CN109908904A - A kind of monatomic catalyst of transition metal and its preparation method and application - Google Patents
A kind of monatomic catalyst of transition metal and its preparation method and application Download PDFInfo
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- CN109908904A CN109908904A CN201910288682.3A CN201910288682A CN109908904A CN 109908904 A CN109908904 A CN 109908904A CN 201910288682 A CN201910288682 A CN 201910288682A CN 109908904 A CN109908904 A CN 109908904A
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Abstract
The present invention provides a kind of monatomic catalyst of transition metal, and the catalyst is monatomic for active component with transition metal, and using carbon black as carrier, the monoatomic load capacity of transition metal is 0.5-6wt%, and highest load capacity is 2~3 times of the prior art.For the monatomic catalyst preparation of transition metal provided by the invention using the Phen with strong coordination effect as ligand, the carbon black with high conductivity and high surface as carrier, induction confinement forms a variety of monatomic catalyst of cheap transition metal with polymolecularity and high load type.And the preparation method has universality, can be used for preparing the monatomic catalyst of a variety of transition metal, realizes the preparation of the monatomic catalyst of Cr, Nb, Rh, Cd, Os and Ir for the first time by this method.In addition, the preparation method is low in cost, simple process, can be mass produced.Secondly, the catalyst electro-catalysis preparing carbon monoxide from carbon dioxide application in, selectivity with higher and faradic efficiency.
Description
Technical field
The present invention relates to technical field of micro nano material preparation.More particularly, to a kind of transition metal list of universality
Catalyst atom and its preparation method and application.
Background technique
Homogeneous catalyst and heterogeneous catalysis have been widely used in chemical industry as two class catalyst, he
Have its respective feature and advantage respectively.The active site of homogeneous catalyst is uniform, atom utilization is high, active site holds
The advantages of easily adjusting, but its stability is poor and is difficult to separate with reactant.And heterogeneous catalysis stability is high, be easy to instead
Object is answered to separate, but its atom utilization is low, only the atom on surface can contact participation catalysis reaction with reactant.How
It is enough the hot spot and problem of catalyticing research in conjunction with the advantage of two class catalyst.Monatomic catalyst is because it has nearly 100%
Atom utilization, active site facilitate adjusting, be easy be considered as with the advantages such as reactants separate link up homogeneous catalyst and
The bridge of heterogeneous catalysis.
However, the surface energy high due to single atom, easily reunites, causes monatomic catalyst to be difficult to synthesize, synthesis side
Method limits it and is widely applied.The method for synthesizing monatomic catalyst at present mainly include atomic layer deposition, photoreduction,
The methods of metal ion and presoma dipping calcining.The method of atomic layer deposition is with high costs, and the device is complicated, it is difficult to answer extensively
With；The method narrow application range of photoreduction, low output equally limit its application.What metal ion and carrier impregnation were calcined
For method because its use scope is wide, synthetic method is relatively easy and is favored by people.However, metal ion and carrier impregnation are calcined
Method still have synthetic method complexity, can not large scale preparation the problems such as.And with MOFs or C3N4It is needed Deng for carrier
Very high temperature lower calcination could be carbonized, and the warm-up movement aggravation of atom causes metal to be easy to reunite so that Metal Supported at high temperature
Amount can not improve.And current some monatomic process for synthetic catalyst do not have extensive universality, can not use a kind of side
Method synthesizes a variety of monatomic catalyst, therefore can not effect of the Correlation Centre metallic atom played in catalytic activity.
Accordingly, it is desirable to provide a kind of monatomic catalyst of transition metal and preparation method thereof and electro-catalysis carbon dioxide also
One of original prepares the application in carbon monoxide, at least solve the above problems.
Summary of the invention
It is an object of the present invention to provide a kind of monatomic catalyst of transition metal, which is to carry with carbon black
Body has the high monatomic load capacity of transition metal.
It is another object of the present invention to provide the monatomic method for preparing catalyst of above-mentioned transition metal, the preparation methods
With the monatomic catalyst preparation of a variety of transition metal is suitable for, and preparation temperature is low, and active component transition metal is monatomic negative
The big advantage of carrying capacity.
Third object of the present invention be to provide the monatomic catalyst of above-mentioned transition metal electro-catalysis carbon dioxide also
Original prepares the application in carbon monoxide, catalyst selectivity with higher and faradic efficiency.
