DK1719737T3 - FREMGANGSMÅDE TIL FREMSTILLING AF ET TEMPERATURSTABILT TiO2/SiO2-BLANDINGSOXID OG DETS ANVENDELSE SOM KATALYSATORBÆRER - Google Patents
FREMGANGSMÅDE TIL FREMSTILLING AF ET TEMPERATURSTABILT TiO2/SiO2-BLANDINGSOXID OG DETS ANVENDELSE SOM KATALYSATORBÆRER Download PDFInfo
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- DK1719737T3 DK1719737T3 DK06009137.8T DK06009137T DK1719737T3 DK 1719737 T3 DK1719737 T3 DK 1719737T3 DK 06009137 T DK06009137 T DK 06009137T DK 1719737 T3 DK1719737 T3 DK 1719737T3
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- Prior art keywords
- hydrolysis
- silicic acid
- process according
- titanium
- compound
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 153
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 115
- 229910052681 coesite Inorganic materials 0.000 title claims description 101
- 229910052906 cristobalite Inorganic materials 0.000 title claims description 101
- 229910052682 stishovite Inorganic materials 0.000 title claims description 101
- 229910052905 tridymite Inorganic materials 0.000 title claims description 101
- 238000000034 method Methods 0.000 title claims description 55
- 235000012239 silicon dioxide Nutrition 0.000 title claims description 55
- 239000003054 catalyst Substances 0.000 title claims description 46
- 239000000377 silicon dioxide Substances 0.000 title claims description 11
- 239000000203 mixture Substances 0.000 title claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 76
- 239000010936 titanium Substances 0.000 claims description 65
- 229910052719 titanium Inorganic materials 0.000 claims description 65
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 54
- 230000007062 hydrolysis Effects 0.000 claims description 54
- 239000011148 porous material Substances 0.000 claims description 53
- 230000032683 aging Effects 0.000 claims description 48
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 48
- 230000008569 process Effects 0.000 claims description 43
- 238000001354 calcination Methods 0.000 claims description 25
- 239000002002 slurry Substances 0.000 claims description 16
- -1 silicic acid compound Chemical class 0.000 claims description 12
- 239000003729 cation exchange resin Substances 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 150000003609 titanium compounds Chemical class 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 6
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 229940023913 cation exchange resins Drugs 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 238000004448 titration Methods 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
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- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 150000004677 hydrates Chemical class 0.000 claims 4
- 150000003628 tricarboxylic acids Chemical class 0.000 claims 4
- 150000001413 amino acids Chemical class 0.000 claims 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims 2
- 229910052751 metal Inorganic materials 0.000 claims 2
- 239000002184 metal Substances 0.000 claims 2
- 150000002739 metals Chemical class 0.000 claims 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims 1
- 229910004283 SiO 4 Inorganic materials 0.000 claims 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims 1
- 125000003277 amino group Chemical group 0.000 claims 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims 1
- 150000001768 cations Chemical class 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 229910052802 copper Inorganic materials 0.000 claims 1
- 238000004821 distillation Methods 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- 150000002736 metal compounds Chemical class 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 125000004043 oxo group Chemical group O=* 0.000 claims 1
- 229910052763 palladium Inorganic materials 0.000 claims 1
- 230000002093 peripheral effect Effects 0.000 claims 1
- 229910052697 platinum Inorganic materials 0.000 claims 1
- 229910052707 ruthenium Inorganic materials 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 239000000969 carrier Substances 0.000 description 35
- 229960004029 silicic acid Drugs 0.000 description 31
- 239000000047 product Substances 0.000 description 26
- 238000002441 X-ray diffraction Methods 0.000 description 19
- 239000000725 suspension Substances 0.000 description 16
- LMHHRCOWPQNFTF-UHFFFAOYSA-N s-propan-2-yl azepane-1-carbothioate Chemical compound CC(C)SC(=O)N1CCCCCC1 LMHHRCOWPQNFTF-UHFFFAOYSA-N 0.000 description 14
