CN113862727A - A kind of cleaning and regeneration method of alkaline electrolysis hydrogen production cathode net - Google Patents
A kind of cleaning and regeneration method of alkaline electrolysis hydrogen production cathode net Download PDFInfo
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Abstract
本发明涉及电解水制氢技术领域，公开了一种碱性电解制氢阴极网的清洗再生方法，包括以下步骤：将使用过的阴极网用纯水冲洗后，置于酸液中进行超声清洗；将酸洗后的阴极网用纯水再次进行冲洗后，将阴极网浸于电镀液中，负载催化层；将重新负载催化层的阴极网进行煅烧；将煅烧后的阴极网置于碱液中进行鼓泡清洗；将碱液鼓泡清洗后的阴极网用纯水清洗干净，烘干后得到清洗再生的阴极网。通过电镀法使得阴极网表面重新负载催化层，使得阴极网的催化活性得到恢复和提高；通过碱液鼓泡清洗，洗掉了不稳定的催化层，减轻了阴极网实际使用过程中催化层的脱落问题。清洗再生的阴极网，析氢过电位明显低于旧阴极网，能够提高电解水制氢过程中的产氢效率。The invention relates to the technical field of hydrogen production by electrolysis of water, and discloses a cleaning and regeneration method of a cathode net for alkaline electrolysis hydrogen production. ; Rinse the acid-washed cathode mesh with pure water again, immerse the cathode mesh in the electroplating solution, and load the catalytic layer; calcine the cathode mesh with the reloaded catalytic layer; place the calcined cathode mesh in the alkaline solution Bubbling cleaning is carried out in the lye solution; the cathode net after the lye bubbling cleaning is cleaned with pure water, and the cleaned and regenerated cathode net is obtained after drying. The surface of the cathode mesh is reloaded with the catalytic layer by electroplating, so that the catalytic activity of the cathode mesh is restored and improved; the unstable catalytic layer is washed away by bubbling and cleaning with alkaline solution, which reduces the catalytic activity of the cathode mesh in the actual use process. shedding problem. After cleaning and regenerating the cathode net, the hydrogen evolution overpotential is significantly lower than that of the old cathode net, which can improve the hydrogen production efficiency in the process of hydrogen production by electrolysis of water.
Description
Technical Field
The invention relates to the technical field of hydrogen production by water electrolysis, in particular to a cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode net.
Background
The hydrogen is regarded as the most ideal energy carrier due to the advantages of green, low carbon, high efficiency, storage and transportation and the like. The hydrogen production by water electrolysis by utilizing renewable energy sources such as wind power, photovoltaic and the like is one of the most important production modes of hydrogen in the future. At present, the water electrolysis hydrogen production technology mainly comprises alkaline water electrolysis hydrogen production, solid polymer water electrolysis hydrogen production and solid oxide water electrolysis hydrogen production, and the alkaline water electrolysis hydrogen production technology is relatively mature, the equipment manufacturing cost is low, and the scale of a single device is large, so the water electrolysis hydrogen production technology is mainly adopted at present.
The key components for producing hydrogen by alkaline electrolysis of water are an electrolytic cell, which generally comprises end plates, pole plates, a pole net, a diaphragm, sealing materials and fasteners, wherein the pole net is an important part for producing hydrogen by electrolysis of water. The polar plate is mainly made of nickel, and in order to improve the generation efficiency of hydrogen, the surface of the cathode mesh is usually loaded with a multi-element alloy catalytic material such as nickel, iron, molybdenum, cobalt and the like. In the long-term use process of hydrogen production by water electrolysis, due to factors such as gas production, scouring of electrolyte and the like, the catalyst layer on the surface of the cathode mesh falls off, and meanwhile, part of impurities are adhered and accumulated on the surface of the polar mesh, so that the catalytic area of the polar mesh is reduced, the hydrogen production efficiency of the electrolytic cell is reduced, and the energy consumption is increased. At present, the polar net is usually replaced, and the old polar net is not effectively treated.
