CN104874394A - Cheap low-temperature SCR catalyst with sulfur resistance and preparation method thereof - Google Patents
Cheap low-temperature SCR catalyst with sulfur resistance and preparation method thereof Download PDFInfo
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Abstract
The invention provides a cheap low-temperature SCR catalyst with sulfur resistance and a preparation method thereof, and belongs to the field of atmosphere pollution prevention NH3-SCR denitration. The catalyst adopts gamma-Al2O3 as a carrier, manganese oxide as an active ingredient and cerium oxide as a modification agent, and the molar ratio of Ce to Mn to Al is (0.02-0.20): 0.4: 1. When in preparation, NH3.H2O is adopted as a precipitating agent to precipitate the carrier precursor Al(NO3)3 to Al(OH)3, dried Al(OH)3 is soaked in a nitric acid solution of the active ingredient, and then Al(OH)3 is dried and calcined to obtain the SCR catalyst. The catalyst is excellent in low-temperature catalytic activity and capacity for resisting toxicity of SO2 and H2O, and the activity is 100 percent under the reaction condition of 120 to 240 DEG C; after 100ppm of SO2 and 3 percent of H2O are added, the activity can be maintained stable for a long time; after SO2 and H2O are cut off, the activity can be completely restored.
Description
Technical field
The present invention relates to prevention and control of air pollution NH
3-SCR (SCR) denitration field, is particularly related to cheapness and the low-temperature SCR catalyst of tool resistance to SO_2 and preparation method, is applicable in the tail gas of coal-burning power plant's discharge containing low concentration SO
2nO
xremove.
Technical background
Nitrogen oxide (NO
x) be one of major pollutants in air, with NO and NO
2proportion is maximum.NO
xhuge harm can be produced to human body and environment.The energy resource structure of China is the few oil of many coals, and " Dissertation of Development of Coal Industry " 12 " planning " that Chinese energy office issues is pointed out: coal is the main body energy of China, in primary energy structure, account for about 70%.Future quite over a long time in, coal can not change as the status of the main body energy.The NO of artificial generation
xthe overwhelming majority is the burning due to coal, and wherein power industry is coal in China consumption " rich and influential family " always." energy-saving and emission-reduction " 12 " planning " that State Council issues for 2012 proposes target: reach 95% to coal unit desulfuration efficiency in 2015, denitration efficiency reaches more than 75%.Focus on " desulfurization " compared to the Eleventh Five-Year Plan period power industry reduction of discharging, " 12 " period " denitration " will become electricity enterprise emission reduction work emphasis.SCR (SCR) technique controls stationary source nitrogen oxide (NO at present
x) major technique of discharging, catalyst is the core of this technique.
At present, industrial application is have the active V of middle temperature (300 ~ 400 DEG C) mostly
2o
5-WO
3/ TiO
2catalyst.In order to utilize flue-gas temperature, before SCR reactor is arranged in dedusting and desulfurizer, but the dust of this position flue gas middle and high concentration and SO
2can also make it poisoning by erosion catalyst, simultaneously high-temperature flue gas catalyst is easily sintered, inactivation, make the lost of life of catalyst.Low-temperature SCR technique refers to that the Applicable temperature of catalyst is 120-250 DEG C or lower temperature, and SCR denitration device adopts afterbody to arrange, is convenient to like this mate with existing boiler plant, can remove the SO of the overwhelming majority simultaneously
2and flying dust, decrease SO
2with the alkali metal such as Na, K in flying dust to the poisoning effect of catalyst, catalyst can be reacted in comparatively clean atmosphere, and without the need to carrying out reheating to catalyst, become the study hotspot in denitration field both at home and abroad at present.
Because Mn oxide has MnO
2, Mn
2o
3, Mn
3o
4, Mn
5o
8deng many oxide form, electronics mutually can shift between the oxide that they are different, makes it have kinds of surface active oxygen, can the carrying out of accelerating oxidation reduction reaction, makes it have good low temperature active.CeO
2by Ce wherein
4+and Ce
3+redox cycle make it have stronger oxygen storage capacity, low temperature active and the resistance to SO_2 of catalyst can be increased.γ-Al
2o
3have larger specific area, stronger surface acidity, catalyst prepared by its Supported Manganese has higher denitration activity, is cheap SCR catalyst carrier.Therefore the present invention proposes the γ-Al prepared by straightforward procedure
2o
3load MnO
x, and use CeO
2the low-temperature SCR catalyst of modification.
