CN107519859A - Purify the Ce Zr MnO of NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Method for preparing catalyst - Google Patents
Purify the Ce Zr MnO of NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Method for preparing catalyst Download PDFInfo
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- CN107519859A CN107519859A CN201710859959.4A CN201710859959A CN107519859A CN 107519859 A CN107519859 A CN 107519859A CN 201710859959 A CN201710859959 A CN 201710859959A CN 107519859 A CN107519859 A CN 107519859A
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- 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
- 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
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2258/0283—Flue gases
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The present invention provides a kind of Ce Zr MnO for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Method 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 the sample of low temperature while efficient removal NO and VOCs.The sample under cryogenic, has more excellent purification efficiency to NO, at the same can be in efficient removal waste gas VOCs.For SO2And H2O has certain tolerance.This method process conditions are simple, and catalyst performance is excellent, workable, are adapted to large-scale production, have very high practical value.
Description
Technical field
The present invention relates to environmental protection technical field, particularly relates to one kind and is used for low temperature while purifies NO in coal-fired flue-gas
With VOCs Ce-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 volatile organic matter (VOCs), both pollutants not only seriously endangered ecological ring
Border, and bring serious threat to the health of people.And the nitrogen oxides more than 90% in waste gas is made up of NO.
Therefore there is the NO in efficient removal flue gas and VOCs very important environment and health to be 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 to VOCs's present in flue gas there is certain removing to act on, but imitate
Rate is not high, and this is primarily due to SCR catalyst in 300 DEG C of -400 DEG C of denitration efficiency highests.But the catalyst used at present is more
Just there is preferably de- VOCs efficiency in high temperature.But in higher temperature, the efficiency of denitration is not ideal enough, flue gas
In SO2It is also easier to change into SO under catalyst action3.Therefore, low temperature removes the NO and VOCs in coal combustion exhaust simultaneously
With good social value and market application foreground, thus develop can be high under the conditions of a kind of low temperature (100-300 DEG C)
It is significant to imitate the de- VOCs catalyst samples of denitration.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of NO and VOCs in coal-fired flue-gas is purified for low temperature simultaneously
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 is 0.10-0.50:0.15-0.35:0.30-0.75.
The specific preparation process of this method is as follows：
(1) nitrate containing Mn, Ce and Zr is weighed respectively by Mn, Ce and Zr mol ratio, add in deionized water stir in the lump
Mix to being completely dissolved, salting liquid is made, heating water bath is used in course of dissolution, going deionized water dosage to ensure will in room temperature
Each component nitrate dissolves；
(2) mixing salt solution obtained in step (1) is cooled to room temperature, while stirring, while adding a certain amount of ammonia
Water, Mn, Ce and Zr is formed mixed precipitation, after the stirring and aging of certain time, precipitation is filtered, one after washing
Determine to dry at temperature；
(3) sample after step (2) is dried is calcined under constituent of air, then grinds and 100-300 DEG C of low temperature bar is made
Under part simultaneously in high-efficient purification flue gas NO and VOCs Ce-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
8-10, three metal ion species precipitation are complete.After precipitation by metallic ion is complete, stop adding ammoniacal liquor, continuation mixing time is 2-4
Hour, ageing time is 0.5-2 hours.
Drying temperature is 70-100 DEG C in step (2), 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 1-10nm nano particle after calcining and grinding in step (3).
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 prepare mixed sediment, mixed precipitation is then obtained under low temperature high-efficient purification flue gas simultaneously in 400-600 DEG C of calcining
Middle NO and VOCs Ce-Zr-MnO2Composite nanometer particle catalyst sample.The sample under the conditions of low temperature (100-300 DEG C),
There is high purification efficiency to VOCs, 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 Ce-Zr-MnO for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Catalyst system
Preparation Method.
Embodiment 1：
Ce, Zr, Mn mol ratio are weighed as 0.45：0.20：The metal nitrate of 0.35 respective quality, is added in the lump
In deionized water, 90 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,
A certain amount of ammoniacal liquor is added dropwise simultaneously on one side, until pH of mixed reaches 10.Continue aging 2 hours after stirring 2 hours.Thereafter will be heavy
Form sediment and filter, 100 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 10 DEG C/min speed, perseverance
Temperature naturally cools to room temperature after 4 hours.The Ce- of NO and VOCs in high-efficient purification flue gas simultaneously is made under cryogenic in grinding
Zr-MnO2Composite nanometer particle catalyst sample.
