CN104084213B - For the method for making of ferrimanganic titanium catalyst and the catalyst of preparation thereof of the denitration of stationary source flue gas low-temperature - Google Patents
For the method for making of ferrimanganic titanium catalyst and the catalyst of preparation thereof of the denitration of stationary source flue gas low-temperature Download PDFInfo
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Abstract
CTAB auxiliary under, prepare FMT (S) composite oxide catalysts by coprecipitation, when air speed is 30000mLg
– 1h
– 1time, the conversion ratio of gained composite oxide catalysts when 100-350 DEG C reaches 100%, and selective when 75-200 DEG C reaches more than 80%, and has good water repelling property, has certain application prospect in low-temperature denitration field.The invention discloses its method for making.
Description
Technical field
The present invention relates to a kind of ferrimanganic titanium catalyst of low-temperature denitration, be applicable to the denitrating flue gas of the stationary sources such as coal-burning power plant.
Background technology
Nitrogen oxide (NO
x) mainly comprise NO and NO
2, be one of Air Pollutants.According to estimates, the whole world is discharged into the NO in air every year
xmeasure about 5,800 ten thousand tons.NO
xbe not only the main cause forming nitric acid type acid rain, be also damage the ozone layer, one of the main source forming photochemical fog, have very strong toxicity, to human body, healthy and ecological environment balances in serious threat.By sources divide, nitrogen oxide comprises moving source and stationary source two class.Moving source mainly refers to motor-vehicle tail-gas, and stationary source is then of a great variety, comprises coal-burning power plant, cement kiln, steel mill and glass factory etc.In China, along with the quickening of process of industrialization, a large amount of uses of coal resources, make to be discharged into NO in air
xtrend in cumulative year after year.Statistics shows, and stationary source fume emission has become the primary source of China's nitrogen oxide.Therefore, the nitrogen oxide in purification stationary source flue gas is extremely urgent and become one of focus of the current efforts at environmental protection of China, to improvement haze, alleviates atmosphere pollution and has great importance.
In stationary source fume emission is administered, industrial what generally adopt is ammonia (urea) SCR technology, i.e. NH
3(Urea)-SCR.Current business-like NH
3-SCR catalyst is V
2o
5-WO
3(MoO
3)/TiO
2, due to the relation of this catalyst activity temperature, make it can only be applicable to middle temperature (350-400 DEG C) denitration.Also Just because of this, before its denitration unit is arranged on dedusting and desulfurization.But V
2o
5-WO
3(MoO
3)/TiO
2in use there are following problems in catalyst:
1, in practical application, the active temperature range of this catalyst is between 350-400 DEG C, and scope is narrower usually can not meet the larger requirement of variations in temperature under service condition.
2, in high temperature range, such catalyst nitrogen selective is poor.
3, vanadium pentoxide strong toxicity, easily causes environmental pollution.
4, SO
2be converted into SO
3again with excessive NH
3easily there is sulfur poisoning in reaction, makes catalysqt deactivation.Result in financial cost and energy consumption increase.
5, in stationary source emission, flue dust is more, often in flue dust easily causes the material of this catalyst poisoning to cover catalyst surface containing alkali metal or alkaline earth metal compound etc., shortens catalyst service life.
If can invent a kind of catalyst, make its active temperature range be reduced to a certain degree, after its denitrification apparatus can be arranged at desulfurization and dust arrester, thus minimizing sulphur, flying dust etc. are poisoned catalyst contamination.At present, under low temperature with NH
3as reducing agent, carry out Selective catalytic reduction (NH
3-SCR) catalyst research and development are focuses of stationary source denitration research, during using manganese species as active component, manganese oxide based catalyst is due at low temperature NH
3show superior catalytic activity in-SCR reaction and receive much attention.Donovan etc. respectively by V, Cr, Mn, Fe, Cu, Ni, Co load at anatase TiO
2on.Through comparing display, when temperature is 120 DEG C, various metal oxide-loaded activity is: Mn>Cu>Cr>CoGre atT.GreaT.GTFe>V>Ni, Mn/TiO
2activity is the highest, generates N
2selective and NO conversion ratio is all 100%.Kang etc. take sodium carbonate as precipitating reagent, and adopt the precipitation method, calcining heat is 260-350 DEG C and has prepared MNOx catalyst.Find that catalyst has larger specific area, higher Mn load capacity and Surface Oxygen load capacity and high-valence state Mn species (Mn through characterizing
2o
3and Mn
3o
4), the conversion ratio of its temperature NO 150 DEG C ~ 200 DEG C time is more than 90%.N
2selective about 90 DEG C reach 100%.
