CN111424290A - Nickel-tin hydrogen evolution electrode - Google Patents
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Abstract
The invention relates to a nickel-tin hydrogen evolution electrode, which belongs to the technical field of hydrogen preparation and is prepared by the following method that water is used for preparing a plating solution, the formula of the plating solution comprises 40-100 g/L of nickel sulfate, 20-70 g/L of stannous chloride, 120-180 g/L of potassium pyrophosphate, 30-60 g/L of potassium tartrate, 10-25 g/L of potassium chloride, 10-20 g/L of methionine, 2-5 ml/L of ammonia water and 0.02-0.1 g/L of sodium dodecyl sulfate, a nickel net is subjected to electrolytic oil removal and acid cleaning, a constant current method is adopted, a nickel plate is used as an anode, the nickel net is used as a cathode, the pH value is 7.5-9 at 35-60 ℃, and the current density is 0.2-0.6A/dm2And electroplating for 5-15 min under the condition that the electrode spacing is 5-15 mm. The preparation process of the electrode is short, and the required equipment is simple; the electrode has high catalytic hydrogen evolution activity, can reduce the voltage of an alkaline water electrolysis cell, and reduces the electrolysis energy consumption.
Description
Technical Field
The invention relates to a nickel-tin hydrogen evolution electrode, in particular to a high-activity long-service-life nickel-tin hydrogen evolution electrode, and belongs to the technical field of hydrogen preparation.
Background
With the gradual implementation of the development strategy of green and low-carbon energy in China and the actual requirements of environmental pollution treatment and carbon emission reduction, the development of renewable energy in China is more and more intensive, and a serious electricity abandoning phenomenon is generated along with the development strategy. According to statistics, the total electric quantity of wind, light and water abandoned in China in 2018 reaches over 800 hundred million kWh. The alkaline water electrolysis hydrogen production technology is adopted, and the preparation of hydrogen by utilizing waste electricity is an effective way for realizing the conversion, storage and reutilization of renewable energy sources, thereby not only promoting the development of renewable energy sources in China, but also providing power for the development of hydrogen energy industry.
The hydrogen production by alkaline water electrolysis is a mature and safe hydrogen production method, but the method has high energy consumption, which limits the application of the method in the field of hydrogen production by electricity abandonment. The key to reducing the energy consumption of electrolysis is to reduce the cell voltage of the electrolyzer, the emphasis of which is to reduce the overpotential of the cathodic hydrogen evolution reaction. The research and development of the alkaline hydrogen evolution electrode with high catalytic hydrogen evolution activity is the most effective way to reduce the overpotential of the cathode hydrogen evolution reaction, and the electrode with high activity can also improve the electrolysis current density of the electrolytic cell, thus reducing the volume of the electrolytic cell and reducing the hardware investment of equipment. The platinum group noble metal and the alloy thereof have the best catalytic hydrogen evolution performance, but the high price of the noble metal can not be popularized and applied in the industrial field on a large scale, which makes the development of a novel non-noble metal catalyst necessary. The research finds that nickel and its alloy show better catalytic hydrogen evolution activity, including nickel-molybdenum alloy, nickel-molybdenum-sulfur alloy, nickel-cobalt alloy and the like, and the preparation methods of the electrodes comprise powder metallurgy, plasma sintering, chemical reduction method, electrodeposition method and the like. However, they generally have the problem of low chemical stability in a KOH electrolytic solution with a mass fraction of 30%, and the catalytic performance of the catalyst gradually deteriorates after long-term use. Analysis shows that the crystal structure components of the electrodes are more, some structure components are unstable in a strong alkaline electrolytic solution, a metal element dissolving phenomenon exists, and the catalytic hydrogen evolution performance of the electrodes is gradually reduced, and the problem cannot be solved by post-treatment technology such as annealing. At present, researchers are studying the preparation of nickel-tin alloy hydrogen evolution electrodes by an electrodeposition method, and find that the electrodeposited nickel-tin hydrogen evolution electrodes have better performance than other nickel alloy hydrogen evolution electrodes, but practical nickel-tin hydrogen evolution electrodes which can be used for alkaline water electrolysis cells are not developed at present.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a practical nickel-tin hydrogen evolution electrode for an alkaline water electrolyzer, and the nickel-tin hydrogen evolution electrode prepared by electroplating through specific plating solution and electroplating conditions has the characteristics of high activity, long service life, low energy consumption and low cost.
