CN109675558A - Two-dimentional palladium tungsten bimetal nano catalyst, preparation method and application - Google Patents
Two-dimentional palladium tungsten bimetal nano catalyst, preparation method and application Download PDFInfo
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Abstract
Two-dimentional palladium tungsten bimetal nano catalyst, preparation method and application, belong to technical field of function materials.PdW bimetal nano piece is loaded into TiO2On carrier, then passes through calcination and form PdW/TiO2Catalyst.The load capacity of Metal Palladium is 0.67wt%.The preparation method comprises the following steps: restoring palladium acetylacetonate simultaneously with tungsten carbonyl using the method for solvent-thermal process, ultra-thin PdW bimetal nano piece is formed, then bimetal leaf is loaded to by TiO using infusion process2On carrier, Pd load capacity is 0.67wt%.Loaded catalyst is formed into PdW/TiO by 350 DEG C of calcinations2Nanocatalyst.PdW/TiO prepared by the present invention2Nanocatalyst preparation process is simple, has a good application prospect in catalytic field.
Description
Technical field
The present invention relates to a kind of two-dimentional palladium tungsten nanocatalysts and preparation method thereof, and in particular to using solvent-thermal process
Method preparation has the PdW nanometer sheet of ultra-thin two-dimension structure, is loaded to TiO using infusion process2On, after then passing through calcination
Form TiO2The PdW bimetallic catalyst of load.There is the loaded catalyst of higher catalytic activity to benzene oxidatoin, belong to function
Field of material technology.
Background technique
With the development of modern industry science and technology, people's lives level is increasingly improved.But the industrial waste gas generated therewith
Discharge be to cause the one of the major reasons of atmosphere pollution.Severe atmosphere pollution situation makes air treating extremely urgent.It waves
Hair property organic compound (Volatile Organic Compounds, referred to as VOCs) is the main constituents of industrial waste gas
One of, most VOCs is directly detrimental to health, and VOCs is also considered to be fine particle and ozone in atmosphere and is formed
Important as precursors object.Benzene is a kind of VOCs with strong carcinogenicity.In many technologies of purification benzene, catalytic oxidation is mesh
One of preceding the most frequently used and most effective technology for eliminating.And the research and development of effective catalyst are the cores of the technology.
Currently, domestic and international researcher has done a large amount of research to the catalyst for catalytic oxidation of benzene, some achievements are achieved.
Liu et al. (J.Liu, et al., Catal.Today, 2017,297:211-218) has studied γ-Al2O3Load Pd nano particle is urged
Agent finds the TiO in load 2.66%Pd nano particle to the performance of the catalysis oxidation of benzene2The T of upper benzene conversion90%It is 190
DEG C, but Pd load capacity is higher.(T.Tabakova, the et al., Chem.Eng.J., 2015,260:133- such as Tabakova
Etc. 141) load Au is had studied, the oxidation susceptibility of benzene on the Fe-Ce catalyst of Pd.Au is loaded, Pd is bimetallic to pass through dipping
The Fe-Ce catalyst of method preparation realizes the complete oxidation to benzene at 200 DEG C.However expensive price and high temperature easy-sintering
And the characteristics such as inactivation limit the application of noble metal catalyst.Be modified with transition metal to noble metal is a kind of effective side
Formula.It is also generally believed other than the strong interaction between noble metal and carrier, between bimetallic there are stronger interaction,
The electronics and geometry that noble metal would generally be improved using the doping of transition metal, further increase catalytic activity.
Hosseini etc. (M.Hosseini, et al., Catal.Today, 2007,122:391-396) have studied be supported on it is mesoporous
TiO2On a series of Pd-Au bimetallic catalysts, find catalysis oxidation either to toluene or propylene, Pd-Au/TiO2
Catalytic activity be superior to Pd/TiO2。
Usually, the structure of catalyst has with its catalytic performance and closely contacts.Ultra-thin two-dimension nano material due to
Characteristic with covalent bond and thickness strong in Two-dimensional electron effect, plane shows unique physicochemical properties, and has
There are higher specific surface area and active site abundant.(J.Di, the et al., Mater.Today, 2018,21:749- such as Di
770) application of the ultra-thin two-dimension material in photoelectrocatalysis liberation of hydrogen and electrocatalytic hydrogen evolution field is summarized.
As far as we know, there is presently no document and patent report, to cross the PdW with ultra-thin two-dimension flaky nanometer structure bis-
The preparation method and its loaded catalyst of metallic nano crystal are used for the research of catalysis oxidation benzene.