But low temperature NH at present
3there is the deficiency with further aspect or several respects in-SCR catalyst: first, active temperature is low not.In actual applications, the gas temperature that stationary source flue gas discharges after dedusting, desulfurization, usually below 150 DEG C, even reaches less than 100 DEG C sometimes, and the catalyst of great majority research at present can not reach such requirement; Secondly, catalyst choice is good not, has the conversion ratio that many catalyst can reach, but it is selective bad; Finally, the stability of catalyst is good not, the water-resistance particularly under low temperature.Be difficult at present find a low-temperature denitration catalyst that simultaneously can meet these three conditions.
Summary of the invention
The object of this invention is to provide a kind of catalyst that can be widely used in stationary source, particularly coal-burning power plant's low-temp tail gas denitration.
Principle of the present invention is as follows: affect NH
3the principal element of-SCR activity has: sour position and the acid of catalyst are measured, the oxidation-reduction quality, specific area, active intermediate kind etc. of catalyst.Prepare low-temperature denitration catalyst just to set about from following several respects: 1, increase specific surface area of catalyst and pore volume, be conducive to like this increasing the avtive spot in unit are, improve reactant molecule diffusivity in the catalyst, thus be conducive to fast reaction speed; 2, increase the amount of the Lewis acid position of catalyst surface, according to existing document, Lewis acid position is conducive to low-temperature SCR reaction; 3, strengthen the redox property of catalyst, being particularly oxidized NO is NO
2ability, be conducive to like this forming quick NH
3-SCR reacts, thus fast reaction speed; 4, set about from middle species, according to existing data, nitrite species easily decompose at low temperatures, if can generate species in the middle of nitrite, are conducive to low temperature NH
3-SCR reacts.
Technical scheme of the present invention is as follows:
For a ferrimanganic titanium catalyst for stationary source flue gas low-temperature denitration, its typical recipe is as follows:
Get 0.0025 ~ 0.01molFe (NO
3)
39H
2o, 0.0025 ~ 0.01molMn (Ac)
24H
2o and 0.05molTi (SO
4)
2be dissolved in CTAB solution, wherein the mol ratio of Fe and Mn is 1:4 ~ 4:1, the mol ratio of Fe and Mn and Ti is 1 ~ 4:10, dissolve follow-up stirring 30 minutes, then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole course of reaction, system stirs 3 hours with the speed of 300rpm, gained mixture after filtration, after distilled water and absolute ethanol washing, 110 DEG C of air dryings 12 hours, be put in again in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, be cooled to normal temperature, final product is through compressing tablet, 40-60 order sieves, obtain the ferrimanganic titanium catalyst FMT (S) for the denitration of stationary source flue gas low-temperature.
More than one state the ferrimanganic titanium catalyst for the denitration of stationary source flue gas low-temperature prepared by method for making, TiO in described catalyst
2crystal based on anatase, the crystal containing a small amount of Rutile Type, other oxide species with dispersed form exist, the specific area of described catalyst can up to 100m
2/ more than g.
Cationic surfactant softex kw (CTAB) has hydrophilic N
+positive charge and oil loving alkyl functional group, at catalyst preparing by journey, by adding of CTAB cationic surfactant, the low temperature active of catalyst can be improved from the following aspects.The first, the isoelectric point of metallic iron, manganese, titanium oxide is generally less than 8; as the PH>9 of solution; its oxide surface is electronegative; when adding cationic surfactant softex kw (CTAB); its cation is easily adsorbed on the surface of particle; form layer protective layer; hinder growing up further of crystal grain; easily form little micelle between surfactant simultaneously; be conducive to the formation of pore passage structure, thus form larger specific area and pore volume.The second, be conducive to stoping manganese to TiO adding of CTAB
2inductive effect, thus form more anatase TiO
2crystal formation, and reduce rutile TiO
2the generation of crystal formation.Three, be conducive to forming more Lewis acid position adding of CTAB, thus be conducive to NH
2species, are more conducive to low-temperature decomposition.Four, be conducive to forming labile nitrite species under low temperature adding of CTAB.Five, be conducive to increasing Lattice Oxygen quantity adding of CTAB, strengthen redox property.
Feature of the present invention is: in catalyst preparation process, employ cationicsurfactants, the catalyst low-temperature activity of obtained specific composition and better selective.
