CN102921405B - SiO2-containing denitration catalyst and preparation method thereof - Google Patents
SiO2-containing denitration catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of denitration catalysts and particularly relates to a SiO2-containing denitration catalyst and a preparation method thereof. The denitration catalyst comprises the following components in percentage by mass: 1 to 2 percent of V2O5, 5 percent of WO3, 5 to 10 percent of SiO2 and the balance of TiO2. The preparation method of the denitration catalyst comprises the following steps of: preparing a TiO2-SiO2composite carrier by a co-precipitation method; loading V2O5 and WO3 by a one-step impregnation method; and obtaining the catalyst with high low-temperature denitration by roasting. The method has the characteristics of increasing the overall mechanical strength, wear resistance, and other performance of the catalyst; the silica solution used as a cheap silicon source for SiO2 can be well improved in mechanical performance in processing, extruding and forming processes.
Description
Technical field
The invention belongs to denitrating catalyst technical field, be specifically related to a kind of interpolation SiO
2denitrating catalyst and preparation method thereof
Background technology
Nitrogen oxide NOx is one of main atmosphere pollution, and NOx comprises NO, NO
2, N
2o, N
2o
3, and N
2o
4deng, mainly with NO and NO
2form exist.Coal-burning power plant is that NOx discharges topmost source, and China's nitrogen oxide NOx discharges nearly 70% and comes from coal burning.The discharge of nitrogen oxide can cause the environmental problems such as acid rain, greenhouse effects and depletion of the ozone layer, serious harm human health and social development.
At present, the denitration technology of commercial Application is mainly divided into low NOx combusting technology, SNCR technology and SCR technology in the world.SCR (SCR) denitration technology has high NOx extrusion rate, be at present application at most, the most ripe gas denitrifying technology, this technology is to utilize NH under the condition that has catalyst to exist
3deng reducing agent, NOx is reduced into N
2and H
2o, thus reach NO_x removal, the object of pollution abatement.
Catalyst is the core of SCR technology, its one-tenth is grouped into, structure and relevant parameter directly affect SCR technology denitration efficiency and ruuning situation.SCR catalyst by its one-tenth, be grouped into be divided into noble metal type, burning is miniature and zeolite molecular sieve type.At present most widely used is the miniature catalyst of burning, wherein, and vanadium class catalyst (V
2o
5-WO
3/ TiO
2) most widely used general, its catalyst carrier TiO
2for ridgity material, meeting water has certain hydraulicity, and easily, with the bonding such as mould, institute thinks that preparation has definite shape, mechanical strength, specific area and active catalyst, conventionally need interpolation various additives, and as adhesive, extrusion aid, lubricant etc.Research shows in catalyst, and various additives, as composition, the addition of adhesive, extrusion aid, lubricant etc. with add the conditions such as mode huge for the performance impact of SCR catalyst.
Along with the day by day increase of China's economic development to coal demand, NOx discharge capacity, also in continuous increase, is therefore starved of for having dynamical high-quality denitrating catalyst.When denitrating catalyst is prepared by China at present, for improving the performance of denitrating catalyst, the additive adding mainly comprises glass fibre, carboxymethyl cellulose (CMC), polyvinyl alcohol (PVA) etc., adding of these additives makes moderate progress the mechanical performance of catalyst, but effect is not all very desirable; Overseas enterprise grasps and has monopolized catalyst preparation technology at present in addition, and this just causes high-quality and efficient denitrating catalyst cost higher.Therefore developing at present denitrating catalyst high-quality and efficient and with low cost is current gas denitrifying technology field urgent problem.
