CN109468662A - The preparation method of copper-molybdenum composite material and its application in electrolysis water liberation of hydrogen catalyst - Google Patents
The preparation method of copper-molybdenum composite material and its application in electrolysis water liberation of hydrogen catalyst Download PDFInfo
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- CN109468662A CN109468662A CN201811511437.6A CN201811511437A CN109468662A CN 109468662 A CN109468662 A CN 109468662A CN 201811511437 A CN201811511437 A CN 201811511437A CN 109468662 A CN109468662 A CN 109468662A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- C—CHEMISTRY; METALLURGY
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The application of elctro-catalyst the present invention provides the preparation method of copper-molybdenum composite material and its in electrolysis water liberation of hydrogen: it first prepares solution A: precursor A being added in deionized water, obtain solution A；Solution B is prepared again: precursor B being added in deionized water, is 0~13 with ammonium hydroxide and salt acid for adjusting pH, is obtained solution B；Finally solution A is poured into the empty beaker equipped with magneton, is placed it on blender, revolving speed is controlled in 1-1000RPM, solution B is added in above-mentioned beaker again, the time of stirring is that 1-10h pours into solution in centrifuge tube after stirring stops, it is placed in a centrifuge centrifugation, revolving speed is 1-30000RPM, time 1-30min, after centrifugation, lower sediment is placed in 1-100 DEG C of baking oven and is dried, can be obtained by flower-shaped base metal copper-molybdenum composite material in this way.Composite material produced by the present invention produces hydrogen in electro-catalysis, and oxygen is analysed in electro-catalysis, and electrocatalytic oxidation reduction and energy conversion aspect have very big advantage, can be applied to fuel cell and new energy conversion art.
Description
Technical field
The invention belongs to nanocomposite research fields, at room temperature, make two kinds of solution that slow reaction occur,
It forms copper-molybdenum composite material and is used for elctro-catalyst.
Background technique
In recent decades, with the development of science and technology, modern society increasingly increases severely to the demand of the energy, but with ore
Phenomena such as burning of fuel, environmental problem are got worse, air pollution, haze, global warming is more obvious, Er Qiemei, petroleum
The reserves of equal fossil fuels are limited, therefore we will find clean energy resource to replace traditional fossil fuels, in recent years
Hydrogen Energy causes the extensive concern of people, very friendly to environment because the combustion product of hydrogen is water, does not pollute.But
So far, the source of hydrogen depends on fossil energy, such as petroleum cracking, steam methane reforming, water-gas conversion etc..
These preparation methods not only efficiency it is very low, it is at high price, further relate to some specific consersion units, but also in the mistake for preparing hydrogen
The polluted gas such as carbon dioxide are inevitably generated in journey.Therefore, we will find the method that green prepares hydrogen, in recent years
Come, electrolysis aquatic products hydrogen is considered as obtaining a kind of highly effective approach of hydrogen, because the raw material that it is reacted is water, the production of burning
Object is also water, we can use some renewable energy such as wind power generation, hydroelectric generation, solar power generation as electrolysis in the process
Water provides required electric energy to prepare hydrogen, and water is reserves substance extremely abundant in nature, therefore, is electrolysed aquatic products hydrogen
It arouses widespread concern.
However, putative ideal electrolysis water catalyst is the platinum based catalyst of noble metal now, but since these are expensive
Metal price is expensive to be applied on a large scale so limiting it.In recent years, it studies some cheap, no pollution to the environment non-
Noble metal becomes the hot spot of research to substitute platinum-base material, is based on view of the above, we probe into a kind of simple method, synthesis
Composite material of molybdenum and copper, this catalyst belong to non-precious metal catalyst, and synthetic method is simple, there is preferable catalytic performance and stabilization
Property, and cost has been saved, there is stronger practical application value.
