WO2011075277A1 - Titania-containing extrudate - Google Patents
Titania-containing extrudate Download PDFInfo
- Publication number
- WO2011075277A1 WO2011075277A1 PCT/US2010/057365 US2010057365W WO2011075277A1 WO 2011075277 A1 WO2011075277 A1 WO 2011075277A1 US 2010057365 W US2010057365 W US 2010057365W WO 2011075277 A1 WO2011075277 A1 WO 2011075277A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cellulose
- extrudate
- titania
- hydroxyalkyi
- extrudates
- Prior art date
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229920002678 cellulose Polymers 0.000 claims abstract description 56
- 239000001913 cellulose Substances 0.000 claims abstract description 55
- 238000000034 method Methods 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 20
- -1 2-hydroxypropyl Chemical group 0.000 claims description 19
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 6
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims 1
- 229920013821 hydroxy alkyl cellulose Polymers 0.000 abstract description 12
- 238000001125 extrusion Methods 0.000 abstract description 11
- 125000004181 carboxyalkyl group Chemical group 0.000 abstract description 10
- 235000010980 cellulose Nutrition 0.000 description 34
- 235000010215 titanium dioxide Nutrition 0.000 description 33
- 239000003054 catalyst Substances 0.000 description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 14
- 239000001301 oxygen Substances 0.000 description 14
- 229910052760 oxygen Inorganic materials 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 9
- 238000006467 substitution reaction Methods 0.000 description 9
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000009472 formulation Methods 0.000 description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000001354 calcination Methods 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000000908 ammonium hydroxide Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 235000019445 benzyl alcohol Nutrition 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010981 drying operation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001414 amino alcohols Chemical class 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- JTWZVKMWOCBJEV-KLLFFGQPSA-N ethane-1,2-diol (2S,3R,4R,5S,6R)-2-(hydroxymethyl)-6-[(2S,3R,4S,5S,6S)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxane-3,4,5-triol (2S,3S,4R,5S,6S)-2,3,4-trimethoxy-6-(methoxymethyl)-5-[(2R,3S,4R,5S,6S)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxyoxane Chemical compound OCCO.OC[C@@H]1O[C@H](O[C@@H]2[C@@H](O)[C@H](O)[C@@H](O)O[C@H]2CO)[C@@H](O)[C@H](O)[C@H]1O.COC[C@@H]1O[C@H](O[C@H]2[C@H](COC)O[C@H](OC)[C@@H](OC)[C@@H]2OC)[C@@H](OC)[C@H](OC)[C@H]1OC JTWZVKMWOCBJEV-KLLFFGQPSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 210000003746 feather Anatomy 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000012245 magnesium oxide Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000005429 oxyalkyl group Chemical group 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920001308 poly(aminoacid) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920000909 polytetrahydrofuran Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
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- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
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- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/38—Polysaccharides or derivatives thereof
- C04B24/383—Cellulose or derivatives thereof
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- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
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- C04B26/28—Polysaccharides or derivatives thereof
- C04B26/285—Cellulose or derivatives thereof
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
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Definitions
- the invention relates to an extrudate comprising titania, a car oxyalkyl cellulose, and a hydroxyalkyl cellulose.
- Titania (or titanium dioxide) is a well-known white inorganic pigment.
- titania has other applications.
- titania can be used as a catalyst or catalyst carrier (Stiles, A. B., "Supports Other Than Alumina,” Catalyst Supports and Supported Catalysts (1987) Butterworths Publishers, pp. 57-85).
- a catalyst or catalyst carrier Stiles, A. B., "Supports Other Than Alumina,” Catalyst Supports and Supported Catalysts (1987) Butterworths Publishers, pp. 57-85.
- titania is produced as a fine powder.
- the invention is an extrudate comprising titania, a carboxyalkyl cellulose, and a hydroxyalkyl cellulose; and a process for producing the extrudate comprising (a) mixing titania, a carboxyalkyl cellulose, and a hydroxyalkyl cellulose to form a dough; and (b) extruding the dough to produce the extrudate.
- the process has improved processibility and produces extrudates with a smooth outer surface.
- the invention is an extrudate comprising titania.
- Suitable titanias can be rutile, anatase, brookite, or a mixture. Titania may be produced by the chloride process, the sulfate process, the hydrothenmal process, or the flame hydrolysis of titanium tetrachloride. Examples of suitable titanias include TiONA® DT-51 , DT-52, DT-51 D, DT-40, and DT-20 of Millennium Inorganic Chemicals.