In order to achieve the above objectives, the present invention adopts the following technical solutions:
The first aspect present invention provides a kind of monatomic catalyst of transition metal, which is so that transition metal is monatomic
Active component, using carbon black as carrier, transition metal single atomic dispersion is in the surface and inside of carbon black；Wherein, with the transition metal
The total weight of monatomic catalyst is 100% meter, and the monoatomic load capacity of transition metal is 0.5-6.0wt%.
Preferably, the transition metal atoms be selected from Cr, Mn, Co, Cu, Zn, Nb, Mo, Ru, Rh, Pd, Ag, Cd, Os, Ir,
Pt。
Preferably, the carbon black is selected from Ketjenblack EC-300J type carbon black or Vulcan XC-72 type carbon black.
In the monatomic catalyst of transition metal provided by the invention, chain of the transition metal single atomic dispersion in carbon black particle
In shape or botryoidal structure.The high specific surface area and high electric conductivity that carbon black has, can make transition metal atoms abundant
Dispersion, and increase the load capacity of transition metal atoms in carbon black structure.
The specific surface area of Ketjenblack EC-300J type carbon black provided by the invention is greater than 800m2·g-1, the ratio of superelevation
Surface area is conducive to improve transition metal load capacity；The specific surface area of Vulcan XC-72 type carbon black is greater than 200m2·g-1, have
The feature that surface is pure, price is relatively low advantageously reduces surface contamination and reduces cost.
The second aspect of the present invention provides the preparation method of the monatomic catalyst of above-mentioned transition metal, including following step
It is rapid:
Transition metal salt and organic ligand are dissolved in organic solvent, is uniformly mixed, obtains clear transparent solutions；Carbon black is added,
It is uniformly mixed, obtains reaction solution；2~8h of impregnation at 40-80 DEG C, it is dry, obtain crude product；Crude product is placed in argon atmosphere
In, and with 2~10 DEG C of min-1Heating rate is warming up to 300~580 DEG C, calcines 1-5h；Room temperature is down to get the transition gold
Belong to monatomic catalyst.
Specific embodiment according to the present invention after transition metal salt and organic ligand are dissolved in organic solvent, can pass through
The modes such as stirring, ultrasound promote the dissolution and dispersion of transition metal salt and organic ligand in organic solvent, obtain clear
Solution, promote the progress of complex reaction.The mixed dipping process of carbon black is added can then carry out in a water bath, promote carbon black
With coming into full contact with for solution, increase the load capacity of transition metal atoms in carbon black.Calcined temperature-fall period can take nature
Cool to room temperature.
Prepared in the monatomic catalyst process of transition metal in traditional metal ion and carrier impregnation calcining, with MOFs or
C3N4It needs to calcine at very high temperatures and could be carbonized Deng for carrier, the warm-up movement aggravation of atom causes metal to hold at high temperature
It is easy to reunite so that content of metal can not improve.
And in preparation method provided by the invention, the carrier provided is carbon black, and carbon black particle has microstructure and height
Specific surface area, need not move through high temperature cabonization process, so that it may have high electric conductivity, can be to avoid metal caused by high temperature
Agglomeration traits are conducive to abundant diffusion of the transition metal atoms in carbon black, and then increase transition metal atoms in carbon black
Load capacity.
Preferably, in the reaction solution transition metal salt, organic ligand the mass ratio of the material value are as follows: 1:3~1:20.
Preferably, the molar concentration of transition metal salt is 0-0.2molL in reaction solution-1, mole of the organic ligand
Concentration is 0-4molL-1；Wherein, the molar concentration of transition metal salt and organic ligand is not 0 in reaction solution.
Preferably, the mass concentration of carbon black is 10-70mgmL in the reaction solution-1。
Preferably, the organic ligand is selected from Phen, 2,2- bipyridyl, melamine or phenylalanine；Adjacent Féraud
Quinoline has strong coordination effect, can be complexed with transition metal, generate stable complex compound.
The organic solvent that the present invention selects can be the organic solvent of any dissolvable transition metal salt and organic ligand, packet
Include but be not limited to ethyl alcohol or dimethyl sulfoxide.
