CN104084213A - Preparation method of iron manganese titanium catalyst for denitrating fixed-source smoke at low temperature and catalyst prepared through preparation method - Google Patents

Preparation method of iron manganese titanium catalyst for denitrating fixed-source smoke at low temperature and catalyst prepared through preparation method Download PDF

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CN104084213A
CN104084213A CN201410310147.0A CN201410310147A CN104084213A CN 104084213 A CN104084213 A CN 104084213A CN 201410310147 A CN201410310147 A CN 201410310147A CN 104084213 A CN104084213 A CN 104084213A
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catalyst
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ctab
denitration
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CN104084213B (en
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董林
伍士国
汤常金
高飞
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Nanjing University
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Abstract

The invention relates to an iron manganese titanium catalyst. The FMT(S) composite oxide catalyst is prepared by utilizing a co-precipitation method under the assistance of CTAB (cetyltrimethyl ammonium bromide); when the airspeed is 30000mL.g<-1>.h<-1>, the conversion rate of the prepared composite oxide catalyst at the temperature of 100 to 350 DEG C reaches 100 percent, the selectivity at the temperature of 75 to 200 DEG C reaches more than 80 percent; moreover, the prepared iron manganese titanium catalyst is good in water resistance and good in application prospect in the field of low-temperature denitration. The invention also discloses a preparation method of the iron manganese titanium catalyst.