Accompanying drawing explanation
Fig. 1 FMT and FMT (S) composite oxide catalysts is at NH
3nO conversion ratio in-SCR reaction.Reaction condition: [NO]=[NH
3]=500ppm, [O
2]=5%, N
2balance, catalyst quality=200mg, total flow rate=100mLmin
-1, air speed=30,000mLg
– 1h
– 1.
Fig. 2 FMT and FMT (S) composite oxide catalysts is at NH
3n in-SCR reaction
2selective.Reaction condition: [NO]=[NH
3]=500ppm, [O
2]=5%, N
2balance, catalyst quality=200mg, total flow rate=100mLmin
-1, air speed=30,000mLg
– 1h
– 1.
Fig. 3 FMT (S) is catalyst, the NH in water flowing situation
3the conversion ratio of NO in-SCR reaction.Reaction condition: [NO]=[NH
3]=500ppm, [O
2]=5%, N
2balance, the quality of catalyst is 200 milligrams, and overall flow rate is 100mlmin
-1, [H
2o]=3.5%, GHSV=30,000h
-1, T=150 DEG C.
Fig. 4 in 500 DEG C of roasting situations, the XRD characterization result of composite oxide catalysts FMT (S) and FMT.
The pore size distribution result of Fig. 5 composite oxide catalysts FMT (S) and FMT.
The characterization result of Fig. 6 composite oxide catalysts FMT (S) and FMT Adsorption and desorption isotherms.
Fig. 7 catalyst FMT (S) ammonia absorption original position diffuse reflection characterization result.
During Figure 81 25 DEG C, after the absorption of catalyst FMT (S) ammonia is saturated, pass into NO+O
2original position diffuse reflection characterization result.
During Figure 91 25 DEG C, after catalyst FMT (S) NO absorption is saturated, pass into NH
3+ O
2original position diffuse reflection characterization result.
In Figure 10 catalyst FMT (S), H
2the result of temperature programmed desorption.
Detailed description of the invention
Embodiment 1:
Get 0.015molCTAB to add in 400mL distilled water, obtain CTAB solution.Get 0.005molFe (NO
3)
39H
2o, 0.005molMn (Ac)
24H
2o, 0.05molTi (SO
4)
2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then mixed liquor " dropwise " being instilled mass percentage concentration is in the 150ml ammonia solution of 25%, and maintain pH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and obtains the ferrimanganic titanium catalyst FMT (S) for the denitration of stationary source flue gas low-temperature.
Embodiment 2:
In order to compare the effect preparing sample, prepare FMT catalyst by coprecipitation, its method is as follows simultaneously: get 0.005molFe (NO
3)
39H
2o, 0.005molMn (AC)
24H
2o, 0.05molTi (SO
4)
2dissolve follow-up stirring in aqueous 30 minutes.Then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product sieves through compressing tablet, 40-60 order, obtained low-temperature denitration catalyst FMT.
The product of embodiment 1 and embodiment 2 is carried out respectively to the activity and selectivity test of denitration, water-resistance is tested, and carries out the sign such as nitrogen adsorption desorption, wide-angle XRD, TPR, InsituDRIFTS to product.Result is shown in accompanying drawing 1-10 respectively.Fig. 1 and 2 result illustrates that the low-temperature catalytic activity of catalyst FMT (S) is much better than catalyst FMT, when air speed is 30000mLg
– 1h
– 1time, the conversion ratio of gained FMT (S) composite oxide catalysts when 100-350 DEG C reaches 100%, and selective when 75-200 DEG C reaches more than 80%.Fig. 3 result illustrates that FMT (S) composite oxide catalysts has good water repelling property.Fig. 4 XRD result shows: CTAB adds the generation suppressing Rutile Type, iron species and composite oxides exist with amorphous form and are well dispersed in the surface of catalyst, FMT (S) catalyst surface has how active high volence metal ion, and low temperature active is good.Fig. 5 and 6 is tested by nitrogen adsorption desorption, can find that the specific area of product of the present invention can up to 109m
2/ more than g, the specific area that commonsense method prepares sample only has 15m
2/ g.Pore size distribution and pore volume viewed from BJH test result, the aperture of inventive samples is little, and pore volume is large, and CTAB adds, and increases catalyst surface active site quantity, improves reactant gas diffusion property in the catalyst, is conducive to the raising of the activity of catalyst.Fig. 7 ammonia adsorption experiment illustrates that FMT (S) composite oxide catalysts surface is based on Lewis acid position.Fig. 8 and 9 illustrates the NH of Lewis acid position absorption
2with the active intermediate kind that nitrite is reaction.Figure 10 illustrates that FMT (S) composite oxide catalysts has better redox property.