Summary of the invention
The technical problem to be solved by the embodiment of the invention is that provide a kind of copper-molybdenum composite material preparation method and its
Application in electrolysis water liberation of hydrogen catalyst.Preparation method of the present invention is easy to operate, flower-shaped composite active site obtained
It is more, electrochemical impedance is small, Hydrogen Evolution Performance preferably, long catalytic life, which has shown just in terms of electrocatalytic hydrogen evolution
In the advantage of large-scale application.
To achieve the above object, first goal of the invention of the invention is to provide a kind of preparation side of copper-molybdenum composite material
Method, technical solution be the following steps are included:
(1) it prepares precursor A solution: precursor A being added in deionized water, obtains 0 < concentration≤10mol/L forerunner
Body solution A, the precursor A are copper ion compound soluble easily in water；
(2) it configures precursor B solution: precursor B being added in deionized water, be 0~13 with ammonium hydroxide and salt acid for adjusting pH,
0 < concentration≤10mol/L precursor B solution is obtained, the precursor B is molybdenum ion compound soluble easily in water；
(3) it prepares flower-shaped base metal copper-molybdenum composite material: step (1) is prepared into precursor A solution under magnetic stirring
It is uniformly mixed with precursor B solution, obtains mixed solution, be then centrifuged, after centrifugation, lower sediment is placed in baking oven
Middle drying can be obtained by copper-molybdenum composite material in this way.
Further setting is that the revolving speed in step (3), in blender is controlled in 1-1000RPM；The time of stirring is 1-
10h；The revolving speed of centrifuge is 1-30000RPM；The time of centrifugation is 1-30min；The temperature of baking oven is 1-100 DEG C.
It includes that the tip at center and upper end extend connection that further setting, which is the structure of the copper-molybdenum composite material,
In at least four X-shapeds intersect slant edge wall, it is whole be similar to it is flower-shaped.
It is copper sulphate or/and copper chloride that further setting, which is the precursor A,.
It is sodium molybdate or/and four thio ammonium molybdate that further setting, which is the precursor B,.
Further setting is that the volume ratio of precursor A solution and precursor B solution is (1:1) in the step (3).
The present invention also provides copper-molybdenum composite materials prepared by a kind of preparation method as mentioned.
The present invention also provides a kind of users of elctro-catalyst based on the copper-molybdenum composite material in electrolysis water liberation of hydrogen
Method, it is characterised in that: the copper-molybdenum composite material is added in the mixed liquor of second alcohol and water, and sonic oscillation forms suspension, it will
The suspension is added dropwise in glassy carbon electrode surface, dries to form uniform thin layer, obtains the glass-carbon electrode of copper-molybdenum composite material modification,
The glass-carbon electrode that the copper-molybdenum composite material is modified is used for electrolysis water liberation of hydrogen.
Further setting is the glass-carbon electrode before suspension is added dropwise, and is first pre-processed, the pretreatment are as follows: successively
It polished, washed, 20KHz ultrasound 60s.
Further setting is the volume ratio 1:3 of second alcohol and water in the mixed liquor of second alcohol and water.
It is 50KHz ultrasound 2h that further setting, which is the parameter of the sonic oscillation,.
Copper-molybdenum composite material (CuMoS is covered with by prepared by the present inventionX) glass-carbon electrode carry out electro-chemical test,
In three-electrode system, copper-molybdenum composite material (CuMoS is covered with thisX) glass-carbon electrode as working electrode, saturation
Calomel electrode is used as reference electrode, graphite electrode to electrode) in, measure CuMoSXLinear sweep voltammetry curve.Test
Electrolyte solution used is the sulfuric acid solution of 0.5M.
Flower-shaped copper-molybdenum composite material made from the method for the present invention, shows good electrocatalytic hydrogen evolution performance, is your non-gold
The research and probe of metal catalyst goes out a novelty and simple approach.Obviously, above-described embodiment is used for the purpose of clearly saying
The citing that bright technical solution of the present invention is done, and the restriction not to embodiment.To those of ordinary skill in the art,
Other various forms of variations or variation can also be made on the basis of the above description, there is no need and unable to all realities
The scheme of applying is exhaustive.And thus amplify out and this material is applied to electro-catalysis analyses oxygen, electrocatalytic oxidation reduction aspect aobvious and
The variation or variation being clear to are still in protection scope of the present invention.
