CN106757142B - Preparation method and application of carbon fiber loaded nanoscale bimetal PtCo catalytic electrode - Google Patents
Preparation method and application of carbon fiber loaded nanoscale bimetal PtCo catalytic electrode Download PDFInfo
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Abstract
A carbon fiber loaded nano-scale bimetal PtCo catalytic electrode preparation method and application thereof relate to a PtCo preparation method and application thereof, carbon fiber is taken as a substrate of the electrode, acetone is used for washing, the electrode is placed in a drying box, and deionized water is used for preparing a mixed salt solution containing chloroplatinic acid and cobalt nitrate; ultrasonically oscillating the prepared solution; beginning to dip and dry in a drying oven; firstly heating in an inert gas atmosphere, introducing hydrogen under the protection of inert gas, and putting the prepared electrode into a tubular furnace to obtain the carbon fiber loaded nanoscale bimetal PtCo catalytic electrode. The electrode is applied to the hydrogen production by coal slurry electrolysis, and the electrolysis efficiency can be effectively improved. The preparation method of the nano-scale bimetal PtCo catalytic electrode is simple, the price is low, the nano-scale PtCo is uniformly dispersed, and the catalytic efficiency of coal slurry electrolysis is greatly improved.
Description
Technical Field
The invention relates to a preparation method and application of PtCo, in particular to a preparation method and application of a carbon fiber loaded nanoscale bimetal PtCo catalytic electrode.
Background
The hydrogen production by coal slurry electrolysis is a subject integrating clean utilization of coal and development of cheap hydrogen energy. The significance of the problem of hydrogen production by coal slurry electrolysis was proposed as early as 1979 in Robert W, Coughlin, M, Faroque, Nature, 1979, 279, 301 and 303. The mechanism was initially studied by Park et al in Patrick M. Dhooge, David E. Stilwell, and Su-Moon Park. J. electrochem. Soc. 1982, 129: 1719-. In 2004, Botte directly bought binary alloy electrodes from Alfa Aesar company, improved the electrolysis process conditions, added Fe3+And Fe2+So that the current density and the efficiency of electrolysis are greatly improved. However, in order to make them more valuable for use, catalytic anodes with high activity, low cost and long life must be sought.
Botte et al have found that Pt, Rh, Pt-Rh, Pt-Ir, Pt-Ir-Rh (Nilesh Sathe, Gerardine G. Botte. Journal of Power sources 2006, 161:513 one 523) are plated on carbon fibers by electroplating, and the catalytic performance of the electrode is tested by electrolyzing coal and graphite under constant current, and the Pt-Ir electrode has good catalytic effect.
Yin et al studied a titanium-based platinum-iron alloy catalytic electrode. The method comprises the steps of firstly electrodepositing platinum on a titanium substrate by a constant current method, then electrodepositing iron, then placing the titanium substrate in a high-temperature treatment furnace for high-temperature treatment, and then soaking the titanium substrate in sulfuric acid to remove the iron which does not form alloy. The performance of the catalytic electrode was tested using the I-V curve. However, the diameter of the alloy particles formed by the method is about 50 nm-90 nm. (Cheng, Dan-Hong, Liang-Ming, Lv, Shi-Yin, Ji, Xue-Bin, Yin, Ren-He. Acta ChimicaInica. 2008, 66: 511-.
Yin et al also prepared Ti/Pt, Ti/IrO by thermal decomposition2, Ti/IrO2-RuO2, Ti/Pt-IrO2,Ti/Pt-RuO2A catalytic electrode. Coating the mother liquid on the surface of the substrate, and then carrying out heat treatment after coating. All prepared electrodes are in a typical dry mud shape, and the effective contact area of the prepared electrodes is not ideal. (Yin, Ren-He, Zhao, Yong-Gang, Lv, Shi-Yin, Liu, Huai-You, Cao, Wei-Min, Chinese Journal Of applied chemistry 2010,27: 215-.
Yu et al prepared a carbon fiber-supported Pt-Fe bimetallic catalytic electrode by a dip-reduction method. The carbon fiber supported Pt-Fe (1: 1) catalytic electrode is applied to a system for preparing hydrogen by electrolyzing coal slurry, and has the best electrolytic efficiency. (PingYu, Gerardine G. Botte. Journal of Power sources 2015,274: 165-169)
In summary, the traditional anode for hydrogen production by coal slurry electrolysis is a pure platinum electrode, but the pure platinum electrode is high in price and low in storage capacity. In recent years, various alloy catalytic electrodes have been developed, all of which are effective in improving the electrolysis efficiency. Cobalt, as a transition metal, forms an alloy with platinum, has good stability, increases the activity of the catalytic electrode and reduces the price of the electrode. The carbon fiber as a matrix has good chemical stability and large surface area. The electrode is prepared by adopting a dipping reduction method, the metal alloy is nano-scale and is uniformly dispersed, and the method is simple and has low cost. The prepared carbon fiber loaded nano-scale bimetallic PtCo catalytic electrode has high practical value.
