CN104941658A - Low-temperature SCR anti-poisoning catalyst suitable for cement kiln and preparation method of low-temperature SCR anti-poisoning catalyst - Google Patents
Low-temperature SCR anti-poisoning catalyst suitable for cement kiln and preparation method of low-temperature SCR anti-poisoning catalyst Download PDFInfo
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Abstract
The invention provides a low-temperature SCR anti-poisoning catalyst suitable for a cement kiln and a preparation method of the low-temperature SCR anti-poisoning catalyst, belongs to the fields of environment protection techniques and environment catalysis, and in particular relates to a Co-modified Ce-ZrO2 supported MnOx low-temperature SCR catalyst capable of strongly resisting poisoning of alkali metals, SO2 and H2O and a preparation method thereof. The catalyst uses Ce-ZrO2 as a carrier, manganese oxide as an active component and cobalt oxide as a modifier, wherein the molar ratio of Mn: Co+Ce+Zr is 0.4:1, the molar ratio of carrier Co: Co+Ce+Zr is 0.1-0.2 and the molar ratio of Ce: Zr is 1: 1. The prepared catalyst has relative good capability of resisting poisoning of SO2, H2O and alkali metals and has unique advantages in aspect of treatment of low-temperature exhaust such as cement kiln tail gas and biomass fuel boiler flue gas in which the alkali metal content is high and both SO2 and H2O exist simultaneously.
Description
Technical field
The invention belongs to environmental protection technology and environmental catalysis field.Be specifically related to a kind of Co modification Ce-ZrO being applicable to cement kiln
2carrier loaded MnO
xthe anti-poisoned catalyst of low-temperature SCR and preparation technology thereof.
Background technology
Nitrogen oxide (NO
x) be one of atmosphere pollution causing many environmental problems such as acid rain, photochemical fog, greenhouse effects and depletion of the ozone layer, NH
3sCR (NH
3-SCR) technology because having the features such as high selectivity, high stability and high denitration rate, become control NO
xthe mainstream technology of discharge, and at station boiler tail gas NO
xbe used widely in control.In recent years, cement industry NO
xdischarge in rising trend, 2013 annual emissions are 2,450,000 t, account for 11% of national total emission volumn, expect the year two thousand twenty, and discharge capacity will reach 5,700,000 t.But business SCR catalyst is not suitable for using on cement kiln at present: first, business SCR catalyst active temperature windows is at 300 DEG C ~ 400 DEG C, and the position being applicable to installing SCR reactor in cement kiln production line all cannot meet reaction temperature requirement; Secondly, cement kiln flue gas contains alkali metal, SO
2, H
2o etc., easily cause catalyst poisoning inactivation.Therefore, developing low temperature resists poisoning SCR catalyst very necessary.
Research at present for the denitration of cement kiln tail gas focuses mostly on little in SNCR, SCR correlative study.Publication number is the patent of invention of CN103638942A, describes the preparation method of a kind of applicable cement kiln low-temperature smoke catalytic agent, has good low temperature active and anti-SO
2poisoning capability, but the research not carrying out alkali resistant metal poisoning.Publication number is the patent of invention of CN102658172A, describe a kind of reaction temperature has the catalyst of anti-alkali and alkaline earth metal ions poisoning performance preparation at 320 DEG C ~ 520 DEG C, but this catalyst is unfavorable for that the flue-gas temperature after UTILIZATION OF VESIDUAL HEAT IN is all lower than the small-sized industrial boiler of 300 DEG C.Chinese patent, publication No. is CN103990496A, describes a kind of active temperature and have low temperature catalyst and preparation thereof in anti-poisoning performance between 140 DEG C ~ 500 DEG C, has higher alkali resistant metal poisoning ability, but anti-SO
2poisoning capability has much room for improvement.
Therefore, under seeking low temperature, there is higher denitration activity, stronger alkali resistant metal, SO
2, H
2the poisoning SCR catalyst of O is particularly important.
Summary of the invention
The object of the present invention is to provide a kind of denitration activity good, alkali resistant metal, SO
2, H
2low-temperature SCR catalyst that O poisoning capability is strong and preparation method thereof.
Technical scheme of the present invention is as follows:
Be applicable to the anti-poisoned catalyst of low-temperature SCR of cement kiln, this catalyst take Co as modifier, to Ce-ZrO
2modification, with Co-Ce-ZrO
2for carrier, with MnO
xfor active component; Wherein, the mol ratio of Co:Co+Ce+Zr is 0.1 ~ 0.2, and the mol ratio of activity component load quantity Mn:Co+Ce+Zr is 0.4, wherein Ce:Zr=1:1, x=1.5 ~ 2.
