CN108822302B - Janus nano-particle and preparation method and application thereof - Google Patents
Janus nano-particle and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a Janus nano particle and a preparation method and application thereof, wherein the nano particle is of an organic-inorganic two-phase structure, the organic phase is phenolic resin, and the inorganic phase is silicon dioxide; the preparation method comprises the steps of adding a silicon dioxide precursor, a phenolic resin precursor and a surfactant into a mixed solvent, and carrying out hydrothermal treatment to prepare the phenolic resin composite material; the nano-particles are used for preparing multi-structure nitrogen-doped carbon spheres. Compared with the prior art, the preparation method adopts a simple and easily-realized one-step synthesis route, prepares the uniformly-distributed and regularly-structured phenolic resin-silicon dioxide Janus nano-particles by copolymerizing the 3-aminophenol, the formaldehyde and the silicon dioxide primary particles in the TEOS, has wide raw material sources, low cost and simple and green preparation process, provides a new method for preparing the organic-inorganic two-phase Janus nano-particles with anisotropic structures and components, and is suitable for large-scale preparation and production.
Description
Technical Field
The invention belongs to the technical field of nano materials, and relates to Janus nano particles and a preparation method and application thereof.
Background
With the progress and development of nanotechnology, nanomaterials with desired morphology and physicochemical properties have been successfully prepared and have been extensively studied in various fields. Among various nanomaterials, composite nanostructures with two or more components are attracting increasing attention due to their particular properties and potential applications. Janus nano-particles have asymmetric composite nano-structures with two or more different physical or chemical properties, and are characterized in that the structure of the Janus nano-particles is asymmetric, and the Janus nano-particles comprise two or more substances in the composition. Since Gennes proposed this concept in 1992, Janus nanoparticles have been increasingly studied and widely used in sensing, magnetic field imaging (MRI), textiles, drug delivery, catalysis, etc. due to their unique physicochemical properties, such as optical properties, electromagnetic properties, catalytic properties, etc. Currently, there are three main methods for synthesizing Janus nanoparticles: masking, phase separation and self-assembly. The method can realize mass production of Janus nano particles in a liquid phase system through a self-assembly or heterogeneous separation wet chemical method, and has low cost, so that the method is widely applied.
The main problem in the preparation of Janus nanoparticles using wet chemistry is how to selectively modify the surface of the nanoparticles. One of the methods is as follows: au @ SiO was prepared using two different surfactants to achieve selective surface modification, for example, Chen used two different surfactants (4-thiophenylacetic acid, polyacrylic acid) to selectively modify the surface of gold nanoparticles, followed by selective deposition of a silica layer on the 4-thiophenylacetic acid (4-MPAA) sites2Janus nanoparticles (see the documents Chen T, Chen G, Xing S, et al2and ternary Ag-Au-SiO2nanoparticles[J]Chem. mater.,2010,22: 3826-. The sample prepared by the method has controllable appearance, and Janus structures which are difficult to obtain by other methods can be obtained, but the method still only stays in the laboratory research stage at present. The other method is a phase separation method, which mainly utilizes the difference of compatibility between substances, and two polymers which have poor compatibility but can be dissolved in the same solvent with strong volatility to carry out the processes of dissolution, emulsification and solvent volatilization, and the conditions are controlled to cause the phase separation between the substances to further form double-sided particles. The phase separation method has simple process and high yield, is expected to firstly realize industrialized mass production, but the particle size of the prepared nano particles is difficult to control, has wide particle size distribution range and is not beneficial to practical use.
Thus, while some progress has been made in the preparation of Janus nanoparticles, there are still many problems, such as long time consumption, high cost, low yield, etc.
Disclosure of Invention
The present invention aims to overcome the defects of the prior art, and provides a Janus nanoparticle, a preparation method and an application thereof.
The purpose of the invention can be realized by the following technical scheme:
a Janus nanoparticle is a nanoparticle with an organic-inorganic two-phase structure, wherein an organic phase is phenolic resin, and an inorganic phase is silicon dioxide.
The method for preparing Janus nanoparticles as claimed in claim 1, wherein the Janus nanoparticles are prepared by adding a silicon dioxide precursor, a phenolic resin precursor and a surfactant into a mixed solvent and performing hydrothermal treatment.
