CN106215949A - A kind of low-temperature selective catalytic reduction denitration catalyst and preparation method thereof - Google Patents
A kind of low-temperature selective catalytic reduction denitration catalyst and preparation method thereof Download PDFInfo
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- CN106215949A CN106215949A CN201610625594.4A CN201610625594A CN106215949A CN 106215949 A CN106215949 A CN 106215949A CN 201610625594 A CN201610625594 A CN 201610625594A CN 106215949 A CN106215949 A CN 106215949A
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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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
- 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
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Abstract
The present invention relates to a kind of low-temperature selective catalytic reduction denitration catalyst and preparation method thereof, this denitrating catalyst is made up of active component, cocatalyst and carrier three part, with multi-walled carbon nano-tubes as carrier, and FeOxFor cocatalyst, MnOxFor active component;Its preparation method for first carrying out nitric acid vapor process to carrier, then equi-volume impregnating is used to prepare catalyst, utilize nitric acid vapor modified multiwalled carbon nanotube, improve the hydrophilic of CNT, increase the specific surface area of catalyst simultaneously, promote dispersed at carrier surface of active component, and pass through MnOx、FeOxAnd the interaction between multi-walled carbon nano-tubes, improve the denitration activity of catalyst, with ammonia as reducing agent, temperature is all to show in the range of 180 240 DEG C to be well catalyzed activity;The advantages such as the present invention has operation and saves time simply, cost-effective, environmental protection, this catalyst can make the NOx in SCR denitration system efficient removal flue gas at low temperatures.
Description
[technical field]
The invention belongs to environmental conservation and environmental catalysis field, specifically a kind of low-temperature selective catalytic reduction denitration
Catalyst and preparation method thereof.
[background technology]
Along with economical growing, China consumes for coal and the problem of environmental pollution that brought is gone up increasingly
Rise.Based on the fire coal tail gas of nitrogen oxides (NOx) direct/indirectly discharge, be possible not only to cause acid rain, photochemical fog and
The environmental problems such as depletion of the ozone layer, moreover it is possible to the health of people is caused certain threat.Therefore, for NOx pair of the discharges such as fire coal
Destruction in air has become an environmental problem that can not be ignored, and efficiently controlling and reducing the discharge capacity of NOx becomes improvement
The emphasis of atmospheric pollution.
At present, ammine selectivity catalytic reduction technology (NH3-SCR) is most widely used gas denitrifying technology.Traditional vanadium
Base catalyst, its low temperature active is not enough.SCR method is current commercialization successful main flume denitration technology, and denitrating catalyst is again
It is the core of this technology, the high (300-of the most conventional commercial catalysts V2O5-WO3 (MoO3)/TiO2 active temperature windows
400 DEG C), easily affected by SO2 and dust and catalyst poisoning is occurred, next to that this catalyst reaches the temperature needed for optimum activity
Spending higher (300-400 DEG C), before therefore SCR device is often arranged in dedusting and desulfurizer, the dust in such flue gas can be right
Beds causes abrasion and blocking, reduces the service life of catalyst.Exploitation low-temperature SCR catalyst, allows denitrating system
After being placed in dust-removing desulfurating apparatus (< 200 DEG C) it is the important channel solving these problems.
Material with carbon element, as catalyst carrier, because having bigger serface, special pore passage structure, strong absorption property, and embodies
Going out the performance of excellence, wherein CNT is as a kind of special material with carbon element, have that mechanical strength is high, thermo-chemical stability high,
Confinement effect, and the physico-chemical property that good electric conductivity etc. is unique, utilize nitric acid vapor to improve the performance of carrier carbon nanotube,
Utilize the interaction between promoter, active component and CNT to make catalyst have good low-temperature SCR to live simultaneously
Property and stability obtain the low-temperature denitration catalyst of better performances.
[summary of the invention]
Present invention aim to solve above-mentioned deficiency and a kind of low-temperature selective catalytic reduction denitration catalysis is provided
The advantages such as agent, has operation and save time simply, cost-effective, environmental protection, and catalyst prepared by the present invention can make SCR denitration system exist
NOx in efficient removal flue gas under low temperature.
A kind of low-temperature selective catalytic reduction denitration catalyst of design, by catalytic active component, helps for achieving the above object
Catalyst and catalyst carrier three part are constituted, and catalyst activity component is MnOx, promoter is FeOx, and catalyst carrier is
Multi-walled carbon nano-tubes.
