CN110054192B - Preparation method of monodisperse ultra-small silicon dioxide nanoparticles - Google Patents
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Abstract
The invention provides a monodisperse ultra-small silicon dioxide nano particle and a preparation method thereof, belonging to the technical field of silicon dioxide preparation. The preparation method provided by the invention comprises the following steps: mixing SiO2Mixing ball, water and protective agent to SiO2Coating the balls to obtain a coating mixture; and mixing the coating mixture with an etching agent, and carrying out etching reaction under the condition of stirring at room temperature to obtain the monodisperse ultra-small silicon dioxide nanoparticles. The preparation method provided by the invention is simple and low in energy consumption, the etchant can enter the silicon dioxide under the condition of stirring at room temperature, a non-hollow porous structure can be formed in the silicon dioxide, the monodisperse ultra-small silicon dioxide nanoparticles can be prepared after the structure collapses, and the prepared silicon dioxide nanoparticles have good dispersibility.
Description
Technical Field
The invention relates to the technical field of silicon dioxide preparation, in particular to monodisperse ultra-small silicon dioxide nanoparticles and a preparation method thereof.
Background
The silicon dioxide nano-particles have small particle size, so the silicon dioxide nano-particles have large specific surface area, strong surface adsorption force, large surface energy, good dispersibility, easy surface modification and good optical transmittance. The nano silicon dioxide is widely applied to various fields as an additive, a catalyst carrier, a decoloring agent, a delustering agent, a plastic filler, a polishing agent, cosmetics, a medicine carrier and the like due to the excellent stability, thickening property and thixotropy of the nano silicon dioxide. Compared with large-size silica, the ultra-small silica particles have obvious advantages, for example, in the field of medicine, drugs loaded by small silica particles can enter cells more easily, and the utilization rate of the drugs is improved; in the field of materials, smaller silica is added to epoxy resins, and due to the high flowability and small size effect of silica, the wear resistance and surface finish of the material are improved. Therefore, the mass production of monodisperse, ultra-small silica particles is of great significance to the relevant field.
At present, the monodisperse and uniform-particle-size silicon dioxide particles are mainly adopted
The method is characterized in that tetraethoxysilane is catalyzed and hydrolyzed under the condition of taking ammonia water as a catalyst to obtain silicon dioxide particles with uniform particle size. But the particle size of the silica particles produced is generally greater than 50 nm. A plurality of researchers at home and abroad
The method is improved or changed into other methods to prepare the ultra-small silicon dioxide particles. For example, Davis T M, Snyder M A, Krohn J E, et]Hydrolysis of tetraethyl orthosilicate using lysine in Chemistry of materials,2006,18(25): 5814-; finnie K S, Bartlett J R, Barbet C J A, et al.Formation of silico and microorganisms [ J].Langmuir the Acs Journal of Surfaces&Colloidal, 2007,23(6):3017 ", prepared silica particles of 11nm under alkaline conditions using emulsion polymerization; silica particles of 5nm were prepared under acidic conditions. However, these methods have certain limitations, such as complicated operation, long reaction time, high reaction temperature, poor silica dispersibility, difficult particle size control, high preparation cost, and difficulty in mass production.
Therefore, how to solve the problems of high cost, complex preparation process, high energy consumption, low yield and the like in the preparation of the ultra-small silicon dioxide in the prior art becomes an important technical problem to be solved by technical personnel in the field.
Disclosure of Invention
The invention aims to provide monodisperse ultra-small silicon dioxide nano particles and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of monodisperse ultra-small silicon dioxide nanoparticles, which comprises the following steps:
mixing SiO2Mixing ball, water and protective agent to SiO2Coating the balls to obtain a coating mixture;
and mixing the coating mixture with an etching agent, and carrying out etching reaction under the condition of stirring at room temperature to obtain the monodisperse ultra-small silicon dioxide nanoparticles.
Preferably, the SiO2The particle size of the spheres is 50 nm-2 μm.
Preferably, the protective agent is polyvinylpyrrolidone, polyol, oleic acid or aromatic alcohol ester.