The sample that will be obtained in embodiment 1, it is experimental subjects to take 0.600g, using nitrogen as Balance Air, at 100 DEG C -300
DEG C temperature range in, air speed 40000h-1、CNO=1000ppm, CNH3=1000ppm, oxygen concentration=10%, CVOCs=
Under the conditions of 1000ppm, at 260 DEG C, NO removal efficiencies are that 90%, VOCs removal efficiency reaches 90%.
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 270 DEG C, NO removal efficiencies are that 88%, VOCs removal efficiency reaches 90%.With the phase of embodiment 1
Than the temperature rise that de- VOCs efficiency reaches 90%, denitration efficiency is declined slightly.
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 290 DEG C, NO removal efficiencies are that 80%, VOCs removal efficiency reaches 90%.With the phase of embodiment 1
Than the temperature rise that de- VOCs efficiency reaches 90%, denitration efficiency is decreased obviously.
Embodiment 4：
Other conditions are same as Example 1, and difference is that Ce, Zr, Mn mol ratio are 0.32：0.26：0.44, its
His condition and test condition are identical with 1, and for the sample at 270 DEG C, NO removal efficiencies are that 89%, VOCs removal efficiency reaches
90%.The temperature rise that VOCs efficiency reaches 90% is taken off compared with Example 1, and denitration efficiency is declined slightly.
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 260 DEG C, NO removal efficiencies are that 88%, VOCs removal efficiency reaches
90%.Temperature is identical when de- VOCs efficiency reaches 90% compared with Example 1, and denitration efficiency has declined.
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 at 270 DEG C, the removal efficiency that NO removal efficiencies are 90%, VOCs reaches the sample
90%, temperature rise when VOCs efficiency reaches 90% is taken off compared with Example 1, and denitration efficiency is identical.
Embodiment 7：
Other conditions are same as Example 1, and difference is that Ce, Zr, Mn mol ratio are 0.10：0.18：0.72, its
His condition and test condition are identical with 1, and for the sample at 280 DEG C, NO removal efficiencies are that 89%, VOCs removal efficiency is
90%.VOCs efficiency is taken off compared with Example 1 and reaches the rise of 90% temperature, while denitration efficiency has also 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 260 DEG C, NO removal efficiencies are 86%, VOCs's after 5% steam is passed through 10 hours
Removal efficiency is 87%, and VOCs removal efficiency and NO removal efficiency have declined compared with Example 1.Removing 5% steam two
After hour, the removal efficiency that NO removal efficiencies are 89%, VOCs is 89%, and removal efficiency has all recovered.
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 260 DEG C, 1000ppm SO2NO removal efficiencies are 85% after being passed through 10 hours,
VOCs removal efficiency is 87%, and VOCs removal efficiency and NO removal efficiency have all declined compared with Example 1.Removing
1000ppm SO2After two hours, the removal efficiency that NO removal efficiencies are 88%, VOCs is 89%, and removal efficiency has all recovered.
Embodiment 10：
Other conditions are same as Example 1, and difference is in test while is passed through 1000ppm SO2With 5%
Steam, other conditions and test condition are identical with 1, and the sample is at 260 DEG C, 1000 ppm SO2Steam with 5% leads to
The removal efficiency that NO removal efficiencies are 82%, VOCs after entering 10 hours is 83%, compared with Example 1 VOCs removal efficiency and NO
Removal efficiency is all decreased obviously.1000 ppm SO are removed at the same time2After 5% steam two hours, NO removal efficiencies are 88%,
VOCs removal efficiency is 87%, and removal efficiency has all recovered.