Summary of the invention
The object of the present invention is to provide a kind of using solvent process for thermosynthesizing preparation with ultrathin nanometer chip architecture to benzene
TiO with high catalytic activity2The method of/PdW nanocatalyst.
TiO2/ PdW catalyst, which is characterized in that the method for first passing through solvent-thermal process prepares PdW nanometer sheet, then adopts
PdW nanometer sheet is loaded into nano-TiO with infusion process2On carrier, then passes through calcination and form TiO2/ PdW catalyst；Above-mentioned sample
The load capacity of Pd is 0.2-1wt% in product, and the load capacity of preferably 0.67wt%, W is 0.5-1.5wt%, preferably 0.93wt%, such as
The load capacity of Pd is the load capacity of 0.67wt%, W referred to as 0.67wt%Pd 0.93wt%W/TiO when being 0.93wt%2.Pd receives
Rice piece with a thickness of 1nm or so, face is having a size of 100-200nm.
The characteristics of above-mentioned PdW bimetal nano piece, is that the nanometer sheet being prepared has ultra-thin two-dimension structure, system
It is standby to mainly comprise the steps that
(1) palladium acetylacetonate is weighed, toluene, oleyl amine is added, is placed on magnetic stirring apparatus, at room temperature stirring and dissolving 20min
Afterwards, W (CO) is weighed6It is added in the mixed solution, forms mixing precursor solution, continue to be packed into after stirring 5-10min at room temperature
In reaction kettle, the preferred 4h of 3-6h is kept the temperature in 130-200 DEG C preferably 160 DEG C of baking ovens；After being cooled to room temperature, reaction solution is placed in
In centrifuge tube, ethyl alcohol, ultrasound is added, ultra-thin PdW bimetal nano piece is made after washing 3-4 times repeatedly in centrifugation；It finally will system
The PdW nanometer sheet obtained is evenly dispersed to be saved into hexamethylene；
(2) obtained PdW bimetal nano piece is loaded on carrier using infusion process, then passes through calcination process, obtains
To PdW/TiO2Nanocatalyst；Specific step is as follows:
Amount containing PdW nanometer sheet solution required for being calculated according to load capacity, by a certain amount of TiO2Carrier is added to
In the cyclohexane solution containing PdW nanometer sheet measured；Stirring dipping 12h, centrifugation obtain loaded catalyst；It is urged what is obtained
Agent is fitted into porcelain boat and is placed in Muffle furnace, rises to 320 DEG C -380 DEG C preferably 350 DEG C from room temperature with the rate of 5 DEG C/min, and at this
At a temperature of keep 1-3h, preferably 2h, cooling obtains PdW/TiO2Nanocatalyst.
The preferably every 0.02mmol palladium acetylacetonate of step (1), corresponding toluene 1-10ml (preferably 5ml), oleyl amine 2-4ml are (excellent
Select 3.5ml)；W(CO)6Additional amount be added according to W load capacity.
Gained catalyst of the invention is used for the oxidation of benzene, is ultimately oxidized as carbon dioxide and water.
It is preferred that benzene concentration is 1000ppm, benzene/oxygen molar ratio is 1/400 and air speed is the anti-of 40000mL/ (gh)
Under the conditions of answering, catalyst T50%(benzene conversion ratio reaches required reaction temperature when 50%) and T90%(when benzene conversion ratio reaches 90%
Required reaction temperature) it is respectively 178 DEG C and 200 DEG C.
The present invention has many characteristics, such as that preparation process is simple.Especially 0.67wt%Pd0.93wt%W/ prepared by the present invention
TiO2Catalyst has excellent catalytic activity, has a good application prospect in benzene catalysis oxidation field.
Utilize D8ADVANCE type X-ray diffractometer (XRD), JEOL-2010 type transmission electron microscope (TEM) and Shimadzu
Crystal structure, particle morphology and the catalysis oxidation to benzene of catalyst obtained by the Instrument measurings such as GC-2014 gas-chromatography (GC)
Activity.The result shows that all having preferable crystallinity, PdW nanometer sheet pattern using each sample obtained by method of the invention
Regular, bimetal supported catalyst significantly improves the catalytic oxidation activity of benzene compared to purer supported palladium catalyst.