Preferably, the etchant is sodium hydroxide, potassium hydroxide or sodium borohydride.
Preferably, the SiO2The dosage ratio of the ball, the water, the protective agent and the etching agent is 0.3-1.8 g, 10-100 mL, 0.2-1.5 g and 0.2-1.2 g.
Preferably, the etching reaction time is 50 min-10 h.
Preferably, the stirring speed is 300-600 rpm.
Preferably, the coating is carried out under the condition of stirring, the speed of stirring is 300-600 rpm, and the time is 2-5 h.
Preferably, after the etching reaction, the method further comprises sequentially performing centrifugal washing and drying on the solid product of the etching reaction.
The invention also provides the monodisperse ultra-small silicon dioxide nano-particles prepared by the preparation method in the technical scheme, and the particle size of the monodisperse ultra-small silicon dioxide nano-particles is 3-20 nm.
The invention provides a preparation method of monodisperse ultra-small silicon dioxide nanoparticles, which comprises the following steps: mixing SiO2Mixing ball, water and protective agent to SiO2Coating the balls to obtain a coating mixture; and mixing the coating mixture with an etching agent, and carrying out etching reaction under the condition of stirring at room temperature to obtain the monodisperse ultra-small silicon dioxide nanoparticles. The invention uses SiO2Mixing the ball, water and protective agent, and mixing the protective agent with SiO2By hydrogen bonding, at SiO2The surface of the ball is coated with a protective layer; then mixing the coating mixture with an etching agent, and carrying out etching reaction under the condition of stirring at room temperature, wherein SiO is used2The surface of the sphere is coated with a layer of protective agent, the outer layer of the silicon dioxide sphere can be protected from reacting with an etchant, meanwhile, the room-temperature stirring condition is adopted, so that etchant molecules can enter the silicon dioxide at a proper speed, a non-hollow porous structure can be formed in the silicon dioxide, the pore diameter is continuously enlarged along with the advancement of etching, the silicon dioxide sphere forms countless porous structures, monodisperse ultra-small silicon dioxide nano particles can be prepared after the structures collapse, and the prepared silicon dioxide has good dispersibility.
The invention can obtain the monodisperse ultra-small silicon dioxide nano-particles at room temperature, and has the advantages of simple preparation and low energy consumption.
In addition, the present invention can control the particle size of the silicon dioxide nanoparticles by controlling the etching time and the amount of the etchant.
Drawings
FIG. 1 shows SiO before coating in example 12TEM images of the ball;
FIG. 2 shows SiO after coating in example 12TEM images of the ball;
FIG. 3 shows SiO obtained after 5 hours of etching reaction in example 12TEM images of the ball;
FIG. 4 is a TEM image of ultra-small silica particles obtained after etching for 10h in example 1;
FIG. 5 is a TEM image of the silica nanoparticles obtained in example 2;
fig. 6 is a TEM image of the silica nanoparticles obtained in example 3.
Detailed Description
The invention provides a preparation method of monodisperse ultra-small silicon dioxide nanoparticles, which comprises the following steps:
mixing SiO2Mixing ball, water and protective agent to SiO2Coating the balls to obtain a coating mixture;
and mixing the coating mixture with an etching agent, and carrying out etching reaction under the condition of stirring at room temperature to obtain the monodisperse ultra-small silicon dioxide nanoparticles.
Mixing SiO2Mixing ball, water and protective agent to SiO2And coating the balls to obtain a coating mixture.
In the present invention, the SiO2The particle size of the spheres is preferably 50nm to 2 μm, preferably 200nm to 1 μm, and most preferably 300 to 500 nm. The invention is directed to the SiO2The source of the balls is not particularly critical and may be commercially available or known to those skilled in the art
Can be synthesized by the method.