NOx has become global very important problem to the pollution of environment, and China's discharged nitrous oxides nearly 70% comes from coal burning, and coal-burning power plant is the topmost source of NOx discharge, and to the NOx of coal-burning power plant, discharge is controlled significant.At present, SCR (SCR) is the most widely used gas denitrifying technology in current coal-burning power plant, and catalyst is the core of SCR technology, and current commercial SCR catalyst is to have anatase structured TiO mostly
2vanadium class catalyst (V for carrier
2o
5-WO
3/ TiO
2).External own through developing into the stage of comparative maturity, commercialization of the production of SCR denitrating catalyst.Because of catalyst carrier TiO
2for ridgity material, and meet water and have certain hydraulicity, easily, with the bonding such as mould, institute thinks that preparation has definite shape, mechanical strength, specific area and active catalyst, conventionally need interpolation various additives, and as adhesive, extrusion aid, lubricant etc.At present, in moulding commercial catalysts, various adhesives, the additives such as extrusion aid account for 10% left and right of gross weight, but for the composition of various binders and auxiliary agent, content and the mode that adds belong to technology secret, and these conditions are huge for the performance impact of SCR catalyst.Because overseas enterprise grasps and monopolized catalyst preparation technology, cause catalyst cost higher, along with the day by day increase of China's economic development to coal demand.Therefore it is significant for the development of China's gas denitrifying technology that development has the domestic catalyst of low cost and better mechanical property.
Research shows in moulding commercial catalysts, the composition of binding agent, structural promoter, content and add the conditions such as mode huge for the performance impact of SCR catalyst.Utilize domestic raw material to prepare denitrating catalyst, will cause formula for raw stock to change, be therefore necessary binding agent, structural promoter content in catalyst formulation adjust accordingly and optimize.Binding agent comprises glass fibre, carboxymethyl cellulose (CMC), polyvinyl alcohol (PVA) etc., contains a certain amount of aluminosilicate or glass fibre in commercial catalysts, and in catalyst, applicable these inorganic assistants can make the mechanical performance of catalyst make moderate progress.
As the important component part of catalyst, for the denitration catalyst agent addition agent of high-quality and the exploitation of binding agent, be also current gas denitrifying technology field urgent problem.Select composition, the content of suitable catalyst additive, additive and the mode that adds will be to improving catalyst mechanical performance, to reduce catalyst cost significant.
Summary of the invention
For prior art above shortcomings, the object of the present invention is to provide a kind of by adding SiO
2as additive, catalyst is had at wider temperature window and also there is higher denitration activity, can improve the mechanical performance of catalyst, and the denitrating catalyst of the interpolation SiO2 reducing production costs;
Another object of the present invention is to provide a kind of preparation method of described denitrating catalyst.
For achieving the above object, the technical solution used in the present invention is: a kind of denitrating catalyst that adds SiO2, it is characterized in that, and in described denitrating catalyst, the quality percentage composition of each component is as follows: V
2o
5be 1% ~ 2%, WO
3be 5% ~ 10%, SiO
2be 5% ~ 10%, all the other components are TiO
2.
Further described interpolation SiO
2the preparation method of denitrating catalyst, comprise the following steps:
1) get the raw materials ready: according to denitrating catalyst mass percent, calculate, take titanium sulfate, ammonium metavanadate, ammonium tungstate, Ludox; Wherein, Ludox is that acidity, mass fraction are 25%, prepares in addition oxalic acid as cosolvent;
2) coprecipitation is prepared TiO
2-SiO
2complex carrier: get the titanium sulfate Ti (SO that step 1) is prepared
4)
2in temperature, be that 60 ℃ of Water Unders are bathed dissolving, adding mass fraction is that 25% Ludox is uniformly mixed, then drip mass fraction and be 20% ammoniacal liquor stirring and dissolving, the pH scope of dissolving is till 10 ~ 11, the suspension generating is under 40 ℃ of conditions standing 10 hours in temperature, filters, washing obtains solid; By the solid obtaining, in temperature, be under 110 ℃ of conditions dry 10 hours, be finally positioned in Muffle furnace 500 ℃ of roasting temperatures 2 hours, finally mill after cooling, be sieved into 200 orders and obtain TiO
2-SiO
2complex carrier;
3) a step infusion process is prepared V
2o
5-WO
3: getting ammonium metavanadate, ammonium metatungstate that step 1) is prepared, add oxalic acid, is that 60 ℃ of Water Unders are bathed to stir fully and dissolved in temperature, by step 2) TiO for preparing
2-SiO
2complex carrier is immersed in bath solution, fully dissolves and stirs; Then the solution configuring is dried to 12 hours under 110 ℃ of conditions;
4) roasting: the sample that step 3) is prepared is put into Muffle furnace roasting, set temperature is: 260 ℃ of roastings 1 hour, 500 ℃ of roastings obtain catalyst finished product after 2 hours.