In order to achieve the purpose of the invention, the following technical scheme is provided.
The nickel-tin hydrogen evolution electrode is prepared by the following method:
(1) preparing plating solution with water
The formula of the plating solution comprises 40 g/L-100 g/L of nickel sulfate, 20 g/L0-70 g/L1 of stannous chloride, 120 g/L2-180 g/L3 of potassium pyrophosphate, 30 g/L4-60 g/L5 of potassium tartrate, 10 g/L-25 g/L of potassium chloride, 10 g/L-20 g/L of methionine, 2 ml/L-5 ml/L of ammonia water with the mass fraction of 25-28% and 0.02 g/L-0.1 g/L of sodium dodecyl sulfonate.
In the step (1):
the preferable formula of the plating solution is that nickel sulfate is 70 g/L, stannous chloride is 40 g/L, potassium pyrophosphate is 150 g/L, potassium tartrate is 45 g/L, potassium chloride is 18 g/L, methionine is 16 g/L, ammonia water with the mass fraction of 25-28% is 3 ml/L, and sodium dodecyl sulfate is 0.04 g/L.
(2) Pretreatment before electroplating
And carrying out electrolytic degreasing and acid washing on the nickel screen used as the cathode to obtain the pretreated nickel screen.
In the step (2):
preferably, electrolytic degreasing is carried out in the following manner:
preparing electrolytic degreasing liquid with water, wherein the formula of the electrolytic degreasing liquid comprises 20 g/L-30 g/L of sodium carbonate, 15 g/L-25 g/L of sodium sulfate and 60 g/L-80 g/L of sodium silicate;
the electrolytic degreasing method comprises the following steps: heating the electrolytic degreasing liquid to 40-60 ℃, putting a conductive metal plate and a nickel screen into the electrolytic degreasing liquid, using the conductive metal plate as an anode and the nickel screen as a cathode, switching on a power supply, controlling the electrolytic voltage to be 5-8V, and electrolyzing for 5-20 min to obtain the deoiled nickel screen.
The preferred pickling method is as follows: and (3) soaking the deoiled nickel screen in a hydrochloric acid aqueous solution with the mass fraction of 20-50%, wherein the soaking temperature is 20-40 ℃, and the soaking time is 10-20 min, so as to obtain the pretreated nickel screen.
(3) Electroplating of
The temperature of the plating solution is 35-60 ℃, and the pH value is 7.5-9; a nickel plate is used as an anode, a pretreated nickel net is used as a cathode, and the distance between the electrodes is 5 mm-15 mm; electroplating by constant current method with electroplating current density of 0.2A/dm2～0.6A/dm2Electroplating for 5-15 min to obtain the nickel-tin hydrogen evolution electrode;
in the step (3):
the preferred plating conditions are: the temperature of the plating solution was 45 deg.C, pH 8, the distance between the electrodes was 8mm, and the plating current density was 0.4A/dm2Electroplating time is 10 min.
Advantageous effects
1. The invention provides a nickel-tin hydrogen evolution electrode which is prepared by adopting a constant current electrodeposition method, and has short preparation process and simple required equipment;
2. the invention provides a nickel-tin hydrogen evolution electrode, wherein the surface of a plating layer of the nickel-tin hydrogen evolution electrode is rough, the surface area of the electrode is increased, and the minimum hydrogen evolution overpotential can reach η in a KOH solution with the mass fraction of 30 percent300161 mV. The nickel-tin hydrogen evolution electrode has higher catalytic hydrogen evolution activity, is beneficial to reducing the voltage of an alkaline water electrolysis cell and reducing the electrolysis energy consumption;
3. the invention provides a nickel-tin hydrogen evolution electrode, the crystal structure of which is Ni2Sn3The crystal has simple structure and components, has higher chemical stability in KOH solution with the mass fraction of 30 percent, and can be used for hydrogen evolution electrodes in the alkaline water electrolysis hydrogen production industry.
