CN110152678A - A kind of electro-catalysis reduction CO2For the nanometer Cu-Yb alloy catalyst of the energy - Google Patents
A kind of electro-catalysis reduction CO2For the nanometer Cu-Yb alloy catalyst of the energy Download PDFInfo
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- CN110152678A CN110152678A CN201910484291.9A CN201910484291A CN110152678A CN 110152678 A CN110152678 A CN 110152678A CN 201910484291 A CN201910484291 A CN 201910484291A CN 110152678 A CN110152678 A CN 110152678A
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- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
- C07C1/12—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon dioxide with hydrogen
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- C07C2523/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
- C07C2523/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36 with rare earths or actinides
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Abstract
The present invention provides one kind, and there is electro-catalysis to restore CO2For the preparation method of the nanometer Cu-Yb alloy catalyst of the energy, CO can will be restored2For valuable gas-phase product (such as CO, CH4、C2H4) and liquid product.The electro-catalysis for improving Cu based alloy catalyst restores CO2Performance is improved to CH4Reduction select performance.The present invention forms Copper rare earth alloy material by screening variety classes and the rare earth metal of dosage, final to determine that Rare Earth Y b and Cu carries out alloying；The characteristics of to be quenched fast nucleation synthesis, using simple chemical liquid phase reduction method, prepare the Cu-Yb nano metal elctro-catalyst that Cu nanocatalyst and alloy are evenly distributed；It probes into Cu-Yb alloy elctro-catalyst pattern and component and CO is restored to electro-catalysis2The influence of performance provides certain reference for the rational design of elctro-catalyst.The process is easy to operate, securely and reliably, low in cost, has good popularization and application foreground.
Description
Technical field
The present invention relates to a kind of preparation methods of Cu-Yb Nanoalloy material, and gained Cu-Yb Nanoalloy material is answered
CO is restored for catalytic field more particularly to electro-catalysis2Field.
Background technique
CO2As a kind of greenhouse gases, ours is affected slowly and significant on the influence of weather bring
Production and life.And our eager targets are exactly to reduce greenhouse gas emission, reduce harm of the human activity to weather system,
Therefore mitigation of climate change has researcher to propose to mitigate global CO using a variety of methods simultaneously2Maximum discharge bring is negative
It influences, CO in such as atmosphere2Capture seal up for safekeeping, the capacity usage ratio that improves vehicle and building, using alternative energy source etc..Wherein,
By CO2Being converted into high valuable chemicals or fuel not only by catalysis reaction may be implemented CO in atmosphere2The reduction of content,
And it is capable of providing the energy of clean and environmental protection, environment is not only improved, but also provide the energy.Titanium dioxide is restored using electrochemical method
Carbon makes it be converted into the clean energy resourcies such as CO, formic acid, methane, methanol, not only can solve CO2Superfluous problem, also can solve
The problem of thermoelectricity excess capacity.And reaction condition is mild, does not need high temperature and pressure, and equipment operation is flexible, energy utilization efficiency
Height, and selectivity of product and reaction speed can be regulated and controled by simply changing electrolytic condition, therefore be considered as CO2Resource
Most promising a kind of transformation technology in change.But the realization of this approach is dependent on high performance cathodes electrocatalysis material
Exploitation.
In numerous catalysis materials, under same reaction condition, the electroreduction CO of different metal2Product distributional difference is very big,
Since reaction intermediate CO* allows CO* to carry out a variety of reaction paths in the difference of its adsorption ability, and then generate
CH4、CH3OH、C2H4、C2H5The products such as OH.And Cu is unique a kind of effectively to adsorb intermediate CO and further restore it
For the metal of hydrocarbon.But unfortunately, there are still many urgent problems to be solved for Cu base elctro-catalyst at present, such as: (1)
High overpotential leads to the low (CH of energy efficiency4Overpotential about 0.9 V, C2H4About 0.7 V of overpotential)；(2) electron transmission dynamics is slow
Slowly；(3) poor to the selectivity of specific product, up to 16 kinds of reduzate；(4) bias current density is too low；(5) catalyst is steady
Qualitative difference, general 1-5 hours interior i.e. inactivation.The above problem seriously limits the commercial applications of Cu base catalysis material.It is based on
This, researcher from size, pattern, component, surface ligand, etc. structures etc. Cu base elctro-catalyst is optimized, to improve
It is catalyzed performance.Through research discovery compared with single-metal reforming catalyst, alloy catalyst flexible design, many kinds of, structure is more
Sample often shows superior catalytic performance than forming its monometallic, is quite favored by researcher in energy catalytic field.?
CO2In electrocatalytic reduction, alloying process is existed by changing structure and the component of catalyst to regulate and control reaction intermediate
Combination energy on catalyst surface breaks existing linear relationship between intermediate product, to reach reduction reaction overpotential, mentions
The purpose of high specific product selectivity.
