CN109453770A - A kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum - Google Patents
A kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum Download PDFInfo
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- CN109453770A CN109453770A CN201811274035.9A CN201811274035A CN109453770A CN 109453770 A CN109453770 A CN 109453770A CN 201811274035 A CN201811274035 A CN 201811274035A CN 109453770 A CN109453770 A CN 109453770A
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- oxide
- catalyst
- ammoxidation
- gas
- platinum
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000003054 catalyst Substances 0.000 title claims abstract description 74
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 43
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 26
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910017052 cobalt Inorganic materials 0.000 claims abstract 2
- 239000010941 cobalt Substances 0.000 claims abstract 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910052726 zirconium Inorganic materials 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 238000001354 calcination Methods 0.000 claims description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000010936 titanium Substances 0.000 claims description 18
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 16
- 238000004817 gas chromatography Methods 0.000 claims description 16
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 14
- 238000007254 oxidation reaction Methods 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 13
- 230000001376 precipitating effect Effects 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 230000005684 electric field Effects 0.000 claims description 10
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 9
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000008236 heating water Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000006166 lysate Substances 0.000 claims description 6
- 229910052763 palladium Inorganic materials 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000004448 titration Methods 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 claims description 5
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011037 adipic acid Nutrition 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000001272 nitrous oxide Substances 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000510 noble metal Inorganic materials 0.000 abstract description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 239000010970 precious metal Substances 0.000 abstract description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052684 Cerium Inorganic materials 0.000 abstract 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000969 carrier Substances 0.000 abstract 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- 230000003197 catalytic effect Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 229960004756 ethanol Drugs 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 3
- 150000002823 nitrates Chemical class 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 description 1
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 229910019020 PtO2 Inorganic materials 0.000 description 1
- 229910018879 Pt—Pd Inorganic materials 0.000 description 1
- 229910000629 Rh alloy Inorganic materials 0.000 description 1
- QYSYEILYXGRUOM-UHFFFAOYSA-N [Cl].[Pt] Chemical compound [Cl].[Pt] QYSYEILYXGRUOM-UHFFFAOYSA-N 0.000 description 1
- YKIOKAURTKXMSB-UHFFFAOYSA-N adams's catalyst Chemical compound O=[Pt]=O YKIOKAURTKXMSB-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- PCLURTMBFDTLSK-UHFFFAOYSA-N nickel platinum Chemical compound [Ni].[Pt] PCLURTMBFDTLSK-UHFFFAOYSA-N 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- -1 nitrotoleune Chemical compound 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
Classifications
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/54—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
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
-
- B01J35/615—
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/035—Precipitation on carriers
-
- 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
- B01J37/08—Heat treatment
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/342—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electric, magnetic or electromagnetic fields, e.g. for magnetic separation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/24—Nitric oxide (NO)
- C01B21/26—Preparation by catalytic or non-catalytic oxidation of ammonia
- C01B21/265—Preparation by catalytic or non-catalytic oxidation of ammonia characterised by the catalyst
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention discloses a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum, with the nitrate of zirconium, iron, cobalt and cerium, and butyl titanate, titanium tetrachloride, titanium tetraisopropylate are presoma, using pure platinum as raw material, oxide carrier is prepared by sol-gal process, hydro-thermal method and coprecipitation, platinum acid chloride solution is prepared using pure platinum, by the electronation precipitation method in above-mentioned mixed oxide supported on carriers metal platinum, after being calcined by certain temperature, ammoxidation is catalyzed nitric oxide processed under ammonia and Oxygen Condition.Gained specific surface area of catalyst is big, precious metal load capacity is small, ammoxidation is selectively good, high conversion rate, can effectively improve the conversion ratio of ammonia and reduce noble metal dosage.
Description
Technical field
The present invention relates to a kind of preparation of the catalyst of the ammoxidation nitrogen oxides of mixed oxide-loaded platinum and comment
Valence is especially used to prepare ammoxidation in nitric acid and is catalyzed.In ammonia oxidation process, by making gas mixing at elevated temperatures
Object is by the catalyst of oxide carried platinum by ammoxidation at nitrogen oxides.
Background technique
Ammoxidation catalysis reaction is mainly used in the production of nitric acid, hydrogen cyanide, and high-temperature S removal ammonia generates nitric oxide
And HCN, platinum-rhodium alloy mesh catalyst is industrially used always.Nitric acid is important basic chemical industry product, is one of three sour two alkali, is
The extremely wide industrial chemicals of purposes.Other than chemical industry, nitric acid is also used to metallurgy, medicine, fuel, agricultural, nuclear industry etc.
