CN107497419A - NO and Hg in coal-fired flue-gas is purified for low temperature simultaneously0Ce Zr MnO2Method for preparing catalyst - Google Patents

NO and Hg in coal-fired flue-gas is purified for low temperature simultaneously0Ce Zr MnO2Method for preparing catalyst Download PDF

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Publication number
CN107497419A
CN107497419A CN201710860828.8A CN201710860828A CN107497419A CN 107497419 A CN107497419 A CN 107497419A CN 201710860828 A CN201710860828 A CN 201710860828A CN 107497419 A CN107497419 A CN 107497419A
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catalyst
gas
mno
low temperature
coal
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CN201710860828.8A
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Chinese (zh)
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路培
吴婉蓉
邢奕
岳会芳
李锐
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北京科技大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
    • 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
    • B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
    • 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
    • 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
    • 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
    • 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
    • B01J23/32—Manganese, technetium or rhenium
    • B01J23/34—Manganese
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

Abstract

The present invention provides a kind of low temperature that is used for and purifies NO and Hg in coal-fired flue-gas simultaneously0Ce Zr MnO2Method for preparing catalyst, belong to environmental protection technical field.This method is by the way that the nitrate of tri- kinds of metals of Mn, Ce and Zr according to a certain ratio, to be made mixed sediment with coprecipitation and be calcined at 400 600 DEG C so as to obtain low temperature efficient removal NO and Hg simultaneously0Sample.The sample under cryogenic, has more excellent purification efficiency to NO, at the same can be in efficient removal waste gas Hg0.This method process conditions are simple, and catalyst volume is small, and function admirable is workable, are adapted to large-scale production, the NO and Hg in the industry flue gas such as power plant, steel, metallurgy0Synergistic purification in there is very high practical value.

Description

NO and Hg in coal-fired flue-gas is purified for low temperature simultaneously0Ce-Zr-MnO2Catalyst system Preparation Method

Technical field

The present invention relates to environmental protection technical field, particularly relate to it is a kind of be used for low temperature and meanwhile purify in coal-fired flue-gas NO with Hg0Ce-Zr-MnO2Method for preparing catalyst.

Background technology

In technical field of air pollution control, due in the coal combustion exhaust that is discharged in the production processes such as thermal power plant, steel In the presence of substantial amounts of nitrogen oxides (NOx) and element mercury (Hg), both pollutants have not only seriously endangered ecological environment, and give The health of people brings serious threat.And the nitrogen oxides more than 90% in waste gas is made up of NO, and in flue gas In the Hg of existing various forms, Hg0Harm is maximum and is most difficult to remove.Therefore the NO and Hg in efficient removal flue gas0With very Important environment and health is worth.

However, the removing of nitrogen oxides is how non-by SCR (SCR) or selectivity in coal combustion exhaust at present The methods of catalysis reduction (SNCR), is carried out, and SCR method is to Hg present in flue gas0There is certain removing to act on, but efficiency Not high, this is primarily due to SCR catalyst in 300-400 DEG C of denitration efficiency highest.But at this temperature, the efficiency of demercuration It is not ideal enough.SO in flue gas at this temperature simultaneously2Easily SO is changed under SCR catalyst effect3.At present, gas in waste gas The purification of state mercury, mainly by activated carbon injection technique (activated carbon injection technologies), This method can effectively remove gaseous mercury, but the technical operation cost is very big, nor can effectively take off simultaneously Nitrogen oxides in removing exhaust gas.

Therefore, while the NO in coal combustion exhaust and Hg is removed0With good social value and market application foreground, thus Develop under a kind of 100-300 DEG C of cryogenic conditions can NO_x Reduction by Effective demercuration catalyst sample it is significant.

The content of the invention

It is used for low temperature the technical problem to be solved in the present invention is to provide one kind and purifies NO and Hg in coal-fired flue-gas simultaneously0's Ce-Zr-MnO2Method for preparing catalyst.

Ce-Zr-MnO prepared by this method2Catalyst is to prepare to be formed after co-precipitate certain using coprecipitation method Under the conditions of calcining made from CeO2、ZrO2、MnO2Mixing nano-oxide, tri- kinds of elements of Ce, Zr, Mn are shared in the catalyst Mol ratio be 0.12-0.47:0.17-0.32:0.31-0.71.

