CN110280759B - Preparation method of micro-nano core-shell material and device for preparing micro-nano core-shell material - Google Patents
Preparation method of micro-nano core-shell material and device for preparing micro-nano core-shell material Download PDFInfo
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Abstract
The invention belongs to the technical field of micro-nano-grade material preparation, and particularly relates to a preparation method of a micro-nano-grade core-shell material and a device for preparing the micro-nano-grade core-shell material. The invention provides a preparation method of a micro-nano core-shell material, in the preparation method, a solution containing micro-nano metal particles and a metal ion solution are mixed under the condition that the Reynolds number is not less than 2300, and then are dispersed by an atomization method, the solution containing the micro-nano metal particles is fully contacted with the metal ion solution, metal ions form a metal coating layer on the surface of the micro-nano metal particles, so that the dispersed micro-nano core-shell material is obtained, the dispersion degree of the core-shell material can be controlled by the preparation method, the continuous production is realized, and the particle size of the micro-nano core-shell material can be controlled by adjusting the particle size of the micro-nano metal particles and the concentration of the metal ion solution.
Description
Technical Field
The invention belongs to the technical field of micro-nano-grade material preparation, and particularly relates to a preparation method of a micro-nano-grade core-shell material and a device for preparing the micro-nano-grade core-shell material.
Background
The core-shell structure of the core-shell material is an ordered assembly structure formed by coating one material with another material through chemical bonds or other acting forces. The shell coated outside the particle can change the surface property of the core material and endow the particle with optical, electric, magnetic, catalytic and other properties, such as changing the surface charge of the particle, endowing the particle with functionality, enhancing the surface reaction activity, improving the stability of the particle and the like.
Core-shell materials generally consist of a central core and a shell that is coated on the outside. The core-shell material can be polymers, inorganic substances, metals and the like. With the continuous development of core-shell materials, the definition of the core-shell materials becomes more extensive. The core-shell material in a broad sense not only comprises a composite material with a core-shell structure, which is composed of the same or different substances, but also comprises hollow spheres, microcapsules and other materials. The appearance of the core-shell material is generally spherical particles, and can be in other shapes. The core-shell structure powder material cannot be simply considered as a powder product using a powder surface modification technique.
Due to the special geometric structure of the core-shell material, compared with a single element, the core-shell material can generally change the physical and chemical properties thereof, and has a particularly wide application prospect, so that great research interest is aroused. The surface of the functionalized particles can regulate and control various properties of the material, such as mechanics, electricity, optics, magnetism and the like. Firstly, the core-shell material corresponds to the core layer and shell layer properties of the material core layer and shell layer single-layer material, and the type of the core-shell material can be adjusted to control the total properties of the composite material. And secondly, because the properties of the core-shell material are related to the thicknesses of the core layer and the shell layer, the properties of the core-shell material can be adjusted by controlling the preparation process and further controlling the thicknesses of the core layer and the shell layer. Third, core-shell nanocomposites have the potential to achieve more desirable properties due to their more tunable structure for nanoparticles. In addition, the particles can be protected from external chemical and physical changes by coating the surfaces of the particles. In the last decade, core-shell structured materials with specific structural, optical and surface properties in nanometer and submicron scale have been prepared by various powder technologies. Many of these materials have been used in many areas of coatings, electronics, catalysis, separations, diagnostics, and the like. The core-shell structure integrates the properties of the inner material and the outer material due to the unique structural characteristics of the core-shell structure, and mutually supplements the respective defects, so that the core-shell structure is an important research direction of the composite powder material in recent years and has wide application prospects in various fields.
However, in the continuous preparation of the core-shell material, the particle size of the core-shell material is difficult to control, agglomeration is easy to occur, and the continuous production is not facilitated.
Disclosure of Invention
In view of the above, the invention provides a method and a device for preparing a micro-nano core-shell material, which are used for solving the problems that the particle size is difficult to control, agglomeration is easy to occur and continuous production is not facilitated in the continuous preparation of the core-shell material.