Compared to existing technology, the present invention has following beneficial effect:
1, interpolation SiO of the present invention
2denitrating catalyst, owing to adding SiO
2can improve TiO
2anti-agglutinatting property, improves TiO
2crystal transfer temperature and the stability of catalyst, than pure TiO
2there is better performance; While SiO
2add and can increase specific area, catalyst surface water imbibition is strengthened, form more acidic site, there is good chemical stability and heat endurance, denitration effect is better.
2, while SiO
2resistance to compression own, the satisfactory mechanical property such as wear-resisting, by adding SiO
2can effectively strengthen the resistance to compression of catalyst, the mechanical performance such as wear-resisting, can make catalyst represent good processing characteristics in the operations such as production, processing.
3, the additive of cheap Ludox as SCR denitrating catalyst usingd in the present invention, catalyst raw material is all domestic raw material, and reduced the degree of dependence to import denitrating catalyst, take full advantage of domestic raw material resources, catalyst cost is declined, the development that be conducive to promote China's denitrating catalyst industrialization process, promotes China's gas denitrifying technology.
4, the present invention prepares TiO by coprecipitation
2-SiO
2complex carrier, a step infusion process supported V
2o
5and WO
3, then the feature such as the catalyst obtaining through roasting has that low-temperature denitration rate is high, the mechanical strength that can obviously increase catalyst integral body and abrasion resistance, and adopt Ludox as SiO
2silicon source is not only with low cost, can improve well the mechanical performance of the operations such as it is processed, extrudes, moulding in actual production process.There is preparation technology reasonable in design, simple to operate, the advantage that cost is low.
Accompanying drawing explanation
Fig. 1-embodiment 1 make denitrating catalyst XRD spectra.
Fig. 2-embodiment 2 make denitrating catalyst XRD spectra.
Fig. 3-embodiment 3 make denitrating catalyst XRD spectra.
Fig. 4-embodiment 4 make denitrating catalyst XRD spectra.
Fig. 5-embodiment 5 make denitrating catalyst XRD spectra.
Fig. 6-embodiment 1-5 make the catalytic activity figure of denitrating catalyst.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further details.
A kind of interpolation SiO
2denitrating catalyst, in described denitrating catalyst, the quality percentage composition of each component is as follows: V
2o
5be 1% ~ 2%, WO
3be 5%, SiO
2be 5% ~ 10%, all the other components are TiO
2.Specific embodiment is as follows:
(1) embodiment 1 ~ 5 is for the SiO that contains of denitrating flue gas
2denitrating catalyst, in described denitrating catalyst, the quality percentage composition of each component is as following table.
(note: embodiment 1 is not for adding SiO
2blank contrast test, embodiment 4 and embodiment 5 are the present invention to adding SiO
2contrast test, non-preference of the present invention)
| Embodiment | V 2O 5 | WO 3 | SiO 2 | TiO 2 |
| Embodiment 1 | 1 | 5 | 0 | 94 |
| Embodiment 2 | 1 | 5 | 5 | 89 |
| Embodiment 3 | 1 | 5 | 10 | 84 |
| Embodiment 4 | 1 | 5 | 20 | 74 |
| Embodiment 5 | 1 | 5 | 30 | 64 |
Embodiment 1:
(1) take 60g titanium sulfate (Ti (SO
4)
2) in temperature, be that 60 ℃ of Water Unders are bathed dissolving, then drip ammoniacal liquor stirring and dissolving, the pH scope of dissolving is till 10 ~ 11, the suspension generating is under 40 ℃ of conditions standing 10 hours in temperature, filter, wash, the solid obtaining is under 110 ℃ of conditions dry 10 hours in temperature, is finally positioned in Muffle furnace 500 ℃ of roasting temperatures 2 hours, finally mills after cooling, is sieved into 200 orders.
(2) taking 0.274g ammonium metavanadate, 1.131g ammonium metatungstate, add a certain amount of oxalic acid, is that 60 ℃ of Water Unders are bathed fully dissolving of stirring in temperature, by the TiO preparing
2-SiO
2be immersed in bath solution, fully dissolve and stir.Then the solution configuring is dried to 12 hours under 110 ℃ of conditions.
