CN108816225A - Fabricated in situ Pt/MnO for VOCs catalysis burning2@Mn3O4Catalyst, preparation method and applications - Google Patents
Fabricated in situ Pt/MnO for VOCs catalysis burning2@Mn3O4Catalyst, preparation method and applications Download PDFInfo
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Abstract
The invention belongs to environmental catalysis purification techniques field, the fabricated in situ Pt/MnO for VOCs catalysis burning is provided2@Mn3O4Catalyst, preparation method and applications.Using potassium permanganate and oxalic acid as raw material, MnO is prepared using hydro-thermal method2；Again with the MnO2It is reducing agent using sodium borohydride for starting vector, liquid-phase reduction H under normal temperature conditions2PtCl6While, to MnO2Carrier carries out structure regulating, and a step restores to obtain the mixed phase MnO of fabricated in situ2@Mn3O4Carrier load type Pt base catalyst, wherein Pt content is 0.2-0.5wt%.Preparation process of the invention is simple, can a step simultaneously realize active component dispersion load and carrier structure optimization.The catalyst is applied to the catalysis burning of the VOCs such as toluene, dimethylbenzene, shows preferable low temperature active and stability, and generate without other exhaust gas.
Description
Technical field
The invention belongs to environmental catalysis purification techniques fields, specifically provide a kind of in situ closing applied to VOCs catalysis burning
At Pt/MnO2@Mn3O4Catalyst and preparation method thereof.
Background technique
With modern industry and expanding economy, environmental problem is got worse, and Air Contamination phenomenon is very prominent.It waves
Hair property organic matter is one of major pollutants in air, and main source includes the industrial waste gas of chemical industry discharge, car tail
Material used in gas and indoor decorating etc..The release of volatile organic matter will form PM2.5 and photochemical fog, destroy
Environmental health, insulting respiratory system and immune system, wherein benzene homologues (such as toluene, dimethylbenzene) even have teratogenesis cause
The harm of mutation, thus it is very urgent to the removal of VOCs in air.Production by Catalytic Combustion Process may be implemented right at a lower temperature
VOCs is converted, and efficient, rugged catalyst application becomes research emphasis and is of great significance.
The catalyst applied to VOCs catalysis burning mainly includes that transition metal oxide and carried noble metal are urged at present
Agent.Compared to the former, loaded noble metal catalyst has preferable low temperature active, high catalytic efficiency and initiation temperature
Low, wherein Pt base catalyst is considered as a kind of ideal VOCs catalytic combustion material.Chen et al. is with TEOS (positive silicic acid tetrem
Ester) it is raw material, carrier ZSM-5 is obtained using hydro-thermal method, then be prepared for Pt content by processes such as dipping, calcining, reduction and be
The Pt/ZSM-5 catalyst of 1wt%, 160 DEG C can to toluene realize complete catalysts oxidation (Chem.Commun., 2015.51,
5936-5938).Zhang et al. is prepared for layering porous zeolite using hydro-thermal reaction and acid, alkali process, is with aluminium oxide with it
Carrier obtains the Pt loaded catalyst that content is 1wt% by infusion process, reaches 90% toluene in 190 DEG C and 210 DEG C respectively
Conversion ratio (Chem.Eng.J., 2018.334,10-18).It is usually needed by the Pt base catalyst of carrier of inert components such as molecular sieves
High molecular polymer is used, preparation process is complicated, and catalyst is easily poisoned.Utilize transition metal oxide (CeO2、TiO2、
MnOxDeng) supporting Pt can simplify carrier preparation process, stability is preferable, the adjustable Pt of the synergistic effect between carrier and Pt
The chemical valence state of species, active oxidation object lattice surface oxygen, so as to improve the performance of catalyst.Therefore, it is with this type oxide
Carrier loaded Pt has obtained a large amount of research.Chinese patent CN 103386312A obtains CeO using microwave-hydrothermal method2, recycle
Infusion process is prepared for catalyst Pt/CuO-CeO that Pt load capacity is 1wt%2, toluene catalytic combustion is applied it to, at 250 DEG C
Reach 100% toluene removal.Pt is loaded to different MnO by liquid phase reduction by Zhou et al.2On, obtain Pt/ α-MnO2、
Pt/L-MnO2(stratiform MnO2) and Pt/ α-MnO2@L-MnO2, when Pt content is 1wt%, analysis finds Pt/ α-MnO2@L-
MnO2Middle Pt0Content it is most, the presence of mixed phase carrier can promote O2Adsorption activation and product desorption, in room temperature
The removal of one hour PARA FORMALDEHYDE PRILLS(91,95) of lower reaction is up to 92.1%, higher than the above two 81.3% and 75.9% (Appl.Catal.B-
Environ.,2017.207,233-243).Mao et al. prepares cubic and mesoporous CeO2Afterwards, impregnated by stirring,
Grinding reduction obtains Pt/CeO2, the results showed that, the difference of carrier will affect the activity and reducibility of catalyst surface Lattice Oxygen
And the concentration of surface Lacking oxygen, wherein meso-pore Ce O2It is more excellent to load 1wt%Pt performance, benzene can be urged completely at 175 DEG C
Change oxidation (ACS Catal., 2016.6,418-427).Although using the existing many researchs of transition metal oxide supporting Pt,
Catalyst preparation usually requires multistep, and process is more complex, simultaneously as Pt belongs to noble metal (Pt unit price is about 180 yuan/gram),
Expensive, the load capacity of 1wt% is still higher, and application cost is caused to improve, and catalytic activity and stability need into
One step is promoted.