Transition metal salt of the present invention can be any transition metal salt being dispersed in organic solvent, including but
It is not limited to one of transition metal villaumite, transition metal nitrate, transition metal acetate, transition metal sulfate or more
Kind.
Preferably, in preparation process, the drying temperature of crude product is 60~190 DEG C, and drying time is 6~20h.
Third aspect of the present invention provides the above-mentioned monatomic catalyst of transition metal and prepares in electro-catalysis carbon dioxide reduction
Application in carbon monoxide.
Catalyst provided by the invention shows outstanding property in electro-catalysis preparing carbon monoxide from carbon dioxide
Can, it is able to maintain 90% or more carbon monoxide selective in -0.7~-1.5V voltage range, optimality is reached in -1.2V
Can, carbon monoxide selective is up to 98.9%.
Beneficial effects of the present invention are as follows:
The monatomic catalyst of transition metal provided by the invention, it is monatomic for active component with transition metal, be with carbon black
Carrier, the monoatomic load capacity of transition metal are 0.5-6wt%, and highest load capacity is 2~3 times of the prior art.The present invention mentions
The monatomic catalyst preparation of the transition metal of confession using the Phen with strong coordination effect as ligand, have high conductivity and
The carbon black of high surface is carrier, and induction confinement forms a variety of former with polymolecularity and the cheap transition metal list of high load type
Muonic catalysis agent.And the preparation method has universality, can be used for preparing the monatomic catalyst of a variety of transition metal, passes through this method
It is mono- former that the monatomic catalyst of Cr, the monatomic catalyst of Nb, the monatomic catalyst of Rh, the monatomic catalyst of Cd, Os are realized for the first time
Muonic catalysis agent and the preparation of the monatomic catalyst of Ir.In addition, the preparation method is low in cost, simple process, can give birth on a large scale
It produces.Secondly, the catalyst electro-catalysis preparing carbon monoxide from carbon dioxide application in, selectivity and method with higher
Draw efficiency.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 shows powder diffraction (XRD) spectrogram of the 1 monatomic catalyst of Ni obtained of the embodiment of the present invention.
Fig. 2 shows transmission electron microscope (TEM) figures of the 1 monatomic catalyst of Ni obtained of the embodiment of the present invention.
Fig. 3 shows the spherical aberration correction transmission electron microscope (HAADF- of the 1 monatomic catalyst of Ni obtained of the embodiment of the present invention
STEM) figure.
Fig. 4 shows the electro-catalysis carbon dioxide reduction performance map of the 1 monatomic catalyst of Ni obtained of the embodiment of the present invention.
Fig. 5 shows the XRD diagram of the monatomic catalyst of 2-4 of embodiment of the present invention Ni obtained.
Fig. 6 shows the XRD diagram of the 5 monatomic catalyst of Ni obtained of the embodiment of the present invention.
Fig. 7 shows the HAADF-STEM figure of the 8 monatomic catalyst of Ag obtained of the embodiment of the present invention.
Fig. 8 show 9-23 of embodiment of the present invention Cr, Mn obtained, Co, Cu, Zn, Nb, Mo, Ru, Rh, Pd, Cd, Os,
The HAADF-STEM of the monatomic catalyst of Ir, Pt schemes.
Fig. 9 shows the XRD diagram of the monatomic catalyst obtained of the embodiment of the present invention 24,25,26,27.
Figure 10 shows embodiment 6, the XRD diagram of the 7 monatomic catalyst of Ni obtained.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.It will be appreciated by those skilled in the art that specifically described content is illustrative and be not restrictive below, it should not be with this
It limits the scope of the invention.
In the present invention, preparation method is then conventional method unless otherwise specified.Raw material used is equal unless otherwise instructed
It can be obtained from disclosed commercial sources, the percentage is mass percent unless otherwise specified.
Embodiment 1
A kind of monatomic method for preparing catalyst of nickel, includes the following steps:
1) weigh 0.2mmol nickel acetate, 0.6mmol Phen be added test tube in, be added 2mL ethyl alcohol, magnetic agitation is extremely
It is completely dissolved to obtain the solution of clear；
2) it is mixed to after the reaction was completed, weigh in the 69.6mg carbon black addition above-mentioned solution of Ketjenblack EC-300J type
Uniformly, the heating water bath 4h in 60 DEG C of water-baths, then 80 DEG C of dry 12h obtain crude product in an oven；
3) crude product obtained above is in argon atmosphere with 10 DEG C of min-1Heating rate is warming up to 580 DEG C, in the temperature
Degree is lower to keep 2h, after Temperature fall to room temperature, obtain the monatomic catalyst of Ni, be denoted as Ni-SAC, by the side ICP-AES
Method can detecte in the Ni-SAC, and the load capacity of Ni atom is 6.0wt%.