Embodiment 3:
Get in 0.015molCTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.0025molFe (NO
3)
39H
2o, 0.0025molMn (AC)
24H
2o, 0.05molTi (SO
4)
2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, obtained low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 4:
Get in 0.003molCTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.005molFe (NO
3)
39H
2o, 0.005molMn (AC)
24H
2o, 0.05molTi (SO
4)
2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, obtained low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 5:
Get in 0.075molCTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.0075molFe (NO
3)
39H
2o, 0.0075molMn (AC)
24H
2o, 0.05molTi (SO
4)
2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, obtained low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 6:
Get in 0.015molCTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.01molFe (NO
3)
39H
2o, 0.01molMn (AC)
24H
2o, 0.05molTi (SO
4)
2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, obtained low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 7:
Get in 0.015molCTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.0025molFe (NO
3)
39H
2o, 0.01molMn (AC)
24H
2o, 0.05molTi (SO
4)
2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, obtained low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 8:
Get in 0.015molCTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.01molFe (NO
3)
39H
2o, 0.0025molMn (AC)
24H
2o, 0.05molTi (SO
4)
2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, obtained low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 9:
Get in 0.015molCTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.0075molFe (NO
3)
39H
2o, 0.0025molMn (AC)
24H
2o, 0.05molTi (SO
4)
2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then by mixed liquor " dropwise " instillation ammonia (25%) solution 150ml, maintain PH>9, in whole reaction, system stirs 3 hours with the speed of 300rpm.Gained mixture after filtration, distilled water and absolute ethanol washing repeatedly after, 110 DEG C of air dryings 12 hours, then be put in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, obtained low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Claims (2)
1., for a method for making for the ferrimanganic titanium catalyst of stationary source flue gas low-temperature denitration, it is characterized in that it comprises the steps: that getting 0.003 ~ 0.075molCTAB adds in 400mL distilled water, obtains CTAB solution, get 0.0025 ~ 0.01molFe (NO
3)
39H
2o, 0.0025 ~ 0.01molMn (Ac)
24H
2o and 0.05molTi (SO
4)
2be dissolved in CTAB solution, wherein the mol ratio of Fe and Mn is 1:4 ~ 4:1, the mol ratio of Fe and Mn and Ti is 1 ~ 4:10, dissolve follow-up stirring 30 minutes, then mixed liquor " dropwise " is instilled in 25% ammonia solution 150ml, maintain pH>9, in whole course of reaction, system stirs 3 hours with the speed of 300rpm, gained mixture after filtration, after distilled water and absolute ethanol washing, 110 DEG C of air dryings 12 hours, be put in again in Muffle furnace, heat up with the firing rate of 2 DEG C/min, 500 DEG C of roasting 6h, be cooled to normal temperature, final product is through compressing tablet, 40-60 order sieves, obtain the ferrimanganic titanium catalyst for the denitration of stationary source flue gas low-temperature.
2., with the ferrimanganic titanium catalyst for the denitration of stationary source flue gas low-temperature prepared by method for making described in claim 1, it is characterized in that: TiO in described catalyst
2crystal based on anatase, the crystal containing a small amount of Rutile Type, other oxide species with dispersed form exist, the specific area of described catalyst is up to 100m
2/ more than g.
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| CN104971730A (en) * | 2015-06-24 | 2015-10-14 | 方耀 | Catalyst for reducing nitrogen oxides in coal-fired flue gas by ammonia gas |
| CN105854895A (en) * | 2016-04-19 | 2016-08-17 | 四川大学 | Medium and low temperature composite oxide SCR denitration catalyst and preparation method thereof |
| CN105903478B (en) * | 2016-05-11 | 2020-10-13 | 四川大学 | Medium-low temperature SCR catalyst with wider use temperature and preparation method thereof |
| CN113751019A (en) * | 2021-09-28 | 2021-12-07 | 四川恒泰环境技术有限责任公司 | Denitration catalyst, preparation method and application thereof |
| CN114515579A (en) * | 2022-03-11 | 2022-05-20 | 黑龙江大学 | Preparation method of catalyst for low-temperature catalytic oxidation of volatile organic compounds |
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