CN109589967B - High-activity sulfur-resistant SCR denitration catalyst and preparation method thereof - Google Patents
High-activity sulfur-resistant SCR denitration catalyst and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 230000000694 effects Effects 0.000 title claims abstract description 19
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 19
- 239000011593 sulfur Substances 0.000 title claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000005470 impregnation Methods 0.000 claims description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 57
- 239000007788 liquid Substances 0.000 claims description 43
- 238000001035 drying Methods 0.000 claims description 34
- 229910052720 vanadium Inorganic materials 0.000 claims description 31
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 31
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 30
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 30
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 22
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 21
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 21
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 21
- 239000001099 ammonium carbonate Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 21
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 20
- 239000010937 tungsten Substances 0.000 claims description 20
- 229910052721 tungsten Inorganic materials 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 16
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 13
- 239000006229 carbon black Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 12
- 239000003365 glass fiber Substances 0.000 claims description 12
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 12
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 12
- 239000004310 lactic acid Substances 0.000 claims description 11
- 235000014655 lactic acid Nutrition 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims description 9
- 238000004898 kneading Methods 0.000 claims description 8
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 7
- 229920002472 Starch Polymers 0.000 claims description 7
- 239000004917 carbon fiber Substances 0.000 claims description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 7
- 239000008107 starch Substances 0.000 claims description 7
- 235000019698 starch Nutrition 0.000 claims description 7
- 239000002134 carbon nanofiber Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000008929 regeneration Effects 0.000 abstract 1
- 238000011069 regeneration method Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 24
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 22
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 11
- 235000019241 carbon black Nutrition 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910021392 nanocarbon Inorganic materials 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 239000004480 active ingredient Substances 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000003546 flue gas Substances 0.000 description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- -1 polyoxyethylene Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 125000005624 silicic acid group Chemical group 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- ODUCDPQEXGNKDN-UHFFFAOYSA-N Nitrogen oxide(NO) Natural products O=N ODUCDPQEXGNKDN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- HSFQBFMEWSTNOW-UHFFFAOYSA-N sodium;carbanide Chemical group [CH3-].[Na+] HSFQBFMEWSTNOW-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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- 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
- 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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- 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
- B01D53/90—Injecting reactants
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- 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
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
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Abstract
The invention discloses a high-activity sulfur-resistant SCR denitration catalyst, which comprises a carrier and active components, wherein the raw materials of the carrier comprise titanium dioxide, a pore-enlarging agent, a binder, a dispersing agent and a reinforcing agent; the active component is V 2 O 5 And WO 3 Said active component V 2 O 5 、WO 3 And the mass ratio of the carrier is 0.05-0.5: 3-10: 100. the invention also discloses a preparation method of the high-activity sulfur-resistant SCR denitration catalyst. Compared with the prior art, the high-activity sulfur-resistant SCR denitration catalyst provided by the invention has an active component V 2 O 5 Low content, high denitration efficiency and SO 2 /SO 3 Low conversion rate, low preparation cost, high mechanical strength, easy regeneration and the like.
Description
Technical Field
The invention belongs to the field of air pollution treatment, and particularly relates to a high-activity sulfur-resistant SCR denitration catalyst and a preparation method thereof.
Background
Coal-fired power generation is mainly used in the internal structure of thermal power generation in China, and Nitrogen Oxide (NO) is released by the coal-fired power generation x ) And NO discharged to the atmosphere x Is one of the main sources of pollution causing atmospheric acid rain, photochemical smog and the like, so that the environmental protection department of China requires the thermal power plant to strictly control NO x The amount of discharge of (c). At present, more than 90 percent of coal-fired power plants at home and abroad adopt a Selective Catalytic Reduction (SCR) technology to remove NO in tail flue gas of the power plants x . The core of the SCR technology is a denitration catalyst, and the commercial catalyst most applied in engineering is a vanadium-titanium catalyst.
For example, chinese patent document CN105597730A discloses a vanadium-titanium based catalyst. The catalyst is mainly obtained by molding catalyst powder and molding auxiliary agent, wherein the catalyst powder takes anatase titanium dioxide as a carrier, and V is 2 O 5 As an active ingredient, WO 3 The active assistant is a mixture of a reinforcing agent, an inorganic binder, an organic binder, a pore-forming agent and a lubricant. The vanadium-titanium catalyst has a certain improvement in denitration efficiency.
