CN108777309A - A kind of monatomic Pd catalyst of support type and preparation method thereof and catalytic applications - Google Patents
A kind of monatomic Pd catalyst of support type and preparation method thereof and catalytic applications Download PDFInfo
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- CN108777309A CN108777309A CN201810463913.5A CN201810463913A CN108777309A CN 108777309 A CN108777309 A CN 108777309A CN 201810463913 A CN201810463913 A CN 201810463913A CN 108777309 A CN108777309 A CN 108777309A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
- H01M8/1013—Other direct alcohol fuel cells [DAFC]
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Abstract
The invention discloses monatomic Pd catalyst of a kind of support type and preparation method thereof and catalytic applications.The present invention is successfully prepared the monatomic Pd catalyst materials of support type in NiFe hydrotalcite supports, using light deposition reduction method, and the properties such as pattern, structure and valence state for characterizing using a variety of characterization techniques monatomic Pd catalyst materials.The present invention is by comparing the electrocatalytic oxidation ethanol synthesis result of carrier, monatomic Pd catalyst and nano Pd catalyst it is found that monatomic Pd catalyst has electrocatalytic oxidation ethanol synthesis best catalytic activity and stability.And the oxidation peak peak current density of monatomic Pd catalyst is approximately 5 times of NiFe hydrotalcite supports.After different hydrogen reduction treatment, the electro catalytic activity of monatomic catalyst is significantly improved again, is approximately 1.5 times of non-reduction treatment sample.
Description
Technical field
The invention belongs to catalyst technical field, it is related to a kind of monatomic Pd catalyst of support type and preparation method thereof and urges
Change application, especially, is prepared using hydrotalcite as the monatomic Pd catalyst of the support type of carrier and its electricity using light deposition reduction method
The application of catalytic oxidation of alcohol reaction.
Background technology
Fossil fuel persistently consumes and causes serious environmental pollution and lack of energy problem.In order to improve such case,
Development cleaning, efficient regenerative resource and energy device become the strategic objective of today's society.Fuel cell is that one kind can
It chemical energy to be directly converted to the device of electric energy, and is not influenced by Carnot cycle, has many advantages, such as high-efficiency environment friendly.With it is direct
Methanol fuel cell is compared, and it (is about 8.01kWh/kg, energy efficiency is that alcohol fuel cell (DEFC), which has energy density high,
0.97) the advantages that, deriving from a wealth of sources, being convenient for storage and transport, is nontoxic.DEFC is primarily present two problems and limits its big rule at present
Mould business application.One is that the anode catalyst of DEFC is easily poisoned by oxidation of ethanol intermediate product, and catalyst activity is caused to weaken；
And major oxidation product is incomplete oxidation acetic acid product and acetaldehyde etc. in reaction process, without can be achieved on 12 electronics
The CO of transfer2, it is only capable of releasing fraction energy.Therefore antitoxin to Catalytic oxidation of ethanol mechanism while deeply probing into
It is turned into and makes good use of and the exploitation of the higher novel electro-catalytic agent of activity is of great significance to development DEFC.
Direct Ethanol Fuel Cell is divided into the DEFC of acid medium and the DEFC of alkaline medium.In the DEF of alkaline medium,
Pd bases catalyst and Ni base catalyst have caused the concern and research of researcher.This is because Pd has organic molecule alcohols
Higher electro catalytic activity and stability.Ni bases catalyst stabilization is good, but catalytic activity is not high.Compared with base metal, Pd
Noble metal whole world reserves are extremely low, price is high.The transformation efficiency of ethyl alcohol electrocatalytic oxidation, reduction are produced into order to better improve
This, it is effective method to load the monatomic of Pd in nickeliferous hydrotalcite supports.Electrocatalytic oxidation second in alkaline medium
In alcohol reaction, on the electrode of the catalyst of base containing Ni, the catalytic activity of oxidation of ethanol depends primarily on Ni (OH)2/ NiOOH oxidations are also
Original conversion mutual between.Absorption and the fracture of C-C keys of ethyl alcohol and oxidation of ethanol intermediate product are reinforced in the presence of monatomic Pd.
Intermediate mixed oxide (nickel oxide and ferriferous oxide) is also the good medium of electronics transfer in nickel-ferric spinel reaction simultaneously.
Invention content
In view of the above-mentioned problems, by the present invention in that nano Pd catalyst even monatomic Pd catalyst is in hydrotalcite supports
High dispersive, avoid electrode surface from covering, in favor of improve electrocatalytic oxidation ethanol synthesis activity and stability.