The preparation method of this low-temperature selective catalytic reduction denitration catalyst, comprises the steps:
1) first multi-walled carbon nano-tubes being carried out pretreatment, utilize nitric acid vapor to process, then wash, alcohol is washed, and dries,
Obtain pretreated multi-walled carbon nano-tubes;
2) by step 1) the pretreated multi-walled carbon nano-tubes of gained adds in the mixed solution of manganese acetate and ferric nitrate,
Supersound process 30-180min so that manganese acetate and ferric nitrate are dispersed in a solvent, incipient impregnation 10-48h;
3) by step 2) after the mixture of gained dries, tube furnace carries out nitrogen protection calcination processing, calcining heat
For 300-700 DEG C, heating rate 1-5 DEG C/min, it is incubated 1-7h, after cooling down to room temperature, i.e. obtains MnOx-FeOx/
MWCNTs low-temperature denitration catalyst.
Further, step 1) in, when utilizing nitric acid vapor to process, aqueous solution of nitric acid is positioned over high temperature hydro-thermal
Still, is positioned over multi-walled carbon nano-tubes sand core crucible top, then is placed in by crucible in high temperature water heating kettle, finally by high temperature water heating kettle
Being placed in baking oven, oven temperature is set to 150-180 DEG C.
Further, step 1) in, often processing the multi-walled carbon nano-tubes of 1g, the usage amount of nitric acid is 5-20ml.
Further, step 1) in, described drying, for using drying baker to be dried, is dried temperature and is 60-90 DEG C, drying time
For 6-24h.
Further, step 2) in, the solvent of described mixed solution is any one in deionized water and dehydrated alcohol.
Further, step 2) in, in manganese acetate, manganese is 0.05-0.2 with the mass percent of carbon in multi-walled carbon nano-tubes,
In ferric nitrate, ferrum is 0.4-2 with the mass percent of manganese in manganese acetate.
Compared with the existing technology, employing multi-walled carbon nano-tubes is carrier to the present invention, has bigger serface, stronger anti-corruption
The features such as erosion ability, unique pore structure, strong absorption property and mechanical strength are big, and it is dirty that environment does not results in secondary
Dye;Nitric acid vapor carries out process to CNT can improve its specific surface area, improves the surface nature of CNT, improves carbon
Nanotube dispersibility in water or ethanol equal solvent, and then make active component be dispersed in catalyst support surface;With biography
The system method ratio of nitric acid water bath processing CNT, the advantages such as the present invention has operation and saves time simply, cost-effective, environmental protection,
And catalyst prepared by the present invention can make the NOx in SCR denitration system efficient removal flue gas at low temperatures.
[accompanying drawing explanation]
Fig. 1 is the manganese iron axinite load carbon nano tube denitration catalyst that the embodiment of the present invention 1 gained has polymolecularity
Transmission electron microscope (TEM) photo.
[detailed description of the invention]
The present invention is with multi-walled carbon nano-tubes as carrier, FeOxFor cocatalyst, MnOxFor active component, it is thus achieved that receive based on carbon
The low-temperature denitration of flue gas catalyst of mitron.Its preparation method, for first carrier to carry out nitric acid vapor process, then uses equal-volume
Preparation catalyst, specifically includes following steps: 1) first multi-walled carbon nano-tubes is carried out pretreatment, utilizes nitric acid vapor
Processing, then wash, alcohol is washed, and dries, obtains pretreated multi-walled carbon nano-tubes;2) by step 1) after the pretreatment of gained
Multi-walled carbon nano-tubes add in the mixed solution of manganese acetate and ferric nitrate, supersound process 30-180min so that manganese acetate and nitre
Acid ferrum is dispersed in a solvent, incipient impregnation 10-48h;3) by step 2) after the mixture of gained dries, in tube furnace
Carrying out nitrogen protection calcination processing, calcining heat is 300-700 DEG C, heating rate 1-5 DEG C/min, is incubated 1-7h, cooling down
To room temperature, i.e. obtain MnOx-FeOx/ MWCNTs low-temperature denitration catalyst.
Wherein, step 1) in, often processing the multi-walled carbon nano-tubes of 1g, the usage amount of nitric acid is 5-20ml, in this step
Drying as using drying baker to be dried, dry temperature and be 60-90 DEG C, drying time is 6-24h;Step 2) in, mixed solution molten
Agent is any one in deionized water and dehydrated alcohol, and in manganese acetate, manganese with the mass percent of carbon in multi-walled carbon nano-tubes is
0.05-0.2, in ferric nitrate, ferrum is 0.4-2 with the mass percent of manganese in manganese acetate.
The present invention utilizes the feature of the bigger serface of CNT, recycles nitric acid vapor modified multiwalled carbon nanotube,
Specific surface area can be increased further, improve the active substance degree of scatter at carrier surface, improve the hydrophilic of CNT,
Increase the specific surface area of catalyst simultaneously, promote dispersed at carrier surface of active component, owing to the oxidisability of ferrum is fine,
The introducing of Fe can effectively be catalyzed NO and be converted into NO2, the synergism between MnOx, FeOx and CNT, passes through simultaneously
MnOx、FeOxAnd the interaction between multi-walled carbon nano-tubes, improve the denitration activity of catalyst;With ammonia as reducing agent, temperature
Spend all to show in the range of being 180-240 DEG C and be well catalyzed activity.