Aspect.Nitric acid can be divided into two aspects of inorganic chemical industry and organic chemical industry in the application of chemical industry.Wherein, inorganic chemical industry master
To be applied to production ammonium nitrate, nitrophosphate fertilizer, nitro-compound fertilizer, all kinds of nitrate and propellant；Organic chemical industry mainly answers
It is the main former material of MDI, TDI, nylon66 fiber, engineering plastics for producing nitrobenzene, nitrotoleune, adipic acid, nitro-chlorobenzene
Material.
Platinum guaze catalyst has excellent selectivity and conversion ratio, but have a disadvantage in that not only catalyst cost is very high
It is expensive, and in double Pressure Unit use processes, platinum alloy net surface forms volatile platinum oxide (PtO2) platinum is caused to lose.
In order to reduce platinum loss, successively there is under platinum guaze in the trapping air-flows such as installation filling porcelain circle, glass fibre metal particle back and forth
Platinum is received, NiPd net utilizes PdO and PtO2It reacts to form the next trapping gaseous PtO of Pt-Pd solid solution2, recovering effect is good, returns
Yield reaches 70-80%.With rising steadily for Pd price, the cost recovery of the technology is also higher and higher, also promotes simultaneously
The research of the lower catalysis material substitution platinum of price.
Summary of the invention
In order to solve the above technical problems, urging the present invention provides a kind of ammoxidation nitrogen oxides of oxide carried platinum
Agent and preparation and evaluation method, gained catalyst have high-specific surface area, highly selective, high ammonia conversion ratio and low noble metal
The characteristics of dosage.
The technical scheme is that a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum, catalyst
Carrier is zirconium oxide and aoxidizes titanium mixed oxide, titanium oxide and cerium oxide mixed oxide, cobalt oxide, cerium oxide and titanium oxide
Mixed oxide, zirconium oxide, cerium oxide and oxidation titanium mixed oxide, iron oxide, cerium oxide and oxidation titanium mixed oxide, oxygen
Change the combination of one of iron, cobalt oxide, cerium oxide and oxidation titanium mixed oxide；Catalyst Payload element is platinum, platinum palladium, platinum
One or more combination in rhodium, platinum rhodium palladium.
Further, the catalyst preparation the following steps are included:
S1: according to the oxide elements ratio in the catalyst carrier, a certain amount of nitrate is taken to be dissolved in deionization
In water, it is configured to the solution of 0.005mol/L, and PVP is added with the dosage of 10g/L, a certain amount of nitric acid solution is added, makes molten
Liquid pH value between 1 and 2, is placed in agitating and heating in there-necked flask, prepares a certain amount of titaniferous precursor ethanol solution, according to 1 drop/
The speed of 3s is added dropwise in there-necked flask, forms collosol and gel after being added dropwise to complete, and a certain amount of weak aqua ammonia is added and precipitates to complete,
Flow back 2h in the there-necked flask, is then centrifuged for filtering, and dries 48h, then 500 DEG C of calcining 5h, and grinding obtains powdered carrier；
S2: a certain amount of catalyst Payload element is taken, lysate is made with aqua regia dissolution, takes the lysate second
The mixed oxide that 0.005wt.%, 0.05wt.%, 0.5wt.%, 1wt.%, 5wt.% is made in glycol under alkaline condition is negative
Solution is carried,
S3: the mixed oxide-loaded solution of step S2 being added in the ethanol solution of support dispersion, heating water bath stirring
2h is cleaned 1 time after centrifugal filtration with acetone, with washes of absolute alcohol 3 times, is cleaned 2 times with deionized water, and 50 DEG C dry for 24 hours,
500 DEG C of calcining 2h, obtain catalyst；
S4: ammonia and oxygen are passed through evaluating apparatus according to a certain percentage, using gas-chromatography test ammonia, nitrous oxide,
Then nitrogen calculates selectivity and conversion ratio using titration measuring nitric acid yield.
Further, step S1 can be replaced: according to the oxide elements ratio in the catalyst carrier, use is a certain amount of
Butylamine or hexadecylamine or triethylamine, be added in autoclave with a certain amount of nitrate, titanium compound, PVP,
At a temperature of 180 DEG C, 36h is reacted, then cleans, be centrifugated, drying, grinding obtains powder.