Disclosure of Invention
The invention aims to provide a preparation method and application of a carbon fiber loaded nanoscale bimetal PtCo catalytic electrode. The particle size of PtCo nano alloy particles in the catalyst is 20-40 nm, and the electrolytic efficiency of PtCo/CFs in the electrolytic process of coal slurry is improved by 7-25% compared with that of Pt/CFs; and the method is applied to the hydrogen production by coal slurry electrolysis.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a carbon fiber loaded nanoscale bimetal PtCo catalytic electrode comprises the following steps:
A. carbon fibers are taken as a substrate of the electrode, washed by acetone, dried in a drying oven at 100-130 ℃ for 1-3 h, and naturally cooled to room temperature;
B. preparing a mixed salt solution containing chloroplatinic acid and cobalt nitrate by using deionized water, wherein the molar concentration of the chloroplatinic acid is 1-500mmol/L, the concentration of the cobalt nitrate is 1-500mmol/L, and the atomic ratio of the chloroplatinic acid to the cobalt nitrate is 10:1-1: 10; ultrasonically oscillating the prepared solution for 10-30 min;
C. placing the electrode prepared in the step A into the solution prepared in the step B, and beginning to soak; after a plurality of hours, finishing the dipping, and then drying in a drying oven at 100-130 ℃ for 1-3 hours;
D. putting the electrode prepared in the step C into a tube furnace, heating to 200-1000 ℃ in an inert gas atmosphere, introducing hydrogen under the protection of inert gas, and keeping for 1-6 hours; reducing the temperature to room temperature in inert gas after reduction to obtain the carbon fiber loaded nano-scale bimetallic PtCo catalytic electrode.
According to the preparation method of the carbon fiber loaded nanoscale bimetal PtCo catalytic electrode, the average particle size of particles of the nano alloy is 10-40 nm.
An application method of a carbon fiber loaded nano-scale bimetallic PtCo catalytic electrode is to apply the catalyst to the preparation of hydrogen by coal slurry electrolysis.
The invention has the advantages and effects that:
the invention adopts an immersion method to load Pt and Co precursors on the carbon fiber electrode. And then, under the protection of inert gas, performing high-temperature reduction by using hydrogen to prepare the carbon fiber loaded nano-scale bimetallic PtCo catalytic electrode. The electrode is applied to the hydrogen production by coal slurry electrolysis, and the electrolysis efficiency can be effectively improved. The preparation method of the nano-scale bimetal PtCo catalytic electrode is simple, the price is low, the nano-scale PtCo is uniformly dispersed, and the catalytic efficiency of coal slurry electrolysis is greatly improved.
The traditional electrode of the coal slurry electrolysis system is a Pt sheet electrode, and because Pt is a noble metal, Co is doped to form an alloy electrode, so that the cost is reduced, and the catalytic performance is greatly enhanced. The method of dipping reduction is applied, the operation is simple, the price is low, the obtained nano-alloy can be uniformly distributed on the carbon fiber, the contact area of electrolysis can be increased, and the electrolysis efficiency is improved. The system for preparing hydrogen by coal slurry electrolysis has great application prospects in the aspects of clean utilization of coal and development of cheap new energy hydrogen, so that efficient and cheap catalytic electrode preparation is also an important aspect.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a PtCo/CFs catalytic electrode prepared in example 1;
FIG. 2 is an X-ray photoelectron spectroscopy (XPS) graph of the PtCo/CFs catalytic electrode prepared in example 1;
FIG. 3 is a high-power Transmission Electron Microscope (TEM) image of the PtCo/CFs catalytic electrode prepared in example 1.
Detailed Description
The present invention will be described in detail with reference to examples.
Carbon fibers are used as a substrate of the electrode. And (3) after being washed by acetone, drying the mixture in a drying oven at 100-130 ℃ for 1-3 h, and naturally cooling the mixture to room temperature. Preparing a mixed salt solution containing chloroplatinic acid and cobalt nitrate by using deionized water, wherein the concentration of the chloroplatinic acid is 1-500mmol/L, the concentration of the cobalt nitrate is 1-500mmol/L, and the concentration ratio of the chloroplatinic acid to the cobalt nitrate is 10:1-1: 10. And ultrasonically oscillating the prepared solution for 10-30 min. The prepared electrode was placed in the solution prepared in step B and the impregnation was started. And after a plurality of hours, finishing the dipping, and then drying in a drying oven at 100-130 ℃ for 1-3 hours. And putting the prepared electrode into a tubular furnace, firstly introducing inert gas to exhaust air in the furnace, then heating the electrode to 200-1000 ℃ in the inert gas, introducing hydrogen under the protection of argon, and keeping the temperature for 1-3 hours. Reducing the temperature to room temperature in inert gas after reduction to obtain the carbon fiber loaded nano-scale bimetallic PtCo catalytic electrode.
