Preparation method of novel hydrogen production catalyst for alkaline electrolytic cell

Abstract

The invention discloses a preparation method of a novel hydrogen production catalyst for a basic electrolytic cell. The preparation method comprises the following steps: 1, preparing raw materials; step 2, extracting materials; step 3, mixing and processing. Step 4, drying treatment; 5, detecting a finished product; wherein in the first step, transition metal elements, alkaline earth metal elements and rare earth elements are weighed according to the proportion, the transition metal elements, the alkaline earth metal elements and the rare earth elements are put into a ball milling tank, grinding balls are added into the ball milling tank, and a ball mill is started for grinding; and after grinding, the transition metal elements, the alkaline earth metal elements and the rare earth elements are separately stored in a dry and ventilated environment. According to the preparation method, by adjusting parameters such as the ratio of all elements in the mixture, the solvent type, the heat treatment temperature and time, the reduction treatment temperature and time and the like, the performance of the catalyst can be optimized, the hydrogen production efficiency of the alkaline electrolytic cell can be effectively improved, meanwhile, the preparation method is easy to operate, and industrial production is easy to achieve.

Description

Technical Field

[0001] The present invention relates to the technical field of hydrogen energy, and specifically to a preparation method of a novel hydrogen production catalyst for an alkaline electrolyzer. Background Art

[0002] With the increasing demand for clean energy in society, hydrogen energy, as an efficient and environmentally friendly energy form, has attracted more and more attention. The demand for hydrogen is increasing day by day. The alkaline electrolyzer is one of the current mainstream hydrogen production devices, and its performance is greatly affected by the catalyst. However, the existing hydrogen production catalysts for alkaline electrolyzers have problems such as low activity and poor stability, which restrict the development of hydrogen energy technology. Therefore, developing a novel hydrogen production catalyst for an alkaline electrolyzer and its preparation method has important practical significance and application value. Summary of the Invention

[0003] The purpose of the present invention is to provide a preparation method of a novel hydrogen production catalyst for an alkaline electrolyzer to solve the problems raised in the above background art.

[0004] To achieve the above purpose, the present invention provides the following technical solution: A preparation method of a novel hydrogen production catalyst for an alkaline electrolyzer, including Step 1, raw material preparation; Step 2, material extraction; Step 3, mixing and processing; Step 4, drying treatment; Step 5, finished product detection;

[0005] In the above Step 1, the transition metal element, alkaline earth metal element, and rare earth element are weighed according to the proportion. The transition metal element, alkaline earth metal element, and rare earth element are respectively put into a ball milling tank, grinding balls are added to the ball milling tank, and the ball mill is started for grinding. After grinding, the materials of the transition metal element, alkaline earth metal element, and rare earth element are stored separately in a dry and ventilated environment;

[0006] In the above Step 2, 50 g of the transition metal element Fe, 30 g of the alkaline earth metal element Mg, and 20 g of the rare earth element Ce are respectively extracted from the materials of the transition metal element, alkaline earth metal element, and rare earth element and mixed according to the proportion to obtain mixture A;

[0007] In the above Step 3, the obtained mixture A is put into a high-pressure reaction kettle, an appropriate amount of solvent A is added, the high-pressure reaction kettle is sealed, and the mixture and solvent A are fully stirred and mixed by using the high-pressure reaction kettle, and reacted at a certain temperature for a certain time to obtain mixture B;

[0008] In the above Step 4, mixture B is put into an oven for drying treatment. After drying, mixture B is put into a high-temperature furnace for firing treatment. After firing treatment, mixture B is taken out of the high-temperature furnace for natural cooling treatment to obtain a catalyst solidified product;

[0009] In the above step five, the cooled catalyst solid is ground and screened to obtain a catalyst powder. The catalyst powder is characterized and analyzed. By means of scanning electron microscopy, transmission electron microscopy, etc., the morphology and particle size of the catalyst powder are observed, and its microstructure can be understood, and then its performance can be evaluated.

[0010] Preferably, the transition metal elements in step one can be selected from Fe, Co, etc., the alkaline earth metal elements can be selected from Mg, Ca, etc., and the rare earth elements can be selected from Ce, La and other materials.

[0011] Preferably, in the grinding process of step one, an appropriate amount of inhibitor is added to prevent chemical reactions between the grinding medium and the transition metal elements, alkaline earth metal elements and rare earth elements. The ground powder is screened and classified. The classified fine powder can be directly used, while the coarse particles need to be crushed and ground again.

[0012] Preferably, the solvent A in step three can be selected from common organic solvents such as water and ethanol, and the high-pressure reaction kettle is adjusted according to the specific material of the solvent A added.

