CN108525707A - A kind of honeycomb type denitrification catalyst and preparation method - Google Patents
A kind of honeycomb type denitrification catalyst and preparation method Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 18
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 16
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 15
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 15
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 15
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 11
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000004033 plastic Substances 0.000 claims abstract description 9
- 238000011068 loading method Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 12
- 239000012752 auxiliary agent Substances 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012744 reinforcing agent Substances 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 239000004927 clay Substances 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 244000275012 Sesbania cannabina Species 0.000 claims 1
- 230000002708 enhancing effect Effects 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002808 molecular sieve Substances 0.000 description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 11
- 239000002994 raw material Substances 0.000 description 8
- 239000000470 constituent Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910016978 MnOx Inorganic materials 0.000 description 2
- 241000219782 Sesbania Species 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 238000010531 catalytic reduction reaction Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000001404 mediated effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- JYIMWRSJCRRYNK-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4] JYIMWRSJCRRYNK-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical class [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Biomedical Technology (AREA)
- Health & Medical Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of honeycomb type denitrification catalyst and preparation methods, are related to denitration field.The preparation method includes mixing various materials with solvent, is formed and has plastic pug；Wherein, the various materials include：Ferrous sulfate and manganese acetate as catalyst activity component, the catalyst carrier for loading the active component；It is green honeycomb by the mud material forming；The green honeycomb is dried；It is calcined with to the green honeycomb after drying, forms the denitrating catalyst；Wherein, the weight ratio of the active component and the catalyst carrier is 1:(4~12).The present invention also provides the denitrating catalysts prepared using above-mentioned preparation method.There is very high catalytic efficiency by denitrating catalyst prepared by above-mentioned preparation method.
Description
Technical field
The present invention relates to denitration fields, more particularly to a kind of honeycomb type denitrification catalyst and preparation method.
Background technology
Currently, oxynitrides NOXIt is a kind of important atmosphere pollution, is to cause acid rain, haze, photochemical fog
Key factor.Meanwhile the oxynitrides NO in airXIf being inhaled into human body, serious injury can be generated to human body.Cause
This, either to human residential environment or itself consideration, control oxynitrides NOXDischarge it is extremely urgent.
At this stage, selective catalytic reduction (Selective catalytic reduction, SCR) is a kind of effective
Method of denitration, principle be to discharge flue gas in spray into NH3Equal reducing agents, under the action of catalyst with the NO in flue gasXIt generates
Harmless N2And H2O.Wherein, the quality of denitrating catalyst largely determines catalytic efficiency, and its core technology is
Its composition of raw materials and preparation process.
The SCR denitration used at present is substantially with TiO2For base material, with V2O5For main active, and add
Enter a small amount of WO3Or MoO3As auxiliary agent to inhibit SO2It is oxidized to SO3, improve activity, thermal stability and the anti-poisoning of catalyst
Performance.Its chemical lifetime is typically about 24000h.Its chemical lifetime expires over time, it will faces denitrating catalyst
Process problem, since its main active constituent vanadium is extremely toxic substance, catalyst fixed-end forces cost is larger.
Meanwhile also studies have found that, ferrous sulfate FeSO4It, can be in SCR method as denitrating catalyst active constituent
Effectively remove oxynitrides NOX, and compared to vanadium titanium class catalyst, ferrous sulfate have it is cheap, be easy to get, long lifespan, can
The advantages that throwing aside.
Although as described above it has been found that ferrous sulfate can as the active constituent of SCR denitration, and
The technology of preparing for having ripe honeycomb type denitrification catalyst in the prior art, it will be recognized to those skilled in the art that this is simultaneously
It cannot become apparent to a kind of successfully using ferrous sulfate as the honeycomb type denitrification catalyst of active constituent.In order to obtain
Such a denitrating catalyst, it is also necessary to the selection of raw material, raw material proportioning, the addition of raw material is suitable in preparation process
Meticulous research and design are carried out in the one or more technological difficulties such as sequence, technological parameter, and carrying out a large amount of experiment could be real
It is existing.
Invention content
Therefore, it is an object of the invention to overcome above-mentioned one or more technological difficulties.
According to one aspect of the present invention, a kind of preparation method of honeycomb type denitrification catalyst is provided, including：
Various materials are mixed with solvent, is formed and has plastic pug；Wherein, the various materials include：As
The ferrous sulfate and manganese acetate of catalyst activity component, the catalyst carrier for loading the active component；
It is green honeycomb by the mud material forming；
The green honeycomb is dried；With
The green honeycomb after drying is calcined, the denitrating catalyst is formed；
Wherein, the weight ratio of the active component and the catalyst carrier is 1:(4~12).
Further, the catalyst carrier includes TiO2-ZrO2And molecular sieve.
Further, the weight percent of ferrous sulfate is 60-80% in the active component.
Further, TiO in the catalyst carrier2And ZrO2Mass ratio be 1：4.
Further, the various materials further include auxiliary agent.
Further, the auxiliary agent includes at least one of adhesive, extrusion aid and reinforcing agent.
