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 PDF

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CN109529812A
CN109529812A CN201811483627.1A CN201811483627A CN109529812A CN 109529812 A CN109529812 A CN 109529812A CN 201811483627 A CN201811483627 A CN 201811483627A CN 109529812 A CN109529812 A CN 109529812A
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cerium
scr catalyst
tio
ball
catalyst
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邱文革
李世宁
王佳丽
叶婧桐
张宁强
孙炎明
何俊达
何洪
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Beijing University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J23/24—Chromium, molybdenum or tungsten
    • B01J23/28—Molybdenum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

A kind of SCR catalyst and preparation method suitable for high temperature high-humidity gas fume condition, belongs to catalyst preparation technical field.Specific method includes: by the cerium precursor of calculation amount, molybdenum presoma, carrier TiO2It is put into ball grinder, ball milling 1-6h, uniformly mixed powder is roasted in two steps in Muffle furnace, obtains MoO3‑CeO2/TiO2Composite oxide catalysts, wherein CeO2Content is the 5-40wt%, MoO of cerium-titanium composite oxide total amount3Content is 0~10wt% of molybdenum cerium-titanium composite oxide total amount.For SCR catalyst of the present invention under the conditions of high-humidity flue gas, NO conversion ratio is maintained at 85% or more in high temperature degree section (250-500 DEG C).Preparation process of the present invention is simple, and condition is easily controllable, low in raw material price, has potential using value in denitration field.

Description

A kind of SCR catalyst and preparation method suitable for high temperature high-humidity gas fume condition
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.
CN201811483627.1A 2018-12-05 2018-12-05 A kind of SCR catalyst and preparation method suitable for high temperature high-humidity gas fume condition Pending CN109529812A (en)

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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