CN104797333A - 蜂窝结构体 - Google Patents
蜂窝结构体 Download PDFInfo
- Publication number
- CN104797333A CN104797333A CN201280076927.2A CN201280076927A CN104797333A CN 104797333 A CN104797333 A CN 104797333A CN 201280076927 A CN201280076927 A CN 201280076927A CN 104797333 A CN104797333 A CN 104797333A
- Authority
- CN
- China
- Prior art keywords
- structured body
- honeycomb structured
- cellular unit
- vanadium
- oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011230 binding agent Substances 0.000 claims abstract description 42
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 39
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 34
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 26
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 10
- 230000009467 reduction Effects 0.000 claims abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 7
- 210000002421 cell wall Anatomy 0.000 claims abstract description 4
- 230000001413 cellular effect Effects 0.000 claims description 81
- 238000000034 method Methods 0.000 claims description 56
- 239000002994 raw material Substances 0.000 claims description 54
- 239000000463 material Substances 0.000 claims description 42
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 31
- 230000008569 process Effects 0.000 claims description 27
- 229910052721 tungsten Inorganic materials 0.000 claims description 27
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 26
- 238000001354 calcination Methods 0.000 claims description 26
- 238000004519 manufacturing process Methods 0.000 claims description 18
- 239000010937 tungsten Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000011521 glass Substances 0.000 claims description 12
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 239000010456 wollastonite Substances 0.000 claims description 8
- 229910052882 wollastonite Inorganic materials 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 239000012670 alkaline solution Substances 0.000 claims description 6
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 claims description 6
- 229910001593 boehmite Inorganic materials 0.000 claims description 6
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 6
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000004113 Sepiolite Substances 0.000 claims description 3
- 229960000892 attapulgite Drugs 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052627 muscovite Inorganic materials 0.000 claims description 3
