CN107541744B - A kind of nano silver electrode and the preparation method and application thereof that plate silver is formed in situ - Google Patents
A kind of nano silver electrode and the preparation method and application thereof that plate silver is formed in situ Download PDFInfo
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- CN107541744B CN107541744B CN201710689945.2A CN201710689945A CN107541744B CN 107541744 B CN107541744 B CN 107541744B CN 201710689945 A CN201710689945 A CN 201710689945A CN 107541744 B CN107541744 B CN 107541744B
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Abstract
The present invention provides a kind of nano silver electrodes that plate silver is formed in situ, it is prepared as follows to obtain: to pass through pretreated plate silver matrix material as anode, platinized platinum is cathode, saturated calomel electrode is reference electrode, aoxidizes to form Ag through the more current step pulses of 20~30 DEG C of constant temperature in electrolyte+Ag is made in layer+/ Ag electrode；With Ag+/ Ag electrode is cathode, and platinized platinum is anode, and saturated calomel electrode is reference electrode, is placed in electrolyte and restores 10~30min through 20~30 DEG C of constant temperature, -25~-100mA constant current, obtains nano silver electrode；Preparation process of the present invention is simple and easy to control, be not required to added metal ion can in plate silver electrode in-situ preparation nano-silver layer, substantially increase the electrode roughness factor, increase reaction active site, can be by CO using the nano silver electrode of preparation2It is reduced to CO, restores CO2The current efficiency and current density for generating CO greatly increase, and activity and stability improve.
Description
(1) technical field
The present invention relates to a kind of nano silver electrodes and preparation method thereof that plate silver is formed in situ, and restore in electro-catalysis
CO2In application.
(2) background technique
In past 100 years, fossil fuel is that science and technology and economic progress are made that tremendous contribution.However since natural resources has
Limit, we will face serious energy crisis.According to Energy Information Administration, it is expected that energy-consuming will be from 500,000 in 2006
Million Btu rise to the 701.6 gigabit Btu of the year two thousand thirty, and the speed with every year on average 1.1% increases.On the other hand, government in 2001
Between the data of climate change special commission show, CO in atmosphere2Concentration rise to 1999 from 280ppmv in 1750
The 367ppmv in year, growth rate are 1.5ppmv/.The CO released2In, about 57% is discharged into atmosphere, it is remaining then
It is discharged into ocean, so as to cause a series of environmental problems, such as global mean temperature is increased, and Melting Glacierss, sea level rise.
Although CO2Discharge amount increase, which can aggravate greenhouse effects, leads to a series of environmental problems, but itself is also a kind of latent
Contain carbon source materials.A large number of researchers attempt various methods for CO2Be converted into the energy used for the mankind, with reduce its
Content and alleviating energy crisis in atmosphere.It can be produced by renewable energy such as solar energy, wind energy and tide energy in view of electric energy
It is raw, without additional combustion of fossil fuel, therefore by people's extensive concern.Electro-catalysis restores CO2It is a kind of effective means, so
And CO2Thermodynamically stable activates CO2Energy needed for molecule is high, therefore studies high performance electrode material and improve electro-catalysis reduction
Performance is to efficiently restore CO2It is current popular project.
(3) summary of the invention
To solve the deficiencies in the prior art, the present invention provides one kind to be used for CO2Electro-catalysis restores in situ by plate silver
Nano silver electrode of formation and preparation method thereof.The present invention utilizes more current step pulses, first in plate silver electrode surface layer original position
Oxidation forms Ag+Layer, then the Ag that will be formed in situ by electrochemical method+Layer is reduced to simple substance Ag, and electrode surface obtained is to receive
Meter Yin, Adsorption increase, and take-off potential earlier, restores CO2Activity and selectivity is high, the service life is long.
