CN113265672B - Preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide - Google Patents
Preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide Download PDFInfo
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Abstract
The invention discloses a preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide, which comprises the following specific steps: s1, mixing melamine and a formaldehyde aqueous solution, oscillating to obtain a clear prepolymer solution, pouring a mixture of cobalt salt and nickel salt into the prepolymer solution, oscillating to dissolve, preserving heat, and taking out the polymer after polymerization and solidification to obtain Co/Ni-MF; s2, calcining and carbonizing Co/Ni-MF in an inert atmosphere, and naturally cooling to room temperature in a protective gas atmosphere to obtain Co/Ni-NPC; s3, carrying out phosphating reaction on Co/Ni-NPC, cooling, washing and vacuum drying to obtain CoxPy/NixPy-NPC. The catalyst prepared by the method has the characteristics of uniform material, good catalytic activity and the like.
Description
Technical Field
The invention relates to the technical field of material science, in particular to a preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide.
Background
In the preparation process of the supported catalyst, improving the dispersion uniformity of the active components of the catalyst and realizing convenient adjustment of the components of the catalyst carrier are one of the key researches. Carbon is a common support component for supported catalysts. The conventional preparation of the supported solid catalyst mostly adopts methods such as an impregnation method, a mixing method and the like, and the problem of uniform mixing cannot be effectively solved. The catalyst prepared by adopting the precipitation method is also determined by the fact that the activated carbon carrier is easily distributed unevenly in the solution, and the like. The homogeneous reaction of gas phase and liquid phase can solve the problem of inhomogeneous matter effectively and is one promising development direction.
Due to its stable chemistry, carbon is hardly soluble in all solvents and the preparation of carbon from suitable precursors, especially liquids, is one direction to solve this problem. One method is to use liquid polymer monomer to solidify and polymerize into solid polymer, and then the polymer is carbonized to obtain carbon material. Homogeneous preparation of the supported catalyst can be achieved if the catalytically active component can be introduced into the system before the polymer has not cured.
In the field of the research of electrolytic water hydrogen evolution catalysts, transition metal phosphides such as: cobalt phosphide and nickel phosphide are catalyst active components with relatively excellent performance, and can be obtained by a simple substance cobalt or cobalt oxide in a phosphating reaction. In order to be able to introduce the metal element under liquid phase conditions, a metal organic complex may be used. However, complex preparation techniques are complex and expensive, which limits their large-scale application. It is more preferable if the inorganic cobalt salt can be directly introduced.
The conventional organic polymer system has poor solubility to inorganic metal salt, and the introduction of inorganic metal elements is restricted. There is a need to find liquid organic polymer systems that are capable of dissolving relatively large amounts of inorganic metal salts.
Therefore, in combination with the above problems, it is an urgent need to solve the problems of the art to provide a method for preparing cobalt phosphide/nickel phosphide supported on nitrogen-doped porous carbon.