Description

The method for making of ferrimanganic titanium catalyst and the catalyst of preparation thereof for the denitration of stationary source flue gas low-temperature
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 atmosphere every year xmeasure approximately 5,800 ten thousand tons.NO xbeing not only the main cause that forms nitric acid type acid rain, is also to damage the ozone layer, form one of main source of photochemical fog, has very strong toxicity, and serious threat is healthy and ecological environment balance to human body.By sources divide, nitrogen oxide comprises moving source and stationary source two classes.Moving source mainly refers to motor-vehicle tail-gas, and stationary source is 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 atmosphere xthe trend that is cumulative year after year.Statistics demonstration, stationary source fume emission has become the primary source of China's nitrogen oxide.Therefore, purify nitrogen oxide in stationary source flue gas extremely urgent and become one of focus of the current efforts at environmental protection of China, to administering haze, alleviate atmosphere pollution and have great importance.
In stationary source fume emission is administered, industrial that 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 ℃) 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 scope of this catalyst is between 350-400 ℃, 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 is selectively 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.Caused financial cost and energy consumption to increase.
5, in stationary source emission, flue dust is more, often contains alkali metal or alkaline earth metal compound etc. and easily cause that the material of this catalyst poisoning covers catalyst surface in flue dust, shortens catalyst service life.
If can invent a kind of catalyst, its active temperature scope is reduced to a certain degree, after its denitrification apparatus can be arranged at desulfurization and dust arrester, thereby reduce sulphur, flying dust etc., catalyst contamination is poisoned.At present, under low temperature with NH 3as reducing agent, carry out selective catalysis reduction (NH 3-SCR) catalyst research and development are focuses of stationary source denitration research, using manganese species during as active component, and manganese oxide based catalyst is due at low temperature NH 3in-SCR reaction, show superior catalytic activity and receive much attention.Donovan philosophy loads on anatase TiO by V, Cr, Mn, Fe, Cu, Ni, Co 2on.Through relatively showing, when temperature is 120 ℃, various metal oxide-loaded activity are: 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. be take sodium carbonate as precipitating reagent, adopt the precipitation method, and calcining heat is 260-350 ℃ and has prepared MNOx catalyst.Through characterize finding that catalyst has larger specific area, higher Mn load capacity and Surface Oxygen load capacity and high valence state Mn species (Mn 2o 3and Mn 3o 4), the conversion ratio of its temperature NO in the time of 150 ℃～200 ℃ is more than 90%.N 2selective 90 ℃ of left and right reach 100%.
But current low temperature NH 3there is the deficiency of on the one hand following 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 below 150 ℃, even reaches below 100 ℃ conventionally sometimes, and the catalyst of most research can not reach such requirement; Secondly, catalyst selectivity is good not, the conversion ratio that has many catalyst to have reached, but it is selectively bad; Finally, the stability of catalyst is good not, particularly the water-resistance under low temperature.Be difficult at present the low-temperature denitration catalyst that finds can simultaneously meet these three conditions.
Summary of the invention
The object of this invention is to provide and a kind ofly can be widely used in stationary source, the particularly catalyst of 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: the oxidation-reduction quality of the acid position of catalyst and acid amount, catalyst, specific area, active in the middle of species etc.Preparing low-temperature denitration catalyst just must set about from following several respects: 1, increase specific surface area of catalyst and pore volume, be conducive to like this increase the avtive spot in unit are, improve the diffusivity of reactant molecule in catalyst, thereby 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, the redox property that strengthens catalyst, being particularly oxidized NO is NO 2ability, be conducive to like this form quick NH 3-SCR reaction, thereby fast reaction speed; 4, from middle species, set about, according to existing data, nitrite species easily decompose at low temperatures, if can generate the middle species of nitrite, are conducive to low temperature NH 3-SCR reaction.
Technical scheme of the present invention is as follows:
For a ferrimanganic titanium catalyst for stationary source flue gas low-temperature denitration, its typical method for making is as follows:
Get 0.0025～0.01mol Fe (NO 3) 39H 2o, 0.0025～0.01mol Mn (Ac) 24H 2o and 0.05mol Ti (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 splashed in 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 ℃ of air dryings 12 hours, be put in again in Muffle furnace, firing rate with 2 ℃/min heats up, 500 ℃ of roasting 6h, be cooled to normal temperature, final product is through compressing tablet, 40-60 order sieves, make 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 take anatase as main, the crystal that contains a small amount of Rutile Type, other oxide species exists with dispersed form, the specific area of described catalyst can be up to 100m 2more than/g.
Cationic surfactant softex kw (CTAB) has hydrophilic N +positive charge and oil loving alkyl functional group, in catalyst preparation, by journey, by adding of CTAB cationic surfactant, can improve from the following aspects the low temperature active of catalyst.The first, the isoelectric point of metallic iron, manganese, titanium oxide is generally less than 8; when the PH>9 of solution; its oxide surface is electronegative; while adding cationic surfactant softex kw (CTAB); its cation is easily adsorbed on the surface of particle; form layer protective layer; hinder further growing up of crystal grain; between surfactant, easily form little micelle simultaneously; be conducive to the formation of pore passage structure, thereby form larger specific area and pore volume.The second, be conducive to stop manganese to TiO adding of CTAB 2inductive effect, thus more anatase TiO formed 2crystal formation, and reduce rutile TiO 2the generation of crystal formation.Three, be conducive to form more Lewis acid position adding of CTAB, thereby be conducive to NH 2species, are more conducive to low-temperature decomposition.Four, be conducive to form labile nitrite species under low temperature adding of CTAB.Five, be conducive to increase Lattice Oxygen quantity adding of CTAB, strengthen redox property.