The technical solution adopted by the present invention is that:
A kind of nano silver electrode that plate silver is formed in situ, is prepared as follows to obtain:
(1) more current step Ag+Layer:
Using by pretreated plate silver matrix material, as anode, platinized platinum is cathode, and saturated calomel electrode is reference electrode,
It aoxidizes to form Ag through the more current step pulses of 20~30 DEG C of constant temperature in electrolyte A+Ag is made in layer+/ Ag electrode, uses N2Drying,
It is spare；
It is 0.05~0.5mol/L (preferably 0.1mol/ that the electrolyte A, which is by the NaCl concentration soluble in water being formulated,
L solution)；
The current range of more current step pulses is 15~75mA to 0mA, wherein 15~75mA snap time 0.1~
0.4s, 0mA 0.1~0.4s of snap time, step number 5000~15000 times；
The method of the plate silver matrix pretreatment are as follows: plate silver matrix material is polishing to sand paper it is smooth, so
After be sequentially placed into acetone soln, 10~20min of ultrasound in deionized water, to remove the greasy dirt of material surface；
(2) electroreduction Ag+Layer:
With Ag made from step (1)+/ Ag electrode is cathode, and platinized platinum is anode, and saturated calomel electrode is reference electrode, is set
10~30min is restored through 20~30 DEG C of constant temperature, -25~-100mA constant current in electrolyte B, nano silver electrode is obtained, uses N2
Drying；
It is 0.1~0.5mol/L (preferably 0.1mol/ that the electrolyte B, which is by the NaCl concentration soluble in water being formulated,
L solution).
" electrolyte A " of the present invention, " electrolyte B " not special meaning is only intended to distinguish labeled as " A ", " B "
The electrolyte used in different operation step.
Nano silver electrode of the present invention can be applied to electro-catalysis reduction CO2, the application is using following device (such as Fig. 1
It is shown):
Described device is made of H-type reactor 1, electrochemical workstation 2, magnetic stirring apparatus 3, thermostatic water bath 4；The H-type
Reactor 1 includes cathode pool 1-3, anode pool 1-5；It is equipped with cathode 1-1, reference electrode 1-6 in the cathode pool 1-3, and stores
There is catholyte；Anode 1-2 is equipped in the anode pool 1-5, and storage has anolyte；The top rubber stopper of the cathode pool is close
The loss to prevent gas is sealed, is equipped with sample tap 1-7 above the cathode pool；The anode pool and air communication；The cathode
Pond and anode pool side are equipped with interface channel, and being equipped with cation-exchange membrane (Nafion 117) 1-4 in the interface channel will be negative
Pole liquid and anolyte separate；
The method of the application are as follows: using nano silver electrode of the present invention as cathode, platinum electrode be anode, saturated calomel electrode is
Reference electrode, catholyte CO2The 0.1mol/L KHCO of saturation3Aqueous solution, anolyte are 0.5mol/L NaOH aqueous solution,
Magnetic agitation, room temperature (20~30 DEG C) constant temperature, reduction potential be -1.1~-2V under the conditions of with potentiostatic method restore CO2, periodically take
Gas phase and liquid product in cathode pool are analyzed.
The beneficial effects are mainly reflected as follows: nano silver electrode preparation process is simple and easy to control, be not required to added metal from
Son can in plate silver electrode in-situ preparation nano-silver layer, substantially increase the electrode roughness factor, increase reaction active site.Benefit
It can be by CO with the nano silver electrode of preparation2It is reduced to CO, restores CO2The current efficiency and current density for generating CO greatly increase, living
Property and stability improve.
(4) Detailed description of the invention
Fig. 1: nano silver electrode electro-catalysis of the present invention restores CO2Experimental equipment.
(5) specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited in
This.
Embodiment 1
(1) the nano silver electrode preparation method that silver is formed in situ:
A, electrode pre-processes: the plate silver matrix of thick 0.5mm being cut into 2cm × 2cm size first, the silver electricity that will be cut
Pole successively through 1000# and 2000# sand paper be polishing to it is smooth after rinsed with deionized water, be then successively placed in acetone, deionized water
Middle ultrasound 10min, to remove the greasy dirt on surface；Finally, by pretreated plate silver N2Drying；
B, more current step Ag+Layer: using silver electrode made from step a as anode, the platinized platinum (2cm × 2cm) of homalographic is
Cathode, saturated calomel electrode are placed in the more current step pulses of constant temperature in electrolyte and aoxidize to form Ag as reference+Layer, control electricity
Bath temperature is 25 DEG C, and more current step electric currents are 50mA to 0mA, wherein 50mA snap time 0.2s, 0mA snap time
Step number 10000 times, total snap time 4000s, nano silver electrode is made in 0.2s.The electrolyte is 0.1mol/L
NaCl, solvent are water.NaCl 2.93g is taken to be dissolved in 500ml water when specific preparation, plating takes 125ml to use every time, will prepare
Ag+/ Ag electrode is dried up with N2；
C, electroreduction Ag+Layer: Ag is made with step b+/ Ag electrode is cathode, and the platinized platinum of homalographic is saturated sweet as anode
Mercury electrode is placed in constant temperature in electrolyte, constant current restores to obtain nano silver electrode as reference, and control electrolyte temperature is 25
DEG C, constant current is -50mA, recovery time 20min.The electrolyte is 0.1mol/L NaCl, and solvent is water, specific to prepare
When take NaCl 2.93g to be dissolved in 500ml water, take 125ml to use every time, by the nano silver electrode N of preparation2Drying.
