CN104307533B - Natural application of the siderite in SCR denitration is prepared - Google Patents
Natural application of the siderite in SCR denitration is prepared Download PDFInfo
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- CN104307533B CN104307533B CN201410543448.8A CN201410543448A CN104307533B CN 104307533 B CN104307533 B CN 104307533B CN 201410543448 A CN201410543448 A CN 201410543448A CN 104307533 B CN104307533 B CN 104307533B
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Abstract
The invention discloses application of the siderite in SCR denitration is prepared, by the way that siderite is ground into calcining or by siderite is broken, slurrying, coating and calcination processing obtain catalyst, preparation technology is simple, cost is cheap, denitration efficiency is high, while environment-friendly, without poisoning metal element, catalyst waste treatment is easy, can continue on for smelting iron particularly for the denitrating catalyst of fixed bed or fluid bed.
Description
Technical field
The invention belongs to technical field of air pollution control, and in particular to natural siderite is preparing SCR denitration catalysis
Application in agent.
Background technology
Nitrogen oxides (the NO of thermal power plant, industrial furnace and motor vehicles dischargex) it is one of main atmosphere pollution,
Acid rain and photochemical fog are easily formed, damages the ozone layer and causes greenhouse effects, endanger ecological environment；And bring breathing to the mankind
Tract disease, threaten health.As economic development, its discharge standard are also increasingly strict.Therefore, NO is effectively eliminatedxInto
For a technical field to attract people's attention in environmental protection.
Ammonia process Selective Catalytic Reduction of NOxTechnology (NH3- SCR) due to its high efficiency, selectivity and be widely applied to denitration
Field.The core of SCR techniques is catalyst, the outer commercial Application of Now Domestic the most extensively, it is ripe be V2O5/TiO2System's catalysis
Agent.Although such catalyst can produce at home, its complex manufacturing, raw material stills need import, expensive, is produced into
This height；Such catalyst operating temperature is higher, and catalytic unit is generally mounted to before deduster, desulfurizing tower, easy appearance blocking,
The problems such as poisoning；Its important activity composition V2O5With toxicity, the processing of waste catalyst can also increase its operation cost.
In order to reduce cost, a variety of natural minerals are developed as denitrating catalyst.Domestic publication CN1108850C
A kind of method that natural manganese ores prepare SCR denitration is disclosed, and window temperature is relatively low.Southeast China University Gui Ke front yards et al. (king
Virtue；Li Honghong；Jiang Xinfeng；The performance study coals journal 2011 of Gui Ke front yards iron ore SCR method smoke catalytic denitrations, (08),
The bloodstone of different calcining heats processing 1381-1384) is selected as SCR denitration.
Siderite is that one kind is widely distributed in China, is easier the mineral obtained.The comprehensive utilization of siderite
Generally attract much attention.Domestic publication CN 102451662A disclose one kind and prepare fluorine removal suction using natural sparring
Attached dose of method；Publication CN 103787444A disclose a kind of siderite and are used for waste water advanced remove as sand filtration oily filter material
The method of phosphorus.There is not yet the report of efficient SCR denitration is prepared from siderite.
The content of the invention
Goal of the invention：To solve problems of the prior art, the present invention proposes natural siderite and is preparing SCR
Application in denitrating catalyst, and further provide that a kind of raw material sources are extensive, preparation technology is simple, cheap, environment
The friendly and obvious SCR denitration of efficiency.
Technical scheme：To realize above-mentioned technical purpose, the present invention proposes natural siderite and is preparing SCR denitration catalysis
Application in agent.
Preferably, the FeCO of the natural siderite3Content be not less than 80wt%.
Specifically, it is a kind of for filling fixed bed or the SCR denitration of fluid bed when being prepared with described natural siderite
During catalyst, specific preparation method is as follows：
Choose natural siderite, obtained siderite particle is calcined 4~7 at 400~500 DEG C after Mechanical Crushing
Hour, room temperature is then naturally cooled to, obtains the SCR denitration for filling fixed bed or fluid bed.
Preferably, 0.1~1mm of particle diameter after the natural siderite Mechanical Crushing described in above-mentioned preparation process.