In the operation process of the SCR denitration system, due to the fact that a part of ammonia escapes, when escaped ammonia meets SO 3 The ammonia sulfate is generated, the ammonia sulfate forms liquid Ammonium Bisulfate (ABS) in a certain temperature range, and the ABS has strong adhesion, so that dust in the flue gas is easily adhered to the air preheater, the air preheater is blocked, the problems of dust blockage, surge, stall and the like are caused, and the safe operation of the denitration unit is seriously influenced; meanwhile, ABS has strong corrosivity, can corrode low-carbon steel and low-alloy steel in the air preheater, causes damage to the air preheater in different degrees, and brings hidden danger to unit operation.
At present, the problems of insufficient sulfur resistance, easy blockage, high preparation cost, poor product stability and the like of the SCR denitration catalyst generally exist. How to reduce the preparation cost of the catalyst and obviously reduce the SO thereof on the premise of ensuring the catalytic efficiency 2 /SO 3 Thereby preventing ABS production and preventing air preheater blockage and corrosion, which is a technical problem to be solved urgently in the field.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the SCR catalyst SO in the prior art 2 /SO 3 High conversion rate, easy blockage and corrosion of an air preheater, high preparation cost of the catalyst and the like, thereby providing the sulfur-resistant SCR denitration catalyst with high denitration activity and the preparation method thereof.
Therefore, the invention provides a high-activity sulfur-resistant SCR denitration catalyst, which comprises a carrier and an active component loaded on the carrier, wherein the carrier comprises titanium dioxide and a pore-enlarging agent, and the mass ratio of the pore-enlarging agent to the titanium dioxide is (5-10): 300-450, preferably 6-8: 300-450, wherein the pore-enlarging agent is one or more of nano carbon black, water-soluble starch (industrial grade), nano carbon fiber and ammonium bicarbonate.
Further, the pore-expanding agent is nano carbon black and ammonium bicarbonate, or water-soluble starch and ammonium bicarbonate, or nano carbon fiber and ammonium bicarbonate.
Further, the pore-expanding agent is nano-scale carbon black and ammonium bicarbonate, and the mass ratio of the nano-scale carbon black to the ammonium bicarbonate is (2-10): 0.05 to 1, preferably 2 to 5: 0.1-0.6, more preferably 3: 0.5.
further, the nano-scale carbon black has a particle size of 5 to 20nm and a spherical or elliptical particle shape.
Further, the nano-scale carbon fiber has a particle length of 10-50nm and a fibrous particle shape.
Further, the active component is V 2 O 5 And WO 3 Said active component V 2 O 5 、WO 3 And the mass ratio of the carrier is 0.05-0.5: 3-10: 100, more preferably 0.05 to 0.1: 3-10: 100.
further, the V is first loaded on the carrier 2 O 5 And then supported thereon with WO 3 。
Further, the carrier also comprises a binder, a dispersing agent and a reinforcing agent, wherein the mass ratio of the binder to the dispersing agent to the reinforcing agent to the titanium dioxide is 3-13: 10-50: 20-50: 300-450, preferably 4-10: 20-45: 30-50: 300-450.
Further, the binder is one or more of polyethylene oxide and sodium carboxymethyl cellulose (CMC).
Furthermore, the adhesive is prepared from 2-8: 1-5 of a mixture of polyethylene oxide and sodium carboxymethylcellulose.
Further, the dispersant is ammonia water;
further, the reinforcing agent is one or more of silicic acid and glass fiber.
Further, the reinforcing agent is silicic acid and glass fiber.
Furthermore, the reinforcing agent is silicic acid and glass fiber, and the mass ratio of the silicic acid to the glass fiber is 1-2: 5-20.
On the other hand, the invention also provides a preparation method of the high-activity sulfur-resistant SCR denitration catalyst, which comprises the following steps:
(a) carrying out first impregnation on the carrier in a vanadium source impregnation liquid, and drying after the first impregnation to obtain a vanadium source impregnated carrier;
(b) secondly, carrying out second impregnation on the vanadium source-impregnated carrier in a tungsten source impregnation liquid;
(c) and drying and roasting the carrier subjected to the second impregnation in sequence to obtain the SCR denitration catalyst.