The present invention provides monatomic Pd catalyst of a kind of support type and preparation method thereof and catalytic applications, utilize light deposition
Prepared by reduction method uses it for electrocatalytic oxidation ethanol synthesis by the monatomic Pd catalyst of the support type of carrier of hydrotalcite.
A kind of monatomic Pd catalyst of support type, which is characterized in that monatomic Pd is distributed in neatly after light deposition reduction
On stone carrier laminate or between laminate, wherein the load capacity of Pd is 0.1-0.3wt%.
Preferably, the hydrotalcite supports are nickel-ferric spinels, and the molar ratio of Ni/Fe is 3/1.
Preferably, Pd load capacity is 0.1wt% on the nickel-ferric spinel carrier.
A kind of preparation method of the monatomic Pd catalyst of support type, which is characterized in that include the following steps：
(1) double drop methods prepare hydrotalcite supports；
(2) method for utilizing light deposition reduction is reducing loaded in hydrotalcite supports in the form of monatomic Pd by Pd ions
On.
Preferably, in the step (1), the hydrotalcite supports are nickel-ferric spinels, and the molar ratio of Ni/Fe is 3/1.
Preferably, in the step (1), the nickel-ferric spinel is prepared by nickel salt and molysite, the nickel salt includes nitre
At least one of sour nickel, nickel chloride or nickel sulfate, the molysite include at least one of ferric nitrate, iron chloride or ferric sulfate.
Preferably, in the step (2), hydrotalcite supports is dissolved in deionized water, are separately added into alcohol and H2PdCl4Solution,
After ultraviolet light, generate electronics and electron hole after the irradiation excitation of hydrotalcite light, the electronics of excitation state by palladium ion also
Original is supported in the form of monoatomic in hydrotalcite supports at atom, and alcohol is empty in the electronics of hydrotalcite supports as sacrifice agent
Oxidation reaction occurs at cave, supplements the electron hole of hydrotalcite.
Preferably, in the step (2), the hydrotalcite dosage is 1g, and alcohol sacrifice agent is ethylene glycol, dosage 5-
30mL is steady current source for xenon lamp lamp, irradiation time 5-30min using ultraviolet source.
Preferably, in the step (2), the above-mentioned catalyst prepared of further reduction treatment, in a hydrogen atmosphere, with
The heating rate of 5-10 DEG C/min is raised to 200 DEG C -500 DEG C of target temperature, and keeps 2-8h.
Preferably, the target temperature be 200 DEG C, 300 DEG C, 400 DEG C or 500 DEG C any one.
After hydrogen reducing handles the above-mentioned catalyst sample prepared at different temperatures, the interaction of Pd and carrier increases
By force, the activity and stability of electrocatalytic oxidation ethyl alcohol be can vary in.
Use the application of the monatomic Pd Catalysts for Electrocatalytic Oxidation ethyl alcohol of above-mentioned support type.
The monatomic Pd catalyst of support type that the above method is prepared is applied to the tool of electrocatalytic oxidation ethanol synthesis
Gymnastics conduct：2mg catalyst is weighed, deionized water, isopropanol and naphthols, ultrasonic 1h is added and forms uniform suspension, uses liquid relief
Rifle is added drop-wise to the glassy carbon electrode surface of test passes.It is tested in the KOH solution of 1mol/L after natural drying, then in 1mol/
LKOH and the test that electro-catalysis ethyl alcohol is carried out in the solution of 1mol/L ethyl alcohol, data are acquired with forward scan, and the rate of scanning is
50mV/s, scanning is ranging from：-0.2-0.8V.
The present invention successfully prepares monatomic Pd catalyst by the method that light deposition restores in hydrotalcite supports.The list
Catalyst atom is effectively improved the catalytic activity and stability of electrocatalytic oxidation ethanol synthesis, and peak current density is approximately water
5 times of steatite support.By above-mentioned catalyst at 300 DEG C after hydrogen reducing, Pd exists still in the form of monoatomic, monatomic Pd
Enhance with carrier Interaction Force, is applied in electrocatalytic oxidation ethanol synthesis, can further improve its catalytic activity
And stability, peak current density are approximately do not restore monatomic catalyst 1.5 times.And prepare the monatomic Pd catalysis of support type
The activity of agent is higher than nano Pd catalyst.
Description of the drawings
Fig. 1 is that NiFe-LDH catalyst, monatomic Pd/NiFe catalyst and the nano Pd particle/NiFe obtained by embodiment 1 are urged
Agent x-ray diffractogram of powder (being respectively a, c, e) and its corresponding scanning electron microscope diagram (b, d, f).
Fig. 2 is gained after the monatomic Pd/NiFe catalyst obtained by embodiment 1 restores in hydrogen under different temperatures
XRD diagram.
