CN108855051A - A kind of synthetic method of the two-dimentional Mn oxide for low temperature SCR denitration - Google Patents
A kind of synthetic method of the two-dimentional Mn oxide for low temperature SCR denitration Download PDFInfo
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- CN108855051A CN108855051A CN201810637818.2A CN201810637818A CN108855051A CN 108855051 A CN108855051 A CN 108855051A CN 201810637818 A CN201810637818 A CN 201810637818A CN 108855051 A CN108855051 A CN 108855051A
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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
- B01J23/16—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
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- 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
Abstract
A kind of two-dimentional Mn oxide and its synthetic method for low temperature SCR denitration, belongs to pollution control, environmental catalysis field.Synthesis step is as follows：It is placed in certain density in the heating water bath of certain temperature containing one of dodecyl sodium sulfate, lauryl sodium sulfate, neopelex, sodium hexadecyl sulfate or a variety of aqueous surfactant solutions；The metal ion precursor solution of the potassium manganate of ultrasonic wave added dissolution or potassium permanganate is poured into rapidly in above-mentioned surfactant solution, and acid solution is added dropwise simultaneously into mixed solution, certain time is reacted under certain bath temperature, is filtered, washed, drying and roasting is up to two-dimensional Mn oxide.The invention catalyst can realize SCR denitration at a lower temperature, and denitration efficiency is greater than 80% when reaction temperature is 100 DEG C, and 150~250 DEG C of denitration efficiency is up to 90% or more, N2Selectivity is greater than 90%.Two-dimensional structure is presented in catalyst of the present invention, has good water resistant Sulfur tolerance, the synthetic method is easy to operate, and simple process is easy to realize industrial production.
Description
Technical field
The present invention relates to a kind of two-dimentional Mn oxides and its synthetic method for low temperature SCR denitration.The material is applied to
The removal of nitrogen oxides (NOx) in the low-temperature flue gas such as Industrial Stoves, agglomerates of sintered pellets, coking industry, glass industry.Belong to flue gas
Denitration field and environmental catalysis field.
Background technique
With the development of world economy, problem of environmental pollution is more and more prominent in the industrial production.World community is before
Fast, economical development during expanding economy is mostly pushed with the consumption of natural resources, China mainly with coal, petroleum,
The fossil fuels such as natural gas carry out the generation of power, while bring is increasingly severeer environmental problem.The combustion of fossil fuel
Burning is inevitably generated a large amount of environmental pollutants, as one of main atmosphere pollution, nitrogen oxides (NOx, NO,
NO2) acid rain, photochemical fog, depletion of the ozone layer and climate change can be caused and cause certain damage to make human health
With.NO is a kind of gas of no color or smell, and blood anoxic is easily caused in conjunction with ferroheme and nervous centralis is caused to be benumbed；NO2Poison
Property ratio NO strong toxicity, human body sucking after very harmful, NOxHarm be mainly：(1)NOxIt is decomposed under sunlight irradiation and generates oxygen original
Son causes a series of chain reactions to generate with O3, the photochemical fog as main component such as PAN.Photochemical fog is fog-like, energy
Degree of opinion is extremely low, causes traffic accident occurrence probability to rise, while photochemical fog has strong murder by poisoning to eyes, the respiratory tract of people
Effect；(2) haze weather, the NO in coal-fired flue-gas are easily formedxIt is the presoma of nitrate in Atmospheric particulates PM2.5；(3)NOx
It can be with O3Reaction, makes O3Become O2, there is destruction to ozone layer.Therefore the problem that NOx, is urgently to be resolved.
The method mainly selective noncatalytic reduction (SNCR), selective catalytic reduction (SCR) of removing NOx at present
Technology.Since selective non-catalytic reduction method (SNCR) does not need catalyst during processing, in order to reach higher chemistry
Reactivity, which needs to carry out the removing of NOx at a higher temperature, very sensitive for temperature condition, general reason
Temperature is thought at 850 DEG C~1100 DEG C, and reactor is different, and the temperature window needed is also different.When reaction temperature is lower than temperature window
When, due to the limitation of residence time, often it is not enough chemical reaction, to cause the reduction rate of NO lower, simultaneously
Have neither part nor lot in the NH of reaction3Increase the escape that will also result in ammonia, and the NOx removal rate of the technology is only capable of reaching 70%.SCR is mesh
Preceding effective in the world, most widely used gas denitrifying technology, the catalyst of use are mostly vanadium-based materials, this kind of catalyst
Warm window work at 300~400 DEG C, during the reaction the SO of a large amount of dusts in tail gas and high concentration2It will lead in catalyst
Poison inactivation.To solve the above problems, by NH3SCR device is placed in after dedusting and sulfur removal technology, to reduce dust and SO2To urging
The influence of agent, flue-gas temperature at this time will be down to 200 DEG C hereinafter, so the SCR developed under low temperature with high activity is urged
Agent has important practical significance.Mn oxide is since there are a variety of valence states for it, it is prone to redox reaction, therefore at
For the research hotspot of low-temperature SCR catalyst.It is shown according to current result of study, although Mn base catalyst has preferable low temperature to urge
Change activity, but the water resistant sulfur tolerance of such catalyst is bad, therefore develops the catalyst with good sulfur resistive water repelling property
With realistic meaning.
