CN107029736A - A kind of Fe M/CNTs denitrating catalysts, preparation method and its application in ammine selectivity catalytic reduction nitrous oxides - Google Patents
A kind of Fe M/CNTs denitrating catalysts, preparation method and its application in ammine selectivity catalytic reduction nitrous oxides Download PDFInfo
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- CN107029736A CN107029736A CN201710389255.5A CN201710389255A CN107029736A CN 107029736 A CN107029736 A CN 107029736A CN 201710389255 A CN201710389255 A CN 201710389255A CN 107029736 A CN107029736 A CN 107029736A
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- 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
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/881—Molybdenum and iron
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- 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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- 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
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- 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
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
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Abstract
The invention discloses a kind of Fe M/CNTs denitrating catalysts, preparation method and its application in ammine selectivity catalytic reduction nitrous oxides, belong to environmental catalysis purification techniques field.Catalyst is prepared using the high infusion process of repeatability simple to operate, that is, chooses suitable source of iron and the carbon nano tube surface of molybdenum source or tungsten source homogeneous impregnation after acid-treated, dries, denitrating catalyst is obtained after roasting.Fe M/CNTs denitrating catalysts prepared by the present invention, surface-active particles decentralization is high, and middle low-temperature catalytic activity is high, operable temperature window is wide：There is more than 90% NO in 250 400 DEG CxConversion ratio, N2Selectivity maintains more than 85%, and anti-sulfureous in flue gas oxide and water slug ability are strong, it is adaptable to the stationary source catalytic purification of nitroxide device by representative of coal-fired plant flue gas, with wide prospects for commercial application.
Description
Technical field
The invention belongs to environmental catalysis purification techniques field, be related to a kind of Fe-M/CNTs denitrations agent, preparation method and its
Application in ammine selectivity catalytic reduction nitrous oxides technology.
Background technology
Nitrogen oxides is mainly derived from coal-fired plant flue gas and automotive emission, and its conversion in an atmosphere can be caused
A series of problem of environmental pollutions such as haze, photochemical fog, acid rain, threaten health.In numerous nitrogen oxides removal technologies
In, ammine selectivity catalytic reduction nitrous oxides (NH3- SCR) technology has denitration efficiency high, and secondary pollution is small, and reaction efficiency is low
It is widely used etc. advantage.Because it is possible to prevente effectively from the impact of high concentration oxysulfide and dust, extension catalyst use the longevity
Life, the mode of deploying to ensure effective monitoring and control of illegal activities of low grey section is used more and more, and this requires that catalyst has good middle low temperature active, and possesses
Low concentration oxysulfide and steam impact capacity in anti-flue gas.The extensive V of commercial2O5-WO3(MoO3)/TiO2Class is catalyzed
Low-temperature catalyzed effect is undesirable in agent, and V2O5With certain bio-toxicity, therefore, exploitation has good middle low-temperature denitration effect
Environmentally friendly catalyst turn into study hotspot.
Ferriferous oxide be always SCR catalyst research field it is more concerned compared with a class catalytic active center, its originate
Extensively, green is cheap, but catalytic effect is not very good in middle low-temperature range section.In order to meet at this stage in
The need for low-temperature SCR catalyst, increasing researcher lifts the low temperature active of ferrum-based catalyst using auxiliary agent, while
Sight is focused on to the application of novel catalyst carrier.Wherein, " the super fibre of the one-dimensional hollow tubular structure with high-sequential
Dimension " CNT (CNTs) receives much concern.Carbon nanotube chemical property is stable to have larger specific surface area, its special curling
Structure makes its surface there is more electronics movement, and with certain confinement effect, these properties may advantageously facilitate activity
Interaction between center site and carrier, promotes the progress of catalytic reaction process.Qu etc. uses organic solvent deposit and leaching
Fe prepared by stain method2O3/ CNTs catalyst (CN103506121A；Zhenping Qu,Lei Miao,et al.