The method of the present invention is easy to operate, mild condition, has unique novelty, and composite material obtained is produced in electro-catalysis
Oxygen is analysed in hydrogen, electro-catalysis, and electrocatalytic oxidation reduction and energy conversion aspect have very big advantage, can be applied to fuel cell and new
Energy conversion field.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention, for those of ordinary skill in the art, without any creative labor, according to
These attached drawings obtain other attached drawings and still fall within scope of the invention.
Fig. 1 is the scanning electron microscope diagram piece of flower-shaped copper-molybdenum composite material made from the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope picture and EDS mapping figure of flower-shaped copper-molybdenum composite material made from the embodiment of the present invention 1
Piece；
Fig. 3 is the linear volt-ampere curve figure of flower-shaped copper-molybdenum composite material made from the embodiment of the present invention 1.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing
Step ground detailed description.
Embodiment 1: flower-shaped copper-molybdenum composite material (CuMoS is preparedX)
(1) it prepares solution A: copper sulphate being added in deionized water, obtains copper-bath；The concentration of solution is 0-
10mol/L；
(2) it prepares solution B: four thio ammonium molybdate being added in deionized water, be 0~13 with ammonium hydroxide and salt acid for adjusting pH,
Obtain four thio ammonium molybdate solution；The final concentration of 0-10mol/L of solution；
(3) it prepares flower-shaped base metal copper-molybdenum composite material: taking the empty beaker that magneton is housed, step (1) is prepared
Solution A is poured into sky beaker, is subsequently placed on blender, and revolving speed is controlled in 1-1000RPM, then step (2) are prepared
Solution B is added in above-mentioned beaker, and time of stirring is that 1-10h pours into solution in centrifuge tube after stirring stops, being placed in from
It is centrifuged in scheming, revolving speed 1-30000RPM, time 1-30min, after centrifugation, lower sediment is placed in 1-100 DEG C
It is dried in baking oven, can be obtained by flower-shaped base metal copper-molybdenum composite material in this way.
(4) pretreatment of electrode: glass-carbon electrode (PINE USA, rotating disk electrode (r.d.e), diameter 5mm) is taken, is successively thrown
Light, washing, the pretreatment of 20KHz ultrasound 60s；
(5) it prepares the glass-carbon electrode of flower-shaped copper-molybdenum composite material modification: a certain amount of flower-shaped copper-molybdenum composite material is added to
In ethyl alcohol and the mixed liquor of water volume ratio 1:3, suspension is formed in 50KHz ultrasound 2h, which is added dropwise in through step (4)
Pretreated glassy carbon electrode surface, naturally dry form uniform thin layer, obtain the glass carbon electricity of flower-shaped copper-molybdenum composite material modification
Pole；
(6) electro-chemical test: three-electrode system (step (5) preparation be covered with flower-shaped copper-molybdenum composite material (CuMoSX)
Glass-carbon electrode as working electrode, saturated calomel electrode is used as reference electrode, graphite electrode to electrode) in, measurement
CuMoSXLinear sweep voltammetry curve.The sulfuric acid solution that test electrolyte solution used is 0.5M.Fig. 3 can be found that compound
Material is in 10mA/cm2Under, there is lower overpotential, it can be seen that CuMoS made from this embodiment exampleXHydrogen is precipitated
With good catalytic activity.
Fig. 1 is the flying-spot microscope picture of the flower-shaped copper-molybdenum composite material, it can be seen that with mixing time difference, flower
The variation of shape pattern.A, b are the pattern that mixing time is 1 hour in figure, and c, d are the pattern that mixing time is 2 hours, and e, f are
The pattern that mixing time is 3 hours, g, h are the pattern that mixing time is 4 hours.
Fig. 2 is the transmission electron microscope picture (Fig. 2 a) and EDS mapping picture of the flower-shaped copper-molybdenum composite material.