Further, the first impregnation and the second impregnation are equal-volume impregnation.
Further, the preparation method of the vanadium source impregnation liquid comprises the following steps: adding ammonium metavanadate (NH) to water 4 VO 3 ) And ammonia water, wherein the mass ratio of the ammonium metavanadate to the ammonia water to the water is 5-10: 5-10: 250-400, wherein the concentration of the ammonia water is 25-28 wt%; then stirring for 1-3h at 50-80 ℃.
Further, the preparation method of the tungsten source impregnation liquid comprises the following steps: adding ammonium metatungstate (H) to water 28 N 6 O 41 W 12 ) Said offsetThe mass ratio of ammonium tungstate to water is 20-50: 150-200; then, stirring for 1-3h at 50-80 ℃.
Further, the drying temperature is 100-120 ℃, and the drying time is 6-24 h.
Further, the roasting temperature is 500-550 ℃, and the time is 4-6 h.
Further, the preparation method of the carrier comprises the following steps:
(1) carrying out first mixing on the titanium dioxide, the pore-expanding agent and the binder to obtain a mixture;
(2) adding water, a dispersing agent, a reinforcing agent and lactic acid into the mixture for first mixing to obtain a wet material;
(3) and kneading, extruding, drying and roasting the wet material in sequence to obtain the carrier.
Further, the stirring speed of the first mixing is 1000-1500r/min, and the time is 2-10 min.
Further, in the step (2), water, dispersant and lactic acid are added into the mixture, stirred for 10-15min at the rotation speed of 1000-1500r/min, then the reinforcing agent is added into the mixture, and stirred for 10-15min at the rotation speed of 1000-1500 r/min.
Further, in the step (2), the mass ratio of the water, the dispersant, the lactic acid and the reinforcing agent is 100-150: 10-30: 1-10: 20-50.
Further, the water in the step (2) is deionized water.
Further, in the step (3), the rotation speed of the kneading is 300-500r/min, and the time is 2-3 h.
Further, in the step (3), the extrusion pressure is 4-6 Mpa.
Further, in the step (4), the drying temperature is 70-85 ℃ and the drying time is 12-14 h.
Further, in the step (4), the roasting temperature is 500-600 ℃ and the roasting time is 22-26 h.
The active component of the SCR catalyst which has an oxidizing effect is V 2 O 5 Decrease V 2 O 5 Can be effectively reducedLow SO 2 /SO 3 Thereby effectively preventing ABS production and preventing air preheater blockage and corrosion. The invention can effectively reduce the active component V of the catalyst under the condition of maintaining high catalytic activity by improving the pore structure of the SCR catalyst 2 O 5 Thereby effectively reducing SO 2 /SO 3 The catalyst provided by the invention has good hydrothermal stability and high mechanical strength.
Specifically, the technical scheme of the invention has the following advantages:
1. the invention provides a high-activity sulfur-resistant SCR denitration catalyst, which takes titanium dioxide as the main component of a carrier, and is added with at least one of nano-scale carbon black, water-soluble starch, nano-carbon fiber and ammonium bicarbonate in a specific proportion as a pore-enlarging agent, so that the pore structure of the catalyst is effectively improved, the specific surface area is increased, the pore volume of the catalyst is improved, and the high-activity sulfur-resistant SCR denitration catalyst is beneficial to an active component V 2 O 5 The catalyst has excellent denitration efficiency by exposing more catalytic active sites.
2. The invention provides a preparation method of a high-activity sulfur-resistant SCR denitration catalyst, which specifically adopts a step impregnation method, and the current commercial SCR denitration catalyst is mostly prepared by a kneading method, wherein the kneading method ensures that most catalytic active sites are positioned in a catalyst body, and have an agglomeration phenomenon and can not be exposed on the surface of the catalyst to participate in chemical reaction; the SCR denitration catalyst prepared by the step impregnation method has more uniform active sites and is easier to expose on the surface of the catalyst, and the active component V is reduced 2 O 5 The dosage of the catalyst can still maintain higher catalytic activity of the catalyst, and the preparation cost of the catalyst is saved.