Disclosure of Invention
The invention aims to provide a cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode net, which solves the problem that the old cathode net is not effectively treated.
The invention is realized by the following technical scheme:
a cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh comprises the following steps:
1) washing the used cathode mesh with pure water, and then placing the cathode mesh in acid liquor for ultrasonic cleaning;
2) washing the cathode mesh after acid washing with pure water again, and soaking the cathode mesh in electroplating solution to load a catalytic layer; ni is contained in the plating solution2+And also contains Fe2+And Co2+One or two of them;
wherein Ni2+The concentration is (0.08-0.38) mol/L, Fe2+The concentration is (0.02-0.08) mol/L, Co2+Is the concentration (0.01-0.04) mol/L;
3) calcining the cathode mesh which is newly loaded with the catalytic layer;
4) placing the calcined cathode mesh in alkali liquor for bubbling cleaning;
5) and cleaning the cathode mesh cleaned by bubbling alkali liquor with pure water, and drying to obtain the cleaned and regenerated cathode mesh.
Further, in step 1), the solution is washed with pure water until the pH of the solution is 7 to 8.
Further, in the step 1), citric acid or oxalic acid is adopted as the acid solution, and the pH value of the acid solution is 1-3.
Further, in the step 1), the ultrasonic power density is 0.3-0.5W/cm2And the cleaning time is 5-30 min.
Further, in step 2), the solution is washed with pure water until the pH of the solution is 6 to 7.
Further, in the step 2), the parameters of electroplating are as follows: the electro-deposition potential is-1.0 to-1.6V, and the electro-deposition time is 10 to 500 s.
Further, in the step 3), the calcination temperature is 500-600 ℃, and the calcination time is 0.5-2 h.
Further, in the step 5), the alkali liquor is potassium hydroxide solution, and the mass concentration is 10% -30%.
Further, in the step 5), the bubbling intensity aeration intensity is (10-100) mL/cm2The cleaning time is 10-60 min.
Further, in the step 5), the pH value of the solution in the washing with pure water is 7-8;
hot air drying is adopted, the drying temperature is 100-.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh, which comprises the following steps: pure water washing, ultrasonic pickling, catalyst electroplating loading, high-temperature calcination, alkali liquor bubbling cleaning, drying and the like, and crystals, scaling substances and unstable catalyst layers attached to the surface of the electrode are effectively removed through the ultrasonic pickling process; the surface of the cathode net is re-loaded with the catalyst layer by an electroplating method, so that the catalytic activity of the cathode net is recovered and improved; through the washing of alkali liquor bubbling, the unstable catalyst layer is washed away, and the problem of the catalyst layer falling off in the practical use process of the cathode mesh is reduced. The regenerated cathode net is cleaned by adopting the method, the overpotential of hydrogen evolution is obviously lower than that of the old cathode net, and the hydrogen production efficiency in the hydrogen production process by water electrolysis can be improved.
Furthermore, citric acid or oxalic acid solution is adopted in the acid washing process, so that the metal cation chelating effect is achieved, and the cation cleaning effect is better.
Further, the catalyst electroplating load adopts nickel sulfate, ferric sulfate and cobalt sulfate solution, and an unstable catalyst load layer is removed by bubbling and cleaning with alkali liquor after the catalyst electroplating load.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
A cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh comprises the following steps:
1) the cathode mesh is flushed with pure water until the pH value of the solution reaches 7;
the surface of the used cathode mesh can be hung with some alkali liquor, so that the cathode mesh can show alkalinity when being washed by water; and (4) washing to be neutral, which indicates that the alkaline components on the surface of the cathode net are basically washed clean.