- the extrudate comprises a carboxyalkyl cellulose.
- Cellulose is the structural component of the primary cell wall of green plants. Cellulose can be converted into many derivatives.
- the functional properties of carboxyalkyl celluloses depend on the degree of substitution of the cellulose structure (i.e., how many of the hydroxyl groups have taken part in the substitution reaction), as well as the chain length of the cellulose backbone and the degree of clustering of the substituents.
- the average number of substituted hydroxyl groups per glucose unit in cellulose derivatives is referred to as the degree of substitution (DS).
- DS degree of substitution
- a carboxymethyl celluloses is used.
- Preferred carboxymethyl celluloses have a degree of substitution of 0.5 to 0.9 (D. B. Braun and M. R. Rosen, Rheoloav Modifiers Handbook: Practical Use and Applications (2000) William Andrew Publishing, pp. 109-131 ).
- Carboxymethyl celluloses are known as extrusion aids (U.S. Pat. Nos. 5,884,138 and 6,709,570; U.S. Pat. Appl. Pub. No. 2008/0146721 ).
- Carboxyalkyl cellulose, R H, alkyl
- the extrudate also comprises a hydroxyalkyl cellulose.
- a hydroxyalkyl cellulose is a derivative of cellulose in which some of the hydroxy I groups in the repeating glucose units are hydroxyalkylated. Some of the hydroxy I groups in a hydroxyalkyl cellulose may also be alkylated.
- the hydroxyalkyl group is selected from the group consisting of 2-hydroxyethyl, 2-hydroxypropyl, and mixtures thereof. More preferably the hydroxyalkyl cellulose is alkylated.
- the hydroxyalkyl cellulose is selected from the group consisting of methyl 2-hydroxyethyl cellulose, methyl 2- hydroxypropyl cellulose, and mixtures thereof.
- the degree of methyl substitution is from 1 to 2, more preferably from 1.5 to 1.8; and the 2-hydroxyethyl or 2- hydroxypropyl molar substitution is from 0.1 to 0.3.
- METHOCELTM K4M cellulose derivative a product of The Dow Chemical Company having a methyl substitution of 1.4 and a hydroxypropyl molar substitution of 0.21 , Is preferably used.
- Hydroxyalkyl celluloses are known as extrusion aids (U.S. Pat. Nos. 5,884,138, 6,316,383, and 6,709,570).
- the extrudate may comprise an inorganic oxide other than titania, e.g., silicas, aluminas, zirconias, magnesias, silica-aluminas, silica-magnesias, zeolites, clays, and the like, and mixtures thereof.
- Suitable silicas include, e.g., silica gel, precipitated silica, and fumed silica.
- the weight ratio of other inorganic oxides to the titania is preferably less than 50:50, more preferably less than 20:80, most preferably less than 10:90.
- the weight ratio of the carboxyaikyl cellulose to the titania is preferably from 0.2:100 to 5:100, more preferably from 0.5:100 to 4:100, most preferably from 1 :100 to 3:100.
- the weight ratio of the hydroxyaikyi cellulose to the titania is preferably from 0.1 :100 to 2.5:100, more preferably from 0.2:100 to 2:100, most preferably from 0.5:100 to 1 :100.
- the weight ratio of the carboxyaikyl cellulose to the hydroxyaikyi cellulose is preferably from 5:1 to 1 :2, more preferably from 3:1 to 1 :1.
- the titania, the carboxyaikyl cellulose, and the hydroxyaikyi cellulose are made into a well-mixed dough.
- a solvent may be used. Suitable solvents include water, alcohols, ethers, esters, amides, aromatic compounds, halogenated compounds, and the like, and mixtures thereof. Preferred solvents are water, alcohols, and their mixtures. Suitable alcohols include methanol, ethanol, isopropanol, tert-butanol, and benzyl alcohol.
- a titania sol may be used as the source of the titania.
- a titania sol is a colloidal suspension of titania particles in a liquid.
- a titania sol can be prepared by hydrolyzing a titania precursor. Suitable titania precursors include titanium salts, titanium halides, titanium alkoxides, titanium oxyhalides, and the like.