In conjunction with the above status, the present invention is high for Cu base catalyst reaction overpotential, selectivity of product is low, catalytic stability
The deficiencies of poor, it is intended to by optimizing the structure and composition of Cu base catalyst, improve its electro-catalysis reduction CO2Performance.
Summary of the invention
It is an object of the invention to prepare Cu and Cu-Yb alloy elctro-catalyst using simple chemical liquid phase reduction method, lead to
A variety of structural characterizations and catalytic performance test are crossed, Cu-Yb alloy elctro-catalyst component is probed into and CO is restored to electro-catalysis2The shadow of performance
It rings, provides certain reference for the rational design of elctro-catalyst, push electrochemical reduction CO2Process of industrialization.The present invention
Specific technical solution is as follows:
A kind of nanometer Cu-Yb alloy catalyst for being CH4 with electro-catalysis reduction CO2, preparation method includes the following steps:
(1) inert gas is continually fed into the reaction vessel A containing solvent, the solvent is the compound containing alcoholic extract hydroxyl group；
(2) magnetic stirring apparatus is opened, and heating makes reaction temperature control at 200~400 DEG C；
(3) solvent as described above is added in reaction vessel B, metal salt and PVP (K30) are dissolved in the solvent,
The metal salt is one or more of mixing of copper nitrate, copper acetate, ytterbium nitrate or acetic acid ytterbium；
(4) under agitation, the substance in reaction vessel B is injected into container A, reaction temperature is controlled 200~400
DEG C, the reaction time is 5~20 min；
(5) it is centrifuged after being quickly cooled down the material in the reaction vessel A, the solid deionization that will be obtained by filtration
After water and dehydrated alcohol are respectively washed several times, carry out obtaining the Cu-Yb alloy catalyst of the nanometer after normal-temperature vacuum is dry.
Further, the solvent as described in step (1) containing alcoholic extract hydroxyl group is one of diethylene glycol (DEG) or triethylene glycol.
The dosage for selecting excellent, described solvent is 10~30 mL.
Preferably, it is respectively 230,250,280,300 DEG C that maximum temperature point is heated to described in step (2).
Preferably, the investment ratio of metal salt described in step (3) is different, the ratio of mantoquita and ytterbium salt be respectively 1:1,
4:1 or 9:1.
Preferably, the molar concentration of PVP (K30) described in step (3) is respectively 0.5,1 or 1.5 mol/L.
Preferably, the reaction time described in step (4) is respectively 5,10,15 or 20 min.
Present invention feature the most prominent and significant beneficial effect are:
One, easy to operate, the source Cu and Yb is not need pretreated, and raw material carbon black-supported is not necessary to handle by strong acid and strong base, and
And raw material dosage is few；
Two, Cu and Yb is uniformly distributed in gained Cu-Yb alloy particle, is not reunited between alloy particle, has good object
Physicochemical performance and stability；
Three, experiment finds that the Cu-Yb alloy of certain Yb content has the catalytic performance for differing markedly from pure Cu, shows significant
Alloy effect.The addition of Yb can effectively be promoted to CH in Cu9Yb1, Cu4Yb1 and Cu1Yb14Selectivity of product, press down simultaneously
The generation of ethylene processed, Cu4Bi1 show the most obvious, CH4Highest faradic efficiency, up to 40%, is Cu NP in -1.0V
2.2 again.
Four, by various structures characterization and catalytic performance test, the component for probing into copper-based elctro-catalyst restores electro-catalysis
CO2The influence of performance provides certain reference for the rational design of elctro-catalyst, pushes electrochemical reduction CO2Industrialization into
Journey.
Detailed description of the invention
The TEM picture of Fig. 1 Cu-Yb alloy: a) Cu, b) Cu9Yb1；C) Cu4Yb1；D) Cu1Yb1；
Fig. 2 Cu-Yb alloy TEM and EDS distribution diagram of element；
The gas-phase product faradic efficiency figure of Fig. 3 Cu-Yb alloy series catalyst: a) CO；b) CH4；c) C2H4；d) H2；
The CH of the catalyst of Fig. 4 Cu-Yb alloy4Product faradic efficiency figure.
Specific embodiment
Specific embodiment 1: a kind of preparation method of Cu-Yb Nanoalloy elctro-catalyst, it is characterised in that it be by with
What lower step was completed:
One, it is added 20 mL triethylene glycols as solvent in three-necked flask, gas-guide tube and spherical condensation tube is connected, from gas-guide tube
It is passed through N2/ Ar mixed gas, 20 min of Continuous aeration remove dissolved oxygen, guarantee that subsequent reactions carry out under an inert atmosphere；
Two, 280 DEG C are heated to the rate of 5 DEG C/min, appropriate rate magnetic agitation.