Be applicable to a preparation method for the anti-poisoned catalyst of low-temperature SCR of cement kiln, step is as follows:
(1) Co-Ce-Zr complex hydroxide carrier is prepared
According to above-mentioned mol ratio, preparation Ce (NO
3)
36H
2o, ZrO (NO
3)
2, Co (NO
3)
26H
2the mixed solution of O, under the condition of vigorous stirring, dropwise adds the NH that mass fraction is 10% ~ 25%
3h
2o solution, until PH=9 ~ 10., precipitation continued to stir 2.5h ~ 3h, static aging 1h ~ 1.5h, after centrifugal, 80 DEG C of dry 12h, obtain Co-Ce-Zr complex hydroxide carrier;
(2) support type MnO is prepared
x/ Co
yce
(1-y)/2zr
(1-y)/2o
2catalyst
In Co-Ce-Zr complex hydroxide manganese nitrate solution step (1) obtained, room temperature immersion 10h ~ 12h, obtains support type MnO after drying and calcining
x/ Co
yce
(1-y)/2zr
(1-y)/2o
2catalyst, it adopts the dry order of high temperature after first low temperature: first at 70 DEG C ~ 80 DEG C dry 12h ~ 14h, then at 100 DEG C ~ 120 DEG C dry 4h ~ 6h; At 400 DEG C ~ 500 DEG C temperature lower calcination 4h ~ 6h; Wherein x=1.5 ~ 2, y=0.1 ~ 0.2.
The precursor of described support C o-Ce-Zr complex hydroxide is Ce (NO
3)
36H
2o, ZrO (NO
3)
2, Co (NO
3)
26H
2the mixed solution of O.Precipitating reagent NH
3h
2the mass fraction of O controls 10% ~ 25%.Reaction temperature controls at 18 DEG C ~ 25 DEG C.Rate of titration is dripped at 0.5 drop/sec ~ 1 drop/sec.PH value controls 9 ~ 10.Supernatant washing centrifuge tube tube wall or the NH with PH=10 is adopted time centrifugal
3.H
2the mode of washing that O washes.Dry employing drying with water bath, water temperature is 80 DEG C, dry 12h.
Described support type MnO
x/ Co
yce
(1-y)/2zr
(1-y)/2o
2adopt Co-Ce-Zr complex hydroxide for dipping substrate in catalyst soakage method preparation process.Active component adopts manganese nitrate solution to be precursor, and its mass fraction controls 30% ~ 50%.The dry order of high temperature after the first low temperature of dry employing: first dry 12h ~ 14h at 70 DEG C ~ 80 DEG C, then at 100 DEG C ~ 120 DEG C dry 4h ~ 6h.Roasting is in 400 DEG C ~ 500 DEG C temperature lower calcination 4h ~ 6h in air atmosphere.
Effective effect of the present invention is:
Catalyst provided by the invention is not high to serviceability temperature dependence, still has greater activity, thus catalyst can be positioned over the relatively low exhaust emission pipeline afterbody of temperature under low temperature (100 DEG C ~ 240 DEG C).In addition, inventor, by the interaction between metal, utilizes Co modification Ce-ZrO
2carrier significantly improves ratio, the reduction Ce-ZrO of the L acid/B acid of carrier
2the character of the degree of crystallinity of carrier, the specific area of raising catalyst strengthens the anti-poisoning capability of low-temperature SCR catalyst.Support in catalyst is provided to the application of SCR denitration technology on cement furnace.
Accompanying drawing explanation
The denitration efficiency of the catalyst that Fig. 1 is embodiment 1, prepared by embodiment 2.
Denitration efficiency after the catalyst alkali metal that Fig. 2 is embodiment 1, prepared by embodiment 3, embodiment 4 is poisoning.
The catalyst that when Fig. 3 is 180 DEG C prepared by embodiment 1 is at alkali metal, SO
2, H
2denitration efficiency when O exists simultaneously.