Disclosure of Invention
In view of the above, the invention provides a preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide, which adopts a melamine-formaldehyde system, and the method comprises the steps of preparing a liquid-phase prepolymer through the melamine-formaldehyde system, dissolving inorganic metal salt to form an organic-inorganic homogeneous phase mixed substance, and polymerizing and curing to form a compound. The compound is carbonized to obtain a metal salt material loaded with carbon, and the material is subjected to gas-phase phosphating treatment to obtain the loaded cobalt phosphide/nickel phosphide catalytic material. The catalyst prepared by the method has the characteristics of uniform material, good catalytic activity and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide comprises the following specific steps:
s1, preparing melamine formaldehyde resin containing cobalt/nickel: mixing melamine and 35% -40% of formaldehyde aqueous solution, wherein the mass ratio of the melamine to the formaldehyde is 1: 6-40; oscillating the mixture at the set temperature of 50-90 ℃, reacting for 5-20 min to obtain clear prepolymer liquid, pouring the mixture of cobalt salt and nickel salt into the prepolymer liquid, wherein the ratio of the total amount of the cobalt salt and the nickel salt to the amount of melamine is 0.5-4: 1, oscillating and dissolving, keeping the temperature at 50-90 ℃, and taking out the polymer after polymerization and solidification to obtain Co/Ni-MF;
s2, preparing a nitrogen-doped porous carbon-loaded cobalt-nickel material: calcining Co/Ni-MF at 700-950 ℃ for 2-4 h in an inert atmosphere, carbonizing an organic component to obtain NPC, and naturally cooling to room temperature in a protective gas atmosphere to obtain Co/Ni-NPC;
s3, preparing nitrogen-doped porous carbon-supported CoP/NiP: placing a quartz boat loaded with Co/Ni-NPC in a tubular quartz furnace, placing the quartz boat in the downstream of phosphorus steam, driving the phosphorus steam to uniformly flow through the Co/Ni-NPC by inert gas flow to generate a phosphorization reaction at the temperature of 450-600 ℃, reacting for 1-2 h, setting the temperature rise rate to be 5 ℃/min, preserving heat for 1h, then cooling to 250-350 ℃, preserving heat for 2h, cooling to room temperature in inert gas, taking out, washing products twice by deionized water and ethanol respectively, and then drying in vacuum at the temperature of 60-80 ℃ to obtain CoxPy/NixPy-NPC。
Preferably, the cobalt salt and the nickel salt in step S1 are one of nitrate, sulfate, chloride, and organic acid salt, respectively.
Preferably, in step S1, urea and biuret may be added to the prepolymer solution to adjust the nitrogen content of the system, and the added amount is less than or equal to 30% of the total weight of the prepolymer solution.
Preferably, the tubular quartz furnace in step S3 may be replaced with an atmospheric furnace.
Preferably, the vapor source of the phosphorus vapor in the step S3 is red phosphorus or white phosphorus.
Preferably, the inert gas flow in the step S3 is Ar gas flow or N gas flow2Airflow, setting the airflow rate at 25 ℃ to 10-50 ml/min and the absolute pressure at 101 ℃115kPa。
A preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide specifically comprises the following steps:
s1, preparing the melamine formaldehyde resin containing cobalt: mixing melamine and 35% -40% of formaldehyde aqueous solution, wherein the mass ratio of the melamine to the formaldehyde is 1: 6-40; oscillating the mixture at the set temperature of 50-90 ℃, reacting for 5-20 min to obtain clear prepolymer liquid, pouring cobalt salt into the prepolymer liquid, wherein the mass ratio of the cobalt salt to the melamine is 0.5-4: 1, oscillating and dissolving, keeping the temperature at 50-90 ℃, and taking out the polymer after polymerization and solidification to obtain Co-MF;
s2, preparing a nitrogen-doped porous carbon-supported cobalt material: calcining Co-MF at 700-950 ℃ for 2-4 h in an inert atmosphere, carbonizing an organic component to obtain NPC, and naturally cooling to room temperature in a protective gas atmosphere to obtain Co-NPC;