Three, metal salt and PVP (K30) dissolution are obtained into the Cu (Ac) of 0.4 mol/L using 1 mL triethylene glycol as solvent2With
0.1 mol/L Y(NO3)3With the PVP (K30) of 0.5 mol/L；
Four, the metal of above-mentioned dissolution is saline land injected in above-mentioned hot solution, keeps 15 min of reaction.
Five, flask is withdrawn into heating source, be quickly cooled down, centrifuge separation is respectively washed using deionized water and dehydrated alcohol
2-3 is after, the dry 12h of normal-temperature vacuum.
The present invention has studied a kind of with electro-catalysis reduction CO2The preparation method of the nanometer Cu-Yb alloy catalyst of performance,
By changing the feed ratio of Nanoalloy, reaction temperature and reaction time, the electro-catalysis of Cu based alloy catalyst can be improved also
Former CO2Performance increases the distribution of gas-phase product.Cu-Yb bianry alloy is used as elctro-catalyst for the first time by the present invention.Experiment discovery
There is the catalytic performance for differing markedly from pure Cu in the Cu-Yb alloy of certain Yb content, show significant alloy effect.
The addition of Yb can effectively be promoted to CH in Cu9Yb1, Cu4Yb1 and Cu1Yb14Selectivity of product, while the life of ethene suppressing
At Cu4Yb1 shows the most obvious, CH4Highest faradic efficiency is in -1.8V up to 41%.
Specific embodiment 2: the difference of present embodiment and specific embodiment one is: addition described in step 1
Solvent be 20 mL diethylene glycol (DEG)s；Other are same as the specific embodiment one.
Specific embodiment 3: the difference of present embodiment and specific embodiment one is: addition described in step 1
The volume of triethylene glycol solvent is 10 mL；Other are same as the specific embodiment one.
Specific embodiment 4: the difference of present embodiment and specific embodiment one is: addition described in step 1
The volume of triethylene glycol solvent is 30 mL；Other are same as the specific embodiment one.
Specific embodiment 5: the difference of present embodiment and specific embodiment one is: not held described in step 1
It is continuous to be passed through N2/ Ar mixed gas achievees the purpose that remove dissolved oxygen；Other are same as the specific embodiment one.
Specific embodiment 6: the difference of present embodiment and specific embodiment one is: heating described in step 2
To maximum temperature difference, kept for 230 DEG C of maximum temperature；Other are same as the specific embodiment one.
Specific embodiment 7: the difference of present embodiment and specific embodiment one is: heating described in step 2
To maximum temperature difference, kept for 250 DEG C of maximum temperature；Other are same as the specific embodiment one.
Specific embodiment 8: the difference of present embodiment and specific embodiment one is: heating described in step 2
To maximum temperature difference, kept for 300 DEG C of maximum temperature；Other are same as the specific embodiment one.
Specific embodiment 9: the difference of present embodiment and specific embodiment one is: selection described in step 3
Metal be Cu ((NO3)2With Y ((NO3)3Other are same as the specific embodiment one.
Specific embodiment 10: the difference of present embodiment and specific embodiment one is: selection described in step 3
Metal be Cu (Ac)2With Y (Ac)3Other are same as the specific embodiment one.
Specific embodiment 11: the difference of present embodiment and specific embodiment one is: choosing described in step 3
The metal taken is Cu (Ac)2With Y ((NO3)3Other are same as the specific embodiment one.
Specific embodiment 12: the difference of present embodiment and specific embodiment one is: gold described in step 3
Belong to salt (Cu (Ac)2With Y (NO3)3) molar concentration difference, the Cu (Ac) of 0.4 mol/L2；Other and one phase of specific embodiment
Together.
Specific embodiment 13: the difference of present embodiment and specific embodiment one is: gold described in step 3
Belong to salt (Cu (Ac)2With Y (NO3)3) molar concentration difference, the Cu (Ac) of 0.25 mol/L2With 0.25 mol/L Y (NO3)3；Other
It is same as the specific embodiment one.
Specific embodiment 14: the difference of present embodiment and specific embodiment one is: gold described in step 3
Belong to salt (Cu (Ac)2With Y (NO3)3) molar concentration difference, the Cu (Ac) of 0.45 mol/L2With the Y (NO of 0.05 mol/L3)3；Its
He is same as the specific embodiment one.
Specific embodiment 15: the difference of present embodiment and specific embodiment one is: PVP described in step 3
(K30) input amount is different, and additional amount is 1 mol/L；Other are same as the specific embodiment one.
Specific embodiment 16: the difference of present embodiment and specific embodiment one is: PVP described in step 3
(K30) input amount is different, and additional amount is 1.5 mol/L；Other are same as the specific embodiment one.
