A method for rapidly preparing nanometer-sized silicon dioxide and spherical nanometer-sized silicon dioxide

Abstract

The application discloses a method for rapidly preparing nano-silicon dioxide, which comprises the following steps: S1, uniformly coating methyl silicone oil on a glass slide; S2, high-temperature sintering the glass slide coated with the methyl silicone oil, wherein the sintering temperature is 400-1000 DEG C, and the sintering time is 0.5-80 min; and S3, naturally cooling to room temperature and scraping off the solid adhered on the glass slide, thereby obtaining the nano-silicon dioxide. The method overcomes the shortcomings of the previous preparation methods of nano-silicon dioxide, such as complicated steps and harsh conditions, and has the characteristics of simple operation, simple steps, short preparation time, high purity of the prepared spherical nano-silicon dioxide, and the like. In the preparation process, the sintering conditions are adjusted to controllably prepare the nano-silicon dioxide balls with the grain size in the range of 30-300 nm, so that the method has a good market application and promotion prospect.

Description

Technical Field

[0001] This invention relates to the field of silica nanomaterial preparation technology, and particularly to a method for rapidly preparing nano-silica and spherical nano-silica. Background Technology

[0002] Nano-silica possesses excellent properties such as large specific surface area, highly controllable particle size, and good biocompatibility. Furthermore, due to its unique size effect, nano-silica exhibits good optical properties against ultraviolet radiation and is frequently used as an additive in cosmetics. Using nano-silica as an additive, for example in rubber manufacturing, can effectively improve the strength, toughness, and anti-aging properties of the base material. Its excellent biocompatibility also makes it a promising candidate for applications in bioimaging and drug delivery.

[0003] Currently, there are various methods for preparing nano-silica materials, with common methods including solution methods, hydrothermal methods, template methods, and sol-gel methods; however, these methods all have drawbacks such as numerous steps and demanding conditions. Among the currently published research results, there are no reports on the simple and rapid synthesis of nano-silica materials. Therefore, designing a rapid, simple, and efficient method for preparing nano-silica materials is of great significance. Summary of the Invention

[0004] The purpose of this invention is to provide a method for rapidly preparing nano-silica materials in a fast, simple, and efficient manner, which solves the problems of existing technologies.

[0005] Another object of the present invention is to provide spherical nano-silica prepared by the above-described rapid preparation method for nano-silica.

[0006] Therefore, the technical solution of the present invention is as follows:

[0007] A method for rapidly preparing nano-silica, comprising the following steps:

[0008] S1. Coat the glass slide with methyl silicone oil evenly;

[0009] S2. The glass slide coated with methyl silicone oil is sintered at a high temperature of 400℃~1000℃ for 0.5min~80min.

[0010] S3. Allow the slide to cool naturally to room temperature, then scrape off the solid adhering to the slide to obtain nano-silica.

[0011] Preferably, the operation method of step S1 is as follows: first, take a small amount of methyl silicone oil and place it in a beaker, then use a dropper to measure some methyl silicone oil and drop it onto the surface of the glass slide, and slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0012] Preferably, in step S1, methyl silicone oil is uniformly coated on one or both sides of the glass slide.

[0013] Preferably, the operation method of step S2 is as follows: a glass slide uniformly coated with methyl silicone oil is placed at an angle inside a quartz boat so that the methyl silicone oil coated surface of the glass slide does not contact the quartz boat; then, the quartz boat containing the glass slide is placed in a tube furnace for high-temperature sintering.

[0014] Preferably, the viscosity of the methyl silicone oil is 30cs to 80cs.

[0015] Preferably, in step S2, the sintering temperature is 600℃~800℃, and the sintering time is 2min~60min. A spherical nano-silica prepared using the above-described rapid nano-silica preparation method.

[0016] Compared with existing technologies, this rapid method for preparing nano-silica overcomes the shortcomings of previous methods, which involved numerous steps and stringent conditions. It features simple operation, concise steps, and short preparation time. Furthermore, the prepared spherical nano-silica has high purity. By adjusting the sintering conditions during the preparation process, nano-silica spheres with adjustable grain sizes in the range of 30nm to 300nm can be controllably produced, making this method promising for market application and promotion. Attached Figure Description

[0017] Figure 1 This is a flowchart illustrating the rapid preparation method for nano-silica according to the present invention.

[0018] Figure 2 This is a schematic diagram of the structure of spherical nano-silica prepared by the rapid preparation method of nano-silica of the present invention;

[0019] Figure 3 The XRD patterns of the nano-silica prepared in Examples 1 to 12 of this invention are shown below.

[0020] Figure 4 These are scanning electron microscope images of nano-silica prepared in Examples 1 to 12 of the present invention, taken under a 200 nm scale. Figure 4In the image, (a) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 1, (b) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 2, (c) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 3, (d) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 4, (e) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 5, (f) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 6, (g) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 7, (h) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 8, (i) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 9, (j) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 10, (k) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 11, and (l) is a scanning electron microscope (SEM) image of the nano-silica prepared in Example 12.