When preparing a kind of SCR denitration for alveolate texture with described natural siderite, its is specific
Preparation method is as follows：
Natural siderite is chosen, obtained natural siderite particle is added in distilled water after Mechanical Crushing, matched somebody with somebody
Slurry is made, ultrasonic wave disperses, and obtains catalyst pulp, and alkali lye adjusts the pH to 8~9 of catalyst pulp, to after regulation pH
Bonding agent is added in catalyst pulp, cellular skeleton structure is then put into ultrasound leaching in the catalyst pulp added with bonding agent
Stain 4~5 hours, then take out and dried 5 hours at 100~120 DEG C, repeat above-mentioned dipping, drying process 2~3 times, 400
Room temperature is cooled to after calcining 4~7 hours at~500 DEG C, that is, obtains the SCR denitration for alveolate texture.It is preferred that
Ground, described alkali lye are ammoniacal liquor, and mass concentration is 18~23%.
Preferably, in above-mentioned steps, the particle diameter of the natural siderite particle after Mechanical Crushing is micro- less than or equal to 50
Rice.Preferably, the particle diameter of the natural siderite particle after Mechanical Crushing is less than or equal to 10 microns.
In the preparation process of catalyst pulp, the weight of siderite particle is the 30~50% of distilled water weight.
Specifically, described bonding agent is in colloidal alumina, cataloid, polyvinyl alcohol and carboxymethyl cellulose
Any one or it is several.Preferably, described bonding agent is carboxymethyl cellulose.
Preferably, described cellular skeleton structure is cordierite ceramic honeycomb carrier.
The dosage of the bonding agent is 1%~5% of the catalyst pulp weight after regulation pH.Preferably, bonding agent
Dosage is 3% of the catalyst pulp weight after regulation pH.
Preferably, the FeCO of above-mentioned natural siderite3Content be not less than 80wt%.
Beneficial effect：Compared with prior art, the invention has the advantages that：
(1) natural siderite is the siderite found in earth surface mineral deposit, the main component molecule of siderite
Formula is FeCO3, the present invention is that raw material prepares SCR denitration using natural siderite, and raw material sources are extensive, and price is low
It is honest and clean；By by siderite is broken, slurrying, coating and calcination processing, preparation technology is simple, and cost is cheap；
(2) present invention by siderite in calcination process, FeCO3Decompose, discharge CO2, add the ratio table of catalyst
Area, be advantageous to the progress of catalytic reaction；The main active component α Fe of catalyst2O3、γFe2O3And the MnO in impurityxUrge
It is high to change activity, operative temperature scope is wide, is particularly suitable for low temperature SCR denitration reaction；
(3) present invention is environmentally friendly catalyst, and without poisoning metal element, catalyst waste treatment is easy, especially
It can continue on for smelting iron for the denitrating catalyst of fixed bed or fluid bed.
Brief description of the drawings
Fig. 1 siderites I1 and obtained catalyst C1 XRD analysis result；
Fig. 2 is the denitration activity of siderite SCR denitration C1 under different temperatures；
Fig. 3 detects for siderite catalyst C1 water resistants sulfur resistance；
Fig. 4 is the denitration activity of alveolate texture siderite catalyst C5 under different temperatures；
Fig. 5 detects for alveolate texture siderite catalyst C5 water resistants sulfur resistance.
Embodiment
Used below in each embodiment cordierite ceramic honeycomb carrier purchase from described cellular skeleton structure for
Cordierite ceramic honeycomb carrier, is diameter 2cm, high 3.5cm cylinder, per square inch honeycomb hole count 500；Geometrical surface
26.5cm2/cm2；Percent opening 75.9%.
Embodiment 1 is used for the preparation for filling fixed bed or the SCR denitration of fluid bed.
Select natural siderite (being designated as I1), its FeCO3Content be not less than 80wt%, be broken into particle diameter as 0.2
~0.4mm particle, in 450 DEG C of 5 hours of calcining of air atmosphere, natural cooling, obtain siderite SCR catalyst C1.
Embodiment 2 is used for the preparation for filling fixed bed or the SCR denitration of fluid bed.
Select natural siderite (being designated as I1), its FeCO3Content be not less than 80wt%, be broken into particle diameter as 0.4
~0.6mm particle, in 400 DEG C of 7 hours of calcining of air atmosphere, natural cooling, obtain siderite SCR catalyst C2.
Embodiment 3 is used for the preparation for filling fixed bed or the SCR denitration of fluid bed.