The present invention is made further explained below below by specific embodiment:
Embodiment 1
5ml aqueous solution of nitric acid (3mol/L) is positioned over the high temperature water heating kettle of 50ml size, and the CNT of about 1g is put
Being placed in sand core crucible top, be positioned over by crucible in high temperature water heating kettle, be finally placed in baking oven by water heating kettle, oven temperature is arranged
In 180 DEG C, after 5h, water heating kettle is cooled to room temperature, takes out CNT, and through washing, alcohol is washed, and dries 5h, obtains modification for 80 DEG C
After multi-walled carbon nano-tubes.Then equi-volume impregnating is used to prepare MnOx-FeOx/MWCNTs catalyst. weigh 0.31g acetic acid
Manganese and 0.433g Fe(NO3)39H2O prepare the solution of 40ml respectively, join MWCNTs after pretreatment, ultrasonic disperse 1h,
Room temperature immersion about 12h. mixture is dried in 80 DEG C, finally gives in 400 DEG C of roasting 2h. in tube furnace under nitrogen atmosphere
Mn/C is 0.1, and the ratio of Fe/Mn is the denitrating catalyst of 0.6.
Embodiment 2
10ml aqueous solution of nitric acid (3mol/L) is positioned over the high temperature water heating kettle of 50ml size, and the CNT of about 1g is put
Being placed in sand core crucible top, be positioned over by crucible in high temperature water heating kettle, be finally placed in baking oven by water heating kettle, oven temperature is arranged
In 150 DEG C, after 5h, water heating kettle is cooled to room temperature, takes out CNT, and through washing, alcohol is washed, and dries 5h, obtains modification for 80 DEG C
After multi-walled carbon nano-tubes.Then equi-volume impregnating is used to prepare MnOx-FeOx/MWCNTs catalyst. weigh 0.155g second
Acid manganese and 0.361g Fe(NO3)39H2O prepare the solution of 40ml respectively, join MWCNTs after pretreatment, ultrasonic disperse
1h, room temperature immersion about 12h. mixture is dried in 80 DEG C, final in 400 DEG C of roasting 2h. under nitrogen atmosphere in tube furnace
Obtaining Mn/C is 0.05, and the ratio of Fe/Mn is the denitrating catalyst of 1.
Embodiment 3
15ml aqueous solution of nitric acid (3mol/L) is positioned over the high temperature water heating kettle of 50ml size, and the CNT of about 1g is put
Being placed in sand core crucible top, be positioned over by crucible in high temperature water heating kettle, be finally placed in baking oven by water heating kettle, oven temperature is arranged
In 180 DEG C, after 5h, water heating kettle is cooled to room temperature, takes out CNT, and through washing, alcohol is washed, and dries 5h, obtains modification for 80 DEG C
After multi-walled carbon nano-tubes.Then equi-volume impregnating is used to prepare MnOx-FeOx/MWCNTs catalyst. weigh 0.465g second
Acid manganese and 2.164g Fe(NO3)39H2O prepare the solution of 40ml respectively, join MWCNTs after pretreatment, ultrasonic disperse
1h, room temperature immersion about 12h. mixture is dried in 80 DEG C, final in 500 DEG C of roasting 2h. under nitrogen atmosphere in tube furnace
Obtaining Mn/C is 0.15, and the ratio of Fe/Mn is the denitrating catalyst of 2.
Embodiment 4
20ml aqueous solution of nitric acid (3mol/L) is positioned over the high temperature water heating kettle of 50ml size, and the CNT of about 1g is put
Being placed in sand core crucible top, be positioned over by crucible in high temperature water heating kettle, be finally placed in baking oven by water heating kettle, oven temperature is arranged
In 160 DEG C, after 5h, water heating kettle is cooled to room temperature, takes out CNT, and through washing, alcohol is washed, and dries 5h, obtains modification for 80 DEG C
After multi-walled carbon nano-tubes.Then equi-volume impregnating is used to prepare MnOx-FeOx/MWCNTs catalyst. weigh 0.465g second
Acid manganese and 0.649g Fe(NO3)39H2O prepare the solution of 40ml respectively, join MWCNTs after pretreatment, ultrasonic disperse
2h, room temperature immersion about 12h. mixture is dried in 80 DEG C, final in 400 DEG C of roasting 2h. under nitrogen atmosphere in tube furnace
Obtaining Mn/C is 0.15, and the ratio of Fe/Mn is the denitrating catalyst of 0.6.
