CN111717922A - Preparation method of spherical silicon dioxide - Google Patents
Preparation method of spherical silicon dioxide Download PDFInfo
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- CN111717922A CN111717922A CN202010616945.1A CN202010616945A CN111717922A CN 111717922 A CN111717922 A CN 111717922A CN 202010616945 A CN202010616945 A CN 202010616945A CN 111717922 A CN111717922 A CN 111717922A
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The invention relates to a preparation method of spherical silicon dioxide. A method for preparing spherical silica, comprising: (1) preparing a mixed solution of an alcohol-water system; wherein the water contains 0.5% PVA; (2) adding a surfactant into the mixed solution of the alcohol-water system, and uniformly mixing to obtain a mixed solution M; (3) then adding ammonia water at room temperature, uniformly mixing, dropwise adding silicon tetrachloride liquid while stirring, and continuously stirring to obtain a silicon dioxide suspension; (4) and after the silicon dioxide suspension is aged, centrifugally washing, drying the obtained precipitate, and calcining to obtain the spherical silicon dioxide. According to the preparation method of the spherical silicon dioxide, silicon tetrachloride is used as a silicon source, the high-purity spherical silicon dioxide with adjustable size is prepared in one step, the problem of toxicity of the silicon tetrachloride is solved, the preparation cost is reduced, the environment is protected, and the diameter and the aperture of the silicon dioxide spherical particle can be effectively regulated and controlled.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a preparation method of spherical silicon dioxide.
Background
SiO2The material has high specific surface area, low density, high permeability and good biocompatibilityHigh in sexual potency, low in toxicity and high in mechanical stability. Due to the excellent properties, the nano SiO2The material has very wide application in the fields of catalysis, sensors, nano medicine, lithium batteries, ceramic industry and the like, such as a carrier of a catalyst, a carrier of a sensor, a drug controlled release system, an antifouling paint and the like. In addition, silica particles are widely used in the fields of elastomers, films, coatings, toothpastes, and the like, due to their excellent reinforcing, thickening, and thixotropic properties.
Polysilicon has excellent electrical, optical and thermal properties and is the most important and basic functional material in the semiconductor, electronic information and solar photovoltaic cell industries. Thus, the demand for polysilicon is greatly stimulated. However, everything is twofold. The photovoltaic industry inevitably brings certain environmental pollution to our provision of continuous renewable energy. Due to the limitation of production technology, a large amount of highly toxic byproduct silicon tetrachloride can be produced while producing the polysilicon, and the development of polysilicon enterprises is hindered.
To date, the precursors for the preparation of silica have been predominantly silicates or water glass. Silicon sources such as silicate ester and the like are expensive, and the preparation of silicon dioxide by taking silicon tetrachloride as a byproduct of polycrystalline silicon as a silicon source can reduce the cost to a certain extent and create social wealth. Meanwhile, the silicon tetrachloride waste can be more fully utilized, and the damage to the environment is reduced. However, in the prior art, silicon dioxide prepared by silicon tetrachloride is mainly prepared by a gas phase method, which causes great damage to operating equipment, while spherical silicon dioxide prepared by a liquid phase method is not common, because the hydrolysis rate of silicon tetrachloride is far greater than that of sodium silicate and silicate silicon sources, which is not beneficial to regulating and controlling the properties of morphology and the like.
And the successful synthesis of M41S series silicon-based mesoporous material, namely a novel ordered mesoporous material with continuously adjustable pore diameter of 1-10nm and highly ordered pore arrangement, was first announced by the company Mobil Oil research and Development in 1992, and then the mesoporous material received great attention and rapidly developed as a research hotspot. The mesoporous material can be applied to the fields of analysis, catalyst carriers, drug slow release and the like, and the particle size, the pore diameter and the like of the mesoporous silicon oxide material directly determine the application range of the mesoporous silicon oxide material. Generally, when the size of the nanoparticle is less than 100nm, the nanoparticle can show interesting properties due to the nano-size effect, but the smaller nanoparticle has higher cytotoxicity and high hemolytic activity, and the control of the pore size can obtain mesoporous silica which is beneficial to material delivery and slow release. Therefore, the control of the particle size and the pore diameter of the nano mesoporous silica has an important significance for expanding the application range thereof, and becomes a subject of many researchers. Although the preparation method of the mesoporous material is continuously innovated and perfected, the particle cutting preparation is still difficult to realize according to the will and the actual application requirements of people, mainly the synthesis process is difficult to control, and the obtained results are different according to different reaction precursors and reaction conditions.
