CN112719285A - Sacrificial template agent coated nano-gold particles and preparation method thereof - Google Patents
Sacrificial template agent coated nano-gold particles and preparation method thereof Download PDFInfo
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Abstract
A sacrificial template agent coated nano gold particle and a preparation method thereof belong to the technical field of preparation of gold nano particle catalysts. The technical problems to be solved by the invention are particle uniformity, dispersibility and size reduction of particle size. The invention is mainly prepared from 2.6-18.2 parts of chloroauric acid, 21.5-27.5 parts of sodium citrate, 38.7-42.6 parts of F127, 13.4-17.3 parts of P123 and 8.2-10 parts of urea. The invention adds polyoxyethylene polyoxypropylene and polyethylene oxide-polypropylene oxide-polyethylene oxide high molecular block copolymer asThe template agent wrapping the gold particles can enrich a large amount of H on the surfaces of the gold nanoparticles while the chloroauric acid is reduced+The high-molecular block copolymer is adsorbed and coated on the surfaces of the gold particles to form micelles, so that the agglomeration among the particles is prevented, and good dispersibility is obtained.
Description
Technical Field
The invention belongs to the technical field of gold nanoparticle catalyst preparation; in particular to a sacrificial template agent coated nano-gold particle and a preparation method thereof.
Background
The use of gold in catalysis has long been very limited because gold in bulk form (bulk gold) has essentially no catalytic activity. At the end of the last century, m.haruta found that gold, when reduced in particle size to the nanometer size range (3-5nm), exhibited better catalytic activity and high catalytic selectivity. Gold nanoparticles have extremely high surface free energy and tend to spontaneously aggregate and fuse under reaction conditions. Usually it is supported on a support, such as an activated carbon, polymer, molecular sieve or other oxide surface, with the nanogold catalyst being the first to be used in the selective oxidation of hydrocarbons. And Y, A, Kalvachev and the like firstly load the gold nanoparticles in the Ti-MCM-41 pore channel and apply the gold nanoparticles to the epoxidation reaction of propylene. An initial conversion of 2% and a selectivity to propylene oxide of greater than 95% was obtained at 100 c. However, the catalytic activity may decrease with time due to agglomeration of gold nanoparticles or sintering under reaction conditions. Although the gold nanoparticle catalyst has excellent catalytic performance, because of smaller particle size, the gold nanoparticle catalyst must be loaded on a carrier when in use, and how to better load the gold nanoparticle catalyst on the carrier so as to facilitate the gold nanoparticle catalyst to reactThe gold nanoparticles are not easy to fall off in the process, and the gold nanoparticles are ensured not to agglomerate and fuse under the reaction condition, so that the problem to be faced is solved. C, Y.Mou designs and synthesizes a catalyst with a Yolk-Shell structure, which takes nano gold particles as a core and silicon oxide as a Shell, and is used for discussing CO oxidation reaction, but the prepared core-Shell structure particles have uneven size and poor dispersibility. The carbon-coated gold nanoparticles synthesized by Lining et al have poor morphology regularity and weak catalytic performance. Luis M et al prepared Au @ SiO by self-assembly method2The material has long preparation period, complex operation and large particle size. Therefore, the problems of agglomeration or size morphology of the carbon-coated gold nanoparticles with the core-shell structure limit the application of the carbon-coated gold nanoparticles in catalysis, adsorption, electrochemistry, sensors and the like.
Disclosure of Invention
The invention aims to provide a sacrificial template agent coated nano gold particle with uniform microscopic appearance and good dispersibility and a preparation method thereof.
The invention is realized by the following technical scheme:
a sacrificial template agent coated nano-gold particle is mainly prepared from 2.6-18.2 parts by weight of chloroauric acid, 21.5-27.5 parts by weight of sodium citrate, 38.7-42.6 parts by weight of F127, 13.4-17.3 parts by weight of P123 and 8.2-10 parts by weight of urea.
The sacrificial template agent coated nano-gold particle is prepared from 2.6 parts of chloroauric acid, 27.5 parts of sodium citrate, 42.6 parts of F127, 17.3 parts of P123 and 10 parts of urea.
