CN109529808A - A kind of preparation method improving charcoal base SCR catalyst low temperature active - Google Patents
A kind of preparation method improving charcoal base SCR catalyst low temperature active Download PDFInfo
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- CN109529808A CN109529808A CN201811436186.XA CN201811436186A CN109529808A CN 109529808 A CN109529808 A CN 109529808A CN 201811436186 A CN201811436186 A CN 201811436186A CN 109529808 A CN109529808 A CN 109529808A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000003610 charcoal Substances 0.000 title claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012298 atmosphere Substances 0.000 claims abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 9
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000007598 dipping method Methods 0.000 claims abstract description 4
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 244000060011 Cocos nucifera Species 0.000 claims description 2
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 2
- 229910021552 Vanadium(IV) chloride Inorganic materials 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- -1 carbo lignius Substances 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- JTJFQBNJBPPZRI-UHFFFAOYSA-J vanadium tetrachloride Chemical compound Cl[V](Cl)(Cl)Cl JTJFQBNJBPPZRI-UHFFFAOYSA-J 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- OGUCKKLSDGRKSH-UHFFFAOYSA-N oxalic acid oxovanadium Chemical compound [V].[O].C(C(=O)O)(=O)O OGUCKKLSDGRKSH-UHFFFAOYSA-N 0.000 claims 1
- 230000009257 reactivity Effects 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 239000006185 dispersion Substances 0.000 abstract description 3
- 238000010306 acid treatment Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000004220 aggregation Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- 238000003756 stirring Methods 0.000 description 11
- 238000004090 dissolution Methods 0.000 description 10
- 229910003206 NH4VO3 Inorganic materials 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 5
- 230000002045 lasting effect Effects 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 description 1
- 241001466460 Alveolata Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- YXPXHSOOUSXDST-UHFFFAOYSA-N [O].OC(=O)C(O)=O Chemical compound [O].OC(=O)C(O)=O YXPXHSOOUSXDST-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000002803 maceration Methods 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 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
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/20—Reductants
- B01D2251/206—Ammonium compounds
- B01D2251/2062—Ammonia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
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- B01D2258/0283—Flue gases
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Abstract
A kind of preparation method improving charcoal base SCR catalyst low temperature active, belongs to denitrating catalyst preparation technical field.With V2O5For active component, active carbon is as carrier.It weighs active carbon to be handled with nitric acid oxidation, subsequent filtration washing drying.Dissolving oxalic acid is weighed in deionized water, vanadium presoma is added after to be dissolved, the active carbon that nitric acid treatment is crossed is added after becoming blue in solution.Obtained mixture is stirred under different capacity to dipping in microwave cavity, obtains V after then roasting under different atmosphere2O5/ AC catalyst.Process of the present invention is simple, and strong operability, reaction condition is mild, and required time is short.The active component in catalyst carrier is regulated and controled by conditions such as the processing power of microwave and dip times, the V after microwave treatment2O5V on/AC catalyst2O5Species dispersion is more uniform, reduces the aggregation of particle, provides more active sites, improves the denitration performance of catalyst.
Description
Technical field
The present invention relates to a kind of active preparation methods of raising low-temperature SCR catalyst, belong to field of catalyst preparation.
Background technique
As the rapid development of sociaty and economy, high-intensitive energy consumption consequent is serious atmosphere pollution,
Middle nitrogen oxides (NOx) it is one of main atmosphere pollution, and it is broken to also result in acid rain, photochemical fog, ozone layer
The a series of environmental problem such as bad.SCR technology (SCR) is to be most widely used at present and the most efficient
Remove NOxTechnology, wherein catalyst is the core of denitration technology.Present denitrating catalyst is typically placed in cleaner and takes off
After sulphur device, the temperature by the flue gas of denitrating catalyst is relatively low, is avoiding device transformation and reheating, therefore need to develop low temperature
Denitrating catalyst.Low-temperature denitration catalyst research at present is more, such as Mn base, Ce base catalyst etc., such good catalyst activity but
Water resistant sulfur resistance is to be improved.V2O5For NH3- SCR reaction has preferable catalytic performance, therefore studies with more excellent
The catalytic component based on vanadium of low temperature active is particularly important.