Fig. 3 is that the TEM of the monatomic Pd catalyst obtained by embodiment 1 schemes (a) and STEM-HADDF schemes (b).
Fig. 4 is monatomic Pd catalyst obtained by the embodiment 1 gained catalyst sample after hydrogen reducing at 300 DEG C
STEM-HADDF schemes.
Fig. 5 is that NiFe-LDH catalyst, monatomic Pd/NiFe catalyst and the nano Pd particle/NiFe obtained by embodiment 1 are urged
Agent datagram：CV curve graphs in A 1M KOH solutions, B：1M KOH+1M CH3CH2CV curve graphs in OH；C chrono-amperometrics are bent
Line；D electrochemical impedance spectroscopies.
Fig. 6 be embodiment 1 obtained by monatomic Pd/NiFe catalyst and nano Pd particle/NiFe catalyst through different temperatures
The CV curve graphs of electrocatalytic oxidation ethyl alcohol after reduction.
Specific implementation mode
To make those skilled in the art more fully understand technical scheme of the present invention, the present invention is carried below in conjunction with the accompanying drawings
Monatomic Pd catalyst of a kind of support type supplied and preparation method thereof and catalytic applications are described in detail.
Embodiment 1
The preparation of A.NiFe hydrotalcite supports：
Hydrotalcite supports are prepared using double drop methods, the molar ratio of Ni/Fe is 3/1.Before experiment, first by it is used go from
Carbon dioxide in sub- water drains, and with speed maintaining nitrogen purge appropriate, to prevent the carbon dioxide in air from dissolving in again
In deionized water.Suitable experimental drug is weighed with electronic balance, is dissolved in 100ml deionizations, ultrasound accelerates dissolving.Finally match
A concentration of 0.66mol/L NiCl of salt manufacturing solution2·6H2O and 0.22mol/LFeCl3·6H2O, aqueous slkali it is a concentration of
1mol/LNaOH。
Salting liquid and aqueous slkali is added dropwise simultaneously into three-necked flask simultaneously at room temperature, it is 9- during which to keep the pH in flask
10, maintaining nitrogen purge.It is transferred the slurry into polytetrafluoroethylkettle kettle after being added dropwise to complete, by hydrotalcite crystallization 36 at a temperature of 90 DEG C
Hour.Kettle taking-up is cooled to room temperature, is centrifuged repeatedly washing sample until supernatant liquor pH is about 7.Then in vacuum drying oven
Dry at 60 DEG C, the powder sample ground is NiFe-LDH.
B. the preparation of the monatomic Pd catalyst of support type：
The hydrotalcite precursor for weighing 1g preparations first is put into 400mL quartz beakers, and going for 200mL is then added thereto
About 30min is stirred by ultrasonic in the ethylene glycol solution of ionized water and 10mL in ultrasonic machine, until forming evenly dispersed suspension.
Then quartz beaker is placed on magnetic stirring apparatus and is stirred, and quantitative H is added2PdCl4(load capacity of Pd is solution
0.1wt% and 1wt%), then open xenon source direct irradiation quartz beaker 10min.Then acquired solution is centrifuged, is used in combination
Dilute sodium carbonate solution and deionized water centrifuge washing for several times, then three times with ethyl alcohol centrifuge washing, to remove the impurity in solution.It will
Sample after centrifugation is put into 30 DEG C of dryings in vacuum drying chamber.The load capacity of the powder sample obtained after grinding, Pd is 0.1wt%
It is monatomic Pd/NiFe catalyst, monatomic Pd is distributed on hydrotalcite supports laminate or between laminate, the load capacity of Pd
It is nano Pd particle/NiFe catalyst for 1wt%.
C. reducing catalyst sample preparation：Sample is placed on and keeps H2In the atmosphere furnace of atmosphere, with the rate liter of 5 DEG C/min
To certain reduction temperature (200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C), 5h is kept, then instrument is waited for be naturally cooling to room temperature,
It takes out sample and is put into sample cell.
The catalyst sample that above-mentioned three step is prepared is used for electrocatalytic oxidation ethanol synthesis under similarity condition, than
Compared with the effect with the prominent monatomic Pd catalyst of support type.The process conditions of electrocatalytic oxidation ethanol synthesis are：Weigh 2mg catalysis
Agent is added appropriate amount of deionized water, isopropanol and naphthols, ultrasonic 1h and forms uniform suspension.Quantitative suspension is taken with liquid-transfering gun
It is added drop-wise to the glassy carbon electrode surface of test passes.Equal electrodes spontaneously dry after 1mol/L KOH solution and contain 1mol/
The test of electro-catalysis ethyl alcohol is carried out in the solution of LKOH, 1mol/L ethyl alcohol, data are acquired with forward scan, and the rate of scanning is
50mV/s, scanning is ranging from：-0.2-0.8V.Experimental data is finally read and handled on electrochemical workstation.