2) Putting the cathode mesh into a citric acid solution with pH value of 1 for ultrasonic cleaning, wherein the ultrasonic power density is 0.3W/cm2Cleaning for 30 min;
3) washing the cathode mesh subjected to acid washing with pure water until the pH value of the solution reaches 6;
4) by using NiSO4·6H2O、FeSO4·7H2O、CoSO4·7H2O preparing electroplating solution containing 0.08mol/L Ni2+And at the same time contains 0.02mol/L of Fe2+And 0.01mol/L of Co2+The electrodeposition voltage is-1.40V, and the electrodeposition time is 100 s;
5) placing the cathode plate which is re-loaded with the catalytic layer in a high-temperature furnace at 500 ℃ for calcining for 2 h;
6) placing the calcined cathode mesh in 30% potassium hydroxide solution for cleaning, wherein the bubbling strength is 10mL/cm2The cleaning time is 30 min;
7) washing the cathode mesh subjected to alkali liquor bubbling cleaning with pure water until the pH value of the solution is 7;
8) and drying the cathode mesh at 105 ℃ for 2 h.
Example 2
A cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh comprises the following steps:
1) the cathode mesh is flushed with pure water until the pH value of the solution reaches 8;
2) putting the cathode mesh into a citric acid solution with pH value of 1 for ultrasonic cleaning, wherein the ultrasonic power density is 0.3W/cm2Cleaning for 30 min;
3) washing the cathode mesh subjected to acid washing with pure water until the pH value of the solution reaches 8;
4) by using NiSO4·6H2O、FeSO4·7H2O、CoSO4·7H2O preparing a plating solution containing 0.24mol/L of Ni2+And at the same time contains 0.04mol/L Fe2+And 0.02mol/L of Co2+The electrodeposition voltage is-1.40V, and the electrodeposition time is 100 s;
5) placing the cathode plate which is re-loaded with the catalytic layer in a high-temperature furnace at 500 ℃ for calcining for 2 h;
6) the calcined cathode mesh is placed in 30 percent potassium hydroxide solution for cleaning, and the bubbling strength is 10mL/cm2The cleaning time is 30 min;
7) washing the cathode mesh subjected to alkali liquor bubbling cleaning with pure water until the pH value of the solution is 7;
8) and drying the cathode mesh at 105 ℃ for 2 h.
Example 3
A cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh comprises the following steps:
1) the cathode mesh is flushed with pure water until the pH value of the solution reaches 7;
2) putting the cathode mesh into oxalic acid solution with pH value of 1 for ultrasonic cleaning, wherein the ultrasonic power density is 0.3W/cm2Cleaning for 30 min;
3) washing the cathode mesh subjected to acid washing with pure water until the pH value of the solution reaches 7;
4) by using NiSO4·6H2O、FeSO4·7H2O、CoSO4·7H2O preparing a plating solution containing 0.38mol/L of Ni2+And at the same time contains 0.08mol/L of Fe2+And 0.04mol/L of Co2+The electrodeposition voltage is-1.4V, and the electrodeposition time is 100 s;
5) placing the cathode plate which is re-loaded with the catalytic layer in a high-temperature furnace at 500 ℃ for calcining for 2 h;
6) the calcined cathode mesh is placed in 30 percent potassium hydroxide alkali liquor for cleaning, and the bubbling strength is 10mL/cm2The cleaning time is 30 min;
7) washing the cathode mesh subjected to alkali liquor bubbling cleaning with pure water until the pH value of the solution is 7;
8) and drying the cathode mesh at 105 ℃ for 2 h.