Embodiment 2: preparation flowers shape copper-molybdenum composite material (CuMoSX)
(1) it prepares solution A: copper chloride being added in deionized water, obtains copper chloride solution；The concentration of solution is 0-
10mol/L；
(2) it prepares solution B: four thio ammonium molybdate being added in deionized water, be 0~13 with ammonium hydroxide and salt acid for adjusting pH,
Obtain four thio ammonium molybdate solution；The final concentration of 0-10mol/L of solution；
(3) it prepares flower-shaped base metal copper-molybdenum composite material: taking the empty beaker that magneton is housed, step (1) is prepared
Solution A is poured into sky beaker, is subsequently placed on blender, and revolving speed is controlled in 1-1000RPM, then step (2) are prepared
Solution B is added in above-mentioned beaker, and time of stirring is that 1-10h pours into solution in centrifuge tube after stirring stops, being placed in from
It is centrifuged in scheming, revolving speed 1-30000RPM, time 1-30min, after centrifugation, lower sediment is placed in 1-100 DEG C
It is dried in baking oven, can be obtained by flower-shaped base metal copper-molybdenum composite material in this way.
(4) pretreatment of electrode: glass-carbon electrode (PINE USA, rotating disk electrode (r.d.e), diameter 5mm) is taken, is successively thrown
Light, washing, the pretreatment of 20KHz ultrasound 60s；
(5) it prepares the glass-carbon electrode of flower-shaped copper-molybdenum composite material modification: a certain amount of flower-shaped copper-molybdenum composite material is added to
In ethyl alcohol and the mixed liquor of water volume ratio 1:3, suspension is formed in 50KHz ultrasound 2h, which is added dropwise in through step (4)
Pretreated glassy carbon electrode surface, naturally dry form uniform thin layer, obtain the glass carbon electricity of flower-shaped copper-molybdenum composite material modification
Pole；
(6) electro-chemical test: three-electrode system (step (5) preparation be covered with flower-shaped copper-molybdenum composite material (CuMoSX)
Glass-carbon electrode as working electrode, saturated calomel electrode is used as reference electrode, graphite electrode to electrode) in, measurement
CuMoSXLinear sweep voltammetry curve.The sulfuric acid solution that test electrolyte solution used is 0.5M.
Embodiment 3: porous flower-shaped copper-molybdenum composite material (CuMoS is preparedX)
(1) it prepares solution A: copper sulphate being added in deionized water, obtains copper-bath；The concentration of solution is 0-
10mol/L；
(2) it prepares solution B: sodium molybdate being added in deionized water, be 0~13 with ammonium hydroxide and salt acid for adjusting pH, obtain molybdenum
Acid sodium solution；The final concentration of 0-10mol/L of solution；
(3) it prepares flower-shaped base metal copper-molybdenum composite material: taking the empty beaker that magneton is housed, step (1) is prepared
Solution A is poured into sky beaker, is subsequently placed on blender, and revolving speed is controlled in 1-1000RPM, then step (2) are prepared
Solution B is added in above-mentioned beaker, and time of stirring is that 1-10h pours into solution in centrifuge tube after stirring stops, being placed in from
It is centrifuged in scheming, revolving speed 1-30000RPM, time 1-30min, after centrifugation, lower sediment is placed in 1-100 DEG C
It is dried in baking oven, can be obtained by flower-shaped base metal copper-molybdenum composite material in this way.
(4) pretreatment of electrode: glass-carbon electrode (PINE USA, rotating disk electrode (r.d.e), diameter 5mm) is taken, is successively thrown
Light, washing, the pretreatment of 20KHz ultrasound 60s；
(5) it prepares the glass-carbon electrode of flower-shaped copper-molybdenum composite material modification: a certain amount of flower-shaped copper-molybdenum composite material is added to
In ethyl alcohol and the mixed liquor of water volume ratio 1:3, suspension is formed in 50KHz ultrasound 2h, which is added dropwise in through step (4)
Pretreated glassy carbon electrode surface, naturally dry form uniform thin layer, obtain the glass carbon electricity of flower-shaped copper-molybdenum composite material modification
Pole；
(6) electro-chemical test: three-electrode system (step (5) preparation be covered with flower-shaped copper-molybdenum composite material (CuMoSX)
Glass-carbon electrode as working electrode, saturated calomel electrode is used as reference electrode, graphite electrode to electrode) in, measurement
CuMoSXLinear sweep voltammetry curve.The sulfuric acid solution that test electrolyte solution used is 0.5M.