Further, the method comprises the steps of:
1) dissolving a surfactant in a mixed solvent;
2) sequentially adding a silicon dioxide precursor and a phenolic resin precursor, and stirring for 12-36h to obtain a mixed reaction solution;
3) and carrying out hydrothermal treatment on the mixed reaction liquid, and then separating and drying to obtain the phenolic resin-silicon dioxide Janus nano-particles.
Further, in the step 1), the surfactant is cetyl trimethyl ammonium bromide, and the mixed solvent comprises ethanol and water.
As the preferred technical scheme, the purity of the cetyl trimethyl ammonium bromide and the ethanol is more than 99.99 percent; in the mixed solvent, the ratio of alcohol to water is controlled to be 2: 5.
Further, in the step 1), a catalyst is also added into the mixed solvent, and the catalyst is ammonia water.
Preferably, the mass fraction of the ammonia water is 25%.
Further, in step 2), the silicon dioxide precursor is tetraethyl orthosilicate, and the phenolic resin precursor includes m-aminophenol and formaldehyde.
Further, in the step 2), the stirring temperature is 25-35 ℃ in the stirring process.
Further, in step 3), the process conditions of the hydrothermal treatment are as follows: the reaction temperature is 90-110 ℃, and the reaction time is 20-28 h.
Further, in the step 3), the separation is centrifugal separation, and in the centrifugal separation process, the centrifugal rotation speed is 10000-12000 r/min; the drying process comprises the following steps: drying at 50-70 deg.C for 20-28 h.
As a preferred technical scheme, the centrifugal separation process specifically comprises the following steps: dispersing the product in water, centrifuging to obtain a solid, and repeating for three times; the product was then dispersed in alcohol, centrifuged to give a solid, and repeated three times.
Use of Janus nanoparticles for the preparation of multi-structural nitrogen-doped carbon spheres. The prepared phenolic resin-silica Janus nanoparticles are calcined in air and washed in HF to achieve selective removal, enabling multi-structural m-aminophenol/formaldehyde (APF) resins and silica to be obtained. More importantly, the multi-structural phenolic-silica Janus nanoparticles can be further carbonized into a series of corresponding nitrogen-doped carbons with symmetric or asymmetric nanostructures. By designing a corresponding synthesis process, the multi-structure nitrogen-doped carbon spheres can be effectively and feasibly prepared.
In the present invention, the Janus nanoparticles are phenolic resin on one side and silica on the other side. The preparation method of the nano material comprises the steps of taking m-aminophenol/formaldehyde (APF) as a phenolic resin precursor, taking tetraethyl orthosilicate (TEOS) as a silicon dioxide source, taking Cetyl Trimethyl Ammonium Bromide (CTAB) as a surfactant and ammonia water as a reaction catalyst in a mixed solvent of water and ethanol, heating and stirring in a water bath at 25-35 ℃ for reaction for 12-36h, then transferring to a high-pressure kettle with a Teflon (Teflon) lining, heating at 90-110 ℃ for 20-28h under a static condition, and centrifugally drying after hydrothermal reaction is finished, wherein the finally obtained yellow solid is the phenolic resin-silicon dioxide Janus nano particles.
On the basis of the traditional stober method, the temporary Janus amphiphilic property of the nano particles is endowed by using the surfactant, the interface relation of phenolic resin particles and silicon dioxide particles is adjusted, and asymmetric coating is caused by using the speed difference of polymerization balling of the phenolic resin and the silicon dioxide in a stober system, so that the phenolic resin-silicon dioxide Janus nano particles are finally prepared.
Compared with the prior art, the invention has the following characteristics:
1) the invention adopts a simple and easily-realized one-step synthesis route, prepares the uniformly-distributed and regularly-structured phenolic resin-silicon dioxide Janus nano particles by copolymerizing 3-aminophenol, formaldehyde and silicon dioxide primary particles in TEOS, has wide raw material sources, low cost and simple and green preparation process, provides a new method for preparing organic-inorganic two-phase Janus nano particles with anisotropic structures and components, and is suitable for large-scale preparation and production;
2) according to the invention, a surfactant is introduced into the surface of the nanoparticle, the Janus structure is formed by utilizing the rate difference of polymerization balling of raw materials in a reaction system, the polymerization degree is further increased through high-temperature hydrothermal, the Janus nanoparticle with a stable structure is obtained, and different phenolic resin-silicon dioxide Janus nanoparticles can be prepared by changing the conditions of TEOS (tetraethyl orthosilicate) dosage, formaldehyde and m-aminophenol dosage, ammonia water dosage, CTAB (cetyltrimethyl ammonium bromide) dosage and the like, so that the conversion from Janus to core shell and double Janus structures is realized;
3) the Janus nano-particles prepared by the method are complete and uniform in appearance, have a typical Janus structure, and are controllable in particle size.
