CN106166487A - A kind of quaternary composite oxides low-temperature SCR catalyst and preparation method thereof - Google Patents
A kind of quaternary composite oxides low-temperature SCR catalyst and preparation method thereof Download PDFInfo
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- 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
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- 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
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
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- B01D53/34—Chemical or biological purification of waste gases
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Abstract
The invention discloses a kind of quaternary composite oxides low-temperature SCR catalyst and preparation method thereof, this catalyst uses TiO2‑ZrO2For carrier, Supported Manganese cerium oxide on it;In catalyst, the mol ratio of each element of Ti, Zr, Mn, Ce is 1:1:(0.005 1): (0.005 1).The catalyst that the present invention prepares, reduces the operation temperature of SCR so that in SCR technique, with NH3During for reducing agent, it is possible to just can obtain higher NO clearance when 80 180 DEG C, and when system contains SO2And H2During O, remain to possess higher catalytic efficiency, and SO2Murder by poisoning to it has restorability.
Description
Technical field
The present invention relates to a kind of low-temperature SCR catalyst for flue gas removing NOx, particularly there is anti-sulfur dioxide and water
Low-temperature SCR catalyst based on Mn-Ce-Ti-Zr system of performance and preparation method thereof.
Background technology
Utilize ammonia NH3As reducing agent, SCR (SCR) removing NOx technology is the most most widely used
Gas denitrifying technology.NH3, NO and O2Redox reaction is occurred to generate N under catalyst action2And H2O.The catalysis of its application
Agent is mainly V2O5/TiO2Series, this catalyst temperature window is 300-450 DEG C.In order to reduce SCR reaction temperature, research and
Exploitation low temperature (less than 180 DEG C) SCR reaction process and the most active SCR catalyst have important meaning
Justice.
MnOx is carried on TiO2On studied the most widely as low-temperature SCR catalyst, usually used as low-temperature SCR
Major catalyst;CeO2As a kind of cheap, nontoxic material, it is possible to as preferably storage oxygen agent, the oxygen strengthening catalyst follows
Ring, is commonly used for the promoter of low-temperature SCR.
TiO2To SO2There are preferable resistance, ZrO2It is that uniquely there is acid, alkalescence and oxidation, the compound of reproducibility simultaneously,
It is widely applied as catalyst, but and SiO2And Al2O3Compare etc. common carrier, TiO2And ZrO2Specific surface area
Less.
ZrO2With TiO2When being combined as carrier, it is possible to replace the position of Ti in original lattice, form ZrTiO4.With single
Oxide compare, composite oxides have bigger specific surface area, more preferable heat stability and mechanical strength and higher
Surface acidic-basic property, SO2When absorption, these some positions can attract SO2, the active sites on effective guard catalyst surface, due to adding of Zr
Enter to change the bond energy of crystal, SO2At ZrTiO4Surface can be only formed more weak and reversible sulfate;In addition ZrO2Permissible
Interact with active substance, form metal solid solution, so that SO2It is difficult to react generation metal sulfate with active substance
And metal sulphite.
General MnOx-CeO2/TiO2-ZrO2It is divided into carrier to make and dipping two steps, uses and active component is supported on
The TiO of preparation2-ZrO2On prepare catalyst, it is thus achieved that certain denitration activity, but this catalyst activity component is on carrier
Dispersion inequality, easily sintering and peeling, catalyst is at anti-SO2Indifferent with water intoxication, it is difficult to reach wanting of popularization and application
Ask.Therefore, improve Mn, Ce dispersing characteristic on carrier and crystallization characteristic will be to catalyst activity and anti-SO2And water intoxication
Ability produce far-reaching influence, improve the catalyst activity component such as Mn, Ce dispersion on carrier and intensity be research
One emphasis.
Summary of the invention
The invention aims to solve defect present in prior art, it is provided that one can be effective to cryogenic conditions
Under, the catalyst that reacts of the SCR (SCR) of nitrogen oxides.
