AU2021103091A4 - An acid-redox dual sites synergistic nh3-scr catalyst, a preparation method, and an application thereof - Google Patents
An acid-redox dual sites synergistic nh3-scr catalyst, a preparation method, and an application thereof Download PDFInfo
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- AU2021103091A4 AU2021103091A4 AU2021103091A AU2021103091A AU2021103091A4 AU 2021103091 A4 AU2021103091 A4 AU 2021103091A4 AU 2021103091 A AU2021103091 A AU 2021103091A AU 2021103091 A AU2021103091 A AU 2021103091A AU 2021103091 A4 AU2021103091 A4 AU 2021103091A4
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- 239000003054 catalyst Substances 0.000 title claims abstract description 71
- 230000009977 dual effect Effects 0.000 title claims abstract description 30
- 230000002195 synergetic effect Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 19
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims abstract description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003546 flue gas Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 15
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 230000002378 acidificating effect Effects 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 239000010955 niobium Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 claims description 3
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005695 Ammonium acetate Substances 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- 230000032683 aging Effects 0.000 claims description 2
- 235000019257 ammonium acetate Nutrition 0.000 claims description 2
- 229940043376 ammonium acetate Drugs 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 235000011056 potassium acetate Nutrition 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 7
- 230000007547 defect Effects 0.000 abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 4
- 229910010413 TiO 2 Inorganic materials 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 239000011593 sulfur Substances 0.000 abstract description 4
- 229910052717 sulfur Inorganic materials 0.000 abstract description 4
- 229910000831 Steel Inorganic materials 0.000 abstract description 3
- 238000003915 air pollution Methods 0.000 abstract description 3
- 239000004568 cement Substances 0.000 abstract description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000010959 steel Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052681 coesite Inorganic materials 0.000 abstract description 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 229910052682 stishovite Inorganic materials 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229910052905 tridymite Inorganic materials 0.000 abstract description 2
- 229910021274 Co3 O4 Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000007789 gas Substances 0.000 description 10
- 238000003760 magnetic stirring Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 239000000975 dye Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000002468 redox effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—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
- 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
- B01J23/20—Vanadium, niobium or tantalum
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8435—Antimony
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/882—Molybdenum and cobalt
Abstract
The present invention relates to the field of air pollution control technical, in particular to an
acid-redox dual sites synergistic NH 3-SCR catalyst, a preparation method and an application
thereof. Disclosed in the present invention is an acid-redox dual sites synergistic NH3-SCR
catalyst, which the general formula is AOy/RzO,,, and type A elements are different from type
R elements. AOy is selected from W03, MoO 3 , Nb 2 05 , Sb 205 , SiO2 or Mn207, and RzO2, is
selected from Fe2 03, Co3 O4 NiO, MnO 2 , CeO2 or CuO. In this invention, the hydrothermal
with impregnation method was used to synthesis the acid-redox dual sites synergistic
NH3-SCR catalyst, which effectively compensated for the defects of traditional
V2 0 5-WO3/TiO 2, such as poor adsorption capacity and excessive oxidation of NH 3, narrow
temperature window, and weak resistance of sulfur and water under low-temperature. The
catalyst in this invention can tolerate nitrogen oxide flue gas containing 0~1000 mg/m3 SO 2
and 0~20 vol.% water vapor simultaneously under 150~400 C and the space velocity of
10,000~100,000 h-1, and the denitrification efficiency can be stable above 85%, which is
suitable for the control of nitrogen oxide emissions from industrial source flue gas, such as
glass and cement boilers, steel furnaces, and bio-fueled boilers, etc.