Reaction result such as Fig. 5 of hydrotalcite supports, monatomic Pd catalyst and nano Pd catalyst obtained by embodiment 1
It is shown.From Fig. 5 (II) it can be seen that in oxidation of ethanol reaction, the oxidation peak peak current density of NiFe hydrotalcite supports is
0.0029322Amps/cm2, the oxidation peak peak current density of monatomic Pd catalyst is 0.010935Amps/cm2, nano Pd particle urges
The oxidation peak peak current density of agent is 0.0029544Amps/cm2.So activity sequence is monatomic Pd/NiFe catalyst>
1PdNiFe-LDH>NiFe-LDH catalyst.
Fig. 6 is monatomic Pd catalyst and nano Pd catalyst electrocatalytic oxidation ethyl alcohol after reduction treatment at different temperatures
Reaction result figure.As can be seen from the figure the reactivity sequence before and after monatomic Pd catalyst treatments is：300℃>Do not locate
Manage sample>400℃>500℃>200℃.Nano Pd catalyst before and after the processing reactivity sequence be：300℃>200℃>Not
Handle sample>400℃>500℃.
The present invention is successfully prepared the monatomic Pd of support type in NiFe hydrotalcite supports, using light deposition reduction method and is catalyzed
Agent material, and the properties such as pattern, structure and valence state for characterizing using a variety of characterization techniques monatomic Pd catalyst materials.This hair
The bright electrocatalytic oxidation ethanol synthesis result by comparing carrier, monatomic Pd catalyst and nano Pd catalyst is it is found that single former
Sub- Pd catalyst has electrocatalytic oxidation ethanol synthesis best catalytic activity and stability.And monatomic Pd catalyst
Oxidation peak peak current density is approximately 5 times of NiFe hydrotalcite supports.After different hydrogen reduction treatment, monatomic catalyst
Electro catalytic activity is significantly improved again, is approximately 1.5 times of non-reduction treatment sample.
The example of the present invention is explained in detail above in conjunction with attached drawing, but the present invention is not limited to examples detailed above, it is all
Any improvement and modification made for the present invention belong to the protection domain of the claims in the present invention.
Claims (9)
1. a kind of monatomic Pd catalyst of support type, which is characterized in that monatomic Pd is distributed in hydrotalcite after light deposition reduction
On carrier laminate or between laminate, wherein the load capacity of Pd is 0.1-0.3wt%.
2. the monatomic Pd catalyst of support type according to claim 1, which is characterized in that the hydrotalcite supports are ferronickels
The molar ratio of hydrotalcite, Ni/Fe is 3/1.
3. the monatomic Pd catalyst of support type according to claim 2, which is characterized in that on the nickel-ferric spinel carrier
Pd load capacity is 0.1wt%.
4. a kind of preparation method of the monatomic Pd catalyst of support type, which is characterized in that include the following steps：
(1) double drop methods prepare hydrotalcite supports；
(2) method for utilizing light deposition reduction is reducing loaded in hydrotalcite supports in the form of monatomic Pd by Pd ions.
5. the preparation method of the monatomic Pd catalyst of support type according to claim 4, which is characterized in that the step
(1) in, the hydrotalcite supports are nickel-ferric spinels, and the molar ratio of Ni/Fe is 3/1；The nickel is prepared by nickel salt and molysite
Molten iron talcum, the nickel salt include at least one of nickel nitrate, nickel chloride or nickel sulfate, and the molysite includes ferric nitrate, chlorine
Change at least one of iron or ferric sulfate.
6. the preparation method of the monatomic Pd catalyst of support type according to claim 5, which is characterized in that the step
(2) in, hydrotalcite supports is scattered in deionized water, are separately added into alcohol and H2PdCl4Solution, after ultraviolet light, hydrotalcite
Electronics is generated after the irradiation excitation of carrier light and palladium ion is reduced into atom by electron hole, the electronics of excitation state, and with single original
The form of son is supported in hydrotalcite supports, and as sacrifice agent oxidation reaction occurs at the electron hole of hydrotalcite supports for alcohol,
Supplement the electron hole of hydrotalcite supports.
7. the preparation method of the monatomic Pd catalyst of support type according to claim 6, which is characterized in that the step
(2) in, the hydrotalcite supports dosage is 1g, and alcohol sacrifice agent is ethylene glycol, and dosage 5-30mL is xenon using ultraviolet source
Lamp stabilized current supply lamp, irradiation time 5-30min.
