CN108855159B - Cobalt phosphide synthesized by prussian blue derivative and preparation method and application thereof - Google Patents
Cobalt phosphide synthesized by prussian blue derivative and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to cobalt phosphide synthesized by prussian blue derivatives, a preparation method and application thereof. The preparation method comprises the following steps: s1: mixing and stirring a dispersion stabilizer, potassium cobalt cyanide and cobalt salt, standing for reaction, washing and drying to obtain a Prussian blue derivative precursor; s2: heating the Prussian blue derivative precursor in the S1 to 350-450 ℃ at a heating rate of 1-5 ℃/min under the air condition, and roasting for 1-3 h to obtain cobaltosic oxide particles; s3: heating cobaltosic oxide particles and a phosphorus source to 285-350 ℃ at a heating rate of 1-5 ℃/min under the condition of inert gas, and roasting for 1-5 h to obtain the cobalt phosphide. The preparation method provided by the invention is simple and feasible, has good repeatability, and the used raw materials are cheap and easy to obtain, and the product is stable; the prepared cobalt phosphide has good electrocatalytic activity and conductivity and good catalytic performance on oxygen evolution reaction.
Description
Technical Field
The invention belongs to the field of water electrolysis, and particularly relates to cobalt phosphide synthesized by prussian blue derivatives, and a preparation method and application thereof.
Background
With the rapid development of industry, the energy problem faced by human beings is also more serious. Currently, most of our energy sources are from fossil fuels. However, the combustion of fossil fuels poses serious environmental problems. The electrolysis of water has great potential to provide a sustainable and clean source of hydrogen, which is considered to be the most promising new energy source to replace fossil fuels due to its excellent energy density and environmental friendliness. As an important component of water decomposition, the oxygen evolution reaction causes slow kinetics because it undergoes a complex four electron (4 e) transfer process, and research on oxygen evolution reaction catalysts has been increased in order to improve the efficiency of water decomposition. In particular, over the last years, considerable research efforts have focused on the development of non-noble metal catalysts (e.g., transition metal oxides, nitrides, carbides, etc.) rather than some of the high cost limited available catalysts, such as iridium (Ir) and ruthenium (Ru) oxides, which, despite their high catalytic activity for oxygen evolution reactions, have limited reserves, are expensive, and do not meet the mass production requirements for water electrolysis. Therefore, it is of great significance to explore a low-cost oxygen evolution reaction catalyst which can be applied on a large scale.
So far, some non-noble metal electrocatalysts with good electrochemical performance for oxygen evolution reactions have been reported, such as transition metal oxides, hydroxides, Layered Double Hydroxides (LDHs), sulfides, phosphates, and the like. Among the different oxygen evolution reaction electrocatalysts, the Transition Metal Phosphides (TMPs) recently reported are very promising not only because of their high abundance and low cost, but also because of their high alkali stability in alkaline solutions. The transition metal phosphide is a multifunctional material and is widely applied to the fields of energy conversion and storage, catalysts, magnetism, photoelectricity and the like. Recent studies have shown that certain transition metal phosphides (e.g., Ni)5P4And Fe2P), cobalt-based phosphide is not only a conventional hydrogen evolution reaction catalyst in the water decomposition process, but also a promising oxygen evolution reaction catalyst.
Recently, Prussian Blue Analogues (PBA) have been extensively studied as a new class of materials for energy-related applications such as batteries, supercapacitors or oxygen reduction reactions. Although the versatility and stability of prussian blue analogues in electrochemical processes are well explored, there are only a few examples of their application in the field of water oxidation. Cyanide-bridged materials have a poorer water-splitting activity than their metal oxides. In contrast, prussian blue analog-derived oxides, phosphides, selenides, carbides, etc. have been reported for oxygen evolution and hydrogen evolution reactions.
Therefore, the development of a preparation method with simple process to obtain the phosphide of the Prussian blue analogue with excellent oxygen evolution catalytic performance has important research significance and application value.
Disclosure of Invention
The invention aims to overcome the defect and the defect of poor activity of an oxygen evolution reaction catalyst in the prior art and provides a preparation method of cobalt phosphide synthesized by prussian blue derivatives. The preparation method provided by the invention is simple and feasible, has good repeatability, and the used raw materials are cheap and easy to obtain, and the product is stable; the prepared cobalt phosphide can fully exert the electrocatalytic activity of the cobalt phosphide material on oxygen evolution reaction and the good conductivity of the phosphide material, has good catalytic performance on the oxygen evolution reaction, and has 10mA/cm in the oxygen evolution reaction2The current density corresponds to a potential lower than 1.6000V vs.
The invention also aims to provide the cobalt phosphide prepared by the preparation method.
