CN109806884A - A kind of graphene-manganese cerium low temperature SCR denitration catalyst and preparation method thereof - Google Patents
A kind of graphene-manganese cerium low temperature SCR denitration catalyst and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of graphene-manganese cerium low temperature SCR denitration catalysts and preparation method thereof.The preparation method includes step 1: graphite oxide being distributed in deionized water, ultrasonic disperse obtains graphene oxide colloid；Step 2: KMnO is added into the graphene oxide colloid that step 1 obtains4With Ce (NO3)3·6H2O, is stirred at room temperature after ultrasound to be transferred in the water heating kettle with polytetrafluoroethylliner liner and carries out hydro-thermal reaction, after reaction kettle is cooling, reaction solution is centrifuged, gained precipitating is washed with deionized, and finally dries in air dry oven to get graphene-manganese cerium low temperature SCR denitration catalyst is arrived.The present invention has preferable low-temperature catalytic activity.
Description
Technical field
The invention belongs to the Industrial Catalysis fields in chemical engineering, and in particular to a kind of graphene-manganese cerium low-temperature SCR is de-
The preparation method and application of denox catalyst.
Background technique
Ammonia selective catalyst reduction of nitrogen oxides (selective catalytic reduction of NOx with
NH3, NH3- SCR) it is a kind of effective denitration (de-NOx) technology, a large amount of industrial applicability has been obtained. NH3- SCR skill
Art refers in oxygen-containing atmosphere, reducing agent NH3Selectively by the NO in flue gas under catalytic actionxIt is reduced to N2And H2O.It urges
Agent is the core of SCR system, and many chemical reactions all occur on a catalyst, constituent, structure, service life and correlation
Parameter directly affects SCR system denitration efficiency and operating condition.It does not consume, and urges when catalyst promotes to chemically react itself
Agent activity can be gradually reduced with the increase for using the time.Currently, catalyst is used in SCR technology with V2O5/TiO2
Based on, such catalyst makes it that can only be arranged in the higher province's coal of dust concentration since active temperature range is 300~400 DEG C
Between device and air preheater, high-temperature high dust section can be such that catalyst activity reduces while can also shorten its service life, and discards and urge
Agent belongs to dangerous waste object, it is difficult to carry out harmless treatment recycling.The core technology of catalyst rests in external a small number of producers hand
In, domestic factory is given a long price for using the expense of catalyst accounts for the 40% of entire SCR process costs, and needs periodicity
Replacement, use cost is huge, these factors limit the more wide range of industrial applications of SCR technology.
For these reasons, many scholars suggest after reactor is arranged in deduster or desulfurizer in recent years, still
This process section flue-gas temperature is lower, is unable to satisfy existing catalyst activity temperature requirement, to avoid to flue gas Repeat-heating, section
About boiler improvement and operating cost, research and develop cryogenic conditions under the catalyst with high catalytic activity have Important Economic with
Practical significance, and paid attention to by numerous international scientific research personnel.Low-temp reaction device is directly configured at after dedusting or desulfurizer, no
Only convenient for matching with existing boiler system, and big influence will not be generated to other related system apparatus, furthermore also avoid
It consumes energy to smoke pre-heating, substantially reduces denitration cost.Currently, the low temperature catalyst of most study is carbon-based supports catalyst, but
It is that such technique is still immature, low temperature active, water resistant sulfur resistance and service life of catalyst etc. are all to be improved, so
Not yet industrial applications.
MnOxMn with a variety of crystal forms and different valence state, the higher oxygen reducing power that the conversion between valence state generates
It can promote NOxIt is catalyzed the progress of reaction, thus is had received widespread attention.CeOxThen because of its oxygen storage capacity outstanding and oxidation
Reducing power shows good low temperature NH3- SCR performance, and there is preferable anti-H2O and SO2Poisoning capability, with MnOxBetween
The excellent new catalyst system of concertedness can be constituted.Graphene is a kind of new carbon, has unique plane development knot
Structure, great theoretical specific surface area (2630m2/ g), higher electron mobility (2*105cm2/ Vs), conductivity (1*
106) and good mechanical performance and thermal stability S/m.Biggish specific surface area is conducive to improve the dispersion of active component
Degree, excellent characteristic electron can be greatly promoted the transmitting of electronics in oxidation-reduction process, thus accelerate that catalysis reacts into
Row.Meanwhile SCR catalyst is to NH3Adsorption capacity be catalyst activity key factor, NH3Absorption be also reaction certainly
Trot is rapid, studies have shown that graphene is to NH3With preferable adsorptivity, the progress of SCR reaction can promote, and on graphene
Hydrophobic grouping can inhibit H2The absorption of O, to improve the water repelling property of catalyst.Therefore, it is de- to prepare graphene-manganese cerium
Denox catalyst is used for NH3- SCR is worth research.