Oxalic acid (Han Liang≤99.5) as cosolvent, consumption is about ammonium metavanadate consumption, and following examples are identical.
(3) roasting
The sample preparing of evaporate to dryness is put into Muffle furnace roasting, and set temperature is: 260 ℃ of roastings are warming up to 500 ℃ of roastings for 1 hour again and within 2 hours, make catalyst 1.
Embodiment 2:
(1) take 60g titanium sulfate (Ti (SO
4)
2) in temperature, be that 60 ℃ of Water Unders are bathed dissolving, adding 4g mass fraction is that 25% Ludox is uniformly mixed, then drip ammoniacal liquor stirring and dissolving, the pH scope of dissolving is till 10 ~ 11, the suspension generating is under 40 ℃ of conditions standing 10 hours in temperature, filters, washing, and the solid obtaining is under 110 ℃ of conditions dry 10 hours in temperature, finally be positioned in Muffle furnace 500 ℃ of roasting temperatures 2 hours, finally mill after cooling, be sieved into 200 orders and obtain TiO
2-SiO
2complex carrier.
(2) taking 0.287g ammonium metavanadate, 1.187g ammonium metatungstate, add a certain amount of oxalic acid, is that 60 ℃ of Water Unders are bathed fully dissolving of stirring in temperature, by the TiO preparing
2-SiO
2be immersed in bath solution, fully dissolve and stir.Then the solution configuring is dried to 12 hours under 110 ℃ of conditions.
(3) roasting
The sample preparing of evaporate to dryness is put into Muffle furnace roasting, 260 ℃ of roastings 1 hour, then be warming up to 500 ℃ of roastings and within 2 hours, make catalyst sample 2.
Embodiment 3:
(1) take 60g titanium sulfate (Ti (SO
4)
2) in temperature, be that 60 ℃ of Water Unders are bathed dissolving, adding 8g mass fraction is that 25% Ludox is uniformly mixed, then drip ammoniacal liquor stirring and dissolving, the pH scope of dissolving is till 10 ~ 11, the suspension generating is under 40 ℃ of conditions standing 10 hours in temperature, filters, washing, and the solid obtaining is under 110 ℃ of conditions dry 10 hours in temperature, finally be positioned in Muffle furnace 500 ℃ of roasting temperatures 2 hours, finally mill after cooling, be sieved into 200 orders and obtain TiO
2-SiO
2complex carrier; .
(2) taking 0.301g ammonium metavanadate, 1.243g ammonium metatungstate, add a certain amount of oxalic acid, is that 60 ℃ of Water Unders are bathed fully dissolving of stirring in temperature, by the TiO preparing
2-SiO
2be immersed in bath solution, fully dissolve and stir.Then the solution configuring is dried to 12 hours under 110 ℃ of conditions.
(3) roasting
The sample preparing of evaporate to dryness is put into Muffle furnace roasting, 260 ℃ of roastings 1 hour, then be warming up to 500 ℃ of roastings and within 2 hours, make catalyst sample 3.
Embodiment 4:
(1) take 60g titanium sulfate (Ti (SO
4)
2) in temperature, be that 60 ℃ of Water Unders are bathed dissolving, adding 16g mass fraction is that 25% Ludox is uniformly mixed, then drip ammoniacal liquor stirring and dissolving, the pH scope of dissolving is till 10 ~ 11, the suspension generating is under 40 ℃ of conditions standing 10 hours in temperature, filters, washing, and the solid obtaining is under 110 ℃ of conditions dry 10 hours in temperature, finally be positioned in Muffle furnace 500 ℃ of roasting temperatures 2 hours, finally mill after cooling, be sieved into 200 orders and obtain TiO
2-SiO
2complex carrier; .
(2) taking 0.328g ammonium metavanadate, 1.357g ammonium metatungstate, add a certain amount of oxalic acid, is that 60 ℃ of Water Unders are bathed fully dissolving of stirring in temperature, by the TiO preparing
2-SiO
2be immersed in bath solution, fully dissolve and stir.Then the solution configuring is dried to 12 hours under 110 ℃ of conditions.