The invention also aims to provide the application of the cobalt phosphide as a catalyst in an oxygen evolution reaction.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing cobalt phosphide synthesized by prussian blue derivatives comprises the following steps:
s1: mixing and stirring a dispersion stabilizer, potassium cobalt cyanide and cobalt salt, standing for reaction, washing and drying to obtain a Prussian blue derivative precursor; the dispersion stabilizer is one or more of polyvinylpyrrolidone or sodium dodecyl benzene sulfonate; the molar ratio of the potassium cobalt cyanide to the cobalt salt is 1-2: 3;
s2: heating the Prussian blue derivative precursor in the S1 to 350-450 ℃ at a heating rate of 1-5 ℃/min under the air condition, and roasting for 1-3 h to obtain cobaltosic oxide particles;
s3: heating cobaltosic oxide particles and a phosphorus source to 285-350 ℃ at a heating rate of 1-5 ℃/min under the condition of inert gas, and roasting for 1-5 h to obtain cobalt phosphide; the molar ratio of the cobaltosic oxide particles to the phosphorus source is 1: 18-36.
The invention utilizes the dispersion stabilizer to promote the Prussian blue derivative precursor to be betterThe dispersion of (2) avoids agglomeration. The morphology of cobaltosic oxide is regulated and controlled, and the cobaltosic oxide is removed by roasting a dispersion stabilizer to form a porous morphology, so that the finally obtained cobalt phosphide has uniform morphology, is cubic-like particles and has good uniformity; moreover, the cobalt phosphide can fully exert the electrocatalytic activity of the conventional cobalt phosphide material without the Prussian blue analogue on oxygen evolution reaction and the good conductivity of phosphide material derived from the Prussian blue analogue, has good catalytic performance on the oxygen evolution reaction, and in the oxygen evolution reaction, 10mA/cm2The current density corresponds to a potential lower than 1.6000V vs.
The method provided by the invention is simple and easy to implement, good in repeatability, cheap and easily available in raw materials and stable in product.
Polyvinylpyrrolidone (such as polyvinylpyrrolidone with molecular weight of 40000-360000) which is conventional in the art can be used in the invention.
Preferably, the polyvinylpyrrolidone in S1 is one or more of polyvinylpyrrolidone 40000 or polyvinylpyrrolidone 360000.
Preferably, the cobalt salt in S1 is one or more of cobalt sulfate, cobalt nitrate or cobalt acetate.
Preferably, the molar ratio of the potassium cobalt cyanide to the cobalt salt in S1 is 1: 2.
Preferably, the temperature of the standing reaction in S1 is 25-80 ℃, and the time is 18-30 h.
Preferably, the washing process in S1 is washing with deionized water and ethanol in sequence, and centrifuging to neutrality; the drying temperature in S1 is 60 ℃, and the drying time is 12 h.
The dosage of the dispersion stabilizer is based on the realization of uniform dispersion of the potassium cobalt cyanide and the cobalt salt. Generally, when the mass of the dispersion stabilizer is 0.2g to 0.5g, the dispersion stabilizer can be dispersed well.
Preferably, the mixture is roasted for 1h after the temperature is raised to 350 ℃ at the temperature raising rate of 1 ℃/min in S2.
Preferably, the phosphorus source in S3 is one or both of sodium hypophosphite or diammonium phosphate.
Preferably, the molar ratio of the cobaltosic oxide particles to the phosphorus source in S3 is 1: 36.
Preferably, the mixture is roasted for 1h in S3 after the temperature is raised to 285 ℃ at the temperature raising rate of 1 ℃/min.
The invention also claims cobalt phosphide synthesized by the prussian blue derivative, and the cobalt phosphide is obtained by any preparation method.
Preferably, the shape of the cobalt phosphide is similar to a cubic particle, and the particle size is 100-200 nm.
The use of the cobalt phosphide as a catalyst in oxygen evolution reactions is also within the scope of the present invention.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method provided by the invention is simple and feasible, has good repeatability, and the used raw materials are cheap and easy to obtain, and the product is stable; the prepared cobalt phosphide can fully exert the electrocatalytic activity of the cobalt phosphide material on oxygen evolution reaction and the good conductivity of the phosphide material, has good catalytic performance on the oxygen evolution reaction, and has 10mA/cm in the oxygen evolution reaction2The current density corresponds to a potential lower than 1.6000V vs.
Drawings
FIG. 1 is an XRD pattern of cobalt phosphide synthesized with a Prussian blue derivative as provided in example 1;
FIG. 2 is an SEM image of cobalt phosphide synthesized from a Prussian blue derivative at a magnification of 30K as provided in example 1;
FIG. 3 is an SEM image of cobalt phosphide synthesized from Prussian blue derivatives provided in example 1 at a magnification of 50K;
fig. 4 is a graph showing the performance of cobalt phosphide synthesized with prussian blue derivative as an oxygen evolution catalyst in example 1 for catalyzing oxygen evolution.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specific conditions noted in the examples below, generally according to conditions conventional in the art or as suggested by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Example 1
This example provides a cobalt phosphide synthesized from a prussian blue derivative, which can be used as an oxygen evolution reaction catalyst and prepared as follows.
