CN113981481A - Preparation method and application of copper nanoparticle-loaded one-dimensional carbon-based nano material - Google Patents
Preparation method and application of copper nanoparticle-loaded one-dimensional carbon-based nano material Download PDFInfo
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- CN113981481A CN113981481A CN202111140793.3A CN202111140793A CN113981481A CN 113981481 A CN113981481 A CN 113981481A CN 202111140793 A CN202111140793 A CN 202111140793A CN 113981481 A CN113981481 A CN 113981481A
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- C25B11/052—Electrodes comprising one or more electrocatalytic coatings on a substrate
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
Abstract
The invention discloses a preparation method of a copper nanoparticle-loaded one-dimensional carbon-based nano material. The preparation method and the application of the copper nanoparticle-loaded one-dimensional carbon-based nano material can directly obtain the new morphology carbon-based material of the copper nanoparticles loaded with uniform size in one step, have the characteristics of mild synthesis conditions, easiness in realization, better nitrate conversion performance and the like, and can be well applied to the field of design and preparation of carbon-based metal catalysts.
Description
Technical Field
The invention belongs to the technical field of synthesis and electrocatalysis of novel carbon materials, and particularly relates to a preparation method of a copper nanoparticle-loaded one-dimensional carbon-based nano material. The invention also relates to an application of the copper nanoparticle-loaded one-dimensional carbon-based nano material.
Background
Ammonia is an important industrial chemical used in the manufacture of fertilizers, nutrients, pharmaceuticals, and also as a future high energy density solar fuel. The global supply of ammonia relies primarily on the Haber-Bosch process, which uses an iron-based catalyst to catalyze the reaction of nitrogen and hydrogen at high temperatures and pressures. However, as high energy input and high carbon dioxide emissions lead to global climate change, there is an urgent need to develop sustainable methods to replace the Haber-Bosch process. In recent years, carbon materials have been characterized by the following features: (1) there are many existing forms (such as amorphous carbon, graphite, diamond, graphene, and carbon nanotubes) that can provide a variety of material choices for design; (2) the conductive material has high conductivity, and provides an effective electron transfer path in electrochemical reaction; (3) can be easily modified or functionalized to expand the activity, such as doping or non-covalent functionalization, and the like, and is widely applied to the design and preparation of catalysts.
The carbon materials used in the traditional carbon-based catalysis mainly comprise graphene, carbon nanotubes, fullerene and the like, and the synthesis of the materials can be realized by some specific methods. Other nanostructured carbons are typically obtained under extreme conditions, such as hydrothermal processes and high temperature pyrolysis processes. For example, various porous carbons are prepared by soft or hard template methods in combination with high temperature pyrolysis in an inert atmosphere. The preparation of the carbon-based catalyst is also to adopt photo-deposition or other methods to load the metal material on the surface of the carbon-based catalyst after the carbon material is obtained to form the carbon-based catalyst material. For example: jun Wang et al (Nature Communications, 2018, 9, 1) successfully load palladium nanoparticles on carbon black by using a glycol reduction method to obtain a catalyst material with good performance for producing ammonia by nitrogen reduction. CN 202110790312.7 also discloses a preparation method of the carbon material-supported platinum catalyst, and the preparation method is applied to the technical fields of fuel cell material manufacturing and electro-catalysis. The catalyst has good stability and performance superior to that of commercial platinum-carbon catalysts, and can overcome the defect of preparing Pt/C type catalysts by using boron-containing compounds as strong reducing agents. However, this method is also a method in which a palladium precursor is combined with an existing carbon material.
Although the existing synthesis techniques of various carbon materials are mature and can be applied to the preparation of carbon-based metal catalysts, the actual synthesis operation process and the performance of the carbon-based metal catalysts are still influenced to a great extent due to the harsh synthesis conditions, uncontrollable synthesis process and complicated synthesis method.
Disclosure of Invention
The invention aims to provide a preparation method of a copper nanoparticle-loaded one-dimensional carbon-based nano material, which solves the problems of harsh synthesis conditions, uncontrollable synthesis process and complicated synthesis method of the existing carbon material synthesis technology.
The invention also aims to provide application of the one-dimensional carbon-based nano material loaded with the copper nanoparticles.