Prior to mixing, the present invention preferably employs alternating pairs of ethanol and water to SiO2The balls were washed centrifugally. In the invention, the rotation speed of the centrifugal washing is preferably 3000-15000 rpm, and is preferably 8000-12000 rpm; the time for centrifugal washing is preferably 5-20 min. In the present invention, the number of times of the centrifugal washing is preferably 6 times. The invention adopts ethanol and water for alternate washing, water can wash off water-soluble impurities, ethanol can wash off fat-soluble impurities, and SiO is ensured2The surface of the ball is washed clean, so as to be beneficial to the subsequent coating reaction.
After centrifugal washing, the invention preferably treats the washed SiO2The spheres were dried. In the invention, the drying temperature is preferably 60-100 ℃, and more preferably 80 ℃; the drying time is preferably 6 to12h, more preferably 10 h. The invention has no special requirement on the drying atmosphere, and can adopt air atmosphere drying or vacuum atmosphere drying.
After drying, the invention dries the SiO2Mixing ball, water and protective agent to SiO2And coating the balls to obtain a coating mixture.
In the present invention, the protective agent is preferably polyvinylpyrrolidone, a polyol, oleic acid, or an aromatic alcohol ester, and is more preferably polyvinylpyrrolidone. The source of the protective agent is not particularly required in the present invention, and commercially available products well known to those skilled in the art may be used.
In the present invention, the mixing is preferably performed in the following manner: mixing SiO2And ultrasonically mixing the ball and water for 15-25 min, and then adding a protective agent.
In the invention, the coating is preferably carried out under a stirring condition, and the stirring speed is preferably 300-600 rpm, and more preferably 500 rpm; the stirring time is preferably 2 to 5 hours, and more preferably 3 hours. In the stirring process, silicon dioxide and a protective agent are connected through hydrogen bonds, and SiO is added2A protective layer is formed on the surface of the ball.
After the coating mixture is obtained, the coating mixture is mixed with an etching agent, and etching reaction is carried out under the condition of stirring at room temperature, so as to obtain the monodisperse ultra-small silicon dioxide nano-particles.
In the present invention, the etchant is preferably sodium hydroxide, potassium hydroxide, or sodium borohydride, and more preferably sodium hydroxide. In the present invention, the SiO2The dosage ratio of the ball, the water, the protective agent and the etching agent is preferably 0.3-1.8 g, 10-100 mL, 0.2-1.5 g, 0.2-1.2 g, more preferably 0.6g, 40mL, 0.5g and 0.2-0.8 g. The invention preferably adds the etching agent into the coating mixture to realize the mixing of the two.
The invention carries out etching under the condition of stirring at room temperature. In the invention, the stirring speed is preferably 300-600 rpm, and more preferably 500 rpm; the time of the etching reaction is preferably 50min to 10h, more preferably 50min to 5h, and most preferably 50min to 3 h.
During the etching process, because of SiO2The surface of the sphere is coated with a protective layer which can protect the outer layer of the silicon dioxide sphere from reacting with an etchant, and meanwhile, under the condition of stirring at room temperature, the etchant can enter the silicon dioxide sphere to form a non-hollow porous structure in the silicon dioxide sphere, and the monodisperse ultra-small silicon dioxide nanoparticles can be prepared after the structure collapses, and the prepared silicon dioxide has good dispersibility.
In addition, the method can regulate and control the particle size of the finally obtained monodisperse silicon dioxide nanoparticles by controlling the time of the etching reaction and the dosage of the etching agent, and particularly, under the condition that other parameters are the same, the longer the etching time is, the smaller the particle size of the obtained monodisperse silicon dioxide nanoparticles is; under the condition that the etching time and other parameters are the same, the more the dosage of the etchant is, the smaller the particle size of the obtained monodisperse silicon dioxide nano-particles is.
After the etching reaction, the invention preferably further comprises the steps of sequentially carrying out centrifugal washing and drying on the solid product after the etching reaction.
In the invention, the centrifugal washing mode is preferably to alternately wash by adopting ethanol and water, and the rotating speed of the centrifugal washing is preferably 12000-18000 rpm, and more preferably 15000 rpm; the centrifugal washing time is preferably 5-20 min; the number of times of the centrifugal washing is preferably 2, and the number of times of the centrifugal washing refers to the total number of times of washing, namely, washing with ethanol once and washing with water once. The invention has no special requirement on the sequence of the alternate washing by adopting ethanol and water, namely, the washing by adopting ethanol or the washing by adopting water firstly can be realized.
