CN106311213A - Sulfur-resistant and water-resistant low-temperature denitration catalyst and preparation method thereof - Google Patents
Sulfur-resistant and water-resistant low-temperature denitration catalyst and preparation method thereof Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
The invention provides a sulfur-resistant and water-resistant low-temperature denitration catalyst and a preparation method thereof to solve the problems that the catalytic efficiency of denitration catalysts in the prior art under the low-temperature condition does not reach the standard and the sulfur resistance and water resistance are poor in particular. The molecular formula of the low-temperature denitration catalyst is MV2O4, wherein M is any one of Fe, Cu, Mn, Co and Cr. The low-temperature denitration catalyst is prepared from metal nitrate and vanadium pentoxide through ball milling, acidification, calcination and the like, the denitration efficiency within the temperature range of 120-250 DEG C is 90% or above on the basis of detection, and the low-temperature denitration catalyst has higher water resistance and sulfur resistance.
Description
Technical field
The invention belongs to denitrating catalyst preparing technical field, be specifically related to the low-temperature denitration catalyst of a kind of sulfur resistive water resistant
And preparation method thereof.
Background technology
Nitrogen oxides (NOx) it is one of Air Pollutants causing acid rain, photochemical fog, depletion of the ozone layer, right
Health and ecological environment produce serious harm, the most effectively control and reduce NOxDischarge receive various countries' researcher
Concern.
In nitrogen oxides pollution control technology, SCR (SCR) method be most widely used general, technology is the most ripe
Method.And SCR technology remove NOx's it is crucial that catalyst performance quality.The most commercial vanadium titanium denitrating catalyst (V2O5/
TiO2) superior at middle-temperature section (300～450 DEG C) catalytic performance.Substantial amounts of Industrial Boiler, such as coke oven flue gas, iron and steel, cement, glass
The industries such as glass, petrochemical industry, nitric acid production, owing to temperature is relatively low, high temperature denitrating catalyst in causing directly using.Develop novel
Low-temperature denitration catalyst, and keep the high activity of low-temperature denitration catalyst, high stability, sulfur resistive water-resistance be badly in need of solve difficulty
Point.
Metal-oxide such as MnO for low-temperature denitration catalystx、CeOx、Fe2O3、CrOxDeng, the most all tables
Reveal preferable activity, but anti-SO2Poisoning capability is poor.Chinese patent 201610133201.8 is prepared for Mn-Ce/TiO2Catalysis
Agent, within the temperature range of 100-220 DEG C, denitration efficiency reaches 55% ~ 90%, but does not carries out sulfur resistive water-resistance investigation.Chinese patent
101879452A is prepared for MnFeSnCeOxLow-temperature denitration catalyst, within the temperature range of 80 ~ 250 DEG C, nitrogen oxides clean
Change efficiency and reach 71% ~ 100%, there is good sulfur resistance, but water-resistance is not investigated.
Summary of the invention
The present invention is directed to denitrating catalyst of the prior art catalytic efficiency under cryogenic the most up to standard, the most anti-
The problem of sulfur water-resistance difference, it is provided that low-temperature denitration catalyst of a kind of sulfur resistive water resistant and preparation method thereof, this low-temperature denitration is catalyzed
Agent denitration efficiency within the temperature range of 120 ~ 250 DEG C reaches more than 90%, and has stronger water resistant sulfur resistive ability.
The present invention adopts the following technical scheme that
The low-temperature denitration catalyst of a kind of sulfur resistive water resistant, the molecular formula of described low-temperature denitration catalyst is MV2O4, wherein, M is
Any one in Fe, Cu, Mn, Co and Cr.
The preparation method of the low-temperature denitration catalyst of a kind of sulfur resistive water resistant, comprises the following steps:
(1), under room temperature, slaine and vanadic anhydride are carried out ball milling, obtains ball-milled mixtures；
(2) after being vacuum dried by step (1) gained ball-milled mixtures, then under room temperature, carry out acidification, obtain acidifying mixture；
(3) being calcined by step (2) gained acidifying mixture, calcining is ground after terminating and is i.e. obtained described low-temperature denitration catalyst.
Wherein, slaine is 1:2 with the mol ratio of vanadic anhydride.
Further, described slaine is Fe (NO3)3、Cu(NO3)2、Mn(NO3)2、Co(NO3)2With Cr (NO3)2In appoint
Meaning one.
Further, the molecular formula of described low-temperature denitration catalyst is MV2O4, wherein, M is in Fe, Cu, Mn, Co and Cr
Any one.