[0013] Preferably, in step four, the mixture B is placed in a catalyst high-temperature furnace, and appropriate firing temperature and time are set. The heating system will provide the high temperature required by the furnace body, so that the carbonaceous substances and impurities on the surface of the mixture B are burned, decomposed or volatilized, thereby restoring the activity of the catalyst. The control system will monitor the temperature and atmosphere in the furnace and adjust according to the preset parameters to ensure the smooth progress of the firing process.

[0014] Preferably, in step five, the catalyst solid is put into a ball mill or a sand mill for grinding to refine the solid catalyst powder. The ground solid catalyst powder is screened, and catalyst powders with different particle sizes are selected according to needs.

[0015] Compared with the prior art, the beneficial effects of the present invention are:

[0016] The preparation method of the present invention is simple in operation and easy to realize industrial production. By adjusting parameters such as the ratio of each element in the mixture, the type of solvent, the heat treatment temperature and time, and the reduction treatment temperature and time, the performance of the catalyst can be optimized. At the same time, the catalyst of the present invention has the characteristics of high activity and high stability, can effectively improve the hydrogen production efficiency of the alkaline electrolytic cell, and has important practical value and broad market prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic flow chart of the method of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0018] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0019] In the description of the present invention, it should be noted that the orientation or positional relationship indicated by the terms "upper", "lower", "inner", "outer", "front end", "rear end", "both ends", "one end", "the other end", etc. is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as a limitation of the present invention. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0020] In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, the terms "installed", "provided with", "connected", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0021] Please refer to Figure 1 , an embodiment provided by the present invention:

[0022] Embodiment 1

[0023] A preparation method of a novel catalyst for hydrogen production in an alkaline electrolytic cell, including Step 1, raw material preparation; Step 2, material extraction; Step 3, mixing and processing; Step 4, drying treatment; Step 5, finished product detection;

[0024] In the above step 1, the transition metal element, alkaline earth metal element and rare earth element are weighed according to a ratio. The transition metal element, alkaline earth metal element and rare earth element are respectively placed into a ball milling jar, grinding balls are added into the ball milling jar, and the ball mill is started for grinding. After grinding, the materials of the transition metal element, alkaline earth metal element and rare earth element are respectively stored separately in a dry and ventilated environment; the transition metal element can be selected from Fe, Co, etc., the alkaline earth metal element can be selected from Mg, Ca, etc., and the rare earth element can be selected from Ce, La and other materials. During the grinding process, an appropriate amount of inhibitor is added to prevent chemical reactions between the grinding medium and the transition metal element, alkaline earth metal element and rare earth element. The ground powder is sieved and classified. The classified fine powder can be directly used, while the coarse particles need to be crushed and ground again;

[0025] In the above step 2, 50 g of the transition metal element Fe, 30 g of the alkaline earth metal element Mg and 20 g of the rare earth element Ce are respectively extracted from the materials of the transition metal element, alkaline earth metal element and rare earth element and mixed according to a ratio to obtain mixture A;

[0026] In the above step 3, the obtained mixture A is placed into a high-pressure reaction kettle, an appropriate amount of solvent A is added, the high-pressure reaction kettle is sealed, and the mixture and solvent A are fully stirred and mixed by using the high-pressure reaction kettle, and reacted at a certain temperature for a certain time to obtain mixture B; Solvent A can be selected from common organic solvents such as water and ethanol, and the high-pressure reaction kettle is adjusted according to the specific material of the specifically added solvent A;

[0027] In the above step 4, mixture B is placed into an oven for drying treatment. After drying, mixture B is placed into a high-temperature furnace for firing treatment. After the firing treatment, mixture B is taken out of the high-temperature furnace for natural cooling treatment to obtain a catalyst solidified product; Mixture B is placed in a catalyst high-temperature furnace, and appropriate firing temperature and time are set. The heating system will provide the high temperature required by the furnace body to burn, decompose or volatilize the carbonaceous substances and impurities on the surface of mixture B, thereby restoring the activity of the catalyst. The control system will monitor the temperature and atmosphere in the furnace and adjust according to the preset parameters to ensure the smooth progress of the firing process;

[0028] In the above step 5, the cooled catalyst solidified product is ground and sieved to obtain a catalyst powder. The catalyst powder is characterized and analyzed. By means of scanning electron microscopy (SEM) and transmission electron microscopy (TEM), etc., the morphology and particle size of the catalyst powder can be observed to understand its microstructure, and then its performance can be evaluated; The catalyst solidified product is placed into a ball mill or sand mill for grinding to refine the solid catalyst powder. The ground solid catalyst powder is sieved, and catalyst powders with different particle sizes are selected according to needs.

[0029] Example 2

[0030] (1) Mix 100 g of transition metal element Co, 50 g of alkaline earth metal element Ca, and 30 g of rare earth element La in proportion to obtain mixture C.

[0031] (2) Mix mixture C with 200 ml of ethanol to obtain mixture D.