The sacrificial template agent coated nano-gold particle is prepared from 18.2 parts of chloroauric acid, 21.5 parts of sodium citrate, 38.7 parts of F127, 13.4 parts of P123 and 8.2 parts of urea.
The sacrificial template agent coated nano-gold particle is prepared from 10.8 parts of chloroauric acid, 23.2 parts of sodium citrate, 40.8 parts of F127, 16.1 parts of P123 and 9.1 parts of urea.
The preparation method of the sacrificial template agent coated nano gold particles comprises the following steps:
step 1, weighing chloroauric acid and sodium citrate according to parts by weight, dissolving the chloroauric acid and the sodium citrate into purified water with a certain volume according to a material-liquid ratio, and stirring uniformly to obtain a first mixed solution for later use;
step 2, weighing urea according to parts by weight, preparing a urea solution, adding the prepared urea solution into the first mixed solution prepared in the step 1, and uniformly stirring to obtain a second mixed solution for later use;
step 3, weighing F127 and P123 according to parts by weight, and dissolving the materials and the solution in purified water with a certain volume according to the material-to-solution ratio to obtain a mixed solution of the F127 and the P123 for later use;
and 4, slowly dropwise adding the mixed solution of F127 and P123 obtained in the step 3 into the second mixed solution prepared in the step 2, reacting for a certain time under the stirring condition, centrifugally collecting the obtained product, washing the obtained solid phase to be neutral, drying, and calcining in a muffle furnace to obtain the sacrificial template agent coated nano-gold particles.
According to the preparation method of the sacrificial template agent coated nano gold particles, the material-liquid ratio of a mixture of chloroauric acid and sodium citrate to purified water in the step 1 is 1.2-1.5: 100g/ml, the stirring condition in the step 1 is 20-30 ℃, the stirring speed is 50-200 r/min, and the stirring time is 20-60 min.
According to the preparation method of the sacrificial template agent coated nano gold particles, the concentration of the urea solution in the step 2 is 10-12 wt%, the stirring condition in the step 2 is that the urea solution is stirred for 10-20 min at 50-60 ℃, and the stirring speed is 50-200 r/min.
According to the preparation method of the sacrificial template agent coated nano gold particles, the material-liquid ratio of the mixture of F127 and P123 to purified water in step 3 is 4-6: 50 g/ml.
According to the preparation method of the sacrificial template agent coated nano gold particles, stirring is carried out for 2-4 hours at 75-85 ℃ in the step 4, the stirring speed is 50-200 r/min, and the calcining is carried out for 2-3 hours at 500-600 ℃ in a muffle furnace.
The preparation method of the sacrificial template agent coated nano gold particles comprises the steps of washing 3-5 times with purified water in step 4 until the particles are neutral, drying with an oven at the drying temperature of 60-80 ℃ for 1-2 hours.
According to the preparation method of the sacrificial template agent coated nano gold particles, the F127 (polyoxyethylene polyoxypropylene) and P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide) high-molecular block copolymer is added to serve as the template agent for coating the gold particles, and when chloroauric acid is reduced, a large amount of H is enriched on the surfaces of the gold particles+The high-molecular block copolymer is adsorbed and coated on the surfaces of the gold particles to form micelles, so that the agglomeration among the particles is prevented, and good dispersibility is obtained.
The preparation method of the sacrificial template agent coated gold nanoparticles comprises the steps of adding urea as a catalyst (also as a precipitator), adopting a uniform precipitation method, mixing a urea solution and a gold nanoparticle solution at room temperature, slowly dripping a mixed solution of F127 (polyoxyethylene polyoxypropylene) and P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide) under stirring at 50-60 ℃, starting slow hydrolysis reaction of urea to generate ammonia water and carbon dioxide when the temperature reaches about 75-85 ℃, and rapidly decomposing the ammonia water into OH-Uniformly distributed in the solution, and an alkaline environment is provided, so that the high-molecular block copolymer starts to wrap the nano-gold particles to form crystal nuclei. Urea and OH-The existence in the reaction solution is in an equilibrium state, so the reaction rate of the gold particles wrapped by the high-molecular block copolymer is very slow, the nucleation rate of crystal nuclei is greater than the growth rate of the crystal nuclei, and the high-quality sacrificial template agent (high-molecular block copolymer mixture) wrapped gold nanoparticles with small size and uniform particle size can be obtained, and the particle size is about 50 nm.