Drawings
FIG. 1 is a graph showing the relationship between voltage and current density in a KOH solution having a mass fraction of 30% for nickel-tin hydrogen evolution electrodes prepared in examples 1 to 3.
FIG. 2 is a scanning electron microscope photograph of the nickel-tin hydrogen evolution electrode obtained in example 3.
Fig. 3 is a graph showing the X-ray diffractometer measurement results of the nickel-tin hydrogen evolution electrode obtained in example 3.
FIG. 4 is a graph showing the relationship between the operating time of the long-term life test of the nickel-tin hydrogen evolution electrode obtained in example 3 and the cell voltage of the electrolyzer.
Detailed Description
The method for producing a nickel-tin hydrogen evolution electrode according to the present invention will be described in detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
(1) Preparing plating solution with water
The plating solution comprises 45 g/L of nickel sulfate, 20 g/L of stannous chloride, 125 g/L of potassium pyrophosphate, 30 g/L of potassium tartrate, 10 g/L of potassium chloride, 12 g/L of methionine, 2.2 ml/L of ammonia water with the mass fraction of 25-28% and 0.02 g/L of sodium dodecyl sulfate.
(2) Pretreatment before electroplating
Carrying out electrolytic degreasing on a nickel net used as a cathode, and then carrying out acid washing, wherein the specific steps are as follows:
preparing electrolytic degreasing liquid by water, wherein the formula of the electrolytic degreasing liquid comprises 20 g/L of sodium carbonate, 15 g/L of sodium sulfate and 65 g/L of sodium silicate, heating the electrolytic degreasing liquid to 44 ℃, putting a stainless steel plate and a nickel screen into the electrolytic degreasing liquid, taking the stainless steel plate as an anode and the nickel screen as a cathode, switching on a power supply, controlling the electrolytic voltage to be 5.5V, and electrolyzing for 6min to obtain the deoiled nickel screen.
And then soaking the deoiled nickel screen in 25 mass percent hydrochloric acid water solution at the temperature of 25 ℃ for 12min to obtain the pretreated nickel screen.
(3) Electroplating of
The temperature of the plating solution is 40 ℃, and the pH value is 7.5; a nickel plate is used as an anode, a pretreated nickel net is used as a cathode, and the distance between the electrodes is 10 mm; electroplating by constant current method with electroplating current density of 0.25A/dm2Electroplating time is 12min, and the nickel-tin hydrogen evolution electrode is prepared
Example 2
(1) Preparing plating solution with water
The plating solution comprises 95 g/L g of nickel sulfate, 60 g/L g of stannous chloride, 175 g/L g of potassium pyrophosphate, 60 g/L g of potassium tartrate, 25 g/L g of potassium chloride, 20 g/L g of methionine, 4.5 ml/L of ammonia water with the mass fraction of 25-28% and 0.08 g/L of sodium dodecyl sulfate.
(2) Pretreatment before electroplating
Carrying out electrolytic degreasing on a nickel net used as a cathode, and then carrying out acid washing, wherein the specific steps are as follows:
preparing electrolytic degreasing liquid by water, wherein the formula of the electrolytic degreasing liquid comprises 30 g/L of sodium carbonate, 25 g/L of sodium sulfate and 75 g/L of sodium silicate, heating the electrolytic degreasing liquid to 55 ℃, putting a stainless steel plate and a nickel screen into the electrolytic degreasing liquid, taking the stainless steel plate as an anode and the nickel screen as a cathode, switching on a power supply, controlling the electrolytic voltage to be 8V, and electrolyzing for 18min to obtain the deoiled nickel screen.