And carrying out structural characterization on the prepared carbon fiber loaded nanoscale bimetal PtCo catalytic electrode. As can be seen from the Scanning Electron Microscope (SEM) image of fig. 1, the PtCo alloy particles are relatively uniformly dispersed on the carbon fibers. According to X-ray photoelectron spectroscopy (XPS) of fig. 2, the binding energy of the PtCo catalyst is shifted to a higher direction than that of pure Pt, indicating the formation of PtCo alloy. From the Transmission Electron Microscope (TEM) image of fig. 3, it can be seen that the bimetallic PtCo is nanoscale. The prepared catalytic electrode is applied to a coal slurry electrolysis hydrogen production system to test the catalytic performance, and the method is to dissolve 0.1-100 g of coal powder into 10-3000 ml of 0-4 mol/L sulfuric acid to prepare a coal slurry solution with the concentration of 1-500 g/L as an anode solution, and a cathode solution is 10-3000 ml of 0-4 mol/L sulfuric acid solution. The electrolysis apparatus used was an H-cell. The prepared electrode was used as an anode, and a Pt sheet electrode was used as a cathode. And (3) placing the electrolytic cell in a water bath kettle, and keeping the temperature at 30-120 ℃. The electrochemical workstation is used for testing the polarization time of electrolysis under constant current to express the catalytic performance of the electrode. The electrolytic efficiency of PtCo/CFs in the electrolytic process of the coal slurry is improved by 7-25% compared with that of Pt/CFs.
Example 1
Soaking carbon fiber in 0.024 mol L-1H of (A) to (B)2PtCl6·H2O and Co (NO)3)2·6H2The solution of O was immersed for 4 hours. The electrode was then dried in a drying oven at 110 ℃ for 1 h.
And (3) placing the electrode in a tube furnace, heating to 450 ℃ in a nitrogen atmosphere, introducing hydrogen, keeping the constant temperature for 2 hours, and naturally cooling to room temperature in the nitrogen atmosphere. And obtaining the carbon fiber loaded nano-scale bimetallic PtCo catalytic electrode.
Electrochemical testing of hydrogen production by coal electrolysis was performed in an H-type electrolytic cell using the PtCo catalytic electrode prepared in example 1 as the catalytic anode and the cathode as the platinum sheet electrode. Preparing coal slurry solution with coal powder concentration of 0.04 g/mL and about 170 mu m as anode solution, wherein the coal slurry solution contains 1mol/L H2SO4，0.04 mol L-1Ferric sulfate and ferrous sulfate. The cathode chamber is 1mol/L H2SO4And (3) solution. At 80 ℃ the current density was 15.7mA/cm2And (5) testing under the condition.
The polarization time of the PtCo catalytic electrode prepared in example 1 was 47145 s.
Example 2
Soaking carbon fiber in 0.024 mol L-1H2PtCl6·H2In O solution, the rest steps are the same as example 1. The polarization time of the electrochemical test was 38290 s.
Example 3
The prepared electrode was placed in a tube furnace and reduced at 300 ℃ in a hydrogen atmosphere, and the rest of the procedure was the same as in example 1. The polarization time for the electrochemical test was 35085 s.
Example 4
The prepared electrode was placed in a tube furnace and reduced at 400 ℃ in a hydrogen atmosphere, and the rest of the procedure was the same as in example 1. The polarization time for the electrochemical test was 40445 s.
Example 5
The prepared electrode was placed in a tube furnace and reduced at 600 ℃ in a hydrogen atmosphere, and the rest of the procedure was the same as in example 1. The polarization time of the electrochemical test was 40235 s.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and are intended to enable those skilled in the art to understand the present invention, and not to limit the scope of the present invention. Therefore, all equivalent changes and modifications made according to the concept of the present invention should be within the scope defined by the appended claims.
Claims (2)
1. A preparation method of a carbon fiber loaded nanoscale bimetal PtCo catalytic electrode is characterized by comprising the following steps:
A. carbon fibers are taken as a substrate of the electrode, washed by acetone, dried in a drying oven at 100-130 ℃ for 1-3 h, and naturally cooled to room temperature;
B. preparing a mixed salt solution containing chloroplatinic acid and cobalt nitrate by using deionized water, wherein the molar concentration of the chloroplatinic acid is 1-24mmol/L, the concentration of the cobalt nitrate is 1-24mmol/L, and the atomic ratio of the chloroplatinic acid to the cobalt nitrate is 10:1-1: 10; ultrasonically oscillating the prepared solution for 10-30 min;
C. placing the electrode prepared in the step A into the solution prepared in the step B, and beginning to soak; after 4 hours, finishing the dipping, and then drying the mixture in a drying oven at the temperature of 100-130 ℃ for 1-3 hours;
D. putting the electrode prepared in the step C into a tube furnace, heating to 200-1000 ℃ in an inert gas atmosphere, introducing hydrogen under the protection of inert gas, and keeping for 1-6 hours; reducing the temperature to room temperature in inert gas after reduction to obtain the carbon fiber loaded nanoscale bimetal PtCo catalytic electrode;
the average particle size of the particles of the nano alloy is 10-40 nm.
2. An application method of a carbon fiber loaded nano-scale bimetallic PtCo catalytic electrode is characterized in that the method is to use the catalyst in the preparation of hydrogen by coal slurry electrolysis.
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