In view of the above, the invention provides a preparation method of a graded silica sphere, which is low in cost and simple and convenient to operate, is expected to realize industrial production, and can regulate and control the particle size and pore diameter of the silica sphere, so that the function and property of silica can be effectively changed.
Disclosure of Invention
The invention aims to provide a preparation method of spherical silicon dioxide, which takes silicon tetrachloride as a silicon source and adopts a simple mechanical stirring method to prepare high-purity spherical silicon dioxide with adjustable size in one step. The method solves the problem of toxicity of the silicon tetrachloride, reduces the preparation cost, protects the environment and can effectively regulate and control the diameter and the aperture of the silicon dioxide spherulites.
In order to realize the purpose, the adopted technical scheme is as follows:
a preparation method of spherical silicon dioxide comprises the following steps:
(1) preparing a mixed solution of an alcohol-water system; wherein the water contains 0.5% PVA;
(2) adding a surfactant into the mixed solution of the alcohol-water system, and uniformly mixing;
(3) then adding ammonia water at room temperature, uniformly mixing, dropwise adding silicon tetrachloride liquid while stirring, and continuously stirring to obtain a silicon dioxide suspension;
(4) and after the silicon dioxide suspension is aged, carrying out centrifugal washing, drying the obtained precipitate, and then calcining to obtain the spherical silicon dioxide.
Further, in the step (1), the mixed solution of the alcohol-water system is prepared by: to the alcohol solution, an aqueous solution containing 0.5% PVA and aqueous ammonia were sequentially added.
Still further, in the mixed solution of the alcohol-water system, the molar ratio of alcohol to water is 1-3: 1-3.
Further, in the mixed solution of the alcohol-water-ammonia system, the alcohol is any one of methanol, ethanol and propanol.
Further, the surfactant is any one of CTAB, SLS, SDS, P123 and PEG.
Further, in the step (3), the silicon tetrachloride liquid is added dropwise under the stirring condition of the rotation speed of 150-.
Further, after the silicon tetrachloride liquid is dripped, keeping the rotating speed unchanged, and maintaining stirring for reaction for 2-6 h.
Further, in the step (4), the aging time is 3-12 h.
Further, in the step (4), the centrifugal rotation speed is 6000-.
Further, in the step (4), the calcining temperature is 500 ℃ and the calcining time is 4 hours.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with silicate ester or water glass, the method has the advantages that the spherical silicon dioxide is controllably prepared in one step by taking the silicon tetrachloride which is the byproduct of the polycrystalline silicon as a silicon source, the problem of difficulty in processing the byproduct of the polycrystalline silicon is solved, green chemistry is realized, and the method is environment-friendly, economical and capable of creating social benefits.
2. The method takes silicon tetrachloride as a raw material, prepares the spherical silicon dioxide in a controllable way in one step, and can control the particle size and the pore diameter of the silicon dioxide spheres through different water-alcohol ratios, rotating speeds and surfactants, so that the method can be widely applied to a plurality of fields such as catalysis, sensors, nano medicine, lithium batteries, ceramic industry and the like.
3. The invention can not only control the particle size and the pore diameter of the silicon dioxide ball, but also improve the specific surface area of the silicon dioxide through the rotating speed and the surfactant.
4. The invention has relatively low requirements on operation technology and equipment, and is easy to realize industrialization.