(2) using the electrode of above-mentioned steps (1) preparation as cathode, platinum electrode is anode, and saturated calomel electrode is reference, electrode
Area is 2cm × 2cm, and anolyte is 0.5mol/L NaOH solution, and reaction volume 150ml, catholyte is CO2Saturation
0.1mol/L KHCO3 solution, reaction volume 100ml are stirred continuously with magnetic stirring apparatus, electrolyte temperature water bath with thermostatic control
Slot control is 25 DEG C, and reduction potential is -1.9V.Meanwhile gas phase and liquid product periodically being taken to be analyzed, specific device figure is as schemed
1.Nano silver electrode electrochemical reduction CO2It is 90.23% that CO faradaic efficiency (FE), which reaches peak, after 1h.
Embodiment 2
For the preparation manipulation of nano silver electrode in addition to NaCl dosage is 14.65g (0.5mol/L) in step b, remaining operation is equal
It is identical as embodiment 1 step (1).
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 90.73% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 3
The preparation manipulation of nano silver electrode removes more current step Ag+Step current 50mA snap time is changed to 0.1s when layer,
0mA snap time is outside 0.1s, remaining operation is identical as embodiment 1 step (1).
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 89.38% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 4
The preparation manipulation of nano silver electrode removes more current step Ag+The snap time of step current 50mA is changed to when layer
0.4s, 0mA snap time are outside 0.1s, remaining operation is identical as embodiment 1 step (1).
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 89.13% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 5
The preparation manipulation of nano silver electrode removes more current step Ag+Step current is changed to outside 15mA to 0mA when layer, remaining behaviour
Make identical as embodiment 1 step (1).
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 86.36% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 6
The preparation manipulation of nano silver electrode removes more current step Ag+Step current is changed to outside 75mA to 0mA when layer, remaining behaviour
Make identical as embodiment 1 step (1).
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 90.38% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 7
The preparation manipulation of nano silver electrode removes more current step Ag+Step number is changed to 5000 secondly, remaining is operated when layer
It is identical as embodiment 1 step (1).
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 90.11% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 8
The preparation manipulation of nano silver electrode removes more current step Ag+Step number is changed to 15000 secondly, remaining is operated when layer
It is identical as embodiment 1 step (1).
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 93.08% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 9
The preparation manipulation of nano silver electrode restores Ag except constant current+Electric current is changed to outside -25mA when layer, remaining operation and implementation
1 step of example (1) is identical.
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 91.96% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 10
The preparation manipulation of nano silver electrode restores Ag except constant current+Electric current is changed to outside -100mA when layer, remaining operation and reality
It is identical to apply 1 step of example (1).
Use nano silver electrode made above for cathode, remaining operation such as 1 step of embodiment (2), -1.9V potential reduction
CO2It is 87.98% that CO faradaic efficiency, which reaches peak, after 1h.
Embodiment 11
The preparation manipulation of nano silver electrode is identical as embodiment 1 step (1).
It uses nano silver electrode made above for cathode, handles the CO of 35mmol/L2, also except nano silver electrode electro-catalysis
Former CO2Current potential is remaining operation such as 1 step of embodiment (2) outside -1.8V, nano silver electrode electrochemical reduction CO2CO farads after 1h
It is 87.68% that current efficiency, which reaches peak,.
Embodiment 12
The preparation manipulation of nano silver electrode is identical as embodiment 1 step (1).
It uses nano silver electrode made above for cathode, handles the CO of 35mmol/L2, also except nano silver electrode electro-catalysis
Former CO2Current potential is remaining operation such as 1 step of embodiment (2) outside -2V, nano silver electrode electrochemical reduction CO2CO faraday after 1h
It is 85.34% that current efficiency, which reaches peak,.
Embodiment 13
The preparation manipulation of nano silver electrode is identical as embodiment 1 step (1).