Curve is the XRD diagram of Ni-SAC catalyst prepared by embodiment 1 in Fig. 1.
Fig. 2 is the TEM figure of Ni-SAC catalyst prepared by embodiment 1.
Fig. 3 is the HAADF-STEM figure of Ni-SAC catalyst prepared by embodiment 1.
Fig. 4 is Ni-SAC catalyst electro-catalysis carbon dioxide reduction performance map prepared by embodiment 1.
As shown in Figure 1, only there is the peak of carbon in the Ni-SAC catalyst XRD spectra of synthesis, it is high for illustrating Ni wherein
Degree dispersion.As shown in Figure 2, carbon black is only observed in the Ni-SAC catalyst TEM figure of synthesis, it is high for equally illustrating Ni wherein
Degree dispersion, exist without Ni simple substance or its compound nano-particle.From the figure 3, it may be seen that the Ni-SAC catalyst of synthesis
It can be seen that Ni is in single atomic dispersion in synthesized catalyst in HAADF-STEM figure.As shown in Figure 4, the Ni-SAC of synthesis
Catalyst shows outstanding performance in electro-catalysis carbon dioxide reduction, is able to maintain in -0.7~-1.5V voltage range
90% or more carbon monoxide selective, reaches optimum performance in -1.2V, and carbon monoxide selective is up to 98.9%.
Embodiment 2-4
Embodiment 1 is repeated, difference, which is only that, is changed to nickel chloride, nickel nitrate, nickel sulfate for nickel acetate.Obtained Ni is mono- former
The monatomic catalyst that muonic catalysis agent and embodiment 1 obtain has no significant difference, and by ICP-AES method, can detecte
In the Ni-SAC, the load capacity of Ni atom is 6wt%.
Fig. 5 is the XRD diagram of the monatomic catalyst of Ni synthesized by embodiment 2-4, as can be seen from Figure, using chlorination
Nickel, nickel nitrate, only there is the peak of carbon black in the monatomic catalyst of Ni synthesized by nickel sulfate, Ni or its compound does not occur
Peak.This also illustrates that anion species have not significant impact to monatomic catalyst is formed in transition metal salt.
Embodiment 5
Embodiment 1 is repeated, difference, which is only that, is changed to Vulcan XC-72 type for Ketjenblack EC-300J type carbon black
Carbon black, obtained catalyst are monatomic catalyst, and by ICP-AES method, be can detecte in the Ni-SAC, Ni atom
Load capacity be 4.5wt%.
Fig. 6 show the monatomic XRD diagram of Ni synthesized in embodiment 1 and embodiment 5.In figure, using two kinds of model charcoals
The black monatomic peak for there was only carbon black synthesized Ni occurs, and the peak of metal simple-substance or compound does not occur.This illustrates carbon black
Type has not significant impact to monatomic catalyst is formed.
Embodiment 6-7
Embodiment 1 is repeated, difference, which is only that, is changed to 2mmol and 4mmol for Phen additional amount, obtained catalyst
It is denoted as NiN10 and NiN20, two kinds of synthesized catalyst are monatomic catalyst.
Figure 10 shows the XRD diagram of monatomic catalyst synthesized in embodiment 6.Only occurs the width of two corresponding carbon in figure
Peak occurs without the peak of metal or its compound, and two kinds of synthesized catalyst of this explanation are monatomic catalyst.
Embodiment 8
Embodiment 1 is repeated, difference, which is only that, is changed to Ag salt for W metal salt, and the monatomic catalyst of Ag can be obtained.Fig. 7 is
The spherical aberration correction transmission electron microscope picture of the monatomic catalyst of synthesized Ag is clear that Ag atom with monoatomic in figure
Form is dispersed in carbon substrate, and by ICP-AES method, can detecte in the Ni-SAC, the load capacity of Ag atom is
3.0wt%.