Flower-shaped copper-molybdenum composite material made from the method for the present invention, shows good electrocatalytic hydrogen evolution performance, is your non-gold
The research and probe of metal catalyst goes out a novelty and simple approach.Obviously, above-described embodiment is used for the purpose of clearly saying
The citing that bright technical solution of the present invention is done, and the restriction not to embodiment.To those of ordinary skill in the art,
Other various forms of variations or variation can also be made on the basis of the above description, there is no need and unable to all realities
The scheme of applying is exhaustive.And thus amplify out and this material is applied to electro-catalysis analyses oxygen, electrocatalytic oxidation reduction aspect aobvious and
The variation or variation being clear to are still in protection scope of the present invention.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, therefore equivalent changes made in accordance with the claims of the present invention, is still within the scope of the present invention.
Claims (10)
1. a kind of preparation method of copper-molybdenum composite material, it is characterised in that the following steps are included:
(1) it prepares precursor A solution: precursor A being added in deionized water, obtains 0 < concentration≤10mol/L precursor A
Solution, the precursor A are copper ion compound soluble easily in water；
(2) it configures precursor B solution: precursor B being added in deionized water, be 0~13 with ammonium hydroxide and salt acid for adjusting pH, obtain
0 < concentration≤10mol/L precursor B solution, the precursor B are molybdenum ion compound soluble easily in water；
(3) prepare base metal copper-molybdenum composite material: by step (1) prepare precursor A solution under magnetic stirring with precursor B
Solution is uniformly mixed, and is obtained mixed solution, is then centrifuged, after centrifugation, lower sediment is placed in baking oven and is dried, this
Sample can be obtained by copper-molybdenum composite material.
2. a kind of preparation method of copper-molybdenum composite material according to claim 1, it is characterised in that: the copper-molybdenum is compound
The structure of material includes the tip at center and the slant edge wall that at least four X-shapeds that upper end is connected to intersect.
3. a kind of preparation method of copper-molybdenum composite material according to claim 1, it is characterised in that: the precursor A
For copper sulphate or/and copper chloride.
4. a kind of preparation method of copper-molybdenum composite material according to claim 1, it is characterised in that: the precursor B
For sodium molybdate or/and four thio ammonium molybdate.
5. a kind of preparation method of copper-molybdenum composite material according to claim 1, it is characterised in that: the step (3)
The volume ratio of middle precursor A solution and precursor B solution is (1:1).
6. copper-molybdenum composite material prepared by a kind of preparation method as described in one of claim 1-5.
7. a kind of application method of the elctro-catalyst based on copper-molybdenum composite material as claimed in claim 6 in electrolysis water liberation of hydrogen,
It is characterized in that: the copper-molybdenum composite material being added in the mixed liquor of second alcohol and water, and sonic oscillation forms suspension, this is suspended
Drop is added on glassy carbon electrode surface, dries to form uniform thin layer, the glass-carbon electrode of copper-molybdenum composite material modification is obtained, by the copper
The glass-carbon electrode of molybdenum composite material modification is used for electrolysis water liberation of hydrogen.
8. according to the method described in claim 7, it is characterized by: the glass-carbon electrode first carries out before suspension is added dropwise
Pretreatment, the pretreatment are as follows: successively polished, washed, 20KHz ultrasound 60s.
9. according to the method described in claim 7, it is characterized by: in the mixed liquor of second alcohol and water second alcohol and water volume ratio 1:
3。
10. according to the method described in claim 7, it is characterized by: the parameter of the sonic oscillation is 50KHz ultrasound 2h.
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