Description
An acid-redox dual sites synergistic NH 3 -SCR catalyst, a preparation
method, and an application thereof
Field of the invention
The present invention belongs to the field of air pollution control technical, in particular to an acid-redox dual sites synergistic NH 3-SCR catalyst, a preparation method, and an application thereof. The deNO catalyst in this invention exhibit favourable NO, removal efficiency and excellent resistance to ammonium bisulfate at the temperature window of 150-400 C. Description of related art NO, is one of the important precursors of atmospheric pollutants PM 2 .5 and 03. As the NO, emission control standards for coal-fired power plants and mobile sources were improved, the NO, emissions of power plants and mobile sources have been controlled in recent years, but NO, emissions from industrial sources (such as glass and cement boilers, steel furnaces, and bio-fueled boilers) are still large and have not been effectively controlled. This makes the total annual NO, emissions national still high, resulting in high concentrations of PM 2 .5 and 03 in the atmosphere, causing severe haze weather or 03 pollution weather, and bringing great harm to the climate, environment, and human health. Therefore, it is of great significance to control of NO, emissions effectively from industrial sources for improving the air pollution problem in our country. Selective catalytic reduction of NO, with NH3 (NH 3-SCR) is currently the most effective flue gas denitrification (deNO) technology widely used in the world. The technology uses NH 3 as the reducing agent to selectively reduce NO in the flue gas to N 2 and H2 0 with the participation of 02 and the presence of the catalyst, of which the key is the catalyst. Now, the deNO catalyst commonly used internationally is V 2 0-WO 3 (Mo0 3 )/TiO2 designed according to the coal-fired flue gas environment, which has high denitration efficiency and good N 2 selectivity. However, there are also some defects of traditional V 2 0-WO 3 (Mo 3 )/TiO 2 , such as poor adsorption capacity and excessive oxidation of NH 3 ,
narrow temperature window, and weak resistance of sulfur and water under low-temperature, which is not suitable for the deNO of low-temperature industrial flue gas containing water, sulfur and alkaline (earth) metals. In addition, V 2 0 5 , with strong biological toxicity, is harmful to the environment and human health, and the traditional catalyst is easily poisoned and deactivated during the deNO0 process. Therefore, it is urgent to develop a new non-toxic deNO, catalyst. Topsee et al. proposed the reaction mechanism followed on the V 2 0 5/TiO 2 catalyst in 1994, which stated the catalyst needs to have both an acidic site and a redox site to complete the entire NH 3-SCR reaction cooperatively. The reducing agent NH 3 is adsorbed on the acidic site and further activated at the redox site. Here, the invention patent developed a catalyst with both acidic site and redox site, in which RzO, with redox was chosen as supporter and acidic AOy was dispersed on the supporter. Finally, an acid-redox dual sites synergistic NH 3-SCR catalyst AOy/RO2, was obtained.
Chinese invention patents with publication numbers CN102716 A disclosed a catalyst
suitable for low temperature deNO, catalyst at 150-250 °C, which exhibited an enhanced
low-temperature catalytic activity coming from the strong interaction between V and transition
metals forming a solid solution or between V 2 05 and transition metal oxides. While V 2 05 has
strong biological toxicity, and the removing rate of NO, reached only 70% in the
low-temperature flue gas containing 10 vol.% H 2 0 and 300 ppm (860 mg/m 3 ) SO 2 , restricting
the practical application of the catalyst. Therefore, there are broad development prospects to
develop a new-type NH 3 -SCR catalyst with acid-redox dual sites synergistic.
Summary of the invention
The technical problem to be solved by the present invention: Traditional V 2 0-WO 3 /TiO 2 has
some defects of poor adsorption capacity and excessive oxidation of NH 3 , narrow temperature
window, and weak resistance of sulfur and water under low-temperature. To solve the existing
technology defects, this invention provides provided an acid-redox dual sites synergistic
NH 3 -SCR catalyst, a preparation method, and an application thereof. The new-type acid-redox dual sites synergistic NH 3 -SCR catalyst in the present invention has both acidic and redox properties and dual sites synergistic NH 3 -SCR catalyst, and the general formula is AOy/RO,. AOy in the present invention is an acidic oxide, chosen from W03, MoO3, Nb205, Sb 2 05 ,
SiO2 or Mn 2 0 7. RzO,, is a redox oxide, selected from Fe2 03, CoO 4 NiO, MnO 2 , CeO 2 or CuO. In this invention, AOy and RzO,, represent acidic oxide and redox oxide, in which type A elements are different from type R elements. A precursor is one or more of the molybdate, tungstate, acetate, oxalate, nitrate, manganate or silicate of molybdenum, tungsten, niobium, antimony, silicon, manganese, and R precursor is one or more of the nitrate, acetate, sulfate, oxalate or chloride of iron, cobalt, nickel, manganese, cerium, and copper.