Drawings
FIG. 1 is an SEM photograph of gold nanoparticles coated with a sacrificial templating agent prepared according to one embodiment;
FIG. 2 is an XRD plot of one of the sacrificial templating agent coated gold nanoparticles prepared according to one embodiment;
FIG. 3 is an SEM photograph of the gold nanoparticles coated with the sacrificial template prepared by the method according to the second embodiment;
FIG. 4 is a TEM image of the gold nanoparticles coated with the sacrificial template prepared by the method of the second embodiment;
FIG. 5 is an SEM photograph of gold nanoparticles coated with a sacrificial templating agent, prepared by a method according to a third embodiment;
fig. 6 is an XRD curve of one of the sacrificial templating agent coated gold nanoparticles prepared by the third embodiment.
Detailed Description
The first embodiment is as follows:
a preparation method of gold nanoparticles wrapped by a sacrificial template agent comprises the following steps:
step 1, weighing chloroauric acid and sodium citrate according to parts by weight, dissolving the chloroauric acid and the sodium citrate into purified water with a certain volume according to a material-liquid ratio, and stirring uniformly to obtain a first mixed solution for later use;
step 2, weighing urea according to parts by weight, preparing a urea solution, adding the prepared urea solution into the first mixed solution prepared in the step 1, and uniformly stirring to obtain a second mixed solution for later use;
step 3, weighing F127 and P123 according to parts by weight, and dissolving the materials and the solution in purified water with a certain volume according to the material-to-solution ratio to obtain a mixed solution of the F127 and the P123 for later use;
and 4, slowly dropwise adding the mixed solution of F127 and P123 obtained in the step 3 into the second mixed solution prepared in the step 2, reacting for a certain time under the stirring condition, centrifugally collecting the obtained product, washing the obtained solid phase to be neutral, drying, and calcining in a muffle furnace to obtain the sacrificial template agent coated nano-gold particles.
In the preparation method of the sacrificial template-coated gold nanoparticle according to the embodiment, the sacrificial template-coated gold nanoparticle is mainly prepared from chloroauric acid, sodium citrate, F127, P123 and urea, and the sacrificial template-coated gold nanoparticle is prepared from 2.6 parts of chloroauric acid, 27.5 parts of sodium citrate, 42.6 parts of F127, 17.3 parts of P123 and 10 parts of urea.
In the preparation method of the sacrificial template agent-coated gold nanoparticles according to the embodiment, the material-liquid ratio of the mixture of chloroauric acid and sodium citrate to purified water in step 1 is 1.2:100g/ml, the stirring condition in step 1 is 30 ℃ and 30min, and the stirring speed is 100 r/min.
In the preparation method of the sacrificial template agent coated gold nanoparticles according to the embodiment, the concentration of the urea solution in the step 2 is 10 wt%, the stirring condition in the step 2 is stirring at 55 ℃ for 15min, and the stirring speed is 100 r/min.
In the preparation method of the gold nanoparticles wrapped by the sacrificial template in this embodiment, the material-to-liquid ratio of the mixture of F127 and P123 to the purified water in step 3 is 4:50 g/ml.
In the preparation method of the sacrificial template coated gold nanoparticles, in the step 4, stirring is performed at 80 ℃ for 2 hours, the stirring speed is 100r/min, and the muffle furnace calcination is performed at 500 ℃ for 2 hours.
In the preparation method of the sacrificial template agent coated gold nanoparticles, in step 4, purified water is used for washing for 5 times until the particles are neutral, and the particles are dried by an oven at a drying temperature of 80 ℃ for 2 hours.
An SEM photograph of the gold nanoparticles coated with the sacrificial template prepared by the method for preparing gold nanoparticles coated with the sacrificial template according to the present embodiment is shown in fig. 1, and it can be seen from fig. 1 that the prepared particles have uniform size, good dispersibility, and a particle size of about 25 nm.
An XRD curve of the sacrificial templating agent-coated gold nanoparticle prepared by the method for preparing a sacrificial templating agent-coated gold nanoparticle according to the present embodiment is shown in fig. 2, and as can be seen from fig. 2, diffraction peaks appear at 2 θ ═ 37.5 °, 44.5 °, 64.5 °, and 78 °, and there is no overlap phenomenon and no impurity peak, which indicates that the obtained product is a sacrificial templating agent-coated gold nanoparticle.