In order to achieve the above object, the invention provides a kind of quaternary composite oxides low-temperature SCR catalyst, this catalyst
Use TiO2-ZrO2For carrier, Supported Manganese cerium oxide on it;In catalyst, the mol ratio of each element of Ti, Zr, Mn, Ce is 1:1:
(0.005-1): (0.005-1).Preferred molar ratio is 1:1:(0.1-0.7): (0.05-0.4), optimum mole ratio is 1:1:0.1:
0.05。
Above-mentioned catalyst uses following methods step to prepare:
(1) take inorganic titanium salt by mol ratio 1:1 of Ti, Zr and inorganic zirconium salts prepare mixed aqueous solution, be slowly added to alkaline matter,
It is not further added by precipitation, filtration washing, obtains white solid;
(2) adding nitric acid in white solid, stirring is to being completely dissolved;
(3) it is 1:1:(0.005-1 according to the mol ratio of element ti, Zr, Mn, Ce): (0.005-1) prepares to step (2)
Solution in add soluble manganese salt and solubility cerium salt, be uniformly mixing to obtain co-precipitation mother solution;
(4) in the co-precipitation mother solution that step (3) obtains, it is slowly added to alkaline matter while stirring and is co-precipitated, until heavy
Form sediment and be not further added by, filtration washing;
(5) solid that step (4) obtains is dried at 80-150 DEG C, at 400-600 DEG C, then calcine 2-6h, obtain described
Catalyst.
Wherein, inorganic titanium salt is selected from titanium sulfate, titanyl sulfate, titanium tetrachloride or titanous chloride., preferably sulfuric acid titanium;Inorganic zirconium
Salt is selected from Zirconium tetrachloride., basic zirconium chloride or zirconium nitrate, preferably zirconium nitrate;Soluble manganese salt is selected from manganese sulfate, manganese nitrate, manganese chloride
Or manganese acetate, preferably manganese nitrate;Solubility cerium salt is selected from cerous sulfate or cerous nitrate, preferably cerous nitrate.
Alkaline matter in step (1) and step (4) selected from ammonia, ammonium carbonate, ammonium hydrogen carbonate, sodium hydroxide, sodium carbonate,
One or more mixing in sodium bicarbonate;The addition of alkaline matter is to react completely or little over measuring;It is preferably added to ammonia
Water, the concentration of ammonia is 10%-30%, and in ammonia, the mol ratio of N Yu Ti is 8:1.
In step (2), the addition of nitric acid is to react completely or little over measuring;The concentration of nitric acid is 5-20%, preferably
20%, HNO in nitric acid3It is 8:1 with the mol ratio of Ti.
The present invention has the advantage that compared to existing technology
1, the present invention uses quaternary coprecipitation technology to improve manganese, cerium both elements and the composite attribute of titanium Zirconium oxide, improves
The dispersion of active component and bond strength.Co-precipitation mother solution in, containing Titanium ion, metal zirconium ion, manganese from
Son and cerium ion, after adding alkaline precipitating agent, i.e. can get Ce-Mn-Ti-Zr-OxComposite oxides.
2, Mn is as the catalytic active component in catalyst, and it is primarily present form is unformed shape, using the teaching of the invention it is possible to provide catalysis
The active sites of reaction, to reactant NO and NH3Adsorb, and react on neighbouring acid sites.MnOx is as catalysis
During agent, reaction can be promoted to start to occur at about 100 DEG C, and obtain good effect when 120-200 DEG C.And owing to Mn deposits
At the most different oxide types, such as MnO, MnO2、Mn2O3And Mn3O4Deng, various oxides can mutually convert, Qi Zhonghan
The a large amount of active oxygens having so that MnOx completes the circulation of catalysis in catalytic process.
3, Ce is promoter, and Main Function is to promote that NO is to NO2Changing, improve SCR reactivity, Ce can also increase in addition
Add the electron transfer in catalytic reaction, and as preferably storage oxygen agent, strengthen the Oxygen cycle of catalyst, it is ensured that catalytic reaction
Persistently carry out.
4, the present invention uses Ti (NO in co-precipitation simultaneously3)4With Zr (NO3)4As presoma, it is to avoid sulfate radical,
The impact of catalyst (is prevented a part of sulfate ion, chloride ion etc. from can precipitated wrap, by mistake by the impurity such as chloride ion
Filter washing can only wash away the impurity of particle surface, and cannot remove the impurity within particle-removing, and the impurity of catalytic inner can affect
The transformation of crystal formation, reduces the specific surface area of catalyst, reduces the activity of catalyst), and utilize nitric acid favourable to the acidifying of carrier
In improving catalyst to SO2And H2The resistance of O.