[0032] (3) Place mixture D in an oven for drying treatment. After drying, place mixture D in a high-temperature furnace for firing treatment. After firing treatment, take mixture D out of the high-temperature furnace for natural cooling treatment to obtain a catalyst solidified product.

[0033] From the above two embodiments, it can be seen that the preparation method of the present invention is simple to operate and easy to realize industrial production. By adjusting parameters such as the ratio of each element in the mixture, the type of solvent, the heat treatment temperature and time, and the reduction treatment temperature and time, the performance of the catalyst can be optimized. At the same time, the catalyst of the present invention has the characteristics of high activity and high stability, can effectively improve the hydrogen production efficiency of the alkaline electrolyzer, and has important practical value and broad market prospects.

[0034] Those not elaborated in the present invention are all well-known technologies to those skilled in the art.

[0035] Finally, it should be noted that the above specific embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to the embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified and equivalently replaced without departing from the spirit and scope of the technical solutions of the present invention, and they should all be covered within the scope of the claims of the present invention.

Claims

1. Preparation method of a new hydrogen production catalyst for an alkaline electrolyzer, including Step 1, raw material preparation; Step 2, material extraction; Step 3, mixing and processing; Step 4, drying treatment; Step 5, finished product testing; characterized in that: In Step 1 above, transition metal elements, alkaline earth metal elements and rare earth elements are weighed according to proportions. The transition metal elements, alkaline earth metal elements and rare earth elements are respectively placed into a ball milling tank, grinding balls are added to the ball milling tank, and the ball mill is started for grinding. After grinding, the materials of the transition metal elements, alkaline earth metal elements and rare earth elements are stored separately in a dry and ventilated environment; In Step 2 above, 50 g of the transition metal element Fe, 30 g of the alkaline earth metal element Mg and 20 g of the rare earth element Ce are respectively extracted from the materials of the transition metal elements, alkaline earth metal elements and rare earth elements and mixed according to proportions to obtain mixture A; In Step 3 above, the obtained mixture A is put into a high-pressure reaction kettle, an appropriate amount of solvent A is added, the high-pressure reaction kettle is sealed, and the mixture and solvent A are fully stirred and mixed by using the high-pressure reaction kettle, and reacted at a certain temperature for a certain time to obtain mixture B; In Step 4 above, mixture B is put into an oven for drying treatment. After drying, mixture B is put into a high-temperature furnace for firing treatment. After firing treatment, mixture B is taken out of the high-temperature furnace for natural cooling treatment to obtain a catalyst solidified product; In Step 5 above, the cooled catalyst solidified product is ground and sieved to obtain a catalyst powder. The catalyst powder is subjected to characterization analysis. By means of a scanning electron microscope (SEM) and a transmission electron microscope (TEM), etc., the morphology and particle size of the catalyst powder can be observed, its microstructure can be understood, and its performance can be evaluated accordingly.

2. The preparation method of the novel hydrogen production catalyst for an alkaline electrolytic cell according to claim 1, characterized in that: The transition metal elements in Step 1 above can be selected from Fe, Co, etc., the alkaline earth metal elements can be selected from Mg, Ca, etc., and the rare earth elements can be selected from Ce, La, etc.

3. The preparation method of the novel hydrogen production catalyst for the alkaline electrolytic cell according to claim 1, characterized in that: In the grinding process of Step 1 above, an appropriate amount of inhibitor is added to prevent chemical reactions between the grinding medium and the transition metal elements, alkaline earth metal elements and rare earth elements. The ground powder is sieved and classified. The classified fine powder can be directly used, while the coarse particles need to be crushed and ground again.

4. The preparation method of the novel hydrogen production catalyst for the alkaline electrolytic cell according to claim 1, characterized in that: The solvent A in Step 3 above can be selected from common organic solvents such as water and ethanol, and the high-pressure reaction kettle is adjusted according to the specific material of the specifically added solvent A.

5. The preparation method of the novel hydrogen production catalyst for an alkaline electrolytic cell according to claim 1, wherein: In Step 4, mixture B is placed in a catalyst high-temperature furnace, and an appropriate firing temperature and time are set. The heating system will provide the high temperature required by the furnace body, so that the carbonaceous substances and impurities on the surface of mixture B are burned, decomposed or volatilized, thereby restoring the activity of the catalyst. The control system will monitor the temperature and atmosphere in the furnace and adjust according to the preset parameters to ensure the smooth progress of the firing process.

6. The preparation method of the novel hydrogen production catalyst for an alkaline electrolytic cell according to claim 1, wherein: In Step 5 above, the catalyst solidified product is put into a ball mill or a sand mill for grinding to refine the solid catalyst powder. The ground solid catalyst powder is sieved, and catalyst powders of different particle sizes are selected according to needs.

Images