Two-dimensional material has special lamellar structure, shows biggish specific surface area, nano material dimensional effect, puts down
The feature that face electric conductivity is strong, electronics conductance is big.It is found by researches that the catalyst of the structure is in NH3In-SCR reaction system not
Deposition conducive to sulfate on its surface has preferable water-fast sulfur resistance compared with traditional catalyst.Chinese patent
CN105561982A discloses a kind of γ-MnO2Nanometer sheet low-temperature SCR catalyst for denitrating flue gas, catalyst exist to the conversion ratio of NO
It can achieve 90% or more within the scope of 130 DEG C~250 DEG C warm windows, but its low temperature active is poor, when reaction temperature is 90 DEG C,
Catalytic activity is only up to 50%.
Chinese patent CN104289227A discloses a kind of tetra- component NH of low-temperature denitration of flue gas Mn, Co, Ce, Ti3-SCR
Catalyst of support type and preparation method thereof forms multicomponent after roasting and meets metal oxide, prepared catalysis
Agent specific surface area is 115.38cmg-1.But the sulfur resistive of the catalyst is ineffective.Chinese patent CN201510961222.4 is public
A kind of rGO load petal-shaped MoS is opened2The preparation method of heterojunction structure, for improving the efficiency of photocatalytically degradating organic dye.
It is the processing method that annealing is synthesized and passed through using a step hydro-thermal reaction and improves crystallization degree, forms petal-shaped MoS2
The Heterogeneous Composite structure that cluster and rGO are mutually wound, the big specific surface area of the material use two-dimensional material can be dramatically increased to having
The absorption of machine pollutant, and its heterogeneous interface can promote light induced electron to be quickly transferred on graphene sheet layer, stay in MoS2Valence band
In with oxidisability photohole participate in degradable organic pollutant, the photocatalysis characteristic of significant increase material.
Summary of the invention
The problems such as small, water resistant Sulfur tolerance is bad for specific surface area existing for current low temperature SCR denitration catalyst, the present invention
Provide a kind of two-dimentional Mn oxide and synthetic method for low temperature SCR denitration, the catalyst prepared using the method
In 200 DEG C of < conversion rate of NOx, stability and resistances with higher, low temperature SCR denitration can be suitable for.
A kind of synthetic method of the two-dimentional Mn oxide for low temperature SCR denitration, it is characterised in that：Two-dimentional Mn oxide
Microscopic appearance is two-dimensional layer plate shape, and synthetic method is one stage reduction method of surfactant.
A kind of two-dimentional Mn oxide synthetic method for low temperature SCR denitration as described above, it is characterised in that：Synthesis step
It is rapid as follows：(1) certain density aqueous surfactant solution A is configured, is placed in the heating water bath of certain temperature；(2) one is configured
The mangaic acid root aqueous solution B for determining concentration assists dissolving using ultrasonication；(3) solution B is rapidly added solution A, be added dropwise simultaneously
Certain density acid solution, is added dropwise, and obtains solution C；(4) one timing of reaction under bath temperature of the solution C described in (1)
Between after, be filtered, washed and extract the above process formation solid particulate matter D；(5) the solid particulate matter D after drying is placed in one
Roasting temperature certain time is determined to get two-dimentional manganese oxide catalyst.
Further, the surfactant includes dodecyl sodium sulfate, lauryl sodium sulfate, detergent alkylate
Sodium sulfonate, sodium hexadecyl sulfate it is one or more；The mangaic acid root predecessor includes one kind of potassium permanganate, potassium manganate
Or it is a variety of；The acid solution include sulfuric acid, hydrochloric acid, nitric acid it is one or more.
Further, the molar concentration of the surfactant solution A is 0.15~0.75mol/L；The mangaic acid
The molar concentration of root aqueous solution B is 0.01~0.15mol/L；The molar concentration of the acid solution is 0.5~1.5mol/L.
Further, the water bath heating temperature of the solution A and C are 65~95 DEG C；When the described solution C heating water bath
Between be 1~5 hour；The calcination temperature of the solid particulate matter D is 80~450 DEG C, and calcination time is 2~6 hours.