- 229910052625 palygorskite Inorganic materials 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- 229910052624 sepiolite Inorganic materials 0.000 claims description 3
- 235000019355 sepiolite Nutrition 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 26
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 abstract description 4
- 210000004027 cell Anatomy 0.000 abstract 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 229910001935 vanadium oxide Inorganic materials 0.000 abstract 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 95
- 239000002562 thickening agent Substances 0.000 description 45
- 238000000576 coating method Methods 0.000 description 25
- 239000011248 coating agent Substances 0.000 description 24
- 239000000853 adhesive Substances 0.000 description 23
- 230000001070 adhesive effect Effects 0.000 description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 16
- 239000011805 ball Substances 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- 239000002912 waste gas Substances 0.000 description 13
- 239000000835 fiber Substances 0.000 description 12
- 238000005192 partition Methods 0.000 description 10
- 229910021529 ammonia Inorganic materials 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 238000000746 purification Methods 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 230000002093 peripheral effect Effects 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- 238000005238 degreasing Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 230000008676 import Effects 0.000 description 6
- 239000010954 inorganic particle Substances 0.000 description 6
- 239000003595 mist Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- 229920000609 methyl cellulose Polymers 0.000 description 5
- 239000001923 methylcellulose Substances 0.000 description 5
- 235000010981 methylcellulose Nutrition 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 4
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229910052863 mullite Inorganic materials 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 3
- 229940043237 diethanolamine Drugs 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 239000004147 Sorbitan trioleate Substances 0.000 description 2
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 239000008393 encapsulating agent Substances 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000002779 inactivation Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 239000011806 microball Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 235000019337 sorbitan trioleate Nutrition 0.000 description 2