The method for preparing new-type NH3 -SCR catalyst with acid-redox dual sites synergistic mentioned above, and the specific steps are as follows: Method 1: (1) Measure the solvents proportionally into a beaker, and make of even mixture; (2) The R precursor and precipitant were successively weighed and dissolved in the mixture solvents obtained in step (1), and keep stirring until uniform; (3) Transfer the mixture obtained in step (2) to the Teflon-lined stainless steel autoclave, and put it into the oven for hydrothermal reaction, then cool to room temperature after the reaction is over; (4) Centrifugate, wash with de-ionized water and ethanol several times, respectively, and dry the samples obtained in step (3); (5) Grind the dried samples into powders, calcine the powders in a muffle furnace, and then get the RxOy; (6) Weigh and dissolve A precursor in deionized water, and keep stirring until completely dissolved; (7) Add the RxOy obtained in step (5) into the solution obtained in step (6), and sonicate until uniform dispersion; (8) Place the suspension obtained in step (7) into the water bath, and continue stirring until the solution evaporated completely; (9) Dry the samples collected in step (8) in the oven; (10) Grind the dried samples into powders without particles, calcine the powders in a muffle furnace, and then get the catalyst; (11) Granulate the catalyst by sieving with 40~60 mesh, and then get the acid-redox dual sites synergistic NH 3-SCR catalyst. Method 2: (1) Weigh and dissolve R precursor in deionized water, and keep stirring until completely dissolved; (2) Weigh and dissolve the precipitant in deionized water, and keep stirring until completely dissolved; (3) Add the solution obtained in step (1) to the solution obtained in step (2) dropwise, and keep on stirring and aging; (4) Filtrate, wash with de-ionized water several times, and dry the samples obtained in step (3); (5) Grind the dried samples into powders, calcine the powders in a muffle furnace, and then get the RxOy; (6) Weigh and dissolve A precursor in deionized water, and keep stirring until completely dissolved; (7) Add the RxOy obtained in step (5) into the solution obtained in step (6), and sonicate until uniform dispersion; (8) Place the suspension obtained in step (7) into the water bath, and continue stirring until the solution evaporated completely; (9) Dry the samples collected in step (8) in the oven; (10) Grind the dried samples into powders without particles, calcine the powders in a muffle furnace, and then get the catalyst; (11) Granulate the catalyst by sieving with 40~60 mesh, and then get the acid-redox dual sites synergistic NH 3-SCR catalyst. Preferably, the A precursor described is one or more of the molybdate, tungstate, acetate, oxalate, nitrate, manganate or silicate of molybdenum, tungsten, niobium, antimony, silicon, manganese, and the R precursor described is one or more of the nitrate, acetate, sulfate, oxalate or chloride of iron, cobalt, nickel, manganese, cerium, and copper. And the ratio is 1: 1-1: 10. Preferably, the solvent described is a mixture of ethanol and deionized water, and the ratio is 1: 15~1: 30. Preferably, the precipitant described in Method 1 is sodium acetate, ammonium acetate, potassium acetate, and the precipitant described in Method 2 is sodium hydroxide, potassium hydroxide, ammonium hydroxide, oxalic acid. Preferably, the drying temperature described is 60 ~ 120 °C, and the drying time is 8 ~ 20 h. Preferably, the temperature of water bath described is 50 ~ 100 °C. Preferably, the calcination temperature described in step (5) and (10) is 300 ~ 800 °C, the heating rate is 1 ~ 10 °C/min, and the calcination time is 2 ~ 6 h.
