CN109926095B - Cobalt-based oxygen evolution catalyst based on eutectic solvent, preparation method and electrocatalytic oxygen evolution application thereof - Google Patents
Cobalt-based oxygen evolution catalyst based on eutectic solvent, preparation method and electrocatalytic oxygen evolution application thereof Download PDFInfo
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Abstract
The invention provides a cobalt-based oxygen evolution catalyst based on a eutectic solvent, a preparation method and an electrocatalytic oxygen evolution application thereof. The preparation method of the catalyst comprises the following steps: (1) mixing cobalt chloride hexahydrate and urea, stirring at 70-90 ℃ to obtain an eutectic solvent, reacting the eutectic solvent at 150-200 ℃, cooling to room temperature after the reaction is finished, and washing and drying the obtained solid to obtain a cobalt-ammonia complex; (2) modifying the cobalt-ammonia complex obtained in the step (1) on the foamed nickel, activating the nickel by utilizing a timing current method, and obtaining the cobalt-based oxygen evolution catalyst on the surface of the foamed nickel. The cobalt-based oxygen evolution catalyst obtained by the invention is in a flaky shape, and has excellent oxygen evolution catalytic performance and excellent stability. The cobalt-based oxygen evolution catalyst is prepared by using the eutectic solvent, and the preparation method is simple in preparation process, low in cost, green and environment-friendly and suitable for large-scale production.
Description
Technical Field
The invention relates to a cobalt-based oxygen evolution catalyst based on a eutectic solvent, a preparation method and an electrocatalytic oxygen evolution application thereof, belonging to the field of energy materials.
Background
Hydrogen is a novel clean energy, can replace traditional fossil energy, alleviates the energy shortage and environmental pollution scheduling problem. There are many sources of hydrogen, among which electrocatalytic water cracking, which comprises two half-reactions, a hydrogen evolution reaction and an oxygen evolution reaction, is one of the important methods for preparing hydrogen. Among them, the oxygen evolution reaction mechanism is complex, the electrode overpotential required is large, and much electric energy is consumed, and in order to reduce the overpotential of the oxygen evolution reaction, we need to synthesize an oxygen evolution catalyst. Among the commonly used oxygen evolution catalysts at present, noble metal catalysts represented by rhodium metal catalysts and iridium metal catalysts have the highest catalytic activity and the best stability, but due to the scarce reserves and the high price, the noble metal catalysts cannot be applied to large-scale industrial production. Therefore, a low-cost and high-efficiency oxygen evolution catalyst is urgently needed.
Transition metals such as cobalt, nickel and iron have good catalytic activity because of containing unfilled d-orbitals and unpaired electrons,therefore, the transition metal catalyst is a good substitute of a noble metal catalyst, and is expected to put the electrocatalytic water cracking hydrogen production into large-scale industrial production. Among them, cobalt-based catalysts, as a class of transition metal catalysts, exhibit good catalytic performance. For example, chinese patent document CN107308958A provides a method for preparing an electrochemical catalyst for oxygen evolution reaction, which comprises the following steps: 1) adding cobalt salt and a nonionic surfactant polymer into water, uniformly stirring, adding hydrazine hydrate, incubating under a hydrothermal condition to obtain lamellar cobalt hydroxide, 2) adding the obtained lamellar cobalt hydroxide and thiomolybdate into N, N-dimethylformamide, performing ultrasonic dispersion and mixing, then pyrolyzing the thiomolybdate under a solvothermal condition, and obtaining an amorphous molybdenum sulfide layer on the surface of a lamellar substrate. However, the oxygen evolution catalyst obtained by the method is 10mA/cm2The overpotential of the current density of the transformer can reach more than 350mV, and the overpotential of the current density of the transformer is higher and consumes more electric energy. Chinese patent document CN107486233A discloses a preparation method of a carbon nitride-doped carbon-based cobalt oxide nano-catalyst, which mainly comprises the steps of blending raw materials for preparing MOF and an alkaline solution of dicyandiamide to prepare gel, separating the gel to prepare MOF @ dicyandiamide nanocrystals, and heating the crystals in an air atmosphere to prepare the carbon nitride-doped carbon-based cobalt oxide nano-catalyst. However, the preparation method is relatively complex and has high cost.