In view of the above-mentioned problems, the present invention passes through liquid phase reduction fabricated in situ Pt/MnO2@Mn3O4Catalyst, Pt active matter
The load of kind and carrier structure optimize a step and are completed at the same time, and do not need the calcining in later period, and preparation process is simply quick, simultaneously
Pt active component content can be effectively controlled in 0.5wt% hereinafter, greatly reduce application cost, is applied to be catalyzed in VOCs and be fired
In burning, the VOCs that may be implemented under lower temperature is converted completely.
Summary of the invention
The object of the present invention is to provide fabricated in situ Pt/MnO2@Mn3O4Catalyst and its specific preparation method, and be used for
VOCs catalysis burning.The characteristics of catalyst include preparation method is simple, Pt load capacity is low, it is active it is high, stability is good etc., carrier
Material source is extensively and relative low price, the repeatability height of catalyst show good low temperature in VOCs catalysis burning
Activity.
Technical solution of the present invention：
Fabricated in situ Pt/MnO for VOCs catalysis burning2@Mn3O4Catalyst, carrier are mixed phase MnO2@Mn3O4, Pt
Content be 0.2-0.5wt%.
Fabricated in situ Pt/MnO for VOCs catalysis burning2@Mn3O4The preparation method of catalyst, steps are as follows：
(1) potassium permanganate is dissolved in deionized water, the magnetic agitation 20-30min under 60 DEG C of water bath conditions；Again grass
Acid dissolution obtains oxalic acid solution in deionized water；The molar ratio for controlling potassium permanganate and oxalic acid is 1:1-2, the two solution body
Product is identical；Gained oxalic acid solution is added drop-wise in liquor potassic permanganate dropwise, 20-50min is mixed under the conditions of 60 DEG C；With
Mixed solution is poured into reaction kettle afterwards, is placed into baking oven, in 180 DEG C of hydro-thermal reaction 12h；
(2) it is cooled to room temperature to temperature of reaction kettle, gained precipitating deionized water and dehydrated alcohol centrifuge washing is placed
The dry 10-24h in 60-100 DEG C of baking oven；5-8h then is calcined under the conditions of 300-500 DEG C, obtains MnO2；
(3) by MnO obtained by step (2)2Powder is scattered in deionized water, and appropriate H is added2PtCl6Solution is vigorously stirred
30-60min obtains suspension；The NaBH that subsequent compound concentration is 0.01mol/L-0.05mol/L4Solution is added rapidly to
It states in suspension, continues to stir 60-90min；MnO in mixed solution2:Pt4+:NaBH4Molar ratio be 6.55-6.95:0.01-
0.03:0.001-0.005；
(4) it after washing the obtained precipitating deionized water of step (3) and dehydrated alcohol, is done in 60-100 DEG C of baking oven
Dry 10-15h obtains the Pt/MnO of fabricated in situ2@Mn3O4Catalyst, wherein the content of Pt is 0.2-0.5wt%.