Further, described adhesive includes clay；The extrusion aid includes glycerine or sesbania powder；The reinforcing agent includes
Glass fibre.
Further, described to mix various materials with solvent, forming the plastic pug of tool includes：
The active component is added in the solvent first, adds the catalyst carrier, is added after being sufficiently stirred
Enter the auxiliary agent, is finally mixed into pug.
Further, the green honeycomb is dried using drying machine, the heating rate of the drying machine is 5
DEG C/day.
Further, the drying temperature when green honeycomb being dried is 95-100 DEG C.
Further, calcination temperature when being calcined to the green honeycomb after drying is 450-470 DEG C.
It is another aspect of this invention to provide that a kind of honeycomb type denitrification catalyst is provided, according to preceding method preparation
At.
The present invention is in the selection of raw material, the proportioning of raw material, the addition sequence of raw material, technological parameter in preparation process
These aspects propose improvement means to honeycomb type denitrification catalyst, improve the property of final obtained honeycomb type denitrification catalyst
Energy and/or yield rate.It should be noted that the present invention can independently or jointly make in the improvement of above-mentioned several aspects
With so that the industrial applications of honeycomb type denitrification catalyst are possibly realized.It is other types of cellular de- compared to existing
Denox catalyst, the present invention are added manganese acetate as active component, not only improve catalytic efficiency, additionally it is possible to as pore creating material into one
Step improves the activity of catalyst.Meanwhile 1) present invention two kinds of active components can select cheap raw material, greatly reduce denitration
The production cost of catalyst；2) sorting of the invention can be non-toxic, and reducing environment influences and reduce waste catalyst
Post processing cost；3) not only denitration efficiency is high for denitrating catalyst of the invention, and anti-poisoning capability enhances, and with preferable
Mechanical performance and thermal stability, there has also been larger to widen for operating temperature.
According to the following detailed description of specific embodiments of the present invention in conjunction with the accompanying drawings, those skilled in the art will be brighter
The above and other objects, advantages and features of the present invention.
Description of the drawings
Some specific embodiments that the invention will be described in detail by way of example and not limitation with reference to the accompanying drawings hereinafter.
Identical reference numeral denotes same or similar component or part in attached drawing.It should be appreciated by those skilled in the art that these
What attached drawing was not necessarily drawn to scale.In attached drawing：
Fig. 1 is the flow chart of honeycomb type denitrification catalyst preparation method according to an embodiment of the invention；
Fig. 2 is the denitration efficiency of denitrating catalyst according to an embodiment of the invention at different temperatures.
Specific implementation mode
Below in conjunction with specific implementation mode, the present invention is described in more detail.
The selection of material
Catalyst active component uses ferrous sulfate a kind of or the mixture of ferrous sulfate and manganese acetate.Preferably, when
When using the mixture of ferrous sulfate and manganese acetate as catalyst active component, the weight percent of ferrous sulfate in active component
Than that can be 60-80%.The present invention, on the one hand so that catalyst surface has acidity, makes NH by the way that active constituent manganese acetate is added3
It preferably adsorbs on a catalyst, while being heated in catalyst calcination stage manganese acetate and being decomposed into MnOxAnd gas is discharged, wherein
MnOxIt is the good denitrification reducing agent of catalytic activity, while the gas discharged can play the role of good pore-creating, can improve catalysis
The activity of agent.Therefore, the addition of manganese acetate is not required to additionally add pore creating material, and above-mentioned these effectively increase the property of catalyst
Energy.
Solvent can be water.
TiO may be used in catalyst carrier2-ZrO2Complex carrier and molecular sieve, molecular sieve can be type A zeolite molecular sieve,
X-type zeolite molecular sieve, Y-type zeolite molecular sieve, ZSM Series Molecules sieve, MFI molecular sieves, MOR molecular sieves etc., can also be it
His molecular sieve suitable for ferrous sulfate and manganese acetate.In an embodiment of the invention, TiO in preferred catalytic agent carrier2
And ZrO2Mass ratio be 1：4, above-mentioned mass ratio so that the reaction temperature window upper limit of catalyst is widened, and has anti-
SO2The performance of poisoning.
Preferably, the weight ratio of the active component and the catalyst carrier can be 1:(4~12), by a large amount of real
It issues after examination and approval now, above-mentioned mass ratio can effectively improve the catalytic efficiency of denitrating catalyst.
Auxiliary agent may include adhesive, extrusion aid and reinforcing agent.
For bonding agent, it is preferred to use clay.
For extrusion aid, it is preferred to use glycerine or sesbania powder etc..
For reinforcing agent, it is preferred to use glass fibre.
Fig. 1 is the flow chart of honeycomb type denitrification catalyst preparation method according to an embodiment of the invention, such as Fig. 1 institutes
Show, the honeycomb type denitrification catalyst preparation method is general to may include steps of：
S100 mixes various materials with solvent, is formed and has plastic pug；
The mud material forming is green honeycomb by S200；
The green honeycomb is dried in S300；
S400 calcines the green honeycomb after drying, forms the denitrating catalyst.
Specific detailed description will be further done to preparation method below.