Uniformly mixing 0.3g of polyvinylpyrrolidone 360000 and 0.04mmol of potassium cobalt cyanide in 50ml of deionized water, dispersing 0.08mmol of cobalt acetate in 50ml of deionized water, uniformly mixing the above solution in a beaker, standing for 18h at 25 ℃, centrifugally washing with deionized hydrated ethanol, and drying at constant temperature for 24h at 60 ℃ to obtain the Prussian blue derivative precursor.
And (3) putting 200mg of the Prussian blue derivative precursor into a muffle furnace, heating to 350 ℃ at the rate of 1 ℃/min under the air condition, keeping the temperature for 1h, and cooling to room temperature to obtain the cobaltosic oxide particles.
Respectively placing 0.10g of cobaltosic oxide particles and 1.58g of sodium hypophosphite into a lower airflow part and an upper airflow part of a tubular furnace, heating to 285 ℃ at the rate of 1 ℃/min under the condition of inert gas, keeping the temperature for 1h, and cooling to room temperature to obtain the cobalt phosphide material.
The obtained prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst was analyzed by X-ray diffraction characterization, and the result is shown in fig. 1, where fig. 1 is an XRD chart of the prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst prepared in example 1. From FIG. 1, it can be seen that the product obtained by the preparation method is matched with a cobalt phosphide standard card, thereby proving that the obtained catalyst is a Prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst.
Scanning electron microscope scanning analysis was performed on the obtained prussian blue analog-derived cobalt phosphide oxygen evolution reaction catalyst, and the results are shown in fig. 2 and fig. 3, and fig. 2 is an SEM image of the prussian blue analog-derived cobalt phosphide oxygen evolution reaction catalyst prepared in example 1 at a magnification of 30K. FIG. 3 is an SEM photograph of a Prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst prepared in example 1 at a magnification of 50K. From the figures 2 and 3, it can be seen that the prussian blue analogue-derived cobalt phosphide oxygen precipitation reaction catalyst is uniform in morphology, all particles are particles, and the particle size is 100-200 nm, which indicates that the prussian blue analogue-derived cobalt phosphide oxygen precipitation reaction catalyst prepared by the method has better uniformity.
The catalytic activity of the obtained prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst was examined, and the result is shown in fig. 4, where fig. 4 is a graph showing the performance of catalytic oxygen evolution of the prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst prepared in example 1. As can be seen from FIG. 4, the Prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst had a concentration of 10mA/cm2The potential corresponding to the current density is 1.5700V vs. RHE, which shows that the cobalt phosphide oxygen evolution reaction catalyst synthesized by the prussian blue derivative has better catalytic performance for catalyzing oxygen evolution.
Example 2
This example provides a cobalt phosphide synthesized from a prussian blue derivative, prepared as follows.
Uniformly mixing 0.5g of polyvinylpyrrolidone 40000 and 0.04mmol of potassium cobalt cyanide in 50ml of deionized water, dispersing 0.06mmol of cobalt sulfate in 50ml of deionized water, uniformly mixing the above solutions in a beaker, standing for 30h at 60 ℃, centrifugally washing with deionized hydrated ethanol, and drying at constant temperature for 24h at 60 ℃ to obtain the Prussian blue derivative precursor.
And (3) putting 200mg of the Prussian blue derivative precursor into a muffle furnace, heating to 350 ℃ at the rate of 1 ℃/min under the air condition, keeping the temperature for 1h, and cooling to room temperature to obtain the cobaltosic oxide particles.
Respectively placing 0.10g of cobaltosic oxide particles and 1.19g of diammonium phosphate into a lower airflow part and an upper airflow part of a tubular furnace, heating to 285 ℃ at a heating rate of 1 ℃/min under the condition of inert gas, keeping the temperature for 1h, and cooling to room temperature to obtain the cobalt phosphide material.
The catalytic performance of the obtained catalyst with better catalytic performance on catalytic oxygen evolution is detected, and the prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst is obtained10mA/cm2The current density corresponds to a potential of 1.5800V vs.
Example 3
This example provides a cobalt phosphide synthesized from a prussian blue derivative, prepared as follows.
Uniformly mixing 0.3g of polyvinylpyrrolidone 360000 and 0.04mmol of potassium cobalt cyanide in 50ml of deionized water, dispersing 0.12mmol of cobalt sulfate in 50ml of deionized water, uniformly mixing the above solution in a beaker, standing for 18h at 25 ℃, centrifugally washing with deionized hydrated ethanol, and drying at constant temperature for 24h at 60 ℃ to obtain the Prussian blue derivative precursor.