A kind of material that carbon material is widely present as nature, have large specific surface area, chemical stability be good, structure can
The advantages that regulation and surface may modify is widely used in low-temperature selective catalytic reduction reaction.Carbon material is because having biggish ratio
Surface area is often used as catalyst carrier and active component, effectively active component can be made to be dispersed in carrier surface, to mention
High NH3- SCR catalytic activity.Active carbon is widely used in SO in coal-fired flue-gas as adsorbent2And NOxRemoving.Patent
CN 102513095A discloses a kind of preparation method of the medium temperature denitrating catalyst of carbon based material cerium-carrying tungsten, this catalyst exists
In 250-400 DEG C, denitration efficiency is stablized 90% or more.Patent CN 102078753A discloses a kind of Alveolate activated carbon base
The preparation and application method of denitrating catalyst, using the mixed solution of manganese nitrate or manganese acetate and cerous nitrate as maceration extract, using etc.
Volume impregnation prepares honeycombed catalyst, and the denitration with higher in 80-200 DEG C of wider temperature range of this catalyst is living
Property.
Microwave because selective heating, capacity usage ratio is high, the reaction time is short etc. unique performance is concerned by people and
Using." the body heating " of microwave can promptly heating material, effectively reduce the aggregation of particle.In recent years, microwave irradiation
It is widely used in chemical field to synthesize inorganic or organic material and used also as the heating source of catalysis reaction.Patent CN
102489107A discloses a kind of preparation method of microwave intermitant irradiation active carbon desulfurization denitration, and the method effectively realizes activity
The regeneration of the charcoal and rate of recovery is high.The V of load on the activated carbon2O5With preferable low temperature active and good sulfur resistance.Due to
Active carbon has stronger absorption microwave ability, and can quickly absorb microwave makes carrier thermally equivalent, and active component is promoted to carry
Further dispersion on body.Therefore, microwave is introduced into infusion process preparation V by the present invention2O5In the method of/AC catalyst, by changing
Preparation method into catalyst further increases V2O5The low temperature active of/AC denitrating catalyst.
Summary of the invention
The present invention is by utilizing microwave irradiation V2O5/ AC catalyst system is had by simple preparation method
Excellent low temperature NH3The V of-SCR reactivity2O5/ AC catalyst.Raw material required for catalyst preparation is cheap and easy to get, technique letter
It is single, there is potential application prospect in industrial smoke denitration field.
The purpose of the present invention is introducing microwave radiation in the method by preparation catalyst, it is de- low temperature has been obtained
The high V of nitre activity2O5/ AC low-temperature SCR catalyst, to reduce the loss of catalyst.
To achieve the above object, the present invention includes the following steps:
Step 1: weighing certain carbon content active and be added in the nitric acid solution of preparation, by this suspension in 40-80 DEG C of water-bath
Under the conditions of handle 1-3h, then then treated active carbon filtration washing will until filtrate pH is 6-7 after washing repeatedly
Filter cake is placed in 80-120 DEG C of baking oven and dries for use;
Step 2: oxalic acid being added in the container of Xiang Shengyou deionized water and is stirred continuously, vanadium forerunner is added until completely dissolved
Body, stirring is until solution becomes blue clarification;
Step 3: being added a certain amount of step (1) into clear solution treated active carbon, stirred under 60-80 DEG C of water bath condition
10min is mixed, is subsequently placed in microwave cavity, is stirred continuously;
Step 4: the active carbon obtained after processing being placed in baking oven, 5-6h is dried at 110-120 DEG C, is finally forged step by step
It burns: calcining 2-4h under nitrogen atmosphere at 300-500 DEG C in tube furnace, calcine 2-4h under 200-250 DEG C of air atmosphere, can obtain
To the V of microwave treatment2O5/ AC catalyst.
V prepared by the present invention2O5/ AC catalyst, wherein V2O5Mass content be not more than 5%.The dosage of V presoma by
V in final products2O5Mass ratio calculate.
A kind of V for SCR reaction2O5The preparation method of/AC catalyst, nitric acid mass percent concentration used are
10-50%.
The ratio between amount of substance of the oxalic acid of middle addition described in step 2 and vanadium presoma is 1:1-4:1.
A kind of V for SCR reaction2O5The preparation method of/AC catalyst, selected vanadium presoma are selected from oxalic acid oxygen
One or more of classes containing vanadic salts such as vanadium, ammonium metavanadate, vanadic sulfate, vanadyl acetylacetonate, vanadium tetrachloride.
A kind of V for SCR reaction2O5The preparation method of/AC catalyst, selected active carbon are fruit shell carbon, coconut husk
One or more of charcoal, carbo lignius, coal quality charcoal isoreactivity charcoal.
A kind of V for SCR reaction2O5The preparation method of/AC, it is micro- selected by microwave irradiation when impregnating in step 2
Wave power is respectively 0-600W and is not 0, preferably 100-400W.