Drawings
FIG. 1 shows the preparation of nano SiO in example 1 of the present invention2Scanning electron micrographs of the ball;
FIG. 2 shows the preparation of nano SiO in example 2 of the present invention2Scanning electron micrographs of the ball;
FIG. 3 shows the preparation of nano SiO in example 3 of the present invention2Scanning electron micrographs of the ball;
FIG. 4 shows the preparation of nano SiO in example 4 of the present invention2Scanning electron micrographs of the ball;
FIG. 5 shows the sequence of the nano SiO prepared in example 1 of the present invention2Pore volume and pore diameter distribution diagram of the ball;
FIG. 6 shows the sequence of the nano SiO prepared in example 2 of the present invention2Pore volume and pore diameter distribution diagram of the ball;
FIG. 7 shows the sequence of the nano SiO prepared in example 3 of the present invention2Pore volume and pore diameter distribution diagram of the ball;
FIG. 8 shows the sequence of the nano SiO prepared in example 4 of the present invention2Pore volume and pore diameter distribution diagram of the ball;
FIG. 9 shows a nano SiO solid prepared by comparative example 1 of the present invention2Scanning electron micrographs of the spheres.
Detailed Description
In order to further illustrate the preparation method of the spherical silica of the present invention and achieve the intended purpose, the following detailed description is given to the preparation method of the spherical silica according to the present invention, and the detailed implementation, structure, features and effects thereof, in conjunction with the preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The preparation of a spherical silica according to the present invention will be described in further detail with reference to the following specific examples:
the technical scheme of the invention is as follows:
a preparation method of spherical silicon dioxide comprises the following steps:
(1) preparing a mixed solution of an alcohol-water system; wherein the water contains 0.5% PVA;
(2) adding a surfactant into the mixed solution of the alcohol-water system, and uniformly mixing;
(3) then adding ammonia water at room temperature, uniformly mixing, dropwise adding silicon tetrachloride liquid while stirring, and continuously stirring to obtain a silicon dioxide suspension;
(4) and after the silicon dioxide suspension is aged, carrying out centrifugal washing, drying the obtained precipitate, and then calcining to obtain the spherical silicon dioxide.
Preferably, in the step (1), the mixed solution of alcohol-water-ammonia system is prepared by: to the alcohol solution, an aqueous solution containing 0.5% PVA and aqueous ammonia were sequentially added.
Further preferably, in the mixed solution of the alcohol-water-ammonia system, the molar ratio of the alcohol to the water (including PVA) is 1 to 3: 1-3.
Preferably, in the mixed solution of the alcohol-water-ammonia system, the alcohol is any one of methanol, ethanol and propanol.
Preferably, the surfactant is any one of CTAB, SLS, SDS, P123 and PEG.
Preferably, in the step (3), the silicon tetrachloride liquid is added dropwise under the stirring condition of the rotation speed of 150-.
Preferably, after the silicon tetrachloride liquid is dripped, keeping the rotating speed unchanged, and maintaining stirring for reaction for 2-6 h.
Preferably, in the step (4), the aging time is 3-12 h.
Preferably, in the step (4), the centrifugal rotation speed is 6000-.
Preferably, in the step (4), the calcining temperature is 500 ℃ and the calcining time is 4 h.
Example 1.
The specific operation steps are as follows:
ethanol and 0.5% aqueous PVA solution were mixed at room temperature, the molar ratio of the alcohol fraction to water in the 0.5% aqueous PVA solution was 1: 3 (0.5% PVA in water to promote the formation of silica spheres).
Then 2g of CTAB is added and evenly mixed by ultrasonic.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. Then freeze-drying the precipitate for 12h to obtain the spherical silicon dioxide with the specific surface area as high as 913m2/g。
Fig. 1 is a scanning electron microscope image of a silica sphere prepared in example 1 of the present invention, and fig. 5 is a corresponding pore volume and pore diameter distribution diagram, which shows that a sample has a spherical structure with regular morphology and a mesoporous structure.