Chem.Commun.2015,51:956-958) show good low-temperature catalytic activity：225-300 DEG C has more than 90%
NOxConversion ratio, but the catalyst is in anti-SO2Impact capacity is not good, and operable temperature window is narrower.Added into catalyst
Certain auxiliary agent can be effectively improved catalyst surface property, wherein molybdenum oxide (MoOx) and tungsten oxide (WOx) regulation is urged
Agent structure, the chemical property for strengthening catalyst surface is largely effective.Hongliang Zhang et al. (Hongliang
Zhang, Changjin Tang, et al.Micropor. Mesopor.Mat.2012,151,44-55) by MoOxIt is doped in
Fe/SBA-15 catalyst surfaces, it is found that Mo addition is highly beneficial to the meso-hole structure of catalyst formation high-sequential, still
The denitrating catalyst is less efficient, 400 DEG C only reach 60% NOxConversion ratio；(the Jixing Liu, et such as Jixing Liu
al.Appl.Catal. B:Environ.2016) by MoOxIt is doped in Fe/Beta catalyst, and adds a certain amount of CeO2System
For the MoFe/Beta@CeO with nucleocapsid pattern2Catalyst, the denitration efficiency at 250-500 DEG C with more than 90%, N2Choosing
Selecting property is up to more than 90%；But its preparation process is complicated, and organic solvent is needed to use, easily cause pollution, and this seed nucleus
Shell structure stability is poor, easily cave in.Also there is research using tungsten oxide (WOx) modification regulation and control are carried out to ferrum-based catalyst,
(Hui Wang, Qu Zhenping, the et al.Environ. Sci.＆Techno.2016,50,13511- such as HuiWang
13519) the high iron of heat endurance-tungsten composite oxide catalysts are prepared using coprecipitation, had at 250-400 DEG C
More than 90% denitration efficiency and N2Selectivity.
On having in Chinese patent CN105107514A for the Fe-Mo composite oxide catalysts applied in SCR technology
Relevant report is crossed, but the invention uses more complicated sol-gel process, and only under relatively low space velocities
(4000h-1)NOxConversion ratio is good；What CN105214679A disclosed prepared by a kind of use coprecipitation contains 6 groups of Fe, Mo etc.
The catalyst divided, although the catalyst possesses more than 80% NO at 150 DEG CxConversion ratio, but make during preparation
With organic silicon solvent, the use of organic solvent can not only improve the preparation cost of catalyst, but also can cause dirt to environment
Dye.Chinese patent CN104941655A and CN103877986A discloses the Fe-W composite oxides prepared using coprecipitation
Catalyst, they are in 250-400 DEG C of denitration efficiency and N2Selectivity reaches more than 90%, but the system of composite oxide catalysts
Standby raw material usage amount is big, without economic benefit.
At present, on using carbon nanotube loaded iron and molybdenum or iron and tungsten dual-component catalyst, and catalyst is effectively widened
Denitration action pane, the patent and research report for improving catalyst sulfur resistive oxide impact capacity is also seldom.
The content of the invention
In order to meet current NH3Centering cryogenic effect in-SCR fields is good, resist oxysulfide with steam impact capacity by force
The demand of catalyst, the present invention provides a kind of carbon nanotube loaded iron and molybdenum or iron and tungsten two-component denitrating catalyst, preparation side
Method, can be applied to stationary source denitrating flue gas.
A kind of Fe-M/CNTs denitrating catalysts, wherein M be Mo or W, using ferriferous oxide as active component, using with
The CNT of orderly hollow tubular is used as coagent as carrier, addition metal molybdenum or tungsten；Active component content is 20-
40wt%.
A kind of preparation method of Fe-M/CNTs denitrating catalysts, using infusion process simple to operation, it is to avoid using having
The pollution that machine solvent bank comes, step is as follows：
Choose the source of iron, molybdenum source and the solid acid that are adapted to or source of iron, tungsten source and solid acid are uniformly mixed in deionized water
The mol ratio in obtained mixed solution, wherein source of iron and molybdenum source/tungsten source is 10:1~2:1, the quality in solid acid and molybdenum source/tungsten source
Than for 1:1~1:2；By the mixed solution homogeneous impregnation after the processing of strong oxidizing property concentrated acid by CNT (CNTs) table
Face, is dried, and is calcined 3-5h, and sintering temperature is 350-450 DEG C, obtains Fe-M/CNTs denitrating catalysts.
Source of iron described in step is mixed above for one or both of ferric sulfate, iron chloride or ferric acetate.
Molybdenum source described in step is mixed above for one or both of ammonium molybdate, ammonium dimolybdate, ammonium heptamolybdate；Tungsten source
For ammonium metatungstate.
Solid acid described in step is oxalic acid or citric acid.