Summary of the invention
The object of the present invention is to provide a kind of graphene with preferable low temperature active-manganese cerium low temperature SCR denitration catalysis
Agent and preparation method thereof.
In order to achieve the above object, the present invention provides a kind of preparations of graphene-manganese cerium low temperature SCR denitration catalyst
Method characterized by comprising
Step 1: graphite oxide being distributed in deionized water, ultrasonic disperse obtains graphene oxide colloid；
Step 2: KMnO is added into the graphene oxide colloid that step 1 obtains4With Ce (NO3)3·6H2O is stirred at room temperature
It is transferred to after ultrasound in the water heating kettle with polytetrafluoroethylliner liner and carries out hydro-thermal reaction, after reaction kettle is cooling, by reaction solution
Centrifugation, gained precipitating are washed with deionized, and finally dry in air dry oven to get graphene-manganese cerium low-temperature SCR is arrived
Denitrating catalyst.
Preferably, the graphite oxide in the step 1 is by Brodie method, Staudenmaier method or Hummers legal system
?.
Preferably, the KMnO4With Ce (NO3)3·6H2The molar ratio of O is 3:1.
Preferably, in the quality of the graphene oxide and resulting graphene-manganese cerium low temperature SCR denitration catalyst
The ratio of the manganese cerium oxide quality sum contained is 3~30%.(according to addition KMnO4With Ce (NO3)3·6H2The quality of O
Calculate MnO obtained by theoryxAnd CeOxQuality, graphene oxide is proportionally added according to this quality)
Preferably, the temperature of the hydro-thermal reaction in the step 2 be 100~140 DEG C, the hydro-thermal time be 12~for 24 hours.
Preferably, the drying temperature in the step 2 is 100~120 DEG C, and the time is 3~6h.
The present invention also provides above-mentioned graphene-manganese cerium low temperature SCR denitration catalysts in low-temperature SCR denitrating flue gas system
Application in system.
The principle of catalyst of the present invention is KMnO4With Ce (NO3)3·6H2O occurs redox reaction and generates metal oxidation
Object, while the graphene oxide with large specific surface area and high-content surface oxygen functional group is introduced, Lai Tigao catalyst
Dispersion, to reach preferable low-temperature catalytic activity.
The present invention is proposed with KMnO4、Ce(NO3)3·6H2O and GO is raw material, and test will use a step redox precipitation
Method prepares graphene-manganese cerium oxide of different the Nomenclature Composition and Structure of Complexes as NH3SCR catalyst system, and use modern analysis
Characterizing method probes into the denitration principle and performance of redox machinery.
Ce3++H2O→Ce(OH)3+3H+(Ce(NO3)3·6H2The hydrolysis of O)
MnO4 -+2H2O→MnO2+4OH-(MnO4 -The hydrolysis of ion)
6H++2Ce(OH)3+2KMnO4→2MnO2+Ce2O3+2KOH+5H2O
(Ce(OH)3And KMnO4Decomposition reaction)
6H++2Ce(OH)3+2KMnO4→2MnO2+2CeO2+2K++6H2O
(Ce(OH)3And KMnO4Redox reaction)
3C+4MnO4 -+4H2O→CO3 2-+2HCO3 -+4MnO2
The beneficial effects of the present invention are:
(1) selecting new carbon graphene is carrier, and manganese cerium oxide prepares graphene-manganese cerium for active component and urges
Agent is applied to denitration reaction, and compared with traditional vanadium titanium catalyst, such catalyst has high low temperature active, and to ring
Border is friendly, and preparation process is simple, is advantageously implemented industrialization.