3. The preparation method of the high-activity sulfur-resistant SCR denitration catalyst provided by the invention enables active ingredients to be uniformly dispersed on the surface of the catalyst, has high reaction activity, and can effectively reduce the active ingredient V 2 O 5 The amount of (c); the flue gas often contains a large amount of SO 2 Vanadium can catalyze SO 2 Oxidation to produce SO 3 ，SO 3 And NH 3 The reaction produces Ammonium Bisulfate (ABS), which is easy to deposit on the surface of the catalystThe catalyst obtained by applying the preparation method provided by the invention has the advantages of reduced vanadium content and effectively reduced SO 2 Oxidized probability, excellent SO resistance 2 Poisoning performance, effectively preventing the problems of ash blockage, corrosion and the like of the air preheater caused by ABS.
4. The invention provides a high-activity sulfur-resistant SCR denitration catalyst which is prepared by adopting a specific pore-expanding agent, a binder, a dispersant and a reinforcing agent and optimizing the dosage proportion of each raw material. It is well known in the art that physical pore expansion tends to cause a reduction in the mechanical strength of the support, which would make the mechanical strength of the catalyst made therefrom undesirable for industrial use. The pore-enlarging agent, the binder, the lubricant and the reinforcing agent in specific proportions are selected, so that the pore structure of the catalyst is improved, and the catalyst has the advantages of good hydrothermal stability, high mechanical strength and long service life.
Drawings
Figure 1 is an XRD pattern of the catalyst prepared in example 1 of the present invention.
Detailed Description
The following examples are provided to better understand the present invention, not to limit the best mode, and not to limit the content and protection scope of the present invention, and any product that is the same or similar to the present invention and is obtained by combining the present invention with other features of the prior art and the present invention falls within the protection scope of the present invention.
The examples do not indicate specific experimental procedures or conditions, and can be performed according to the procedures or conditions of the conventional experimental procedures described in the literature in the field. The reagents or instruments used are conventional reagent products which are commercially available, and manufacturers are not indicated. The nano-sized carbon blacks used in the following examples and comparative examples have a diameter of 5 to 20mn and are spherical or elliptical particles in shape; the length of the nano-scale carbon fiber is 10-50nm, and the nano-scale carbon fiber is fibrous; the concentration of the ammonia water is 25wt% -28 wt%.
Example 1
The embodiment provides an SCR denitration catalyst, and the preparation method thereof is as follows:
(one) preparation of the support
(1) Adding titanium dioxide, nano carbon black, ammonium bicarbonate, polyethylene oxide and sodium methyl cellulose (CMC) into a mixer, and mixing at the rotating speed of 1200r/min for 5min to obtain a material 1; wherein the mass ratio of titanium dioxide, nano carbon black, ammonium bicarbonate, polyoxyethylene and sodium carboxymethylcellulose is 420: 5: 1: 5: 2;
(2) sequentially adding ionized water, ammonia water and lactic acid into the material 1, keeping the rotating speed unchanged, stirring for 10min, adding glass fiber, and continuously stirring for 15min to obtain a material 2; wherein the ammonia water is an aqueous solution containing 25-28% of ammonia, and the mass ratio of the deionized water to the ammonia water to the lactic acid to the glass fiber to the silicic acid is 120: 25: 30: 45: 5;
(3) and kneading the material 2 at the rotation speed of 400r/min for 2h, and extruding at the extrusion pressure of 4MPa to obtain the honeycomb carrier precursor.
(4) Drying the honeycomb carrier precursor at 80 ℃ for 12h, and then roasting at 550 ℃ for 24h to obtain the carrier of the SCR denitration catalyst.
(II) impregnation of active ingredient
(1) Determination of water absorption of the SCR catalyst support:
weighing 200g of carrier, drying in an oven at 120 ℃ for 2h, weighing, then placing the carrier into a watch glass, slowly dripping distilled water until the carrier does not absorb water any more, slightly absorbing excessive water on the surface of the carrier by using filter paper, weighing again, and calculating the water absorption rate of the carrier.
(2) Preparing an immersion liquid:
mixing ammonium metavanadate (NH) 4 VO 3 ) Adding ammonia water and deionized water, slowly heating the mixed aqueous solution to 65 ℃ by magnetic stirring, and stirring for 2 hours to obtain vanadium source impregnation liquid; wherein the mass ratio of ammonium metavanadate to ammonia water to deionized water is 8: 6: 300.
ammonium metatungstate (H) 28 N 6 O 41 W 12 ) Adding into deionized water, magnetically stirring the mixed aqueous solution, slowly heating to 65 ℃, and stirring for 2h to obtain tungsten source impregnation liquid(ii) a Wherein the mass ratio of ammonium metatungstate to distilled water is 25: 180.