Compared with prior art, the present invention mainly has following effect using after above-mentioned synthetic schemes：The present invention successfully synthesizes
A kind of two-dimentional Mn oxide for low temperature SCR denitration has biggish specific surface area, and preparation method is easy to operate, work
Skill is simple；Made catalyst is applied to NH3In-SCR reaction system, under the warm window of lower reaction (100~250 DEG C),
To reach preferable NOx removal effect, N2Selectivity can achieve 90% or more, while have good water resistant Sulfur tolerance.It should
Method preparation catalyst material structure it is special, apply advantage possessed by two-dimensional material well, be suitable for Industrial Stoves,
The removal of nitrogen oxides (NOx) in the low-temperature flue gas such as agglomerates of sintered pellets, coking industry, glass furnace.
Detailed description of the invention
The catalyst SEM that Fig. 1 is the embodiment of the present invention 1 (Fig. 1 a), prepared by embodiment 2 (Fig. 1 b), embodiment 3 (Fig. 1 c)
Figure；
The catalyst TEM that Fig. 2 is the embodiment of the present invention 1 (Fig. 2 a), prepared by embodiment 2 (Fig. 2 b), embodiment 3 (Fig. 2 c)
Figure；
The XRD diagram for the catalyst that Fig. 3 is the embodiment of the present invention 1, prepared by embodiment 2, embodiment 3；
Fig. 4 is that the catalyst of the embodiment of the present invention 3 (Fig. 4 a) preparation and the precipitation method prepare catalyst (Fig. 4 b) and citric acid
Method prepares catalyst (4c) water resistant Sulfur tolerance datagram；
Specific embodiment
The present invention will be described in detail below in conjunction with the accompanying drawings and the specific embodiments.These embodiments are merely to illustrate this
It invents rather than limits the scope of the invention.
Embodiment 1
(1) it accurately weighs 5g dodecyl sodium sulfate to be dissolved in 200ml deionized water, is configured to solution A, and place it in
Under 65 DEG C of bath temperature；
(2) it accurately weighs 0.3g potassium manganate to be dissolved in a certain amount of deionized water, forms the B solution of 0.03mol/L, be used in combination
Ultrasonic wave added is dissolved；
(3) B solution in step (2) is added in the solution A of step (1) rapidly, while 10ml is added dropwise while stirring
Hydrochloric acid, obtain mixed solution C；
(4) solution C that step (3) obtains is placed under bath temperature described in step (1) after reacting a period of time, mistake
The solid particulate matter D formed in filter, the washing above process；
(5) the solid particulate matter D after drying the Muffle kiln roasting 2h that temperature is 80 DEG C is placed in aoxidize to get two-dimentional manganese
Object.
Embodiment 2
(1) it accurately weighs 7g lauryl sodium sulfate to be dissolved in 300ml deionized water, is configured to solution A, and place it in
Under 80 DEG C of bath temperature；
(2) it accurately weighs 0.2022g potassium manganate to be dissolved in a certain amount of deionized water, forms the B solution of 0.06mol/L,
And it is dissolved with ultrasonic wave added；
(3) B solution in step (2) is added in the solution A of step (1) rapidly, while 13ml is added dropwise while stirring
Nitric acid, obtain mixed solution C；
(4) solution C that step (3) obtains is placed under bath temperature described in step (1) after reacting a period of time, mistake
The solid particulate matter D formed in filter, the washing above process；
(5) the solid particulate matter D after drying is placed in temperature is 200 DEG C of Muffle kiln roasting 4h to get two-dimentional manganese oxygen
Compound.
Embodiment 3
(1) accurately weigh 3.8g neopelex to be dissolved in 350ml deionized water, be configured to solution A, and by its
It is placed under 90 DEG C of bath temperature；
(2) it accurately weighs 0.1680g potassium permanganate to be dissolved in a certain amount of deionized water, forms the B solution of 0.1mol/L,
And it is dissolved with ultrasonic wave added；
(3) B solution in step (2) is added in the solution A of step (1) rapidly, while is added dropwise 9ml's while stirring
Sulfuric acid obtains mixed solution C；
(4) solution C that step (3) obtains is placed under bath temperature described in step (1) after reacting a period of time, mistake
The solid particulate matter D formed in filter, the washing above process；
(5) the solid particulate matter D after drying is placed in temperature is 400 DEG C of Muffle kiln roasting 6h to get two-dimentional manganese oxygen
Compound.The water resistant Sulfur tolerance of catalyst obtained by the present embodiment is tested, the resistance of catalyst can be indicated with the conversion ratio of NOx.