The specific technical scheme of the invention is as follows:
a preparation method of a micro-nano core-shell material comprises the following steps:
mixing a solution containing micro-nano metal particles and a metal ion solution under the condition that the Reynolds number is not less than 2300, and then carrying out atomization and dispersion to form a metal coating layer on the surface of the micro-nano metal particles by the metal ions to obtain a micro-nano core-shell material;
and the metal of the micro-nano metal particles can perform a displacement reaction with the metal ions.
Preferably, the metal of the micro-nano metal particles is selected from one or more of copper, antimony, zinc and nickel;
preferably, the solvent in the solution containing the micro-nano metal particles is selected from deionized water, alcohol organic solvents or ketone organic solvents.
Preferably, the electronegativity of the metal elements in the metal ion solution is stronger than that of the metal elements in the micro-nano metal particles;
the metal ions of the metal ion solution are preferably silver ions.
Preferably, the reynolds number of the mixing is 5000 or more.
Preferably, after the atomization and dispersion, the method further comprises:
the collection was performed under negative pressure.
The invention also provides a device for preparing the micro-nano core-shell material, which comprises the following steps: a gas inlet, a turbulence forming pipe, a first container, a second container, a first branch pipe and a second branch pipe;
the gas inlet is communicated with the first end of the turbulence forming pipe, and the first container and the second container are respectively used for containing a solution containing micro-nano metal particles and a metal ion solution;
first ends of the first branch pipe and the second branch pipe are respectively positioned below the liquid level of the first container and the second container, and second ends of the first branch pipe and the second branch pipe are communicated with the turbulence forming pipe;
and the metal of the micro-nano metal particles can perform a displacement reaction with the metal ions.
Preferably, the second end of the turbulence forming tube is provided with an atomizing structure.
Preferably, the method further comprises the following steps: a collection container;
the collection vessel is in communication with the second end of the turbulence creating tube.
Preferably, the gas inlet is connected with a gas regulator;
the gas in the gas regulator is inert gas and/or nitrogen.
In summary, the invention provides a preparation method of a micro-nano core-shell material, which comprises the following steps: mixing a solution containing micro-nano metal particles and a metal ion solution under the condition that the Reynolds number is not less than 2300, and then carrying out atomization and dispersion to form a metal coating layer on the surface of the micro-nano metal particles by the metal ions to obtain a micro-nano core-shell material; and the metal of the micro-nano metal particles can perform a displacement reaction with the metal ions. According to the preparation method, a solution containing micro-nano metal particles and a metal ion solution are mixed under the condition that the Reynolds number is not less than 2300, and then are dispersed by an atomization method, the solution containing the micro-nano metal particles is fully contacted with the metal ion solution, and metal ions form a metal coating layer on the surface of the micro-nano metal particles, so that the dispersed micro-nano core-shell material is obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
Fig. 1 is a schematic structural diagram of an apparatus for preparing a micro-nano core-shell material provided by the invention;
illustration of the drawings: 1. a solution containing micro-nano metal particles; 2. a metal ion solution; 3. a micro-nano core-shell material; 4. a turbulence-forming tube; 5. a first control valve; 6. a second control valve; 7. inert gas and/or nitrogen; 8. and (4) a vent.
Detailed Description
The invention provides a preparation method of a micro-nano core-shell material and a device for preparing the micro-nano core-shell material, which are used for solving the technical defects in the prior art.
The technical solutions in the embodiments of the present invention will be 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.
The embodiment of the preparation method of the micro-nano core-shell material provided by the invention comprises the following steps:
mixing a solution containing micro-nano metal particles and a metal ion solution under the condition that the Reynolds number is not less than 2300, and then carrying out atomization and dispersion to form a metal coating layer on the surface of the micro-nano metal particles by the metal ions to obtain a micro-nano core-shell material;
wherein, the metal of the micro-nano metal particles can generate displacement reaction with metal ions.