(3) roasting
The sample preparing of evaporate to dryness is put into Muffle furnace roasting, 260 ℃ of roastings 1 hour, then be warming up to 500 ℃ of roastings and within 2 hours, make catalyst 4.
Implement
example 5:
(1) take 60g titanium sulfate (Ti (SO
4)
2) in temperature, be that 60 ℃ of Water Unders are bathed dissolving, adding 24g mass fraction is that 25% Ludox is uniformly mixed, then drip ammoniacal liquor stirring and dissolving, the pH scope of dissolving is till 10 ~ 11, the suspension generating is under 40 ℃ of conditions standing 10 hours in temperature, filters, washing, and the solid obtaining is under 110 ℃ of conditions dry 10 hours in temperature, finally be positioned in Muffle furnace 500 ℃ of roasting temperatures 2 hours, finally mill after cooling, be sieved into 200 orders and obtain TiO
2-SiO
2complex carrier.
(2) taking 0.356g ammonium metavanadate, 1.469g ammonium metatungstate, add a certain amount of oxalic acid, is that 60 ℃ of Water Unders are bathed fully dissolving of stirring in temperature, by the TiO preparing
2-SiO
2be immersed in bath solution, fully dissolve and stir.Then the solution configuring is dried to 12 hours under 110 ℃ of conditions.
(3) roasting
The sample preparing of evaporate to dryness is put into Muffle furnace roasting, 260 ℃ of roastings 1 hour, then be warming up to 500 ℃ of roastings and within 2 hours, make catalyst 5.
(3) denitrating catalyst performance evaluation embodiment 1 ~ 5 being made is as follows.
1, denitrating catalyst finished product phase structure analysis result embodiment 1 ~ 5 being made is as table 1:
Table 1 denitrating catalyst anatase crystal grain size
| Embodiment | SiO 2Content (%) | anatase-TiO 2Main peak | Corresponding grain size/nm |
| Implement 1 | 0 | 2θ=25.24° 47.98° 55.06° | 11.5，12.8， 13.8 |
| Implement 2 | 5 | 2θ=25.24° 47.96° 55.02° | 11，11.7， 10.9 |
| Implement 3 | 10 | 2θ=25.24° 47.9° 54.08° | 11.6，11.9，11.2 |
| Implement 4 | 20 | 2θ=25.28° 48° 55° | 11.8， 11.7，11.5 |
| Implement 5 | 30 | 2θ=25.26° 47.96° 55° | 11.7，11.9，11.9 |
2, embodiment 1 ~ 5 is made denitrating catalyst carry out thing and detect mutually analysis, its XRD spectra is as shown in Fig. 1 ~ 5.Relatively find, the XRD collection of illustrative plates of catalyst is substantially similar, has all occurred anatase-TiO
2typical diffraction maximum, just its peak intensity has difference a little.There is not SiO
2crystalline phase, shows SiO
2with amorphous state, exist.TiO
2for anatase crystal, grain size size is 11-12nm, does not occur rutile TiO
2, all there is not in addition V yet
2o
5, WO
3and SiO
2crystal.SiO in catalyst
2when content is 5%, anatase-TiO
2crystal property best.A small amount of SiO
2to anatase-TiO
2phase transformation and grain growth all have certain inhibitory action.