s3, preparing nitrogen-doped porous carbon-supported CoP: placing a quartz boat loaded with Co-NPC in a tubular quartz furnace, placing the quartz boat in the downstream of phosphorus steam, driving the phosphorus steam to uniformly flow through the Co-NPC by inert gas flow to carry out a phosphorization reaction at the temperature of 450-600 ℃ for 1-2 h, setting the temperature rise rate to be 5 ℃/min, preserving heat for 1h, cooling to 250-350 ℃, preserving heat for 2h, cooling to room temperature in inert gas, taking out, washing products twice by deionized water and ethanol respectively, and carrying out vacuum drying at the temperature of 60-80 ℃ to obtain CoxPy-NPC。
A preparation method of nitrogen-doped porous carbon-loaded nickel phosphide comprises the following specific steps:
s1, preparing cobalt-containing melamine formaldehyde resin: mixing melamine and 35% -40% of formaldehyde aqueous solution, wherein the mass ratio of the melamine to the formaldehyde is 1: 6-40; oscillating the mixture at the set temperature of 50-90 ℃, reacting for 5-20 min to obtain clear prepolymer liquid, pouring nickel salt into the prepolymer liquid, wherein the mass ratio of the nickel salt to the melamine is 0.5-4: 1, oscillating and dissolving, keeping the temperature at 50-90 ℃, and taking out the polymer after polymerization and solidification to obtain Ni-MF;
s2, preparing a nitrogen-doped porous carbon supported nickel material: calcining the Ni-MF in an inert atmosphere at 700-950 ℃ for 2-4 h, carbonizing the organic component to obtain NPC, and naturally cooling to room temperature in a protective gas atmosphere to obtain Ni-NPC;
s3, preparing nitrogen-doped porous carbon-loaded NiP: placing a quartz boat loaded with Ni-NPC in a tubular quartz furnace, placing the quartz boat in the downstream of phosphorus steam, driving the phosphorus steam to uniformly flow through the Ni-NPC by inert gas flow to carry out a phosphorization reaction at the temperature of 450-600 ℃ for 1-2 h, setting the temperature rise rate to be 5 ℃/min, preserving heat for 1h, cooling to 250-350 ℃, preserving heat for 2h, cooling to room temperature in inert gas, taking out, washing products twice by deionized water and ethanol respectively, and carrying out vacuum drying at the temperature of 60-80 ℃ to obtain NixPy-NPC。
The chemical equation related to nitrate as an example in the invention is as follows:
2Ni(NO3)2·6H2O＝Ni2O3+2HNO3+2NO2+11H2O (1)
6Ni2O3＝4Ni3O4+O2 (2)
2Ni3O4＝6NiO+O2 (3)
2Co(NO3)2·6H2O＝2Co2O3+N2O4+N2O5+12H2O (4)
3Co(NO3)2·6H2O＝Co3O4+N2O4+2N2O5+18H2O (5)
NiO+CO＝Ni+CO2 (6)
Co2O3+3CO＝2Co+3CO2 (7)
Co3O4+4CO＝3Co+4CO2 (8)
by adopting the technical scheme, the invention has the following beneficial effects:
the invention discloses a method for preparing nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide by three steps, which comprises the steps of firstly synthesizing a polymer containing metal salt, wherein inorganic metal salt is difficult to dissolve in a polymer solvent system; and then calcining the mixture at 700-950 ℃ for 2-4 h in an inert atmosphere, converting the MF resin into carbon with a porous structure, simultaneously, reserving a large amount of N elements doped in the MF resin in the carbon material to form an N-doped carbon material, decomposing metal salt in the polymer into metal oxide in the inert atmosphere, and reducing the metal oxide into a metal simple substance by MF resin pyrolysis gas (containing carbon monoxide) at high temperature to obtain Co-NPC or Ni-NPC or Co/Ni-NPC, and carrying out gas-solid reaction on the Co-NPC or Ni-NPC or Co/Ni-NPC in phosphorus steam to obtain the target metal phosphide. Because the metal salt can be uniformly dispersed in the prepolymer, the metal can be well dispersed on the N-doped porous carbon. The invention has the advantages of uniform sample distribution in the whole preparation process, no solvent and little pollution of the synthesis process.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required in the description of the embodiments are briefly introduced below, the drawings in the description below are merely the embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is an XRD spectrum of cobalt phosphide/nickel phosphide supported on nitrogen-doped porous carbon according to the present invention;
FIG. 2 is an XRD spectrum of cobalt phosphide supported on nitrogen-doped porous carbon according to the present invention;
FIG. 3 is an XRD spectrum of nickel phosphide supported on nitrogen-doped porous carbon in accordance with the present invention;
FIG. 4 shows the invention of CoxPy/NixPy-NPC、CoxPy-NPC and NixPyComparison of the LSV curves of NPC and Pt/C (both measured in 1mol/L aqueous KOH at room temperature).
