CN109529812A - A kind of SCR catalyst and preparation method suitable for high temperature high-humidity gas fume condition - Google Patents
A kind of SCR catalyst and preparation method suitable for high temperature high-humidity gas fume condition Download PDFInfo
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Abstract
一种适用于中高温高湿烟气条件的SCR催化剂及制备方法，属于催化剂制备技术领域。具体方法包括：将计算量的铈前驱体、钼前驱体、载体TiO2放入球磨罐中，球磨1‑6h，将混合均匀的粉体在马弗炉中分两步焙烧，得到MoO3‑CeO2/TiO2复合氧化物催化剂，其中CeO2含量为铈钛复合氧化物总量的5‑40wt％，MoO3含量为钼铈钛复合氧化物总量的0～10wt％。本发明所述的SCR催化剂在高湿度烟气条件下，NO转化率在中高温度区间(250‑500℃)保持在85％以上。本发明制备过程简单，条件易于控制，原料价格低廉，在脱硝领域有潜在应用价值。An SCR catalyst suitable for medium-high-temperature and high-humidity flue gas conditions and a preparation method thereof belong to the technical field of catalyst preparation. The specific method includes: putting calculated amounts of cerium precursor, molybdenum precursor, and carrier TiO 2 into a ball-milling tank, ball-milling for 1-6 hours, and calcining the uniformly mixed powder in a muffle furnace in two steps to obtain MoO 3- CeO 2 /TiO 2 composite oxide catalyst, wherein the CeO 2 content is 5-40 wt % of the total amount of cerium-titanium composite oxide, and the MoO 3 content is 0-10 wt % of the total molybdenum-cerium-titanium composite oxide. Under the condition of high humidity flue gas, the NO conversion rate of the SCR catalyst of the present invention is kept above 85% in the middle and high temperature range (250-500°C). The preparation process of the invention is simple, the conditions are easy to control, the raw material price is low, and the invention has potential application value in the field of denitrification.
Description
Technical field
The present invention relates to a kind of preparation method of SCR catalyst applied to high temperature high-humidity flue gas condition and its in ammonia
It is applied in selective catalyst reduction of nitrogen oxides reaction, belongs to catalyst preparation technical field.
Background technique
Nitrogen oxides (NOx) it is Air Pollutants, it is to cause the severe day such as acid rain, photochemical fog and haze
One of important arch-criminal of gas.In addition, these nitrogen oxides, which enter stratosphere, O occurs with ozone under the catalytic action of light3Hair
Biochemical reaction destroys ozone layer.Ammine selectivity catalytic reduction (Selective Catalysis Reduction, NH3-SCR)
It is the maximally efficient gas denitrifying technology having been commercialized at present, commercial catalyst is mainly vanadium titanium-based (V2O5-WO3/
TiO2Or V2O5-MoO3/TiO2).It is widely applied in firepower electrical plant denitrating flue gas, NOxRemoval efficiency is high, technology maturation.However
The applicable flue-gas temperature window of traditional vanadium titanium-based SCR catalyst is only 300 DEG C~
450 DEG C, when temperature is more than above range, the activity of vanadium Ti-base catalyst can be remarkably decreased, and catalyst activity
Component, which is easy to be lost, enters atmosphere, has harm to human body and environment；Spent catalyst has been put into
" National Hazard waste register ", processing can generate secondary pollution to environment.
For non-thermal power generation place, for most of gas turbines using coal bed gas power generation, flue-gas temperature is all
At 420 DEG C or more.And since combustion heat source is mainly CH4, smoke moisture is also very high by (20
- 30%).With the execution of " state VI " standard in 2019, sulfide contains in the combustion of natural gas tail gas of purified mistake
Amount is very low, therefore can not consider influence of the sulphur to catalyst.Therefore, for the spy of above-mentioned gas turbine flue gas high temperature and humidity
Point, the green non-poisonous Novel SCR catalyst that exploitation can efficiently be run in high temperature high-humidity gas fume denitrating system have important
Theoretical and practical significance.