- 239000000126 substance Substances 0.000 description 14
- 235000010215 titanium dioxide Nutrition 0.000 description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 11
- 239000004408 titanium dioxide Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- KTXWGMUMDPYXNN-UHFFFAOYSA-N 2-ethylhexan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCCC(CC)C[O-].CCCCC(CC)C[O-].CCCCC(CC)C[O-].CCCCC(CC)C[O-] KTXWGMUMDPYXNN-UHFFFAOYSA-N 0.000 description 5
- 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 5
- 230000003197 catalytic effect Effects 0.000 description 5
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- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 4
- 230000011514 reflex Effects 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
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- KOARADCEQDEFIO-UHFFFAOYSA-N hexan-1-olate;titanium(4+) Chemical compound CCCCCCO[Ti](OCCCCCC)(OCCCCCC)OCCCCCC KOARADCEQDEFIO-UHFFFAOYSA-N 0.000 description 3
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- 239000011777 magnesium Substances 0.000 description 3
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- 230000000704 physical effect Effects 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
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- 238000001256 steam distillation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000264877 Hippospongia communis Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- PWCPICBHDZRXLL-UHFFFAOYSA-N [Ti+4].CCC(CC)C[O-].CCC(CC)C[O-].CCC(CC)C[O-].CCC(CC)C[O-] Chemical compound [Ti+4].CCC(CC)C[O-].CCC(CC)C[O-].CCC(CC)C[O-].CCC(CC)C[O-] PWCPICBHDZRXLL-UHFFFAOYSA-N 0.000 description 2
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 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
- 229910010165 TiCu Inorganic materials 0.000 description 1
- 229910026551 ZrC Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- CXRBBEVQTFFESQ-UHFFFAOYSA-N [Ti+4].CCCCCCC(C[O-])CCCC.CCCCCCC(C[O-])CCCC.CCCCCCC(C[O-])CCCC.CCCCCCC(C[O-])CCCC Chemical compound [Ti+4].CCCCCCC(C[O-])CCCC.CCCCCCC(C[O-])CCCC.CCCCCCC(C[O-])CCCC.CCCCCCC(C[O-])CCCC CXRBBEVQTFFESQ-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
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- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
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- 239000003546 flue gas Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
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- MKWYFZFMAMBPQK-UHFFFAOYSA-J sodium feredetate Chemical compound [Na+].[Fe+3].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O MKWYFZFMAMBPQK-UHFFFAOYSA-J 0.000 description 1
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- DVQHRBFGRZHMSR-UHFFFAOYSA-N sodium methyl 2,2-dimethyl-4,6-dioxo-5-(N-prop-2-enoxy-C-propylcarbonimidoyl)cyclohexane-1-carboxylate Chemical compound [Na+].C=CCON=C(CCC)[C-]1C(=O)CC(C)(C)C(C(=O)OC)C1=O DVQHRBFGRZHMSR-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
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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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- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- B01J35/613—
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
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- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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Claims (24)
1. Fremgangsmåde til fremstilling af Ti02/Si02-blandingsoxider eller deres hydrater og/eller oxidhydrater, indeholdende 0,5 til 95 vægt-% Si, baseret på summen af Ti og Si og beregnet som Si02 og Ti02, ved sammenføring af en titanforbindelse eller dens hydrolyseprodukt med en kiselsyreforbindelse i et vandigt miljø, hvor - titanforbindelsen er eller omfatter et titanalkoholat, udvisende mindst én C1-til C6-alkoholatgruppe, - fremgangsmåden omfatter hydrolyse af titanforbindelsen, idet hydrolysen af titanforbindelsen finder sted i nærvær eller fravær af kiselsyreforbindelsen, og - kiselsyreforbindelsen er fremstillet via kationbyttere, kiselsyreforbindelsen er en vandig kiselsyresol, der indeholder kiselsyre, og kiselsyreforbindelsen har en gennemsnitlig partikeldiameter fra 1,8 til 6 nm, bestemt ved titrering ifølge Sears.
2. Fremgangsmåde ifølge krav 1, kendetegnet ved, at fremgangsmåden endvidere omfatter mindst 30 min. tørring af det fremkomne produkt og/eller kalcinering ved over 350°C, især over 550°C.
3. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at hydrolysen af titanforbindelsen finder sted ved 25 til 100°C, idet der, når hydrolysen gennemføres i nærvær af ammoniumhydrogencarbonat eller aminosyrer, foretrækkes hydrolysetemperaturer fra 25 til 35°C og i fravær deraf foretrækkes hydrolysetemperaturer fra 70 til 100°C.
4. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at kiselsyresolen indeholder 1,0 til 8,0 vægt-%, fortrinsvis 2,0 til 5,0 vægt-% kiselsyre, beregnet som Si02.
5. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at fremgangsmåden endvidere omfatter fjernelse af overskydende alkohol ved azeotrop vanddampdestillation, idet fjernelsen finder sted efter trinnet til hydrolysen af titanforbindelsen eller efter tilsætningen af kiselsyreforbindelsen, fortrinsvis efter tilsætningen af kiselsyreforbindelsen.
6. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at der før, under eller efter tilsætningen af kiselsyreforbindelsen, fortrinsvis efter tilsætningen af kiselsyreforbindelsen, udføres en hydrotermisk ældning ved temperaturer fra 90 til 235°C, fortrinsvis fra 150 til 210°C, over mindst 1 time, fortrinsvis fra 4 til 24 timer og uafhængigt heraf, især ved det tryk, der dannes under disse temperaturer i en lukket beholder, og den hydrotermiske ældning eventuelt også i form af flere behandlingstrin finder sted ved forskellige temperaturer og tryk.
7. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at hydrolysen og/eller den hydrotemiske ældning finder sted i nærvær af tilsætninger, valgt fra gruppen omfattende ammoniak, ammoniumhydrogencarbonat, aminosyrer og mono-, di- og tricarboxylsyrer eller deres blandinger, især blandingerne omfattende - ammoniak og aminosyrer, - ammoniak på den ene side og mono-, di- og/eller tricarboxylsyrer på den anden side, og - aminosyrer på den ene side og mono-, di- og/eller tricarboxylsyrer på den anden side, hvor mono-, di- og/eller tricarboxylsyrerne eventuelt yderligere er substitueret med mindst én hydroxy- eller carboxyl- eller oxo- og/eller aminogruppe.
8. Fremgangsmåde ifølge krav 7, kendetegnet ved, at tilsætningerne anvendes i mængder fra 0,1 til 8,0 vægt-%, fortrinsvis 0,2 til 2,5 vægt-%.
9. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at hydrolysen og/eller den hydrotermiske ældning finder sted ved en phl-værdi for den fremkomne vandige opslæmning på mindre end pH = 10,0, fortrinsvis mindre end pH = 7,0. 3
10. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at det fremkomne blandingsoxidprodukt tørres ved spraytørring.
11. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at Ti02/SiC>2-blandingsoxidet eller dets hydrater og/eller oxidhydrater indeholder mere end 5 og mindre end 40 vægt-% Si, især mindre end 25 vægt-% Si, baseret på summen af Ti og Si og beregnet som Si02 og Ti02.
12. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at titanforbindelsen hydrolyseres i nærvær af kiselsyreforbindelsen.
13. Fremgangsmåde ifølge ét af kravene 1 til 11, kendetegnet ved, at titanforbindelsen først hydrolyseres, alkoholforbindelserne eventuelt fjernes, og kiselsyreforbindelsen efterfølgende tilsættes.
14. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at kiselsyreforbindelsen i vandig opløsning har en gennemsnitlig partikeldiameter på fra 1,8 til 3 nm, bestemt ved titrering ifølge Sears.
15. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at kiselsyresolen har en viskositet på mindre end 10 mPas ved 25°C.
16. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at kiselsyreforbindelsen indføres under anvendelse af kationbytterharpikser og indføring af natriumvandglas (Na4Si04) eller dettes oligomere, og fortrinsvis inden for 24 timer efter fremstilling.
17. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at der under hydrolysen og/eller under den hydrotermiske ældning foregår en blandingsenergitilførsel, der svarer til en omrørerperiferihastighed på fra 1 til 6 m/s, fortrinsvis 1,5 til 5 m/s.
18. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at mindst 90 vægt-% af titanforbindelsen er hydrolyserbar og uafhængigt heraf er mindst 60 vægt-% et titanalkoholat.