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment 1 of the invention discloses a preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide, which adopts the following technical scheme:
s1, preparing melamine formaldehyde resin containing cobalt/nickel: mixing 4.0mmol melamine and 28mmol 37% formaldehyde solution in a test tube, reacting at 60 deg.C for 10min, shaking for several times until clear prepolymer solution is obtained, and adding 2.0mmol Co (NO)3)2·6H2O and 2.0mmol of Ni (NO)3)2·6H2Pouring the powder mixture of O into the prepolymer liquid, shaking to dissolve, and keeping the temperature at 60 ℃ until a solid polymer is formed. Taking out after polymerization and solidification to obtain a compound of melamine formaldehyde resin (MF) and inorganic metal salt, namely Co/Ni-MF;
s2, preparing a nitrogen-doped porous carbon-loaded cobalt-nickel material: Co/Ni-MF in N2Calcining at 800 deg.C for 2h under constant temperature, carbonizing organic component to obtain porous carbon material (NPC), and calcining in N2Naturally cooling to room temperature in the atmosphere to obtain Co/Ni-NPC;
s3, preparing nitrogen-doped porous carbon-supported CoP/NiP: placing a quartz boat loaded with 1g of Co/Ni-NPC in a tubular quartz furnace, placing the quartz boat in the downstream of red phosphorus steam, flowing Ar gas flow through a quartz tube, wherein the flow rate of the Ar gas is 10ml/min, the pressure is about 115kPa, the temperature of the quartz tube is increased to 500 ℃ at the temperature increasing rate of 5 ℃/min, reacting at a constant temperature for 2h, cooling to 350 ℃ at the temperature of 5 ℃/min, preserving the heat for 2h, cooling to room temperature in the Ar atmosphere, taking out, washing the product twice by deionized water and ethanol respectively, and drying at 75 ℃ in vacuum to obtain CoxPy/NixPy-NPC material.
This example, as shown in FIG. 1, resultedCoxPy/NixPyXRD spectrum analysis of the NPC material confirmed the formation of the phosphatized metal compound phase. The material can be used for hydrogen evolution reaction in 1mol/L KOH and electrochemical linear volt-ampere (LSV, start-stop potential 0.02V-0.5V or other suitable potentials, the potential is relative to a reversible hydrogen electrode RHE, and the scanning speed is 5mV s-1) Scanning of η10(Current Density 10mA cm-2RHE potential value at time) of 145mV, as shown in FIG. 4, versus the currently accepted most elegant hydrogen evolution catalyst, Pt, η, under the same test conditions10About 62mV, CoxPy/NixPyEta of NPC material10Eta of Pt10The height is about 83mV, which confirms that the catalyst has better electrocatalytic hydrogen evolution effect.
Example 2
The embodiment 2 of the invention discloses a preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide, which adopts the following technical scheme:
similar to the technical scheme of example 1, in step S1 `2.0 mmol of Co (NO)3)2·6H2O and 2.0mmol of Ni (NO)3)2·6H2Powder mixture of O "replaced by: 4.0mmol of Co (NO)3)2·6H2O, without adding Ni salt, the other steps were the same as in example 1, and Co was finally obtained in this examplexPy-NPC material. As shown in fig. 2, the analysis confirmed the presence of cobalt phosphide. The LSV scan is also performed, as shown in FIG. 4, with η10Is 158 mV.
Example 3
The embodiment 3 of the invention discloses a preparation method of nitrogen-doped porous carbon-loaded nickel phosphide, which adopts the following technical scheme:
similar to the technical scheme of example 1, in step S1 `2.0 mmol of Co (NO)3)2·6H2O and 2.0mmol of Ni (NO)3)2·6H2Powder mixture of O "replaced by: 5.0mmol of Ni (NO)3)2·6H2O, without adding cobalt salt, the other steps are the same as example 1, this example finally obtains NixPy-NPC material. As shown in the figure 3 of the drawings,analysis confirmed the presence of nickel phosphide. The LSV scan is also performed, as shown in FIG. 4, with η10Is 176 mV.
Example 4
The embodiment 4 of the invention discloses a preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide, which adopts the following technical scheme:
similar to the technical scheme of example 1, in step S1 `2.0 mmol of Co (NO)3)2·6H2O and 2.0mmol of Ni (NO)3)2·6H2Powder mixture of O "replaced by: 2.0mmol of cobalt acetate tetrahydrate Co (CH)3COO)2·4H2O and 3.0mmol of Ni (CH) acetate tetrahydrate3COO)2·4H2O, other steps are the same as example 1, and Co is finally obtained in this examplexPy/NixPyNPC (b sample) material, also LSV scanned, eta10Is 159 mV.