CeO2With outstanding oxygen storage capacity and excellent redox ability, therefore, Ce base SCR catalyst is by pass
Note.Gao etc. (Gao X., et al., J.Hazard.Mater., 2010,174,734-739) compares different preparation methods pair
CeO2/TiO2The influence of catalyst denitration activity, the CeO that discovery is prepared using sol-gel method2/TiO2Catalyst has higher
Catalytic activity, temperature be 300~400 DEG C, air speed 50000h-1Under the conditions of, NOxConversion ratio is up to 93%~98%.To mention
High Ce base SCR catalyst sulfur resistive water resistance, usual way are to modify CeO using additive2/TiO2Catalyst, such as specially
The cerium-titanium composite oxide that sharp (application publication number CN 102302930) discloses a kind of transition metal (iron, tungsten, molybdenum) doping is urged
The catalyst temperature window of the preparation method of agent, preparation is wider, and has preferable low temperature active；Patent (application publication number CN
103846083) a kind of preparation method of the catalyst of titanium composite oxide-carried cerium oxide of tungsten, the CeO of preparation are disclosedxUniformly
It is distributed to Woy-TiO2Surface, gained catalyst can be used as the NO of exhaust gas from diesel vehiclexCatalytic purification；Patent (application publication number
CN103406124 a kind of iron cerium zirconium ternary complex catalyst) is disclosed, is applied to lean-combustion engine vent gas treatment, in catalyst
Component forms Ceria-zirconia solid solution, enhances the oxygen storage capacity of catalyst, so that the low temperature for improving catalyst is living
Property；It is carrier, oxygen that patent (application publication number CN 104492422), which discloses a kind of rare earth oxide-zirconia composite oxides,
Change the preparation method for the high-temperature flue gas denitrating catalyst that tungsten or molybdenum oxide or both mixture are active component, the catalyst of preparation
Can with used under 450-600 DEG C of high temperature range, denitration efficiency is up to 80% or more；Patent (application publication number CN 107262144) is public
Opened a kind of preparation method applied to distributed busbar protection internal combustion engine fume high-temperature denitrating catalyst, catalyst be sial when
The controllable Cu/SSZ-13 of copper content, catalyst inactivation resistant to high temperatures obtained, working window mouth width；Patent (application publication number CN
107754849) a kind of preparation method of support type high temperature denitrating catalyst is disclosed, using infusion process by soluble activating gold
Belong to component precursor salt and promoter metal component precursor salt is immersed in molecular sieve surface, by changing iron or cerium in catalyst
The dispersibility and ratio on surface form metal composite to adjust the catalytic activity of catalyst；Patent (application publication number CN
107715858) a kind of preparation method of high temperature resistant to sulfur Ce base SCR catalyst is disclosed, the cerium titanium using ball-milling method preparation is multiple
Oxide is closed within the scope of 280-550 DEG C, NO conversion ratio maintains 90% or more.Peng etc. (Peng Y., et al.,
Chem.Commun., 2013,49,6215-6217) in CeO2/TiO2Doping molybdenum improves the water-resistance of cerium base catalyst in system
Energy.But the SCR catalyst under the conditions of being suitable for gas turbine high temperature high-humidity gas fume so far is but rarely reported.
Summary of the invention
The purpose of the present invention is to provide a kind of simple processs, environmental-friendly molybdenum cerium-titanium composite oxide SCR catalyst
Preparation method and its ammine selectivity catalytic reduction nitrous oxides reaction in application.Raw material needed for catalyst preparation is inexpensively easy
, simple process.Using the molybdenum cerium and titanium compound oxide catalyst of this method preparation in high humidity (water content 10%~30%) cigarette
Under the conditions of gas, excellent denitration activity, i.e. ammonia selective catalyst are shown in wider temperature range (250 DEG C~500 DEG C)
Nitrogen oxides reduction (NH3- SCR) reaction in apply.
To realize foregoing invention effect, the technical solution adopted is as follows:
A kind of SCR catalyst suitable for high temperature high-humidity gas fume condition, which is characterized in that the catalyst is molybdenum cerium
Titanium compound oxide catalyst, that is, MoO3-CeO2/TiO2.CeO in above-mentioned molybdenum cerium-titanium composite oxide SCR catalyst2Content is
MoO3-CeO2/TiO2That is the 5-40wt% of total amount, MoO3Content is molybdenum cerium-titanium composite oxide, that is, MoO3-CeO2/TiO2Total amount
0~10wt%, and be not 0.
A kind of preparation method of the SCR catalyst applied to high temperature high-humidity gas fume condition, which is characterized in that including as follows
Step:
(1) by cerium precursor, molybdenum presoma and carrier TiO2It is put into ball grinder and carries out ball milling；
(2) by the powder after ball milling in Muffle kiln roasting, maturing temperature is 200-300 DEG C, heating rate is 5 DEG C/
Min, atmosphere are air, and calcining time is 1-4 hours；
(3) powder after low-temperature bake is subjected to after baking in Muffle furnace, maturing temperature is 450-550 DEG C, heating
Speed is 5 DEG C/min, and atmosphere is air, and calcining time is 1-4 hours；
(4) substance obtained in step (3) is ground, obtains powdered molybdenum cerium-titanium composite oxide SCR catalyst.