- 229960000391 sorbitan trioleate Drugs 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- PAJMKGZZBBTTOY-UHFFFAOYSA-N 2-[[2-hydroxy-1-(3-hydroxyoctyl)-2,3,3a,4,9,9a-hexahydro-1h-cyclopenta[g]naphthalen-5-yl]oxy]acetic acid Chemical compound C1=CC=C(OCC(O)=O)C2=C1CC1C(CCC(O)CCCCC)C(O)CC1C2 PAJMKGZZBBTTOY-UHFFFAOYSA-N 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 241001455273 Tetrapoda Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical group CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 230000004941 influx Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 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
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- OGUCKKLSDGRKSH-UHFFFAOYSA-N oxalic acid oxovanadium Chemical compound [V].[O].C(C(=O)O)(=O)O OGUCKKLSDGRKSH-UHFFFAOYSA-N 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 229940063821 oxygen 21 % Drugs 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
- 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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Abstract
本发明提供使用TiO2/V2O5/WO3催化剂且NOx净化率和热耐久性优异的蜂窝结构体。一种蜂窝结构体,其至少含有钛氧化物、钒氧化物、钨氧化物和无机粘结剂,并且具备沿长度方向从一个端面延伸至另一个端面的2个以上的孔室被孔道壁划分开的形状的蜂窝单元,所述蜂窝结构体的特征在于,氢-程序升温还原法(H2-TPR)中的每1g蜂窝结构体的钒还原导致的氢消耗量为0.6mmol以上,且钨原子和钒原子的摩尔比(W/V)为0.8~1.2。
Description
技术领域
本发明涉及作为将废气中的氮氧化物(NOx)除去的脱硝催化剂的蜂窝结构体。
背景技术
作为用于净化废气中的NOx的***,已知使用氨将NOx还原为氮气和水的SCR(Selective Catalytic Reduction,选择性催化还原)***。作为该SCR***中使用的催化剂,已知五氧化二钒(V2O5)具有高脱硝性能,使用在二氧化钛(TiO2)上负载有V2O5、三氧化钨(WO3)的材料。并且,作为这样的在钛氧化物上负载有V2O5、WO3的催化剂(以下也称为“TiO2/V2O5/WO3催化剂”),例如公开在专利文献1中。
现有技术文献
专利文献
专利文献1:日本特开2005-21780号公报
发明内容
发明所要解决的课题
但是,如上所述的使用TiO2/V2O5/WO3催化剂的SCR***存在下述问题。
TiO2/V2O5/WO3催化剂的NOx净化性能依赖于作为催化剂种的V和W的添加量而变化,在V和W的添加量、比例不适当的情况下,成为活性点的V无法均匀分散,形成块体而无法有效地使用。而且,还存在V受热形成块体而失活等问题。另外,在增多V和W的添加量的情况下,催化剂的成本方面也成为问题。
本发明鉴于上述现有问题而完成,其目的在于提供使用TiO2/V2O5/WO3催化剂且NOx净化率和热耐久性优异的蜂窝结构体。
用于解决课题的手段
用于解决上述课题的本发明如下。
(1)一种蜂窝结构体,其至少含有钛氧化物、钒氧化物、钨氧化物和无机粘结剂,并且具备沿长度方向从一个端面延伸至另一个端面的2个以上的孔室被孔道壁划分开的形状的蜂窝单元,所述蜂窝结构体的特征在于,
氢-程序升温还原法(H2-TPR)中的每1g蜂窝结构体的钒还原导致的氢消耗量为0.6mmol以上,且钨原子和钒原子的摩尔比(W/V)为0.8~1.2。
(2)根据上述(1)所述的蜂窝结构体,其特征在于,所述无机粘结剂为选自由氧化铝溶胶、硅溶胶、二氧化钛溶胶、水玻璃、海泡石、凹凸棒石、膨润土和勃姆石组成的组中的一种以上所含的固体成分。
(3)根据上述(1)或(2)所述的蜂窝结构体,其特征在于,所述蜂窝单元还含有选自由无机纤维、鳞片状物质、四角(Tetrapod)状物质和三维针状物质组成的组中的一种以上。