Further, in described step (1), during ball milling, add 5 ~ 10mL glycerol, first in 300 ~ 500rad/min ball
Mill 30 ~ 60min, then in 200 ~ 300rad/min ball milling 4 ~ 6h.
Further, in described step (2), vacuum drying is 80 ~ 100 DEG C of dry 8 ~ 10h in vacuum drying oven.
Further, in described step (2), acidification is acidification 1 ~ 2h in the sulphuric acid of 0.5 ~ 3mol/L.
Further, in described step (3), during calcining, first 300 DEG C pre-burning 4 ~ 6h, take out after grinding, then at 600 ~
800 DEG C of calcining 6 ~ 8h.
Beneficial effects of the present invention is as follows:
Low-temperature denitration catalyst MV of the present invention2O4Denitration efficiency within the temperature range of 120 ~ 250 DEG C reaches more than 90%,
And there is stronger water resistant sulfur resistive ability.Specific to the preparation process of this catalyst, following advantage:
(1) present invention uses glycerol as dispersant, the low-temperature denitration catalyst MV prepared2O4For nano-particle, compare table
Area is big, and catalyst reaction contact area is big, it is possible to be effectively improved catalysis active, and in wider low temperature range (120 ~
250 DEG C) can show and be preferably catalyzed activity；
(2) mechanical milling process of the present invention divides multistage ball milling, and each component in gained ball-milled mixtures is uniformly dispersed, and active sites reaches
Effectively dispersion；
(3) each component in gained ball-milled mixtures has stronger interaction relationship, and acidified process, further
Increase denitration acidity active sites and sulfur resistive water-resistance；
(4) calcination process of the present invention is designed as many section calcinings, and is attended by grinding operation, it is ensured that the fineness of catalyst granules
With preferable crystal property, be conducive to improving its sulfur resistive water-resistance；
(5) preparation method of the present invention is simple, and raw material is readily available, it is easy to industrialized production, and environmental pollution is little, low cost, tool
There is stronger application value.
Accompanying drawing explanation
Fig. 1 is embodiment 1 gained FeV2O4Catalysis Activity determination result under different condition；
Fig. 2 is embodiment 2 gained CuV2O4Catalysis Activity determination result under different condition；
Fig. 3 is embodiment 3 gained MnV2O4Catalysis Activity determination result under different condition；
Fig. 4 is embodiment 4 gained CoV2O4Catalysis Activity determination result under different condition；
Fig. 5 is embodiment 5 gained CrV2O4Catalysis Activity determination result under different condition.
Detailed description of the invention
In order to make the technical purpose of the present invention, technical scheme and beneficial effect clearer, below in conjunction with the accompanying drawings and specifically
Technical scheme is further illustrated by embodiment, but described embodiment is intended to explain the present invention, and can not manage
Solving is limitation of the present invention, and unreceipted concrete technology or condition person in embodiment, described by the document in this area
Technology or condition or carry out according to product description, agents useful for same or instrument unreceipted production firm person, be and can pass through
City available from conventional products.
Embodiment 1: low-temperature denitration catalyst FeV2O4Preparation
(1) under room temperature, by Fe (NO3)3, vanadic anhydride adds in zirconia ball grinding jar according to 1:2 mol ratio, and adds 10mL
Dispersant made by glycerol, after first 500rad/min ball milling 30min, followed by 300rad/min ball milling 6h, obtains ball milling and mixes
Compound；
(2) by step (1) gained ball-milled mixtures after 100 DEG C of dry 8h of vacuum drying oven, then acid in 0.5mol/L sulphuric acid
Change processes 2h, obtains acidifying mixture；
(3) by step (2) gained acidifying mixture 300 DEG C of pre-burning 6h in Muffle furnace, take out after grinding, then 600 DEG C of calcining 8h,
Calcining is ground after terminating and is i.e. obtained described low-temperature denitration catalyst FeV2O4。
Embodiment 2: low-temperature denitration catalyst CuV2O4Preparation
(1) under room temperature, by Cu (NO3)2, vanadic anhydride adds in zirconia ball grinding jar according to 1:2 mol ratio, and adds 8mL
Dispersant made by glycerol, after first 300rad/min ball milling 60min, followed by 200rad/min ball milling 4h, obtains ball milling and mixes
Compound；