And (3) putting 200mg of the Prussian blue derivative precursor into a muffle furnace, heating to 450 ℃ at the rate of 5 ℃/min under the air condition, keeping the temperature for 5 hours, and cooling to room temperature to obtain the cobaltosic oxide particles.
Respectively placing 0.10g of cobaltosic oxide particles and 1.32g of sodium hypophosphite into a lower airflow part and an upper airflow part of a tubular furnace, heating to 350 ℃ at the rate of 5 ℃/min under the condition of inert gas, keeping the temperature for 5 hours, and cooling to room temperature to obtain the cobalt phosphide material.
The catalytic performance of the obtained catalyst with better catalytic performance on catalytic oxygen evolution is detected, and the Prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst has 10mA/cm2The current density corresponds to a potential of 1.5750V vs.
Example 4
This example provides a cobalt phosphide synthesized from a prussian blue derivative, prepared as follows.
Uniformly mixing 0.5g of sodium dodecyl benzene sulfonate and 0.04mmol of potassium cobalt cyanide in 50ml of deionized water, dispersing 0.06mmol of cobalt nitrate in 50ml of deionized water, uniformly mixing the above solutions in a beaker, standing for 30h at 60 ℃, centrifugally washing with deionized hydrated ethanol, and drying at constant temperature for 24h at 60 ℃ to obtain the precursor of the prussian blue derivative.
And (3) putting 200mg of the Prussian blue derivative precursor into a muffle furnace, heating to 450 ℃ at the rate of 5 ℃/min under the air condition, keeping the temperature for 5 hours, and cooling to room temperature to obtain the cobaltosic oxide particles.
Respectively placing 0.10g of cobaltosic oxide particles and 1.06g of diammonium phosphate into a lower airflow part and an upper airflow part of a tubular furnace, heating to 350 ℃ at a heating rate of 5 ℃/min under the condition of inert gas, keeping the temperature for 5 hours, and cooling to room temperature to obtain the cobalt phosphide material.
The catalytic performance of the obtained catalyst with better catalytic performance on catalytic oxygen evolution is detected, and the Prussian blue analogue-derived cobalt phosphide oxygen evolution reaction catalyst has 10mA/cm2The current density corresponds to a potential of 1.5850V vs.
Claims (10)
1. A preparation method of cobalt phosphide oxygen evolution catalyst synthesized by prussian blue derivative is characterized by comprising the following steps:
s1: mixing and stirring a dispersion stabilizer, potassium cobalt cyanide and cobalt salt, standing for reaction, washing and drying to obtain a Prussian blue derivative precursor; the dispersion stabilizer is one or more of polyvinylpyrrolidone or sodium dodecyl benzene sulfonate; the molar ratio of the potassium cobalt cyanide to the cobalt salt is 1-2: 3;
s2: heating the Prussian blue derivative precursor in the S1 to 350-450 ℃ at a heating rate of 1-5 ℃/min under the air condition, and roasting for 1-3 h to obtain cobaltosic oxide particles;
s3: heating cobaltosic oxide particles and a phosphorus source to 285-350 ℃ at a heating rate of 1-5 ℃/min under the condition of inert gas, and roasting for 1-5 h to obtain cobalt phosphide; the molar ratio of the cobaltosic oxide particles to the phosphorus source is 1: 18-36.
2. The preparation method according to claim 1, wherein the polyvinylpyrrolidone in S1 is one or more of polyvinylpyrrolidone 40000 or polyvinylpyrrolidone 360000.
3. The preparation method of claim 1, wherein the cobalt salt in S1 is one or more of cobalt sulfate, cobalt nitrate and cobalt acetate.
4. The method according to claim 1, wherein the molar ratio of the potassium cobalt cyanide to the cobalt salt in S1 is 1: 2.
5. The method according to claim 1, wherein the step of S2 is carried out by heating to 350 ℃ at a heating rate of 1 ℃/min and then calcining for 1 hour.
6. The method according to claim 1, wherein the phosphorus source in S3 is one or both of sodium hypophosphite and diammonium phosphate.
7. The method according to claim 1, wherein the molar ratio of the tricobalt tetroxide particles to the phosphorus source in S3 is 1: 36.
8. The method according to claim 1, wherein the step of S3 is carried out by baking for 1h after the temperature is raised to 285 ℃ at a rate of 1 ℃/min.
9. Cobalt phosphide synthesized by prussian blue derivatives, which is obtained by the preparation method according to any one of claims 1 to 8.
10. Use of the cobalt phosphide of claim 9 as a catalyst in an oxygen evolution reaction.
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| CN109985648A (en) * | 2019-04-15 | 2019-07-09 | 安徽大学 | Porous cubic double-metal phosphide catalyst of one kind and its preparation method and application |
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