Therefore, in order to reduce the cost of industrial production of hydrogen by water cracking, the synthesized cobalt-based catalyst needs to have the following characteristics: (1) the synthetic method is simple and convenient, has low cost and no pollution and toxicity; (2) the surface area of the catalyst should be as large as possible to expose more catalytic sites and enhance the catalytic activity, which requires that the synthesized catalyst should be in a sheet shape or other structure with large specific surface area. However, most of the currently reported cobalt-based catalysts cannot take the above two points into consideration, which greatly limits the application of the electrocatalytic water cracking industrialization.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a cobalt-based oxygen evolution catalyst based on a eutectic solvent, a preparation method and an electrocatalytic oxygen evolution application thereof. The preparation method of the invention has low cost and is simple and convenient, and accords with the atomic economic theory of green chemistry.
The technical scheme of the invention is as follows:
a cobalt-based oxygen evolution catalyst based on a eutectic solvent, the catalyst is prepared in the eutectic solvent consisting of cobalt chloride hexahydrate and urea; the catalyst is in a sheet shape, and the particle size is 400-600 nm.
According to the invention, the preparation method of the cobalt-based oxygen evolution catalyst based on the eutectic solvent comprises the following steps:
(1) mixing cobalt chloride hexahydrate and urea, stirring at 70-90 ℃ to obtain a eutectic solvent, and reacting the eutectic solvent at 150-200 ℃; after the reaction is finished, cooling to room temperature, washing and drying the obtained solid to obtain a cobalt-ammonia complex;
(2) modifying the cobalt-ammonia complex obtained in the step (1) on the foamed nickel, activating the nickel by utilizing a timing current method, and obtaining the cobalt-based oxygen evolution catalyst on the surface of the foamed nickel.
According to the preparation method of the invention, the molar ratio of the cobalt chloride hexahydrate and the urea in the step (1) is preferably 1 (2-4), and more preferably 1 (3.5-4).
According to the preparation method of the invention, preferably, the stirring temperature in the step (1) is 80 ℃, and the stirring time is 4-10 min.
According to the preparation method of the present invention, preferably, the reaction temperature in the step (1) is 180 ℃; the reaction time is 18 to 24 hours, and more preferably 21 hours.
According to the production method of the present invention, preferably, the reaction in the step (1) is a high-temperature reaction carried out in a closed vessel.
According to the preparation method of the present invention, preferably, the washing in the step (1) is 3 times with anhydrous ethanol; the drying is vacuum drying at 30-40 deg.C for 10-30 h.
According to the invention, the cobalt-ammonia complex obtained in the step (1) is porous and flaky, and the size of the pores is 30-100 nm.
According toIn the preparation method of the present invention, preferably, the modification step in the step (2) is: uniformly mixing the cobalt-ammonia complex obtained in the step (1) with absolute ethyl alcohol, distilled water and 5 wt% of Nafion reagent to prepare suspension, and modifying the suspension on foamed nickel, wherein the modification amount of the cobalt-ammonia complex is 0.4-0.6mg/cm2；
More preferably, the volume ratio of the mass of the cobalt-ammonia complex to the absolute ethyl alcohol is (8-12):1mg/mL, and the volume ratio of the absolute ethyl alcohol, the distilled water and the Nafion reagent is 1:1: 0.08.
According to the preparation method of the present invention, preferably, the condition of chronoamperometry described in the step (2) is: the NiCuk electrochemical counter electrode is characterized in that a Chenghua CHI 760E electrochemical workstation is utilized, foamed nickel modified with a cobalt-ammonia complex is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a carbon rod is used as a counter electrode, a 1mol/L KOH solution is used as electrolyte, and the voltage applied by a chronoamperometry method is 1.56V.
According to the preparation method of the present invention, it is preferable that the activation time in the step (2) is 20 to 24 hours, and it is further preferable that 22 hours.
According to the invention, the application of the cobalt-based oxygen evolution catalyst based on the eutectic solvent in electrocatalytic oxygen evolution is applied to electrocatalytic water cracking oxygen evolution; preferably, the catalyst is used as a water cracking oxygen evolution catalyst and applied to photoelectrocatalysis, an alkaline hydrolysis hydrogen generator or an APE hydrolysis battery.
The invention has the following technical characteristics and beneficial effects:
1. according to the invention, a cobalt source and urea are mixed to obtain a eutectic solvent, then the eutectic solvent is heated to react to obtain a cobalt-ammonia complex, and the cobalt-ammonia complex is activated by a chronoamperometry to obtain the cobalt-based catalyst. The invention has the advantages of cheap and easily obtained raw materials, simple preparation process, low cost, environmental protection and suitability for large-scale production.
2. The invention uses the synthesized eutectic solvent as all reactants, and the cobalt ammonia complex obtained after heating can be used for electrocatalytic oxygen evolution, thereby conforming to the atomic economy theory of green chemistry.
