CN116651436A - Water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst and preparation method thereof - Google Patents
Water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 110
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 27
- 239000011593 sulfur Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical group CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 24
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 23
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004327 boric acid Substances 0.000 claims abstract description 20
- 239000003365 glass fiber Substances 0.000 claims abstract description 20
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 17
- 239000004310 lactic acid Substances 0.000 claims abstract description 16
- 235000014655 lactic acid Nutrition 0.000 claims abstract description 16
- 239000004480 active ingredient Substances 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 36
- 150000001875 compounds Chemical class 0.000 claims description 28
- 235000010215 titanium dioxide Nutrition 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 26
- 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 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical group [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 16
- 239000002131 composite material Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 16
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 12
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 12
- 235000006408 oxalic acid Nutrition 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 10
- 239000002518 antifoaming agent Substances 0.000 claims description 9
- 239000011651 chromium Substances 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 6
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000001038 titanium pigment Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 24
- 230000000607 poisoning effect Effects 0.000 abstract description 11
- 231100000572 poisoning Toxicity 0.000 abstract description 10
- 239000013078 crystal Substances 0.000 abstract description 8
- 230000002195 synergetic effect Effects 0.000 abstract description 7
- 239000013530 defoamer Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- 229910000420 cerium oxide Inorganic materials 0.000 description 5
- 238000006477 desulfuration reaction Methods 0.000 description 5
- 230000023556 desulfurization Effects 0.000 description 5
- 239000003546 flue gas Substances 0.000 description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 5
- 229910000428 cobalt oxide Inorganic materials 0.000 description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 4
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 3
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 229910000423 chromium oxide Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000003303 reheating Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- -1 industrial boilers Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000004056 waste incineration Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/56—Nitrogen oxides
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01J23/22—Vanadium
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- 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
- B01J23/26—Chromium
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- 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
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
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Abstract
The invention relates to the technical field of denitration catalysts, in particular to a water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst which comprises a carrier, active ingredients, strength auxiliary agents, low-temperature and wide-temperature active auxiliary agents and defoamers, wherein the carrier is a catalyst with high strength; the carrier is titanium dioxide and active carbon mixture; the active ingredient is a crystal phase V 2 O 5 The method comprises the steps of carrying out a first treatment on the surface of the The strength auxiliary agent is glass fiber, boric acid and silicon dioxide; the low-temperature and wide-temperature active auxiliary agent is CeO 2 、CoO、Cr 2 O 3 One or two of the following components; the defoamer is lactic acid. The invention adopts V 2 O 5 The CeO takes the mixture of active components, titanium dioxide and active carbon as a carrier 2 、CoO、Cr 2 O 3 One or two of the components are low-temperature and wide-temperature active auxiliary agents, and pass through a crystal phase V 2 O 5 With CeO 2 、CoO、Cr 2 O 3 One or two substances of the three-phase catalyst have synergistic effect, broaden low-temperature activity window, obviously improve the activity of the catalyst at the temperature of 80-130 ℃ in a low-temperature section, resist 15% water poisoning and resist 300mg/m in a low-temperature environment 3 SO 2 Poisoning performance.
Description
Technical Field
The invention relates to the technical field of denitration catalysts, in particular to a water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst and a preparation method thereof.
Background
In recent years, the proportion of non-electric industry in atmospheric treatment is gradually increased, and the temperature of flue gas discharged by some industries is lower, such as coking, cement, glass, industrial boilers, garbage incineration and other industries, so that research on efficient low-temperature denitration technology is an important direction of the existing denitration technology. The main component of the commercial catalyst is V 2 O 5 -WO 3 、MoO 3 /TiO 2 In the form of TiO 2 Is a carrier, V 2 O 5 As active ingredient, WO 3 Or MoO 3 The addition of the active auxiliary agent improves the high-low temperature activity of the catalyst and effectively inhibits side reactions. However, the catalyst belongs to a medium-high temperature catalyst, the activity temperature window is 300-400 ℃, the denitration activity of the catalyst begins to be reduced in a temperature range lower than or higher than the activity temperature window, reversible/irreversible poisoning deactivation occurs, the requirement of the industry that the temperature of discharged flue gas is lower than 300 ℃ can not be met, and if a denitration process after flue gas reheating is adopted, the energy consumption is increased. The denitration process can be placed after the dedusting or desulfurization process by utilizing the ultralow-temperature SCR denitration, so that the abrasion and poisoning effects of smoke dust on the catalyst can be reduced, and the reheating of the smoke gas is avoided, thereby improving the energy efficiency and saving the running cost. However, in ultra-low temperature environment, water vapor is often present on the surface of the catalyst in the form of a liquid film, which is extremely liable to cause active coverage and poisoning, and in addition, SO at low temperature 2 The presence may also lead to sulfur formationThe ammonium bisulfate covers the surface of the catalyst to cause the deactivation of the catalyst, so that the research of the water-resistant sulfur-resistant ultralow temperature denitration catalyst has very important significance for the ultralow temperature denitration industry.