And then soaking the deoiled nickel screen in 45 mass percent hydrochloric acid water solution at the temperature of 40 ℃ for 20min to obtain the pretreated nickel screen.
(3) Electroplating of
The temperature of the plating solution is 55 ℃, and the pH value is 8.8; a nickel plate is used as an anode, a pretreated nickel net is used as a cathode, and the distance between the electrodes is 12 mm; electroplating by constant current method with electroplating current density of 0.5A/dm2And the electroplating time is 8min, thus obtaining the nickel-tin hydrogen evolution electrode.
Example 3
(1) Preparing plating solution with water
The plating solution comprises 70 g/L of nickel sulfate, 40 g/L of stannous chloride, 150 g/L of potassium pyrophosphate, 45 g/L of potassium tartrate, 18 g/L of potassium chloride, 16 g/L of methionine, 3 ml/L of ammonia water with the mass fraction of 25-28% and 0.04 g/L of sodium dodecyl sulfate.
(2) Pretreatment before electroplating
Carrying out electrolytic degreasing on a nickel net used as a cathode, and then carrying out acid washing, wherein the specific steps are as follows:
preparing electrolytic degreasing liquid by water, wherein the formula of the electrolytic degreasing liquid comprises 25 g/L of sodium carbonate, 20 g/L of sodium sulfate and 70 g/L of sodium silicate, heating the electrolytic degreasing liquid to 50 ℃, putting a stainless steel plate and a nickel screen into the electrolytic degreasing liquid, taking the stainless steel plate as an anode and the nickel screen as a cathode, switching on a power supply, controlling the electrolytic voltage to be 6V, and electrolyzing for 12min to obtain the deoiled nickel screen.
And then soaking the deoiled nickel screen in 35% hydrochloric acid water solution at the soaking temperature of 30 ℃ for 15min to obtain the pretreated nickel screen.
(3) Electroplating of
The temperature of the plating solution is 45 ℃ and the pH value is 8; a nickel plate is used as an anode, a pretreated nickel net is used as a cathode, and the distance between the electrodes is 8 mm; electroplating by constant current method with electroplating current density of 0.4A/dm2And the electroplating time is 10min, so that the nickel-tin hydrogen evolution electrode is prepared.
The nickel-tin hydrogen evolution electrode prepared in the examples 1 to 3 was tested as follows:
(1) cathodic polarization curve test
The cathode polarization curve of the nickel-tin hydrogen evolution electrode is tested by using a Chenghua CHI660D type electrochemical workstation, a three-electrode system is adopted, a saturated calomel electrode is used as a reference electrode, a platinum sheet electrode is used as an auxiliary electrode, a nickel-tin hydrogen evolution electrode is used as a working electrode, a test solution is a KOH solution with the mass fraction of 30%, the test temperature is 25 ℃, and forced stirring is added during the test, the test result is shown in figure 1, which shows a voltage-current density relation diagram of the nickel-tin hydrogen evolution electrode obtained in example 1, example 2 and example 3 in the KOH solution with the mass fraction of 30%, the hydrogen evolution activity of the nickel-tin hydrogen evolution electrode obtained in different examples is represented, the catalytic activity of the hydrogen evolution electrode obtained in example 3 is the highest, the hydrogen evolution overpotential η mV of the nickel-tin hydrogen evolution electrode obtained in example 1 is obtained in accordance with the Nernst process is 36300 mV 193mV, the hydrogen evolution overpotential of the nickel-tin hydrogen evolution electrode obtained in example 2 is η, and the hydrogen evolution overpotential of the nickel-tin hydrogen evolution electrode sprayed with alkaline water is 175mV 161mV, 175mV, 341 is obtained in the current industrial hydrogen electrolysis bath using alkali.