Embodiment 9-23
Repeat embodiment 1, difference be only that by metal salt be changed to Cr, Mn, Co, Cu, Zn, Nb, Mo, Ru, Rh, Pd, Cd,
Os, Ir, Pt salt.Obtained catalyst is monatomic catalyst.Specifically, the spherical aberration of this 14 kinds of monatomic catalyst of metal
Transmission electron microscope picture is corrected as shown in figure 8, white bright spot is that metal is monatomic it can be found that being all with monatomic shape in transition metal
Formula is dispersed in the surface and inside of carbon black.Embodiment 9-23 also illustrates that the monatomic process for synthetic catalyst of the transition metal has
Extensive universality.
Embodiment 24-27
Embodiment 1 is repeated, difference, which is only that, is changed to the bimetallics such as Fe/Co, Fe/Ru, Ni/Ru, Co/Ru for metal salt
Salt.Obtained catalyst is capable of forming monatomic catalyst.
Fig. 9 is the XRD spectra of the synthesized monatomic catalyst of Fe/Co, Fe/Ru, Ni/Ru, Co/Ru, by can be in figure
Find out that four kinds of synthesized monatomic catalyst only have the diffraction maximum of carbon, metal simple-substance or alloy or its compound does not occur
Peak.This illustrates that the monatomic process for synthetic catalyst of the transition metal can synthesize polymetallic monatomic catalyst.
Comparative example
Embodiment 1 is repeated, difference, which is only that, is changed to SiO for carbon black2.Obtained catalyst is capable of forming monatomic
Catalyst.It tests to obtain its load capacity to be only 0.5wt% by ICP-AES.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate examples made by the present invention, and is not to this
The restriction of the embodiment of invention for those of ordinary skill in the art on the basis of the above description can be with
It makes other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to the present invention
The obvious changes or variations extended out of technical solution still in the scope of protection of the present invention.
Claims (10)
1. a kind of monatomic catalyst of transition metal, which is characterized in that the catalyst is monatomic for active group with transition metal
Point, using carbon black as carrier, transition metal single atomic dispersion is in the surface and inside of carbon black；Wherein, monatomic with the transition metal
The total weight of catalyst is 100% meter, and the monoatomic load capacity of transition metal is 0.5-6wt%.
2. the monatomic catalyst of transition metal according to claim 1, which is characterized in that the transition metal atoms are selected from
Cr, Mn, Co, Cu, Zn, Nb, Mo, Ru, Rh, Pd, Ag, Cd, Os, Ir or Pt.
3. the monatomic catalyst of transition metal according to claim 1, which is characterized in that the carbon black is selected from
Ketjenblack EC-300J type carbon black or Vulcan XC-72 type carbon black.
4. the preparation method of the monatomic catalyst of transition metal as described in claim 1-3 is any, which is characterized in that including as follows
Step:
Transition metal salt and organic ligand are dissolved in organic solvent, is uniformly mixed, obtains clear transparent solutions；Carbon black, mixing is added
Uniformly, reaction solution is obtained；2~8h of impregnation at 40-80 DEG C, it is dry, obtain crude product；Crude product is placed in argon atmosphere, and
With 2~10 DEG C of min-1Heating rate is warming up to 300~580 DEG C, calcines 1-5h；Room temperature is down to get the transition metal list
Catalyst atom.
5. the preparation method according to claim 4, which is characterized in that transition metal salt, organic ligand in the reaction solution
The mass ratio of the material value are as follows: 1:3~1:20.
6. the preparation method according to claim 4, which is characterized in that the mass concentration of carbon black is 10- in the reaction solution
70mg·mL-1。
7. the preparation method according to claim 4, which is characterized in that the organic ligand is selected from Phen, 2,2- joins
Pyridine, melamine or phenylalanine；Preferably, the organic solvent is selected from ethyl alcohol or dimethyl sulfoxide.
8. the preparation method according to claim 4, which is characterized in that the transition metal salt be selected from transition metal villaumite,
One of transition metal nitrate, transition metal acetate, transition metal sulfate are a variety of.
9. the preparation method according to claim 4, which is characterized in that dry temperature is 60~190 DEG C, and drying time is
6~20h.
10. the monatomic catalyst of transition metal prepares an oxygen in electro-catalysis carbon dioxide reduction as described in claim 1-3 is any
Change the application in carbon.
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