3. The prepared eutectic solvent has a template effect, can regulate and control the morphological growth of the catalyst, promotes the catalyst to form a flaky morphology, and can improve the electrochemical oxygen evolution performance of the catalyst.
4. The flaky cobalt-based oxygen evolution catalyst prepared by the invention has excellent performance of catalyzing electrolyzed water to evolve oxygen, is applied to catalyzing electrolyzed water to evolve oxygen, has high activity, and is proved by experiments to have the current density of 10mA/cm2When the catalyst is used, the required overpotential is only 291mV, which indicates that the catalytic activity is higher; and experiments prove that the catalyst prepared by the invention has excellent stability.
Drawings
FIG. 1 is an X-ray diffraction pattern of the cobalt ammine complex prepared in example 1.
FIG. 2 is an X-ray diffraction pattern of the cobalt-based oxygen evolution catalyst prepared in example 1.
FIG. 3 is a TEM image of the cobalt ammine complex prepared in example 1, wherein a is a TEM image of the low magnification cobalt ammine complex and b is a TEM image of the high magnification cobalt ammine complex.
Fig. 4 is a transmission electron micrograph of the cobalt-based oxygen evolution catalyst prepared in example 1, wherein a is a transmission electron micrograph of a low magnification cobalt-based oxygen evolution catalyst, and b is a transmission electron micrograph of a high magnification cobalt-based oxygen evolution catalyst.
FIG. 5 is a graph showing the oxygen evolution performance of catalytic electrolyzed water of the cobalt ammonia complex and the cobalt-based oxygen evolution catalyst prepared in example 1.
FIG. 6 is a graph showing the stability of oxygen evolution from catalytic electrolyzed water of the cobalt-based oxygen evolution catalyst prepared in example 1.
FIG. 7 is a graph showing a test of oxygen evolution performance by catalytic electrolysis of water of the cobalt-based oxygen evolution catalyst prepared in comparative example 1.
Detailed Description
The present invention will be further described with reference to the following examples, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A preparation method of a cobalt-based oxygen evolution catalyst based on a eutectic solvent comprises the following steps:
(1) mixing 1.19g of cobalt chloride hexahydrate and 1.10g of urea in a beaker, stirring for 5min in a water bath at 80 ℃ to obtain a blue eutectic solvent, transferring the blue eutectic solvent into a reaction kettle, and reacting for 21h at 180 ℃; after the reaction is finished, putting the reaction kettle into cold water to be cooled to room temperature to obtain a reddish brown solid product; washing the obtained solid product with absolute ethyl alcohol for 3 times, then putting the solid product into a vacuum drying oven, and drying the solid product for 24 hours at the temperature of 30 ℃ to obtain a cobalt-ammonia complex;
(2) uniformly mixing the cobalt-ammonia complex obtained in the step (1) with absolute ethyl alcohol, distilled water and 5 wt% of Nafion reagent to prepare suspension, and modifying the suspension on foamed nickel, wherein the modification amount of the cobalt-ammonia complex is 0.5mg/cm2(ii) a The ratio of the mass of the cobalt-ammonia complex to the volume of the absolute ethyl alcohol is 10:1mg/mL, and the ratio of the volume of the absolute ethyl alcohol, the volume of the distilled water and the volume of the Nafion reagent is 1:1: 0.08; the cobalt-ammonia complex is activated for 22 hours by utilizing a Chenghua CHI 760E electrochemical workstation, taking foamed nickel modified with a cobalt-ammonia complex as a working electrode, a saturated calomel electrode as a reference electrode, a carbon rod as a counter electrode, 1mol/L KOH solution as electrolyte and a voltage applied by a timing current method of 1.56V, and a cobalt-based oxygen evolution catalyst is obtained on the surface of the foamed nickel.
The X-ray diffraction spectrum of the cobalt-ammonia complex prepared in this example is shown in FIG. 1, and it can be seen from FIG. 1 that the synthesized substance has good crystallinity, and the structural formula of the synthesized substance is [ Co (NH)3)4CO3]Cl。
The X-ray diffraction pattern of the cobalt-based oxygen evolution catalyst prepared in this example is shown in fig. 2, and it can be seen from fig. 2 that the cobalt-based oxygen evolution catalyst is an amorphous substance.
The transmission electron micrograph of the cobalt-ammonia complex prepared in this example is shown in fig. 3, and it can be seen from fig. 3 that the morphology of the obtained cobalt-ammonia complex is porous and flaky, and the size of the pores is 30-100 nm.