(2) Observation by scanning electron microscope
The surface structure and morphology of the nickel-tin hydrogen evolution electrode obtained in example 3 are observed by using a PHI L IPS X L30 type environmental scanning electron microscope, and the results are shown in FIG. 2, wherein the left side of FIG. 2 is a scanning electron microscope photograph with the magnification of 100 times, and the right side of FIG. 2 is a scanning electron microscope photograph with the magnification of 500 times.
The surface structure and morphology of the nickel-tin hydrogen evolution electrode obtained in examples 1 and 2 were observed by a PHI L IPS X L30 environment scanning electron microscope, and as a result, similar to example 3, both of them had rough surfaces, increasing the surface area of the electrode, and contributing to the improvement of the hydrogen evolution catalytic activity of the electrode.
(3) X-ray diffractometer testing
The structure of the nickel-tin hydrogen evolution electrode obtained in example 3 was tested using a Philips PANALYTICAL X' pert MPD X-ray diffractometer, for exampleFIG. 3 shows that the coating layer is mainly made of Ni3Sn2And (4) forming.
The structure of the nickel-tin hydrogen evolution electrode obtained in examples 1 and 2 was tested by means of Philips PANALYTIC X' pert MPD X-ray diffractometer, which showed that the plating layer consisted mainly of Ni3Sn2And (4) forming.
(4) Electrode long-term life test
The alkaline water electrolytic cell was assembled by using the nickel-tin hydrogen evolution electrode obtained in example 3, and the service life of the nickel-tin hydrogen evolution electrode obtained in example 3 was tested by using the XCDQ-1.0/1.6 alkaline water electrolysis hydrogen production apparatus developed by the seventh and eighth research institute of the national Ship re-engineering group corporation, and the test data is the cell voltage of the electrolytic cell at different times when the electrolytic cell was operated, and as a result, as shown in FIG. 4, the electrolytic cell used 30% by mass of KOH solution as an electrolyte, the operating temperature was 80 ℃, and the operating current density was 2000A/m2. The number of cells of the electrolytic cell assembled in the experiment was 6, and the nickel-tin hydrogen evolution electrode obtained in example 3 was an electrolytic cell cathode mesh, and an electrolytic cell anode mesh was a nickel mesh. The used nickel-tin hydrogen evolution electrode is pretreated by three methods of not soaking, soaking in a KOH solution with the mass fraction of 30% for 3 months and soaking in a KOH solution with the mass fraction of 30% for 6 months respectively. The results of fig. 4 show that the nickel-tin hydrogen evolution electrode obtained in example 3 can maintain high catalytic hydrogen evolution performance for a long time.
Under the same experimental conditions, the service life of the nickel-tin hydrogen evolution electrode obtained in the examples 1 and 2 is tested by utilizing XCDQ-1.0/1.6 alkaline water electrolysis hydrogen production equipment developed by the seventh and eighth research institute of China Ship re-engineering group company, which shows that the nickel-tin hydrogen evolution electrode obtained in the examples 1 and 2 can keep higher catalytic hydrogen evolution performance for a long time.
The tests show that the method can obtain the high-quality nickel-tin hydrogen evolution electrode, and overcomes the defects of poor electrode chemical stability, gradual reduction of catalytic activity after long-term use and the like in the prior art.
Claims (6)
1. A nickel-tin hydrogen evolution electrode is characterized in that: the nickel-tin hydrogen evolution electrode is prepared by adopting the following method:
(1) preparing plating solution with water
The formula of the plating solution comprises 40 g/L-100 g/L of nickel sulfate, 20 g/L0-70 g/L1 of stannous chloride, 120 g/L2-180 g/L3 of potassium pyrophosphate, 30 g/L4-60 g/L5 of potassium tartrate, 10 g/L-25 g/L of potassium chloride, 10 g/L-20 g/L of methionine, 2 ml/L-5 ml/L of 25-28% ammonia water by mass fraction and 0.02 g/L-0.1 g/L of sodium dodecyl sulfonate;
(2) pretreatment before electroplating
Carrying out electrolytic degreasing and acid washing on the nickel screen used as the cathode to obtain a pretreated nickel screen;
(3) electroplating of
The temperature of the plating solution is 35-60 ℃, and the pH value is 7.5-9; a nickel plate is used as an anode, a pretreated nickel net is used as a cathode, and the distance between the electrodes is 5 mm-15 mm; electroplating by constant current method with electroplating current density of 0.2A/dm2～0.6A/dm2And electroplating for 5-15 min to obtain the nickel-tin hydrogen evolution electrode.