(4)根据上述(3)所述的蜂窝结构体,其特征在于,
所述无机纤维为选自由氧化铝、二氧化硅、碳化硅、硅铝(silica-alumina)、玻璃、硅灰石、钛酸钾和硼酸铝组成的组中的一种以上,
所述鳞片状物质为选自由玻璃、白云母、氧化铝和二氧化硅组成的组中的一种以上,
所述四角状物质为氧化锌,
所述三维针状物质为选自由氧化铝、二氧化硅、碳化硅、硅铝、玻璃、硅灰石、钛酸钾、硼酸铝和勃姆石组成的组中的一种以上。
(5)一种蜂窝结构体的制造方法,其为得到上述(1)~(4)中任一项所述的蜂窝结构体的制造方法,其特征在于,
该制造方法包括:
将含有钛氧化物、钒原料、钨原料和无机粘结剂的材料成形为蜂窝状而得到蜂窝成形体的成形工序;和
将所述蜂窝成形体进行煅烧的煅烧工序,
所述煅烧工序中,使氧浓度为21%以上且使温度为450~650℃。
(6)一种蜂窝结构体的制造方法,其为得到上述(1)~(4)中任一项所述的蜂窝结构体的制造方法,其特征在于,
该制造方法包括:
将钛氧化物、钒原料、钨原料和无机粘结剂混合的混合工序;
将混合后的所述材料成形为蜂窝状而得到蜂窝成形体的成形工序;和
将所述蜂窝成形体进行煅烧的煅烧工序,
所述混合工序中,所述钒原料为将偏钒酸铵预先溶解于碱性溶液中而得到的溶液。
发明的效果
根据本发明,能够提供使用TiO2/V2O5/WO3催化剂且NOx净化率和热耐久性优异的蜂窝结构体。
附图说明
图1为表示TiO2/V2O5/WO3催化剂的NOx净化循环的图。
图2为表示本发明的蜂窝结构体的一例的立体图。
图3为表示具有本发明的蜂窝结构体的废气净化装置的一例的截面图。
图4为表示本发明的蜂窝结构体的另一例的立体图。
图5为表示构成图4的蜂窝结构体的蜂窝单元的立体图。
具体实施方式
本发明的蜂窝结构体为如下蜂窝结构体:至少含有钛氧化物、钒氧化物、钨氧化物和无机粘结剂,并且具备沿长度方向从一个端面延伸至另一个端面的2个以上的孔室被孔道壁划分开的形状的蜂窝单元,该蜂窝结构体的特征在于,氢-程序升温还原法(H2-TPR)中的每1g蜂窝结构体的钒还原导致的氢消耗量为0.6mmol以上,且钨原子和钒原子的摩尔比(W/V)为0.8~1.2。
如图1所示,TiO2/V2O5/WO3催化剂的SCR反应通过TiO2上的的氧化还原反应来进行,因此,通过增加TiO2上的V(5价)的量,反应性提高。为了增加TiO2上的V(5价)的量,在TiO2上使W与V结合而形成V-O-W即可,由此能够维持V的分散状态,并且能够防止V受热形成块体而失活。即,通过在TiO2上使W与V结合而形成V-O-W,能够使TiO2上的5价V离子的量总是保持在多的状态。并且,为了在TiO2上使V成为5价离子而全部有效使用,认为需要使TiO2上的V和W以至少达到1:1的摩尔比的方式结合。
本发明人在汽车废气的通常条件下、即在250℃、SV(空速)60000小时-1、NO2/NOx=0时,对V的分散状态、即对反应有贡献的V(5价)的量(以下称为“有效V量”)进行了定量,结果发现,NOx净化率随着W添加量的增加而提高,进而随着有效V量的增加而提高,在0.3mmol/g以上达到饱和。
此处,作为导出有效V量的方法,使用氢-程序升温还原法(H2-TPR)。并且,为了满足每1g蜂窝结构体的有效V量为0.3mmol以上,根据由来自5价钒还原的峰(350~580℃)计算出的氢消耗量和与之相伴的钒价数变化的关系,本测定中的氢消耗量必须为0.6mmol/g以上。
由以上可知,通过使氢-程序升温还原法中的每1g蜂窝结构体的钒还原导致的氢消耗量为0.6mmol以上(有效V量为0.3mmol/g以上)、使W/V添加量的摩尔比为0.8~1.2,能够提高初始的NOx净化性能和热耐久性。
如上所述,通过提高TiO2/V2O5/WO3催化剂中的有效V量,能够提高初始的NOx净化性能和热耐久性。即,使V均匀分散且不存在块体即可,本发明人发现,(1)将成形体煅烧时,如果使氧浓度为高浓度,则未反应的V原料减少,能够使V均匀分散;以及(2)在将各原料混合的混合工序中,使用将偏钒酸铵预先溶解于碱性溶液中而得到的溶液作为V原料与钛氧化物和钨原料等混合时,能够降低不显示活性的V块体的存在比例。V在充分分散到溶液中的状态下,能够附着到TiO2原料上,因此,V的分散状态高于将TiO2原料和V原料以固体相互混合的情况,能够防止形成块体。即,在上述(1)中,使煅烧工序中的氧浓度为21%以上、使温度为450~600℃,另外,在上述(2)中,在煅烧前形成预先在TiO2上均匀分散有V原料的状态,由此,在任意一种情况下,均能够在煅烧后也使V均匀分散,进而能够提高NOx净化性能和热耐久性。
图2示出本发明的蜂窝结构体的一例。蜂窝结构体10含有钛氧化物、钒氧化物、钨氧化物和无机粘结剂,并且具有将2个以上的贯通孔11a隔着间壁11b沿长度方向并列设置的单个的蜂窝单元11。另外,在蜂窝单元11的除两端面以外的外周面上,形成有外周涂层12。
蜂窝单元11中,钒原子与钨原子的摩尔比(W/V)为0.8~1.2。如上所述,通过使W/V添加量的摩尔比为0.8~1.2,能够提高初始的NOx净化性能和热耐久性。该摩尔比更优选为0.9~1.1,进一步优选为0.95~1.05。
另外,钛原子相对于钨原子和钒原子的合计的摩尔比((W+V)/Ti)优选为0.02~0.2,更优选为0.05~0.1。
作为蜂窝单元11中含有的无机粘结剂,没有特别限定,从保持作为蜂窝结构体的强度的方面考虑,可以举出氧化铝溶胶、硅溶胶、二氧化钛溶胶、水玻璃、海泡石、凹凸棒石、膨润土、勃姆石等所含的固体成分作为优选的无机粘结剂,也可以并用两种以上。