5, the catalyst that the present invention prepares is in the range of 80-200 DEG C, and the highest catalytic efficiency can be close
100%.Catalysis activity is significantly better than existing low-temperature SCR catalyst.At SO2And H2O affects aspect, has SO in systems2With
H2In the presence of O, the removal efficiency of NO is slightly reduced, but works as SO2And H2After O removes, the clearance of NO is returned to substantially original water
Flat.
6, the catalyst that the present invention prepares, reduces the operation temperature of SCR so that in SCR technique, with NH3For
During reducing agent, it is possible to just can obtain higher NO clearance when 80-120 DEG C, and when system contains SO2And H2During O, still
Higher catalytic efficiency, and SO can be possessed2Murder by poisoning to it has restorability.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
Titanium sulfate and Zirconium tetrachloride. are dissolved in water (ice-water bath), are added dropwise over the ammonia of 30%, obtain white precipitate, to be precipitated complete
Quan Hou, filters, is washed with deionized precipitate, remove chloride ion and sulfate ion.Nitric acid with 20% is complete by white precipitate
CL, after adding manganese nitrate, cerous nitrate, in the ammonia of 30% be gradually dropped in whipping process by solution, obtains in this solution
Must precipitate, filter, be washed with deionized precipitate, be dried at 120 DEG C, at 550 DEG C, then calcine 4.5h, it is thus achieved that Mn-
Ce-Ti-Zr-OxCatalyst.Wherein Mn:Ce:Ti:Zr=0.3:0.05:1:1.
Catalyst filling carries out on fixed bed reactors catalyst activity experiment, and application processes NO:NH3=1, O2Concentration
6%, GHSV (gas space velocity per hour)=10000h-1SCR method denitrating flue gas, during reaction temperature 140 DEG C, catalytic efficiency 85.4%,
Add the SO of 150ppm2With 8% H2After O, at 140 DEG C, catalytic efficiency is still more than 80.2%.
Embodiment 2
Titanium sulfate and zirconium nitrate are dissolved in water, are added dropwise over the ammonia of 30%, obtain white precipitate, to be precipitated completely after, filter,
Washing, removes chloride ion and sulfate ion.With the nitric acid of 20%, white precipitate is completely dissolved, in this solution, adds nitric acid
After manganese, cerous nitrate, in the ammonia of 30% that solution is gradually dropped in whipping process, it is thus achieved that precipitation, filter, wash, at 120 DEG C
Lower dry, at 550 DEG C, then calcine 4.5h, it is thus achieved that Mn-Ce-Ti-Zr-OxCatalyst.Wherein Mn:Ce:Ti:Zr=0.1:
0.05:1:1.
Application processes NO:NH3=1, O2Concentration 6%, GHSV (gas space velocity per hour)=10000h-1SCR method flue gas take off
Nitre, during reaction temperature 140 DEG C, catalytic efficiency 89.1%, add the SO of 150ppm2With 8% H2After O, at 140 DEG C, catalytic efficiency is
85.4%。
Embodiment 3
Titanyl sulfate and Zirconium tetrachloride. are dissolved in water (ice-water bath), are added dropwise over the ammonia of 30%, obtain white precipitate, to be precipitated
After Wan Quan, filter, wash, remove chloride ion and sulfate ion.With the nitric acid of 20%, white precipitate is completely dissolved, molten to this
After liquid adds manganese nitrate, cerous nitrate, in the ammonia of 30% that solution is gradually dropped in whipping process, it is thus achieved that precipitation, filter,
Washing, is dried at 120 DEG C, then calcines 4.5h at 550 DEG C, it is thus achieved that Mn-Ce-Ti-Zr-OxCatalyst.Wherein Mn:Ce:
Ti:Zr=0.6:0.4:1:1.