Comparative example 1 (without surfactant)
The specific operation steps are as follows:
ethanol and 0.5% aqueous PVA solution were mixed at room temperature, the molar ratio of the alcohol fraction to water in the 0.5% aqueous PVA solution was 1: 3.
and (4) ultrasonically mixing uniformly.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze dried for 12h to give the spherical silica.
FIG. 9 is a scanning electron microscope image of the silica spheres prepared in comparative example 1, and it can be seen by comparison that the morphology of the silica prepared without any surfactant is significantly inferior to the morphology of the product with the surfactant.
Comparative example 2.
The specific operation steps are as follows:
ethanol and 0.5% aqueous PVA solution were mixed at room temperature, the molar ratio of the alcohol fraction to water in the 0.5% aqueous PVA solution was 1: 3.
then 2g of CTAB is added and evenly mixed by ultrasonic.
Quickly adding 3mL of ammonia water at the rotating speed of 10000r/min, stirring for 10min, and then starting dropwise adding SiCl4Liquid, and reacting for 0.5h at 10000/min to obtain the silicon dioxide suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze-dried for 12h to give the spherical silica with a specific surface area of up to 652m2/g。
As can be seen from comparison with example 1, the technical solution of the present invention can not only control the particle size and pore size of the silica spheres, but also increase the specific surface area of the silica by the rotation speed and the surfactant.
Example 2.
The specific operation steps are as follows:
ethanol and 0.5% aqueous PVA solution were mixed at room temperature, the molar ratio of the alcohol fraction to water in the 0.5% aqueous PVA solution was 1: 3.
adding 2g of SLS, and uniformly mixing by ultrasonic.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze dried for 12h to give the spherical silica.
Fig. 2 is a scanning electron microscope image of the silica spheres prepared in example 2 of the present invention, and fig. 6 is a corresponding pore volume and pore diameter distribution diagram, which shows that the sample has a spherical structure with regular morphology and a mesoporous structure.
Example 3.
The specific operation steps are as follows:
ethanol and 0.5% aqueous PVA solution were mixed at room temperature, the molar ratio of the alcohol fraction to water in the 0.5% aqueous PVA solution was 1: 3.
adding 2gP123, and mixing evenly by ultrasonic.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze dried for 12h to give the spherical silica.
Fig. 3 is a scanning electron microscope image of the silica spheres prepared in example 3 of the present invention, and fig. 7 is a corresponding pore volume and pore diameter distribution diagram, which shows that the sample has a spherical structure with regular morphology and a mesoporous structure.
Example 4.
The specific operation steps are as follows:
ethanol and 0.5% aqueous PVA solution were mixed at room temperature, the molar ratio of the alcohol fraction to water in the 0.5% aqueous PVA solution was 1: 3.
add 2g PEG, mix well by ultrasound.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze dried for 12h to give the spherical silica.
Fig. 4 is a scanning electron microscope image of the silica spheres prepared in example 4 of the present invention, and fig. 8 is a corresponding pore volume and pore diameter distribution diagram, which shows that the sample has a spherical structure with regular morphology and a mesoporous structure.
Example 5.
The specific operation steps are as follows:
preparing a mixed solution of an alcohol-water system; ethanol and 0.5% aqueous PVA solution were mixed at room temperature in a 1: 2 in a molar ratio.
Adding 2g CTAB, and uniformly mixing by ultrasonic.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze dried for 12h to give the spherical silica.
Example 6.
The specific operation steps are as follows:
preparing a mixed solution of an alcohol-water system; ethanol and 0.5% aqueous PVA solution were mixed at room temperature in a 1: 1 in a molar ratio.
Adding 2g CTAB, and uniformly mixing by ultrasonic.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze dried for 12h to give the spherical dioxides.
Example 7.
The specific operation steps are as follows:
preparing a mixed solution of an alcohol-water system; ethanol and 0.5% aqueous PVA solution were mixed at room temperature as a 2: 1 in a molar ratio.