Publication No. CN110961114A discloses a desulfurization and denitrification catalyst and a preparation method thereof, and the active component of the catalyst is V 2 O 5 Or V 2 O 5 And Fe (Fe) 2 O 3 The catalyst promoter is at least one of Co, ce and Mn, and the carrier is modified active coke. The invention adopts an impregnation method to load active ingredients of vanadium pentoxide, ferrous oxide, and cocatalysts of cobalt oxide, cerium oxide and manganese oxide, and the loaded active coke has good effect on desulfurization and denitration, so that the integrated purification emission standard of desulfurization and denitration for large-scale flue gas emission enterprises can be met. However, the catalyst belongs to a medium-high temperature catalyst, the activity window is 300-500 ℃, and the catalyst has good effect on desulfurization and denitration.
Disclosure of Invention
The invention aims to solve the technical problems of poor water-resistance sulfur-resistance poisoning-resistance performance and low denitration catalyst efficiency of the catalyst in an ultralow temperature environment in the prior art.
The invention solves the technical problems by the following technical means:
the invention provides a water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst, which comprises a carrier, an active ingredient, a strength auxiliary agent, a low-temperature and wide-temperature active auxiliary agent, a defoaming agent and an adhesive;
the carrier is titanium dioxide and active carbon mixture;
the active ingredient is V 2 O 5 ；
The strength auxiliary agent is glass fiber, boric acid and silicon dioxide;
the low-temperature and wide-temperature active auxiliary agent is CeO 2 、CoO、Cr 2 O 3 One or two substances of (a) and (b);
the defoaming agent is lactic acid;
the adhesive is pseudo-boehmite.
The beneficial effects are that: the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst provided by the invention takes a crystal phase V 2 O 5 The active component, titanium dioxide and active carbon mixture are used as carriers, and the active carbon and titanium dioxide mixed carrier can provide active sites with larger specific surface area and stronger selectivity; glass fiber, boric acid and silicon dioxide are used as strength auxiliary agents, the glass fiber provides a catalyst skeleton function, strength, boric acid and silicon dioxide can be provided during catalyst extrusion, and the compressive strength of the catalyst can be maintained by adding the catalyst, so that the low-temperature activity level is maintained; the pseudo-boehmite is used as a binder, so that the strength of the catalyst is improved, and the internal pore size distribution of the catalyst is regulated; lactic acid is a defoaming agent, and bubbles in the powder mixing process are removed; ceO (CeO) 2 、CoO、Cr 2 O 3 One or two of the substances are low-temperature and wide-temperature active auxiliary agents, and pass through a crystal phase V 2 O 5 With CeO 2 、CoO、Cr 2 O 3 One or two substances of the three-phase catalyst have synergistic effect, broaden low-temperature activity window, obviously improve the activity of the catalyst at the temperature of 80-130 ℃ in a low-temperature section, resist 15% water poisoning and resist 300mg/m in a low-temperature environment 3 SO 2 Poisoning performance.
The second aspect of the present invention provides a method for preparing the above catalyst, comprising the steps of:
(1) Weighing a proper amount of oxalic acid, adding deionized water, stirring, adding ammonium metavanadate, stirring and dissolving to obtain a compound clear solution 1;
(2) Weighing a proper amount of one or two substances of cerium nitrate, cobalt nitrate and chromium nitrate, and adding deionized water for dissolution to obtain a compound clarified solution 2; uniformly mixing the compound clarified solution 1 and the compound clarified solution 2 to obtain a compound clarified solution 3;
(3) Uniformly mixing titanium dioxide and activated carbon powder, adding the mixture into the composite clarified solution 3, uniformly stirring, and simultaneously adding a proper amount of lactic acid, boric acid, glass fiber, silicon dioxide and pseudo-boehmite to obtain uniform bulk slurry;
(4) Extruding and molding the uniform bulk slurry by using a strip extruder to obtain a strip catalyst;
(5) And drying the bar-shaped catalyst, and placing the dried bar-shaped catalyst into a muffle furnace for calcination to obtain the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst.