19. Fremgangsmåde ifølge ét af de foregående krav, kendetegnet ved, at kiselsyreforbindelsen i form af den vandige kiselsyresol er i det væsentlige fri for kiselsyresalte med under 300 ppm, især under 200 ppm, metalioner, fortrinsvis inklusive ammonium.
20. Ti02/Si02-blandingsoxid, kendetegnet ved, at dette - indeholder mindre end 25 vægt-% Si02, baseret på summen af Si02 og Ti02, - baseret på Ti02-indholdet foreligger i en mængde på over 95 vægt-%, baseret på det samlede blandingsoxid, i anatasfasen, - har porerumfang på mere end 0,50 ml/g, - har et indhold af sulfat på under 200 ppm og udviser en rutilomdannelsestemperatur på over 1000 °C.
21. Blandingsoxid ifølge krav 20, kendetegnet ved, at dette har en totalrenhed på over 99,9 vægt-%, baseret på mængden af Ti02 og Si02 i forhold til den oxidiske totalmasse.
22. Blandingsoxid ifølge mindst ét af kravene 20 eller 21, kendetegnet ved, at dette kan fås ved en fremgangsmåde ifølge kravene 1 til 19.
23. Blandingsoxid ifølge mindst ét af kravene 20 til 22, kendetegnet ved, at dette har Si02-indhold på mindre end 20 vægt-% og særlig foretrukket på mindre end 15 vægt-%.
24. Anvendelse af blandingsoxidet ifølge mindst ét af kravene 20 til 23 som katalysatorbærer, især til metaller eller metalforbindelser omfattende metaller valgt fra gruppen: sølv, kobber, ruthenium, palladium, cobalt og/eller platin.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102005021623A DE102005021623A1 (de) | 2005-05-04 | 2005-05-04 | Verfahren zur Herstellung eines temperaturstabilen TiO2/SiO2 - Mischoxids und dessen Verwendung als Katalysatorträger |
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Country Status (4)
| Country | Link |
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| US (2) | US7790138B2 (da) |
| EP (1) | EP1719737B1 (da) |
| DE (1) | DE102005021623A1 (da) |
| DK (1) | DK1719737T3 (da) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20080108497A1 (en) * | 2006-11-08 | 2008-05-08 | Holland Brian T | Metal-rich siliceous compositions and methods of producing same |
| DE102008041470A1 (de) | 2008-08-22 | 2010-02-25 | Evonik Degussa Gmbh | Verwendung eines pyrogen hergestellten Silicium-Titan-Mischoxidpulvers als Katalysator |
| US8545796B2 (en) | 2009-07-31 | 2013-10-01 | Cristal Usa Inc. | Silica-stabilized ultrafine anatase titania, vanadia catalysts, and methods of production thereof |
| US9433924B2 (en) * | 2009-11-09 | 2016-09-06 | Wayne State University | Metaloxide—ZrO2 catalysts for the esterification and transesterification of free fatty acids and triglycerides to obtain bio-diesel |
| DE102010003652A1 (de) * | 2010-04-06 | 2011-10-06 | Evonik Degussa Gmbh | Siliciumdioxid und Titandioxid enthaltendes Granulat |
| DE102011051334A1 (de) * | 2010-06-29 | 2011-12-29 | Sachtleben Chemie Gmbh | Alkaliarmes Katalysatormaterial und Verfahren zu dessen Herstellung |
| PL219301B1 (pl) | 2010-11-29 | 2015-04-30 | Inst Włókiennictwa | Sposób wytwarzania barierowych materiałów włókienniczych |
| TWI651269B (zh) * | 2013-09-23 | 2019-02-21 | 歐洲泰奧色得有限公司 | 二氧化鈦粒子及其製備方法 |
| CN104258836A (zh) * | 2014-09-18 | 2015-01-07 | 安徽工程大学 | 二氧化钛/二氧化硅纳米复合材料及其制备方法和应用 |