(2) by step (1) gained ball-milled mixtures after 80 DEG C of dry 10h of vacuum drying oven, then it is acidified in 3mol/L sulphuric acid
Process 1h, obtain acidifying mixture；
(3) by step (2) gained acidifying mixture 300 DEG C of pre-burning 4h in Muffle furnace, take out after grinding, then 800 DEG C of calcining 6h,
Calcining is ground after terminating and is i.e. obtained described low-temperature denitration catalyst CuV2O4。
Embodiment 3: low-temperature denitration catalyst MnV2O4Preparation
(1) under room temperature, by Mn (NO3)2, vanadic anhydride adds in zirconia ball grinding jar according to 1:2 mol ratio, and adds 5mL
Dispersant made by glycerol, after first 400rad/min ball milling 45min, followed by 300rad/min ball milling 6h, obtains ball milling and mixes
Compound；
(2) by step (1) gained ball-milled mixtures after 100 DEG C of dry 10h of vacuum drying oven, then it is acidified in 3mol/L sulphuric acid
Process 2h, obtain acidifying mixture；
(3) by step (2) gained acidifying mixture 300 DEG C of pre-burning 4h in Muffle furnace, take out after grinding, then 600 DEG C of calcining 8h,
Calcining is ground after terminating and is i.e. obtained described low-temperature denitration catalyst MnV2O4。
Embodiment 4: low-temperature denitration catalyst CoV2O4Preparation
(1) under room temperature, by Co (NO3)2, vanadic anhydride adds in zirconia ball grinding jar according to 1:2 mol ratio, and adds 10mL
Dispersant made by glycerol, after first 500rad/min ball milling 60min, followed by 200rad/min ball milling 4h, obtains ball milling and mixes
Compound；
(2) by step (1) gained ball-milled mixtures after 100 DEG C of dry 8h of vacuum drying oven, then it is acidified in 2mol/L sulphuric acid
Process 2h, obtain acidifying mixture；
(3) by step (2) gained acidifying mixture 300 DEG C of pre-burning 5h in Muffle furnace, take out after grinding, then 750 DEG C of calcining 8h,
Calcining is ground after terminating and is i.e. obtained described low-temperature denitration catalyst CoV2O4。
Embodiment 5: low-temperature denitration catalyst CrV2O4Preparation
(1) under room temperature, by Cr (NO3)2, vanadic anhydride adds in zirconia ball grinding jar according to 1:2 mol ratio, and adds 10mL
Dispersant made by glycerol, after first 500rad/min ball milling 60min, followed by 300rad/min ball milling 6h, obtains ball milling and mixes
Compound；
(2) by step (1) gained ball-milled mixtures after 80 DEG C of dry 9h of vacuum drying oven, then in 1mol/L sulphuric acid at acidifying
Reason 2h, obtains acidifying mixture；
(3) by step (2) gained acidifying mixture 300 DEG C of pre-burning 6h in Muffle furnace, take out after grinding, then 700 DEG C of calcining 6h,
Calcining is ground after terminating and is i.e. obtained described low-temperature denitration catalyst CrV2O4。
Test example 1: " without sulfur+H2O 10% " under the conditions of catalyst activity detection
Low-temperature denitration catalyst embodiment 1 to 5 prepared carries out Activity determination, and test condition is: NO 500ppm, NH3
500ppm, O2 3%, H2O 10%, N2For Balance Air, air speed 20000h-1, detect temperature range 120 ~ 250 DEG C.
Test result (Fig. 1 to Fig. 5 respectively corresponding embodiment 1 to 5) as shown in Figures 1 to 5, be labeled as from figure without sulfur+
H2The broken line of O 10% is it can be seen that the low-temperature denitration catalyst for preparing of embodiment 1 to 5, " without sulfur+H2O 10% " (without sulfur
I.e. it is added without SO2Gas) under the conditions of denitration efficiency all more than 90%, and along with temperature raise (temperature range 120 ~ 250
DEG C), denitration efficiency improves the most therewith.
Test example 2: " 300ppm SO2+H2O 15% " under the conditions of catalyst activity detection
Low-temperature denitration catalyst embodiment 1 to 5 prepared carries out Activity determination, and test condition is: NO 500ppm,
NH3 500ppm, O2 3%, 300ppm SO2, H2O 15%, N2For Balance Air, air speed 20000h-1, detection temperature range 120 ~
250℃。
Test result (the most corresponding embodiment 1 to 5 of Fig. 1 to Fig. 5) as shown in Figures 1 to 5, is labeled as 300ppm from figure
SO2+H2The broken line of O 15% is it can be seen that the low-temperature denitration catalyst for preparing of embodiment 1 to 5, at " 300ppm SO2+H2O
15% " denitration efficiency under the conditions of remains to keep more than 90%, and along with temperature raises (temperature range 120 ~ 250 DEG C), denitration is imitated
Rate improves the most therewith, illustrates that gained low-temperature denitration catalyst has preferable sulfur resistive water-resistance.