Specific embodiment 17: the difference of present embodiment and specific embodiment one is: guarantor described in step 4
Reaction time difference is held, the reaction time is 5 min；Other are same as the specific embodiment one.
Specific embodiment 18: the difference of present embodiment and specific embodiment one is: guarantor described in step 4
Reaction time difference is held, the reaction time is 10 min；Other are same as the specific embodiment one.
Specific embodiment 19: the difference of present embodiment and specific embodiment one is: guarantor described in step 4
Reaction time difference is held, the reaction time is 20 min；Other are same as the specific embodiment one.
Claims (7)
1. there is one kind electro-catalysis to restore CO2For CH4Nanometer Cu-Yb alloy catalyst, which is characterized in that preparation method packet
Include following steps:
(1) inert gas is continually fed into the reaction vessel A containing solvent, the solvent is the compound containing alcoholic extract hydroxyl group；
(2) magnetic stirring apparatus is opened, and heating makes reaction temperature control at 200~400 DEG C；
(3) solvent as described above is added in reaction vessel B, metal salt and PVP (K30) are dissolved in the solvent,
The metal salt is one or more of mixing of copper nitrate, copper acetate, ytterbium nitrate or acetic acid ytterbium；
(4) under agitation, the substance in reaction vessel B is injected into container A, reaction temperature is controlled 200~400
DEG C, the reaction time is 5~20 min；
(5) it is centrifuged after being quickly cooled down the material in the reaction vessel A, the solid deionization that will be obtained by filtration
After water and dehydrated alcohol are respectively washed several times, carry out obtaining the Cu-Yb alloy catalyst of the nanometer after normal-temperature vacuum is dry.
2. the preparation method of a kind of nanometer of Cu-Yb alloy catalyst according to claim 1, it is characterised in that step (1)
Described in the solvent containing alcoholic extract hydroxyl group be one of diethylene glycol (DEG) or triethylene glycol.
3. the preparation method of a kind of nanometer of Cu-Yb alloy catalyst according to claim 1, it is characterised in that step (1)
Described in solvent dosage be 10~30 mL.
4. the preparation method of a kind of nanometer of Cu-Yb alloy catalyst according to claim 1, it is characterised in that step (2)
Described in the maximum temperature point that is heated to be respectively 230,250,280,300 DEG C.
5. the preparation method of a kind of nanometer of Cu-Yb alloy catalyst according to claim 1, it is characterised in that step (3)
Described in metal salt investment ratio it is different, the ratio of mantoquita and ytterbium salt is respectively 1:1,4:1 or 9:1.
6. the preparation method for a kind of nanometer of Cu-Yb alloy catalyst stated according to claim 1, it is characterised in that in step (3)
The molar concentration of the PVP (K30) is respectively 0.5,1 or 1.5 mol/L.
7. the preparation method of a kind of nanometer of Cu-Yb alloy catalyst according to claim 1, it is characterised in that step (4)
Described in reaction time be respectively 5,10,15 or 20 min.
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Cited By (4)
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| CN110560075A (en) * | 2019-09-25 | 2019-12-13 | 哈尔滨工业大学 | Nano Cu-Eu alloy catalyst with core-shell structure and preparation method and application thereof |
| CN110560076A (en) * | 2019-09-25 | 2019-12-13 | 哈尔滨工业大学 | Preparation method and application of nano Cu-Bi alloy catalyst |
| CN111229253A (en) * | 2020-03-14 | 2020-06-05 | 北京工业大学 | Electro-catalytic reduction of CO2Preparation method of nano Cu-Au alloy catalyst as energy source |
| CN112517020A (en) * | 2020-12-17 | 2021-03-19 | 哈尔滨工业大学 | Preparation method and application of nano Cu-Ce alloy catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110560075A (en) * | 2019-09-25 | 2019-12-13 | 哈尔滨工业大学 | Nano Cu-Eu alloy catalyst with core-shell structure and preparation method and application thereof |
| CN110560076A (en) * | 2019-09-25 | 2019-12-13 | 哈尔滨工业大学 | Preparation method and application of nano Cu-Bi alloy catalyst |
| CN110560076B (en) * | 2019-09-25 | 2022-03-25 | 哈尔滨工业大学 | Preparation method and application of nano Cu-Bi alloy catalyst |
| CN110560075B (en) * | 2019-09-25 | 2022-03-25 | 哈尔滨工业大学 | Nano Cu-Eu alloy catalyst with core-shell structure and preparation method and application thereof |
| CN111229253A (en) * | 2020-03-14 | 2020-06-05 | 北京工业大学 | Electro-catalytic reduction of CO2Preparation method of nano Cu-Au alloy catalyst as energy source |
| CN112517020A (en) * | 2020-12-17 | 2021-03-19 | 哈尔滨工业大学 | Preparation method and application of nano Cu-Ce alloy catalyst |
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