蜂窝单元11中的无机粘结剂的含量在蜂窝单元11中优选为5~30质量%,更优选为10~20质量%。蜂窝单元11中的无机粘结剂的含量低于5质量%时,蜂窝结构体的强度降低。另一方面,蜂窝结构体中的无机粘结剂的含量超过30质量%时,难以将蜂窝成形体挤出成形。
蜂窝单元11中,为了提高强度,优选在原料糊料中添加选自由无机纤维、鳞片状物质、四角状物质和三维针状物质组成的组中的一种以上。
优选:蜂窝单元11中含有的无机纤维为选自由氧化铝、二氧化硅、碳化硅、硅铝、玻璃、硅灰石、钛酸钾和硼酸铝组成的组中的一种以上,上述鳞片状物质为选自由玻璃、白云母、氧化铝和二氧化硅组成的组中的一种以上,上述四角状物质为氧化锌,上述三维针状物质为选自由氧化铝、二氧化硅、碳化硅、硅铝、玻璃、硅灰石、钛酸钾、硼酸铝和勃姆石组成的组中的一种以上。
这是因为,上述任意一种材料的耐热性高,即使在作为SCR***中的催化剂载体使用时也没有熔损等,能够使作为增强材料的效果持续。
上述无机纤维的长径比优选为2~1000,更优选为5~800,进一步优选为10~500。蜂窝单元11中含有的无机纤维的长径比小于2时,提高蜂窝单元11的强度的效果减小。另一方面,蜂窝单元11中含有的无机纤维的长径比超过1000时,将蜂窝单元11挤出成形时,模具发生堵塞等,或者无机纤维折断而使提高蜂窝单元11的强度的效果减小。
上述鳞片状物质是指平坦的物质,厚度优选为0.2~5.0μm,最大长度优选为10~160μm,最大长度相对于厚度之比优选为3~250。
上述四角状物质是指针状部以三维方式延伸的物质,针状部的平均针状长度优选为5~30μm,针状部的平均直径优选为0.5~5.0μm。
上述三维针状物质是指针状部之间利用玻璃等无机化合物在各针状部的中央附近结合而成的物质,针状部的平均针状长度优选为5~30μm,针状部的平均直径优选为0.5~5.0μm。
另外,三维针状物质中,2个以上的针状部也可以以三维方式连接,针状部的直径优选为0.1~5.0μm,长度优选为0.3~30.0μm,长度相对于直径之比优选为1.4~50.0。
无机纤维、鳞片状物质、四角状物质和三维针状物质的含量在蜂窝单元11中优选为3~50质量%,更优选为3~30质量%,进一步优选为5~20质量%。蜂窝结构体中的无机纤维、鳞片状物质、四角状物质和三维针状物质的含量低于3质量%时,提高蜂窝结构体的强度的效果减小。另一方面,蜂窝结构体中的无机纤维、鳞片状物质、四角状物质和三维针状物质的含量超过50质量%时,蜂窝结构体中的TiO2/V2O5/WO3催化剂的含量降低,NOx的净化性能降低。
蜂窝单元11优选孔隙率为30~60%。蜂窝单元11的孔隙率小于30%时,废气难以侵入至蜂窝单元11的间壁11b的内部,TiO2/V2O5/WO3催化剂无法有效地利用于NOx的净化。另一方面,蜂窝单元11的孔隙率超过60%时,蜂窝单元11的强度不充分。
需要说明的是,蜂窝单元11的孔隙率可以使用压汞法来测定。
蜂窝单元11的垂直于长度方向的截面的开口率优选为50~75%。蜂窝单元11的垂直于长度方向的截面的开口率小于50%时,TiO2/V2O5/WO3催化剂无法有效地利用于NOx的净化。另一方面,蜂窝单元11的垂直于长度方向的截面的开口率超过75%时,蜂窝单元11的强度不充分。
蜂窝单元11的垂直于长度方向的截面的贯通孔11a的密度优选为31~155个/cm2。蜂窝单元11的垂直于长度方向的截面的贯通孔11a的密度低于31个/cm2时,TiO2/V2O5/WO3催化剂与废气难以接触,NOx的净化性能降低。另一方面,蜂窝单元11的垂直于长度方向的截面的贯通孔11a的密度超过155个/cm2时,蜂窝结构体10的压力损失增大。
蜂窝单元11的间壁11b的厚度优选为0.1~0.4mm,更优选为0.1~0.3mm。蜂窝单元11的间壁11b的厚度小于0.1mm时,蜂窝单元11的强度降低。另一方面,蜂窝单元11的间壁11b的厚度超过0.4mm时,废气难以侵入至蜂窝单元11的间壁11b的内部,TiO2/V2O5/WO3催化剂无法有效地利用于NOx的净化。
外周涂层12的厚度优选为0.1~2.0mm。外周涂层12的厚度小于0.1mm时,提高蜂窝结构体10的强度的效果不充分。另一方面,外周涂层12的厚度超过2.0mm时,蜂窝结构体10的每单位体积的TiO2/V2O5/WO3催化剂的含量降低,NOx的净化性能降低。
作为蜂窝结构体10的形状,不限定于圆柱状,可以举出棱柱状、椭圆柱状、长圆柱状、圆倒角的棱柱状(例如圆倒角的三棱柱状)等。
作为贯通孔11a的形状,不限定于四棱柱状,可以举出三棱柱状、六棱柱状等。
接着,对蜂窝结构体10的制造方法的一例进行说明。该制造方法包括:将钛氧化物、钒原料、钨原料和无机粘结剂混合的混合工序、将混合后的上述材料成形为蜂窝状而得到蜂窝成形体的成形工序、和将蜂窝成形体进行煅烧的煅烧工序,根据需要还包括其他工序。
以下对各工序进行说明。需要说明的是,本发明的蜂窝结构体的制造中,如前所述,为了使V均匀分散且不存在块体而采用预定的方法,关于该方法在下文中记述。
上述混合工序中,将钛氧化物、钒原料、钨原料和无机粘结剂以及根据需要使用的选自由无机纤维、鳞片状物质、四角状物质和三维针状物质组成的组中的一种以上混合、混炼,制备原料糊料。
作为钛氧化物,优选使用比表面积高的锐钛矿型的二氧化钛。
作为钒原料,可以举出偏钒酸铵、偏钒酸钠、偏钒酸钾、草酸氧钒、乙酸氧钒等,其中,从容易处理的方面考虑,优选为偏钒酸铵。偏钒酸铵(NH4VO3)通过NH4VO3→V2O5+2NH3+H2O这样的分解反应生成V2O5,作为SCR***中的催化剂发挥作用。
作为钨原料,可以举出偏钨酸铵、氧化钨、仲钨酸铵等,其中,优选偏钨酸铵。
原料糊料中,上述钒原料中的钒原子与上述钨原料中的钨原子的摩尔比(W/V)设定为0.8~1.2。这是因为,如上所述,通过使蜂窝结构体中的W/V添加量的摩尔比为0.8~1.2,能够提高初始的NOx净化性能和热耐久性。