(2) present invention prepares catalyst by redox precipitation method, and reaction process does not need that precipitating reagent is added, reduces
The use of chemical reagent reduces costs to simplify preparation process simultaneously.Especially in simplest synthetic strategy
In, without any additional precipitating and high-temperature burning process, its original appearance and pore structure can be kept, is avoided because calcining to catalysis
The pore structure and micromorphology of agent damage, and reduce catalyst activity.
Detailed description of the invention
Fig. 1 is GR (20%)-MnOx-CeOxThe SCR activity figure of catalyst.
Fig. 2 is GR (20%)-MnOx-CeOxThe XRD spectra of catalyst.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, this field skill
Art personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims
Limited range.
Each raw material used in following embodiment is commercial product.
Embodiment 1
Graphite oxide, specific steps are prepared using Hummers method is improved are as follows:
96mL (mass fraction 98%) concentrated sulfuric acid is poured into dry round-bottomed flask, is then added into flask
2gNaNO3, 2g crystalline flake graphite is added after stirring and dissolving, after waiting crystalline flake graphites to be uniformly dispersed in the solution, at leisure to flask
Middle addition 12gKMnO4, 1.45h is reacted, whole process carries out under ice bath system, and temperature is maintained at 0 DEG C.Then by temperature
35 DEG C are risen to, after reacting 2h under this condition, 80mL deionized water is then slowly added, is warming up to 95 DEG C, reaction
30min adds 200mL deionized water, and the H of 10mL30% is then added2O2Solution, react 10min, reaction solution while hot from
The heart, the salt acid elution that gained precipitating is 5% with 1000mL concentration, to remove the metal ion that precipitating contains.Then deionization is used
Water washing places it in drying in 60 DEG C of vacuum ovens and for 24 hours, obtains graphite oxide to pH value of solution close to neutrality.
Embodiment 2
A kind of preparation method of graphene-manganese cerium low temperature SCR denitration catalyst, specific steps are as follows:
(1) graphite oxide made from 2.5g embodiment 1 is distributed in 500mL deionized water, it is ultrasonic under 80W, 40KHz
Disperse 60min, obtains graphene oxide colloid, concentration 5mg/mL；
(2) the graphene oxide colloid addition 94.6mL deionized water that the step of measuring 5.4mL (1) obtains, 80W,
It is ultrasonically treated 60min under 40KHz, 1.0g KMnO is added4With 0.92g Ce (NO3)3·6H230min is stirred at room temperature in O, then
30min is ultrasonically treated under 80W, 40KHz.Solution transfer is set in the water heating kettle with polytetrafluoroethylliner liner, 100 DEG C of hydro-thermals
React 12h.Reaction solution is centrifuged after reaction kettle is cooling, gained precipitating is washed with deionized three times, is finally put into precipitating
In air dry oven, 100 DEG C of dry 3h are denoted as GR (3%)-to get graphene-manganese cerium low temperature SCR denitration catalyst is arrived
MnOx-CeOx.(according to addition KMnO4With Ce (NO3)3·6H2The Mass Calculation of O goes out theoretical gained MnOxAnd CeOxQuality, root
Graphene oxide is proportionally added according to this quality, graphene oxide is reduced to graphene in water-heat process, theoretical
On think the manganese cerium oxide that contains in the quality and resulting graphene-manganese cerium low temperature SCR denitration catalyst of graphene oxide
3%) ratio of quality sum is
Embodiment 3
A kind of preparation method of graphene-manganese cerium low temperature SCR denitration catalyst, specific steps are as follows:
(1) graphite oxide made from 2.5g embodiment 1 is distributed in 500mL deionized water, it is ultrasonic under 80W, 40KHz
Disperse 60min, obtains graphene oxide colloid, concentration 5mg/mL；
(2) 82mL deionized water is added in the graphene oxide colloid that the step of measuring 18mL (1) obtains, under 80W, 40KHz
It is ultrasonically treated 60min, 1.0g KMnO is added4With 0.92g Ce (NO3)3·6H230min, then 80W, 40KHz is stirred at room temperature in O
Lower ultrasonic treatment 30min.Solution transfer is set in the water heating kettle with polytetrafluoroethylliner liner, 120 DEG C of hydro-thermal reaction 18h.To
Reaction solution is centrifuged after reaction kettle is cooling, gained precipitating is washed with deionized three times, and precipitating is finally put into air dry oven