Detailed description of the invention
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1
Be the Ce (NO of 99.5% by mass fraction
3)
36H
2o, 99% ZrO (NO
3)
2, 98.5% Co (NO
3)
26H
2o is dissolved in the deionized water of 80 DEG C according to Co:Ce:Zr=0.2:0.4:0.4 (mol ratio), be made into the solution of 0.3mol/L, cool to room temperature, when vigorous stirring, reaction temperature are under 20 DEG C of conditions, dropwise adds by the speed of 0.5 drop/sec the NH that mass fraction is 25%
3h
2o solution, until PH=10, stops adding NH
3h
2o, will continue at being now deposited in 20 DEG C to stir 3h, static aging 1h, after centrifugal, adopts supernatant washing centrifuge tube tube wall, after by precipitation 80 DEG C of drying with water bath 12h, obtained Co-Ce-Zr complex hydroxide.According to Mn:(Ce+Zr+Co) the mol ratio of=0.4:1 mass fraction that measures certain volume be 50% Mn (NO
3)
24H
2o solution, impregnated on Co-Ce-Zr complex hydroxide, room temperature immersion 12h, 80 DEG C of dry 12h, then 110 DEG C of dry 5h, and 500 DEG C of air atmosphere calcining 6h, obtain support type MnO
x/ Co
0.2ce
0.4zr
0.4o
2catalyst.
Catalyst activity is tested:
The catalyst of preparation is ground, sieves, gets 0.4mL40 order ~ 60 object catalyst and put into fixed bed stainless steel tube reactor, pass into by N
2, O
2, NO and NH
3the simulated flue gas of composition is tested, wherein [NO]=600ppm, [NH
3]=600ppm, [O
2]=3vol.%, N
2for Balance Air, total flow is 300mL/min, air speed 45000h
-1, reaction temperature is 100 DEG C ~ 240 DEG C, and the conversion ratio of NO maintains 100%.
Alkali resistant metal poisoning performance test:
The KNO of certain mass is taken according to the mol ratio of K:Mn=0.1
3be made into certain density solution, incipient impregnation MnO
x/ Co
0.2ce
0.4zr
0.4o
2catalyst 3h, 80 DEG C of dry 0.5h, 500 DEG C of air atmosphere calcining 3h.Institute's controlling catalyst simulates alkali metal oxide K in this approach
2o intoxication conditions.By load K
2the catalyst of O grinds, sieves, and gets 0.4mL40 order ~ 60 object catalyst and is placed in fixed bed stainless steel tube reactor, pass into by N
2, O
2, NO and NH
3the simulated flue gas of composition is tested, wherein [NO]=600ppm, [NH
3]=600ppm, [O
2]=3vol.%, N
2for Balance Air, total flow is 300mL/min, air speed 45000h
-1, reaction temperature is 140 DEG C ~ 240 DEG C, and the NO conversion ratio of the poisoning rear catalyst of alkali metal still maintains more than 88%.
Alkali resistant metal, SO
2, H
2o performance test:
There is alkali metal, SO in cement kiln flue gas simultaneously
2, H
2o, makes catalyst poisoning.100ppm SO is added in above-mentioned simulated flue gas
2, 2.5vol.%H
2o, chooses above-mentioned load K
2the catalyst of O carries out alkali resistant metal, SO
2, H
2o performance test, test reaction temperature is 180 DEG C, logical H
2o and SO
2in process, NO conversion ratio is stabilized in more than 78%, cuts off H
2o and SO
2after, NO conversion ratio returns to 96%.
Embodiment 2
Catalyst preparing:
Be the Ce (NO of 99.5% by mass fraction
3)
36H
2o, 99% ZrO (NO
3)
2, 98.5% Co (NO
3)
26H
2o is dissolved in the deionized water of 80 DEG C according to Co:Ce:Zr=0.1:0.45:0.45 (mol ratio), be made into the solution of 0.3mol/L, cool to room temperature, when vigorous stirring, reaction temperature are under 20 DEG C of conditions, dropwise adds by the speed of 0.5 drop/sec the NH that mass fraction is 25%
3h
2o solution, until PH=10, stops adding NH
3h
2o, will continue at being now deposited in 20 DEG C to stir 3h, static aging 1h, after centrifugal, adopts supernatant washing centrifuge tube tube wall, after by precipitation 80 DEG C of drying with water bath 12h, obtained Co-Ce-Zr complex hydroxide.According to Mn:(Ce+Zr+Co) the mol ratio of=0.4:1 mass fraction that measures certain volume be 50% Mn (NO
3)
24H
2o solution impregnated on Co-Ce-Zr complex hydroxide, room temperature immersion 12h, 80 DEG C of dry 12h, then 110 DEG C of dry 5h, 500 DEG C of air atmospheres calcining 6h, obtain support type MnO
x/ Co
0.1ce
0.45zr
0.45o
2catalyst.