Publication number is low-temperature SCR sulfur resistant catalyst and the preparation method that the Chinese patent literature of CN103990496A discloses a kind of graphene-supported titanium base nucleocapsid structure.This catalyst is with nano particle MnO
x-CeO
2for core and TiO
2for shell structure becomes nano-core-shell structure MnO
x-CeO
2tiO
2, then by MnO
x-CeO
2tiO
2form graphene-supported titanium base catalyst with core-casing structure with Graphene phase compound, this invention, by nucleocapsid catalyst prolection center, reduces the accumulation of sulphur ammonium salt by Graphene, thus strengthens catalyst sulfur resistance.But the preparation technology of this catalyst is comparatively complicated, and the Mn-Ce/TiO that cost is prepared compared to infusion process
2catalyst is larger, if be applied to actual coal-burning power plant denitrating catalyst can increase denitration cost.
Publication number is the preparation method that the Chinese patent literature of CN102716752A discloses a kind of low temperature SCR denitration catalyst.Ammonium metavanadate, transition metal salt and titanium tungsten powder are dissolved in the water by the method, and prepare low temperature SCR denitration catalyst through super-dry and calcining.This catalyst can keep certain NO between 150 ~ 250 DEG C
xremoval efficiency and water resistant resistance to SO_2.But to this catalyst at 500ppm NO, 500ppmNH
3, 300ppm SO
2, 10%H
2test its denitration activity under O condition, when 150 DEG C, NO conversion ratio only has 50%, is 68% when being 72%, 250 DEG C when 200 DEG C.This catalyst can not keep very high denitration activity at low temperatures, and this catalyst cost also costly.
Publication number is the preparation method and application that the Chinese patent literature of CN101590404A discloses a kind of low-vanadium denitration catalyst.Prepared by this catalyst infusion process, with Detitanium-ore-type TiO
2for carrier, V
2o
5be main active component, WO
3and CeO
2for playing the secondary active component of cooperative effect.NO within the scope of 200 ~ 450 DEG C
xconversion ratio is more than 90%, and 350 DEG C at 100ppm SO
2under existence condition, in 7h, NO conversion ratio maintains about 90%.But this catalyst just has higher denitration activity and resistance to SO_2 under middle hot conditions, and denitration performance is not good under cryogenic.
Publication number is the preparation method that the Chinese patent literature of CN102553574A discloses a kind of flue gas SCR denitration catalyst, and ammonium metavanadate, oxalic acid and Mn salt and water are made mixed solution by the method, then add TiO in mixed solution
2powder, heating water bath also stirs, and leaves standstill and obtains colloidal sol.Again this colloidal sol microwave is dried, be placed in Muffle furnace calcining and obtain catalyst.When temperature is 250 DEG C, NO conversion ratio is 83.6%.But this catalyst is when being less than 200 DEG C, NO low conversion rate is in 70%, and when 100 DEG C, NO conversion ratio is only 50%.
Publication number is that the Chinese patent literature of CN104289227A discloses a kind of low-temperature denitration of flue gas Four composition NH
3-SCR load type metal catalyst and preparation method thereof.The nitrate of the elements such as this catalyst Mn, Co, Ce is carried on nanoscale P with infusion process
25on, obtain finished catalyst through tube furnace calcining.This catalyst has good low temperature active at the low-temperature range of 150 ~ 200 DEG C, and NO conversion ratio is more than 90%.But the nitrate that this catalyst uses and P
25cost is relatively high.
Therefore develop a kind of cheapness and there is the catalyst of the active and resistance to SO_2 of good low temperature and relative simple preparation method is just necessary very much.
Summary of the invention
The object of this invention is to provide a kind of cheapness, the low-temperature SCR catalyst of tool resistance to SO_2 and preparation method, SCR catalyst can be prepared with simple method, and improve catalyst anti-SO at low temperatures
2poisoning capability, reduces costs.