Detailed description of the invention
Fig. 1 is obtained PdW/TiO2And Pd/TiO2The XRD spectra of sample, wherein curve (a) and (b) are respectively embodiment
1 and contrast sample Pd/TiO2XRD spectra；
Fig. 2 is the TEM photo of obtained PdW and Pd sample, wherein figure (a), (b), (c) and (d) be respectively Pd
The TEM photo of grain and the different proportion of embodiment 1；
Fig. 3 is PdW/TiO obtained by embodiment 12And Pd/TiO2The activity curve of catalysis oxidation benzene on sample.
Specific embodiment
In order to further appreciate that the present invention, elaborated below with embodiment, but the present invention is not limited to following implementations
Example.
Embodiment 1
0.02mmol palladium acetylacetonate is weighed, toluene 5mL is added, oleyl amine 3.5mL is placed on magnetic stirring apparatus, at room temperature
After stirring and dissolving 20min, 0.14mmol W (CO) is weighed6It is added in the mixed solution, forms mixing precursor solution, continue room
It is fitted into reaction kettle after the lower stirring 5-10min of temperature, keeps the temperature 4h in 160 DEG C of baking ovens.After being cooled to room temperature, reaction solution is placed in
In centrifuge tube, ethyl alcohol, ultrasound is added, ultra-thin PdW bimetal nano piece is made after washing 3-4 times repeatedly in centrifugation.It finally will system
The PdW nanometer sheet obtained is evenly dispersed to be saved into 10mL hexamethylene.
Obtained PdW bimetal nano piece is loaded on carrier using infusion process, calcination process is then passed through, obtains
PdW/TiO2Nanocatalyst.Specific step is as follows:
Amount containing PdW bimetallic solution required for being calculated according to certain load capacity, by a certain amount of TiO2Carrier adds
Enter into the cyclohexane solution containing bimetal nano crystalline substance of measurement.Stirring dipping 12h, centrifugation obtain loaded catalyst.It will
Obtained catalyst is fitted into porcelain boat and is placed in Muffle furnace, rises to 350 DEG C from room temperature with the rate of 5 DEG C/min, and at such a temperature
2h is kept, cooling obtains PdW/TiO2Nanocatalyst.
Benzene concentration is 1000ppm, benzene/oxygen molar ratio is 1/400 and air speed is the reaction item of 40000mL/ (gh)
Under part, catalyst T50%(benzene conversion ratio reaches required reaction temperature when 50%) and T90%(benzene conversion ratio reaches required when 90%
Reaction temperature) it is respectively 178 DEG C and 200 DEG C.Oxidation product is carbon dioxide and water.
Claims (7)
1.TiO2/ PdW catalyst, which is characterized in that the method for first passing through solvent-thermal process prepares PdW nanometer sheet, then using leaching
PdW nanometer sheet is loaded to nano-TiO by stain method2On carrier, then passes through calcination and form TiO2/ PdW catalyst.
2. TiO described in accordance with the claim 12/ PdW catalyst, which is characterized in that the load capacity of Pd is 0.2- in sample
1wt%, preferably 0.67wt%, the load capacity of W are 0.5-1.5wt%, preferably 0.93wt%.
3. TiO described in accordance with the claim 12/ PdW catalyst, which is characterized in that Pd nanometer sheet with a thickness of 1nm, face size
For 100-200nm.
4. preparing the described in any item TiO of claim 1-32The method of/PdW catalyst, which comprises the following steps:
(1) palladium acetylacetonate is weighed, toluene, oleyl amine is added, is placed on magnetic stirring apparatus, at room temperature after stirring and dissolving 20min, is claimed
Take W (CO)6It is added in the mixed solution, forms mixing precursor solution, continue to be packed into reaction kettle after stirring 5-10min at room temperature
In, the preferred 4h of 3-6h is kept the temperature in 130-200 DEG C preferably 160 DEG C of baking ovens；After being cooled to room temperature, reaction solution is placed in centrifuge tube
In, ethyl alcohol, ultrasound is added, ultra-thin PdW bimetal nano piece is made after washing 3-4 times repeatedly in centrifugation；Finally by PdW obtained
Nanometer sheet is evenly dispersed to be saved into hexamethylene；
(2) obtained PdW bimetal nano piece is loaded on carrier using infusion process, then passes through calcination process, obtains
PdW/TiO2Nanocatalyst；Specific step is as follows:
Amount containing PdW nanometer sheet solution required for being calculated according to load capacity, by a certain amount of TiO2Carrier is added to measurement
In cyclohexane solution containing PdW nanometer sheet；Stirring dipping 12h, centrifugation obtain loaded catalyst；Obtained catalyst is filled
Enter porcelain boat to be placed in Muffle furnace, rises to 320 DEG C -380 DEG C preferably 350 DEG C from room temperature with the rate of 5 DEG C/min, and at such a temperature
1-3h, preferably 2h are kept, cooling obtains PdW/TiO2Nanocatalyst.