Drawings
FIG. 1 is a TEM image of phenolic resin-silica Janus nanoparticles prepared in example 1;
FIG. 2 is an SEM image of phenolic resin-silica Janus nanoparticles prepared in example 1;
FIG. 3 is a TEM image of the product of selective removal of phenolic resin-silica Janus nanoparticles of example 2;
FIG. 4 is a TEM image of phenolic resin-silica Janus nanoparticles prepared with different TEOS loadings in example 3;
FIG. 5 is a TEM image of phenolic resin-silica Janus nanoparticles made with different formaldehyde and m-aminophenol additions in example 3;
FIG. 6 is TEM spectra of phenolic resin-silica Janus nanoparticles prepared by different amounts of ammonia in example 3;
FIG. 7 is a TEM image of phenolic resin-silica Janus nanoparticles made with different CTAB addition in example 3.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
a low cost Janus nanoparticle having a phenolic resin on one side and silica on the other side; as a yellow powdery solid; is nontoxic.
The preparation method of the Janus nano-particles comprises the following steps:
1) constructing a reaction system: CTAB (0.1g) was first dissolved in a solution containing 4mL of absolute ethanol (EtOH) and 10mL of deionized water (H)2O) and stirred at room temperature for 10 minutes, 0.05mL of an aqueous ammonia solution (NH) was added4OH), stirring for 10 minutes;
2) adding a precursor: 1mL of TEOS was added to the reaction solution, and after half an hour of reaction, 0.14mL of formaldehyde solution (HCHO) and 0.1g of m-aminophenol (C) were added6H7ON) and stirred for 24 hours;
3) hydrothermal treatment: the product was transferred to a Teflon-lined autoclave and heated at 100 ℃ for 24 hours under static conditions;
4) centrifugal drying: and centrifuging to obtain a solid product, placing the solid product in an oven at 60 ℃, and preserving heat for 24 hours to finally obtain a solid material, namely the phenolic resin-silicon dioxide Janus nano-particles.
In the step 1), the purity of CTAB and absolute ethyl alcohol is more than 99.99 percent, the alcohol-water ratio is controlled to be 2:5, and the mass fraction of ammonia water is 25 percent.
In the step 2), stirring is carried out under heating, and the heating process comprises the following steps: the heating was carried out hydrothermally, with the temperature being kept at 30 ℃.
In the step 4), the centrifugation process specifically comprises the following steps: dispersing the product in water, centrifuging to obtain a solid, and repeating for three times; the product was then dispersed in alcohol, centrifuged to give a solid, and repeated three times. Wherein the centrifugal rotation speed is 10000-12000 r/min.
Fig. 1 and fig. 2 are a TEM spectrum and an SEM spectrum of the prepared phenolic resin-silica Janus nanoparticles, respectively. As can be seen from fig. 1 and 2: the prepared phenolic resin-silicon dioxide Janus nano-particles are asymmetric two-phase structure particles, namely Janus structures.
Example 2:
the phenolic resin-silica Janus nanoparticles prepared in example 1 were calcined in air, and the phenolic resin was selectively removed to obtain different morphologies as shown by a and c in fig. 3, and it can be seen that the obtained silica nanoparticles had a special structure with hemispherical head and a long handle composed of silica embedded in APF resin. In addition, the phenolic resin-silica Janus nanoparticles prepared in example 1 were washed in 15 wt% HF for selective removal and the silica was etched away to give different morphologies as shown by b, d in fig. 3, which can be seen as a sphere with cavities in the phenolic resin morphology.
Example 3:
the reaction conditions for preparing the phenolic resin-silica Janus nanoparticles in example 1, such as TEOS addition, formaldehyde and m-aminophenol addition, ammonia addition, CTAB addition, and the like, were changed, and the other conditions were the same as example 1, to prepare different phenolic resin-silica Janus nanoparticles, and the results are shown in fig. 4 to 7.