Further, two kinds of zirconium oxide, cerium oxide, cobalt oxide, iron oxide and titanium oxide are prepared by sol-gal process
Or two or more mixed oxide particles, the mixed oxide particle partial size are less than 20nm.
Further, spherical or sheet zirconium oxide, cerium oxide, cobalt oxide, iron oxide and oxygen are prepared by hydro-thermal method
Change two or more mixed oxide particle of titanium, the mixed oxide particle partial size is less than 20nm.
Further, using titration measuring nitric acid yield, gas mixture is collected with airbag and is then examined with gas-chromatography
It surveys, analyzes selectivity and conversion ratio.
Further, it is handled in step S3 heating water bath whipping process every the impulse electric field of the additional 8-400ms of 1-2min
Until precipitating completely, wherein impulse electric field field strength is 50-80kV/cm, pulse frequency 200-1100Hz, pulse width 30-120 μ
S, impulse waveform are rectangular wave.In the above way and under the conditions of handle, the uniformity of this catalyst loaded article and heavy can be improved
The effect in shallow lake, and then the catalytic effect and raw material availability of catalyst of the present invention are improved, save cost.
Further, the actual conditions calcined in the step S1 are as follows: it is 5-15T that substance after drying, which is placed on magnetic field strength,
Superconducting intense magnetic field in rise magnetic, be warming up to 370-420 DEG C with 50-60 DEG C/h, activate 0.5-1.5 hour, drop magnetic to 0T, then with
20-30 DEG C is continuously heating to 500 DEG C, and calcining total time is 5h, and nitrogen is added to be cooled to room temperature.By the above method and condition to forging
It burns object to be handled, the load effect of carrier can be improved.
Further, the actual conditions calcined in the step S3 are as follows: 2h is calcined at 500 DEG C, in 270-290 DEG C of temperature
Under, nitrogen hydrogen is than being passed through inert gas later and continuing to calcine 5-10min, then again to calcine 20-35min under the atmosphere of 8:2
It is secondary to be warming up to 500 DEG C, and it is passed through air calcining at constant temperature, calcining total time is 2h, and subsequent cooled to room temperature obtains catalyst.
Last calcination processing is carried out to catalyst of the present invention by the different atmosphere under different temperatures, and catalyst of the present invention can be improved
Stability, and enhance the catalytic effect of this catalyst.
Further, the evaluating apparatus mainly includes controller, reaction tube, gas-chromatography, computer, gas collection bottle
One, gas collection bottle two, gas collection bottle three and airbag；The reaction tube upper end is connected with ammonia bottle, oxygen cylinder and pressure gauge,
A mass flowmenter, the controller and reaction tube are respectively installed in the ammonia bottle and oxygen cylinder and reaction tube connecting pipe
It is connected in pipe, controller upper end is equipped with temperature sensor and temperature controller, and it is gentle that the reaction tube lower end is connected with gas-chromatography
A ball valve, gas phase are respectively installed in body receiving flask one, the gas-chromatography and gas receiving flask one and reaction tube connecting pipe
Chromatography is connect with argon bottle, computer, and the gas collection bottle one is sequentially connected in series gas collection bottle two, gas collection bottle from right to left
Three and airbag.
Further, which is used for ammoxidation process, under the conditions of 800 DEG C, nitric oxide production selectivity is connect
Nearly 97%, conversion ratio can reach 100%.
The beneficial effects of the present invention are:
(1) catalyst of the ammoxidation nitrogen oxides of oxide carried platinum of the invention, platinum load capacity is small, compared to biography
Similar catalyst precious metal load capacity of uniting is small, and catalyst of the present invention only needs 0.005wt.%-1.0wt.% i.e. and can reach above-mentioned
Catalytic effect can reduce noble metal dosage, and cost is lower, and catalytic effect is unaffected, have a good application prospect.
(2) specific surface area of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum of the invention is high, catalytic effect
More preferably, the specific surface area of loaded catalyst of the present invention is up to 270m2/ g, ammoxidation is selectively good, high conversion rate, can effectively mention
The conversion ratio of high ammonia.
(3) evaluating apparatus of the invention is easy to operate, as a result accurately, easy to use, is convenient for and catalyst complex of the present invention
It uses.