该摩尔比更优选为0.9~1.1,进一步优选为0.95~1.05。
原料糊料中含有的无机粘结剂与前述的蜂窝单元11中含有的无机粘结剂相同。
另外,原料糊料中可以根据需要适当添加有机粘结剂、分散介质、成形助剂等。
作为有机粘结剂,没有特别限定,可以举出甲基纤维素、羧甲基纤维素、羟乙基纤维素、聚乙二醇、酚醛树脂、环氧树脂等,也可以并用两种以上。需要说明的是,有机粘结剂的添加量相对于钛氧化物、钒氧化物、钨氧化物、无机粘结剂、无机纤维、鳞片状物质、四角状物质和三维针状物质的总质量优选为1~10%。
作为分散介质,没有特别限定,可以举出水、苯等有机溶剂、甲醇等醇等,也可以并用两种以上。
作为成形助剂,没有特别限定,可以举出乙二醇、糊精、脂肪酸、脂肪酸皂、多元醇等,也可以并用两种以上。
制备原料糊料时,优选混合混炼,可以使用混合器、超微磨碎机等进行混合,也可以使用捏合机等进行混炼。
接着,使用微波干燥机、热风干燥机、高频干燥机、减压干燥机、真空干燥机、冷冻干燥机等干燥机,对蜂窝成形体进行干燥。
接着,成形工序中,使用上述原料糊料进行挤出成形,制作隔着间壁沿长度方向并列设置有2个以上的贯通孔的圆柱状蜂窝成形体。
将所得到的蜂窝脱脂体进行煅烧,由此得到圆柱状的蜂窝单元11(煅烧工序)。煅烧温度优选为450~750℃,更优选为550~650℃。煅烧温度低于450℃时,无法进行烧结,蜂窝单元11的强度降低。另一方面,煅烧温度超过750℃时,烧结进行过度,TiO2/V2O5/WO3的反应位点减少。
在上述煅烧工序之后,可以设置形成外周涂层的工序等其他工序。
形成外周涂层的工序中,在圆柱状的蜂窝单元11的除两端面以外的外周面上涂布外周涂层用糊料。
作为外周涂层用糊料,没有特别限定,可以举出无机粘结剂与无机颗粒的混合物、无机粘结剂与无机纤维的混合物、无机粘结剂、无机颗粒以及无机纤维的混合物等。
外周涂层用糊料中含有的无机粘结剂没有特别限定,以硅溶胶、氧化铝溶胶等的形式添加,也可以并用两种以上。其中,优选以硅溶胶的形式添加。
作为外周涂层用糊料中含有的无机颗粒,没有特别限定,可以举出碳化硅颗粒等碳化物颗粒;氮化硅颗粒、氮化硼颗粒等氮化物颗粒等,也可以并用两种以上。其中,从热传导性优异的方面考虑,优选碳化硅颗粒。
作为外周涂层用糊料中含有的无机纤维,没有特别限定,可以举出硅铝纤维、莫来石纤维、氧化铝纤维、二氧化硅纤维等,也可以并用两种以上。其中,优选氧化铝纤维。
外周涂层用糊料可以进一步含有有机粘结剂。
作为外周涂层用糊料中含有的有机粘结剂,没有特别限定,可以举出聚乙烯醇、甲基纤维素、乙基纤维素、羧甲基纤维素等,也可以并用两种以上。
外周涂层用糊料可以进一步含有作为氧化物系陶瓷的微小空心球体的空心球、造孔剂等。
作为外周涂层用糊料中含有的空心球,没有特别限定,可以举出氧化铝空心球、空心玻璃微球、火山灰空心球、飞灰空心球、莫来石空心球等,也可以并用两种以上。其中,优选氧化铝空心球。
作为外周涂层用糊料中含有的造孔剂,没有特别限定,可以举出球状丙烯酸类颗粒、石墨等,也可以并用两种以上。
接着,将涂布有外周涂层用糊料的蜂窝单元11干燥固化,制作圆柱状的蜂窝结构体10。此时,在外周涂层用糊料中含有有机粘结剂的情况下,优选进行脱脂。脱脂条件可以根据有机物的种类和量适当选择,优选为700℃下20分钟。
本发明中,如前所述,为了提高TiO2/V2O5/WO3催化剂中的有效V量,采用下述方法:(1)在煅烧成形体时,使氧浓度为高浓度;或者,(2)在将各原料进行混合的混合工序中,使用将偏钒酸铵预先溶解于碱性溶液中而得到的溶液作为V原料,与钛氧化物和钨原料等混合。以下,对该方法进行说明。
上述(1)的方法中,在上述煅烧工序中,使氧浓度为21%以上,且使温度为450~650℃。从能够使V更均匀地分散、能够提高NOx净化性能和热耐久性的方面考虑,该氧浓度优选设定为30~50%,更优选为35~45%。为了在煅烧工序中使氧浓度在上述范围内来进行煅烧,将含有上述浓度的氧气的混合气体以任意的流量导入到煅烧炉内即可。该混合气体中的氧以外的成分没有特别限定,例如可以举出氮。
另外,如上所述,煅烧温度为450~650℃,优选为500~600℃。煅烧温度低于450℃时,无法进行烧结,蜂窝单元11的强度降低。另一方面,煅烧温度超过650℃时,随着烧结的进行,TiO2/V2O5/WO3的NOx净化性能降低。作为达到上述煅烧温度为止的升温速度,优选设定为0.1~10℃/分钟。
煅烧时间为直至煅烧结束为止的时间,适当设定即可,例如可以设定为1~5小时。
上述(2)的方法中,在上述混合工序中,将钛氧化物、钒原料、钨原料和无机粘结剂以及根据需要使用的选自由无机纤维、鳞片状物质、四角状物质和三维针状物质组成的组中的一种以上进行混合,制备原料糊料。
并且,作为钒原料,使用将偏钒酸铵预先溶解于碱性溶液中而得到的溶液(以下也称为“预混合溶液”)。即,制备原料糊料时,不是将全部原料成分一次性地混合,而是仅将钒原料另外制备上述预混合溶液,然后,将该预混合溶液与其他成分混合。
更具体而言,本工序按照以下(1)、(2)的顺序实行。
(1)制备将偏钒酸铵溶解于碱性溶液中而得到的预混合溶液。
(2)将预混合溶液与至少钛氧化物、钨原料和无机粘结剂混合。
图3示出具有本发明的蜂窝结构体的废气净化装置的一例。废气净化装置100可以通过在蜂窝结构体10的外周部配置有保持密封材料20的状态下将蜂窝结构体10封装(キャニング)到金属容器(壳体)30中来制作。另外,在废气净化装置100中,设置有向相对于废气流动的方向位于蜂窝结构体10的上游侧的配管(未图示)内喷射氨或分解产氨的化合物的喷射喷嘴等喷射装置(未图示)。由此,向在配管中流动的废气中添加氨,因此,利用蜂窝单元11中含有的TiO2/V2O5/WO3催化剂,将废气中含有的NOx还原。