In FIG. 4, a, b, c, d, and e correspond to the amounts of TEOS added, respectively, of 0mL, 0.1mL, 0.5mL, 1mL, and 2 mL. As can be seen from fig. 4: with the increase of TEOS amount, the phenolic resin-silicon dioxide nano composite structure is converted into an eccentric structure from a core-shell structure, and then is in a Janus structure until the structure is changed into a pure silicon dioxide microsphere.
In FIG. 5, a, b, c and d correspond to 0mL of formaldehyde and 0g of m-aminophenol, 0.07mL of formaldehyde and 0.05g of m-aminophenol, 0.14mL of formaldehyde and 0.1g of m-aminophenol, and 0.28mL of formaldehyde and 0.2g of m-aminophenol, respectively. As can be seen from fig. 5: adding no formaldehyde and m-aminophenol, and enabling TEOS to react to generate silicon dioxide microspheres; after the formaldehyde and the m-aminophenol are added, the phenolic resin part is gradually enlarged along with the increase of the input amount, and finally, the silicon dioxide can be coated to form an eccentric core-shell structure.
In FIG. 6, a, b and c correspond to the amounts of ammonia water added, respectively, of 0.01mL, 0.05mL and 1 mL. As can be seen from fig. 6: the ammonia firstly affects the phenolic resin and then the silicon dioxide, namely when the input amount of the ammonia is less, the added ammonia is consumed by the synthesis of the phenolic resin, when the input amount of the ammonia is increased, the phenolic resin is not changed greatly, and the silicon dioxide is increased along with the increase of the input amount of the ammonia.
In FIG. 7, a, b, c and d correspond to CTAB added amounts of 0.1g, 0.05g, 0.035g and 0.025g, respectively. As can be seen from fig. 7: when the CTAB addition was reduced to 0.05g, most of the structure was Janus two-phase structure, but a complex of silica microspheres with two phenolic resins attached to the left and right sides appeared. As the CTAB addition continues to decrease, the complex structure gradually increases until the respective microsphere structures of silica and phenolic resin are formed.
Example 4:
a Janus nanoparticle is a nanoparticle with an organic-inorganic two-phase structure, wherein an organic phase is phenolic resin, and an inorganic phase is silicon dioxide.
The preparation method of the Janus nano-particles comprises the steps of adding a silicon dioxide precursor, a phenolic resin precursor and a surfactant into a mixed solvent, and carrying out hydrothermal treatment to prepare the Janus nano-particles.
The preparation method comprises the following steps:
1) dissolving a surfactant (cetyl trimethyl ammonium bromide) in a mixed solvent of ethanol and water, and adding a catalyst ammonia water;
2) sequentially adding a silicon dioxide precursor (tetraethyl orthosilicate) and a phenolic resin precursor (m-aminophenol and formaldehyde), and stirring at 25 ℃ for 36 hours to obtain a mixed reaction solution;
3) carrying out hydrothermal treatment on the mixed reaction liquid, wherein the process conditions of the hydrothermal treatment are as follows: the reaction temperature is 90 ℃, and the reaction time is 28 h; and then centrifugally separating at the rotating speed of 10000r/min, and drying at 70 ℃ for 20h to obtain the phenolic resin-silicon dioxide Janus nano-particles.
The nano-particles are used for preparing multi-structure nitrogen-doped carbon spheres.
Example 5:
a Janus nanoparticle is a nanoparticle with an organic-inorganic two-phase structure, wherein an organic phase is phenolic resin, and an inorganic phase is silicon dioxide.
The preparation method of the Janus nano-particles comprises the steps of adding a silicon dioxide precursor, a phenolic resin precursor and a surfactant into a mixed solvent, and carrying out hydrothermal treatment to prepare the Janus nano-particles.
The preparation method comprises the following steps:
1) dissolving a surfactant (cetyl trimethyl ammonium bromide) in a mixed solvent of ethanol and water, and adding a catalyst ammonia water;
2) sequentially adding a silicon dioxide precursor (tetraethyl orthosilicate) and a phenolic resin precursor (m-aminophenol and formaldehyde), and stirring at 35 ℃ for 12 hours to obtain a mixed reaction solution;
3) carrying out hydrothermal treatment on the mixed reaction liquid, wherein the process conditions of the hydrothermal treatment are as follows: the reaction temperature is 110 ℃, and the reaction time is 20 h; and then carrying out centrifugal separation at the rotating speed of 12000r/min, and drying for 28h at the temperature of 50 ℃ to prepare the phenolic resin-silicon dioxide Janus nano-particles.