Technical scheme of the present invention is as follows:
Cheapness and a low-temperature SCR catalyst for tool resistance to SO_2, low-temperature SCR catalyst Mn-Ce (x)/γ-Al
2o
3comprise catalyst carrier and active component, with γ-Al
2o
3for catalyst carrier, load MnO on a catalyst support
xfor active component, CeO
2as modifier, the mol ratio of Ce, Mn, Al three is 0.02 ~ 0.20:0.4:1; Wherein, x=0.02,0.04,0.08,0.12 or 0.20.
The preparation method of described low-temperature SCR catalyst, step is as follows:
(1) preparation of carrier: compound concentration is the Al (NO of 2.5mol/L
3)
3solution, with vigorous stirring, slowly drips the NH of 25%
3h
2o solution, to pH=8 ~ 9, continue to stir 3h, leave standstill aging 1h, centrifugal, dry 12h at 80 DEG C, obtains Al (OH)
3solid;
(2) active component dipping: be 0.02 ~ 0.20:0.4:1 by the mol ratio of Ce, Mn, Al three, by Ce (NO
3)
2be dissolved in Mn (NO
3)
2in solution, then the Al (OH) that will obtain
3solid impregnating is 12h in mixed solution;
(3) catalyst is dry: by impregnation product dry 12h in 80 DEG C of water-baths, be then placed in 110 DEG C of baking ovens and continue dry 2h, obtain black solid;
(4) catalyst calcination: be placed in by black solid in Muffle furnace and calcine 6h at 500 DEG C, obtains γ-Al
2o
3;
(5) finished catalyst is prepared: by the catalyst grinding after calcining, cross 40-60 mesh sieve, obtain catalyst, the amount ratio that Ce accounts for carrier mass is 0.02 ~ 0.20, is designated as Mn-Ce (x)/γ-Al
2o
3, x=0.02,0.04,0.08,0.12 or 0.20.
Low-temperature SCR catalyst of the present invention is with γ-Al
2o
3for carrier, MnO
xfor active component, CeO
2for modifier.γ-Al
2o
3there is larger specific area, can MnO be improved
xand CeO
2decentralization, increase catalytic activity.Doped Ce O
2after, SO
2more be adsorbed on CeO
2on, sulphur ammonium salt is easier at Ce Surface Creation, protects active component MnO
xnot by sulphation, reduce the heat endurance of catalyst surface sulphur ammonium salt simultaneously, improve the anti-SO of catalyst
2poisoning capability.Compared with existing catalyst, this catalyst cost is lower, and method is simple, has certain anti-SO simultaneously
2poisoning capability, has application prospect.
Accompanying drawing explanation
Fig. 1 is the catalyst denitration activity figure of embodiment 1, embodiment 2 and embodiment 3 preparation.
Fig. 2 is that the catalyst of embodiment 1, embodiment 2 and embodiment 3 preparation is at H
2o and SO
2denitration activity figure in atmosphere.
Fig. 3 is that the catalyst of embodiment 4 preparation is at H
2o and SO
2denitration activity figure in atmosphere.
Fig. 4 is that the catalyst of embodiment 5 preparation is at 100ppm SO
2denitration activity figure in atmosphere.
Detailed description of the invention
Below in conjunction with accompanying drawing and technical scheme, further illustrate the specific embodiment of the present invention.
Embodiment 1:
Catalyst preparing: take a certain amount of Al (NO
3)
3powder, adds the Al (NO that appropriate amount of deionized water is made into 2.5mol/L
3)
3solution, with vigorous stirring, slowly drips the NH of 25%
3h
2o solution, to pH=8 ~ 9, stop dripping, continue to stir 3h, leave standstill aging 1h, centrifugal, dry 12h at 80 DEG C, obtains Al (OH)
3solid.Mn (the NO of Ce:Mn:Al=0.02:0.4:1 measured amounts in molar ratio
3)
2solution and Ce (NO
3)
2solid, adds a small amount of deionized water and makes Ce (NO
3)
2dissolution of solid, by the Al (OH) obtained
3solid impregnating is in Mn (NO
3)
2with Ce (NO
3)
2mixed solution in 12h, afterwards by impregnation product dry 12h in 80 DEG C of water-baths, be then placed in 110 DEG C of baking ovens and continue dry 2h, obtain black solid.Again this black solid is placed in Muffle furnace and calcines 6h at 500 DEG C, grinding, cross 40-60 mesh sieves, obtain catalyst Mn-Ce (0.02)/γ-Al
2o
3.