Benefits of the invention
In the present invention, an electrospinning technique combined with a sintering process is used to synthesis the low-dimensional heterostructured nano-material photocatalyst. Low dimensional nano-material has the advantages of large specific surface area and favorable charge transfer. Bi2 WO 6 is a visible light responsive semiconductor, which can effectively compensate for the defects of the large band gap and low sunlight utilization rate of commercial TiO2 . The heterojunctions effectively promote the separation and inhibit the recombination of photogenerated electron-hole. The photodegradation ratio of photocatalyst in the present invention reached above 80% for degrading the organic dyes with certain concentration under ultraviolet-visible light. The photocatalyst is specifically applicable for controlling sewage discharge from some factories, such as chemical indicators, printing and dyeing textiles, biological dyes, colored glass, pharmaceuticals and the like. The advantages of the new-type acid-redox dual sites synergistic NH 3 -SCR catalyst in the present invention are: The acid-redox dual sites synergistic NH 3 -SCR catalyst, prepared by the hydrothermal with impregnation method, possesses acid and redox dual active sites formed at the interface between AOy and RzO.. This characteristic sites are conducive to adsorption of the reducing agent NH 3, and the redox oxide RzO, will further activate NH 3 to participate in the reaction directly, which improve the utilization efficiency of NH 3 and accelerate the NH 3 -SCR reaction process. The catalyst in this invention can tolerate nitrogen oxide flue gas containing 0~1000 mg/m3 SO2 and 0~20 vol.% water vapor simultaneously under 150~400 C and the space velocity of 10,000~100,000 h-1, and the denitrification efficiency can be stable above 85%, which is suitable for the control of nitrogen oxide emissions from industrial source flue gas, such as glass and cement boilers, steel furnaces, and bio-fueled boilers, etc.
Specific implementation modalities
The present invention will be further elaborated below in conjunction with specific embodiments. It should be understood these embodiments are merely as illustrative of the inventions and not in limitation thereof. The experimental methods without indicated specific conditions in the following embodiments usually follow the conventional conditions or the conditions suggested by the manufacturer.
Embodiment 1:
1. The preparation of catalyst: In a typical experiment, 0.90 g CeCl 3 7H 20 was dissolved in 10 mL deionized water under magnetic stirring at room temperature, then the above solution was added into 50 mL NaOH solution (9 mol/L). The mixture was sealed in a Teflon-lined stainless steel autoclave (100 mL) and maintained in the oven at 140 °C for 48 h. After natural cooling to room temperature, the resulting solid was washed with de-ionized water and ethanol several times, respectively, dried at 60 °C for 4 h and calcined at 400 °C in air for 4 h. 6.64 g Nb(HC 2 0 4 ) 5was solved in 40 mL de-ionized water to form an aqueous solution, to which the CeO2 powder (2.00 g) was added under vigorously magnetic stirring at 80 °C until the water was evaporated. Then the samples were dried at 80 °C for 12 h, and calcined at 550 °C at a rate of 2 °C/min in air for 3 h. 2. The performance test of catalyst: SCR activity measurements were performed in a fixed-bed quartz reactor (inner diameter 8 mm) under atmospheric pressure. The feed gas contained 500 ppm NO, 500 ppm NH 3 , 3.0 vol% 02, and balanced N 2 . H 2 0 (20 vol.%) and SO2 (1200 mg/m 3) were turn on when needed. The total flow rate was 500 mL min' and 0.6 g sample (40-60 mesh) was used. The gas hourly space velocity (GHSV) was calculated to be
840,000 hand the reaction temperature was set to 150~400 °C. The concentration of NO in the outlet and N 2 selectivity in the SCR process were continually monitored by a online Fourier-transform infrared spectrometer (Thermo Scientific Antaris IGS analyzer). Under the condition without H2 0 or S02, the deNO, efficiency and the N 2 selectivity of the catalyst is stable above 95% and 98%, respectively, and when H 2 0 or S02 were turn on, the deNOx efficiency and the N 2 selectivity still remained stable above 90% and 94%, respectively, which proved the catalyst has strong resistance to H 2 0 or S02.