The nano-particles are used for preparing multi-structure nitrogen-doped carbon spheres.
Example 6:
a Janus nanoparticle is a nanoparticle with an organic-inorganic two-phase structure, wherein an organic phase is phenolic resin, and an inorganic phase is silicon dioxide.
The preparation method of the Janus nano-particles comprises the steps of adding a silicon dioxide precursor, a phenolic resin precursor and a surfactant into a mixed solvent, and carrying out hydrothermal treatment to prepare the Janus nano-particles.
The preparation method comprises the following steps:
1) dissolving a surfactant (cetyl trimethyl ammonium bromide) in a mixed solvent of ethanol and water, and adding a catalyst ammonia water;
2) sequentially adding a silicon dioxide precursor (tetraethyl orthosilicate) and a phenolic resin precursor (m-aminophenol and formaldehyde), and stirring at 30 ℃ for 24 hours to obtain a mixed reaction solution;
3) carrying out hydrothermal treatment on the mixed reaction liquid, wherein the process conditions of the hydrothermal treatment are as follows: the reaction temperature is 100 ℃, and the reaction time is 24 hours; and then carrying out centrifugal separation at the rotating speed of 11000r/min, and drying for 24h at the temperature of 60 ℃ to obtain the phenolic resin-silicon dioxide Janus nano-particles.
The nano-particles are used for preparing multi-structure nitrogen-doped carbon spheres.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (2)
1. A preparation method of Janus nano-particles is characterized in that,
the nano particles are of an organic-inorganic two-phase structure, the organic phase is phenolic resin, and the inorganic phase is silicon dioxide;
the preparation method comprises the steps of adding a silicon dioxide precursor, a phenolic resin precursor and a surfactant into a mixed solvent, and carrying out hydrothermal treatment to prepare the phenolic resin composite material;
the preparation method comprises the following steps:
1) dissolving a surfactant in a mixed solvent;
2) sequentially adding a silicon dioxide precursor and a phenolic resin precursor, and stirring for 12-36h to obtain a mixed reaction solution;
3) carrying out hydro-thermal treatment on the mixed reaction liquid, and then separating and drying to obtain phenolic resin-silicon dioxide Janus nano particles;
in the step 1), the surfactant is cetyl trimethyl ammonium bromide, and the mixed solvent comprises ethanol and water;
in the step 1), a catalyst is also added into the mixed solvent, and the catalyst is ammonia water;
in the step 2), the silicon dioxide precursor is tetraethyl orthosilicate, and the phenolic resin precursor comprises m-aminophenol and formaldehyde;
in the step 2), the stirring temperature is 25-35 ℃ in the stirring process;
in the step 3), the process conditions of the hydrothermal treatment are as follows: the reaction temperature is 90-110 ℃, and the reaction time is 20-28 h;
the ammonia water is added in an amount of 0.05mL, the tetraethyl orthosilicate is added in an amount of 0.5-1mL, the m-aminophenol is added in an amount of 0.1-0.2g, the formaldehyde is added in a formaldehyde solution in an amount of 0.14-0.28mL, and the hexadecyl trimethyl ammonium bromide is added in an amount of 0.05-0.1 g.
2. The method as claimed in claim 1, wherein the step 3) is a centrifugal separation, and the centrifugal speed is 10000-; the drying process comprises the following steps: drying at 50-70 deg.C for 20-28 h.
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| US20140030527A1 (en) * | 2010-12-22 | 2014-01-30 | Universite Bordeaux 1 | Dissymmetric particles (janus particles), and method for synthesizing same by means of bipolar electrochemistry |
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| CN102133802A (en) * | 2010-01-21 | 2011-07-27 | 中国科学院化学研究所 | Flaky material with front and back surfaces having different properties and preparation method thereof |
| US20140030527A1 (en) * | 2010-12-22 | 2014-01-30 | Universite Bordeaux 1 | Dissymmetric particles (janus particles), and method for synthesizing same by means of bipolar electrochemistry |
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