Application processes NO:NH3=1, O2Concentration 6%, GHSV=10000h-1SCR method denitrating flue gas, reaction temperature 140 DEG C
Time, catalytic efficiency 84.2%, add the SO of 150ppm2With 8% H2After O, at 140 DEG C, catalytic efficiency is 80.1%.
Embodiment 4
Titanium tetrachloride and Zirconium tetrachloride. are dissolved in water (ice-water bath), are added dropwise over the ammonia of 10%, obtain white precipitate, to be precipitated
After Wan Quan, filter, wash, remove removing chloride.With the nitric acid of 20%, white precipitate is completely dissolved, in this solution, adds acetic acid
Manganese, cerous nitrate, in the ammonia of 30% be gradually dropped in whipping process by solution, it is thus achieved that precipitation, filters, washs, at 120 DEG C
It is dried, at 500 DEG C, then calcines 4.5h, it is thus achieved that Mn-Ce-TiOxCatalyst.Wherein Mn:Ce:Ti:Zr=0.7:0.3:1:1.
Application processes NO:NH3=1, O2Concentration 6%, GHSV=10000h-1SCR method denitrating flue gas, reaction temperature 140 DEG C
Time, catalytic efficiency 89.2%, add the SO of 150ppm2With 8% H2After O, at 140 DEG C, catalytic efficiency is 83.4%.
Embodiment 5
Titanous chloride. and basic zirconium chloride are dissolved in water (ice-water bath), are added dropwise over the ammonia of 10%, obtain white precipitate, to be precipitated
After Wan Quan, filter, wash, remove removing chloride.With the nitric acid of 20%, white precipitate is completely dissolved, in this solution, adds nitric acid
Manganese, cerous nitrate, in the ammonia of 30% be gradually dropped in whipping process by solution, it is thus achieved that precipitation, filters, washs, at 120 DEG C
It is dried, at 500 DEG C, then calcines 4h, it is thus achieved that Mn-Ce-TiOxCatalyst.Wherein Mn:Ce:Ti:Zr=0.7:0.3:1:1.
Application processes NO:NH3=1, O2Concentration 6%, GHSV=10000h-1SCR method denitrating flue gas, reaction temperature 140 DEG C
Time, catalytic efficiency 92.3%, add the SO of 150ppm2With 8% H2After O, at 140 DEG C, catalytic efficiency is 82.5%.
Claims (8)
1. a quaternary composite oxides low-temperature SCR catalyst, it is characterised in that: described catalyst uses TiO2-ZrO2For carrying
Body, Supported Manganese cerium oxide on it;In described catalyst, the mol ratio of each element of Ti, Zr, Mn, Ce is 1:1:(0.005-1):
(0.005-1).
Catalyst the most according to claim 1, it is characterised in that: the mol ratio of described Ti, Zr, Mn, Ce is 1:1:(0.1-
0.7): (0.05-0.4).
Catalyst the most according to claim 1, it is characterised in that: the mol ratio of described Ti, Zr, Mn, Ce is 1:1:0.1:
0.05。
4. the preparation method of the arbitrary described catalyst of claims 1 to 3, it is characterised in that: described preparation method includes following step
Rapid:
(1) take inorganic titanium salt by mol ratio 1:1 of Ti, Zr and inorganic zirconium salts prepare mixed aqueous solution, be slowly added to alkaline matter,
It is not further added by precipitation, filtration washing, obtains white solid;
(2) adding nitric acid in white solid, stirring is to being completely dissolved;
(3) it is 1:1:(0.005-1 according to the mol ratio of element ti, Zr, Mn, Ce): (0.005-1) prepares to step (2)
Solution in add soluble manganese salt and solubility cerium salt, be uniformly mixing to obtain co-precipitation mother solution;
(4) in the co-precipitation mother solution that step (3) obtains, it is slowly added to alkaline matter while stirring and is co-precipitated, until heavy
Form sediment and be not further added by, filtration washing;
(5) solid that step (4) obtains is dried at 80-150 DEG C, at 400-600 DEG C, then calcine 2-6h, obtain described
Catalyst.