After centrifugal washing, the invention dries the washed solid product. In the invention, the drying temperature is preferably 75-85 ℃, and more preferably 80 ℃; the drying time is preferably 9 to 11 hours, and more preferably 10 hours. The invention has no special requirement on the drying atmosphere, and can adopt air atmosphere drying or vacuum atmosphere drying.
The invention also provides the monodisperse ultra-small silicon dioxide nano-particles prepared by the preparation method in the technical scheme, and the particle size of the monodisperse ultra-small silicon dioxide nano-particles is 3-20 nm.
The monodisperse ultra small silica nanoparticles and the preparation method thereof provided by the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
By using
Method for synthesizing SiO with particle size of 340nm2The ball, ethanol and water are alternately centrifugally washed for 6 times at 8000rpm for 5min, and dried in a vacuum drying oven at 80 ℃ for 10 h. 0.6g of synthetic SiO were weighed2Dispersing the spheres in a beaker filled with 40mL of water by ultrasonic treatment for 20min, adding 0.5g of polyvinylpyrrolidone (PVP) as a protective agent, stirring at the rotating speed of 300rpm for 3h at room temperature to coat the PVP on the surface of the silica nanospheres, then adding 0.20g of NaOH as an etching agent, reacting at the room temperature for 10h, alternately and centrifugally washing the product with ethanol and water for 2 times at the rotating speed of 15000rpm for 10min, and drying in a vacuum drying oven at the temperature of 80 ℃ for 10h to obtain the monodisperse ultra-small silica nanoparticles.
Respectively to SiO before coating2Ball, coated SiO2Performing ball and etching reaction for 5h to obtain SiO2The transmission electron microscope observation of the ball and the product after the etching reaction is carried out for 10 hours is shown in figures 1-4, wherein figure 1 is SiO before coating2Ball, FIG. 2 is SiO after coating2Ball, FIG. 3 is SiO obtained after etching reaction for 5h2And (4) a ball, wherein the silicon dioxide nano-particles are obtained after the etching reaction is carried out for 10 hours. The use of which can be seen from FIG. 1
The particle size of the silicon dioxide ball synthesized by the method is about 340nm, and the silicon dioxide ball has uniform particle size and good dispersibility; as can be seen from FIG. 2, a PVP protective layer was applied after 3h of high speed mechanical stirring, at which point the silica spheres had an average particle size of about 360nm, indicating a coating thickness of about 10 nm; when etching reactionWhen the reaction is carried out for 5h, the critical point from the porous nano spherical structure to collapse can be seen in figure 3, and a little collapsed structure in the figure can be seen, namely SiO2The ball has no hollow structure but a porous structure in the etching process, the aperture is continuously enlarged, if the hollow silicon dioxide structure is formed, the etchant etches from the inner side and the outer side, and ultra-small silicon dioxide cannot be formed; as can be seen from FIG. 4, after an etching reaction time of 10 hours, the present invention produced ultra-small silica particles having a particle size of about 10 nm.
Example 2
By using
Method for synthesizing SiO with particle size of 340nm2And (3) alternately centrifuging and washing the nanospheres, ethanol and water for 6 times at the rotation speed of 8000rpm for 5min, and drying in a vacuum drying oven at the temperature of 80 ℃ for 10 h. 0.6g of synthetic SiO were weighed2Dispersing nanospheres in a beaker filled with 40mL of water by ultrasonic treatment for 20min, adding 0.5g of polyvinylpyrrolidone (PVP) as a protective agent, stirring at the rotating speed of 300rpm for 3h at room temperature to coat PVP on the surfaces of the silica nanospheres, then adding 0.36g of NaOH as an etching agent, reacting at the room temperature for 5h, alternately centrifuging and washing the product with ethanol and water for 2 times at the rotating speed of 15000rpm for 10min, and drying in a vacuum drying oven at the temperature of 80 ℃ for 10h to obtain the silica nanoparticles.