It uses nano silver electrode made above for cathode, handles the CO of 35mmol/L2, also except nano silver electrode electro-catalysis
Former CO2Current potential is remaining operation such as 1 step of embodiment (2) outside -1.7V, nano silver electrode electrochemical reduction CO2CO farads after 1h
It is 82.93% that current efficiency, which reaches peak,.
Embodiment 14
The preparation manipulation of nano silver electrode is identical as embodiment 1 step (1).
It uses nano silver electrode made above for cathode, handles the CO of 35mmol/L2, also except nano silver electrode electro-catalysis
Former CO2Current potential is remaining operation such as 1 step of embodiment (2) outside -1.2V, nano silver electrode electrochemical reduction CO2CO farads after 1h
It is 63.65% that current efficiency, which reaches peak,.
Embodiment 15
The preparation manipulation of nano silver electrode is identical as embodiment 1 step (1).
It uses nano silver electrode made above for cathode, handles the CO of 35mmol/L2, also except nano silver electrode electro-catalysis
Former CO2Current potential is remaining operation such as 1 step of embodiment (2) outside -1.1V, nano silver electrode electrochemical reduction CO2CO farads after 1h
It is 53.78% that current efficiency, which reaches peak,.
Claims (6)
1. a kind of nano silver electrode that plate silver is formed in situ, which is characterized in that the nano silver electrode is prepared as follows
It obtains:
(1) more current step Ag+Layer:
Using by pretreated plate silver matrix material, as anode, platinized platinum is cathode, and saturated calomel electrode is reference electrode, in electricity
It aoxidizes to form Ag through the more current step pulses of 20~30 DEG C of constant temperature in solution liquid A+Ag is made in layer+/ Ag electrode, uses N2Drying, it is spare；
The electrolyte A is the solution for being 0.05~0.5mol/L by the NaCl concentration soluble in water being formulated；
The current range of more current step pulses is 15~75mA to 0mA, wherein 15~75mA snap time 0.1~
0.4s, 0mA 0.1~0.4s of snap time, step number 5000~15000 times；
(2) electroreduction Ag+Layer:
With Ag made from step (1)+/ Ag electrode is cathode, and platinized platinum is anode, and saturated calomel electrode is reference electrode, is placed in electrolysis
10~30min is restored through 20~30 DEG C of constant temperature, -25~-100mA constant current in liquid B, nano silver electrode is obtained, uses N2Drying；
The electrolyte B is the solution for being 0.1~0.5mol/L by the NaCl concentration soluble in water being formulated.
2. nano silver electrode as described in claim 1, which is characterized in that in step (1), the plate silver matrix material is located in advance
The method of reason are as follows: plate silver matrix material is polishing to sand paper smooth, is then sequentially placed into acetone soln, surpasses in deionized water
10~20min of sound, to remove the greasy dirt of material surface.
3. nano silver electrode as described in claim 1, which is characterized in that in step (1), the electrolyte A is molten by NaCl
The concentration that Yu Shuizhong is formulated is the solution of 0.1mol/L.
4. nano silver electrode as described in claim 1, which is characterized in that in step (2), the electrolyte B is molten by NaCl
The concentration that Yu Shuizhong is formulated is the solution of 0.1mol/L.
5. nano silver electrode as described in claim 1 restores CO in electro-catalysis2In application.
6. application as claimed in claim 5, which is characterized in that the method for the application are as follows:
It is anode using the nano silver electrode as cathode, platinum electrode, saturated calomel electrode is reference electrode, catholyte CO2Saturation
0.1mol/L KHCO3Aqueous solution, anolyte are 0.5mol/L NaOH aqueous solution, in magnetic agitation, room temperature constant temperature, reduction electricity
Position be -1.1~-2V under the conditions of with potentiostatic method restore CO2, gas phase and liquid product in cathode pool is periodically taken to be analyzed.
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| CN112126943B (en) * | 2020-08-21 | 2022-04-05 | 佛山方竹科技有限公司 | Mesoporous silver electrode and preparation method and application thereof |
| CN112813480A (en) * | 2021-01-07 | 2021-05-18 | 江苏大学 | In-situ grown silver nanocluster material, preparation method thereof and electro-catalytic reduction of CO2Applications of |
| CN112981452A (en) * | 2021-02-05 | 2021-06-18 | 深圳职业技术学院 | Water oxidation electrocatalyst and preparation method thereof, and water oxidation electrode and preparation method thereof |
| CN114959761B (en) * | 2022-05-05 | 2023-11-03 | 中国科学院上海高等研究院 | Preparation method and application of silver hollow fiber electrode |
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