Detailed description of the invention
Fig. 1 is evaluating catalyst process and evaluating apparatus annexation figure.
Fig. 2 is the scanning electron microscope (SEM) photograph of load platinum catalyst.
Fig. 3 is the partial enlarged view of scanning electron microscope (SEM) photograph.
Fig. 4 is scanning electron microscope energy spectrum diagram.
Fig. 5 is that the BET of load platinum catalyst schemes.
Fig. 6 is the selectivity and conversion ratio figure of load platinum catalyst.
Wherein, 1- ammonia bottle, 2- oxygen cylinder, 3- mass flowmenter, 4- controller, 5- temperature sensor, 6- temperature controller, 7-
Reaction tube (wherein, reaction tube lateral shadow is bringing-up section, middle part black section is Catalyst packing position in reaction tube), 8- pressure
Table, 9- ball valve, 10- argon bottle, 11- gas-chromatography, 12- computer, 13- gas collection bottle one, 14- gas collection bottle two, 15- gas
Body receiving flask three, 16- airbag.
Specific embodiment
Embodiment 1
Prepare Ti0.3Ce0.7O2The mixed oxide catalyst of Pt0.05%,
S1: it according to the oxide elements ratio in iron oxide, cobalt oxide, cerium oxide and oxidation titanium mixed oxide, weighs
8.6 grams of cerous nitrates prepare the solution of 0.005mol/l, and 8.7 grams of titanium tetraisopropylates are dissolved in dehydrated alcohol, 40 grams of PVP are added, add
Enter 20ml nitric acid, makes pH value 1.8.Prepared cerous nitrate solution is heated and stirred in water-bath, when water temperature reaches 80
DEG C when, start be added dropwise titanium tetraisopropylate ethanol solution, by rate of titration control in 1 drop/3s, after being added dropwise, be added dropwise about
The ammonia spirit of 50ml makes pH value 8.5, makes to precipitate complete precipitating.Period precipitating becomes khaki from milky.Described three
Flow back 2h in mouth bottle, ultrasonic cleaning 3 times, is then centrifuged for filtering, dries 48h.500 DEG C of calcining 5h, grinding obtain powdered
Carrier.
S2: taking 1.0wt.% platinum-nickel alloys, and lysate is made with aqua regia dissolution, takes the lysate sodium hydroxide and second
The mixed oxide-loaded solution of 1.0wt.% is made under the alkaline condition of glycol,
S3: the mixed oxide-loaded solution of step S2 being added in the ethanol solution of support dispersion, and chlorine platinum is then added
Acid and chlorine palladium acid mixed solution, heating water bath stirs 2h, is cleaned 1 time after centrifugal filtration with acetone, with washes of absolute alcohol 3 times,
It is cleaned 2 times with deionized water.For 24 hours, 500 DEG C of calcining 2h obtain catalyst for 50 DEG C of drying.
S4: being passed through in oxidation furnace evaluating apparatus after ammonia and oxygen mix, which uses 0-1200 DEG C of temperature range；It rises
0-40 DEG C of warm rate/min, within temperature stability ± 2 DEG C, within 1 DEG C of precision of control；Burner hearth internal diameter 44mm, in outer reactor
Diameter 34mm；Furnace superintendent 900mm, flat-temperature zone 400mm (± 2 DEG C), interior reactor diameter 14mm；Ammonia flow measures journey 100ml/min,
Oxygen flow meter range 500ml/min.Platinum guaze is connected by high-temperature flange, and solid powder th-1 catalyst is made by Aludirome web
It heats up 10 DEG C/minute to 800 DEG C by 1 gram of Catalyst packing into reaction tube 7 for support package, it is ammonia that experiment, which is passed through gas flow rate,
Gas 10ml/min, pure oxygen 200ml/min, as experimental gas flow velocity, rear end is connected with online gas-chromatography.Ammonia reaction gas
It is totally converted, conversion ratio 100%, gas-chromatography 11 measures the content of nitrogen and nitrogen oxide, then determines nitric oxide production selection
Property 97.25% or more, be passed through 1h collection nitric acid yield it is consistent.