A kind of V for low-temperature SCR reaction2O5The preparation method of/AC catalyst, the time irradiated in microwave is
0.5-3h。
(1) preparation process of the present invention is simple, and preparation condition is easily controllable, raw materials used cheap, and capacity usage ratio is high.
(2) V of microwave-assisted dipping preparation2O5/ AC catalyst, wherein the biggish specific surface area of active carbon is NH3- SCR is anti-
That answers provide place, and microwave treatment promotes dispersion of the active component on carrier, exposes more active sites
Point is conducive to the absorption and activation of reactant molecule, promotes the progress of denitration reaction.
(3) denitration activity that catalyst is effectively increased using the microwave-assisted method for preparing catalyst, in test condition:
1000ppm NH3, 1000ppmNO, 6%O2, Balance Air N2, 30000h-1Under air speed, at 250 DEG C, V2O5/ AC catalyst takes off
Nitre efficiency improves the low-temperature catalytic activity of catalyst close to 100%.
Detailed description of the invention
Fig. 1 is the XRD comparison diagram of the catalyst of preparation of the embodiment of the present invention and the catalyst of comparative example preparation.
Fig. 2 is the denitration activity comparison diagram of the catalyst of preparation of the embodiment of the present invention and the catalyst of conventional method preparation.
Specific embodiment
The present invention is explained below with reference to embodiment, but the present invention is not limited to following embodiments.
Comparative example:
Accurately weigh 1.66g C2H2O4It is added in the beaker of 100ml, then the deionized water of 30ml is added thereto, put
It is complete to be allowed to dissolution for stirring on magnetic stirring apparatus.Weigh 0.7718g NH4VO3It is added in above-mentioned solution, is sufficiently stirred and is allowed to
Dissolution is complete.Lasting stirring, until solution colour becomes blue, the active carbon after 19.4g nitric acid treatment is added is in above-mentioned blue
In solution, in 60 DEG C of stirred in water bath 1h, 6h is dried in 120 DEG C of baking oven, finally 500 DEG C of roasting 3h in nitrogen atmosphere,
250 DEG C of roasting 3h, can be obtained V in air atmosphere2O5/ AC catalyst.
Embodiment 1:
Accurately weigh 1.66g C2H2O4It is added in the beaker of 100ml, then the deionized water of 30ml is added thereto, put
It is complete to be allowed to dissolution for stirring on magnetic stirring apparatus.Weigh 0.7718g NH4VO3It is added in above-mentioned solution, is sufficiently stirred and is allowed to
Dissolution is complete.19.4g is added treated active carbon in above-mentioned blue solution until solution colour becomes blue in lasting stirring.
Above-mentioned beaker is placed in microwave cavity, adjusting microwave power is 100W, in 60 DEG C of stirred in water bath 1h, in 120 DEG C of baking
6h is dried in case, finally 500 DEG C of roasting 3h in nitrogen atmosphere, V can be obtained in 250 DEG C of roasting 3h in air atmosphere2O5/ AC is urged
Agent is denoted as 1#.
Embodiment 2:
Accurately weigh 1.66g C2H2O4It is added in the beaker of 100ml, then the deionized water of 30ml is added thereto, put
It is complete to be allowed to dissolution for stirring on magnetic stirring apparatus.Weigh 0.7718g NH4VO3It is added in above-mentioned solution, is sufficiently stirred and is allowed to
Dissolution is complete.19.4g is added treated active carbon in above-mentioned blue solution until solution colour becomes blue in lasting stirring.
Above-mentioned beaker is placed in microwave cavity, adjusting microwave power is 200W, in 60 DEG C of stirred in water bath 1h, in 120 DEG C of baking
6h is dried in case, finally 500 DEG C of roasting 3h in nitrogen atmosphere, V can be obtained in 250 DEG C of roasting 3h in air atmosphere2O5/ AC is urged
Agent is denoted as 2#.
Embodiment 3:
Accurately weigh 1.66g C2H2O4It is added in the beaker of 100ml, then the deionized water of 30ml is added thereto, put
It is complete to be allowed to dissolution for stirring on magnetic stirring apparatus.Weigh 0.7718g NH4VO3It is added in above-mentioned solution, is sufficiently stirred and is allowed to
Dissolution is complete.19.4g is added treated active carbon in above-mentioned blue solution until solution colour becomes blue in lasting stirring.
Above-mentioned beaker is placed in microwave cavity, adjusting microwave power is 300W, in 60 DEG C of stirred in water bath 1h, in 120 DEG C of baking
6h is dried in case, finally 500 DEG C of roasting 3h in nitrogen atmosphere, V can be obtained in 250 DEG C of roasting 3h in air atmosphere2O5/ AC is urged
Agent is denoted as 3#.