According to the preparation method, a solution containing micro-nano metal particles and a metal ion solution are mixed under the condition that the Reynolds number is not less than 2300, and then are dispersed through an atomization method, the solution containing the micro-nano metal particles is fully contacted with the metal ion solution, metal ions form a metal coating layer on the surface of the micro-nano metal particles, so that the dispersed micro-nano core-shell material is obtained.
In the embodiment of the invention, the metal of the micro-nano metal particles is selected from one or more of copper, antimony, zinc and nickel.
The solvent in the solution containing the micro-nano metal particles is selected from deionized water, alcohol organic solvents or ketone organic solvents, and preferably deionized water, ethanol or acetone.
In the embodiment of the invention, the electronegativity of metal elements in the metal ion solution is stronger than that of metal elements in the micro-nano metal particles;
the metal ions of the metal ion solution are preferably silver ions. The metal ion solution containing silver ions is preferably a silver potassium cyanide solution or a silver ammonia solution.
In the embodiment of the present invention, the reynolds number for mixing is 5000 or more.
In the embodiment of the present invention, after the atomization and dispersion, the method further includes:
the collection was performed under negative pressure. The collection is carried out under the negative pressure condition, the atomization and dispersion process is also under the negative pressure condition, the solute concentration and the reaction speed can be improved, and the solvent evaporation in the obtained micro-nano core-shell material solution is facilitated.
According to the preparation method, reactants are fully mixed, atomized and dispersed by adjusting the Reynolds number of the mixing condition, so that the aim of continuously preparing the micro-nano core-shell material with high dispersibility is fulfilled.
In the embodiment of the invention, the size of the micro-nano core-shell material is 7 nm-200 μm, the diameter of the core layer is 5 nm-100 μm, and the thickness of the shell layer is 1 nm-50 μm.
In the prior art, the traditional method of centrifugally collecting after a micro-nano core-shell material is prepared by using solution type chemistry cannot meet the requirement. According to the preparation method, a solution containing micro-nano metal particles and a metal ion solution are mixed under the condition that the Reynolds number is not less than 2300, and then are dispersed through an atomization method, the solution containing the micro-nano metal particles is fully contacted with the metal ion solution, metal ions form a metal coating layer on the surface of the micro-nano metal particles, and then are collected under the negative pressure condition, so that the dispersed micro-nano core-shell material is obtained.
The above is a detailed description of an embodiment of a method for preparing a micro-nano core-shell material provided in an embodiment of the present invention, and an embodiment of an apparatus for preparing a micro-nano core-shell material provided in an embodiment of the present invention is described in detail below.
Fig. 1 is a schematic structural diagram of an apparatus for preparing a micro-nano core-shell material according to the present invention.
The embodiment of the device for preparing the micro-nano core-shell material provided by the invention comprises the following steps: an air inlet, a turbulence forming pipe 4, a first container, a second container, a first branch pipe and a second branch pipe;
the air inlet is communicated with the first end of the turbulence forming pipe 4, and the first container and the second container are respectively used for containing a solution 1 containing micro-nano metal particles and a metal ion solution 2;
the first ends of the first branch pipe and the second branch pipe are respectively positioned below the liquid level of the first container and the liquid level of the second container, and the second ends of the first branch pipe and the second branch pipe are communicated with the turbulence forming pipe 4;
wherein, the metal of the micro-nano metal particles can generate displacement reaction with metal ions.
When the device for preparing the micro-nano core-shell material is used, inert gas and/or nitrogen 7 can be introduced into the turbulence forming pipe 4 through the air inlet, a principle that high-speed fluid in a Bernoulli equation generates negative pressure is utilized, the solution 1 containing the micro-nano metal particles and the metal ion solution 2 are respectively sucked into the turbulence forming pipe 4 from the first container and the second container through the first branch pipe and the second branch pipe, the sucked solution 1 containing the micro-nano metal particles and the metal ion solution 2 form turbulence in the turbulence forming pipe 4 under extremely high air velocity, the solution 1 containing the micro-nano metal particles and the metal ion solution 2 are fully contacted and subjected to displacement reaction, metal ions deposit metal layers on the surfaces of the micro-nano metal particles to obtain the dispersed micro-nano core-shell material 3, reactants can be fully mixed, and the dispersion degree of the core-shell material 3 can be controlled, and a large amount of continuous production is realized, and the particle size of the micro-nano core-shell material 3 can be controlled by adjusting the particle size of the micro-nano metal particles and the concentration of the metal ion solution.