Catalyst denitration activity is tested: simulated flue gas consists of, 600ppm NO, 600ppm NH
3, 3%O
2, N
2for carrier gas.0.4mL catalyst is loaded, gas flow rate 300mL/min, air speed 45000h in reactor
-1, reaction temperature is 120 ~ 240 DEG C, and NO conversion ratio maintains more than 98%.
Catalyst water resistant sulfur resistance is tested: simulated flue gas consists of, 600ppm NO, 600ppm NH
3, 100ppm SO
2, 3%vol.H
2o, 3%O
2, N
2for carrier gas.0.4mL catalyst is loaded, gas flow rate 300mL/min, air speed 45000h in reactor
-1, reaction temperature is 180 DEG C.Logical H
2o and SO
2in process, NO conversion ratio is stabilized in more than 70%, cuts off H
2o and SO
2after, NO conversion ratio returns to 100%.
Embodiment 2:
Catalyst preparing: take a certain amount of Al (NO
3)
3powder, adds the Al (NO that appropriate amount of deionized water is made into 2.5mol/L
3)
3solution, with vigorous stirring, slowly drips the NH of 25%
3h
2o solution, to pH=8 ~ 9, stop dripping, continue to stir 3h, leave standstill aging 1h, centrifugal, dry 12h at 80 DEG C, obtains Al (OH)
3solid.Mn (the NO of Ce:Mn:Al=0.12:0.4:1 measured amounts in molar ratio
3)
2solution and Ce (NO
3)
2solid, adds a small amount of deionized water and makes Ce (NO
3)
2dissolution of solid, by the Al (OH) obtained
3solid impregnating is in Mn (NO
3)
2with Ce (NO
3)
2mixed solution in 12h, afterwards by impregnation product dry 12h in 80 DEG C of water-baths, be then placed in 110 DEG C of baking ovens and continue dry 2h, obtain black solid.Again this black solid is placed in Muffle furnace and calcines 6h at 500 DEG C, grinding, cross 40-60 mesh sieves, obtain catalyst Mn-Ce (0.12)/γ-Al
2o
3.
Catalyst denitration activity is tested: simulated flue gas consists of, 600ppm NO, 600ppm NH
3, 3%O
2, N
2for carrier gas.0.4mL catalyst is loaded, gas flow rate 300mL/min, air speed 45000h in reactor
-1, reaction temperature is 120 ~ 240 DEG C, and NO conversion ratio maintains 100%.
Catalyst water resistant sulfur resistance is tested: simulated flue gas consists of, 600ppm NO, 600ppm NH
3, 100ppm SO
2, 3%vol.H
2o, 3%O
2, N
2for carrier gas.0.4mL catalyst is loaded, gas flow rate 300mL/min, air speed 45000h in reactor
-1, reaction temperature is 180 DEG C.Logical H
2o and SO
2in process, NO conversion ratio is stabilized in more than 75%, cuts off H
2o and SO
2after, NO conversion ratio returns to 100%.
Embodiment 3:
Catalyst preparing: take a certain amount of Al (NO
3)
3powder, adds the Al (NO that appropriate amount of deionized water is made into 2.5mol/L
3)
3solution, with vigorous stirring, slowly drips the NH of 25%
3h
2o solution, to pH=8 ~ 9, stop dripping, continue to stir 3h, leave standstill aging 1h, centrifugal, dry 12h at 80 DEG C, obtains Al (OH)
3solid.Mn (the NO of Ce:Mn:Al=0.20:0.4:1 measured amounts in molar ratio
3)
2solution and Ce (NO
3)
2solid, adds a small amount of deionized water and makes Ce (NO
3)
2dissolution of solid, by the Al (OH) obtained
3solid impregnating is in Mn (NO
3)
2with Ce (NO
3)
2mixed solution in 12h, afterwards by impregnation product dry 12h in 80 DEG C of water-baths, be then placed in 110 DEG C of baking ovens and continue dry 2h, obtain black solid.Again this black solid is placed in Muffle furnace and calcines 6h at 500 DEG C, grinding, cross 40-60 mesh sieves, obtain catalyst Mn-Ce (0.20)/γ-Al
2o
3.