Embodiment 4:
Accurately weigh 1.66g C2H2O4It is added in the beaker of 100ml, then the deionized water of 30ml is added thereto, put
It is complete to be allowed to dissolution for stirring on magnetic stirring apparatus.Weigh 0.7718g NH4VO3It is added in above-mentioned solution, is sufficiently stirred and is allowed to
Dissolution is complete.19.4g is added treated active carbon in above-mentioned blue solution until solution colour becomes blue in lasting stirring.
Above-mentioned beaker is placed in microwave cavity, adjusting microwave power is 350W, in 60 DEG C of stirred in water bath 1h, in 120 DEG C of baking
6h is dried in case, finally 500 DEG C of roasting 3h in nitrogen atmosphere, V can be obtained in 250 DEG C of roasting 3h in air atmosphere2O5/ AC is urged
Agent is denoted as 4#.
Embodiment 5:
Catalyst prepared by above-mentioned comparative example and embodiment 1, embodiment 2, embodiment 3 and embodiment 4 XRD survey has been subjected to
Examination, as a result as shown in Figure 1.
Catalyst prepared by above-mentioned comparative example and embodiment 1, embodiment 2, embodiment 3 and embodiment 4 activity has been subjected to
Evaluation test, as a result as shown in Figure 2.
Test condition: 1000ppm NH3, 1000ppmNO, 6%O2, Balance Air N2, 30000h-1Under air speed, at 250 DEG C,
V2O5The denitration efficiency of/AC catalyst improves the low-temperature catalytic activity of catalyst close to 100%.
Claims (8)
1. one kind improves V by microwave irradiation2O5The method of the SCR low-temperature reactivity of/AC catalyst, which is characterized in that including
Following steps:
Step 1: weighing certain carbon content active and be added in the nitric acid solution of preparation, by this suspension in 40-80 DEG C of water bath condition
Lower processing 1-3h, then will treated active carbon filtration washing, until filtrate pH is 6-7, then by filter cake after washing repeatedly
It is placed in 80-120 DEG C of baking oven and dries for use.
Step 2: oxalic acid is added in the container of Xiang Shengyou deionized water and is stirred continuously, vanadium presoma is added until completely dissolved,
And be stirred continuously, until becoming blue clear solution;Then to treated active carbon, 60 DEG C of water-bath items are added in clear solution
10min is stirred under part, is subsequently placed to impregnate in microwave cavity, be stirred continuously;
Step 3: the active carbon obtained after processing is placed in baking oven, 5-6h is dried at 110-120 DEG C, last step calcination:
It calcines 2-4h under nitrogen atmosphere at 300-500 DEG C in tube furnace, calcines 2-4h under 200-250 DEG C of air atmosphere, can be obtained
Target V2O5/ AC catalyst.
2. according to the method for claim 1, which is characterized in that nitric acid mass percent concentration used is 10- in step (1)
50%.
3. according to the method for claim 1, which is characterized in that vanadium presoma described in step (2) be selected from vanadyl oxalate,
One or more of ammonium metavanadate, ammonium vanadate, positive ammonium vanadate, vanadium tetrachloride.
4. according to the method for claim 1, which is characterized in that selected active carbon is fruit shell carbon, coconut palm during step (1) is described
One or more of shell charcoal, carbo lignius, coal quality charcoal.
5. according to the method for claim 1, which is characterized in that the oxalic acid of step (1) the middle addition and vanadium presoma
The ratio between amount of substance is 1:1-4:1.
6. according to the method for claim 1, which is characterized in that microwave selected by microwave irradiation when dipping in step (2)
Power 0-600W and not be 0, preferably 100-400W.
7. according to the method for claim 1, which is characterized in that in step (2) when dipping selected under microwave irradiation
Between be 0.5-3h.
8. according to the method for claim 1, which is characterized in that the V of gained microwave treatment2O5In/AC catalyst, V2O5Matter
It measures content and is not more than 5%;The dosage of V presoma is by V in final products2O5Mass ratio calculate.
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Cited By (4)
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CN113751014A (en) * | 2021-09-16 | 2021-12-07 | 福州大学 | Monodisperse spindle-shaped monatomic catalyst for denitration and sulfur resistance and preparation method thereof |
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CN117861644A (en) * | 2024-01-08 | 2024-04-12 | 山东蒙稀新材料有限责任公司 | Harmless preparation process of nano cerium oxide |
CN117861644B (en) * | 2024-01-08 | 2024-07-19 | 山东蒙稀新材料有限责任公司 | Harmless preparation process of nano cerium oxide |
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