Embodiment 2:
1. The preparation of catalyst: In a typical experiment, 0.90 g CeCl 3 7H 20 was dissolved in 10 mL deionized water under magnetic stirring at room temperature, then the above solution was added into 50 mL NaOH solution (9 mol/L). The mixture was sealed in a Teflon-lined stainless steel autoclave (100 mL) and maintained in the oven at 140 °C for 48 h. After natural cooling to room temperature, the resulting solid was washed with de-ionized water and ethanol several times, respectively, dried at 60 °C for 4 h and calcined at 400 °C in air for 4 h. 2.97 g H 28 N 6 O4 1W 2 1was solved in 40 mL de-ionized water to form an aqueous solution, to which the CeO2 powder (2.00 g) was added under vigorously magnetic stirring at 80 °C until the water was evaporated. Then the samples were dried at 80 °C for 12 h, and calcined at 550 °C at a rate of 2 °C/min in air for 3 h. 2. The performance test of catalyst: SCR activity measurements were performed in a fixed-bed quartz reactor (inner diameter 8 mm) under atmospheric pressure. The feed gas contained 500 ppm NO, 500 ppm NH 3 , 3.0 vol% 02, and balanced N 2 . H 2 0 (20 vol.%) and S02 (1200 mg/m 3) were turn on when needed. The total flow rate was 500 mL min' and 0.6 g sample (40-60 mesh) was used. The gas hourly space velocity (GHSV) was calculated to be 840,000 hand the reaction temperature was set to 150~400 °C. The concentration of NO in the outlet and N 2 selectivity in the SCR process were continually monitored by a online Fourier-transform infrared spectrometer (Thermo Scientific Antaris IGS analyzer). Under the condition without H2 0 or S02, the deNO, efficiency and the N 2 selectivity of the catalyst is stable above 98% and 99%, respectively, and when H 2 0 or S02 were turn on, the deNOx efficiency and the N 2 selectivity still remained stable above 95% and 96%, respectively, which proved the catalyst has strong resistance to H 2 0 or SO 2 .
Embodiment 3:
1. The preparation of catalyst: In a typical experiment, 0.54 g FeCl 3 -6H20 was dissolved in a mixed solution of ethanol (30.0 mL) and deionized water (1.5 mL) under vigorously magnetic stirring until completely dissolved, to which 1.91 g CH 3COONa was added under stirring. The mixture was sealed in a Teflon-lined stainless steel autoclave (100 mL) and maintained in the oven at 180 °C for 12 h. After natural cooling to room temperature, the resulting solid was washed with de-ionized water and ethanol several times, respectively, dried at 80 °C for 12 h. Then 4.126 g H 2 8 N 6 O4 1W 21 was solved in de-ionized water to form an aqueous solution, to which the a-Fe 2 03 powder (2.00 g) was added under vigorously magnetic stirring at 80 °C until the water was evaporated. Then the samples were dried at 80 °C for 12 h, and calcined at 550 °C at a rate of 2 °C/min in air for 3 h. 2. The performance test of catalyst: SCR activity measurements were performed in a fixed-bed quartz reactor (inner diameter 8 mm) under atmospheric pressure. The feed gas contained 500 ppm NO, 500 ppm NH 3 , 3.0 vol% 02, and balanced N 2 . H 2 0 (20 vol.%) and SO2 (1200 mg/m 3) were turn on when needed. The total flow rate was 500 mL min' and 0.6 g sample (40-60 mesh) was used. The gas hourly space velocity (GHSV) was calculated to be 840,000 hand the reaction temperature was set to 150~400 °C. The concentration of NO in the outlet and N 2 selectivity in the SCR process were continually monitored by a online Fourier-transform infrared spectrometer (Thermo Scientific Antaris IGS analyzer). Under the condition without H2 0 or SO2 , the deNO, efficiency and the N 2 selectivity of the catalyst is stable above 92% and 98%, respectively, and when H 2 0 or SO 2 were turn on, the deNOx efficiency and the N 2 selectivity still remained stable above 88% and 95%, respectively, which proved the catalyst has strong resistance to H 2 0 or SO 2 .
