用いて数μm(3〜5μm)になるまで粉砕する。次いで、粉砕された粒子の30重量%分を最初の溶液と同じ配合を有する溶液へと再び供給した後、懸濁液を上述の「一流体型」ノズルによって再び噴霧し、その後小滴を本発明の明細書に上記された手順によって、本発明の主要な方法の段階g)に従い、100〜120℃で乾燥させる。次いで、バッグフィルター中に集められた粉体をT=550℃で5時間にわたり空気中で焼成し、界面活性剤(CTAB)を除去する。本発明による主要な方法の第2の噴霧(段階e))の前の、懸濁液中に存在する不揮発性化合物の体積百分率は、10.4%である。固体物は、小角X線回折、窒素吸着等温線分析、透過型電子顕微鏡法、およびX線蛍光によって特徴づけられる。透過型電子顕微鏡法による分析は、最終材料が、バーミキュラ状の構造によって特徴付けられる組織化されたメソ多孔性を有することを示す。窒素吸着等温線分析により、最終材料の比表面積がSBET=800m2/gであり、メソ細孔径がφ=2.4nmであることがわかる。小角X線回折分析により、角度2θ=2.4にある相関ピークが可視化されるに至る。ブラッグの関係式:2d*sin(1.2)=1.5406によって、メソ構造化マトリクスの細孔間の相関距離dの計算が可能となり、すなわち、d=3.7nmである。式e=d−φによって定義されるメソ構造化材料の壁の厚みは、従ってe=1.3nmである。従って、このようにして得られた基本球状粒子のSEM画像は、これらの粒子が15〜100μmの範囲にわたる径によって特徴付けられるサイズを有することを示し、これらの粒子のサイズ分布はおよそ50μmである。
520gの三塩化アルミニウム六水和物をエタノール10kg、水5L、HCl 36mL、および1.4kgの界面活性剤P123を含む溶液に添加する。集合物を、周囲温度で、アルミナ前駆体が完全に溶解するまで攪拌したままにする。次いで、4.0kgのオルトケイ酸テトラエチル(TEOS)を添加する。周囲温度で18時間攪拌した後、集合物を、乾燥空気/窒素混合物であるキャリアガスが送られる室内に「一流体型」スプレーノズルによって噴霧する。噴霧により得られた小滴を、本発明の明細書に上記された手順によって、本発明の主要な方法の段階c)に従い、100〜120℃で乾燥させる。粒子をバッグフィルター中に集める。前記粒子を、ジェットミルを用いて数μm(3〜5μm)になるまで粉砕する。次いで、粉砕された粒子の30重量%分を最初の溶液と同じ配合を有する溶液へと再び供給した後、懸濁液を上述の「一流体型」ノズルによって再び噴霧し、その後小滴を本発明の明細書に上記された手順によって、本発明の主要な方法の段階g)に従い、100〜120℃で乾燥させる。次いで、バッグフィルター中に集められた粉体をT=550℃で5時間にわたり空気中で焼成し、界面活性剤(P123)を除去する。本発明による主要な方法の第二噴霧(段階e))の前の、懸濁液中に存在する不揮発性化合物の体積百分率は、10.4%である。固体物は、小角X線回折、窒素吸着等温線分析、透過型電子顕微鏡法、およびX線蛍光によって特徴づけられる。透過型電子顕微鏡法による分析は、最終材料が、バーミキュラ状の構造によって特徴付けられる組織化されたメソ多孔性を有することを示す。窒素吸着等温線分析により、最終材料の比表面積がSBET=420m2/gであり、メソ細孔径がφ=5.3nmであることがわかる。小角X線回折分析により、角度2θ=0.72にある相関ピークが可視化されるに至る。ブラッグの関係式:2d*sin(0.36)=1.5406によって、メソ構造化マトリクスの細孔間の相関距離dの計算が可能となり、すなわち、d=12.2nmである。式e=d−φによって定義されるメソ構造化材料の壁の厚みは、従ってe=6.9nmである。従って、このようにして得られた基本球状粒子のSEM画像は、これらの粒子が15〜100μmの範囲にわたる径によって特徴付けられるサイズを有することを示し、これらの粒子のサイズ分布はおよそ50μmである。
520gの三塩化アルミニウム六水和物をエタノール10kg、水5L、HCl 36mL、および1.4kgの界面活性剤P123を含む溶液に添加する。集合物を、周囲温度で、アルミナ前駆体が完全に溶解するまで攪拌したままにする。次いで、4.0kgのオルトケイ酸テトラエチル(TEOS)を添加する。周囲温度で18時間攪拌した後、集合物を、乾燥空気/窒素混合物であるキャリアガスが送られる室内に「一流体型」スプレーノズルによって噴霧する。噴霧により得られた小滴を、本発明の明細書に上記された手順によって、本発明の単純化された方法の段階c)に従い、100〜120℃で乾燥させる。粉体の形態の粒子をバッグフィルター中に集め、次いで、この粉体をT=550℃で5時間にわたり空気中で焼成し、界面活性剤(P123)を除去する。噴霧の前の、溶液中に存在する不揮発性化合物の体積百分率は、10.4%である。固体物は、小角X線回折、窒素吸着等温線分析、透過型電子顕微鏡法、およびX線蛍光によって特徴づけられる。透過型電子顕微鏡法による分析は、最終材料が、バーミキュラ状の構造によって特徴付けられる組織化されたメソ多孔性を有することを示す。窒素吸着等温線分析により、最終材料の比表面積がSBET=420m2/gであり、メソ細孔径がφ=5.3nmであることがわかる。小角X線回折分析により、角度2θ=0.72にある相関ピークが可視化されるに至る。ブラッグの関係式:2d*sin(0.36)=1.5406によって、メソ構造化マトリクスの細孔間の相関距離dの計算が可能となり、すなわち、d=12.2nmである。式e=d−φによって定義されるメソ構造化材料の壁の厚みは、従ってe=6.9nmである。従って、このようにして得られた基本球状粒子のSEM画像は、これらの粒子が11〜35μmの範囲にわたる径によって特徴付けられるサイズを有することを示し、これらの粒子のサイズ分布はおよそ25μmである。