Pt/MnO of the invention2@Mn3O4Catalyst is applied to VOCs catalysis burning, and reaction gas is 100-1000ppm volatilization
Property organic gas, Balance Air be Ar and O2Gaseous mixture, wherein O2Volume fraction is 20%, and hybrid reaction gas air speed is 20000h-1-60000h-1, continuous operation carries out active testing on micro-reaction device.The catalyst can be in 30-180 DEG C of realization VOCs
Removal.
Pt/MnO of the invention2@Mn3O4Catalyst can realize that VOCs is catalyzed burning completely at a lower temperature, and have compared with
Good stability.Meanwhile the catalyst also can be applied to the removal of ammonia selective catalytic oxidation and nitrogen oxides.
The beneficial effects of the invention are that：In conjunction with hydro-thermal method and liquid phase reduction fabricated in situ Pt/MnO2@Mn3O4Catalyst.
With mixed phase Mn oxide supporting Pt, the ability of activation of catalyst oxygen is can be improved in the synergistic effect of carrier and noble metal, keeps its right
The catalyst combustion reaction of benzene homologues (such as toluene, dimethylbenzene) has good low temperature active and stability in VOCs.Preparation side
Method is simple, and Pt load capacity is low (≤0.5wt%), and carrier material is from a wealth of sources and price is relatively low, and catalyst is reproducible, answers
With at low cost, it can be catalyzed completely burning removal VOCs in lower temperature, there is good commercial application potentiality.
Detailed description of the invention
Fig. 1 is the XRD spectra of catalyst A, B, C, D prepared by embodiment 1 and comparative example 1-3.
Fig. 2 is the toluene catalytic combustion activity figure of catalyst A, B, C, D prepared by embodiment 1 and comparative example 1-3.
Fig. 3 is catalyst A reaction stability activity figure prepared by embodiment 1.
Specific embodiment
With reference to the accompanying drawing and technical solution, a specific embodiment of the invention is further illustrated.
Embodiment 1
Fabricated in situ Pt/MnO2@Mn3O4The preparation of catalyst：
(1) 0.02mol potassium permanganate is dissolved in 35mL deionized water, is placed under 60 DEG C of water bath conditions and is vigorously stirred；It will
0.036mol oxalic acid is dissolved in 35mL deionized water, obtains oxalic acid solution；While agitating, oxalic acid solution is added drop-wise to dropwise
In liquor potassic permanganate, in 60 DEG C of stirring 30min after mixing；Mixed solution is transferred in reaction kettle again, is reacted in 180 DEG C
12h.By the precipitating deionized water and dehydrated alcohol centrifuge washing after reaction, dry 12h is put into 80 DEG C of baking ovens, later in horse
Not 400 DEG C of calcining 5h in furnace, obtain MnO2；
(2) MnO for taking 0.6g to prepare2It is scattered in 8mL deionized water, it is 0.0193mol/L's that 0.8mL concentration, which is added,
H2PtCl6Solution stirs 60min at normal temperature；Prepare the NaBH of 0.005mol/L4Solution takes solution 0.95mL to be added aforementioned
In mixed liquor, continue to stir 60min.By obtained material centrifuge washing, it is put in 80 DEG C of baking ovens dry 12h, obtains fabricated in situ
Pt/MnO2@Mn3O4, it is denoted as catalyst A, wherein the mass content of Pt is 0.3wt%.
Comparative example 1
Pt/MnO2The preparation of catalyst：It weighs 0.034g PVP (polyvinylpyrrolidone) and 0.09g sodium citrate is dissolved in
In 50mL deionized water, it is stirred and heated to 80 DEG C in oil bath；Take 0.8mL H2PtCl6Solution is added drop-wise to mixed solution dropwise
In, stir 5min；0.054g ascorbic acid is dissolved in 5mL water again, is added dropwise in mixed solution, is stirred under the conditions of 80 DEG C
60min；Take the MnO prepared in 0.6g embodiment 12In 50mL deionized water aforementioned colloidal solution is added, in 80 in ultrasonic disperse
DEG C continue to stir 4h.By the solid centrifuge washing after reaction, dry 12h, obtains Pt/MnO in 80 DEG C of baking ovens2, it is denoted as catalysis
Agent B, wherein the mass content of Pt is 0.3wt%.