Feature of the present invention is: in catalyst preparation process, used cationicsurfactants, the catalyst low-temperature activity of the specific composition making 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 2selectively.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, overall flow rate is 100ml min -1, [H 2o]=3.5%, GHSV=30,000h -1, T=150 ℃.
Fig. 4 in 500 ℃ 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 25 ℃ of Figure 81, after the absorption of catalyst FMT (S) ammonia is saturated, pass into NO+O 2original position diffuse reflection characterization result.
During 25 ℃ of Figure 91, 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.
The specific embodiment
Embodiment 1:
Get 0.015molCTAB and 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 " is splashed into mass percentage concentration and be in 25% 150ml ammonia solution, 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and makes the ferrimanganic titanium catalyst FMT (S) for the denitration of stationary source flue gas low-temperature.
Embodiment 2:
In order relatively to prepare the effect of sample, by coprecipitation, prepare FMT catalyst simultaneously, its method is as follows: get 0.005molFe (NO 3) 39H 2o, 0.005mol Mn (AC) 24H 2o, 0.05molTi (SO 4) 2be dissolved in the aqueous solution follow-up stirring 30 minutes.Then mixed liquor " dropwise " is splashed in 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product sieves through compressing tablet, 40-60 order, makes 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 test, and product is carried out to the signs such as nitrogen adsorption desorption, wide-angle XRD, TPR, In situ DRIFTS.Result is shown in respectively accompanying drawing 1-10.The low-temperature catalytic activity of Fig. 1 and 2 presentation of results 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 in the time of 100-350 ℃ reaches 100%, selectively reaching more than 80% in the time of 75-200 ℃.Fig. 3 presentation of results FMT (S) composite oxide catalysts has good water repelling property.Fig. 4 XRD result shows: CTAB adds the generation that suppresses Rutile Type, with amorphous form, there is and be well dispersed in the surface of catalyst in iron species and composite oxides, FMT (S) catalyst surface has how active high volence metal ion, and low temperature active is good.Fig. 5 and 6 tests by nitrogen adsorption desorption, can find that the specific area of product of the present invention can be up to 109m 2more than/g, commonsense method is prepared the specific area of sample and is only had 15m 2/ g.From BJH test result, see pore size distribution and pore volume, the aperture of sample of the present invention is little, and pore volume is large, and CTAB adds, and has increased catalyst surface active site quantity, has improved the diffusion property of reactant gas in catalyst, is conducive to the active raising of catalyst.Lewis acid position be take as main in Fig. 7 ammonia adsorption experiment explanation FMT (S) composite oxide catalysts surface.The NH of Fig. 8 and 9 explanation Lewis acid position absorption 2with nitrite be reaction activity in the middle of species.Figure 10 illustrates that FMT (S) composite oxide catalysts has better redox property.
Embodiment 3:
Get in 0.015mol CTAB 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 mixed liquor " dropwise " is splashed in 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and makes 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, 0.005mol Mn (AC) 24H 2o, 0.05mol Ti (SO 4) 2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then mixed liquor " dropwise " is splashed in 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and makes low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 5:
Get in 0.075mol CTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.0075mol Fe (NO 3) 39H 2o, 0.0075mol Mn (AC) 24H 2o, 0.05mol Ti (SO 4) 2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then mixed liquor " dropwise " is splashed in 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and makes low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 6:
Get in 0.015mol CTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.01mol Fe (NO 3) 39H 2o, 0.01mol Mn (AC) 24H 2o, 0.05mol Ti (SO 4) 2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then mixed liquor " dropwise " is splashed in 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and makes low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 7:
Get in 0.015mol CTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.0025mol Fe (NO 3) 39H 2o, 0.01molMn (AC) 24H 2o, 0.05mol Ti (SO 4) 2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then mixed liquor " dropwise " is splashed in 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and makes low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 8:
Get in 0.015mol CTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.01mol Fe (NO 3) 39H 2o, 0.0025mol Mn (AC) 24H 2o, 0.05mol Ti (SO 4) 2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then mixed liquor " dropwise " is splashed in 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and makes low-temperature denitration catalyst FMT (S).Its test result is as embodiment 1.
Embodiment 9:
Get in 0.015mol CTAB to 400ml distilled water, obtain CTAB solution.Get appropriate 0.0075mol Fe (NO 3) 39H 2o, 0.0025mol Mn (AC) 24H 2o, 0.05mol Ti (SO 4) 2be dissolved in the follow-up stirring of CTAB solution 30 minutes.Then mixed liquor " dropwise " is splashed in 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 ℃ of air dryings 12 hours, then be put in Muffle furnace, with the firing rate of 2 ℃/min, heat up, 500 ℃ of roasting 6h, are cooled to normal temperature.Final product is through compressing tablet, and 40-60 order sieves, and makes 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:
Get 0.003～0.075mol CTAB and add in 400mL distilled water, obtain CTAB solution, get 0.0025～0.01molFe (NO 3) 39H 2o, 0.0025～0.01mol Mn (Ac) 24H 2o and 0.05mol Ti (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 splashed in 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 ℃ of air dryings 12 hours, be put in again in Muffle furnace, firing rate with 2 ℃/min heats up, 500 ℃ of roasting 6h, be cooled to normal temperature, final product is through compressing tablet, 40-60 order sieves, make the ferrimanganic titanium catalyst FMT (S) for the denitration of stationary source flue gas low-temperature.
2. the ferrimanganic titanium catalyst for the denitration of stationary source flue gas low-temperature of preparing with method for making described in claim 1, is characterized in that: TiO in described catalyst 2crystal take anatase as main, the crystal that contains a small amount of Rutile Type, other oxide species exists with dispersed form, the specific area of described catalyst can be up to 100m 2more than/g.
CN201410310147.0A 2014-07-01 2014-07-01 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 Expired - Fee Related CN104084213B (en)

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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
CN105903478A (en) * 2016-05-11 2016-08-31 四川大学 Medium and low temperature SCR (selective catalytic reduction) catalyst with wide use temperature 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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