Select natural siderite (being designated as I1), its FeCO3Content be not less than 80wt%, be broken into particle diameter as 0.6
~1.0mm particle, in 500 DEG C of 4 hours of calcining of air atmosphere, natural cooling, obtain siderite SCR catalyst C3.
Embodiment 4 is used for the preparation for filling fixed bed or the SCR denitration of fluid bed.
Select natural siderite (being designated as I1), its FeCO3Content be not less than 80wt%, be broken into particle diameter as 0.6
~0.8mm particle, in 450 DEG C of 6 hours of calcining of air atmosphere, natural cooling, obtain siderite SCR catalyst C4.
Embodiment 5 is used for the preparation of the SCR denitration of alveolate texture.
The powder for being about 10 microns into average grain diameter by siderite I1 mechanical lappings, 400g siderite powders are added to
In 1000g distilled water, slurry is configured to, is disperseed with ultrasonic wave, then the pH value for adjusting slurry with ammoniacal liquor adds to 8 into slurry
Enter 50g carboxymethyl celluloses, disperseed with ultrasonic wave and stirred.Cordierite ceramic honeycomb carrier is put into the slurry prepared
Ultrasonic immersing 2~3 hours, then take out and dried 5 hours at 100~120 DEG C, repeated impregnations are dried 3 times.Then in air gas
With natural cooling after 450 DEG C of 5 hours of temperature calcination under atmosphere, that is, obtain the siderite denitrating catalyst for alveolate texture
C5。
Embodiment 6 is used for the preparation of the SCR denitration of alveolate texture.
The powder for being about 20 microns into average grain diameter by siderite I1 mechanical lappings, 350g siderite powders are added to
In 1000g distilled water, slurry is configured to, is disperseed with ultrasonic wave, with the pH value of ammoniacal liquor regulation slurry to 8.5, then into slurry
40g carboxymethyl celluloses are added, is disperseed with ultrasonic wave and stirred.Cordierite ceramic honeycomb carrier is put into the slurry prepared
Middle ultrasonic immersing 2~3 hours, then take out and dried 5 hours at 100~120 DEG C, repeated impregnations are dried 3 times.Then in air
With natural cooling after 400 DEG C of 7 hours of temperature calcination under atmosphere, that is, obtain the siderite denitration catalyst for alveolate texture
Agent C6.
Embodiment 7 is used for the preparation of the SCR denitration of alveolate texture.
The powder for being about 30 microns into average grain diameter by siderite I1 mechanical lappings, 450g siderite powders are added to
In 1000g distilled water, slurry is configured to, is disperseed with ultrasonic wave, then the pH value for adjusting slurry with ammoniacal liquor adds to 8 into slurry
Enter 35g carboxymethyl celluloses, disperseed with ultrasonic wave and stirred.Cordierite ceramic honeycomb carrier is put into the slurry prepared
Ultrasonic immersing 2~3 hours, then take out and dried 5 hours at 100~120 DEG C, repeated impregnations are dried 3 times.Then in air gas
With natural cooling after 500 DEG C of 4 hours of temperature calcination under atmosphere, that is, obtain the siderite denitrating catalyst for alveolate texture
C7。
Embodiment 8 is used for the preparation of the SCR denitration of alveolate texture.
The powder for being about 40 microns into average grain diameter by siderite I1 mechanical lappings, 400g siderite powders are added to
In 1000g distilled water, slurry is configured to, is disperseed with ultrasonic wave, then the pH value for adjusting slurry with ammoniacal liquor adds to 8 into slurry
Enter 25g carboxymethyl celluloses, disperseed with ultrasonic wave and stirred.Cordierite ceramic honeycomb carrier is put into the slurry prepared
Ultrasonic immersing 2~3 hours, then take out and dried 5 hours at 100~120 DEG C, repeated impregnations are dried 3 times.Then in air gas
With natural cooling after 450 DEG C of 6 hours of temperature calcination under atmosphere, that is, obtain the siderite denitrating catalyst for alveolate texture
C8。
Embodiment 9 is used for the preparation of the SCR denitration of alveolate texture.