Claims (11)
- メソ構造化アルミノケイ酸塩材料であって、少なくとも2つの基本球状粒子からなり、前記球状粒子はそれぞれ酸化ケイ素および酸化アルミニウムをベースとするメソ構造化マトリクスからなり、前記メソ構造化マトリクスの細孔径は1.5〜30nmの範囲であり、Si/Alモル比は1〜5の範囲であり、無定形壁の厚さは1〜30nmの範囲であり、前記基本球状粒子の径Dは11〜70μmの範囲である、材料。
- 前記基本球状粒子の径Dは11〜50μmの範囲である、請求項1に記載の材料。
- 前記基本球状粒子の径Dは15〜50μmの範囲である、請求項2に記載の材料。
- 前記マトリクスの細孔径は1.5〜10nmの範囲である、請求項1〜3のいずれか1つに記載の材料。
- 200〜1200m2/gの範囲にわたる比表面積を有する、請求項1〜4のいずれか1つに記載の材料。
- 300〜1000m2/gの範囲にわたる比表面積を有する、請求項5に記載の材料。
- 酸化ケイ素および酸化アルミニウムをベースとする前記マトリクスは、六方晶系、バーミキュラ状、または立方晶系の構造を有する、請求項1〜6のいずれか1つに記載の材料。
- 請求項1〜7のいずれか1つに記載のメソ構造化アルミノケイ酸塩材料を調製する方法であって、
a)少なくとも1種の界面活性剤と、少なくとも1種のアルミナ前駆体と、少なくとも1種のシリカ前駆体とを溶液に混合する段階;
b)スプレーノズルを用いて段階a)において得られた溶液をエアロゾル噴霧し、300μm以下の径の液状小滴を形成させる段階;
c)前記小滴を乾燥させる段階;
d)段階c)において得られた固体生成物を粉砕する段階;
e)少なくとも1種の界面活性剤と、少なくとも1種のアルミナ前駆体と、少なくとも1種のシリカ前駆体と、段階d)において得られた固体生成物の少なくとも一部を溶液に混合する段階;
f)スプレーノズルを用いて段階e)において得られた懸濁液をエアロゾル噴霧し、懸濁小滴を形成させる段階であって、該小滴は、本発明による材料の径D11〜70μmの範囲にある基本球状粒子の前駆体である、段階;
g)段階f)において得られた前記小滴を乾燥させる段階;および
h)段階a)および段階e)において導入された前記界面活性剤を除去して、メソ構造化多孔性材料を得る段階
を含む方法。
- 前記段階e)による懸濁液中に存在する不揮発性化合物の体積百分率は、少なくとも7%である、請求項8に記載の調製方法。
- 請求項1〜7のいずれか1つに記載のメソ構造化アルミノケイ酸塩材料を含むか、または請求項8〜9のいずれか1つに記載の方法によって調製される吸着剤。
- 請求項1〜7のいずれか1つに記載のメソ構造化アルミノケイ酸塩材料を含むか、または請求項8〜9のいずれか1つに記載の方法によって調製される炭化水素転化または有機化合物の合成用の触媒。
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FR08/01763 | 2008-03-31 | ||
PCT/FR2009/000209 WO2009122022A2 (fr) | 2008-03-31 | 2009-02-26 | Matériau aluminosilicate mesostructure forme de particules spheriques de taille specifique |
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FR3022237B1 (fr) * | 2014-06-13 | 2017-09-01 | Ifp Energies Now | Alumine mesoporeuse amorphe a distribution poreuse optimisee et son procede de preparation |
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CN109749774B (zh) * | 2019-01-31 | 2020-01-14 | 东方傲立石化有限公司 | 一种石脑油芳构化方法 |
WO2021005693A1 (ja) * | 2019-07-08 | 2021-01-14 | 株式会社ジェーエフシーテック | 炭化水素燃料から硫黄化合物を除去する吸着剤、吸着剤の製造方法、吸着剤の製造装置、硫黄化合物の除去方法および除去装置 |
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US8563135B2 (en) | 2013-10-22 |
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CN101980961B (zh) | 2016-02-10 |
WO2009122022A3 (fr) | 2009-12-10 |
ATE556989T1 (de) | 2012-05-15 |
WO2009122022A2 (fr) | 2009-10-08 |
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