Embodiment 2
Prepare Ti0.5Ce0.5O2The mixed oxide catalyst of Pt1.0%,
S1: it according to the oxide elements ratio in iron oxide, cobalt oxide, cerium oxide and oxidation titanium mixed oxide, weighs
8.6 grams of cerous nitrates prepare the solution of 0.005mol/l, and 8.7 grams of titanium tetraisopropylates are dissolved in dehydrated alcohol, 40 grams of PVP are added, add
Enter 20ml nitric acid, makes pH value 1.8.Prepared cerous nitrate solution is heated and stirred in water-bath, when water temperature reaches 80
DEG C when, start be added dropwise titanium tetraisopropylate ethanol solution, by rate of titration control in 1 drop/3s, after being added dropwise, be added dropwise about
The ammonia spirit of 50ml makes pH value 8.5, makes to precipitate complete precipitating.Period precipitating becomes khaki from milky.In there-necked flask
Middle reflux 2h ultrasonic cleaning 3 times, is then centrifuged for filtering, and dries 48h.500 DEG C of calcining 5h, grinding obtain powdered carrier.
S2: taking 1.0 grams of above-mentioned carrier to be dissolved in acetone soln, and stirring for 24 hours, weighs 0.001 gram of acetylacetone,2,4-pentanedione platinum conduct
Platinum element source, is dissolved in above-mentioned acetone soln, and then under 80 DEG C of heating water bath states, excessive hydrazine hydrate is added dropwise.Centrifugation
It uses washes of absolute alcohol 3 times after filtering, is cleaned 2 times with deionized water.For 24 hours, 500 DEG C of calcining 2h obtain catalyst for 50 DEG C of drying.
S3: it by 1.0 grams of Catalyst packings into reaction tube 7, heats up 10 DEG C/minute to 750 DEG C, is passed through ammonia and oxygen, ammonia
Throughput 10ml/min, oxygen flow 200ml/min, ammonia reaction gas are totally converted, conversion ratio 100%, gas-chromatography 11
Then the content for measuring nitrogen and nitrogen oxide determines that nitric oxide production selectivity is 97.7%, receive with the nitric acid for being passed through 1h collection
Rate is consistent.
Embodiment 3
3 difference from Example 1 of embodiment is that step S1 can be replaced: according to the oxygen in the catalyst carrier
High pressure is added with 8.6 cerous nitrates, 8.7 grams of titanium tetraisopropylates, 40 grams of PVP with 3.2 grams of hexadecylamine in compound element ratio
In reaction kettle, at a temperature of 180 DEG C, 36h is reacted, then cleans, be centrifugated, drying, grinding obtains powder.
Embodiment 4
4 difference from Example 1 of embodiment is, every the additional 8ms of 1min in step S3 heating water bath whipping process
Impulse electric field handle until precipitating completely, wherein impulse electric field field strength be 50kV/cm, pulse frequency 200Hz, pulse width
30 μ s, impulse waveform are rectangular wave.In the above way and under the conditions of handle, can be improved this catalyst loaded article the uniformity and
The effect of precipitating, and then the catalytic effect and raw material availability of catalyst of the present invention are improved, save cost.
Embodiment 5
5 difference from Example 1 of embodiment is, additional every 1.6min in step S3 heating water bath whipping process
The impulse electric field of 270ms is handled until precipitating completely, wherein impulse electric field field strength is 65kV/cm, pulse frequency 750Hz, pulse
80 μ s of width, impulse waveform is rectangular wave.In the above way and under the conditions of handle, the uniform of this catalyst loaded article can be improved
The effect of degree and precipitating, and then the catalytic effect and raw material availability of catalyst of the present invention are improved, save cost.
The actual conditions calcined in step S1 are as follows: be placed on substance after drying in the superconducting intense magnetic field that magnetic field strength is 12T
Magnetic is risen, 410 DEG C is warming up to 55 DEG C/h, activates 1.2 hours, drop magnetic to 0T, then 500 DEG C are continuously heating to 27 DEG C, calcining is total
Time is 5h, and nitrogen is added to be cooled to room temperature.Calcined material is handled by the above method and condition, the negative of carrier can be improved
Carry effect.
Embodiment 6
6 difference from Example 1 of embodiment is, additional every 2min in step S3 heating water bath whipping process
The impulse electric field of 400ms is handled until precipitating completely, wherein impulse electric field field strength is 80kV/cm, pulse frequency 1100Hz, arteries and veins
120 μ s of width is rushed, impulse waveform is rectangular wave.In the above way and under the conditions of handle, this catalyst loaded article can be improved
The effect of the uniformity and precipitating, and then the catalytic effect and raw material availability of catalyst of the present invention are improved, save cost.