The above is a detailed description of an embodiment of an apparatus for preparing a micro-nano core-shell material according to an embodiment of the present invention, and another embodiment of an apparatus for preparing a micro-nano core-shell material according to an embodiment of the present invention is described in detail below.
Referring to fig. 1, another embodiment of an apparatus for preparing a micro-nano core-shell material according to an embodiment of the present invention includes: an air inlet, a turbulence forming pipe 4, a first container, a second container, a first branch pipe and a second branch pipe;
the air inlet is communicated with the first end of the turbulence forming pipe 4, and the first container and the second container are respectively used for containing a solution 1 containing micro-nano metal particles and a metal ion solution 2;
the first ends of the first branch pipe and the second branch pipe are respectively positioned below the liquid level of the first container and the liquid level of the second container, and the second ends of the first branch pipe and the second branch pipe are communicated with the turbulence forming pipe 4;
wherein, the metal of the micro-nano metal particles can generate displacement reaction with metal ions.
In an embodiment of the invention, the second end of the turbulence creating tube 4 is provided with an atomizing structure.
In the embodiment of the invention, the method further comprises the following steps: a collection container;
the collecting container communicates with the second end of the turbulence creating tube 4.
In the embodiment of the invention, the gas inlet is connected with the gas regulator; the gas in the gas regulator is inert gas and/or nitrogen 7. The inert gas comprises argon.
The micro-nano core-shell material 3 obtained by reaction can be fully atomized and dispersed by the arrangement of the atomization structure, the micro-nano core-shell material 3 is collected by the collection container, negative pressure can be pumped in advance by the collection container, so that the micro-nano core-shell material 3 is easier to atomize and disperse when entering the collection container, the micro-nano core-shell material 3 collected by the collection container is highly uniformly dispersed, and the dispersibility is better. The temperature of the collection vessel can be adjusted as desired.
In an embodiment of the present invention, a first control valve 5 and a second control valve 6 may be provided at the first end of the turbulence creating pipe 4 and the air vent 8 of the collecting device for controlling the flow rate of the fluid.
In the device for preparing the micro-nano core-shell material, each part can be flexibly disassembled and assembled, and more functions can be added.
For a further understanding of the invention, reference will now be made in detail to the following examples.
Example 1
The first container contains ethanol solution containing nano-copper particles, and the second container contains silver ammonia solution. Introducing mixed gas of nitrogen and argon into the turbulence forming pipe, wherein the Reynolds number of the mixed gas reaches 4000, sucking ethanol solution containing nano copper particles and silver-ammonia solution into the turbulence forming pipe under the action of negative pressure generated by high flow rate, enabling the fluid in the turbulence forming pipe to form turbulence and fully mix, performing displacement reaction, depositing silver on the surface of the nano copper particles, pumping a collecting container into a negative pressure of 0.05MPa in advance, atomizing and dispersing the micro nano core-shell material solution when the micro core-shell material solution enters, depositing the micro core-shell material solution on the inner wall of the collecting container, and finally collecting the micro core-shell material solution on the inner wall of the collecting container to obtain the micro core-shell material solution, namely the nano silver. Wherein the diameter of copper in the nano silver-coated copper particles is 100nm, and the thickness of silver is 10 nm.