A kind of Fe-M/CNTs, wherein M are Mo or W, denitrating catalyst answering in ammonia selective catalysis nitrogen oxides reduction
With material mixed gas volume proportioning is 400-1000ppm NH3, 400-1000ppm NO, 3-10vol.%O2, 100-400ppm
SO2, 5-10vol.%H2O, gas overall flow rate is 200-400mL/min, active testing continuous operation；Operation temperature is
100-450 DEG C, the consumption of denitrating catalyst is 0.05-0.3g, and air speed is 40 000-100 000h-1。
The beneficial effects of the invention are as follows：Operating method is simple, and lower cost is reproducible.Used CNTs carriers
Specific surface area is big, and in order, itself unique electronic property makes active particle and there is stronger phase interaction between it pore passage structure
With the high degree of dispersion beneficial to active component and being stabilized inside duct；Active component content is 20-40wt%, effectively
Reduce the use of catalyst raw material, economy.The carbon nanotube loaded iron prepared and molybdenum or iron and tungsten two-component denitration
Catalyst has excellent middle low-temperature denitration performance, and more than 90% denitration efficiency and holding 85% are reached in 250-400 DEG C
N above2Selectivity, anti-sulfureous in flue gas oxide is strong with steam impact capacity, and oxygen concentration in high-speed and flue gas is changed
It is insensitive, with good prospects for commercial application.
Brief description of the drawings
Fig. 1 be by abscissa of reaction temperature, NOxConversion ratio is surveyed for the SCR activity of the different denitrating catalysts of ordinate
Attempt.
Fig. 2 is the XRD spectrum of Fe-Mo/CNTs denitrating catalysts.
Embodiment
Below in conjunction with accompanying drawing and technical scheme, the embodiment of the present invention is further illustrated.
Embodiment 1
Carbon nano-tube material acid treatment：3g CNTs are added in 150mL concentrated acid solution, wherein concentrated nitric acid and concentrated sulfuric acid body
Product is than being 1:After 1, ultrasonic disperse 60min, condensing reflux 5h, is diluted and cooled down with deionized water in 110 DEG C of oil bath pans, to be washed
When washing mixed solution pH=6~7, suction filtration, and be put into 80 DEG C of baking ovens and dry, grind standby.
Embodiment 2
Weigh a small amount of H of the CNTs obtained in 0.6g embodiments 12O infiltrates；Weigh 2.4g ferric nitrates, the molybdic acids of 0.1 g seven
Ammonium, 0.1g citric acids are dissolved in 10mL H2In O after solution is well mixed, by solution homogeneous impregnation to the CNTs surfaces moistened,
Stir to moisture and volatilize in 40 DEG C of water-baths, 12h is dried in 80 DEG C of baking ovens, finally by the sample of drying in 400 DEG C of Muffle furnace
Lower roasting 3h, is made carbon nanotube loaded iron and molybdenum dual-component catalyst A.Other conditions are constant, and lemon is replaced using 0.1g oxalic acid
Lemon acid, prepares carbon nanotube loaded iron and molybdenum dual-component catalyst B.
Embodiment 3
According to the A catalyst methods of the invention of embodiment 2,0.1g ammonium heptamolybdates, system are replaced using 0.2g ammonium heptamolybdates
It is standby to obtain carbon nanotube loaded iron and molybdenum dual-component catalyst C；0.1g ammonium heptamolybdates are replaced using 0.6g ammonium heptamolybdates, carbon is obtained
Nano tube supported iron and molybdenum dual-component catalyst D.
Embodiment 4
Weigh a small amount of H of the CNTs obtained in 0.6g embodiments 12O infiltrates；Weigh 2.4g ferric nitrates, 1.5g metatungstic acids
Ammonium, 0.1g citric acids are dissolved in 10mL H2In O after solution is well mixed, by solution homogeneous impregnation to the CNTs surfaces moistened,
Stir to moisture and volatilize in 40 DEG C of water-baths, 12h is dried in 80 DEG C of baking ovens, finally by the sample of drying in 400 DEG C of Muffle furnace
Lower roasting 3h, is made carbon nanotube loaded iron and tungsten dual-component catalyst.
Embodiment 5
With catalyst A-D made from embodiment 2-3 catalytic activity survey is carried out in homemade miniature fixed bed point reactor
Examination, reactor is internal diameter 6mm glass U-tube, and loaded catalyst is 0.3g, unstripped gas composition：1000ppm NH3,
1000ppm NO, 3vol%O2, Ar is Balance Air, and gas flow rate is 300 mL/min, after reaction 30min is stable in product gas
NOxThere is NO-NO2-NOxAnalyzer (42i-HL, Thermo Fisher Scientific) carries out on-line checking.Reaction result
As shown in Figure 1.