In the preparation method of the sacrificial template agent coated gold nanoparticles, urea is added as a catalyst (also as a precipitator), a uniform precipitation method is adopted, urea is unchanged at room temperature, after the urea solution and the gold nanoparticle solution are mixed, a mixed solution of F127 (polyoxyethylene polyoxypropylene) and P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide) is slowly dripped into the mixed solution under stirring at 50-60 ℃, when the temperature reaches about 75-85 ℃, the urea starts to perform slow hydrolysis reaction to generate ammonia water and carbon dioxide, and the ammonia water is rapidly decomposed into OH-Uniformly distributed in the solution, and an alkaline environment is provided, so that the high-molecular block copolymer starts to wrap the nano-gold particles to form crystal nuclei. Urea and OH-The existence in the reaction solution is in an equilibrium state, so the reaction rate of the gold particles wrapped by the high-molecular block copolymer is very slow, the nucleation rate of crystal nuclei is greater than the growth rate of the crystal nuclei, and the high-quality sacrificial template agent (high-molecular block copolymer mixture) wrapped gold nanoparticles with small size and uniform particle size can be obtained, and the particle size is about 50 nm.
The second embodiment is as follows:
a preparation method of gold nanoparticles wrapped by a sacrificial template agent comprises the following steps:
step 1, weighing chloroauric acid and sodium citrate according to parts by weight, dissolving the chloroauric acid and the sodium citrate into purified water with a certain volume according to a material-liquid ratio, and stirring uniformly to obtain a first mixed solution for later use;
step 2, weighing urea according to parts by weight, preparing a urea solution, adding the prepared urea solution into the first mixed solution prepared in the step 1, and uniformly stirring to obtain a second mixed solution for later use;
step 3, weighing F127 and P123 according to parts by weight, and dissolving the materials and the solution in purified water with a certain volume according to the material-to-solution ratio to obtain a mixed solution of the F127 and the P123 for later use;
and 4, slowly dropwise adding the mixed solution of F127 and P123 obtained in the step 3 into the second mixed solution prepared in the step 2, reacting for a certain time under the stirring condition, centrifugally collecting the obtained product, washing the obtained solid phase to be neutral, drying, and calcining in a muffle furnace to obtain the sacrificial template agent coated nano-gold particles.
In the preparation method of the sacrificial template-coated gold nanoparticle according to the embodiment, the sacrificial template-coated gold nanoparticle is prepared from 18.2 parts of chloroauric acid, 21.5 parts of sodium citrate, 38.7 parts of F127, 13.4 parts of P123 and 8.2 parts of urea.
In the preparation method of the sacrificial template agent-coated gold nanoparticles according to the embodiment, the material-liquid ratio of the mixture of chloroauric acid and sodium citrate to purified water in step 1 is 1.5:100g/ml, the stirring condition in step 1 is stirring at 20 ℃ for 40min, and the stirring speed is 60 r/min.
In the preparation method of the sacrificial template agent coated gold nanoparticles according to the embodiment, the concentration of the urea solution in the step 2 is 12 wt%, the stirring condition in the step 2 is stirring at 50 ℃ for 20min, and the stirring speed is 60 r/min.
In the preparation method of the gold nanoparticles wrapped by the sacrificial template in this embodiment, the material-to-liquid ratio of the mixture of F127 and P123 to the purified water in step 3 is 6:50 g/ml.
In the preparation method of the sacrificial template coated gold nanoparticles, in the step 4, stirring is performed at 80 ℃ for 3 hours, the stirring speed is 50r/min, and the muffle furnace calcination is performed at 500 ℃ for 2.5 hours.
In the preparation method of the sacrificial template agent coated gold nanoparticles, in step 4, purified water is used for washing for 3 times until the particles are neutral, and the particles are dried by an oven at 75 ℃ for 2 hours.
An SEM photograph of the gold nanoparticles coated with the sacrificial templating agent, which is prepared by the method for preparing gold nanoparticles coated with the sacrificial templating agent according to the embodiment, is shown in fig. 3, and it can be seen from fig. 3 that the prepared particles have uniform size and good dispersibility.