The actual conditions calcined in step S1 are as follows: be placed on substance after drying in the superconducting intense magnetic field that magnetic field strength is 15T
Magnetic is risen, 420 DEG C is warming up to 60 DEG C/h, activates 1.5 hours, drop magnetic to 0T, then 500 DEG C are continuously heating to 30 DEG C, calcining is total
Time is 5h, and nitrogen is added to be cooled to room temperature.Calcined material is handled by the above method and condition, the negative of carrier can be improved
Carry effect.
The actual conditions calcined in step S3 are as follows: calcine 2h at 500 DEG C, at a temperature of 290 DEG C, nitrogen hydrogen is than for 8:2's
35min is calcined under atmosphere, is passed through inert gas later and is continued to calcine 10min, is then warming up to 500 DEG C again, and be passed through
Air calcining at constant temperature, calcining total time are 2h, and subsequent cooled to room temperature obtains catalyst.Pass through the difference under different temperatures
Atmosphere carries out last calcination processing to catalyst of the present invention, the stability of catalyst of the present invention can be improved, and enhance and originally urge
The catalytic effect of agent.
As shown in Figure 1, evaluating apparatus mainly includes controller 4, reaction tube 7, gas-chromatography 11, computer 12, gas collection
Bottle 1, gas collection bottle 2 14, gas collection bottle 3 15 and airbag 16；7 upper end of reaction tube is connected with ammonia bottle 1, oxygen cylinder 2
With pressure gauge 8, a mass flowmenter 3, controller 4 are respectively installed in ammonia bottle 1 and oxygen cylinder 2 and 7 connecting pipe of reaction tube
It is connected in pipe with reaction tube 7,4 upper end of controller is equipped with temperature sensor 5 and temperature controller 6, and 7 lower end of reaction tube is connected with gas phase
It is respectively equipped in chromatography 11 and gas receiving flask 1, gas-chromatography 11 and gas receiving flask 1 and 7 connecting pipe of reaction tube
One ball valve 9, gas-chromatography 11 are connect with argon bottle 10, computer 12, and gas collection bottle 1 is sequentially connected in series gas from right to left
Receiving flask 2 14, gas collection bottle 3 15 and airbag 16.
Predetermined purpose and technical means and efficacy achieved for the present invention is further explained pass through (the preparation of embodiment 1
Ti0.3Ce0.7O2The mixed oxide catalyst of Pt0.05%) and (the preparation Ti of embodiment 20.5Ce0.5O2The mixed oxidization of Pt1.0%
Object catalyst) invention is further explained, and by analyzing catalyst of the present invention, Fig. 2-4 show catalyst
Scanning electron microscope result figure, Fig. 5 are that the BET of load platinum catalyst schemes, and Fig. 6 is the selectivity and conversion ratio figure of load platinum catalyst.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment or equivalent replacement of some of the technical features；And
These are modified or replaceed, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (10)
1. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum, which is characterized in that catalyst carrier is oxidation
Zirconium and oxidation titanium mixed oxide, titanium oxide and cerium oxide mixed oxide, cobalt oxide, cerium oxide and titanium oxide mixed oxidization
Object, zirconium oxide, cerium oxide and oxidation titanium mixed oxide, iron oxide, cerium oxide and oxidation titanium mixed oxide, iron oxide, oxygen
Change the combination of one of cobalt, cerium oxide and oxidation titanium mixed oxide；Catalyst Payload element is platinum, platinum palladium, platinum rhodium, platinum rhodium palladium
Middle one or more combination.
2. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In, the catalyst preparation the following steps are included:
S1: according to the oxide elements ratio in the catalyst carrier, taking a certain amount of nitrate to be dissolved in deionized water,
It is configured to the solution of 0.005mol/L, and PVP is added with the dosage of 10g/L, a certain amount of nitric acid solution is added, makes solution ph
Between 1 and 2, it is placed in agitating and heating in there-necked flask, prepares a certain amount of titaniferous precursor ethanol solution, according to 1 drop/3s speed
Degree is added dropwise in there-necked flask, forms collosol and gel after being added dropwise to complete, and a certain amount of weak aqua ammonia is added to complete precipitating, described three
Flow back 2h in mouth bottle, is then centrifuged for filtering, dries 48h, then 500 DEG C of calcining 5h, grinding obtains powdered carrier；
S2: a certain amount of catalyst Payload element is taken, lysate is made with aqua regia dissolution, takes the lysate spent glycol
The mixed oxide-loaded that 0.005wt.%, 0.05wt.%, 0.5wt.%, 1wt.%, 5wt.% are made under alkaline condition is molten
Liquid,
S3: the mixed oxide-loaded solution of step S2 being added in the ethanol solution of support dispersion, and heating water bath stirs 2h, from
It is cleaned 1 time, with washes of absolute alcohol 3 times, is cleaned 2 times with deionized water, for 24 hours, 500 DEG C are forged for 50 DEG C of drying with acetone after heart filtering
2h is burnt, catalyst is obtained；
S4: ammonia and oxygen are passed through evaluating apparatus according to a certain percentage, test ammonia, nitrous oxide, nitrogen using gas-chromatography,
Using titration measuring nitric acid yield, selectivity and conversion ratio are then calculated.
3. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In preparing the mixed of two or more of zirconium oxide, cerium oxide, cobalt oxide, iron oxide and titanium oxide by sol-gal process
Oxide particle is closed, the mixed oxide particle partial size is less than 20nm.
4. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In preparing two kinds or two of spherical or sheet zirconium oxide, cerium oxide, cobalt oxide, iron oxide and titanium oxide by hydro-thermal method
Kind or more mixed oxide particle, the mixed oxide particle partial size be less than 20nm.
5. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In, using titration measuring nitric acid yield, collect gas mixture with airbag and then use gas chromatographic detection, analysis selectivity and
Conversion ratio.
6. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In, it is handled every the impulse electric field of the additional 8-400ms of 1-2min until precipitating completely in step S3 heating water bath whipping process,
In, impulse electric field field strength is 50-80kV/cm, and pulse frequency 200-1100Hz, pulse width 30-120 μ s, impulse waveform is square
Shape wave.
7. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In the actual conditions calcined in the step S1 are as follows: be placed on substance after drying in the superconducting intense magnetic field that magnetic field strength is 5-15T
Magnetic is risen, 370-420 DEG C is warming up to 50-60 DEG C/h, activates 0.5-1.5 hours, drop magnetic to 0T, then continue to heat up with 20-30 DEG C
To 500 DEG C, calcining total time is 5h, and nitrogen is added to be cooled to room temperature.
8. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In the actual conditions calcined in the step S3 are as follows: calcine 2h at 500 DEG C, at a temperature of 270-290 DEG C, nitrogen hydrogen ratio is 8:2
Atmosphere under calcine 20-35min, be passed through later inert gas continue calcine 5-10min, be then warming up to 500 DEG C again,
And it is passed through air calcining at constant temperature, calcining total time is 2h, and subsequent cooled to room temperature is stand-by.
9. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In one kind or combination of three kinds of elements of platinum rhodium palladium, aqua regia dissolution, adipic acid is reducing loaded under alkaline condition, load capacity
0.005wt.%-5wt.%.
10. a kind of catalyst of the ammoxidation nitrogen oxides of oxide carried platinum according to claim 1, feature exist
In the evaluating apparatus mainly includes controller (4), reaction tube (7), gas-chromatography (11), computer (12), gas collection bottle one
(13), gas collection bottle two (14), gas collection bottle three (15) and airbag (16)；Reaction tube (7) upper end is connected with ammonia
Respectively pacify in bottle (1), oxygen cylinder (2) and pressure gauge (8), the ammonia bottle (1) and oxygen cylinder (2) and reaction tube (7) connecting pipe
Equipped with a mass flowmenter (3), the controller (4) and reaction tube (7) are connected in pipe, and controller (4) upper end is equipped with temperature
Degree sensor (5) and temperature controller (6), reaction tube (7) lower end are connected with gas-chromatography (11) and gas receiving flask one (13),
A ball valve (9), gas are respectively installed in the gas-chromatography (11) and gas receiving flask one (13) and reaction tube (7) connecting pipe
Phase chromatography (11) is connect with argon bottle (10), computer (12), and the gas collection bottle one (13) is sequentially connected in series gas from right to left
Receiving flask two (14), gas collection bottle three (15) and airbag (16).
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| CN114797893A (en) * | 2022-04-25 | 2022-07-29 | 昆明理工大学 | Ammonia oxidation catalyst and preparation method and application thereof |
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