The first technical scheme adopted by the invention is as follows: a preparation method of a copper nanoparticle-loaded one-dimensional carbon-based nano material comprises the following steps:
step 1, dissolving citric acid in ultrapure water, and stirring to obtain a uniform solution;
step 2, preparing copper nanoparticles and dispersing the copper nanoparticles in water to obtain uniform dispersion liquid;
step 3, adding the dispersion liquid obtained in the step 2 into the solution obtained in the step 1, and performing ultrasonic treatment to obtain a uniform mixed liquid;
step 4, putting the mixed solution obtained in the step 3 into an oil bath, stirring at the reaction temperature, and controlling the reaction time to obtain the mixed solution of the one-dimensional carbon-based nano material loaded with the copper nanoparticles;
and 5, centrifugally separating the mixed solution obtained in the step 4, and washing the precipitate to obtain the compound.
The first technical solution of the present invention is also characterized in that,
the concentration of the solution obtained in the step 1 is 5-25 mol/L.
The specific steps for preparing the copper nanoparticles in the step 2 include:
step 2.1, dispersing copper chloride, hexadecylamine and glucose in 5-15mL of water, and carrying out ultrasonic treatment for 5-20min to obtain a uniform mixed solution;
2.2, putting the mixed solution obtained in the step 2.1 into an oil bath, stirring at the reaction temperature, and controlling the reaction time to obtain a mixed solution containing copper nanoparticles;
and 2.3, centrifugally separating the mixed liquid containing the copper nanoparticles obtained in the step 2.2, and washing precipitates to obtain the copper nanoparticle washing agent.
The concentration of copper chloride in the mixed solution obtained in the step 2.1 is 0.01-0.02mol/L, the concentration of hexadecylamine is 0.03-0.05mol/L, and the concentration of glucose is 0.02-0.03 mol/L.
The reaction temperature in the step 2.2 is 80-150 ℃, and the reaction time is 4-8 h.
The washing procedure in step 2.3 is as follows: the precipitate obtained by centrifuging the mixed solution is firstly washed by ethanol until the supernatant is colorless, and then is separated and washed by deionized water.
In the step 3, the volume of the citric acid solution is 1-3mL, the volume of the copper nanoparticle dispersion liquid is 1-3mL, and the ultrasonic treatment is carried out for 5-20 min.
In the step 4, the reaction temperature is 80-150 ℃, and the reaction time is 10-24 h.
The washing procedure in step 5 was as follows: the precipitate obtained by centrifuging the mixture is washed with deionized water until the supernatant is clear.
The second technical scheme adopted by the invention is as follows: the application of the copper nanoparticle-loaded one-dimensional carbon-based nanomaterial obtained by the preparation method comprises the steps of coating the copper nanoparticle-loaded one-dimensional carbon-based nanomaterial on a glassy carbon electrode, drying the glassy carbon electrode in a drying oven at the temperature of 30-60 ℃ for 6-10H, and then placing the glassy carbon electrode in an H-type electrolytic cell for converting nitrate to generate ammonia.
The invention has the beneficial effects that: according to the preparation method and application of the copper nanoparticle-loaded one-dimensional carbon-based nano material, the carbon-based material with the new morphology of the loaded copper nanoparticles with uniform size can be directly obtained in one step, and the preparation method has the characteristics of mild synthesis conditions, easiness in realization, better nitrate conversion performance and the like, and can be well applied to the field of design and preparation of carbon-based metal catalysts.
Drawings
FIG. 1 is an SEM image of a product obtained by the preparation method of the copper nanoparticle-loaded one-dimensional carbon-based nanomaterial;
FIG. 2 is a TEM image of a product obtained by the preparation method of the copper nanoparticle-loaded one-dimensional carbon-based nanomaterial of the present invention, with a 50nm scale;
FIG. 3 is a TEM image of a product obtained by the preparation method of the copper nanoparticle-loaded one-dimensional carbon-based nanomaterial of the present invention, with a 500nm scale;
FIG. 4 is a performance diagram of the copper nanoparticle-loaded one-dimensional carbon-based nanomaterial obtained by the preparation method of the invention for ammonia production through nitrate conversion.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of a copper nanoparticle-loaded one-dimensional carbon-based nano material, which comprises the following steps:
step 1, dissolving citric acid in ultrapure water, and stirring to obtain a uniform solution with the concentration of 5-25 mol/L;
step 2, preparing copper nanoparticles and dispersing the copper nanoparticles in water to obtain uniform dispersion liquid; the preparation method of the copper nanoparticles comprises the following specific steps:
step 2.1, dispersing copper chloride, hexadecylamine and glucose in 5-15mL of water, and carrying out ultrasonic treatment for 5-20min to obtain a uniform mixed solution, wherein the concentration of the copper chloride in the mixed solution is 0.01-0.02mol/L, the concentration of the hexadecylamine in the mixed solution is 0.03-0.05mol/L, and the concentration of the glucose in the mixed solution is 0.02-0.03 mol/L;
2.2, putting the mixed solution obtained in the step 2.1 into an oil bath, stirring at the temperature of 80-150 ℃, and controlling the reaction time for 4-8h to obtain a mixed solution containing copper nanoparticles;
and 2.3, centrifugally separating and washing the mixed solution containing the copper nanoparticles obtained in the step 2.2 to obtain dark red precipitates, and dispersing the precipitates in water to obtain a dispersion liquid containing the copper nanoparticles. Wherein the washing process is as follows: the precipitate obtained by centrifuging the mixed solution is firstly washed by ethanol until the supernatant is colorless, and then is separated and washed by deionized water.