The powder for being about 15 microns into average grain diameter by siderite I1 mechanical lappings, 400g siderite powders are added to
In 1000g distilled water, slurry is configured to, is disperseed with ultrasonic wave, then the pH value for adjusting slurry with ammoniacal liquor adds to 8 into slurry
Enter 20g carboxymethyl celluloses, disperseed with ultrasonic wave and stirred.Cordierite ceramic honeycomb carrier is put into the slurry prepared
Ultrasonic immersing 2~3 hours, then take out and dried 5 hours at 100~120 DEG C, repeated impregnations are dried 3 times.Then in air gas
With natural cooling after 450 DEG C of 6 hours of temperature calcination under atmosphere, that is, obtain the siderite denitrating catalyst for alveolate texture
C9。
The performance test of embodiment 10SCR denitrating catalysts.
(1) it is used for the performance test for filling fixed bed or the SCR denitration of fluid bed.
Elementary analysis XRF elementary analyses, the test result such as institute of table 1 are carried out to certain siderite I1 used in embodiment 1~9
Show.Carry out BET analyses and XRD analysis to siderite catalyst C1 prepared by siderite I1 and embodiment 1, analysis result is respectively such as
Shown in table 2, Fig. 1.XRF analysis understand that main metal element is Fe in siderite, and contains a small amount of Mn elements, manganese oxidation
Thing has SCR catalytic activity, plays a part of co-catalysis in siderite catalyst.XRD analysis are visible, make in calcination process
Siderite main component FeCO3It is converted into the α Fe with SCR catalytic activity2O3、γFe2O3.BET analysis results are shown, at calcining
Specific surface area of catalyst after reason greatly increases than sparring green ore, is advantageous to the progress of SCR reactions, also denitration efficiency is increased
Add.
The siderite I1 of table 1 XRF analysis result
Table 2 is to siderite I1 and obtained catalyst BET analysis results
The catalyst C1 of preparation is seated in the stainless steel fixed bed reactors that internal diameter is 2cm, using air speed 9000h-1,
It is passed through 500ppmNO, 500ppmNH3And the O of volume fraction 3%2.Aforesaid operations are repeated 3 times, to gained denitration under different temperatures
Efficiency is mapped, referring to Fig. 2.For siderite catalyst within the scope of 150~330 DEG C of very wide temperature, denitration efficiency is higher than 95%.
270 DEG C, it is passed through 100ppmSO2With the H that volume fraction is 5%2O, its denitration efficiency are changed over time such as Fig. 3.It is being passed through SO2With
H25 hours after O, the denitration efficiency of siderite catalyst maintains 86% or so, has certain water resistant sulfur resistive ability.
From certain natural hematite as a comparison case, the natural hematite is broken into that particle diameter is 0.2~0.4mm
Grain, in 450 DEG C of 5 hours of calcining of air atmosphere, natural cooling, obtain hematite catalyst H1.
Elementary analysis XRF elementary analyses are carried out to certain bloodstone of use, test result is as shown in table 3.It is former to bloodstone
Ore deposit and hematite catalyst C2 carry out BET analyses, and analysis result is as shown in table 4.
Table 3 is to bloodstone H1XRF analysis results
Table 4 is to bloodstone H1 and obtained catalyst BET analysis results
The catalyst HS1 of preparation is seated in the stainless steel fixed bed reactors that internal diameter is 2cm, using air speed 9000h-1, it is passed through 500ppmNO, 500ppmNH3And the O of volume fraction 3%2.Aforesaid operations 3 times are repeated, gained during to different temperatures
Mapped to denitration efficiency, referring to Fig. 2.It can be seen that in 90~330 DEG C of temperature range, siderite catalyst efficiency is above
Hematite catalyst, gap is particularly evident in the range of 120~240 DEG C.So siderite catalyst is substantially better than previous research
The hematite catalyst crossed.
(2) performance test of the SCR denitration of alveolate texture.
C5 catalyst prepared by embodiment 5 is placed in the reactor that internal diameter is 5cm, using air speed 9000h-1, it is passed through
500ppmNO、500ppmNH3And the O of volume fraction 3%2, experiment 3 times is repeated, resulting denitration efficiency is made during to different temperatures
Figure, referring to Fig. 4.
At 270 DEG C, 100ppmSO is passed through2With the H that volume fraction is 5%2O, its denitration efficiency are changed over time such as Fig. 5.
It is passed through SO2And H24.5 hours after O, the denitration efficiency of siderite catalyst maintains 88% or so, equally with certain water resistant
Sulfur resistive ability.