(3) secondary isometric impregnation:
respectively measuring vanadium source impregnation liquid and tungsten source impregnation liquid according to the water absorption rate of a carrier, fully and uniformly mixing the prepared vanadium source impregnation liquid with the carrier while the vanadium source impregnation liquid is hot, standing for 1h, then putting the obtained mixture into a 120 ℃ drying oven for drying for 8h, taking out the carrier, then fully and uniformly mixing the prepared tungsten source impregnation liquid with the obtained mixture, standing for 1h, then putting the obtained product into the 120 ℃ drying oven for drying for 8h, and finally roasting the obtained product in a 550 ℃ muffle furnace for 4h in an air environment to obtain the SCR denitration catalyst.
Example 2
The embodiment provides an SCR denitration catalyst, and the preparation method thereof is as follows:
(one) preparation of the support
(1) Adding titanium dioxide, water-soluble starch, ammonium bicarbonate, polyethylene oxide and sodium carboxymethylcellulose (CMC) into a mixer, and mixing at a rotating speed of 1500r/min for 4min to obtain a material 1; wherein the mass ratio of titanium dioxide, water-soluble starch, ammonium bicarbonate, polyethylene oxide and sodium carboxymethyl cellulose is 420: 5: 1: 5: 2;
(2) sequentially adding ionized water, ammonia water and lactic acid into the material 1, keeping the rotating speed unchanged, stirring for 12min, adding glass fiber, and continuously stirring for 12min to obtain a material 2; wherein the ammonia water is an aqueous solution containing 25-28% of ammonia, and the mass ratio of the deionized water to the ammonia water to the lactic acid to the glass fiber to the silicic acid is 120: 30: 25: 40: 5;
(3) and kneading the material 2 at the rotation speed of 350r/min for 2.5h, and extruding at the extrusion pressure of 5MPa to obtain the honeycomb carrier precursor.
(4) Drying the honeycomb carrier precursor at 80 ℃ for 12h, and then roasting at 500 ℃ for 25h to obtain the carrier of the SCR denitration catalyst.
(II) impregnation of active ingredient
(1) Determination of water absorption of the SCR catalyst support:
weighing 200g of carrier, drying in an oven at 120 ℃ for 2h, weighing, then putting into a watch glass, slowly dripping distilled water until the carrier does not absorb water any more, slightly absorbing the excessive water on the surface of the carrier by using filter paper, weighing again, and calculating the water absorption rate of the carrier.
(2) Preparing an immersion liquid:
mixing ammonium metavanadate (NH) 4 VO 3 ) Adding ammonia water and deionized water, slowly heating the mixed aqueous solution to 70 ℃ by magnetic stirring, and stirring for 2 hours to obtain vanadium source impregnation liquid; wherein the mass ratio of ammonium metavanadate to ammonia water to deionized water is 10: 7: 300.
ammonium metatungstate (H) 28 N 6 O 41 W 12 ) Adding the mixture into deionized water, slowly heating the mixed aqueous solution to 70 ℃ by magnetic stirring, and stirring for 2 hours to obtain a tungsten source impregnation solution; wherein the mass ratio of ammonium metatungstate to distilled water is 30: 180.
(3) secondary isometric impregnation:
respectively measuring vanadium source impregnation liquid and tungsten source impregnation liquid according to the water absorption rate of a carrier, fully and uniformly mixing the prepared vanadium source impregnation liquid and the carrier while the vanadium source impregnation liquid is hot, standing for 1h, then putting the mixture into a 120 ℃ drying oven for drying for 10h, taking out the carrier, then fully and uniformly mixing the prepared tungsten source impregnation liquid and the carrier, standing for 1h, then putting the mixture into the 120 ℃ drying oven for drying for 8h, and finally roasting in a 500 ℃ muffle furnace for 5h in an air environment to obtain the SCR denitration catalyst.