Step 3, adding 1-3mL of the copper nanoparticle dispersion liquid obtained in the step 2 into 1-3mL of the citric acid solution obtained in the step 1, and performing ultrasonic treatment for 5-20min to obtain a uniform mixed solution;
step 4, putting the mixed solution obtained in the step 3 into an oil bath, stirring at the temperature of 80-150 ℃, and controlling the reaction time for 10-24h to obtain a light green mixed solution of the one-dimensional carbon-based nano material loaded with the copper nano particles;
and 5, centrifugally separating and washing the light green mixed solution containing the one-dimensional carbon-based nano material loaded with the copper nano particles obtained in the step 4 to obtain light green precipitates, and dispersing the precipitates in an aqueous solution to obtain light green dispersed solution containing the one-dimensional carbon-based nano material loaded with the copper nano particles, so as to obtain the copper nano particle-loaded light green dispersion solution. Wherein the washing process is as follows: the precipitate obtained by centrifuging the mixture is washed with deionized water until the supernatant is clear.
Through the way, the preparation method of the copper nanoparticle-loaded one-dimensional carbon-based nano material can directly obtain the new morphology carbon-based material loaded with copper nanoparticles with uniform size in one step. As shown in fig. 1, the prepared material has a one-dimensional strip shape with a width of about 500nm and different lengths; as shown in fig. 2 and 3, the prepared material is a carbon-based material with nanoparticles grown on a carbon substrate, and the nanoparticles are about 10 nm in size and are distributed on the carbon substrate more uniformly.
The invention also provides application of the copper nanoparticle-loaded one-dimensional carbon-based nano material obtained by the preparation method, wherein the copper nanoparticle-loaded one-dimensional carbon-based nano material is coated on a glassy carbon electrode, dried in an oven at 30-60 ℃ for 6-10H, and then placed in an H-type electrolytic cell for nitrate conversion to produce ammonia. As can be seen from FIG. 4, with the gradual negative shift of the applied voltage, the nitrate conversion performance of the prepared material firstly increases and then decreases, and the highest performance point appears at-0.4V (vs. RHE) of 220 mu g h-1mg-1The faraday efficiency tends to decrease first, then increase, then decrease. At the highest performance point, the faradaic efficiency is the highest, which is 65%.
Example 1
Dispersing copper chloride, hexadecylamine and glucose in 5mL of water, performing ultrasonic treatment for 5min to obtain a mixed solution with the concentration of 0.01mol/L of copper chloride, the concentration of 0.03mol/L of hexadecylamine and the concentration of 0.02mol/L of glucose, putting the mixed solution into an oil bath, stirring at 80 ℃, controlling the reaction time for 8h to obtain a mixed solution containing copper nanoparticles, and then performing centrifugal separation and washing to obtain the copper nanoparticles; dispersing copper nanoparticles in water to obtain a dispersion liquid, adding 1mL of the dispersion liquid into 1mL of a citric acid solution with the concentration of 5mol/L, and performing ultrasonic treatment for 5min to obtain a uniform mixed solution; putting the mixed solution into an oil bath, stirring at 80 ℃, and controlling the reaction time for 24 hours to obtain a light green mixed solution containing the copper nanoparticle-loaded one-dimensional carbon-based nano material; and centrifugally separating and washing the bright green mixed solution to obtain bright green precipitates, and dispersing the precipitates in an aqueous solution to obtain a bright green dispersion liquid of the one-dimensional carbon-based nano material loaded with the copper nano particles.