A TEM photograph of the gold nanoparticle coated with the sacrificial template prepared by the method for preparing a gold nanoparticle coated with the sacrificial template according to the embodiment is shown in fig. 4, and it can be seen from fig. 4 that the prepared gold nanoparticle coated with the sacrificial template has a regular spherical shape, good dispersibility, uniform coating, and a particle size of about 50 nm.
In the preparation method of the sacrificial template-coated gold nanoparticle according to this embodiment, a polymer block copolymer of F127 (polyoxyethylene polyoxypropylene) and P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide) is added as a template agent for coating the gold nanoparticle, and when chloroauric acid is reduced, a large amount of H is enriched on the surface of the gold nanoparticle+The high-molecular block copolymer is adsorbed and coated on the surfaces of the gold particles to form micelles, so that the agglomeration among the particles is prevented, and good dispersibility is obtained.
The third concrete implementation mode:
a preparation method of gold nanoparticles wrapped by a sacrificial template agent comprises the following steps:
step 1, weighing chloroauric acid and sodium citrate according to parts by weight, dissolving the chloroauric acid and the sodium citrate into purified water with a certain volume according to a material-liquid ratio, and stirring uniformly to obtain a first mixed solution for later use;
step 2, weighing urea according to parts by weight, preparing a urea solution, adding the prepared urea solution into the first mixed solution prepared in the step 1, and uniformly stirring to obtain a second mixed solution for later use;
step 3, weighing F127 and P123 according to parts by weight, and dissolving the materials and the solution in purified water with a certain volume according to the material-to-solution ratio to obtain a mixed solution of the F127 and the P123 for later use;
and 4, slowly dropwise adding the mixed solution of F127 and P123 obtained in the step 3 into the second mixed solution prepared in the step 2, reacting for a certain time under the stirring condition, centrifugally collecting the obtained product, washing the obtained solid phase to be neutral, drying, and calcining in a muffle furnace to obtain the sacrificial template agent coated nano-gold particles.
In the preparation method of the sacrificial template-coated gold nanoparticle according to the embodiment, the sacrificial template-coated gold nanoparticle is prepared from 10.8 parts of chloroauric acid, 23.2 parts of sodium citrate, 40.8 parts of F127, 16.1 parts of P123 and 9.1 parts of urea.
In the preparation method of the sacrificial template agent-coated gold nanoparticles according to the embodiment, the material-liquid ratio of the mixture of chloroauric acid and sodium citrate to purified water in step 1 is 1.3:100g/ml, the stirring condition in step 1 is stirring at 30 ℃ for 20min, and the stirring speed is 100 r/min.
In the preparation method of the sacrificial template agent coated gold nanoparticles according to the embodiment, the concentration of the urea solution in the step 2 is 11 wt%, the stirring condition in the step 2 is stirring at 55 ℃ for 15min, and the stirring speed is 100 r/min.
In the preparation method of the gold nanoparticles wrapped by the sacrificial template in this embodiment, the material-to-liquid ratio of the mixture of F127 and P123 to the purified water in step 3 is 5:50 g/ml.
In the preparation method of the sacrificial template coated gold nanoparticles, in the step 4, stirring is performed at 80 ℃ for 4 hours, the stirring speed is 100r/min, and the muffle furnace calcination is performed at 600 ℃ for 3 hours.
In the preparation method of the sacrificial template agent coated gold nanoparticles, in step 4, purified water is used for washing for 4 times until the particles are neutral, and the particles are dried by an oven at 70 ℃ for 2 hours.
An SEM photograph of the gold nanoparticles coated with the sacrificial template prepared by the method for preparing gold nanoparticles coated with the sacrificial template according to the present embodiment is shown in fig. 5, and it can be seen from fig. 5 that the prepared particles have uniform morphology, high dispersion degree, and small particle size, and the particle size is about 50 nm.
An XRD curve of the sacrificial templating agent-coated gold nanoparticle prepared by the method for preparing a sacrificial templating agent-coated gold nanoparticle according to this embodiment is shown in fig. 6, and it can be seen from the XRD characterization chart that diffraction peaks appear at 2 θ ═ 37.5 °, 44.5 °, 64.5 °, and 78 °, no overlap phenomenon occurs and no impurity peak appears, indicating that the obtained product is the sacrificial templating agent-coated gold nanoparticle.