By embodiment 1, embodiment 2, embodiment 3 it is more visible, when calcining heat be 500 DEG C when catalyst simultaneously
The performance that denitration takes off VOCs is optimal.By embodiment 1, embodiment 4, embodiment 5, embodiment 6, embodiment 7 it is more visible,
Work as Ce-Zr-MnO2Composite nanometer particle catalyst is 0.45 by Ce, Zr, Mn mol ratio：0.20：The gold of 0.35 respective quality
When genus nitrobacter is prepared, it is optimal that low temperature denitration simultaneously takes off VOCs performances.By embodiment 1, embodiment 8, embodiment 9, implementation
Example 10 is more visible, steam and SO2Gas takes off VOCs to catalyst denitration simultaneously has certain inhibitory action, is removing water
Vapour and SO2The performance of rear catalyst has been recovered.Catalyst is to steam and SO2With certain resistance.
In summary, denitration takes off VOCs's while the sample in the present invention has excellent under low temperature (100-300 DEG C)
Performance.Sample preparation is simple, catalyst pellets 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
Also it should be regarded as protection scope of the present invention.
Claims (8)
- A kind of 1. Ce-Zr-MnO for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Method for preparing catalyst, its feature It is：The 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 0.10- to tri- kinds of elements of Ce, Zr, Mn in the catalyst 0.50:0.15-0.35:0.30-0.75。
- 2. the Ce-Zr-MnO according to claim 1 for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Catalyst Preparation method, it is characterised in that：Specific preparation process is as follows：(1) weigh the nitrate containing Mn, Ce and Zr respectively by Mn, Ce and Zr mol ratio, in the lump add deionized water in stir to It is completely dissolved, salting liquid is made, uses heating water bath in course of dissolution, goes deionized water dosage to ensure 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 the stirring and aging of certain time, precipitation are filtered, in certain temperature after washing Lower drying；(3) sample after step (2) is dried is calcined under constituent of air, is then ground and is made under 100-300 DEG C of cryogenic conditions Simultaneously in high-efficient purification flue gas NO and VOCs Ce-Zr-MnO2Composite nanometer particle catalyst sample.
- 3. the Ce-Zr-MnO according to claim 2 for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Catalyst Preparation method, it is characterised in that：The temperature of heating water bath is 60-90 DEG C in the step (1).
- 4. the Ce-Zr-MnO according to claim 2 for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Catalyst 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 liquor pH value reaches 8-10, and three metal ion species precipitation is complete.
- 5. the Ce-Zr-MnO according to claim 2 for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Catalyst Preparation method, it is characterised in that：After precipitation by metallic ion is complete in the step (2), stops adding ammoniacal liquor, continue mixing time For 2-4 hours, ageing time is 0.5-2 hours.
- 6. the Ce-Zr-MnO according to claim 2 for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Catalyst Preparation method, it is characterised in that：Drying temperature is 70-100 DEG C in the step (2), and drying time is 6-12 hours.
- 7. the Ce-Zr-MnO according to claim 2 for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Catalyst 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, calcined Cheng Zhong, heating and cooling rate are 1-30 DEG C/min.
- 8. the Ce-Zr-MnO according to claim 2 for purifying NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Catalyst Preparation method, it is characterised in that：Sample is 1-10nm nano particle after calcining and grinding in the step (3).
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| CN201710859959.4A CN107519859A (en) | 2017-09-21 | 2017-09-21 | Purify the Ce Zr MnO of NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Method for preparing catalyst |
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| CN201710859959.4A CN107519859A (en) | 2017-09-21 | 2017-09-21 | Purify the Ce Zr MnO of NO and VOCs in coal-fired flue-gas simultaneously for low temperature2Method for preparing catalyst |
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Cited By (3)
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| CN112264027A (en) * | 2020-10-27 | 2021-01-26 | 南京工业大学 | Copper-cobalt-cerium composite oxide catalytic combustion catalyst and preparation method and application thereof |
| CN114160147A (en) * | 2021-11-29 | 2022-03-11 | 华南理工大学 | Composite oxide catalyst for synchronously removing VOCs and NOx in sulfur-containing flue gas and preparation method and application thereof |
| CN114768794A (en) * | 2022-04-27 | 2022-07-22 | 华南理工大学 | Composite manganese oxide catalyst for synchronously removing VOCs and NOx in medium-low temperature flue gas and preparation method and application thereof |
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Application publication date: 20171229 |
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