Example 2
Dispersing copper chloride, hexadecylamine and glucose in 15mL of water, performing ultrasonic treatment for 20min to obtain a mixed solution with the concentration of 0.02mol/L of copper chloride, 0.05mol/L of hexadecylamine and 0.03mol/L of glucose, putting the mixed solution into an oil bath, stirring at 150 ℃, controlling the reaction time for 4h to obtain a mixed solution containing copper nanoparticles, and then performing centrifugal separation and washing to obtain the copper nanoparticles; dispersing copper nanoparticles in water to obtain a dispersion liquid, adding 3mL of the dispersion liquid into 3mL of a citric acid solution with the concentration of 25mol/L, and performing ultrasonic treatment for 20min to obtain a uniform mixed liquid; putting the mixed solution into an oil bath, stirring at 150 ℃, and controlling the reaction time for 10 hours to obtain a light green mixed solution containing the copper nanoparticle-loaded one-dimensional carbon-based nano material; and centrifugally separating and washing the bright green mixed solution to obtain bright green precipitates, and dispersing the precipitates in an aqueous solution to obtain a bright green dispersion liquid of the one-dimensional carbon-based nano material loaded with the copper nano particles.
Example 3
Dispersing copper chloride, hexadecylamine and glucose in 10mL of water, performing ultrasonic treatment for 5min to obtain a mixed solution with the concentration of 0.015mol/L of copper chloride, the concentration of 0.03mol/L of hexadecylamine and the concentration of 0.02mol/L of glucose, putting the mixed solution into an oil bath, stirring at 80 ℃, controlling the reaction time for 8h to obtain a mixed solution containing copper nanoparticles, and then performing centrifugal separation and washing to obtain the copper nanoparticles; dispersing copper nanoparticles in water to obtain a dispersion liquid, adding 2mL of the dispersion liquid into 2mL of a citric acid solution with the concentration of 10mol/L, and carrying out ultrasonic treatment for 5min to obtain a uniform mixed liquid; putting the mixed solution into an oil bath, stirring at 80 ℃, and controlling the reaction time for 24 hours to obtain a light green mixed solution containing the copper nanoparticle-loaded one-dimensional carbon-based nano material; and centrifugally separating and washing the bright green mixed solution to obtain bright green precipitates, and dispersing the precipitates in an aqueous solution to obtain a bright green dispersion liquid of the one-dimensional carbon-based nano material loaded with the copper nano particles.
Example 4
Dispersing copper chloride, hexadecylamine and glucose in 10mL of water, performing ultrasonic treatment for 10min to obtain a mixed solution with the concentration of 0.02mol/L of copper chloride, the concentration of 0.04mol/L of hexadecylamine and the concentration of 0.02mol/L of glucose, putting the mixed solution into an oil bath, stirring at 100 ℃, controlling the reaction time for 6h to obtain a mixed solution containing copper nanoparticles, and then performing centrifugal separation and washing to obtain the copper nanoparticles; dispersing copper nanoparticles in water to obtain a dispersion liquid, adding 2.5mL of the dispersion liquid into 2.5mL of a citric acid solution with the concentration of 15mol/L, and performing ultrasonic treatment for 10min to obtain a uniform mixed liquid; putting the mixed solution into an oil bath, stirring at 90 ℃, and controlling the reaction time for 18h to obtain a light green mixed solution containing the copper nanoparticle-loaded one-dimensional carbon-based nano material; and centrifugally separating and washing the bright green mixed solution to obtain bright green precipitates, and dispersing the precipitates in an aqueous solution to obtain a bright green dispersion liquid of the one-dimensional carbon-based nano material loaded with the copper nano particles.
Example 5
Dispersing copper chloride, hexadecylamine and glucose in 15mL of water, performing ultrasonic treatment for 20min to obtain a mixed solution with the concentration of 0.02mol/L of copper chloride, 0.04mol/L of hexadecylamine and 0.03mol/L of glucose, putting the mixed solution into an oil bath, stirring at 120 ℃, controlling the reaction time for 6h to obtain a mixed solution containing copper nanoparticles, and then performing centrifugal separation and washing to obtain the copper nanoparticles; dispersing copper nanoparticles in water to obtain a dispersion liquid, adding 3mL of the dispersion liquid into 3mL of a citric acid solution with the concentration of 20mol/L, and carrying out ultrasonic treatment for 15min to obtain a uniform mixed liquid; putting the mixed solution into an oil bath, stirring at 120 ℃, and controlling the reaction time for 15h to obtain a light green mixed solution containing the copper nanoparticle-loaded one-dimensional carbon-based nano material; and centrifugally separating and washing the bright green mixed solution to obtain bright green precipitates, and dispersing the precipitates in an aqueous solution to obtain a bright green dispersion liquid of the one-dimensional carbon-based nano material loaded with the copper nano particles.