2. The nickel-tin hydrogen evolution electrode according to claim 1, characterized in that: in the step (1):
the plating solution comprises 70 g/L of nickel sulfate, 40 g/L of stannous chloride, 150 g/L of potassium pyrophosphate, 45 g/L of potassium tartrate, 18 g/L of potassium chloride, 16 g/L of methionine, 3 ml/L of ammonia water with the mass fraction of 25-28% and 0.04 g/L of sodium dodecyl sulfate.
3. The nickel-tin hydrogen evolution electrode according to claim 1, wherein in the step (2), the electrolytic degreasing adopts a mode of preparing electrolytic degreasing liquid with water, and the formula of the electrolytic degreasing liquid comprises 20 g/L-30 g/L of sodium carbonate, 15 g/L-25 g/L of sodium sulfate and 60 g/L-80 g/L of sodium silicate;
heating the electrolytic degreasing liquid to 40-60 ℃, putting a conductive metal plate and a nickel net into the electrolytic degreasing liquid, using the conductive metal plate as an anode and the nickel net as a cathode, switching on a power supply, controlling the electrolytic voltage to be 5-8V, and electrolyzing for 5-20 min.
4. The nickel-tin hydrogen evolution electrode according to claim 1, characterized in that: in the step (2): the acid washing method comprises the following steps: and (3) soaking the deoiled nickel screen in 20-50% hydrochloric acid water solution at 20-40 deg.c for 10-20 min.
5. The nickel-tin hydrogen evolution electrode according to claim 1, characterized in that: in the step (3): the electroplating conditions are as follows: the temperature of the plating solution was 45 deg.C, pH 8, the distance between the electrodes was 8mm, and the plating current density was 0.4A/dm2Electroplating time is 10 min.
6. The nickel-tin hydrogen evolution electrode according to claim 1, wherein in the step (1), the formula of the plating solution comprises 70 g/L of nickel sulfate, 40 g/L of stannous chloride, 150 g/L of potassium pyrophosphate, 45 g/L of potassium tartrate, 18 g/L of potassium chloride, 16 g/L of methionine, 3 ml/L of ammonia water with the mass fraction of 25-28% and 0.04 g/L of sodium dodecyl sulfonate;
in the step (2), the electrolytic degreasing adopts the following mode that water is used for preparing electrolytic degreasing liquid, and the formula of the electrolytic degreasing liquid comprises 20 g/L-30 g/L of sodium carbonate, 15 g/L-25 g/L of sodium sulfate and 60 g/L-80 g/L of sodium silicate;
heating the electrolytic degreasing liquid to 40-60 ℃, putting a conductive metal plate and a nickel net into the electrolytic degreasing liquid, using the conductive metal plate as an anode and the nickel net as a cathode, switching on a power supply, controlling the electrolytic voltage to be 5-8V, and electrolyzing for 5-20 min;
the acid washing method comprises the following steps: soaking the deoiled nickel screen in 20-50 wt% concentration hydrochloric acid solution at 20-40 deg.c for 10-20 min;
in the step (3): the electroplating conditions are as follows: the temperature of the plating solution was 45 deg.C, pH 8, the distance between the electrodes was 8mm, and the plating current density was 0.4A/dm2Electroplating time is 10 min.
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| CN116377501B (en) * | 2023-04-10 | 2024-01-02 | 陕西华秦新能源科技有限责任公司 | Electrocatalytic hydrogen evolution material and preparation method and application thereof |
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