Embodiment 6
Using the catalyst C of the invention of embodiment 2, the type catalyst is investigated on micro fixed-bed reactor for anti-cigarette
The ability of gas sulphur oxide impact.Reaction test condition be the same as Example 5 is similar, and difference is after stable reaction 60min, to anti-
Answer and 200ppm SO are added in atmosphere2Follow-on test 12h, observes catalyst n O afterwardsxConversion ratio situation of change, as a result such as the institute of table 1
Show.Under the conditions of relatively low reaction temperature (<250 DEG C) catalyst activity reduction rate is only 3.3%, hot conditions (>250℃)
Lower NOxConversion ratio is kept approximately constant.
The catalyst sulfur resistive oxide impact capacity performance evaluation of table 1
Embodiment 7
Using catalyst C, the SCR catalytic performance test be the same as Example 5 of the invention of embodiment 2, the difference is that changing anticaltalysis
Agent consumption 0.05-0.3g, correspondence 96000-46000h-1Air speed, is 300 DEG C by the temperature of catalyst reaction bed, test is urged
Agent C NOxConversion ratio, as a result as shown in table 2.
The anti-high-speed ability performance evaluation of the catalyst of table 2
Claims (6)
1. a kind of Fe-M/CNTs denitrating catalysts, wherein M is Mo or W, it is characterised in that using ferriferous oxide as active component,
Using the CNT with orderly hollow tubular as carrier, addition metal molybdenum or tungsten are used as coagent；Active component contains
Measure as 20-40wt%.
2. the preparation method of Fe-M/CNTs denitrating catalysts described in claim 1, it is characterised in that use infusion process, step is such as
Under：
Source of iron, molybdenum source or tungsten source, solid acid are uniformly mixed in the mixed solution obtained in deionized water；Wherein, source of iron and molybdenum
The mol ratio in source is 10:1~2:1, the mol ratio in source of iron and tungsten source is 10:1~2:1；Solid acid and the mass ratio of molybdenum source are 1:1
~1:2, the mass ratio in solid acid and tungsten source is 1:1~1:2；
By carbon nano tube surface of the mixed solution homogeneous impregnation after being handled through strong oxidizing property concentrated acid, dry, be calcined 3-5h, roasting
Temperature is 350-450 DEG C, obtains Fe-M/CNTs denitrating catalysts.
3. preparation method according to claim 2, it is characterised in that：Described source of iron is ferric nitrate, ferric sulfate, chlorination
One or both of iron, ferric acetate are mixed above.
4. the preparation method according to Claims 2 or 3, it is characterised in that：Described molybdenum source be ammonium molybdate, ammonium dimolybdate,
One or both of ammonium heptamolybdate is mixed above；Described tungsten source is ammonium metatungstate.
5. the preparation method according to Claims 2 or 3, it is characterised in that：Described solid acid is oxalic acid or citric acid.
6. application of the Fe-M/CNTs denitrating catalysts in ammonia selective catalysis nitrogen oxides reduction described in claim 1, it is special
Levy and be：Material mixed gas volume proportioning is 400-1000ppm NH3, 400-1000ppm NO, 3-15vol.%O2, 100-
400ppm SO2, 5-10vol.%H2O, gas overall flow rate is 200-400mL/min, active testing continuous operation；Operation temperature
Spend for 100-450 DEG C, the consumption of denitrating catalyst is 0.05-0.3g, and air speed is 40000-100000h-1。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108404967A (en) * | 2018-02-11 | 2018-08-17 | 山东科技大学 | A kind of preparation method of Ag/MSU-1@FeCeOx/CNTs catalyst with core-casing structure |
| CN113318749A (en) * | 2021-06-23 | 2021-08-31 | 贵州大学 | High-efficiency medium-low temperature NH for resisting heavy metal poisoning3-SCR denitration catalyst and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108404967A (en) * | 2018-02-11 | 2018-08-17 | 山东科技大学 | A kind of preparation method of Ag/MSU-1@FeCeOx/CNTs catalyst with core-casing structure |
| CN113318749A (en) * | 2021-06-23 | 2021-08-31 | 贵州大学 | High-efficiency medium-low temperature NH for resisting heavy metal poisoning3-SCR denitration catalyst and preparation method and application thereof |
| CN113318749B (en) * | 2021-06-23 | 2023-05-09 | 贵州大学 | High-efficiency medium-low temperature NH for resisting heavy metal poisoning 3 SCR denitration catalyst, and preparation method and application thereof |
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