Preferably, the molar ratio of oxalic acid to ammonium metavanadate in the step (1) is 1:1-3.
Preferably, cerium nitrate in the step (2) accounts for 8-10% of the mass of the titanium dioxide.
Preferably, the mass of the activated carbon powder in the step (3) is 1-5% of the mass of the titanium dioxide, the mass of the glass fiber is 2-5% of the mass of the titanium dioxide, and the mass of the boric acid and the silicon dioxide is 7-15% of the mass of the titanium dioxide.
Preferably, the lactic acid in the step (3) is 1% -3% of the mass of the titanium pigment.
Preferably, the pseudo-boehmite in the step (3) accounts for 10-20% of the mass of the titanium white powder.
Preferably, in the step (5), the materials are dried in an oven at 80-100 ℃ for 2-6 hours.
Preferably, the calcination temperature in step (5) is 270 ℃ and the time is 3-5h.
The invention has the advantages that:
1. the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst provided by the invention takes a crystal phase V 2 O 5 The active component is titanium dioxide and active carbon mixture which is used as a carrier, and the active carbon and titanium dioxide mixture carrier can provide active sites with larger specific surface area and stronger selectivity; glass fiber, boric acid and silicon dioxide are strength aids, wherein the glass fiber provides a catalyst skeleton function, strength can be provided when the catalyst is extruded, and the boric acid and the silicon dioxide are added simultaneously to maintain the compressive strength of the catalyst and the low-temperature activity level; the pseudo-boehmite is used as a binder, so that the strength of the catalyst is improved, and the internal pore size distribution of the catalyst is regulated; lactic acid is a defoaming agent, and bubbles in the powder mixing process are removed; ceO (CeO) 2 、CoO、Cr 2 O 3 One or two of the substances are low-temperature and wide-temperature active auxiliary agents, and pass through a crystal phase V 2 O 5 With CeO 2 、CoO、Cr 2 O 3 One or two substances of the two substances cooperate to widen the low-temperature activity window, have obvious promotion effect on the activity of the catalyst at the low-temperature section of 80-130 ℃, and are used for preparing the catalystHas 15% water poisoning resistance and 300mg/m resistance under low temperature environment 3 SO 2 Poisoning performance.
2. The invention firstly obtains clarified composite solution by mixing active components, then evenly mixes the carrier and the composite clarified solution, and dissolves ammonium metavanadate by oxalic acid to lead V to be 2 O 5 V converted to crystalline state 2 O 5 The active space is improved, meanwhile, one or two substances of cerium nitrate, cobalt nitrate and chromium nitrate with high oxidation activity are calcined to be converted into cerium oxide, cobalt oxide and chromium oxide which are used as low-temperature active auxiliary agents and active temperature window auxiliary agents, the denitration efficiency of the prepared catalyst can reach more than 80% in a low-temperature range of 80-130 ℃, meanwhile, the catalyst strength is high, the contact area of the strip-shaped catalyst and gas is large, the preparation process is simple, the catalyst can be applied to various industries such as coking, cement, glass, industrial boilers and waste incineration, and the energy consumption loss of flue gas reheating is reduced.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Those of skill in the art, without any particular mention of the techniques or conditions, may follow the techniques or conditions described in the literature in this field or follow the product specifications.
A water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst comprises a carrier, an active ingredient, a strength auxiliary agent, a low-temperature and wide-temperature active auxiliary agent, a defoaming agent and an adhesive;
the carrier is titanium dioxide and active carbon mixture;
the active ingredient is V 2 O 5 ；
The strength auxiliary agent is glass fiber, boric acid and silicon dioxide;
the low-temperature and wide-temperature active auxiliary agent is CeO 2 、CoO、Cr 2 O 3 One or two substances of (a) and (b);
the defoaming agent is lactic acid;
the adhesive is pseudo-boehmite.