In, 110 DEG C of dry 3h are denoted as GR (10%)-MnO to get graphene-manganese cerium low temperature SCR denitration catalyst is arrivedx-CeOx.It (presses
According to addition KMnO4With Ce (NO3)3·6H2The Mass Calculation of O goes out theoretical gained MnOxAnd CeOxQuality, pressed according to this quality
Graphene oxide is added according to ratio, graphene oxide is reduced to graphene in water-heat process, it could be theoretically argued that graphite oxide
The ratio of the manganese cerium oxide quality sum contained in the quality of alkene and resulting graphene-manganese cerium low temperature SCR denitration catalyst
For 10%)
Embodiment 4
A kind of preparation method of graphene-manganese cerium low temperature SCR denitration catalyst, specific steps are as follows:
(1) graphite oxide made from 2.5g embodiment 1 is distributed in 500mL deionized water, it is ultrasonic under 80W, 40KHz
Disperse 60min, obtains graphene oxide colloid, concentration 5mg/mL；
(2) 64mL deionized water is added in the graphene oxide colloid that the step of measuring 36mL (1) obtains, under 80W, 40KHz
It is ultrasonically treated 60min, 1.0g KMnO is added4With 0.92g Ce (NO3)3·6H230min, then 80W, 40KHz is stirred at room temperature in O
Lower ultrasonic treatment 30min.Solution transfer is set in the water heating kettle with polytetrafluoroethylliner liner, 120 DEG C of hydro-thermal reaction 12h.To
Reaction solution is centrifuged after reaction kettle is cooling, gained precipitating is washed with deionized three times, and precipitating is finally put into air dry oven
In, 110 DEG C of dry 3h are denoted as GR (20%)-MnO to get graphene-manganese cerium low temperature SCR denitration catalyst is arrivedx-CeOx, GR
(20%)-MnOx-CeOxThe XRD spectra of catalyst is as shown in Figure 2.(according to addition KMnO4With Ce (NO3)3·6H2The quality of O
Calculate MnO obtained by theoryxAnd CeOxQuality, graphene oxide is proportionally added according to this quality, in water-heat process
Middle graphene oxide is reduced to graphene, it could be theoretically argued that the quality of graphene oxide and resulting graphene-manganese cerium low temperature
20%) ratio of the manganese cerium oxide quality sum contained in SCR denitration is
Embodiment 5
A kind of preparation method of graphene-manganese cerium low temperature SCR denitration catalyst, specific steps are as follows:
(1) graphite oxide made from 2.5g embodiment 1 is distributed in 500mL deionized water, it is ultrasonic under 80W, 40KHz
Disperse 60min, obtains graphene oxide colloid, concentration 5mg/mL；
(2) 46mL deionized water is added in the graphene oxide colloid that the step of measuring 54mL (1) obtains, under 80W, 40KHz
It is ultrasonically treated 60min, 1.0g KMnO is added4With 0.92g Ce (NO3)3·6H230min, then 80W, 40KHz is stirred at room temperature in O
Lower ultrasonic treatment 30min.Solution transfer is set in the water heating kettle with polytetrafluoroethylliner liner, 140 DEG C of hydro-thermal reactions are for 24 hours.To
Reaction solution is centrifuged after reaction kettle is cooling, gained precipitating is washed with deionized three times, and precipitating is finally put into air dry oven
In, 120 DEG C of dry 6h are denoted as GR (30%)-MnO to get graphene-manganese cerium low temperature SCR denitration catalyst is arrivedx-CeOx.It (presses
According to addition KMnO4With Ce (NO3)3·6H2The Mass Calculation of O goes out theoretical gained MnOxAnd CeOxQuality, pressed according to this quality
Graphene oxide is added according to ratio, graphene oxide is reduced to graphene in water-heat process, it could be theoretically argued that graphite oxide
The ratio of the manganese cerium oxide quality sum contained in the quality of alkene and resulting graphene-manganese cerium low temperature SCR denitration catalyst
For 30%)
Embodiment 6
Graphene prepared by above-described embodiment-manganese cerium low-temperature denitration catalyst is sized to 40~80 mesh, is placed in fixation
Denitration performance test is carried out in bed quartz tube reactor, simulated flue gas is by NO, NH3、O2、N2Composition, wherein NO be 500ppm,
NH3For 500ppm, O2For 5.0vol%, N2As Balance Air, reaction velocity 14400h-1, total flow 120mL/min.Instead
Answer the NO in the gas of front and back by online point of MIC-600 type stationary gas detector (Shenzhen ease skies Electronics Co., Ltd.)