Adding 2g CTAB, and uniformly mixing by ultrasonic.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze dried for 12h to give the spherical silica.
Example 8.
The specific operation steps are as follows:
preparing a mixed solution of an alcohol-water system; ethanol and 0.5% aqueous PVA solution were mixed at room temperature as a 3: 1 in a molar ratio.
Adding 2g CTAB, and uniformly mixing by ultrasonic.
Rapidly adding 3mL of ammonia water at the rotating speed of 150r/min, stirring for 10min, and then beginning to dropwise add SiCl4Liquid, and reacting for 3 hours at the speed of 150r/min to obtain a silica suspension.
After aging for 3h at 40 ℃, centrifugally washing the mixture until the pH is neutral under the condition of 8000r/min of rotation speed. The precipitate was then freeze dried for 12h to give the spherical silica.
The method takes the silicon tetrachloride which is the byproduct of the polysilicon as the raw material to controllably prepare the spherical silicon dioxide, the silicon source of the method is the silicon tetrachloride which is the waste from the polysilicon industry, and the spherical silicon dioxide with adjustable grain diameter and aperture and high specific surface area is obtained by adjusting and controlling the water-alcohol molar ratio, the rotating speed and the type of a surfactant. The invention solves the problem of toxicity of the silicon tetrachloride, reduces the preparation cost and protects the environment; in addition, the invention can effectively regulate and control the particle size and the pore diameter of the silicon dioxide spheres in a simple reaction system. The invention can also be applied to the hydrolysis preparation of chloride such as aluminum trichloride, titanium tetrachloride and the like, thereby obtaining the corresponding spherical oxide. The preparation method has low requirements on equipment and operation, and is convenient for realizing industrialization.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the spherical silicon dioxide is characterized by comprising the following steps:
(1) preparing a mixed solution of an alcohol-water system; wherein the water contains 0.5% PVA;
(2) adding a surfactant into the mixed solution of the alcohol-water system, and uniformly mixing;
(3) then adding ammonia water at room temperature, uniformly mixing, dropwise adding silicon tetrachloride liquid while stirring, and continuously stirring to obtain a silicon dioxide suspension;
(4) and after the silicon dioxide suspension is aged, carrying out centrifugal washing, drying the obtained precipitate, and then calcining to obtain the spherical silicon dioxide.
2. The production method according to claim 1,
in the step (1), the mixed solution of the alcohol-water system is prepared by the following steps: to the alcohol solution, an aqueous solution containing 0.5% PVA and aqueous ammonia were sequentially added.
3. The production method according to claim 2,
in the mixed solution of the alcohol-water system, the molar ratio of alcohol to water is 1-3: 1-3.
4. The method according to claim 1, wherein the alcohol is any one of methanol, ethanol, and propanol in the mixed solution of the alcohol-water-ammonia system.
5. The production method according to claim 1,
the surfactant is any one of CTAB, SLS, SDS, P123 and PEG.
6. The production method according to claim 1,
in the step (3), the silicon tetrachloride liquid is dropwise added under the stirring condition of the rotation speed of 150-.
7. The production method according to claim 1,
after the silicon tetrachloride liquid is dripped, keeping the rotating speed unchanged, and keeping stirring for reaction for 2-6 h.
8. The production method according to claim 1,
in the step (4), the aging time is 3-12 h.
9. The production method according to claim 1,
in the step (4), the centrifugal rotation speed is 6000-.
10. The production method according to claim 1,
in the step (4), the calcining temperature is 500 ℃ and the calcining time is 4 hours.
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| CN112938995A (en) * | 2021-04-08 | 2021-06-11 | 昆明理工大学 | Method for preparing spherical silicon dioxide |
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| CN112938995A (en) * | 2021-04-08 | 2021-06-11 | 昆明理工大学 | Method for preparing spherical silicon dioxide |
| CN112938995B (en) * | 2021-04-08 | 2022-11-29 | 昆明理工大学 | Method for preparing spherical silicon dioxide |
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