The beneficial effects are that: the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst provided by the invention takes a crystal phase V 2 O 5 The active component, titanium dioxide and active carbon mixture are used as carriers, and the active carbon and titanium dioxide mixed carrier can provide active sites with larger specific surface area and stronger selectivity; glass fiber, boric acid and silicon dioxide are strength aids, wherein the glass fiber provides a catalyst skeleton function, strength can be provided when the catalyst is extruded, and the boric acid and the silicon dioxide are added simultaneously to maintain the compressive strength of the catalyst and the low-temperature activity level; the pseudo-boehmite is used as a binder, so that the strength of the catalyst is improved, and the internal pore size distribution of the catalyst is regulated; lactic acid is a defoaming agent, and bubbles in the powder mixing process are removed; ceO (CeO) 2 、CoO、Cr 2 O 3 One or two of the substances are low-temperature and wide-temperature active auxiliary agents, and pass through a crystal phase V 2 O 5 With CeO 2 、CoO、Cr 2 O 3 One or two substances of the three-phase catalyst have synergistic effect, broaden low-temperature activity window, obviously improve the activity of the catalyst at the temperature of 80-130 ℃ in a low-temperature section, resist 15% water poisoning and resist 300mg/m in a low-temperature environment 3 SO 2 Poisoning performance.
Example 1
The embodiment provides a preparation method of a water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst, which comprises the following specific steps:
(1) 12g of oxalic acid is weighed and dissolved in 40ml of deionized water, and then 15.4g of ammonium metavanadate is weighed and stirred uniformly to obtain a clear composite solution 1;
(2) Weighing 3.4g of cerium nitrate, adding 5ml of deionized water for dissolution to obtain a compound clarified solution 2, and uniformly mixing the compound clarified solutions 1 and 2 to obtain a compound clarified solution 3;
(3) Uniformly mixing 40g of titanium dioxide and 0.8g of activated carbon, adding the mixture into the composite clarified solution 3, uniformly stirring, and simultaneously adding 0.4g of lactic acid, 2.8g of boric acid, 0.8g of glass fiber, 3g of silicon dioxide and 3.5g of pseudo-boehmite, uniformly mixing and stirring to obtain uniform bulk slurry;
(4) Extruding and molding the uniform bulk slurry by using a strip extruder to obtain a strip catalyst, and drying the strip catalyst in an oven at 80 ℃ for 6 hours;
(5) And (3) placing the dried bar-shaped catalyst into a muffle furnace for calcining at 270 ℃ for 3 hours to obtain the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst.
Example 2
The embodiment provides a preparation method of a water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst, which comprises the following specific steps:
(1) Weighing 20g of oxalic acid, dissolving in 40ml of deionized water, weighing 19.3g of ammonium metavanadate, and uniformly stirring to obtain a clear composite solution 1;
(2) Weighing 2g of cerium nitrate and 2g of chromium nitrate, adding 6ml of deionized water for dissolution to obtain a compound clarified solution 2, and uniformly mixing the compound clarified solutions 1 and 2 to obtain a compound clarified solution 3;
(3) Uniformly mixing 40g of titanium dioxide and 1g of activated carbon, adding the mixture into the composite clarified solution 3, uniformly stirring, and simultaneously adding 0.7g of lactic acid, 4g of boric acid, 1g of glass fiber, 5g of silicon dioxide and 4g of pseudo-boehmite, uniformly mixing and stirring to obtain uniform bulk slurry;
(4) Extruding and molding the uniform bulk slurry by using a strip extruder to obtain a strip catalyst, and drying the strip catalyst in an oven at 90 ℃ for 4 hours;
(5) And (3) placing the dried bar-shaped catalyst into a muffle furnace for calcining at 270 ℃ for 4 hours to obtain the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst.
Example 3
The embodiment provides a preparation method of a water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst, which comprises the following specific steps:
(1) 18g of oxalic acid is weighed and dissolved in 40ml of deionized water, and then 23g of ammonium metavanadate is weighed and stirred uniformly to obtain a clear composite solution 1;
(2) Weighing 5g of cerium nitrate and 3g of cobalt nitrate, adding 6ml of deionized water for dissolution to obtain a compound clarified solution 2, and uniformly mixing the compound clarified solutions 1 and 2 to obtain a compound clarified solution 3;
(3) Uniformly mixing 40g of titanium dioxide and 2g of activated carbon, adding the mixture into the composite clarified solution 3, uniformly stirring, and simultaneously adding 1.2g of lactic acid, 6g of boric acid, 2g of glass fiber, 6g of silicon dioxide and 4g of pseudo-boehmite, uniformly mixing and stirring to obtain uniform bulk slurry;
(4) Extruding and molding the uniform bulk slurry by using a strip extruder to obtain a strip catalyst, and drying the strip catalyst in an oven at 100 ℃ for 2 hours;
(5) And (3) placing the dried bar-shaped catalyst into a muffle furnace for calcining at 270 ℃ for 5 hours to obtain the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst.