Example 4
A cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh comprises the following steps:
1) the cathode mesh is flushed with pure water until the pH value of the solution reaches 7;
2) the cathode mesh was placed at pH ═1, ultrasonic cleaning is carried out in citric acid solution with the ultrasonic power density of 0.5W/cm2Cleaning for 10 min;
3) washing the cathode mesh subjected to acid washing with pure water until the pH value of the solution reaches 7;
4) by using NiSO4·6H2O、FeSO4·7H2O preparing electroplating solution containing 0.08mol/L Ni2+And at the same time contains 0.02mol/L of Fe2+The electrodeposition voltage is-1.4V, and the electrodeposition time is 100 s;
5) placing the cathode plate which is re-loaded with the catalytic layer in a high-temperature furnace at 600 ℃ for calcining for 0.5 h;
6) the calcined cathode mesh is placed in 30 percent potassium hydroxide alkali liquor for cleaning, and the bubbling strength is 100mL/cm2The cleaning time is 10 min;
7) washing the cathode mesh subjected to alkali liquor bubbling cleaning with pure water until the pH value of the solution is 7;
8) and drying the cathode mesh at 110 ℃ for 2 h.
Example 5
A cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh comprises the following steps:
1) the cathode mesh is flushed with pure water until the pH value of the solution reaches 7;
2) putting the cathode mesh into a citric acid solution with pH value of 1 for ultrasonic cleaning, wherein the ultrasonic power density is 0.5W/cm2Cleaning for 10 min;
3) washing the cathode mesh subjected to acid washing with pure water until the pH value of the solution reaches 7;
4) by using NiSO4·6H2O、FeSO4·7H2O preparing a plating solution containing 0.38mol/L of Ni2+And at the same time contains 0.08mol/L of Fe2+The electrodeposition voltage is-1.4V, and the electrodeposition time is 100 s;
5) placing the cathode plate which is re-loaded with the catalytic layer in a high-temperature furnace at 600 ℃ for calcining for 0.5 h;
6) the calcined cathode mesh is placed in 30 percent potassium hydroxide alkali liquor for cleaning, and the bubbling strength is 100mL/cm2Min, cleaningThe time is 10 min;
7) washing the cathode mesh subjected to alkali liquor bubbling cleaning with pure water until the pH value of the solution is 7;
8) and drying the cathode mesh at 110 ℃ for 2 h.
Example 6
A cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh comprises the following steps:
1) the cathode mesh is flushed with pure water until the pH value of the solution reaches 7;
2) putting the cathode mesh into a citric acid solution with pH value of 1 for ultrasonic cleaning, wherein the ultrasonic power density is 0.4W/cm2Cleaning for 20 min;
3) washing the cathode mesh subjected to acid washing with pure water until the pH value of the solution reaches 7;
4) by using NiSO4·6H2O、CoSO4·7H2O preparing electroplating solution containing 0.08mol/L Ni2+While containing 0.01mol/L of Co2+The electrodeposition voltage is-1.4V, and the electrodeposition time is 500 s;
5) placing the cathode plate which is re-loaded with the catalytic layer in a high-temperature furnace at 500 ℃ for calcining for 2 h;
6) the calcined cathode mesh is placed in 30 percent potassium hydroxide alkali liquor for cleaning, and the bubbling strength is 30mL/cm2The cleaning time is 30 min;
7) washing the cathode mesh subjected to alkali liquor bubbling cleaning with pure water until the pH value of the solution is 7;
8) and drying the cathode mesh at 105 ℃ for 2 h.
Example 7
A cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh comprises the following steps:
1) the cathode mesh is flushed with pure water until the pH value of the solution reaches 7;
2) putting the cathode mesh into a citric acid solution with pH value of 1 for ultrasonic cleaning, wherein the ultrasonic power density is 0.4W/cm2Cleaning for 20 min;
3) washing the cathode mesh subjected to acid washing with pure water until the pH value of the solution reaches 7;
4) by using NiSO4·6H2O、CoSO4·7H2O preparing a plating solution containing 0.38mol/L of Ni2+While containing 0.04mol/L of Co2+The electrodeposition voltage is-1.4V, and the electrodeposition time is 100 s;
5) placing the cathode plate which is re-loaded with the catalytic layer in a high-temperature furnace at 550 ℃ for calcining for 2 h;
6) the calcined cathode mesh is placed in 30 percent potassium hydroxide alkali liquor for cleaning, and the bubbling strength is 30mL/cm2The cleaning time is 30 min;
7) washing the cathode mesh subjected to alkali liquor bubbling cleaning with pure water until the pH value of the solution is 7;
8) and drying the cathode mesh at 105 ℃ for 2 h.