The specific preparation method of the catalyst is as follows：

(1) nitrate containing Mn, Ce and Zr is weighed respectively by Mn, Ce and Zr mol ratio, be added in the lump in deionized water Salting liquid is made to being completely dissolved in stirring, heating water bath is used in course of dissolution to promote the dissolving of nitrate, deionized water is used Amount ensures to dissolve each component nitrate in room temperature；

(2) mixing salt solution obtained in step (1) is cooled to room temperature, while stirring, while a certain amount of ammoniacal liquor is added, Mn, Ce and Zr is formed mixed precipitation, after certain time stirring and aging, precipitation is filtered, in certain temperature after washing Lower drying；

(3) step (2) dried sample is calcined under constituent of air, then grinds and 100-300 DEG C of low temperature bar is made NO and Hg in high-efficient purification flue gas simultaneously under part0Ce-Zr-MnO2Composite nanometer particle catalyst sample.

Wherein, the temperature of heating water bath is 60-90 DEG C in step (1).

The pH value that ammoniacal liquor is added in step (2) is 8-14, is added dropwise and continuously stirs, until mixed liquor pH value reaches 9- 14, three metal ion species precipitation is complete.After precipitation by metallic ion is complete, stop adding ammoniacal liquor, it is that 2-4 is small to continue mixing time When, ageing time is 0.5-3 hours.Drying temperature is 70-120 DEG C, and drying time is 6-12 hours.

Calcining heat is 400-600 DEG C in step (3), and calcination time be 4-5 hours, in calcination process, heating and is cooled Speed is 1-30 DEG C/min.Sample is 5-10nm nano particle after calcining and grinding.

The above-mentioned technical proposal of the present invention has the beneficial effect that：

This method by by three kinds of cerium, zirconium, manganese metal-nitrate solutions according to certain ratio and proportioning, with co-precipitation Method prepares mixed sediment, then calcines mixed precipitation under certain condition to obtain under low temperature while in high-efficient purification flue gas NO and Hg0Ce-Zr-MnO2Composite nanometer particle catalyst sample.The sample is under 100-300 DEG C of cryogenic conditions, to Hg0Tool There is high purification efficiency, while can efficiently remove the NO in mixed gas.

Embodiment

To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with specific implementation Example is described in detail.

The present invention provides a kind of low temperature that is used for and purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Catalyst preparation Method.

Embodiment 1

Ce, Zr, Mn mol ratio are weighed as 0.47：0.22：The metal nitrate of 0.31 respective quality, is added in the lump In ionized water, 80 DEG C of heating water baths and being continuously stirring to are completely dissolved, and salting liquid to be mixed is cooled to room temperature, while stirring, one A certain amount of ammoniacal liquor is added dropwise simultaneously in side, until pH of mixed reaches 10.Continue aging 1 hour after stirring 3 hours.Thereafter precipitation is taken out Filter, 80 DEG C of drying in baking oven are put into after washing.It is placed in again in Muffle furnace and rises to 500 DEG C with 5 DEG C/min speed, constant temperature 5 hours After naturally cool to room temperature.NO and Hg in high-efficient purification flue gas simultaneously is made under cryogenic in grinding0Ce-Zr-MnO2It is compound Nanoparticle catalyst sample.

The sample that will be obtained in embodiment 1, it is experimental subjects to take 0.800g, using nitrogen as Balance Air, 100-300 DEG C In temperature range, air speed 40000h-1、CNO=1000ppm, CNH3=1000ppm, oxygen concentration=10%, CHg0=42 μ g/m3 Under the conditions of, at 200 DEG C, NO removal efficiencies are 99%, Hg0Removal efficiency be 100%.At 150 DEG C, NO removal efficiencies are 98%, Hg0Removal efficiency be 100%

Embodiment 2：

Other conditions are same as Example 1, and difference is that calcining heat is 400 DEG C, other conditions and test-strips Part is identical with 1, and for the sample at 200 DEG C, NO removal efficiencies are 95%, Hg0Removal efficiency be 99%.Take off compared with Example 1 Mercury efficiency, denitration efficiency have all declined.At 150 DEG C, NO removal efficiencies are 96%, Hg0Removal efficiency be 99%, denitration demercuration Efficiency has all declined.