| CN107530681B (zh) | 2015-05-15 | 2021-09-10 | 亨斯迈培爱德国有限公司 | 粉状氧化钛、其制备方法及其用途 |
| EP3257816A1 (de) * | 2016-06-14 | 2017-12-20 | Kronos International, Inc. | Herstellung von nano-partikulärem titandioxid |
| CN106044783B (zh) * | 2016-07-27 | 2019-01-04 | 昆明理工大学 | 一种二氧化硅纳米线的制备方法 |
| CN106745218B (zh) * | 2016-11-30 | 2018-05-08 | 中国科学院广州能源研究所 | 一种高温稳定二氧化钛纳米管粉体的制备方法 |
| WO2020094714A1 (en) * | 2018-11-08 | 2020-05-14 | Rhodia Operations | Precipitated silica and process for its manufacture |
| CN109499562A (zh) * | 2018-12-06 | 2019-03-22 | 怀化学院 | 二氧化钛/二氧化硅光催化剂及其制备方法 |
| CN111747445B (zh) * | 2020-07-31 | 2022-09-09 | 重庆工商大学 | 一种TiO2-SiO2氧化物复合材料及其制备方法 |
| RU2761822C1 (ru) * | 2021-06-16 | 2021-12-13 | федеральное государственное бюджетное образовательное учреждение высшего образования «Санкт-Петербургский горный университет» | СПОСОБ ПОЛУЧЕНИЯ КАРКАСНЫХ СТРУКТУР НА ОСНОВЕ SiO2-Al2O3 |
| CN114634721A (zh) * | 2022-03-01 | 2022-06-17 | 华南理工大学 | 一种硅铝氧化物包覆型二氧化钛及其制备方法和应用 |
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| US2253595A (en) * | 1938-11-26 | 1941-08-26 | Du Pont | Titanium oxide production |
| US2787586A (en) * | 1955-02-07 | 1957-04-02 | Exxon Research Engineering Co | Dehydration of isopropanol |
| US4801571A (en) * | 1986-07-31 | 1989-01-31 | Amoco Corporation | Catalyst and process for production of an alpha, beta-ethylenically unsaturated monocarboxylic acid |
| DE3739854A1 (de) | 1987-11-25 | 1989-06-08 | Philips Patentverwaltung | Verfahren zur herstellung von titandioxid-pulver |
| DE3803894A1 (de) * | 1988-02-09 | 1989-08-10 | Degussa | Presslinge auf basis von pyrogen hergestelltem titandioxid, verfahren zu ihrer herstellung und ihre verwendung |
| DE3839580C1 (da) | 1988-11-24 | 1990-07-05 | Condea Chemie Gmbh, 2212 Brunsbuettel, De | |
| US5128114A (en) * | 1989-04-14 | 1992-07-07 | E. I. Du Pont De Nemours And Company | Silica microspheres, method of improving attrition resistance |
| US5162283A (en) * | 1991-01-22 | 1992-11-10 | Mobil Oil Corporation | Highly porous amorphous titania and titania/silica phases |
| DE4322022A1 (de) * | 1993-07-02 | 1995-01-12 | Basf Ag | Kristalline Oxide des Titans |
| EP1060128A4 (en) | 1998-02-24 | 2005-08-03 | Rotem Amfert Negev Ltd | MODIFIED TITANIUM DIOXIDE AND PROCESS FOR PREPARING THE SAME |
| JP2000254493A (ja) | 1999-03-11 | 2000-09-19 | Kansai Electric Power Co Inc:The | 触媒担体用シリカ修飾チタニアの製造方法 |
| WO2001014054A1 (en) | 1999-08-23 | 2001-03-01 | Rotem Amfert Negev Ltd. | Silicon-containing titanium dioxyde, method for preparing the same and catalytic compositions thereof |
| JP3425602B2 (ja) | 1999-11-16 | 2003-07-14 | 独立行政法人産業技術総合研究所 | 結晶性酸化チタンを細孔壁とする無機多孔体及びその製造方法 |
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| Publication number | Publication date |
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| US8647599B2 (en) | 2014-02-11 |
| US7790138B2 (en) | 2010-09-07 |
| US20070003464A1 (en) | 2007-01-04 |
| EP1719737B1 (de) | 2016-03-09 |
| DE102005021623A1 (de) | 2006-11-09 |
| US20110020200A1 (en) | 2011-01-27 |
| EP1719737A1 (de) | 2006-11-08 |
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