The preferred carrier TiO in above-mentioned steps (1)2For commercially available anatase phase titanium dioxide powder commodity, particle size
About 10~50 nanometers, specific surface area (BET) is 60~150m2/ g, TiO2Content is 94.0~99.5%.
Cerium precursor is at least the one of the cerium salts such as cerium oxalate, cerous nitrate, ammonium ceric nitrate or cerous acetate in above-mentioned steps (1)
Kind.
Molybdenum presoma used is ammonium molybdate in above-mentioned steps (1).
Abrading-ball used is having a size of 5~20mm in above-mentioned steps (1), it is preferred to use the three of diameter 20mm, 15mm and 10mm
The mixture of kind agate ball, preferred mass ratio are 50:100:20, and ratio of grinding media to material is 5:1~20:1, and Ball-milling Time is 1~6h, ball
The revolving speed of grinding machine is 300-1000r/min.
The beneficial effects of the present invention are: raw material is cheap and easy to get, preparation process is simple, and preparation condition is easily controllable, and experiment is former
Expect that environmental sound, gained catalyst are a kind of environmentally friendly SCR catalysts.
According to one kind described in above technical scheme applied to molybdenum cerium titanium combined oxidation under the conditions of high temperature high-humidity flue gas
The catalyst of the preparation method of object SCR catalyst, preparation is applied in NH3In-SCR reaction, have in wider temperature window higher
Catalytic activity and its catalytic performance can be kept for a long time under high temperature super-humid conditions.The catalyst can not only be applied to
Coal bed gas power plant stack gas processing system, also can be applied to distributed energy natural gas power, combustion gas and diesel engine, life
Object engine fuel, waste incinerator etc. have in the denitration process of high temperature and humidity characteristic tail gas.In smoke moisture 10%-30%
Under the conditions of, in 250~500 DEG C of temperature windows, NO conversion ratio can maintain 85% or more.
Detailed description of the invention
Prepared 1#, 2#, 3# in Fig. 1 embodiment 1,2,3,4, NH of 4# catalyst sample in the presence of 10% water3-SCR
Catalytic activity curve.
Prepared 1# in Fig. 2 embodiment 1,2,2# catalyst sample 250 DEG C of NH in the presence of 10-30% water3- SCR is urged
Agent life curve.
Prepared 1# in Fig. 3 embodiment 1,2,2# catalyst sample 500 DEG C of NH in the presence of 10-30% water3- SCR is urged
Agent life curve.
Prepared 1#, 2#, 3#, the XRD spectrum of 4# catalyst sample in Fig. 4 embodiment 1,2,3,4.
Specific embodiment
The contents of the present invention are further described below with reference to embodiment, but the present invention is not limited to following embodiments.
NH3SCR activity evaluation condition are as follows: 1000ppm NH3, 1000ppm NO, 6%O2, 10~30%H2O, N2For Balance Air, air speed
For 30000h-1.Reaction temperature is 100~550 DEG C.
Embodiment 1:
Weigh nine oxalic acid hydrate cerium 8.21g, TiO216g is put into ball grinder, and a certain number of 20mm, 15mm is then added
And the agate ball of 10mm, ratio of grinding media to material 10:1 are put into planetary ball mill, grind 1h.Uniformly mixed powder is put into horse
Not furnace, 250 DEG C roast 2 hours, and 500 DEG C roast 2 hours, obtain 1# catalyst sample.
Embodiment 2:
Weigh nine oxalic acid hydrate cerium 8.21g, TiO216g, Ammonium Molybdate Tetrahydrate 0.76g are put into ball grinder, are then added
The agate ball of a certain number of 20mm, 15mm and 10mm, ratio of grinding media to material 10:1, are put into planetary ball mill, grind 1h, will mix
Uniform powder is put into Muffle furnace, and 250 DEG C roast 2 hours, and 500 DEG C roast 2 hours, obtain 2# catalyst sample.