Comparative example 2
Pt/Mn3O4The preparation of catalyst：Weigh the Mn of 0.6g purchase3O4It is scattered in 10mL deionized water, 0.8mL is added
H2PtCl610min is mixed in solution；It takes suitable sodium borohydride, sodium hydroxide, sodium citrate to be dissolved in deionized water, makes
Its concentration is respectively 0.572mol/L, 0.250mol/L and 0.001mol/L, and by 5mL, the mixed solution rapidly joins at 60 DEG C
In aforementioned liquids, it is vigorously stirred 60min.By obtained material centrifuge washing, dry 12h, obtains Pt/Mn in 80 DEG C of baking ovens3O4,
It is denoted as catalyst C, wherein the mass content of Pt is 0.3wt%.
Comparative example 3
Substep synthesis Pt/MnO2@Mn3O4The preparation of catalyst：
(1) MnO prepared in 1g embodiment 1 is taken2, it is added to the NaBH that 100mL concentration is 0.15mol/L4It is acute in solution
Strong stirring 1h；By obtained solid centrifuge washing, the dry 12h in 80 DEG C of baking ovens, then will it is dry after sample in 200 DEG C of roasting 5h,
Obtain required carrier；
(2) according to the method supporting Pt in comparative example 1, the difference is that, used carrier is to obtain obtained by step (1)
The Pt/MnO of substep synthesis2@Mn3O4, it is denoted as catalyst D, wherein the mass content of Pt is 0.3wt%.
Embodiment 2
To catalyst A, B, C prepared by embodiment 1 and comparative example 1-3, D progress X-ray diffraction test is obtained corresponding
XRD spectra, as a result as shown in Figure 1.All catalyst do not occur the diffraction maximum of Pt.The catalyst of embodiment 1 and comparative example 3
It is shown as MnO2And Mn3O4Mixed phase, comparative example 1 and 2 respectively only have MnO2And Mn3O4Corresponding diffraction maximum.
Embodiment 3
Toluene catalytic combustion active testing is carried out to catalyst obtained by embodiment 1 and comparative example 1-3, the device used is certainly
The continuous microreactor of fixed bed processed carries out quantitative analysis oxidation reaction by the gas-chromatography GC 7900 configured with fid detector
The concentration of front and back toluene.The actual conditions of test include：Toluene initial concentration is 500ppm, using argon gas as Balance Air, reaction gas
Body air speed is 24000h-1；Chromatographic column is benzene homologues dedicated columns, and column temperature is 80 DEG C when detection, and detector temperature is 200 DEG C.Respectively urge
The reactivity of agent is as shown in Fig. 2, wherein the activity of catalyst A preferably, realizes that the removal rate of toluene reaches at 150 DEG C
97%.
Embodiment 4
Catalyst A prepared by embodiment 1 is used for catalytic combustion reaction for xylene reaction, the initial concentration of dimethylbenzene is
500ppm, chromatographic column column temperature is 100 DEG C when detection, remaining condition is same as Example 3.Test result is as shown in table 1.
1 active testing result of table
Embodiment 5
Stability test is carried out to catalyst A prepared by embodiment 1, reaction condition is in the same manner as in Example 3, as a result as schemed
Shown in 3.By it in 160 DEG C of follow-on test 48h, toluene conversion is always held at 99% or more, show the catalyst have compared with
Good stability.
Embodiment 6
Adjustment gas flow makes toluene concentration increase to 1000ppm, keeps other conditions in the same manner as in Example 3, to reality
It applies 1 gained catalyst A of example and carries out active testing.Measurement result shows that the catalyst can achieve 97% toluene conversion at 160 DEG C
Rate, concrete outcome are as shown in table 2.
2 active testing result of table
Claims (3)
1. a kind of fabricated in situ Pt/MnO for VOCs catalysis burning2@Mn3O4Catalyst, which is characterized in that the original position
Synthesize Pt/MnO2@Mn3O4The carrier of catalyst is mixed phase MnO2@Mn3O4, the content of Pt is 0.2-0.5wt%.