5. according to the method for claim 4, which is characterized in that the every 0.02mmol palladium acetylacetonate of step (1), corresponding toluene
1-10ml (preferably 5ml), oleyl amine 2-4ml (preferably 3.5ml).
6. according to the method for claim 4, which is characterized in that W (CO)6Additional amount be added according to W load capacity.
7. the described in any item TiO of claim 1-32The application of/PdW catalyst is ultimately oxidized as dioxy for the oxidation of benzene
Change carbon and water.
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Cited By (7)
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| CN110639549A (en) * | 2019-09-19 | 2020-01-03 | 北京工业大学 | Universal method for preparing high-stability noble metal monatomic catalyst |
| CN110639548A (en) * | 2019-09-19 | 2020-01-03 | 北京工业大学 | Monoatomic palladium-cobalt bimetallic nano-catalyst for efficiently catalyzing benzene oxidation |
| CN111185166A (en) * | 2020-01-14 | 2020-05-22 | 北京工业大学 | Supported platinum-tungsten bimetallic nano catalyst for efficiently catalyzing and oxidizing benzene |
| CN112643045A (en) * | 2020-12-18 | 2021-04-13 | 华侨大学 | Palladium-ruthenium ultrathin nanosheet, preparation method thereof and application of palladium-ruthenium ultrathin nanosheet as electrocatalyst |
| CN112676571A (en) * | 2020-12-14 | 2021-04-20 | 北京化工大学 | Preparation method of supported PdW bimetallic elementary substance nanoparticles |
| CN114768801A (en) * | 2022-04-26 | 2022-07-22 | 海南大学 | Preparation method and application of supported palladium-gold alloy nanosheet catalyst |
| CN115301263A (en) * | 2022-08-19 | 2022-11-08 | 常州大学 | Ag/SiC catalyst, preparation method and application thereof in styrene epoxidation reaction |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110639549A (en) * | 2019-09-19 | 2020-01-03 | 北京工业大学 | Universal method for preparing high-stability noble metal monatomic catalyst |
| CN110639548A (en) * | 2019-09-19 | 2020-01-03 | 北京工业大学 | Monoatomic palladium-cobalt bimetallic nano-catalyst for efficiently catalyzing benzene oxidation |
| CN110639548B (en) * | 2019-09-19 | 2022-06-14 | 北京工业大学 | Monoatomic palladium-cobalt bimetallic nano-catalyst for efficiently catalyzing benzene oxidation |
| CN111185166A (en) * | 2020-01-14 | 2020-05-22 | 北京工业大学 | Supported platinum-tungsten bimetallic nano catalyst for efficiently catalyzing and oxidizing benzene |
| CN112676571A (en) * | 2020-12-14 | 2021-04-20 | 北京化工大学 | Preparation method of supported PdW bimetallic elementary substance nanoparticles |
| CN112643045A (en) * | 2020-12-18 | 2021-04-13 | 华侨大学 | Palladium-ruthenium ultrathin nanosheet, preparation method thereof and application of palladium-ruthenium ultrathin nanosheet as electrocatalyst |
| CN112643045B (en) * | 2020-12-18 | 2023-04-18 | 华侨大学 | Palladium-ruthenium ultrathin nanosheet, preparation method thereof and application of palladium-ruthenium ultrathin nanosheet as electrocatalyst |
| CN114768801A (en) * | 2022-04-26 | 2022-07-22 | 海南大学 | Preparation method and application of supported palladium-gold alloy nanosheet catalyst |
| CN114768801B (en) * | 2022-04-26 | 2023-12-01 | 海南大学 | Preparation method and application of supported palladium-gold alloy nanosheet catalyst |
| CN115301263A (en) * | 2022-08-19 | 2022-11-08 | 常州大学 | Ag/SiC catalyst, preparation method and application thereof in styrene epoxidation reaction |
| CN115301263B (en) * | 2022-08-19 | 2024-03-12 | 常州大学 | Ag/SiC catalyst, preparation method and application thereof in styrene epoxidation reaction |
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