Comparative example 1
(1) 15.4g of ammonium metavanadate is weighed and dissolved in 40ml of deionized water to obtain a clear composite solution 1;
(2) Weighing 3.4g of cerium nitrate, adding 5ml of deionized water for dissolution to obtain a compound clarified solution 2, and uniformly mixing the compound clarified solutions 1 and 2 to obtain a compound clarified solution 3;
(3) Uniformly mixing 40g of titanium dioxide and 0.8g of activated carbon, adding the mixture into the composite clarified solution 3, uniformly stirring, and simultaneously adding 0.4g of lactic acid, 2.8g of boric acid, 0.8g of glass fiber, 3g of silicon dioxide and 3.5g of pseudo-boehmite, uniformly mixing and stirring to obtain uniform bulk slurry;
(4) Extruding and molding the uniform bulk slurry by using a strip extruder to obtain a strip catalyst, and drying the strip catalyst in an oven at 80 ℃ for 6 hours;
(4) And (3) placing the dried bar catalyst into a muffle furnace for calcining at 270 ℃ for 3 hours to obtain the bar catalyst.
Comparative example 2
(1) 12g of oxalic acid is weighed and dissolved in 40ml of deionized water, and then 15.4g of ammonium metavanadate is weighed and stirred uniformly to obtain a clear composite solution 1;
(2) Weighing 4g of niobium oxalate, adding 6ml of deionized water for dissolution to obtain a compound clarified solution 2, and uniformly mixing the compound clarified solutions 1 and 2 to obtain a compound clarified solution 3;
(3) Uniformly mixing 40g of titanium dioxide and 0.8g of activated carbon, adding the mixture into the composite clarified solution 3, uniformly stirring, and simultaneously adding 0.4g of lactic acid, 2.8g of boric acid, 0.8g of glass fiber, 3g of silicon dioxide and 43.5g of pseudo-boehmite, uniformly mixing and stirring to obtain uniform bulk slurry;
(4) Extruding and molding the uniform slurry by using a strip extruder to obtain a strip catalyst, and drying the strip catalyst in an oven at 80 ℃ for 6 hours;
(5) And (3) placing the dried bar catalyst into a muffle furnace for calcining at 270 ℃ for 3 hours to obtain the bar catalyst.
Comparative example 3
(1) 12g of oxalic acid is weighed and dissolved in 40ml of deionized water, and then 15.4g of ammonium metavanadate is weighed and stirred uniformly to obtain a clear composite solution 1;
(2) Weighing 8g of antimony trichloride, adding 6ml of deionized water for dissolution to obtain a compound clarified solution 2, and uniformly mixing the compound clarified solutions 1 and 2 to obtain a compound clarified solution 3;
(3) Uniformly mixing 40g of titanium dioxide and 0.8g of activated carbon, adding the mixture into the composite clarified solution 3, uniformly stirring, and simultaneously adding 0.4g of lactic acid, 2.8g of boric acid, 0.8g of glass fiber, 3g of silicon dioxide and 3.5g of pseudo-boehmite, uniformly mixing and stirring to obtain uniform bulk slurry;
(4) Extruding and molding the uniform bulk slurry by using a strip extruder to obtain a strip catalyst, and drying the strip catalyst in an oven at 80 ℃ for 6 hours;
(5) And (3) placing the dried bar catalyst into a muffle furnace for calcining at 270 ℃ for 3 hours to obtain the bar catalyst.
Example 4
The catalysts of examples 1-3 and comparative examples 1-3 were used at NOx=350 mg/m 3 、SO 2 ＝300mg/m 3 、H 2 O=15%, and the test results are shown in table 1.
TABLE 1
According to the invention, after the vanadium in ammonium metavanadate is converted into crystalline-phase vanadium pentoxide through oxalic acid, one or two substances (cerium nitrate, cobalt nitrate and chromium nitrate as precursors) of cerium oxide, cobalt oxide and chromium oxide are cooperated, so that a low-temperature window is widened, and the catalyst activity in the low-temperature section of 80-130 ℃ can be obviously improved under the synergic action. As can be seen from Table 1, the catalysts of examples 1-3 were exposed to 15% H 2 O and 300mg/m 3 SO 2 The post-catalytic activity has no obvious change in the temperature range of 100-130 ℃, which shows that the synergistic effect of the crystalline phase vanadium pentoxide and one or two substances of cerium oxide, cobalt oxide and chromium oxide has certain water-resistant and sulfur-resistant properties, while the activity of the catalyst of comparative examples 1-3 is obviously attenuated, which shows that the catalyst has no water-resistant and sulfur-resistant properties.