2. a kind of fabricated in situ Pt/MnO for VOCs catalysis burning2@Mn3O4The preparation method of catalyst, which is characterized in that
Steps are as follows：
(1) potassium permanganate is dissolved in deionized water, the magnetic agitation 20-30min under 60 DEG C of water bath conditions；It is again that oxalic acid is molten
Solution obtains oxalic acid solution in deionized water；The molar ratio for controlling potassium permanganate and oxalic acid is 1:1-2, the two liquor capacity phase
Together；Gained oxalic acid solution is added drop-wise in liquor potassic permanganate dropwise, 20-50min is mixed under the conditions of 60 DEG C；Then will
Mixed solution pours into reaction kettle, is placed into baking oven, in 180 DEG C of hydro-thermal reaction 12h；
(2) it is cooled to room temperature to temperature of reaction kettle, gained precipitating deionized water and dehydrated alcohol centrifuge washing is placed in
Dry 10-24h in 60-100 DEG C of baking oven；5-8h then is calcined under the conditions of 300-500 DEG C, obtains MnO2；
(3) by MnO obtained by step (2)2Powder is scattered in deionized water, and appropriate H is added2PtCl6Solution is vigorously stirred 30-
60min obtains suspension；The NaBH that subsequent compound concentration is 0.01mol/L-0.05mol/L4Solution is added rapidly to above-mentioned
In suspension, continue to stir 60-90min；MnO in mixed solution2:Pt4+:NaBH4Molar ratio be 6.55-6.95:0.01-
0.03:0.001-0.005；
(4) dry in 60-100 DEG C of baking oven after washing the obtained precipitating deionized water of step (3) and dehydrated alcohol
10-15h obtains the Pt/MnO of fabricated in situ2@Mn3O4Catalyst, wherein the content of Pt is 0.2-0.5wt%.
3. a kind of fabricated in situ Pt/MnO2@Mn3O4Application of the catalyst for VOCs catalysis burning, which is characterized in that reaction gas
For 100-1000ppm volatile organic gases, Balance Air is Ar and O2Gaseous mixture, wherein O2Volume fraction is 20%, and mixing is anti-
Should gas air speed be 20000h-1-60000h-1, reaction temperature is 30-180 DEG C, and continuous operation carries out activity on micro-reaction device
Test.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111496268A (en) * | 2020-05-13 | 2020-08-07 | 华侨大学 | Size-controllable Pt/MnO2Nano material and preparation method thereof |
| CN112604686A (en) * | 2020-11-20 | 2021-04-06 | 珠海格力电器股份有限公司 | Normal-temperature formaldehyde removal catalyst, and preparation method and application thereof |
| CN113181956A (en) * | 2021-05-10 | 2021-07-30 | 中国科学院大学 | Combined catalyst and method for treating nitrogen-containing volatile organic compound pollutants |
| CN115155579A (en) * | 2022-07-23 | 2022-10-11 | 重庆科技学院 | Reductive noble metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas and preparation method thereof |
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| CN102728356A (en) * | 2011-04-01 | 2012-10-17 | 中国科学院理化技术研究所 | Pt nanparticle-supported MnO2 catalyst, its preparation method and application thereof |
| CN106475090A (en) * | 2016-10-13 | 2017-03-08 | 中国人民解放军后勤工程学院 | A kind of Mn3O4‑MnO2Nano composite material preparation method and applications |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102728356A (en) * | 2011-04-01 | 2012-10-17 | 中国科学院理化技术研究所 | Pt nanparticle-supported MnO2 catalyst, its preparation method and application thereof |
| CN106475090A (en) * | 2016-10-13 | 2017-03-08 | 中国人民解放军后勤工程学院 | A kind of Mn3O4‑MnO2Nano composite material preparation method and applications |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111496268A (en) * | 2020-05-13 | 2020-08-07 | 华侨大学 | Size-controllable Pt/MnO2Nano material and preparation method thereof |
| CN112604686A (en) * | 2020-11-20 | 2021-04-06 | 珠海格力电器股份有限公司 | Normal-temperature formaldehyde removal catalyst, and preparation method and application thereof |
| CN113181956A (en) * | 2021-05-10 | 2021-07-30 | 中国科学院大学 | Combined catalyst and method for treating nitrogen-containing volatile organic compound pollutants |
| WO2022194306A1 (en) * | 2021-05-10 | 2022-09-22 | 中国科学院大学 | Composite catalyst and method for treating nitrogen-containing volatile organic composite pollutants |
| CN115155579A (en) * | 2022-07-23 | 2022-10-11 | 重庆科技学院 | Reductive noble metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas and preparation method thereof |
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