Embodiment 3：

Other conditions are same as Example 1, and difference is that calcining heat is 600 DEG C, other conditions and test-strips Part is identical with 1, and for the sample at 200 DEG C, NO removal efficiencies are 90%, Hg0Removal efficiency be 95%.Take off compared with Example 1 Mercury efficiency, denitration efficiency have all declined.At 150 DEG C, NO removal efficiencies are 89%, Hg0Removal efficiency be 94%, denitration demercuration Efficiency is all decreased obviously.

Embodiment 4：

Other conditions are same as Example 1, and difference is that Ce, Zr, Mn mol ratio are 0.37：0.26：0.37, its His condition and test condition are identical with 1, and for the sample at 200 DEG C, NO removal efficiencies are 96%, Hg0Removal efficiency be 100%.Demercuration efficiency is identical compared with Example 1, and denitration efficiency has declined.At 150 DEG C, NO removal efficiencies are 98%, Hg0Removal efficiency be 100%, it is same as Example 1.

Embodiment 5：

Other conditions are same as Example 1, and difference is that Ce, Zr, Mn mol ratio are 0.23：0.32：0.45, its His condition and test condition are identical with 1, and for the sample at 200 DEG C, NO removal efficiencies are 99%, Hg0Removal efficiency be 99%. Denitration efficiency is identical compared with Example 1, and demercuration efficiency is slightly decreased.At 150 DEG C, NO removal efficiencies are 71%, Hg0It is de- Except rate is 99%, demercuration efficiency is slightly decreased compared with Example 1, and denitration efficiency declines to a great extent.

Embodiment 6：

Other conditions are same as Example 1, and difference is that Ce, Zr, Mn mol ratio are 0.16：0.22：0.62, its His condition and test condition are identical with 1, and for the sample at 200 DEG C, NO removal efficiencies are 97%, Hg0Removal efficiency be 100%, demercuration efficiency is identical compared with Example 1, and denitration efficiency has declined.At 150 DEG C, NO removal efficiencies are 98%, Hg0Removal efficiency be 100%, it is same as Example 1.

Embodiment 7：

Other conditions are same as Example 1, and difference is that Ce, Zr, Mn mol ratio are 0.12：0.17：0.71, its His condition and test condition are identical with 1, and for the sample at 200 DEG C, NO removal efficiencies are 99%, Hg0Removal efficiency be 100%.Demercuration denitration efficiency is all identical compared with Example 1.At 150 DEG C, NO removal efficiencies are 92%, Hg0Removal efficiency be 100%, demercuration efficiency is identical compared with Example 1, and denitration efficiency has declined.

Embodiment 8：

Other conditions are same as Example 1, difference be test when be passed through 5% steam, other conditions and Test condition is identical with 1, and for the sample at 200 DEG C, NO removal efficiencies are 86%, Hg after 5% steam is passed through 8 hours0It is de- Except rate is 93%, Hg compared with Example 10Removal efficiency and NO removal efficiency it is all poor.Removing 5% steam two hours Afterwards, NO removal efficiencies are 93%, Hg0Removal efficiency be 97%.

Embodiment 9：

Other conditions are same as Example 1, and difference is to be passed through 1000ppm SO in test2, other conditions with And test condition is identical with 1, the sample is at 200 DEG C, 1000 ppm SO2NO removal efficiencies are 83%, Hg after being passed through 8 hours0 Removal efficiency be 92%, Hg compared with Example 10Removal efficiency and NO removal efficiency it is all poor.Removing 1000ppm SO2Two After hour, NO removal efficiencies are 89%, Hg0Removal efficiency be 94%.