The transmission electron micrograph of the cobalt-based oxygen evolution catalyst prepared in the example is shown in fig. 4, and it can be seen from fig. 4 that the obtained cobalt-based oxygen evolution catalyst is flaky in morphology and has a particle size of about 500 nm.
The cobalt-ammonia complex and the cobalt-based oxygen evolution catalyst prepared in the embodiment are subjected to a test of the performance of oxygen evolution by catalytic electrolysis of water, and the specific method is as follows: the electrochemical workstation used was Chenhua CHI 760E, in which foamed nickel was used as the working electrode, a saturated calomel electrode as the reference electrode, a carbon rod as the counter electrode, and 1mol/L KOH solution as the electrolyte. The electrochemical test is carried out by applying a polarization curve, the voltage is 1.2-1.8V, and the scanning rate is 5 mV/s.
The used nickel foam working electrode was treated as follows:
a. placing the foamed nickel in 1mol/L hydrochloric acid, and carrying out ultrasonic treatment for 10min to remove surface oxides; then respectively carrying out ultrasonic treatment for 10min by using distilled water and absolute ethyl alcohol; vacuum drying at room temperature for 24 h.
b. Taking 5mg of the cobalt-based oxygen evolution catalyst prepared in the embodiment, uniformly mixing the cobalt-based oxygen evolution catalyst with 0.5mL of distilled water, 0.5mL of absolute ethyl alcohol and 40 muL of 5 wt% Nafion reagent, and carrying out ultrasonic treatment for 20min to prepare an electrode modification solution.
c. Uniformly coating the modifying solution on the surface of the foamed nickel, wherein the modifying amount of the cobalt-based oxygen evolution catalyst is 0.5mg/cm2。
The test chart of the oxygen evolution performance of the cobalt ammonia complex and the cobalt-based oxygen evolution catalyst prepared in the example in the case of catalytic electrolysis of water is shown in FIG. 5, and it can be seen from FIG. 5 that the current density is 10mA/cm2The overpotential of the cobalt-ammonia complex is 321mV, and the overpotential of the cobalt-based oxygen evolution catalyst is 291mV, which shows that the cobalt-based oxygen evolution catalyst prepared by the implementation method has higher catalytic performance.
The cobalt-based oxygen evolution catalyst prepared in the example is subjected to catalytic electrolysis of water for oxygen evolution for 12h, the catalytic stability is shown in figure 6, and as can be seen from figure 6, the current density is 15mA/cm2And the current density can be kept unchanged basically in 12h, which shows that the cobalt-based oxygen evolution catalyst prepared by the invention has stable performance.
Example 2
A preparation method of a cobalt-based oxygen evolution catalyst based on a eutectic solvent comprises the following steps:
(1) mixing 1.19g of cobalt chloride hexahydrate and 0.90g of urea in a beaker, stirring for 5min in a water bath at 80 ℃ to obtain a blue eutectic solvent, transferring the blue eutectic solvent into a reaction kettle, and reacting for 21h at 180 ℃; after the reaction is finished, putting the reaction kettle into cold water to be cooled to room temperature to obtain a reddish brown solid product; washing the obtained product with absolute ethyl alcohol for 3 times, then putting the product into a vacuum drying oven, and drying the product for 24 hours at the temperature of 40 ℃ to obtain a cobalt-ammonia complex;
(2) the procedure was as described in step (2) of example 1.
Example 3
A preparation method of a cobalt-based oxygen evolution catalyst based on a eutectic solvent comprises the following steps:
(1) mixing 1.19g of cobalt chloride hexahydrate and 1.10g of urea in a beaker, stirring for 5min in a water bath at 80 ℃ to obtain a blue eutectic solvent, transferring the blue eutectic solvent into a reaction kettle, and reacting for 21h at 150 ℃; after the reaction is finished, putting the reaction kettle into cold water to be cooled to room temperature to obtain a reddish brown solid product; washing the obtained product with absolute ethyl alcohol for 3 times, then putting the product into a vacuum drying oven, and drying the product for 24 hours at the temperature of 40 ℃ to obtain a cobalt-ammonia complex;
(2) the procedure was as described in step (2) of example 1.
Comparative example 1
A preparation method of a cobalt-based oxygen evolution catalyst comprises the following steps:
(1) mixing 1.19g of cobalt chloride hexahydrate and 1.10g of urea in a beaker, stirring for 5min in a water bath at 80 ℃ to obtain a blue eutectic solvent, transferring the blue eutectic solvent into a reaction kettle, and reacting for 10h at 180 ℃; after the reaction is finished, putting the reaction kettle into cold water to be cooled to room temperature to obtain a reddish brown solid product; washing the obtained product with absolute ethyl alcohol for 3 times, then putting the product into a vacuum drying oven, and drying the product for 24 hours at the temperature of 30 ℃ to obtain a cobalt-ammonia complex;
(2) the procedure was as described in step (2) of example 1.