Comparative example 1
In the same way as the technical scheme of the example 1, a metal blank pure MF organic polymer is obtained without adding any cobalt/nickel salt, other steps are the same as the example 1, the blank NPC is finally obtained in the example, LSV scanning is carried out in the same way, and eta of the blank NPC is eta10669mV, almost without catalytic effect.
The scan rate is shown in FIG. 2 to be 5mV s-1Of Ti-CoxPyNPC (example 2), NixPyNPC (example 3) and CoxPy/NixPyLSV curves of NPC (example 1) and Pt/C. Under the conditions of the experiment, CoxPy/NixPy-NPC and CoxPyThe activity of-NPC is superior to that of NixPy-NPC. At the same time, CoxPy-NPC and NixPy-NPC exhibits a relatively low η at 158mV and 176mV10。
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. A preparation method of nitrogen-doped porous carbon-loaded cobalt phosphide/nickel phosphide is characterized by comprising the following specific steps:
s1, preparing melamine formaldehyde resin containing cobalt/nickel: mixing melamine and 35% -40% of formaldehyde aqueous solution, wherein the mass ratio of the melamine to the formaldehyde is 1: 6-40; oscillating the mixture at the set temperature of 50-90 ℃, reacting for 5-20 min to obtain clear prepolymer liquid, pouring the mixture of cobalt salt and nickel salt into the prepolymer liquid, wherein the ratio of the total amount of the cobalt salt and the nickel salt to the amount of melamine is 0.5-4: 1, oscillating and dissolving, keeping the temperature at 50-90 ℃, and taking out the polymer after polymerization and solidification to obtain Co/Ni-MF;
s2, preparing a nitrogen-doped porous carbon-loaded cobalt-nickel material: calcining Co/Ni-MF at 700-950 ℃ for 2-4 h in an inert atmosphere, carbonizing an organic component to obtain NPC, and naturally cooling to room temperature in a protective gas atmosphere to obtain Co/Ni-NPC;
s3, preparing nitrogen-doped porous carbon-supported CoP/NiP: placing a quartz boat loaded with Co/Ni-NPC in a tubular quartz furnace, placing the quartz boat in the downstream of phosphorus steam, driving the phosphorus steam to uniformly flow through the Co/Ni-NPC by inert gas flow to generate a phosphorization reaction at the temperature of 450-600 ℃, reacting for 1-2 h, setting the temperature rise rate to be 5 ℃/min, preserving heat for 1h, then cooling to 250-350 ℃, preserving heat for 2h, cooling to room temperature in inert gas, taking out, washing products twice by deionized water and ethanol respectively, and then drying in vacuum at the temperature of 60-80 ℃ to obtain CoxPy/NixPy-NPC。
2. The method for preparing nitrogen-doped porous carbon-supported cobalt phosphide/nickel phosphide as claimed in claim 1, wherein the cobalt salt and the nickel salt in step S1 are respectively one of nitrate, sulfate, chloride and organic acid salt.
3. The method for preparing nitrogen-doped porous carbon-supported cobalt phosphide/nickel phosphide as claimed in claim 1, wherein urea and biuret can be added into the prepolymer solution in step S1 to adjust the nitrogen content of the system, and the addition amount is less than or equal to 30% of the total weight of the prepolymer solution.
4. The method for preparing nitrogen-doped porous carbon-supported cobalt phosphide/nickel phosphide as claimed in claim 1, wherein the vapor source of phosphorus vapor in step S3 is red phosphorus or white phosphorus.
5. The method for preparing nitrogen-doped porous carbon-supported cobalt phosphide/nickel phosphide as claimed in claim 1, wherein the inert gas flow in the step S3 is Ar gas flow or N gas flow2And the airflow is set to be 10-50 ml/min at 25 ℃ and the absolute pressure is 101-115 kPa.
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