The transmission electron microscope observation was performed on the finally obtained silica nanoparticles, and the results are shown in fig. 5. FIG. 5 shows that after etching with 0.36g NaOH for 5h, ultra-small silica particles with a particle size of about 5nm are obtained and the silica nanoparticles exhibit good monodispersity.
Example 3
The same procedure as in example 2 was followed, except that the etching reaction time was 5.5 hours.
The silica nanoparticles obtained in example 3 were observed by transmission electron microscopy, and the results are shown in fig. 6. FIG. 6 shows that after 0.36g NaOH etching for 5.5h, ultra-small silica particles with a particle size of about 3nm are obtained and the silica nanoparticles exhibit good monodispersity.
From the results of example 2 and example 3, it is known that the particle size of the silica nanoparticles can be controlled by adjusting the etching time.
Example 4
Unlike example 2, the amount of the etchant NaOH was 0.32 g. The observation of the transmission electron microscope on the silica nanoparticles obtained in example 2 shows that after etching with 0.32g of NaOH for 5 hours, the prepared silica particles have a particle size of about 12nm and good monodispersity.
From the results of example 2 and example 4, it is known that the particle size of the silica nanoparticles can be controlled by adjusting the amount of the etchant.
Example 5
By using
Method for synthesizing SiO with particle size of 700nm2And (3) alternately centrifuging and washing the nanospheres, ethanol and water for 6 times at the rotation speed of 8000rpm for 5min, and drying in a vacuum drying oven at the temperature of 80 ℃ for 10 h. Weigh 0.6g of presynthesized SiO2Dispersing nanospheres in a beaker filled with 40mL of water by ultrasonic treatment for 20min, adding 0.8g of polyvinylpyrrolidone (PVP) as a protective agent, stirring at the rotating speed of 300rpm for 3h at room temperature to coat PVP on the surfaces of the silica nanospheres, then adding 1.2g of NaOH as an etching agent, reacting at room temperature for 50min, alternately centrifuging and washing the product with ethanol and water for 2 times at the rotating speed of 15000rpm for 10min, and drying in a vacuum drying oven at 80 ℃ for 10h to obtain the silica nanoparticles.
The silica nanoparticles obtained in example 5 were observed by transmission electron microscopy, and the result was similar to the photograph of example 2, and the obtained silica showed good monodispersity and a particle size of about 10 nm.
The embodiments can show that the monodisperse ultra-small silica nanoparticle and the preparation method thereof are simple, and the monodisperse ultra-small silica nanoparticle can be obtained at room temperature, and has the advantages of simple preparation and low energy consumption.
In addition, the invention can control the grain diameter of the silicon dioxide nano-particles by controlling the etching time and the dosage of the etching agent.
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 (4)
1. A preparation method of monodisperse ultra-small silicon dioxide nano particles is characterized by comprising the following steps:
mixing SiO2Mixing ball, water and protective agent to SiO2Coating the balls to obtain a coating mixture;
mixing the coating mixture with an etching agent, and carrying out etching reaction under the condition of stirring at room temperature to obtain monodisperse ultra-small silicon dioxide nanoparticles;
the protective agent is polyvinylpyrrolidone, polyalcohol, oleic acid or aromatic alcohol ester;
the etching agent is sodium hydroxide, potassium hydroxide or sodium borohydride;
the SiO2The dosage ratio of the ball, the water, the protective agent and the etching agent is 0.3-1.8 g, 10-100 mL, 0.2-1.5 g and 0.2-1.2 g;
the etching reaction time is 50 min-10 h;
the stirring speed is 300-600 rpm.
2. The method of claim 1, wherein the SiO is2The particle size of the spheres is 50 nm-2 μm.
3. The preparation method according to claim 1, wherein the coating is carried out under stirring conditions, wherein the stirring speed is 300-600 rpm, and the stirring time is 2-5 hours.
4. The method according to claim 1, wherein after the etching reaction, the method further comprises sequentially performing centrifugal washing and drying on the solid product of the etching reaction.
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