The test chart of the oxygen evolution performance of the cobalt-based oxygen evolution catalyst prepared in the comparative example in the case of catalytic electrolysis of water is shown in FIG. 7, and it can be seen from FIG. 7 that the current density is 10mA/cm2Cobalt ammonia complexThe overpotential of the compound is 355mV, which is much higher than that of the compound in the embodiment 1, and the catalyst prepared by the invention can effectively reduce the overpotential and has higher catalytic electrolysis water oxygen evolution activity.
Comparative example 2
A preparation method of a cobalt-based oxygen evolution catalyst comprises the following steps:
1.46g of cobalt nitrate hexahydrate and 1.10g of urea were mixed in a beaker and stirred in a water bath at 80 ℃ for 5min, whereby a eutectic solvent was not obtained.
From the comparative example, it can be seen that the eutectic solvent can be prepared only by mixing the specific cobalt salt and urea, and further the oxygen evolution catalyst with excellent morphology and performance can be further prepared.
Claims (9)
1. A cobalt-based oxygen evolution catalyst based on a eutectic solvent is characterized in that the catalyst is prepared in the eutectic solvent consisting of cobalt chloride hexahydrate and urea; the catalyst is in a sheet shape, and the particle size is 400-600 nm;
the preparation method of the cobalt-based oxygen evolution catalyst based on the eutectic solvent comprises the following steps:
(1) mixing cobalt chloride hexahydrate and urea, stirring at 70-90 ℃ to obtain a eutectic solvent, and reacting the eutectic solvent at 150-200 ℃; after the reaction is finished, cooling to room temperature, washing and drying the obtained solid to obtain a cobalt-ammonia complex;
(2) modifying the cobalt-ammonia complex obtained in the step (1) on the foamed nickel, activating the nickel by utilizing a timing current method, and obtaining the cobalt-based oxygen evolution catalyst on the surface of the foamed nickel.
2. The cobalt-based oxygen evolution catalyst according to claim 1, wherein the molar ratio of cobalt chloride hexahydrate and urea in step (1) is 1 (2-4).
3. The cobalt-based oxygen evolution catalyst according to claim 1, wherein the stirring temperature in step (1) is 80 ℃ and the stirring time is 4-10 min.
4. The cobalt-based oxygen evolution catalyst according to claim 1, characterized in that the reaction temperature in step (1) is 180 ℃; the reaction time is 18-24 h.
5. The cobalt-based oxygen evolution catalyst according to claim 1, wherein the washing in step (1) is 3 times with anhydrous ethanol; the drying is vacuum drying at 30-40 deg.C for 10-30 h.
6. The cobalt-based oxygen evolution catalyst according to claim 1, wherein the modification step in step (2) is: uniformly mixing the cobalt-ammonia complex obtained in the step (1) with absolute ethyl alcohol, distilled water and 5 wt% of Nafion reagent to prepare suspension, and modifying the suspension on foamed nickel, wherein the modification amount of the cobalt-ammonia complex is 0.4-0.6mg/cm2(ii) a The ratio of the mass of the cobalt-ammonia complex to the volume of the absolute ethyl alcohol is (8-12):1mg/mL, and the ratio of the volume of the absolute ethyl alcohol, the volume of the distilled water and the volume of the Nafion reagent is 1:1: 0.08.
7. The cobalt-based oxygen evolution catalyst according to claim 1, wherein the chronoamperometric condition in the step (2) is: the NiCuk electrochemical counter electrode is characterized in that a Chenghua CHI 760E electrochemical workstation is utilized, foamed nickel modified with a cobalt-ammonia complex is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a carbon rod is used as a counter electrode, a 1mol/L KOH solution is used as electrolyte, and the voltage applied by a chronoamperometry method is 1.56V.
8. The cobalt-based oxygen evolution catalyst according to claim 1, characterized in that the activation time in step (2) is 20-24 h.
9. The application of the cobalt-based oxygen evolution catalyst based on eutectic solvent as claimed in claim 1 to electrocatalytic water-splitting oxygen evolution; the catalyst is used as a water splitting oxygen evolution catalyst and is applied to photoelectrocatalysis, an alkaline hydrolysis hydrogen generator or an APE hydrolysis battery.
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