Attached drawing 4 (a) shows to prepare MnO2Catalyst is in 150 DEG C of resistance 8%H2The SO of O and 150ppm2Test condition under, in 6 hours
Testing time in nitrogen oxide removal efficiency only decline 16%, illustrate the catalyst have good water resistant sulfur tolerance.
Catalyst performance test
Catalyst activity test is carried out in the fixed bed reactors for place it in quartz tube type, and catalyst is placed in reactor
Centre, reaction temperature are controlled by electric tube furnace by voltage regulator, and reaction temperature control is realized by programmed temperature control instrument.Pass through
Steel cylinder gas simulates coking flue gas, and the control of gas flow, reaction velocity 32000h are carried out by mass flowmenter-1, reaction gas
Body is by NO, NH3、O2、N2Composition carries out NOx removal rate and N by inlet and outlet gas concentration before and after test catalyst treatment2Selection
The calculating of property, and water resistant Sulfur tolerance test is carried out to it.The manganese oxide catalyst of embodiment preparation preferred for this invention exists
Denitration efficiency is greater than 80% when reaction temperature is 100 DEG C, and 150~250 DEG C of denitration efficiency is up to 90% or more, N2Selectivity is big
In 90%
The above, preferable specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto, appoints
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of, all by what those familiar with the art
It should be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (5)
1. a kind of synthetic method of the two-dimentional Mn oxide for low temperature SCR denitration, it is characterised in that：The Mn oxide
Microscopic appearance is two-dimensional layer plate shape；The synthetic method is one stage reduction method of surfactant.
2. the synthetic method of the two-dimentional Mn oxide of low temperature SCR denitration according to claim 1, it is characterised in that：Synthesis
Steps are as follows：(1) certain density aqueous surfactant solution A is configured, is placed in the heating water bath of certain temperature；(2) it configures
Certain density mangaic acid root aqueous solution B assists dissolving using ultrasonication；(3) solution B is rapidly added solution A, dripped simultaneously
Add certain density acid solution, be added dropwise, obtains solution C；(4) react certain under bath temperature of the solution C described in (1)
After time, the solid particulate matter D of above process formation is filtered, washed and extracted；(5) the solid particulate matter D after drying is placed in
Certain time is roasted under certain temperature to get the two-dimentional Mn oxide of low temperature SCR denitration.
3. the synthetic method of the two-dimentional Mn oxide of low temperature SCR denitration according to claim 2, it is characterised in that：It is described
Surfactant include dodecyl sodium sulfate, lauryl sodium sulfate, neopelex, sodium hexadecyl sulfate
It is one or more；The mangaic acid root predecessor include potassium manganate, potassium permanganate it is one or more；The acid solution packet
Include sulfuric acid, hydrochloric acid, nitric acid it is one or more.
4. the synthetic method of the two-dimentional Mn oxide of low temperature SCR denitration according to claim 2, it is characterised in that：It is described
Surfactant solution A molar concentration be 0.15~0.75mol/L；The molar concentration of the mangaic acid root aqueous solution B is
0.01~0.15mol/L；The molar concentration of the acid solution is 0.5~1.5mol/L.
5. the synthetic method of the two-dimentional Mn oxide of low temperature SCR denitration according to claim 2, it is characterised in that：It is described
Solution A and solution C water bath heating temperature be 65~95 DEG C；The solution C heating water bath time is 1~5 hour；It is described
Solid particulate matter D calcination temperature be 80~450 DEG C, calcination time be 2~6 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115430417A (en) * | 2022-08-31 | 2022-12-06 | 兰润环保技术(烟台)有限公司 | Flue gas denitration catalyst and preparation method thereof |
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| CN105618032A (en) * | 2016-01-19 | 2016-06-01 | 中国建筑材料科学研究总院 | Supported manganese based low-temperature denitration catalyst and preparation method thereof |
| GB2536530A (en) * | 2014-12-19 | 2016-09-21 | Johnson Matthey Plc | Catalyst manufacturing method |
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2018
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| US20090291838A1 (en) * | 2008-05-22 | 2009-11-26 | Hyundai Motor Company | Urea SCR catalyst and manufacturing method for the same |
| CN104001520A (en) * | 2013-11-27 | 2014-08-27 | 大连理工大学 | Synthesis method for low-temperature manganese-based compound metal oxide denitration catalysts |
| GB2536530A (en) * | 2014-12-19 | 2016-09-21 | Johnson Matthey Plc | Catalyst manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115430417A (en) * | 2022-08-31 | 2022-12-06 | 兰润环保技术(烟台)有限公司 | Flue gas denitration catalyst and preparation method thereof |
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Application publication date: 20181123 |