Using bloodstone H1 as a comparison case, the powder for being about 10 microns into average grain diameter by bloodstone H1 mechanical lappings,
400g hematite powders are added in 1000g distilled water, are configured to slurry, are disperseed with ultrasonic wave, slurry is adjusted with ammoniacal liquor
Then pH value adds 50g carboxymethyl celluloses into slurry, is disperseed with ultrasonic wave and stirred to 8.By cordierite ceramic honeybee
Nest carrier is put into ultrasonic immersing 2~3 hours in the slurry prepared, then takes out and is dried 5 hours at 100~120 DEG C, repeats to soak
Stain is dried 3 times.Then obtained for cellular with natural cooling after 450 DEG C of 5 hours of temperature calcination in air atmosphere
The bloodstone denitrating catalyst HS2 of structure.
HS2 catalyst is placed in the reactor that internal diameter is 5cm, using air speed 9000h-1, be passed through 500ppm NO,
500ppm NH3And the O of volume fraction 3%2, experiment 3 times is repeated, resulting denitration efficiency mapping during to different temperatures, referring to
Fig. 4.
Claims (1)
- A kind of 1. method that SCR denitration is prepared using natural siderite, it is characterised in that comprise the following steps：Choose natural siderite, the FeCO of the natural siderite3Content be not less than 80wt%, be added to after Mechanical Crushing In distilled water, the particle diameter after Mechanical Crushing is less than or equal to 50 microns, is configured to slurry, the weight of natural siderite particle is distillation The 30 ~ 50% of water weight, ultrasonic wave disperses, and obtains catalyst pulp, and alkali lye adjusts the pH to 8 ~ 9 of catalyst pulp, to regulation pH Bonding agent is added in catalyst pulp afterwards, then cellular skeleton structure is put into the catalyst pulp for adding bonding agent and surpassed Sound impregnates 4 ~ 5 hours, and the cellular skeleton structure is cordierite ceramic honeycomb carrier, then takes out and is done at 100 ~ 120 DEG C Dry 5 hours, repeat above-mentioned dipping, drying process 2 ~ 3 times, room is cooled to after finally calcining 4 ~ 7 hours at 400 ~ 500 DEG C Temperature, that is, the SCR denitration for alveolate texture is obtained, wherein, in the preparation process of catalyst pulp, natural siderite The weight of particle is the 30 ~ 50% of distilled water weight, and the dosage of the bonding agent is 1% of the catalyst pulp weight after regulation pH ~5%；Described bonding agent is any one in colloidal alumina, cataloid, polyvinyl alcohol and carboxymethyl cellulose It is or several.
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| CN105214670B (en) * | 2015-10-14 | 2018-03-20 | 东南大学 | Preparation and method of testing using former iron ore as the middle low temperature support type denitrating catalyst of carrier |
| CN107282066A (en) * | 2016-04-13 | 2017-10-24 | 安徽工业大学 | A kind of SCR denitration and its methods for making and using same based on Natural Manganese iron ore |
| CN105854894A (en) * | 2016-04-15 | 2016-08-17 | 东南大学 | Modified iron-ore SCR denitration catalyst and preparing method and application thereof |
| CN107185549B (en) * | 2017-05-12 | 2020-03-31 | 东南大学 | Modified siderite SCR denitration catalyst and preparation method and application thereof |
| CN108837839B (en) * | 2018-05-03 | 2020-09-11 | 东南大学 | Low-temperature flaky SCR denitration catalyst and SPS (semi-permeable plasma) tabletting preparation method and application thereof |
| CN112495406A (en) * | 2020-12-10 | 2021-03-16 | 重庆大学 | Manganese slag low-temperature denitration catalyst and preparation method thereof |
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| US4793981A (en) * | 1986-11-19 | 1988-12-27 | The Babcock & Wilcox Company | Integrated injection and bag filter house system for SOx -NOx -particulate control with reagent/catalyst regeneration |
| JP4617253B2 (en) * | 2005-12-26 | 2011-01-19 | エヌ・イーケムキャット株式会社 | NOx removal catalyst, honeycomb structure type NOx removal catalyst, and NOx removal method using the same |
| KR100781726B1 (en) * | 2006-09-15 | 2007-12-03 | 한국중부발전(주) | Method for manufacturing de-nox scr coating catalyst using porous ceramic substrate |
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