It should be noted last that: above-described embodiment is merely to illustrate and unrestricted technical scheme, any right
The equivalent that the present invention is carried out and amendment or local without departing from spirit and scope of the invention are replaced, and it all should be contained at this
Within bright protective scope of the claims.
Claims (9)
1. the low-temperature denitration catalyst of a sulfur resistive water resistant, it is characterised in that: the molecular formula of described low-temperature denitration catalyst is
MV2O4, wherein, M is any one in Fe, Cu, Mn, Co and Cr.
2. the preparation method of the low-temperature denitration catalyst of a sulfur resistive water resistant, it is characterised in that comprise the following steps:
(1), under room temperature, slaine and vanadic anhydride are carried out ball milling, obtains ball-milled mixtures；
(2) after being vacuum dried by step (1) gained ball-milled mixtures, then under room temperature, carry out acidification, obtain acidifying mixture；
(3) being calcined by step (2) gained acidifying mixture, calcining is ground after terminating and is i.e. obtained described low-temperature denitration catalyst.
Wherein, slaine is 1:2 with the mol ratio of vanadic anhydride.
The preparation method of the low-temperature denitration catalyst of sulfur resistive water resistant the most according to claim 2, it is characterised in that: described metal
Salt is Fe (NO3)3、Cu(NO3)2、Mn(NO3)2、Co(NO3)2With Cr (NO3)2In any one.
The preparation method of the low-temperature denitration catalyst of sulfur resistive water resistant the most according to claim 3, it is characterised in that: described low temperature
The molecular formula of denitrating catalyst is MV2O4, wherein, M is any one in Fe, Cu, Mn, Co and Cr.
The preparation method of the low-temperature denitration catalyst of sulfur resistive water resistant the most according to claim 4, it is characterised in that: described step
(1), in, during ball milling, add 5 ~ 10mL glycerol, first in 300 ~ 500rad/min ball milling 30 ~ 60min, then in 200 ~
300rad/min ball milling 4 ~ 6h.
The preparation method of the low-temperature denitration catalyst of sulfur resistive water resistant the most according to claim 4, it is characterised in that: described step
(2), in, vacuum drying is 80 ~ 100 DEG C of dry 8 ~ 10h in vacuum drying oven.
The preparation method of the low-temperature denitration catalyst of sulfur resistive water resistant the most according to claim 4, it is characterised in that: described step
(2), in, acidification is acidification 1 ~ 2h in the sulphuric acid of 0.5 ~ 3mol/L.
The preparation method of the low-temperature denitration catalyst of sulfur resistive water resistant the most according to claim 4, it is characterised in that: described step
(3) in, during calcining, first 300 DEG C pre-burning 4 ~ 6h, take out after grinding, then at 600 ~ 800 DEG C of calcining 6 ~ 8h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107537514A (en) * | 2017-07-21 | 2018-01-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Ferromanganese cobalt monoblock type SCR low temperature catalysts preparation method, product and its application |
| CN107930619A (en) * | 2017-11-22 | 2018-04-20 | 常州大学 | A kind of porous spongy CrMnOXThe preparation of/aluminosilicate fiber cotton low-temperature denitration of flue gas catalyst |
| CN109351358A (en) * | 2018-10-18 | 2019-02-19 | 中国科学院城市环境研究所 | A kind of transition metal oxide composite catalyst and its preparation method and application |
| CN109663499A (en) * | 2019-02-15 | 2019-04-23 | 山东首丰环保设备有限公司 | Quadruple effect denitrfying agent composition and its method of denitration |
| CN113368898A (en) * | 2021-06-16 | 2021-09-10 | 福州大学 | Method for preparing high-water-resistance filter material by ball milling method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107930619A (en) * | 2017-11-22 | 2018-04-20 | 常州大学 | A kind of porous spongy CrMnOXThe preparation of/aluminosilicate fiber cotton low-temperature denitration of flue gas catalyst |
| CN109351358A (en) * | 2018-10-18 | 2019-02-19 | 中国科学院城市环境研究所 | A kind of transition metal oxide composite catalyst and its preparation method and application |
| CN109663499A (en) * | 2019-02-15 | 2019-04-23 | 山东首丰环保设备有限公司 | Quadruple effect denitrfying agent composition and its method of denitration |
| CN113368898A (en) * | 2021-06-16 | 2021-09-10 | 福州大学 | Method for preparing high-water-resistance filter material by ball milling method |
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