Embodiment 4:
1. The preparation of catalyst: In a typical experiment, 0.54 g FeCl 3 -6H 20 was dissolved in a mixed solution of ethanol (30.0 mL) and deionized water (1.5 mL) under vigorously magnetic stirring until completely dissolved, to which 1.91 g CH 3COONa was added under stirring. The mixture was sealed in a Teflon-lined stainless steel autoclave (100 mL) and maintained in the oven at 180 °C for 12 h. After natural cooling to room temperature, the resulting solid was washed with de-ionized water and ethanol several times, respectively, dried at 80 °C for 12 h. Then 4.98 g Sb(CH 3COO) 3 was solved in de-ionized water to form an aqueous solution, to which the a-Fe 203 powder (2.00 g) was added under vigorously magnetic stirring at 80 °C until the water was evaporated. Then the samples were dried at 80 °C for 12 h, and calcined at 550 °C at a rate of 2 °C/min in air for 3 h. 2. The performance test of catalyst: SCR activity measurements were performed in a fixed-bed quartz reactor (inner diameter 8 mm) under atmospheric pressure. The feed gas contained 500 ppm NO, 500 ppm NH 3 , 3.0 vol% 02, and balanced N 2 . H 2 0 (20 vol.%) and SO2 (1200 mg/m 3) were turn on when needed. The total flow rate was 500 mL min' and 0.6 g sample (40-60 mesh) was used. The gas hourly space velocity (GHSV) was calculated to be 840,000 h-'and the reaction temperature was set to 150~400 °C. The concentration of NO in the outlet and N 2 selectivity in the SCR process were continually monitored by a online
Fourier-transform infrared spectrometer (Thermo Scientific Antaris IGS analyzer). Under the condition without H2 0 or S02, the deNO, efficiency and the N 2 selectivity of the catalyst is stable above 90% and 96%, respectively, and when H 2 0 or S02 were turn on, the deNOx efficiency and the N 2 selectivity still remained stable above 86% and 92%, respectively, which proved the catalyst has strong resistance to H 2 0 or S02.
Embodiment 5:
1. The preparation of catalyst: In a typical experiment, 0.71 g CoCl2-6H20 and 0.38 g H 2 C2 0 4 were dissolved in deionized water, respectively, under vigorously magnetic stirring until completely dissolved. The CoCl2 solution was added into H 2 C 2 0 4 solution dropwise, and keep on stirring for 30 min. The resulting solid was washed with de-ionized water and ethanol several times, respectively, dried at 80 °C for 12 h. Then 2.63 g (NH 4 )AMo7024-4H 2 0 was solved in
de-ionized water to form an aqueous solution, to which the C0304 powder (2.00 g) was added under vigorously magnetic stirring at 80 °C until the water was evaporated. Then the samples were dried at 80 °C for 12 h, and calcined at 550 °C at a rate of 2 °C/min in air for 3 h. 2. The performance test of catalyst: SCR activity measurements were performed in a fixed-bed quartz reactor (inner diameter 8 mm) under atmospheric pressure. The feed gas contained 500 ppm NO, 500 ppm NH 3 , 3.0 vol% 02, and balanced N 2 . H 2 0 (20 vol.%) and S02 (1200 mg/m 3) were turn on when needed. The total flow rate was 500 mL min' and 0.6 g sample (40-60 mesh) was used. The gas hourly space velocity (GHSV) was calculated to be 840,000 hand the reaction temperature was set to 150~400 °C. The concentration of NO in the outlet and N 2 selectivity in the SCR process were continually monitored by a online Fourier-transform infrared spectrometer (Thermo Scientific Antaris IGS analyzer). Under the condition without H2 0 or SO 2 , the deNO, efficiency and the N 2 selectivity of the catalyst is stable above 92% and 95%, respectively, and when H 2 0 or SO 2 were turn on, the deNOx efficiency and the N 2 selectivity still remained stable above 88% and 92%, respectively, which proved the catalyst has strong resistance to H 2 0 or SO 2 .
Claims (11)
1. An acid-redox dual sites synergistic NH 3-SCR catalyst, the characteristics of which lie in that there are both acidic sites and redox sites, and the general formula is AOy/ROW in which type A elements are different from type R elements. AOy is selected from acidic oxides W03, MoO 3 ,Nb 2 0 5 Sb 2 0 or Mn 20 7, and RzO, is selected from redox oxides Fe 2 03, Co0O4 5 SiO 2
NiO, MnO2, CeO 2 or CuO.