According to the examples, comparative examples and Table 1, the solvent of comparative example 1 does not form a crystalline phase V with oxalic acid 2 O 5 The active component additives of niobium pentoxide (the precursor is niobium oxalate), antimony trichloride (the precursor is antimony trichloride) and the like which also promote the activity of the catalyst are added in comparative examples 2-3 because of having no synergistic effect with the active additive cerium oxide 2 O 5 No obvious synergistic effect, low catalyst activity in the low temperature range of 80-130 deg.c, no water resistance and no sulfur resistance.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. The water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst is characterized by comprising a carrier, an active ingredient, a strength auxiliary agent, a low-temperature and wide-temperature active auxiliary agent and a defoaming agent;
the carrier is titanium dioxide and active carbon mixture;
the active ingredient is V 2 O 5 ；
The strength auxiliary agent is glass fiber, boric acid and silicon dioxide;
the low-temperature and wide-temperature active auxiliary agent is CeO 2 、CoO、Cr 2 O 3 One or two substances of (a) and (b);
the defoaming agent is lactic acid;
the adhesive is pseudo-boehmite.
2. The method for preparing the water-resistant sulfur-resistant ultra-low Wen Tiaozhuang denitration catalyst as claimed in claim 1, which is characterized by comprising the following steps:
(1) Weighing a proper amount of oxalic acid, adding deionized water, stirring, adding ammonium metavanadate, stirring and dissolving to obtain a compound clear solution 1;
(2) Weighing a proper amount of one or two substances of cerium nitrate, cobalt nitrate and chromium nitrate, and adding deionized water for dissolution to obtain a compound clarified solution 2; uniformly mixing the compound clarified solution 1 and the compound clarified solution 2 to obtain a compound clarified solution 3;
(3) Uniformly mixing titanium dioxide and activated carbon powder, adding the mixture into the composite clarified solution 3, uniformly stirring, and simultaneously adding a proper amount of boric acid, glass fiber, silicon dioxide and pseudo-boehmite to obtain uniform bulk slurry;
(4) Extruding and molding the uniform bulk slurry by using a strip extruder to obtain a strip catalyst;
(5) And drying the bar-shaped catalyst, and placing the dried bar-shaped catalyst into a muffle furnace for calcination to obtain the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst.
3. The method for preparing the water-resistant sulfur-tolerant ultra-low Wen Tiaozhuang denitration catalyst according to claim 2, wherein the molar ratio of oxalic acid to ammonium metavanadate in the step (1) is 1:1-3.
4. The method for preparing the water-resistant sulfur-tolerant ultra-low Wen Tiaozhuang denitration catalyst according to claim 2, wherein one or two substances of cerium nitrate, cobalt nitrate and chromium nitrate in the step (2) account for 8-10% of the titanium white.
5. The method for preparing the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst according to claim 2, wherein the mass of the activated carbon powder in the step (3) is 1-5% of the mass of the titanium white powder, the mass of the glass fiber is 2-5% of the mass of the titanium white powder, and the mass of the boric acid and the silicon dioxide is 7-15% of the mass of the titanium white powder.
6. The method for preparing the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst according to claim 2, wherein the lactic acid in the step (3) is 1-3% of the mass of the titanium pigment.
7. The method for preparing the water-resistant sulfur-resistant ultralow Wen Tiaozhuang denitration catalyst according to claim 2, wherein the pseudo-boehmite in the step (3) accounts for 10-20% of the mass of the titanium white powder.
8. The method for preparing the water-resistant sulfur-tolerant ultra-low Wen Tiaozhuang denitration catalyst according to claim 2, wherein in the step (5), the catalyst is dried in an oven at 80-100 ℃ for 2-6 hours.
9. The method for preparing the water-resistant sulfur-tolerant ultra-low Wen Tiaozhuang denitration catalyst according to claim 2, wherein the calcining temperature in the step (5) is 270 ℃ and the time is 3-5h.
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