3, denitrating catalyst specific surface area of finished products embodiment 1 ~ 5 being made and active testing analysis result are as table 2:
Table 2 specific area test result
| Embodiment | Specific area (m 2/g) | Aperture (nm) | Pore volume (cm 3/g) |
| Implement 1 | 68.0117 | 15.226 | 0.306384 |
| Implement 2 | 70.6901 | 13.48 | 0.297294 |
| Implement 3 | 73.4099 | 13.0836 | 0.296594 |
| Implement 4 | 73.6585 | 12.2018 | 0.288990 |
| Implement 5 | 73.1167 | 12.0828 | 0.284461 |
According to table 1 and table 2, as seen along with SiO in catalyst
2the increase of content, the aperture of catalyst presents and reduces trend, and pore volume also has reducing to a certain extent, and specific area is corresponding reducing also.This is mainly owing to adding SiO
2after, SiO
2density ratio TiO
2little, the density of the middle quartz of crystalline state, high temperature tridymite, high temperature cristobalite is respectively 2.65,2.26 and 2.32g/cm
3, amorphous Si O
2solid matter degree not as good as crystalline state SiO
2, their density is also less than the SiO of crystalline state
2.In addition, TiO
2after the calcining of higher temperature, crystal grain starts to grow up, and specific area also declines, in calcination process, the speed ratio TiO that declines of specific area
2slowly.This makes to introduce SiO
2rear composite carried catalyst specific area increases, and promotes that active material disperses at carrier surface.V from table 2
2o
5-WO
3/ TiO
2-SiO
2catalyst aperture distribution map can find out, the aperture of catalyst is all concentrated and is distributed between 10-20nm, and in catalyst SiO
2when content increases, micropore reduces gradually.Larger pore volume and aperture are conducive to reactant and product carries out adsorption desorption on catalyst, thereby accelerates NH
3the carrying out of-SCR reaction.Catalyst micropore provides catalyst intrinsic activity necessary high-specific surface area; The effect of mesopore is to hold a large amount of arsenic and other poisonous substance component; The effect of macropore is to improve NO and these two kinds of reactants of ammonia to catalyst diffusion inside, thereby realizes the overall catalytic activity of catalyst.
SiO
2doped Ti O
2the Ti-O-Si key generating can improve TiO
2anti-agglutinatting property, improves TiO
2crystal transfer temperature and the stability of catalyst, than pure TiO
2there is better performance; While SiO
2add and can increase specific area, suppress anatase-TiO
2particle diameter increases, and catalyst surface water imbibition is strengthened, and forms more acidic site.Work as SiO
2when content is 5%, the properties of catalyst is put up the best performance.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (1)
1. one kind is added SiO
2denitrating catalyst, it is characterized in that, adopt and prepare with the following method and obtain:
(1) take 60g titanium sulfate (Ti (SO
4)
2) in temperature, be that 60 ℃ of Water Unders are bathed dissolving, adding 4g mass fraction is that 25% Ludox is uniformly mixed, then drip ammoniacal liquor stirring and dissolving, the pH scope of dissolving is till 10 ~ 11, the suspension generating is under 40 ℃ of conditions standing 10 hours in temperature, filters, washing, and the solid obtaining is under 110 ℃ of conditions dry 10 hours in temperature, finally be positioned in Muffle furnace 500 ℃ of roasting temperatures 2 hours, finally mill after cooling, be sieved into 200 orders and obtain TiO
2-SiO
2complex carrier;
(2) taking 0.287g ammonium metavanadate, 1.187g ammonium metatungstate, add a certain amount of oxalic acid, is that 60 ℃ of Water Unders are bathed fully dissolving of stirring in temperature, by the TiO preparing
2-SiO
2be immersed in bath solution, fully dissolve and stir; Then the solution configuring is dried to 12 hours under 110 ℃ of conditions;
(3) roasting: the sample preparing of evaporate to dryness is put into Muffle furnace roasting, 260 ℃ of roastings 1 hour, then be warming up to 500 ℃ of roastings and within 2 hours, make catalyst.
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| CN101791551A (en) * | 2010-04-23 | 2010-08-04 | 沈炳龙 | Honeycomb catalyst for denitration of glass furnace fume and preparation method thereof |
| CN101869833A (en) * | 2010-07-16 | 2010-10-27 | 天津市塘沽区鑫宇环保科技有限公司 | Catalyst for SCR denitration of furnace middle temperature fume and preparation method thereof |
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| JP3554252B2 (en) * | 2000-05-23 | 2004-08-18 | トーカロ株式会社 | Thermal spray coating member excellent in corrosion resistance and environmental purification properties, method for producing the same, and composite thermal spray material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791551A (en) * | 2010-04-23 | 2010-08-04 | 沈炳龙 | Honeycomb catalyst for denitration of glass furnace fume and preparation method thereof |
| CN101869833A (en) * | 2010-07-16 | 2010-10-27 | 天津市塘沽区鑫宇环保科技有限公司 | Catalyst for SCR denitration of furnace middle temperature fume and preparation method thereof |
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| JP特开2001-335913A 2001.12.07 |
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