Embodiment 5
10ml aqueous solution of nitric acid (3mol/L) is positioned over the high temperature water heating kettle of 50ml size, and the CNT of about 1g is put
Being placed in sand core crucible top, be positioned over by crucible in high temperature water heating kettle, be finally placed in baking oven by water heating kettle, oven temperature is arranged
In 180 DEG C, after 5h, water heating kettle is cooled to room temperature, takes out CNT, and through washing, alcohol is washed, and dries 5h, obtains modification for 80 DEG C
After multi-walled carbon nano-tubes.Then equi-volume impregnating is used to prepare MnOx-FeOx/MWCNTs catalyst. weigh 0.31g acetic acid
Manganese and 0.289g Fe(NO3)39H2O prepare the solution of 40ml respectively, are slowly added to MWCNTs after pretreatment, ultrasonic point
Dissipating 2h, room temperature immersion about 12h. mixture is dried in 80 DEG C, in 500 DEG C of roasting 2h under nitrogen atmosphere in tube furnace.?
Obtaining Mn/C eventually is 0.1, and the ratio of Fe/Mn is the denitrating catalyst of 0.4.
The present invention is not limited by above-mentioned embodiment, other any spirit without departing from the present invention and principle
Lower made change, modify, substitute, combine, simplify, all should be the substitute mode of equivalence, be included in the protection model of the present invention
Within enclosing.
Claims (7)
1. a low-temperature selective catalytic reduction denitration catalyst, it is characterised in that: by catalytic active component, promoter with urge
Agent carrier three part is constituted, and catalyst activity component is MnOx, promoter is FeOx, and catalyst carrier is multi-wall carbon nano-tube
Pipe.
2. the preparation method of low-temperature selective catalytic reduction denitration catalyst as claimed in claim 1, it is characterised in that include
Following steps:
1) first multi-walled carbon nano-tubes being carried out pretreatment, utilize nitric acid vapor to process, then wash, alcohol is washed, and dries, obtains
Pretreated multi-walled carbon nano-tubes;
2) by step 1) the pretreated multi-walled carbon nano-tubes of gained adds in the mixed solution of manganese acetate and ferric nitrate, ultrasonic
Process 30-180min so that manganese acetate and ferric nitrate are dispersed in a solvent, incipient impregnation 10-48h;
3) by step 2) after the mixture of gained dries, tube furnace carries out nitrogen protection calcination processing, calcining heat is
300-700 DEG C, heating rate 1-5 DEG C/min, it is incubated 1-7h, after cooling down to room temperature, i.e. obtains MnOx-FeOx/MWCNTs
Low-temperature denitration catalyst.
3. preparation method as claimed in claim 2, it is characterised in that: step 1) in, when utilizing nitric acid vapor to process, will
Aqueous solution of nitric acid is positioned over high temperature water heating kettle, multi-walled carbon nano-tubes is positioned over sand core crucible top, then crucible is placed in high temperature
In water heating kettle, being finally placed in baking oven by high temperature water heating kettle, oven temperature is set to 150-180 DEG C.
4. preparation method as claimed in claim 2, it is characterised in that: step 1) in, often process the multi-walled carbon nano-tubes of 1g, nitre
The usage amount of acid is 5-20ml.
5. preparation method as claimed in claim 2, it is characterised in that: step 1) in, described drying is dried for employing drying baker,
Drying temperature and be 60-90 DEG C, drying time is 6-24h.
6. preparation method as claimed in claim 2, it is characterised in that: step 2) in, the solvent of described mixed solution for go from
Any one in sub-water and dehydrated alcohol.
7. preparation method as claimed in claim 2, it is characterised in that: step 2) in, manganese and multi-walled carbon nano-tubes in manganese acetate
The mass percent of middle carbon is 0.05-0.2, and in ferric nitrate, ferrum is 0.4-2 with the mass percent of manganese in manganese acetate.
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CN110544592A (en) * | 2019-09-26 | 2019-12-06 | 北京航空航天大学 | Electrochemical energy storage electrode plate without metal current collector |
CN111773919A (en) * | 2020-06-11 | 2020-10-16 | 山东迅达化工集团有限公司 | Fine purification agent for NOx-containing gas flow and application thereof |
CN113649037A (en) * | 2021-08-31 | 2021-11-16 | 武汉科技大学 | Catalyst suitable for low-temperature catalytic oxidation of mercury in oxygen-rich combustion flue gas 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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CN108493432A (en) * | 2018-05-16 | 2018-09-04 | 杭州电子科技大学 | A kind of preparation method and application of multi-walled carbon nanotube/silicon and silica/carbon composite nano-material |
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CN113649037A (en) * | 2021-08-31 | 2021-11-16 | 武汉科技大学 | Catalyst suitable for low-temperature catalytic oxidation of mercury in oxygen-rich combustion flue gas 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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Application publication date: 20161214 |