Mixing step
In mixing step, afore-mentioned materials and solvent are mixed, is formed and has plastic pug.The material is preferably
Ferrous sulfate and manganese acetate, catalyst carrier TiO as active component2-ZrO2With molecular sieve, auxiliary agent.
Mixing step adds the catalyst carrier, is then added specifically, first by active component addition solvent
Clay, glycerine are put into kneader after stirring and are fully mediated.When material basically forms toughness plastic type in kneader
When pug (kneader is mediated about 30~40 minutes), it is gradually added glass fibre into kneader, then proceedes to mediate until institute
There is material to be sufficiently mixed, ultimately forms uniform plastic type pug.
By above-mentioned hybrid mode, active component can be made equably to carry over a molecular sieve, catalysis can be effectively improved
The catalytic performance of agent.
Forming step
The pug formed in mixing step is sent in extruder.The outlet of extruder adds as required equipped with a set pattern
The honeycomb moulding mold (preferably rectangular honeycomb) of lattice, to become continuous honeycomb ceramics base after pug is squeezed out by mold
Material.It is cut using automatic synchronous cutting machine, forms the green honeycomb module with certain size.
Herein, the selection of molding die and the selection of module size are all well-known to those skilled in the art,
This is repeated no more.
Drying steps
In drying steps, the heating rate that need to strictly control drying machine is 5 DEG C/day, until reaching 95-100 DEG C, together
When, stop is no longer heated in this temperature range, and drying process no longer changes ability substantially until the weight of green honeycomb
It terminates.
Calcining step
Dried green honeycomb is sent into calcining kiln and is calcined, honeycomb type denitrification catalyst is formed.In calcination process
In, average heating speed after calcination temperature reaches 450-470 DEG C of section, maintains calcining preferably between 10-20 DEG C/h
It is temperature-resistant, meanwhile, it is calcined 30-45 hours in this temperature range, is finally completed calcination process, obtains required honeycomb fashion
Denitrating catalyst finished product module.
In above process, by the addition sequence of material, the kneading time of kneader, drying steps in mixing step
The selection in calcination temperature section, greatly improves in the heating rate of drying machine and the selection in drying temperature section and calcining step
The denitration efficiency of denitrating catalyst.
Fig. 2 is the denitration efficiency of denitrating catalyst according to an embodiment of the invention at different temperatures.Such as Fig. 2 institutes
Show, catalytic efficiency is 85% or more in 280-450 DEG C of temperature range for denitrating catalyst, especially in 320-370 DEG C of range, catalysis
Efficiency is 95% or more.It can be seen that the catalyst of the present invention has wider operating temperature range and higher catalytic efficiency.
So far, although those skilled in the art will appreciate that present invention has been shown and described in detail herein is exemplary
Embodiment still without departing from the spirit and scope of the present invention, still can be determined directly according to the present disclosure
Or derive many other variations or modifications consistent with the principles of the invention.Therefore, the scope of the invention should be understood and defined as
Cover other all these variations or modifications.
Claims (12)
1. a kind of preparation method of honeycomb type denitrification catalyst, including：
Various materials are mixed with solvent, is formed and has plastic pug；Wherein, the various materials include：As catalysis
The ferrous sulfate and manganese acetate of agent active component, the catalyst carrier for loading the active component；
It is green honeycomb by the mud material forming；
The green honeycomb is dried；With
The green honeycomb after drying is calcined, the denitrating catalyst is formed；
Wherein, the weight ratio of the active component and the catalyst carrier is 1:(4~12).
2. preparation method according to claim 1, which is characterized in that the catalyst carrier includes TiO2-ZrO2And molecule
Sieve.
3. preparation method according to claim 1 or 2, which is characterized in that the weight of ferrous sulfate in the active component
Percentage is 60-80%.
4. preparation method according to claim 2, which is characterized in that TiO in the catalyst carrier2And ZrO2Quality
Than being 1：4.
5. preparation method according to claim 4, which is characterized in that the various materials further include auxiliary agent.
6. preparation method according to claim 5, which is characterized in that the auxiliary agent includes adhesive, extrusion aid and enhancing
At least one of agent.
7. preparation method according to claim 6, which is characterized in that
Described adhesive includes clay；
The extrusion aid includes glycerine or sesbania powder；
The reinforcing agent includes glass fibre.
8. according to the preparation method described in any one of claim 5-7, which is characterized in that described to mix various materials and solvent
It closes, forming the plastic pug of tool includes：
The active component is added in the solvent first, the catalyst carrier is added, institute is added after being sufficiently stirred
Auxiliary agent is stated, pug is finally mixed into.
9. preparation method according to claim 8, which is characterized in that done to the green honeycomb using drying machine
Dry, the heating rate of the drying machine is 5 DEG C/day.
10. preparation method according to claim 9, which is characterized in that done when the green honeycomb is dried
Dry temperature is 95-100 DEG C.
11. preparation method according to claim 9 or 10, which is characterized in that the green honeycomb after drying into
Calcination temperature when row calcining is 450-470 DEG C.
12. a kind of honeycomb type denitrification catalyst, the method according to any one of claim 1-11 is prepared.
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