- the extrudate of the invention is made by extrusion, a process in which a dough is pushed through a die or an orifice to create long objects of a fixed cross- section. Extrusion is commonly used to process plastics or food, and to form adsorbents, catalysts, or catalyst carriers. Any conventional extruder may be used. A suitable screw-type extruder is described in "Particle Size Enlargement,” Handbook of Powder Technology, vol. 1 (1980) pp. 1 12-22.
- the carboxyaikyl cellulose and the hydroxyaikyi cellulose are used as extrusion aids.
- An extrusion aid helps the mixing, mulling, and extruding operation and may improve the mechanical and/or physical properties of the extrudate such as crushing strength, surface area, pore size, or pore volume.
- the extrudate comprising titania, the carboxyaikyl cellulose and the hydroxyaikyi cellulose has a smooth outer surface. They do not tend to stick to each other while being formed, dried, and calcined, which is suitable for large scale production.
- the extrudate may comprise other extrusion aids, including, e.g., alkyl amines, carboxylic acids, alkyl ammonium compounds, amino alcohols, starch, polyacrylates, polymethacrylates, polyvinyl alcohol)s,
- extrusion aids including, e.g., alkyl amines, carboxylic acids, alkyl ammonium compounds, amino alcohols, starch, polyacrylates, polymethacrylates, polyvinyl alcohol)s,
- poly(amino acid)s polyethers, poly(tetrahydrofuran)s, metal carboxylates, and the like, and mixtures thereof.
- Preferred poly(alkylene oxide)s are poly(ethylene oxide)s, poly( propylene oxide)s, or copolymers of ethylene oxide and propylene oxide.
- Organic extrusion aids are usually removed by calcination.
- the extrudate is generally dried after it is formed.
- the drying operation generally removes most of the solvents (e.g., greater than 90%) from the extrudate.
- the drying operation may be performed at 30 to 200°C at atmospheric pressure or under vacuum. The drying may occur in air or an inert atmosphere. Sometimes, it is preferable to raise the drying temperature slowly so the extrudate will not be cracked or weakened.
- the invention includes a calcined extrudate.
- the calcination is carried out in an oxygen-containing gas to burn off the organic materials (e.g., residual solvent and extrusion aids) contained in the extrudate.
- the calcination may be carried out at 400 to 1000°C, more preferably from 450 to 800°C, most preferably from 650 to 750°C.
- an inert gas e.g., nitrogen, helium
- a calcined extrudate after the calcination contains less than 0.5 wt% carbon. Preferably, it contains less than 0.1 wt% carbon.
- the invention additionally includes a process for producing an extrudate comprising (a) mixing titania, a carboxyalkyl cellulose, and a hydroxyalkyf cellulose to form a dough; (b) extruding the dough to produce the extrudate.
- a process for producing an extrudate comprising (a) mixing titania, a carboxyalkyl cellulose, and a hydroxyalkyf cellulose to form a dough; (b) extruding the dough to produce the extrudate.
- the dough produced is placed in the hopper of a Bonnot 2-inch extruder (The Bonnot Company) equipped with a die face of 25 holes with a diameter of 1/8 inch.
- the extrusion is performed at a rate of approximately 0.25 kg/min.
- the extrudates produced have smooth outer surface and there is minimal sticking each other occuring. Almost no feathering is observed.
- the extrudates are piled 1 inch deep on a collection tray and dried in air at
- the calcination temperature is raised from room temperature to 500°C at a rate of 2°C/min, held at 500°C for 2 h, raised from 500°C to 700°C at a rate of 10°C/min, held at 700°C for 3 h, then lowered to room temperature.
- the crush strength of the calcined titania extrudate is measured with a Chatillon crush strength analyzer (Model DPP 50). The force necessary for failure in 25 measurements is averaged to give the reported value.
- Bulk density is measured by placing 40 g of the calcined extrudates in a 100-mL graduated cylinder (1" nominal outer diameter). The graduated cylinder is tapped until the apparent volume no longer changes, and then this value is divided into the mass to calculate the bulk density.
- Voidage is determined by adding the pellets to 50 ml_ water in a second graduated cylinder and then tapping until all voids are filled. The resulting water level is subtracted from the total volume of the water and the pellets taken separately to determine the void volume occupied by water.
- Total pore volume is determined by pouring the mixture through a sieve basket, shaking to remove excess water and then weighing the wet extrudates. The increase in mass over the initial 40 g of extrudates divided by the density of water is taken as the measure of the pore volume.