2. The method for preparing an acid-redox dual sites synergistic NH 3-SCR catalyst described according to claim 1, the characteristics of which lie in that the specific steps are as follows: (1) Measure the solvents proportionally into a beaker, and make of even mixture; (2) The R precursor and precipitant were successively weighed and dissolved in the mixture solvents obtained in step (1), and keep stirring until uniform; (3) Transfer the mixture obtained in step (2) to the Teflon-lined stainless steel autoclave, and put it into the oven for hydrothermal reaction, then cool to room temperature after the reaction is over; (4) Centrifugate, wash with de-ionized water and ethanol several times, respectively, and dry the samples obtained in step (3); (5) Grind the dried samples into powders, calcine the powders in a muffle furnace, and then get the RxOy; (6) Weigh and dissolve A precursor in deionized water, and keep stirring until completely dissolved; (7) Add the RxOy obtained in step (5) into the solution obtained in step (6), and sonicate until uniform dispersion; (8) Place the suspension obtained in step (7) into the water bath, and continue stirring until the solution evaporated completely; (9) Dry the samples collected in step (8) in the oven; (10) Grind the dried samples into powders without particles, calcine the powders in a muffle furnace, and then get the catalyst; (11) Granulate the catalyst by sieving with 40~60 mesh, and then get the acid-redox dual sites synergistic NH 3-SCR catalyst.
3. The preparation method of the acid-redox dual sites synergistic NH 3-SCR catalyst defined according to claim 2, the characteristics of which lie in that the solvent described in step (1) of the above method is a mixture of ethanol and deionized water, and the ratio is 1: ~1: 30.
4. The preparation method of the acid-redox dual sites synergistic NH 3-SCR catalyst defined according to claim 2, the characteristics of which lie in that the precipitant described in step (2) is sodium acetate, ammonium acetate, potassium acetate.
5. The method for preparing an acid-redox dual sites synergistic NH 3-SCR catalyst described according to claim 1, the characteristics of which lie in that the specific steps are as follows: (1) Weigh and dissolve R precursor in deionized water, and keep stirring until completely dissolved; (2) Weigh and dissolve the precipitant in deionized water, and keep stirring until completely dissolved; (3) Add the solution obtained in step (1) to the solution obtained in step (2) dropwise, and keep on stirring and aging; (4) Filtrate, wash with de-ionized water several times, and dry the samples obtained in step (3); (5) Grind the dried samples into powders, calcine the powders in a muffle furnace, and then get the RxOy; (6) Weigh and dissolve A precursor in deionized water, and keep stirring until completely dissolved; (7) Add the ROy obtained in step (5) into the solution obtained in step (6), and sonicate until uniform dispersion; (8) Place the suspension obtained in step (7) into the water bath, and continue stirring until the solution evaporated completely; (9) Dry the samples collected in step (8) in the oven; (10) Grind the dried samples into powders without particles, calcine the powders in a muffle furnace, and then get the catalyst; (11) Granulate the catalyst by sieving with 40~60 mesh, and then get the acid-redox dual sites synergistic NH 3-SCR catalyst.
6. The preparation method of the acid-redox dual sites synergistic NH 3-SCR catalyst defined according to claim 5, the characteristics of which lie in that the precipitant described in step (2) is sodium hydroxide, potassium hydroxide, ammonium hydroxide, oxalic acid.
7. The preparation method of the acid-redox dual sites synergistic NH 3-SCR catalyst defined according to claim 2 and 5, the characteristics of which lie in that the A precursor described in step (6) is one or more of the molybdate, tungstate, acetate, oxalate, nitrate, manganate or silicate of molybdenum, tungsten, niobium, antimony, silicon, manganese, and the R precursor described in step (6) is one or more of the nitrate, acetate, sulfate, oxalate or chloride of iron, cobalt, nickel, manganese, cerium, and copper. And the ratio is 1: 1~1: 10.
8. The preparation method of the acid-redox dual sites synergistic NH 3-SCR catalyst defined according to claim 2 and 5, the characteristics of which lie in that the drying temperature described in step (4) and (9) is 60 ~ 120 °C, and the drying time is 8 ~ 20 h.
9. The preparation method of the acid-redox dual sites synergistic NH 3-SCR catalyst defined according to claim 2 and 5, the characteristics of which lie in that the temperature of water bath described in step (8) is 50 ~ 100 °C.
10. The preparation method of the acid-redox dual sites synergistic NH 3-SCR catalyst defined according to claim 2 and 5, the characteristics of which lie in that the calcination temperature described in step (5) and (10) is 300 ~ 800 °C, the heating rate is 1 ~ 10 °C/min, and the calcination time is 2 ~ 6 h.
11. The acid-redox dual sites synergistic NH 3-SCR catalyst described according to claim 1, is suitable for the control of nitrogen oxide emissions from industrial source flue gas.
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