作为分解产生氨的化合物,只要能够在配管内被废气加热而产生氨,则没有特别限定,优选尿素水溶液,因为其储存稳定性优异。
尿素水溶液在配管内被废气加热,发生水解而产生氨。
图4示出本发明的蜂窝结构体的另一例。需要说明的是,蜂窝结构体10’除了借助粘接层13将2个以上的蜂窝单元11’粘接、该蜂窝单元11’中隔着间壁11b沿长度方向并列设置有2个以上的贯通孔11a(参见图5)以外,为与蜂窝结构体10相同的构成。
蜂窝单元11’的垂直于长度方向的截面的截面积优选为10~200cm2。蜂窝单元11’的垂直于长度方向的截面的截面积小于10cm2时,蜂窝结构体10’的压力损失增大。另一方面,蜂窝单元11’的垂直于长度方向的截面的截面积超过200cm2时,对蜂窝单元11’中产生的热应力的强度不充分。
需要说明的是,蜂窝单元11’除了垂直于长度方向的截面的截面积以外,为与蜂窝单元11相同的构成。
粘接层13的厚度优选为0.5~2.0mm。粘接层13的厚度小于0.5mm时,蜂窝单元11’的粘接强度不充分。另一方面,粘接层13的厚度超过2.0mm时,蜂窝结构体10’的压力损失增大。
接着,对蜂窝结构体10’的制造方法的一例进行说明。首先,与蜂窝结构体10同样地制作四棱柱状的蜂窝单元11’。接着,在蜂窝单元11’的除两端面以外的外周面上涂布粘接层用糊料,将蜂窝单元11’依次粘接,干燥固化,由此制作蜂窝单元11’的集合体。
作为粘接层用糊料,没有特别限定,可以举出无机粘结剂与无机颗粒的混合物、无机粘结剂与无机纤维的混合物、无机粘结剂、无机颗粒以及无机纤维的混合物等。
粘接层用糊料中含有的无机粘结剂没有特别限定,以硅溶胶、氧化铝溶胶等的形式添加,也可以并用两种以上。其中,优选以硅溶胶的形式添加。
作为粘接层用糊料中含有的无机颗粒,没有特别限定,可以举出碳化硅颗粒等碳化物颗粒;氮化硅颗粒、氮化硼颗粒等氮化物颗粒等,也可以并用两种以上。其中,从热传导性优异的方面考虑,优选碳化硅颗粒。
作为粘接层用糊料中含有的无机纤维,没有特别限定,可以举出硅铝纤维、莫来石纤维、氧化铝纤维、二氧化硅纤维等,也可以并用两种以上。其中,优选氧化铝纤维。
另外,粘接层用糊料可以含有有机粘结剂。
作为粘接层用糊料中含有的有机粘结剂,没有特别限定,可以举出聚乙烯醇、甲基纤维素、乙基纤维素、羧甲基纤维素等,也可以并用两种以上。
粘接层用糊料可以进一步含有作为氧化物系陶瓷的微小空心球体的空心球、造孔剂等。
作为粘接层用糊料中含有的空心球,没有特别限定,可以举出氧化铝空心球、空心玻璃微球、火山灰空心球、飞灰空心球、莫来石空心球等,也可以并用两种以上。其中,优选氧化铝空心球。
作为粘接层用糊料中含有的造孔剂,没有特别限定,可以举出球状丙烯酸类颗粒、石墨等,也可以并用两种以上。
接着,将蜂窝单元11’的集合体切削加工为圆柱状后,根据需要进行研磨,由此制作圆柱状的蜂窝单元11’的集合体。
需要说明的是,代替将蜂窝单元11’的集合体切削加工为圆柱状的操作,也可以通过将垂直于长度方向的截面成形为预定形状的蜂窝单元11’粘接来制作圆柱状的蜂窝单元11’的集合体。此时,蜂窝单元11’的垂直于长度方向的截面的形状优选为圆心角为90°的扇形。
接着,在圆柱状的蜂窝单元11’的集合体的除两端面以外的外周面上涂布外周涂层用糊料。
外周涂层用糊料可以与粘接层用糊料相同,也可以不同。
接着,将涂布有外周涂层用糊料的圆柱状的蜂窝单元11’的集合体干燥固化,由此制作圆柱状的蜂窝结构体10’。此时,在粘接层用糊料和/或外周涂层用糊料中含有有机粘结剂的情况下,优选进行脱脂。脱脂条件可以根据有机物的种类和量适当选择,优选为700℃下20分钟。
需要说明的是,蜂窝结构体10和10’也可以不形成外周涂层12。
实施例
以下,通过实施例更具体地说明本发明,但本发明不限定于以下实施例。
[实施例1]
将二氧化钛3910质量份、作为钒原料的偏钒酸铵210质量份、作为钨原料的偏钨酸铵(50%溶液)670质量份、氧化铝粘结剂300质量份、硅灰石纤维170质量份、作为成形助剂的甲基纤维素300质量份、作为成形润滑剂的失水山梨醇三油酸酯80质量份、作为pH调节剂的二乙醇胺150质量份、离子交换水1750质量份混合混炼,制备原料糊料1。钒原料中的钒原子与钨原料中的钨原子的摩尔比(W/V)为0.8。
接着,使用挤出成形机,将原料糊料1挤出成形,制作正四棱柱状的蜂窝成形体。然后,使用间歇式微波干燥机,将蜂窝成形体在86.7kPa的干燥压力下干燥6分钟后,将蜂窝成形体投入气体流通炉中,以5℃/分钟的升温速度升温至550℃,将该温度保持3小时并进行煅烧,制作蜂窝煅烧体。需要说明的是,煅烧时,以20L/分钟的气体流量导入氧浓度21%、氮浓度79%的混合气体。
蜂窝单元11’是边长为35mm、长度为150mm的正四棱柱状,贯通孔11a的密度为62个/cm2,间壁11b的厚度为0.28mm。
接着,将平均纤维直径为0.5μm、平均纤维长度为15μm的氧化铝纤维767份、二氧化硅玻璃2500份、羧甲基纤维素17份、固体成分为30质量%的硅溶胶600份、聚乙烯醇167份、表面活性剂167份和氧化铝空心球17份混合混炼,制作粘接层用糊料。
在蜂窝单元11’的除两端部以外的外周面上涂布粘接层用糊料,使粘接层13的厚度达到2.0mm,将16个蜂窝单元11’粘接,在150℃下干燥固化10分钟。接着,使用金刚石切割器,以使垂直于长度方向的截面大致呈点对称的方式切削加工为圆柱状,制作蜂窝单元11’的集合体。