A2 cm × 2cm cathode mesh was cut out and placed in a KOH solution with a mass concentration of 30%, a 2cm × 2cm platinum mesh was used as a counter electrode, saturated calomel was used as a reference electrode, the hydrogen evolution overpotential of the cathode mesh was measured and compared with an unrenewed cathode mesh, and the results were as follows:
examples 1-7 demonstrate that the regenerated cathode mesh cleaned by the method of the present invention has hydrogen evolution overpotential significantly lower than that of the old cathode mesh, and can improve the hydrogen production efficiency in the hydrogen production process by water electrolysis.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
Claims (10)
1. A cleaning and regenerating method of an alkaline electrolysis hydrogen production cathode mesh is characterized by comprising the following steps:
1) washing the used cathode mesh with pure water, and then placing the cathode mesh in acid liquor for ultrasonic cleaning;
2) washing the cathode mesh after acid washing with pure water again, and soaking the cathode mesh in electroplating solution to load a catalytic layer; ni is contained in the plating solution2+And also contains Fe2+And Co2+One or two of them;
wherein Ni2+The concentration is (0.08-0.38) mol/L, Fe2+The concentration is (0.02-0.08) mol/L, Co2+Is the concentration (0.01-0.04) mol/L;
3) calcining the cathode mesh which is newly loaded with the catalytic layer;
4) placing the calcined cathode mesh in alkali liquor for bubbling cleaning;
5) and cleaning the cathode mesh cleaned by bubbling alkali liquor with pure water, and drying to obtain the cleaned and regenerated cathode mesh.
2. The method for cleaning and regenerating the cathode net for the alkaline electrolytic hydrogen production according to claim 1, characterized in that in the step 1), the solution is washed by pure water until the pH value is 7-8.
3. The method for cleaning and regenerating the cathode mesh for alkaline electrolytic hydrogen production according to claim 1, wherein in the step 1), citric acid or oxalic acid is adopted as the acid solution, and the pH value of the acid solution is 1-3.
4. The cleaning and regeneration method of the cathode mesh for alkaline electrolytic hydrogen production according to claim 1, characterized in that in step 1), the ultrasonic power density is 0.3-0.5W/cm2And the cleaning time is 5-30 min.
5. The method for cleaning and regenerating the cathode net for the alkaline electrolytic hydrogen production according to claim 1, characterized in that in the step 2), the solution is washed by pure water until the pH value is 6-7.
6. The cleaning and regeneration method of the alkaline electrolytic hydrogen production cathode mesh according to claim 1, characterized in that in step 2), the parameters of electroplating are as follows: the electro-deposition potential is-1.0 to-1.6V, and the electro-deposition time is 10 to 500 s.
7. The method for cleaning and regenerating the cathode net for hydrogen production by alkaline electrolysis as claimed in claim 1, wherein the calcination temperature in step 3) is 500-600 ℃, and the calcination time is 0.5-2 h.
8. The method for cleaning and regenerating the cathode mesh for hydrogen production by alkaline electrolysis as claimed in claim 1, wherein in the step 5), the alkali liquor is potassium hydroxide solution with the mass concentration of 10-30%.
9. The method for cleaning and regenerating the cathode net for the alkaline electrolytic hydrogen production according to claim 1, wherein in the step 5), the bubbling intensity aeration intensity is (10-100) mL/cm2The cleaning time is 10-60 min.
10. The method for cleaning and regenerating the cathode net for the alkaline electrolytic hydrogen production according to claim 1, characterized in that in the step 5), the pH of the solution in the washing with pure water is 7-8;
hot air drying is adopted, the drying temperature is 100-.
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Application publication date: 20211231 |