- Example 1 The procedure of Example 1 is repeated with the formulation shown in Table 1 , The extrudates are droopy as they exit the die face of the extruder and tend to stick to each other as they lay on the collection tray.
- Example 1 The procedure of Example 1 is repeated with the formulation shown in Table 1.
- the extrudates are droopy as they exit the die face of the extruder and tend to stick to each other as they lay on the collection tray.
- Example 2 The procedure of Example 1 is repeated, except that the formulation is as follows: DT-51 (2000 g), TAMOLTM 1124 dispersant (a hydrophilic polyelectrolyte copolymer from The Dow Chemical Company, 32.6 g), METHOCELTM K4M (54.6 g), lactic acid (6 g), water (950 g), aqueous ammonium hydroxide (14.8 M, 70 g). COMPARATIVE EXAMPLE 5
- Example 4 The procedure of Example 4 is repeated, except that alumina (DISPERAL ® P2, available from Sasol, 20 g) is used.
- alumina DISPERAL ® P2, available from Sasol, 20 g
- the extrudates are droopy as they exit the die face of the extruder and tend to stick to each other as they lay on a metal tray.
- the calcined extrudate contains 1 wt% alumina and 99 wt% titan ia.
- Example 1 The procedure of Example 1 is repeated, except that the formulation is as follows: DT51 (300 g), TAMOLTM 1124 dispersant (5 g), WALOCELTM C cellulose ⁇ 6 g), METHOCELTM K4M cellulose (6 g), lactic acid (4.5 g), water (155 g), and aqueous ammonium hydroxide (14.8 M, 11 g).
- the extrudates have smooth outer surface. Minimal feathering is observed. Almost no extrudate is observed to stick to others.
- Example 6 The procedure of Example 6 is repeated, except that the formulation is shown in Table 3. The extrudates slump upon exiting the die. They stick to each other on the collection tray.
- Example 6 The procedure of Example 6 is repeated, except that the formulation is shown in Table 3.
- the extrudates do not tend to stick to each other after laying the on the collection tray. However, they appear to be feathering.
- NaHCO 3 powder (27 g) is slowly added to an aqueous solution containing Na 2 PdCI 4 '3H 2 O (31.4 g), NaAuCI 4 *2H 2 O (11.3 g), and water (235.4 g). The mixture is stirred at room temperature for 10 min. The solution is sprayed with a pipette on calcined titania extrudates prepared in Example 1 (1000 g) while they are being tumbled in a rotating flask. Once the impregnation is finished, the rotating flask is heated to about 100°C with a heat gun. The impregnated extrudates are tumbled for another 30 min at 00°C, then placed in an oven at 80°C for 2 h before they are cooled to room temperature.
- the dried extrudates are washed with warm water (50-80°C) until no chloride can be detected by mixing the wash filtrate solution with a 1 wt% silver nitrate solution to observe precipitation.
- the catalyst is dried at 80 to 100°C to remove water. Then they are heated at 230°C for 3 h in air, and at 230°C for 30 min under a nitrogen flow. The temperature is raised to 500°C under a flow of 10 mol% hydrogen in nitrogen gas, and held for 3 h before it is cooled to room temperature.
- the extrudates are washed with an aqueous solution containing 10 wt% potassium acetate and 1 wt% potassium hydroxide (10 L).
- the washed extrudates are dried under nitrogen at 125°C for 2 h.
- a palladium-gold catalyst is obtained. It contains 0.93 wt% Pd, 0.54 wt% Au, and 1.5 wt% K.
- the palladium-gold catalyst prepared in Example 9 is tested for vinyl acetate production in a fixed-bed reactor (stainless steel, 1 inch O.D.).
- the reactor is charged with a mixture of the catalyst (10 g) and an inert alpha alumina cylindrical pellets (1/8" in diameter, surface area 4 m 2 /g, pore volume 0.25 mL/g, 25 g).
- the feed contains 46.1 mol% helium, 33.9 mo!% ethylene, 11.48 mol% acetic acid, 4.2 mol% oxygen, and 4.2 mol% nitrogen.
- the reactor pressure is 80 psig and the space velocity relative to the volume of the catalyst is 3050 h ' at standard temperature and pressure.
- the reactor is cooled using a fluidized sand bath, the temperature of which is set at 130°C.
- the product stream is analyzed by gas chromatography (GC).