Claims (10)
1. A preparation method of a copper nanoparticle-loaded one-dimensional carbon-based nano material is characterized by comprising the following steps:
step 1, dissolving citric acid in ultrapure water, and stirring to obtain a uniform solution;
step 2, preparing copper nanoparticles and dispersing the copper nanoparticles in water to obtain uniform dispersion liquid;
step 3, adding the dispersion liquid obtained in the step 2 into the solution obtained in the step 1, and performing ultrasonic treatment to obtain a uniform mixed liquid;
step 4, putting the mixed solution obtained in the step 3 into an oil bath, stirring at the reaction temperature, and controlling the reaction time to obtain the mixed solution of the one-dimensional carbon-based nano material loaded with the copper nanoparticles;
and 5, centrifugally separating the mixed solution obtained in the step 4, and washing the precipitate to obtain the compound.
2. The method for preparing the copper nanoparticle-supported one-dimensional carbon-based nanomaterial according to claim 1, wherein the concentration of the solution obtained in the step 1 is 5-25 mol/L.
3. The method for preparing the copper nanoparticle-supported one-dimensional carbon-based nanomaterial according to claim 1, wherein the step 2 for preparing the copper nanoparticles comprises the following specific steps:
step 2.1, dispersing copper chloride, hexadecylamine and glucose in 5-15mL of water, and carrying out ultrasonic treatment for 5-20min to obtain a uniform mixed solution;
2.2, putting the mixed solution obtained in the step 2.1 into an oil bath, stirring at the reaction temperature, and controlling the reaction time to obtain a mixed solution containing copper nanoparticles;
and 2.3, centrifugally separating the mixed liquid containing the copper nanoparticles obtained in the step 2.2, and washing precipitates to obtain the copper nanoparticle washing agent.
4. The method for preparing the copper nanoparticle-supported one-dimensional carbon-based nanomaterial according to claim 3, wherein the mixed solution obtained in the step 2.1 has a copper chloride concentration of 0.01-0.02mol/L, a hexadecylamine concentration of 0.03-0.05mol/L, and a glucose concentration of 0.02-0.03 mol/L.
5. The method for preparing the copper nanoparticle-supported one-dimensional carbon-based nanomaterial as claimed in claim 3, wherein the reaction temperature in the step 2.2 is 80-150 ℃ and the reaction time is 4-8 h.
6. The method for preparing the copper nanoparticle-supported one-dimensional carbon-based nanomaterial as claimed in claim 3, wherein the washing process in the step 2.3 is as follows: the precipitate obtained by centrifuging the mixed solution is firstly washed by ethanol until the supernatant is colorless, and then is separated and washed by deionized water.
7. The method for preparing the copper nanoparticle-supported one-dimensional carbon-based nanomaterial according to claim 1, wherein in the step 3, the volume of the citric acid solution is 1-3mL, the volume of the copper nanoparticle dispersion is 1-3mL, and the ultrasound is performed for 5-20 min.
8. The method for preparing the copper nanoparticle-supported one-dimensional carbon-based nanomaterial according to claim 1, wherein the reaction temperature in the step 4 is 80-150 ℃ and the reaction time is 10-24 hours.
9. The method for preparing the copper nanoparticle-supported one-dimensional carbon-based nanomaterial according to claim 1, wherein the washing process in the step 5 is as follows: the precipitate obtained by centrifuging the mixture is washed with deionized water until the supernatant is clear.
10. The application of the copper nanoparticle-loaded one-dimensional carbon-based nanomaterial obtained by the preparation method of claim 1 is characterized in that the copper nanoparticle-loaded one-dimensional carbon-based nanomaterial is coated on a glassy carbon electrode, dried in an oven at 30-60 ℃ for 6-10H, and then placed in an H-type electrolytic cell for nitrate conversion to produce ammonia.
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| CN116495770A (en) * | 2023-04-28 | 2023-07-28 | 西安电子科技大学 | Plasmon enhanced copper-based sulfide semiconductor and preparation method and application thereof |
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