Catalyst activity is tested:
The catalyst of preparation is ground, sieves, gets 0.4mL40 order ~ 60 object catalyst and put into fixed bed stainless steel tube reactor, pass into by N
2, O
2, NO and NH
3the simulated flue gas of composition is tested, wherein [NO]=600ppm, [NH
3]=600ppm, [O
2]=3vol.%, N
2for Balance Air, total flow is 300mL/min, air speed 45000h
-1, reaction temperature 100 DEG C ~ 240 DEG C, when when 100 DEG C, the conversion ratio of NO is 95%, 120 DEG C ~ 240 DEG C, the conversion ratio of NO maintains 100%.
Embodiment 3
Be the Ce (NO of 99.5% by mass fraction
3)
36H
2o, 99% ZrO (NO
3)
2, 98.5% Co (NO
3)
26H
2o is dissolved in the deionized water of 80 DEG C according to Co:Ce:Zr=0.1:0.45:0.45 (mol ratio), be made into the solution of 0.3mol/L, cool to room temperature, when vigorous stirring, reaction temperature are under 20 DEG C of conditions, dropwise adds by the speed of 0.5 drop/sec the NH that mass fraction is 25%
3h
2o solution, until PH=10, stops adding NH
3h
2o, will continue at being now deposited in 20 DEG C to stir 3h, static aging 1h, after centrifugal, adopts supernatant washing centrifuge tube tube wall, after by precipitation 80 DEG C of drying with water bath 12h, obtained Co-Ce-Zr complex hydroxide.According to Mn:(Ce+Zr+Co) the mol ratio of=0.4:1 mass fraction that measures certain volume be 50% Mn (NO
3)
24H
2o solution impregnated on Co-Ce-Zr complex hydroxide, room temperature immersion 12h, 80 DEG C of dry 12h, then 110 DEG C of dry 5h, 500 DEG C of air atmospheres calcining 4h, obtain loaded catalyst.
Alkali resistant metal poisoning performance test:
The KNO of certain mass is taken according to the mol ratio of K:Mn=0.1
3be made into certain density solution, the above-mentioned catalyst 3h of incipient impregnation, 80 DEG C of dry 0.5h, 500 DEG C of air atmosphere calcining 3h.Institute's controlling catalyst simulates K in this approach
2o intoxication conditions.By load K
2the catalyst of O grinds, sieves, and gets 0.4mL40 order ~ 60 object catalyst and puts into fixed bed stainless steel tube reactor, pass into by N
2, O
2, NO and NH
3the simulated flue gas of composition is tested, wherein [NO]=600ppm, [NH
3]=600ppm, [O
2]=3vol.%, N
2for Balance Air, total flow is 300mL/min, air speed 45000h
-1, reaction temperature 140 DEG C ~ 240 DEG C, when the poisoning rear NO conversion ratio of alkali metal is 64%, 160 DEG C ~ 240 DEG C 140 DEG C time, NO conversion ratio maintains more than 83% always.
Embodiment 4
Be the Ce (NO of 99.5% by mass fraction
3)
36H
2o, 99% ZrO (NO
3)
2, 98.5% Co (NO
3)
26H
2o is dissolved in the deionized water of 80 DEG C according to Co:Ce:Zr=0.1:0.45:0.45 (mol ratio), be made into the solution of 0.3mol/L, cool to room temperature, when vigorous stirring, reaction temperature are under 20 DEG C of conditions, dropwise adds by the speed of 0.5 drop/sec the NH that mass fraction is 25%
3h
2o solution, until PH=10, stops adding NH
3h
2o, will continue at being now deposited in 20 DEG C to stir 3h, static aging 1h, after centrifugal, adopts supernatant washing centrifuge tube tube wall, after by precipitation 80 DEG C of drying with water bath 12h, obtained Co-Ce-Zr complex hydroxide.According to Mn:(Ce+Zr+Co) the mol ratio of=0.4:1 mass fraction that measures certain volume be 50% Mn (NO
3)
24H
2o solution impregnated on Co-Ce-Zr complex hydroxide, room temperature immersion 12h, 80 DEG C of dry 12h, then 110 DEG C of dry 5h, 400 DEG C of air atmospheres calcining 6h, obtain loaded catalyst.