Preparation method the most according to claim 4, it is characterised in that: described inorganic titanium salt selected from titanium sulfate, titanyl sulfate,
Titanium tetrachloride or titanous chloride.;Described inorganic zirconium salts is selected from Zirconium tetrachloride., basic zirconium chloride or zirconium nitrate;Described soluble manganese salt selects
From manganese sulfate, manganese nitrate, manganese chloride or manganese acetate;Described solubility cerium salt is selected from cerous sulfate or cerous nitrate.
Preparation method the most according to claim 5, it is characterised in that: described inorganic titanium salt is titanium sulfate;Described inorganic zirconium
Salt is zirconium nitrate;Described soluble manganese salt is manganese nitrate;Described solubility cerium salt is cerous nitrate.
Preparation method the most according to claim 4, it is characterised in that: described alkaline matter is selected from ammonia, ammonium carbonate, carbonic acid
One or more mixing in hydrogen ammonium, sodium hydroxide, sodium carbonate, sodium bicarbonate;The concentration of described ammonia is 10%-30%, ammonia
The mol ratio of middle N Yu Ti is 8:1.
Preparation method the most according to claim 4, it is characterised in that: the concentration of described nitric acid is 5-20%;HNO in nitric acid3
It is 8:1 with the mol ratio of Ti.
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Cited By (6)
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CN107694576A (en) * | 2017-09-30 | 2018-02-16 | 中晶蓝实业有限公司 | Dry desulfurization denitrfying agent and its production method and application |
CN108404922A (en) * | 2018-02-07 | 2018-08-17 | 山东大学 | One kind being used for low temperature NOxThe quick regenerated catalyst of alternating sorbent-and preparation method |
CN109603815A (en) * | 2018-12-10 | 2019-04-12 | 北京科技大学 | A kind of highly selective manganese-based low-temperature denitration catalyst and preparation method thereof |
CN112742371A (en) * | 2020-12-31 | 2021-05-04 | 华中科技大学 | Efficient catalytic CO2Preparation method of Zr-In spherical oxide catalyst for hydrogenation reaction |
CN113952947A (en) * | 2021-11-08 | 2022-01-21 | 贵州大学 | Hollow core-shell catalyst, and preparation method and application thereof |
CN115970678A (en) * | 2022-12-22 | 2023-04-18 | 南昌航空大学 | MCeTiOx catalyst, preparation method and application thereof |
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CN102114424A (en) * | 2010-12-29 | 2011-07-06 | 国电科学技术研究院 | Low-temperature smoke denitration SCR (silicon controlled rectifier) catalyst and preparation method |
CN105498755A (en) * | 2016-01-14 | 2016-04-20 | 东南大学 | SCR denitration catalyst and preparation method thereof |
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CN102008956A (en) * | 2010-12-27 | 2011-04-13 | 国电科学技术研究院 | Preparation method of low-temperature selective catalytic reduction (SCR) catalyst by removing NOx from flue gas |
CN102114424A (en) * | 2010-12-29 | 2011-07-06 | 国电科学技术研究院 | Low-temperature smoke denitration SCR (silicon controlled rectifier) catalyst and preparation method |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN107694576A (en) * | 2017-09-30 | 2018-02-16 | 中晶蓝实业有限公司 | Dry desulfurization denitrfying agent and its production method and application |
CN108404922A (en) * | 2018-02-07 | 2018-08-17 | 山东大学 | One kind being used for low temperature NOxThe quick regenerated catalyst of alternating sorbent-and preparation method |
CN109603815A (en) * | 2018-12-10 | 2019-04-12 | 北京科技大学 | A kind of highly selective manganese-based low-temperature denitration catalyst and preparation method thereof |
CN112742371A (en) * | 2020-12-31 | 2021-05-04 | 华中科技大学 | Efficient catalytic CO2Preparation method of Zr-In spherical oxide catalyst for hydrogenation reaction |
CN113952947A (en) * | 2021-11-08 | 2022-01-21 | 贵州大学 | Hollow core-shell catalyst, and preparation method and application thereof |
CN115970678A (en) * | 2022-12-22 | 2023-04-18 | 南昌航空大学 | MCeTiOx catalyst, preparation method and application thereof |
CN115970678B (en) * | 2022-12-22 | 2023-09-01 | 南昌航空大学 | MCeTiOx catalyst and preparation method and application thereof |
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Application publication date: 20161130 |