Analysis, the temperature range of activity rating are 80~320 DEG C, NOxConversion ratio calculates as follows:
In formula, ηNOxFor NOxConversion ratio, [NOx]in[NOx]outReactor imports and exports NO respectively under stable statexConcentration.
Activity evaluation is as shown in table 1:
The denitration activity of the catalyst of 1 embodiment of table preparation
Fig. 1 is graphene-manganese cerium oxide denitrating catalyst SCR activity evaluation figure prepared by embodiment 4, can be seen
It is with preferable low temperature active out, 160 DEG C can reach 100% NO conversion ratio.
In conclusion a kind of graphene of the invention-manganese cerium low temperature SCR denitration catalyst resulting catalyst of method,
Its preparation process is simple, easy to industrialized production, has potential practical application value in environment protection field.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, without departing from the technical principles of the invention, several improvement can also be made, these improvement also should be regarded as
Protection scope of the present invention.
Claims (8)
1. a kind of graphene-manganese cerium low temperature SCR denitration catalyst preparation method characterized by comprising
Step 1: graphite oxide being distributed in deionized water, ultrasonic disperse obtains graphene oxide colloid；
Step 2: KMnO is added into the graphene oxide colloid that step 1 obtains4With Ce (NO3)3·6H2O, after ultrasound is stirred at room temperature
It is transferred in the water heating kettle with polytetrafluoroethylliner liner and carries out hydro-thermal reaction, after reaction kettle is cooling, reaction solution is centrifuged, institute
It must precipitate and be washed with deionized, finally dry in air dry oven and be catalyzed to get to graphene-manganese cerium low temperature SCR denitration
Agent.
2. graphene as described in claim 1-manganese cerium low temperature SCR denitration catalyst preparation method, which is characterized in that described
Step 1 in graphite oxide be made by Brodie method, Staudenmaier method or Hummers method.
3. graphene as described in claim 1-manganese cerium low temperature SCR denitration catalyst preparation method, which is characterized in that described
KMnO4With Ce (NO3)3·6H2The molar ratio of O is 1:1-5:1.
4. graphene as described in claim 1-manganese cerium low temperature SCR denitration catalyst preparation method, which is characterized in that described
Graphene oxide quality and resulting graphene-manganese cerium low temperature SCR denitration catalyst in the manganese cerium oxide quality that contains
The sum of ratio be 3~30%.
5. graphene as described in claim 1-manganese cerium low temperature SCR denitration catalyst preparation method, which is characterized in that described
Step 2 in hydro-thermal reaction temperature be 100~140 DEG C, the hydro-thermal time be 12~for 24 hours.
6. graphene as described in claim 1-manganese cerium low temperature SCR denitration catalyst preparation method, which is characterized in that described
Step 2 in drying temperature be 100~120 DEG C, the time be 3~6h.
7. graphene prepared by preparation method of any of claims 1-5-manganese cerium low temperature SCR denitration catalyst.
8. graphene as claimed in claim 6-manganese cerium low temperature SCR denitration catalyst answering in low-temperature SCR flue gas denitrification system
With.
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| CN114345321A (en) * | 2021-12-31 | 2022-04-15 | 广州工业智能研究院 | Sulfur-resistant Ce-Mn-Zr catalyst and preparation method and application thereof |
| CN114768794A (en) * | 2022-04-27 | 2022-07-22 | 华南理工大学 | Composite manganese oxide catalyst for synchronously removing VOCs and NOx in medium-low temperature flue gas and preparation method and application thereof |
| CN114768794B (en) * | 2022-04-27 | 2024-03-15 | 华南理工大学 | Composite manganese oxide catalyst for synchronously removing VOCs and NOx in medium-low temperature flue gas, and preparation method and application thereof |
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