Catalyst denitration activity is tested: simulated flue gas consists of, 600ppm NO, 600ppm NH
3, 3%O
2, N
2for carrier gas.0.4mL catalyst is loaded, gas flow rate 300mL/min, air speed 45000h in reactor
-1, reaction temperature is 120 ~ 240 DEG C, and NO conversion ratio maintains more than 90%.
Catalyst water resistant sulfur resistance is tested: simulated flue gas consists of, 600ppm NO, 600ppm NH
3, 100ppm SO
2, 3%vol.H
2o, 3%O
2, N
2for carrier gas.0.4mL catalyst is filled out, gas flow rate 300mL/min, air speed 45000h in reactor
-1, reaction temperature is 180 DEG C.Logical H
2o and SO
2in process, NO conversion ratio is stabilized in more than 71%, cuts off H
2o and SO
2after, NO conversion ratio returns to 100%.
Embodiment 4:
Catalyst preparing: take a certain amount of Al (NO
3)
3powder, adds the Al (NO that appropriate amount of deionized water is made into 2.5mol/L
3)
3solution, with vigorous stirring, slowly drips the NH of 25%
3h
2o solution, to pH=8 ~ 9, stop dripping, continue to stir 3h, leave standstill aging 1h, centrifugal, dry 12h at 80 DEG C, obtains Al (OH)
3solid.Mn (the NO of Ce:Mn:Al=0.12:0.4:1 measured amounts in molar ratio
3)
2solution and Ce (NO
3)
2solid, adds a small amount of deionized water and makes Ce (NO
3)
2dissolution of solid, by the Al (OH) obtained
3solid impregnating is in Mn (NO
3)
2with Ce (NO
3)
2mixed solution in 12h, afterwards by impregnation product dry 12h in 80 DEG C of water-baths, be then placed in 110 DEG C of baking ovens and continue dry 2h, obtain black solid.Again this black solid is placed in Muffle furnace and calcines 6h at 500 DEG C, grinding, cross 40-60 mesh sieves, obtain catalyst Mn-Ce (0.12)/γ-Al
2o
3.
Catalyst water resistant sulfur resistance is tested: simulated flue gas consists of, 600ppm NO, 600ppm NH
3, 100ppm SO
2, 3%vol.H
2o, 3%O
2, N
2for carrier gas.0.4mL catalyst is loaded, gas flow rate 300mL/min, air speed 45000h in reactor
-1, reaction temperature is 140 DEG C.Logical H
2o and SO
2in process, NO conversion ratio is stabilized in more than 69%, cuts off H
2o and SO
2after, NO conversion ratio returns to 98%.
Embodiment 5:
Catalyst preparing: take a certain amount of Al (NO
3)
3powder, adds the Al (NO that appropriate amount of deionized water is made into 2.5mol/L
3)
3solution, with vigorous stirring, slowly drips the NH of 25%
3h
2o solution, to pH=8 ~ 9, stop dripping, continue to stir 3h, leave standstill aging 1h, centrifugal, dry 12h at 80 DEG C, obtains Al (OH)
3solid.Mn (the NO of Ce:Mn:Al=0.12:0.4:1 measured amounts in molar ratio
3)
2solution and Ce (NO
3)
2solid, adds a small amount of deionized water and makes Ce (NO
3)
2dissolution of solid, by the Al (OH) obtained
3solid impregnating is in Mn (NO
3)
2with Ce (NO
3)
2mixed solution in 12h, afterwards by impregnation product dry 12h in 80 DEG C of water-baths, be then placed in 110 DEG C of baking ovens and continue dry 2h, obtain black solid.Again this black solid is placed in Muffle furnace and calcines 6h at 500 DEG C, grinding, cross 40-60 mesh sieves, obtain catalyst Mn-Ce (0.12)/γ-Al
2o
3.