Alkali resistant metal poisoning performance test:
The KNO of certain mass is taken according to the mol ratio of K:Mn=0.1
3be made into certain density solution, the above-mentioned catalyst 3h of incipient impregnation, 80 DEG C of dry 0.5h, 400 DEG C of air atmosphere calcining 3h.Institute's controlling catalyst simulates K in this approach
2o intoxication conditions.By load K
2the catalyst of O grinds, sieves, and gets 0.4mL40 order ~ 60 object catalyst and puts into fixed bed stainless steel tube reactor, pass into by N
2, O
2, NO and NH
3the simulated flue gas of composition is tested, wherein [NO]=600ppm, [NH
3]=600ppm, [O
2]=3vol.%, N
2for Balance Air, total flow is 300mL/min, air speed 45000h
-1, reaction temperature 140 DEG C ~ 240 DEG C, 160 DEG C ~ 240 DEG C time, the conversion ratio of the poisoning rear NO of alkali metal maintains more than 70% always.
Claims (2)
1. be applicable to the anti-poisoned catalyst of low-temperature SCR of cement kiln, it is characterized in that: this catalyst is modifier with Co, to Ce-ZrO
2modification, with Co-Ce-ZrO
2for carrier, with MnO
xfor active component; Wherein, the mol ratio of Co:Co+Ce+Zr is 0.1 ~ 0.2, and the mol ratio of activity component load quantity Mn:Co+Ce+Zr is 0.4, wherein Ce:Zr=1:1, x=1.5 ~ 2.
2. a kind of preparation method being applicable to the anti-poisoned catalyst of low-temperature SCR of cement kiln according to claim 1, it is characterized in that, step is as follows:
(1) Co-Ce-Zr complex hydroxide carrier is prepared
According to mol ratio according to claim 1, preparation Ce (NO
3)
36H
2o, ZrO (NO
3)
2, Co (NO
3)
26H
2the mixed solution of O, under the condition of vigorous stirring, dropwise adds the NH that mass fraction is 10% ~ 25%
3h
2o solution, until PH=9 ~ 10, precipitation continued to stir 2.5h ~ 3h, static aging 1h ~ 1.5h, after centrifugal, 80 DEG C of dry 12h, obtain Co-Ce-Zr complex hydroxide carrier;
(2) support type MnO is prepared
x/ Co
yce
(1-y)/2zr
(1-y)/2o
2catalyst
The Co-Ce-Zr complex hydroxide that step (1) obtains be impregnated in manganese nitrate solution, room temperature immersion 10h ~ 12h, after drying and calcining, obtain support type MnO
x/ Co
yce
(1-y)/2zr
(1-y)/2o
2catalyst, it adopts the dry order of high temperature after first low temperature: first at 70 DEG C ~ 80 DEG C dry 12h ~ 14h, then at 100 DEG C ~ 120 DEG C dry 4h ~ 6h; At 400 DEG C ~ 500 DEG C temperature lower calcination 4h ~ 6h; Wherein x=1.5 ~ 2, y=0.1 ~ 0.2.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106732511A (en) * | 2017-01-23 | 2017-05-31 | 中国环境科学研究院 | A kind of biomass carbon denitrating catalyst and its preparation method and application |
| CN111167473A (en) * | 2020-03-18 | 2020-05-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Copromoted cobaltosic oxide/silicon dioxide catalyst with Mn and Co, and preparation method and application thereof |
| CN113522274A (en) * | 2021-08-06 | 2021-10-22 | 上海环境卫生工程设计院有限公司 | Alkali metal poisoning-resistant low-temperature manganese-based SCR denitration catalyst and preparation method thereof |
| CN114602479A (en) * | 2022-04-18 | 2022-06-10 | 苏州西热节能环保技术有限公司 | Co modified low-temperature denitration catalyst based on Ce-Zr oxide carrier |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106732511A (en) * | 2017-01-23 | 2017-05-31 | 中国环境科学研究院 | A kind of biomass carbon denitrating catalyst and its preparation method and application |
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| CN113522274A (en) * | 2021-08-06 | 2021-10-22 | 上海环境卫生工程设计院有限公司 | Alkali metal poisoning-resistant low-temperature manganese-based SCR denitration catalyst and preparation method thereof |
| CN113522274B (en) * | 2021-08-06 | 2023-09-01 | 上海环境卫生工程设计院有限公司 | Alkali metal poisoning resistant low-temperature manganese-based SCR denitration catalyst and preparation method thereof |
| CN114602479A (en) * | 2022-04-18 | 2022-06-10 | 苏州西热节能环保技术有限公司 | Co modified low-temperature denitration catalyst based on Ce-Zr oxide carrier |
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