Embodiment 10：

Other conditions are same as Example 1, and difference is in test while is passed through 1000 ppm SO2With 5% Steam, other conditions and test condition are identical with 1, and the sample is at 200 DEG C, 1000ppm SO2Steam with 5% is passed through NO removal efficiencies are 82%, Hg after 8 hours0Removal efficiency be 90%, Hg compared with Example 10Removal efficiency and NO removal efficiency It is all poor.1000ppm SO are removed at the same time2After 5% steam two hours, NO removal efficiencies are 88%, Hg0Removal efficiency be 94%

Pass through more visible, the catalyst performance when calcining heat is 500 DEG C of embodiment 1, embodiment 2, embodiment 3 Go out optimal low temperature denitration demercuration performance simultaneously.Pass through case study on implementation 1, embodiment 4, embodiment 5, embodiment 6, embodiment 7 It can be seen that work as Ce-Zr-MnO2Composite nanometer particle catalyst is 0.47 by Ce, Zr, Mn mol ratio：0.22：0.31 it is corresponding When the metal nitrate of quality is prepared, denitration demercuration performance is optimal simultaneously for low temperature.By embodiment 1, embodiment 8, embodiment 9th, embodiment 10 is more visible, steam and SO2To catalyst, denitration demercuration has certain inhibitory action to gas simultaneously, is removing Steam and SO2The performance of rear catalyst has been recovered.Catalyst is to steam and SO2With certain resistance.

In summary, the performance of denitration demercuration while the sample in the present invention has excellent at low temperature.It is prepared by sample Process is simple, and catalyst particle size is small, function admirable, has good application prospect.

Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art For, on the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (8)

1. one kind is used for low temperature purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Method for preparing catalyst, its feature exist In：Described Ce-Zr-MnO2Catalyst is to prepare to be formed using coprecipitation method to calcine system after co-precipitate under certain condition The CeO obtained2、ZrO2、MnO2Mixing nano-oxide, shared mol ratio is tri- kinds of elements of Ce, Zr, Mn in the catalyst 0.12-0.47:0.17-0.32:0.31-0.71。
2. the low temperature according to claim 1 that is used for purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Catalyst system Preparation Method, it is characterised in that：Specific preparation process is as follows：
(1) nitrate containing Mn, Ce and Zr is weighed respectively by Mn, Ce and Zr mol ratio, be added in deionized water stir in the lump To being completely dissolved, salting liquid is made, heating water bath is used in course of dissolution, deionized water dosage ensures each component in room temperature Nitrate dissolves；
(2) mixing salt solution obtained in step (1) is cooled to room temperature, while stirring, while adding a certain amount of ammoniacal liquor, makes Mn, Ce and Zr form mixed precipitation, after certain time stirring and aging, precipitation are filtered, after washing at a certain temperature Drying；
(3) step (2) dried sample is calcined under constituent of air, then grinds and be made under 100-300 DEG C of cryogenic conditions NO and Hg in high-efficient purification flue gas simultaneously0Ce-Zr-MnO2Composite nanometer particle catalyst sample.
3. the low temperature according to claim 2 that is used for purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Catalyst system Preparation Method, it is characterised in that：The temperature of heating water bath is 60-90 DEG C in the step (1).
4. the low temperature according to claim 2 that is used for purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Catalyst system Preparation Method, it is characterised in that：The pH value that ammoniacal liquor is added in the step (2) is 8-14, is added dropwise and continuously stirs, until mixed Close liquid pH value and reach 9-14, three metal ion species precipitation is complete.
5. the low temperature according to claim 2 that is used for purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Catalyst system Preparation Method, it is characterised in that：After precipitation by metallic ion is complete in the step (2), stop adding ammoniacal liquor, continuing mixing time is 2-4 hours, ageing time are 0.5-3 hours.
6. the low temperature according to claim 2 that is used for purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Catalyst system Preparation Method, it is characterised in that：Drying temperature is 70-120 DEG C in the step (2), and drying time is 6-12 hours.
7. the low temperature according to claim 2 that is used for purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Catalyst system Preparation Method, it is characterised in that：Calcining heat is 400-600 DEG C in the step (3), and calcination time is 4-5 hours, calcination process In, heating and cooling rate are 1-30 DEG C/min.
8. the low temperature according to claim 2 that is used for purifies NO and Hg in coal-fired flue-gas simultaneously0Ce-Zr-MnO2Catalyst system Preparation Method, it is characterised in that：Sample is 5-10nm nano particle after calcining and grinding in the step (3).
CN201710860828.8A 2017-09-21 2017-09-21 NO and Hg in coal-fired flue-gas is purified for low temperature simultaneously0Ce Zr MnO2Method for preparing catalyst CN107497419A (en)

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CN109908885A (en) * 2019-04-16 2019-06-21 中南大学 A kind of rhombohedron cerium oxide and its preparation method and application

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