Catalyst water resistant sulfur resistance is tested: simulated flue gas consists of, 600ppm NO, 600ppm NH
3, 150ppm SO
2, 3%vol.H
2o, 3%O
2, N
2for carrier gas.0.4mL catalyst is loaded, gas flow rate 300mL/min, air speed 45000h in reactor
-1, reaction temperature is 180 DEG C.Logical H
2o and SO
2in process, NO conversion ratio is stabilized in more than 59%, cuts off H
2o and SO
2after, NO conversion ratio returns to 100%.
Claims (2)
1. cheapness and a low-temperature SCR catalyst for tool resistance to SO_2, is characterized in that, low-temperature SCR catalyst Mn-Ce (x)/γ-Al
2o
3comprise catalyst carrier and active component, with γ-Al
2o
3for catalyst carrier, load MnO on a catalyst support
xfor active component, CeO
2as modifier, the mol ratio of Ce, Mn, Al three is 0.02 ~ 0.20:0.4:1; Wherein, x=0.02,0.04,0.08,0.12 or 0.20.
2. the preparation method of low-temperature SCR catalyst according to claim 1, is characterized in that, step is as follows:
(1) preparation of carrier: compound concentration is the Al (NO of 2.5mol/L
3)
3solution, with vigorous stirring, slowly drips the NH of 25%
3h
2o solution, to pH=8 ~ 9, continue to stir 3h, leave standstill aging 1h, centrifugal, dry 12h at 80 DEG C, obtains Al (OH)
3solid;
(2) active component dipping: be 0.02 ~ 0.20:0.4:1 by the mol ratio of Ce, Mn, Al three, by Ce (NO
3)
2be dissolved in Mn (NO
3)
2in solution, then the Al (OH) that will obtain
3solid impregnating is 12h in mixed solution;
(3) catalyst is dry: by impregnation product dry 12h in 80 DEG C of water-baths, be then placed in 110 DEG C of baking ovens and continue dry 2h, obtain black solid;
(4) catalyst calcination: be placed in by black solid in Muffle furnace and calcine 6h at 500 DEG C, obtains γ-Al
2o
3;
(5) finished catalyst is prepared: by the catalyst grinding after calcining, cross 40-60 mesh sieve, obtain catalyst, the amount ratio that Ce accounts for carrier mass is 0.02 ~ 0.20, is designated as Mn-Ce (x)/γ-Al
2o
3, x=0.02,0.04,0.08,0.12 or 0.20.
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| CN107583448A (en) * | 2017-11-03 | 2018-01-16 | 河南理工大学 | A kind of coal-fired flue gas denitration sulfur method |
| CN111530453A (en) * | 2020-04-30 | 2020-08-14 | 山东理工大学 | Ce-Mn composite catalyst for low-temperature SCR denitration reaction and preparation method thereof |
| CN112439409A (en) * | 2020-11-27 | 2021-03-05 | 西安理工大学 | Hydrolysis catalyst for blast furnace gas desulfurization and preparation method thereof |
| CN114054039A (en) * | 2021-12-01 | 2022-02-18 | 合肥工业大学 | Preparation of MnOx/alpha-Fe by utilizing artificially synthesized goethite2O3Method for preparing composite denitration catalyst and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105709572A (en) * | 2016-04-12 | 2016-06-29 | 华中科技大学 | Device and method for reducing toxic effect of SO2 on SCR (selective catalytic reduction) catalyst |
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| CN106824173B (en) * | 2017-03-01 | 2019-06-11 | 石河子大学 | A kind of SCR catalyst for denitrating flue gas and preparation method thereof |
| CN107583448A (en) * | 2017-11-03 | 2018-01-16 | 河南理工大学 | A kind of coal-fired flue gas denitration sulfur method |
| CN111530453A (en) * | 2020-04-30 | 2020-08-14 | 山东理工大学 | Ce-Mn composite catalyst for low-temperature SCR denitration reaction and preparation method thereof |
| CN112439409A (en) * | 2020-11-27 | 2021-03-05 | 西安理工大学 | Hydrolysis catalyst for blast furnace gas desulfurization and preparation method thereof |
| CN114054039A (en) * | 2021-12-01 | 2022-02-18 | 合肥工业大学 | Preparation of MnOx/alpha-Fe by utilizing artificially synthesized goethite2O3Method for preparing composite denitration catalyst and application thereof |
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