Example 3
The embodiment provides an SCR denitration catalyst, and the preparation method thereof is as follows:
(one) preparation of the support
(1) Adding titanium dioxide, carbon nanofibers, ammonium bicarbonate, polyethylene oxide and sodium carboxymethylcellulose (CMC) into a mixer, and mixing at the rotating speed of 1000r/min for 10min to obtain a material 1; wherein the mass ratio of titanium dioxide, carbon nanofibers, ammonium bicarbonate, polyethylene oxide and sodium carboxymethylcellulose is 420: 6: 1: 5: 2;
(2) sequentially adding ionized water, ammonia water and lactic acid into the material 1, keeping the rotating speed unchanged, stirring for 8min, adding glass fiber, and continuously stirring for 10min to obtain a material 2; wherein the ammonia water is an aqueous solution containing 25-28% of ammonia, and the mass ratio of the deionized water to the ammonia water to the lactic acid to the glass fiber to the silicic acid is 100: 20: 30: 25: 3;
(3) and kneading the material 2 at the rotation speed of 550r/min for 2h, extruding the kneaded material at the extrusion pressure of 6MPa to obtain the honeycomb carrier precursor.
(4) Drying the honeycomb carrier precursor at 70 ℃ for 14h, and then roasting at 600 ℃ for 22h to obtain the carrier of the SCR denitration catalyst.
(II) impregnation of active ingredient
(1) Determination of water absorption of the SCR catalyst support:
weighing 200g of carrier, drying in an oven at 120 ℃ for 2h, weighing, then putting into a watch glass, slowly dripping distilled water until the carrier does not absorb water any more, slightly absorbing the excessive water on the surface of the carrier by using filter paper, weighing again, and calculating the water absorption rate of the carrier.
(2) Preparing an immersion liquid:
ammonium metavanadate (NH) 4 VO 3 ) Adding ammonia water and deionized water, slowly heating the mixed aqueous solution to 70 ℃ by magnetic stirring, and stirring for 2 hours to obtain vanadium source impregnation liquid; wherein the mass ratio of ammonium metavanadate to ammonia water to deionized water is 6: 5: 300.
ammonium metatungstate (H) 28 N 6 O 41 W 12 ) Adding the mixture into deionized water, slowly heating the mixed aqueous solution to 70 ℃ by magnetic stirring, and stirring for 2 hours to obtain a tungsten source impregnation solution; wherein the mass ratio of ammonium metatungstate to distilled water is 50: 180.
(3) secondary isometric impregnation:
respectively measuring vanadium source impregnation liquid and tungsten source impregnation liquid according to the water absorption rate of a carrier, fully and uniformly mixing the prepared vanadium source impregnation liquid with the carrier while the vanadium source impregnation liquid is hot, standing for 1h, then putting the vanadium source impregnation liquid into a 100 ℃ drying oven for drying for 16h, taking out the carrier, then fully and uniformly mixing the prepared tungsten source impregnation liquid with the tungsten source impregnation liquid, standing for 1h, then putting the tungsten source impregnation liquid into the 100 ℃ drying oven for drying for 10h, and finally roasting in a 500 ℃ muffle furnace for 6h in an air environment to obtain the SCR denitration catalyst.
Example 4
The preparation method of the catalyst provided by the embodiment is that the mass ratio of titanium dioxide, nano-scale carbon black, ammonium bicarbonate, polyethylene oxide and sodium carboxymethylcellulose is 420: 6: 1: 5: except for 2, the same procedure was repeated as in example 3.
Comparative example 1
The catalyst provided by the comparative example was prepared according to the preparation method disclosed in example 3 of patent CN 105597730A.
Comparative example 2
The preparation method of the catalyst provided by the comparative example uses activated carbon as a pore-enlarging agent, wherein the activated carbon is activated carbon particles with the particle size of less than 200 meshes, and the mass ratio of the titanium dioxide to the activated carbon to the polyethylene oxide to the sodium carboxymethylcellulose is 420: 6: 5: except for 2, the same procedure was repeated as in example 1.
Comparative example 3
In the step of preparing the carrier, the mass ratio of titanium dioxide, nano carbon black, ammonium bicarbonate, polyoxyethylene and sodium carboxymethylcellulose is 420: 2.5: 2: 10: 5, deionized water, ammonia water, lactic acid, glass fiber and silicic acid in a mass ratio of 120: 15: 30: 45: the procedure of example 1 was repeated except for the fact that.