8. the preparation method of the monatomic Pd catalyst of support type according to claim 7, which is characterized in that further reduction
The catalyst that processing step (2) is prepared is raised to 200 DEG C -500 DEG C with the heating rate of 5-10 DEG C/min in a hydrogen atmosphere,
And keep 2-8h.
9. the monatomic Pd Catalysts for Electrocatalytic Oxidation ethyl alcohol of support type that the method according to claim 4-8 is prepared
Using.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110164699A (en) * | 2019-05-16 | 2019-08-23 | 北京化工大学 | A kind of Fe2O3 doping nickel oxide being pyrolyzed using hydrotalcite as presoma and its application in photocatalytic fuel cell |
| CN110247061A (en) * | 2019-06-05 | 2019-09-17 | 北京氦舶科技有限责任公司 | Carbon carries the monatomic elctro-catalyst of bimetallic and its preparation and application |
| CN110270348A (en) * | 2019-07-15 | 2019-09-24 | 郑州轻工业学院 | A kind of monatomic catalyst of noble metal and its preparation and application |
| CN110449176A (en) * | 2019-08-16 | 2019-11-15 | 江南大学 | A kind of preparation method and application of the monatomic catalyst of base metal |
| CN111063902A (en) * | 2019-12-03 | 2020-04-24 | 上海理工大学 | Preparation method of nano metal intercalated hydrotalcite material electrode catalyst |
| CN111054333A (en) * | 2020-02-14 | 2020-04-24 | 郑州轻工业大学 | Hydrotalcite-supported palladium catalyst for preparing styrene by selective hydrogenation of phenylacetylene, and preparation method and application thereof |
| CN111871426A (en) * | 2020-06-11 | 2020-11-03 | 安徽师范大学 | Pd nanoparticle-loaded nickel-iron double hydroxide nanosheet array structure material, preparation method and application thereof |
| CN112138652A (en) * | 2020-10-14 | 2020-12-29 | 绍兴文理学院 | Preparation method of monoatomic palladium catalyst and application of monoatomic palladium catalyst in carbon-carbon coupling |
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| CN110164699A (en) * | 2019-05-16 | 2019-08-23 | 北京化工大学 | A kind of Fe2O3 doping nickel oxide being pyrolyzed using hydrotalcite as presoma and its application in photocatalytic fuel cell |
| CN110247061A (en) * | 2019-06-05 | 2019-09-17 | 北京氦舶科技有限责任公司 | Carbon carries the monatomic elctro-catalyst of bimetallic and its preparation and application |
| CN110270348A (en) * | 2019-07-15 | 2019-09-24 | 郑州轻工业学院 | A kind of monatomic catalyst of noble metal and its preparation and application |
| CN110449176A (en) * | 2019-08-16 | 2019-11-15 | 江南大学 | A kind of preparation method and application of the monatomic catalyst of base metal |
| WO2021031967A1 (en) * | 2019-08-16 | 2021-02-25 | 江南大学 | Preparation method and application for non-precious metal monoatomic catalyst |
| CN111063902A (en) * | 2019-12-03 | 2020-04-24 | 上海理工大学 | Preparation method of nano metal intercalated hydrotalcite material electrode catalyst |
| CN111054333A (en) * | 2020-02-14 | 2020-04-24 | 郑州轻工业大学 | Hydrotalcite-supported palladium catalyst for preparing styrene by selective hydrogenation of phenylacetylene, and preparation method and application thereof |
| CN111054333B (en) * | 2020-02-14 | 2022-11-01 | 郑州轻工业大学 | Hydrotalcite supported palladium catalyst for preparing styrene by selective hydrogenation of phenylacetylene, and preparation method and application thereof |
| CN111871426A (en) * | 2020-06-11 | 2020-11-03 | 安徽师范大学 | Pd nanoparticle-loaded nickel-iron double hydroxide nanosheet array structure material, preparation method and application thereof |
| CN111871426B (en) * | 2020-06-11 | 2023-08-29 | 安徽师范大学 | Pd nanoparticle-supported nickel-iron double hydroxide nanosheet array structure material, preparation method and application thereof |
| CN112138652A (en) * | 2020-10-14 | 2020-12-29 | 绍兴文理学院 | Preparation method of monoatomic palladium catalyst and application of monoatomic palladium catalyst in carbon-carbon coupling |
| CN112138652B (en) * | 2020-10-14 | 2022-07-15 | 绍兴文理学院 | Preparation method of monoatomic palladium catalyst and application of monoatomic palladium catalyst in carbon-carbon coupling |
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Application publication date: 20181109 |