进而,在蜂窝单元11’的集合体的除两端部以外的外周面上涂布粘接层用糊料,使外周涂层12的厚度达到1.0mm,然后,使用微波干燥机和热风干燥机,将粘接层用糊料在150℃下干燥固化10分钟,在400℃下脱脂2小时,制作直径为160mm、长度为150mm的圆柱状蜂窝结构体10’。
[实施例2]
除了使煅烧时导入的混合气体中的氧浓度为40%(氮浓度:60%)以外,与实施例1同样地制作蜂窝结构体10’。
[实施例3]
将偏钒酸铵170质量份添加到由二乙醇胺150质量份和离子交换水1750质量份制备的8%二乙醇胺水溶液中,加热至100℃,得到溶解预混合溶液。接着,添加作为钨原料的偏钨酸铵(50%溶液)670质量份、作为成形润滑剂的失水山梨醇三油酸酯80质量份,制备溶液原料。
接着,将二氧化钛3950质量份、氧化铝粘结剂300质量份、硅灰石纤维170质量份、作为成形助剂的甲基纤维素300质量份混合后,添加上述预备混合液并进行混合、混炼,制备原料糊料2。钒原料中的钒原子与钨原料中的钨原子的摩尔比(W/V)为0.80。
接着,使用原料糊料2,与实施例1同样地制作蜂窝结构体10’。
[比较例1]
除了使煅烧时导入的混合气体中的氧浓度为0%(氮浓度:100%)以外,与实施例1同样地制作蜂窝结构体10’。
[有效V量]
将实施例1~3、比较例1中制作的蜂窝单元粉碎而制成粉末状,按照以下顺序进行H2-TPR测定。将作为测定结果的氢消耗量的1/2作为有效V量。结果示于表1。
(1)作为预处理,以50cm3/分钟的流量向炉内导入He,从100℃开始以10℃/分钟的升温速度升温至500℃,将该温度保持1小时。接着,降温至100℃。
(2)接着,以30cm3/分钟的流量向炉内导入H2:5.04%、Ar:94.96%的混合气体,从100℃开始以10℃/分钟的升温速度升温至700℃,将该温度保持20分钟。接着,以50cm3/分钟的流量向炉内导入He,降温至100℃。
[NOx的净化性能]
使用金刚石切割器,从实施例1~3、比较例1中制作的蜂窝单元上切下边长为30mm、长度为40mm的正四棱柱状的试验片。以80000/小时的空速(SV)向这些试验片中通入200℃的模拟气体,使用催化剂评价装置(堀场制作所公司制造,SIGU-2000/MEXA-6000FT)测定从试样流出的NOx的流出量,计算出由下式表示的NOx的净化率[%]:
(NOx的流入量-NOx的流出量)/(NOx的流入量)×100
计算的结果示于表1。需要说明的是,模拟气体的构成成分为一氧化氮350ppm、氨气350ppm、氧气14%、水10%、氮气(平衡)。
[热耐久性]
使用金刚石切割器,从实施例1~3、比较例1中制作的蜂窝单元上切下边长为30mm、长度为40mm的正四棱柱状的试验片。使用催化剂耐久装置(堀场制作所公司制造,SIGU-1000),在550℃下对这些试验片进行100小时热处理,在上述NOx净化率测定条件下实施性能评价。
热处理时的模拟气体条件为氧气21%、水10%、氮气(平衡)、流量1L/分钟。
[表1]
由表1可知,实施例1~3的蜂窝结构体的有效V量为0.3mmol/g以上(氢-程序升温还原法(H2-TPR)中的每1g蜂窝结构体的钒还原导致的氢消耗量为0.6mmol以上),且钨原子与钒原子的摩尔比(W/V)均为0.8,得到了热耐久前后的NOx净化性能均能够令人满意的结果。与此相对,比较例1的有效V量低于0.3mmol/g,在NOx净化性能方面差。
符号的说明
10、10’ 蜂窝结构体
11、11’ 蜂窝单元
11a 贯通孔
11b 间壁
12 外周涂层
13 粘接层
20 保持密封材料
30 金属容器
100 废气净化装置
Claims (6)
1.一种蜂窝结构体,其至少含有钛氧化物、钒氧化物、钨氧化物和无机粘结剂,并且具备沿长度方向从一个端面延伸至另一个端面的2个以上的孔室被孔道壁划分开的形状的蜂窝单元,所述蜂窝结构体的特征在于,
氢-程序升温还原法(H2-TPR)中,每1g蜂窝结构体的钒还原导致的氢消耗量为0.6mmol以上,且钨原子和钒原子的摩尔比(W/V)为0.8~1.2。
2.根据权利要求1所述的蜂窝结构体,其特征在于,所述无机粘结剂为选自由氧化铝溶胶、硅溶胶、二氧化钛溶胶、水玻璃、海泡石、凹凸棒石、膨润土和勃姆石组成的组中的一种以上所含的固体成分。
3.根据权利要求1或2所述的蜂窝结构体,其特征在于,所述蜂窝单元还含有选自由无机纤维、鳞片状物质、四角状物质和三维针状物质组成的组中的一种以上。
4.根据权利要求3所述的蜂窝结构体,其特征在于,
所述无机纤维为选自由氧化铝、二氧化硅、碳化硅、硅铝、玻璃、硅灰石、钛酸钾和硼酸铝组成的组中的一种以上,
所述鳞片状物质为选自由玻璃、白云母、氧化铝和二氧化硅组成的组中的一种以上,
所述四角状物质为氧化锌,
所述三维针状物质为选自由氧化铝、二氧化硅、碳化硅、硅铝、玻璃、硅灰石、钛酸钾、硼酸铝和勃姆石组成的组中的一种以上。
5.一种蜂窝结构体的制造方法,其为得到权利要求1~4中任一项所述的蜂窝结构体的制造方法,其特征在于,
该制造方法包括:
将含有钛氧化物、钒原料、钨原料和无机粘结剂的材料成形为蜂窝状而得到蜂窝成形体的成形工序;和
将所述蜂窝成形体进行煅烧的煅烧工序,
所述煅烧工序中,使氧浓度为21%以上且使温度为450~650℃。
6.一种蜂窝结构体的制造方法,其为得到权利要求1~4中任一项所述的蜂窝结构体的制造方法,其特征在于,
该制造方法包括:
将钛氧化物、钒原料、钨原料和无机粘结剂混合的混合工序;
将混合后的所述材料成形为蜂窝状而得到蜂窝成形体的成形工序;和
将所述蜂窝成形体进行煅烧的煅烧工序,
所述混合工序中,所述钒原料为将偏钒酸铵预先溶解于碱性溶液中而得到的溶液。
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