Comparative example 4
The preparation method of the catalyst is the same as the example 1 except that the configuration and the impregnation method of the vanadium source impregnation liquid are different from those of the example 1, and the configuration method of the vanadium source impregnation liquid of the comparative example is as follows:
mixing ammonium metavanadate (NH) 4 VO 3 ) Adding ammonia water and deionized water, slowly heating the mixed aqueous solution to 65 ℃ by magnetic stirring, and stirring for 2 hours to obtain vanadium source impregnation liquid; wherein the mass ratio of ammonium metavanadate to ammonia water to deionized water is 16: 3: 300.
the impregnation method of this comparative example was:
fully and uniformly mixing the prepared tungsten source impregnation liquid and the carrier, standing for 1h, then putting the mixture into a 140 ℃ drying oven for drying for 12h, taking out the carrier, fully and uniformly mixing the prepared vanadium source impregnation liquid and the carrier, standing for 1h, then putting the mixture into the 140 ℃ drying oven for drying for 8h, and finally roasting in a 500 ℃ muffle furnace for 8h in an air environment to obtain the SCR denitration catalyst.
Experimental example 1
Physical property analysis was performed on the catalysts of examples 1 to 4 and comparative examples 1 to 4, and the X-Ray diffraction (XRD) pattern of example 1 is shown in fig. 1, and the results of X-Ray Fluorescence spectrum (XRF) analysis of example 1 and comparative example 1 are shown in table 1, and the results of examples 1 to 4 and comparative examples 1 to 4 and texture properties are shown in table 2.
Table 1 XRF test results (unit:%)
| Main component | TiO 2 | SiO 2 | V 2 O 5 | WO 3 |
| Example 1 | 85.62 | 9.01 | 0.46 | 4.63 |
| Comparative example 1 | 86.78 | 3.18 | 1.22 | 4.98 |
TABLE 2 texture Properties of SCR catalysts
| Number of | Specific surface area (m) 2 /g) | Average pore diameter (nm) | Total pore volume (cm) 3 /g) |
| Example 1 | 58.98 | 18.64 | 0.32 |
| Example 2 | 57.68 | 18.47 | 0.29 |
| Example 3 | 58.12 | 18.32 | 0.31 |
| Example 4 | 59.10 | 18.76 | 0.33 |
| Comparative example 1 | 54.91 | 9.30 | 0.24 |
| Comparative example 2 | 55.58 | 15.36 | 0.26 |
| Comparative example 3 | 56.68 | 17.44 | 0.28 |
| Comparative example 4 | 57.87 | 18.62 | 0.29 |
Experimental example 2
The SCR denitration catalysts of examples 1 to 4 and comparative examples 1 to 4 were subjected to a performance test on a fixed bed reactor, and the denitration efficiency is shown in table 3.
TABLE 3 denitration efficiency of SCR denitration catalyst (unit:%)
| Catalyst numbering | Denitration efficiency |
| Example 1 | 96.5 |
| Example 2 | 95.7 |
| Example 3 | 95.3 |
| Example 4 | 96.1 |
| Comparative example 1 | 88.4 |
| Comparative example 2 | 90.6 |
| Comparative example 3 | 91.0 |
| Comparative example 4 | 94.5 |
And (3) testing conditions are as follows: the flue gas temperature is 400 ℃, the airspeed is 10000/h, and NH is 3 /NO x ＝1，5vol％O 2 ，16vol％H 2 O，NO x (dry basis) 400mg/m 3 ，SO 2 (dry basis) 1550mg/m 3 。
Experimental example 3
Performance tests were performed on the SCR denitration catalysts of examples 1 to 4 and comparative examples 1 to 4, SO 2 /SO 3 The conversion is shown in Table 4.
TABLE 4 SO 2 /SO 3 Results of conversion test
And (3) testing conditions are as follows: the flue gas temperature is 400 ℃, the airspeed is 10000/h, and NH 3 /NO x ＝1，5vol％O 2 ，16vol％H 2 O，NO x (dry basis) 400mg/m 3 ，SO 2 (dry basis) 1550mg/m 3 。
Experimental example 4
The SCR denitration catalysts of examples 1 to 4 and comparative examples 1 to 4 were subjected to a compressive strength test using a universal material testing machine (HF-9006, jiangsu high detection equipment limited), and the test results are shown in table 6.