Embodiment 3:
Weigh nine oxalic acid hydrate cerium 8.21g, TiO216g, Ammonium Molybdate Tetrahydrate 1.29g are put into ball grinder, are then added
The agate ball of a certain number of 20mm, 15mm and 10mm, ratio of grinding media to material 10:1, are put into planetary ball mill, grind 1h, will mix
Uniform powder is put into Muffle furnace, and 250 DEG C roast 2 hours, and 500 DEG C roast 2 hours, obtain 3# catalyst sample.
Embodiment 4:
Weigh nine oxalic acid hydrate cerium 8.21g, TiO216g, Ammonium Molybdate Tetrahydrate 2.72g are put into ball grinder, are then added
The agate ball of a certain number of 20mm, 15mm and 10mm, ratio of grinding media to material 10:1, are put into planetary ball mill, grind 1h, will mix
Uniform powder is put into Muffle furnace, and 250 DEG C roast 2 hours, and 450 DEG C roast 2 hours, obtain 4# catalyst sample.
The NH of the catalyst sample of above embodiments3- SCR catalytic activity curve is shown in attached drawing.
Claims (9)
1. a kind of SCR catalyst suitable for high temperature high-humidity gas fume condition, which is characterized in that the catalyst is molybdenum cerium titanium
Composite oxide catalysts, that is, MoO3-CeO2/TiO2。
2. a kind of SCR catalyst suitable for high temperature high-humidity gas fume condition described in accordance with the claim 1, which is characterized in that
CeO in molybdenum cerium-titanium composite oxide SCR catalyst2Content is MoO3-CeO2/TiO2That is the 5-40wt% of total amount, MoO3Content is
Molybdenum cerium-titanium composite oxide, that is, CeO2、TiO2、MoO30~10wt% of total amount, and be not 0.
3. the method for preparing a kind of SCR catalyst suitable for high temperature high-humidity gas fume condition of any of claims 1 or 2,
It is characterized in that, includes the following steps:
(1) by cerium precursor, molybdenum presoma and carrier TiO2It is put into ball grinder and carries out ball milling；
(2) by the powder after ball milling in Muffle kiln roasting, maturing temperature is 200-300 DEG C, and heating rate is 5 DEG C/min, gas
Atmosphere is air, and calcining time is 1-4 hours；
(3) powder after low-temperature bake is subjected to after baking in Muffle furnace, maturing temperature is 450-550 DEG C, heating rate
For 5 DEG C/min, atmosphere is air, and calcining time is 1-4 hours；
(4) substance obtained in step (3) is ground, obtains powdered molybdenum cerium-titanium composite oxide SCR catalyst.
4. according to the method for claim 3, which is characterized in that the preferred carrier TiO in step (1)2, particle size is about
It is 10~50 nanometers, specific surface area (BET) is 60~150m2/ g, TiO2Mass percentage is 94.0~99.5%.
5. according to the method for claim 3, which is characterized in that cerium precursor is cerium oxalate, cerous nitrate, nitre in step (1)
At least one of sour cerium ammonium or cerous acetate.
6. according to the method for claim 3, which is characterized in that molybdenum presoma used is ammonium molybdate in step (1).
7. according to the method for claim 3, which is characterized in that abrading-ball used is having a size of 5~20mm, ball material in step (1)
Than for 5:1~20:1, Ball-milling Time is 1~6h, the revolving speed of ball mill is 300-1000r/min.
8. according to the method for claim 7, which is characterized in that abrading-ball size diameter used is 20mm, 15mm in step (1)
And the mixture of three kinds of agate balls of 10mm, mass ratio 50:100:20.
9. a kind of application of SCR catalyst suitable for high temperature high-humidity gas fume condition of any of claims 1 or 2 is selected in ammonia
Selecting property catalyzing and reducing nitrogen oxides (NH3- SCR) reaction in apply, under 10%~30% flue gas condition of high humidity, that is, water content and
It is reacted under the conditions of wider temperature range i.e. 250 DEG C~500 DEG C.
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| CN112808264A (en) * | 2021-01-05 | 2021-05-18 | 北京工业大学 | Preparation method of vanadium-molybdenum-titanium composite oxide low-temperature SCR catalyst |
| CN115591553A (en) * | 2022-09-09 | 2023-01-13 | 西安科技大学（Cn） | High-temperature NH using ball milling method to prepare carbonate as precursor 3 Method for SCR rare earth catalysts |
| CN115869936A (en) * | 2022-11-17 | 2023-03-31 | 安徽元琛环保科技股份有限公司 | Preparation method of wide-temperature cerium-based denitration catalyst and catalyst prepared by using same |
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Application publication date: 20190329 |