- Oxygen conversion, oxygen selectivity, oxygen yield to vinyl acetate, and ethylene selectivity to vinyl acetate between 75 to 100 h on stream are calculated from the GC results and listed in Table 4.
- Oxygen conversion is calculated by dividing the amount of oxygen consumed by the total amount of oxygen fed to the reactor.
- Oxygen selectivity to vinyl acetate is the amount of oxygen consumed in making vinyl acetate divided by the total amount of oxygen consumed.
- Oxygen yield to vinyl acetate is the product of oxygen conversion multiplied by oxygen selectivity.
- Ethylene selectivity to vinyl acetate is the amount of ethylene consumed in making vinyl acetate divided by the total amount of ethylene consumed.
- Catalyst productivity is the grams of vinyl acetate produced per liter of the catalyst per hour. Table 4
Abstract
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Claims
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SG2012042925A SG181640A1 (en) | 2009-12-16 | 2010-11-19 | Titania-containing extrudate |
BR112012014697A BR112012014697A2 (en) | 2009-12-16 | 2010-11-19 | extruded containing titania |
CN2010800578488A CN102725063A (en) | 2009-12-16 | 2010-11-19 | Titania-containing extrudate |
JP2012544545A JP2013514174A (en) | 2009-12-16 | 2010-11-19 | Extruded products containing titania |
EP10787215A EP2512655A1 (en) | 2009-12-16 | 2010-11-19 | Titania-containing extrudate |
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US12/653,563 | 2009-12-16 | ||
US12/653,592 US8273682B2 (en) | 2009-12-16 | 2009-12-16 | Preparation of palladium-gold catalyst |
US12/653,563 US8329611B2 (en) | 2009-12-16 | 2009-12-16 | Titania-containing extrudate |
US12/653,592 | 2009-12-16 |
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CN (2) | CN102740964A (en) |
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EP2703078A1 (en) * | 2012-09-03 | 2014-03-05 | Saudi Basic Industries Corporation | Photocatalyst comprising gold-palladium alloy, method for preparation, photolysis system |
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WO2011075277A1 (en) * | 2009-12-16 | 2011-06-23 | Lyondell Chemical Technology, L.P. | Titania-containing extrudate |
US8507720B2 (en) | 2010-01-29 | 2013-08-13 | Lyondell Chemical Technology, L.P. | Titania-alumina supported palladium catalyst |
US8329611B2 (en) | 2009-12-16 | 2012-12-11 | Lyondell Chemical Technology, L,P. | Titania-containing extrudate |
US8273682B2 (en) | 2009-12-16 | 2012-09-25 | Lyondell Chemical Technology, L.P. | Preparation of palladium-gold catalyst |
US20140081040A1 (en) * | 2012-09-20 | 2014-03-20 | Lyondell Chemical Technology, L.P. | Process for pre-treatment of a catalyst support and catalyst prepared therefrom |
KR101964275B1 (en) | 2015-09-01 | 2019-04-01 | 주식회사 엘지화학 | Manufacturing method of catalyst for production of acrylic acid and the catalyst therefrom |
JP7260545B2 (en) | 2017-12-20 | 2023-04-18 | ビーエーエスエフ ソシエタス・ヨーロピア | Catalyst and method for producing dimethyl ether |
CN112517065B (en) * | 2019-09-18 | 2023-05-02 | 中国石油化工股份有限公司 | Preparation method of catalyst for vinyl acetate process by ethylene gas phase method |
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JP2013514174A (en) | 2013-04-25 |
TW201129642A (en) | 2011-09-01 |
BR112012014795A2 (en) | 2016-06-21 |
SG189707A1 (en) | 2013-05-31 |
CN102740964A (en) | 2012-10-17 |
SG181640A1 (en) | 2012-07-30 |
JP2013514175A (en) | 2013-04-25 |
KR20120102080A (en) | 2012-09-17 |
WO2011075278A1 (en) | 2011-06-23 |
KR20120102079A (en) | 2012-09-17 |
EP2512654A1 (en) | 2012-10-24 |
BR112012014697A2 (en) | 2016-04-12 |
TW201129455A (en) | 2011-09-01 |
SG188923A1 (en) | 2013-04-30 |
CN102725063A (en) | 2012-10-10 |
EP2512655A1 (en) | 2012-10-24 |
SG181647A1 (en) | 2012-07-30 |
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