Claims (10)
1. A sacrificial template agent coated nano-gold particle is characterized in that: the sacrificial template agent coated nano gold particles are mainly prepared from 2.6-18.2 parts by weight of chloroauric acid, 21.5-27.5 parts by weight of sodium citrate, 38.7-42.6 parts by weight of F127, 13.4-17.3 parts by weight of P123 and 8.2-10 parts by weight of urea.
2. The sacrificial templating agent-coated gold nanoparticle of claim 1, wherein: the sacrificial template agent coated nano-gold particle is prepared from 2.6 parts of chloroauric acid, 27.5 parts of sodium citrate, 42.6 parts of F127, 17.3 parts of P123 and 10 parts of urea.
3. The sacrificial templating agent-coated gold nanoparticle of claim 1, wherein: the sacrificial template agent coated nano-gold particle is prepared from 18.2 parts of chloroauric acid, 21.5 parts of sodium citrate, 38.7 parts of F127, 13.4 parts of P123 and 8.2 parts of urea.
4. The sacrificial templating agent-coated gold nanoparticle of claim 1, wherein: the sacrificial template agent coated nano gold particle is prepared from 10.8 parts of chloroauric acid, 23.2 parts of sodium citrate, 40.8 parts of F127, 16.1 parts of P123 and 9.1 parts of urea.
5. A method for preparing the gold nanoparticles coated with the sacrificial template according to any one of claims 1 to 4, wherein the method comprises the following steps: the method comprises the following steps:
step 1, weighing chloroauric acid and sodium citrate according to parts by weight, dissolving the chloroauric acid and the sodium citrate into purified water with a certain volume according to a material-liquid ratio, and stirring uniformly to obtain a first mixed solution for later use;
step 2, weighing urea according to parts by weight, preparing a urea solution, adding the prepared urea solution into the first mixed solution prepared in the step 1, and uniformly stirring to obtain a second mixed solution for later use;
step 3, weighing F127 and P123 according to parts by weight, and dissolving the materials and the solution in purified water with a certain volume according to the material-to-solution ratio to obtain a mixed solution of the F127 and the P123 for later use;
and 4, slowly dropwise adding the mixed solution of F127 and P123 obtained in the step 3 into the second mixed solution prepared in the step 2, reacting for a certain time under the stirring condition, centrifugally collecting the obtained product, washing the obtained solid phase to be neutral, drying, and calcining in a muffle furnace to obtain the sacrificial template agent coated nano-gold particles.
6. The method for preparing gold nanoparticles coated with sacrificial template according to claim 5, wherein the method comprises the following steps: in the step 1, the material-liquid ratio of the mixture of the chloroauric acid and the sodium citrate to the purified water is 1.2-1.5: 100g/ml, the stirring condition in the step 1 is that the mixture is stirred for 20-60 min at the temperature of 20-30 ℃, and the stirring speed is 50-200 r/min.
7. The method for preparing gold nanoparticles coated with sacrificial template according to claim 6, wherein the method comprises the following steps: the concentration of the urea solution in the step 2 is 10-12 wt%, the stirring condition in the step 2 is that the urea solution is stirred for 10-20 min at 50-60 ℃, and the stirring speed is 50-200 r/min.
8. The method for preparing gold nanoparticles coated with sacrificial template according to claim 7, wherein the method comprises the following steps: in the step 3, the material-liquid ratio of the mixture of F127 and P123 to the purified water is 4-6: 50 g/ml.
9. The method for preparing gold nanoparticles coated with sacrificial template according to claim 8, wherein the method comprises the following steps: in the step 4, stirring is carried out for 2-4 hours under the stirring condition of 75-85 ℃, the stirring speed is 50-200 r/min, and the muffle furnace calcination condition is 500-600 ℃ for 2-3 hours.
10. The method for preparing gold nanoparticles coated with sacrificial template according to claim 9, wherein the method comprises the following steps: and 4, washing the mixture for 3-5 times by using purified water until the mixture is neutral, and drying the mixture by using an oven at the drying temperature of 60-80 ℃ for 1-2 h.
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