TABLE 6 compressive strength of SCR denitration catalyst
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (5)
1. The high-activity sulfur-resistant SCR denitration catalyst is characterized by comprising a carrier and active components loaded on the carrier, wherein the preparation raw materials of the carrier comprise titanium dioxide, a pore-enlarging agent, a binder, a dispersing agent and a reinforcing agent, and the mass ratio of the pore-enlarging agent to the titanium dioxide is (5-10): 300-450, wherein the mass ratio of the binder, the dispersant, the reinforcing agent and the titanium dioxide is 3-13: 10-50: 20-50: 300-450;
the pore-expanding agent is nano-scale carbon black and ammonium bicarbonate, or water-soluble starch and ammonium bicarbonate, or nano-scale carbon fiber and ammonium bicarbonate;
the active component is V 2 O 5 And WO 3 Said active component V 2 O 5 、WO 3 And the mass ratio of the carrier is 0.05-0.5: 3-10: 100, respectively;
the mass ratio of the nano-scale carbon black to the ammonium bicarbonate is 2-10: 0.05 to 1; the mass ratio of the water-soluble starch to the ammonium bicarbonate is 5: 1; the mass ratio of the carbon nanofibers to the ammonium bicarbonate is 6: 1;
the preparation method of the SCR denitration catalyst comprises the following steps:
(a) carrying out first impregnation on the carrier in a vanadium source impregnation liquid, and drying after the first impregnation to obtain a vanadium source impregnated carrier;
(b) secondly, carrying out second impregnation on the vanadium source-impregnated carrier in a tungsten source impregnation liquid;
(c) drying and roasting the second impregnated carrier in sequence to obtain the SCR denitration catalyst;
the preparation method of the vanadium source impregnation liquid comprises the following steps: adding ammonium metavanadate and ammonia water into water, wherein the mass ratio of the ammonium metavanadate to the ammonia water to the water is (5-10): 5-10: 250-400, wherein the concentration of the ammonia water is 25-28 wt%; then stirring for 1-3h at 50-80 ℃;
the preparation method of the tungsten source impregnation liquid comprises the following steps: adding ammonium metatungstate into water, wherein the mass ratio of ammonium metavanadate to tungsten to water is 20-50: 150-200; then, stirring is carried out for 1-3h at 50-80 ℃.
2. The high-activity sulfur-resistant SCR denitration catalyst according to claim 1, wherein the binder is one or more of polyethylene oxide and sodium carboxymethylcellulose; the dispersant is ammonia water;
the reinforcing agent is one or more of glass fiber and silicic acid.
3. The high-activity sulfur-resistant SCR denitration catalyst according to claim 2, wherein the binder is a mixture of 2 to 8: 1-5 of a mixture of polyethylene oxide and sodium carboxymethylcellulose.
4. A method for preparing the high-activity sulfur-resistant SCR denitration catalyst according to any one of claims 1 to 3, comprising the steps of:
(a) carrying out first impregnation on the carrier in a vanadium source impregnation liquid, and drying after the first impregnation to obtain a vanadium source impregnated carrier;
(b) secondly, carrying out second impregnation on the vanadium source-impregnated carrier in a tungsten source impregnation liquid;
(c) drying and roasting the second impregnated carrier in sequence to obtain the SCR denitration catalyst;
the preparation method of the vanadium source impregnation liquid comprises the following steps: adding ammonium metavanadate and ammonia water into water, wherein the mass ratio of the ammonium metavanadate to the ammonia water to the water is 5-10: 5-10: 250-400, wherein the concentration of the ammonia water is 25-28 wt%; then stirring for 1-3h at 50-80 ℃;
the preparation method of the tungsten source impregnation liquid comprises the following steps: adding ammonium metatungstate into water, wherein the mass ratio of ammonium metavanadate to tungsten to water is 20-50: 150-200; then, stirring for 1-3h at 50-80 ℃.
5. The method according to claim 4, wherein the method for preparing the carrier comprises the steps of:
(1) carrying out first mixing on the titanium dioxide, the pore-expanding agent and the binder to obtain a mixture;
(2) adding water, a dispersing agent, a reinforcing agent and lactic acid into the mixture for first mixing to obtain a wet material;
(3) and kneading, extruding, drying and roasting the wet material in sequence to obtain the carrier.
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