Example 2
The first container contains ethanol solution containing nano-copper particles, and the second container contains silver potassium cyanide solution. Introducing mixed gas of nitrogen and argon into the turbulence forming pipe, wherein the Reynolds number of the mixed gas reaches 4000, sucking ethanol solution containing nano copper particles and silver-ammonia solution into the turbulence forming pipe under the action of negative pressure generated by high flow rate, enabling the fluid in the turbulence forming pipe to form turbulence and fully mix, performing displacement reaction, depositing silver on the surface of the nano copper particles, pumping a collecting container into a negative pressure of 0.05MPa in advance, atomizing and dispersing the micro nano core-shell material solution when the micro core-shell material solution enters, depositing the micro core-shell material solution on the inner wall of the collecting container, and finally collecting the micro core-shell material solution on the inner wall of the collecting container to obtain the micro core-shell material solution, namely the nano silver. Wherein the diameter of copper in the nano silver-coated copper particles is 200nm, and the thickness of silver is 10 nm.
Example 3
The first container holds propanol solution containing nano-copper particles, and the second container holds silver ammonia solution. Introducing mixed gas of nitrogen and argon into the turbulence forming pipe, wherein the Reynolds number of the mixed gas reaches 5000, sucking ethanol solution containing nano copper particles and silver-ammonia solution into the turbulence forming pipe under the action of negative pressure generated by high flow rate, enabling the fluid in the turbulence forming pipe to form turbulence and fully mix, performing displacement reaction, depositing silver on the surface of the nano copper particles, pumping a collecting container into a negative pressure of 0.05MPa in advance, atomizing and dispersing the micro nano core-shell material solution when the micro core-shell material solution enters, depositing the micro core-shell material solution on the inner wall of the collecting container, and finally collecting the micro core-shell material solution on the inner wall of the collecting container to obtain the nano silver-coated copper particle solution. Wherein the diameter of copper in the nano silver-coated copper particles is 50nm, and the thickness of silver is 5 nm.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A preparation method of a micro-nano core-shell material is characterized by comprising the following steps:
introducing inert gas and/or nitrogen into a turbulence forming pipe to form negative pressure, sucking a solution containing micro-nano metal particles in a first container and a solution containing metal ions in a second container into the turbulence forming pipe to mix under the condition that the Reynolds number is not less than 2300, then carrying out atomization and dispersion, forming metal coating layers on the surfaces of the micro-nano metal particles by the metal ions, and collecting under the negative pressure condition to obtain a micro-nano core-shell material;
and the metal of the micro-nano metal particles can perform a displacement reaction with the metal ions.
2. The preparation method according to claim 1, wherein the metal of the micro-nano scale metal particles is selected from one or more of copper, antimony, zinc and nickel.
3. The preparation method according to claim 1, wherein the solvent in the solution containing the micro-nano-scale metal particles is selected from deionized water, alcohol organic solvents or ketone organic solvents.
4. The preparation method according to claim 2, wherein the metal element in the metal ion solution has stronger electronegativity than the metal element in the micro-nano-scale metal particles;
the metal ions of the metal ion solution are silver ions.
5. The production method according to claim 1, wherein the reynolds number of the mixing is 5000 or more.
6. A device for preparing a micro-nano core-shell material is characterized by comprising the following steps: the device comprises an air inlet, a turbulence forming pipe, a first container, a second container, a first branch pipe, a second branch pipe and a collecting container in a negative pressure state;
the gas inlet is communicated with the first end of the turbulence forming pipe, and the first container and the second container are respectively used for containing a solution containing micro-nano metal particles and a metal ion solution;
first ends of the first branch pipe and the second branch pipe are respectively positioned below the liquid level of the first container and the second container, and second ends of the first branch pipe and the second branch pipe are communicated with the turbulence forming pipe;
wherein, the metal of the micro-nano metal particles can perform a displacement reaction with the metal ions;
the second end of the turbulence forming pipe is provided with an atomizing structure;
the gas inlet is connected with a gas regulator;
the gas in the gas regulator is inert gas and/or nitrogen;
the collection vessel is in communication with the second end of the turbulence creating tube;
and the gas regulator feeds inert gas and/or nitrogen into the turbulence forming pipe to form negative pressure, and the solution containing the micro-nano metal particles in the first container and the solution containing the metal ions in the second container are sucked into the turbulence forming pipe to be mixed.
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