[0021] Figure 5 The elemental analysis results of the nano-silica prepared in Example 2 of the present invention are shown in the distribution diagram.

[0022] Figure 6 The elemental analysis results of the nano-silica prepared in Example 6 of this invention are shown in the distribution diagram. Detailed Implementation

[0023] The present invention will be further described below with reference to the accompanying drawings and specific embodiments, but the following embodiments are by no means intended to limit the present invention.

[0024] Example 1

[0025] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0026] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0027] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 600°C for 30 minutes.

[0028] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0029] Example 2

[0030] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0031] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0032] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 600°C for 60 minutes.

[0033] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0034] Example 3

[0035] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0036] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0037] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 650°C for 8 minutes.

[0038] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0039] Example 4

[0040] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0041] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0042] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 650°C for 60 minutes.

[0043] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0044] Example 5

[0045] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0046] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0047] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 700°C for 2 minutes.

[0048] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0049] Example 6

[0050] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0051] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0052] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 700°C for 5 minutes.

[0053] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0054] Example 7

[0055] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0056] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0057] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 700°C for 8 minutes.

[0058] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0059] Example 8

[0060] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0061] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0062] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 700°C for 10 minutes.

[0063] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0064] Example 9

[0065] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0066] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0067] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 700°C for 30 minutes.

[0068] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0069] Example 10

[0070] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0071] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0072] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 700°C for 60 minutes.

[0073] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0074] Example 11

[0075] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0076] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0077] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 750°C for 8 minutes.

[0078] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0079] Example 12

[0080] A method for preparing nano-silica using rapid nano-silica, comprising the following steps:

[0081] S1. Take a small amount of methyl silicone oil with a viscosity of 50 cs and place it in a beaker. Use a dropper to measure some of the methyl silicone oil and drop it onto the surface of a glass slide. Slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

[0082] S2. Place the glass slide uniformly coated with methyl silicone oil at an angle inside the quartz boat, ensuring that the methyl silicone oil-coated surface of the glass slide does not contact the quartz boat. Then, place the quartz boat containing the glass slide in a tube furnace for high-temperature sintering at a temperature of 800°C for 8 minutes.

[0083] S3. Remove the quartz boat and allow it to cool naturally to room temperature. Use a spatula to slowly scrape off the sample adhering to the surface of the glass slide to obtain nano-silica.

[0084] Performance testing:

[0085] (I) Analysis of X-ray diffraction results:

[0086] See Figure 1 X-ray diffraction experiments were conducted on the nano-silica prepared by the rapid preparation method of nano-silica as described in Examples 1 to 12 above.

[0087] like Figure 3 As shown in the X-ray diffraction results of the nano-silica prepared in Examples 1 to 12, the samples prepared from liquid methyl silicone oil with different viscosities in each example all exhibited amorphous properties, which is consistent with the amorphous physical properties of silica. That is, the test results show that nano-silica was indeed prepared in Examples 1 to 12.

[0088] The silica material prepared by the rapid preparation method for nano-silica materials provided by this invention is in the form of nanospheres, with a specific shape as shown in the figure. Figure 2 As shown.

[0089] (II) Analysis of Scanning Electron Microscopy Results:

[0090] Scanning electron microscopy (SEM) experiments were performed on the nano-silica materials prepared in Examples 1 to 12, and the results were as follows: Figure 4 The SEM image shown is from... Figure 4 As can be seen from the electron microscope images shown in (a) to (l), the nano-silica prepared in Examples 1 to 12 all exhibit the following characteristics: Figure 2 The spherical shape shown.

[0091] In Examples 3, 7, 11, and 12, the sintering time during the preparation of nano-silica was 8 minutes, and the sintering temperatures were 650℃, 700℃, 750℃, and 800℃, respectively. The corresponding SEM images are shown below. Figure 4As shown in (c), (g), (k), and (l), it can be deduced from the figures that, under the condition that the sintering time is 8 min, the average grain size of nano-silica increases with the increase of the sintering temperature gradient, becoming 50 nm, 120 nm, 180 nm, and 220 nm respectively. In Examples 1 and 9, the sintering time in the preparation of nano-silica was 30 min, and the sintering temperatures were 600 °C and 700 °C respectively, as shown in the corresponding SEM images. Figure 4 As shown in (a) and (i), it can be deduced from the figures that, under the condition that the sintering time is 30 min, the average grain size of nano-silica increases with increasing sintering temperature, becoming 100 nm and 230 nm respectively. In Examples 2, 4, and 10, the sintering time in the preparation of nano-silica was 60 min, and the sintering temperatures were 600 °C, 650 °C, and 700 °C respectively, as shown in the corresponding SEM images. Figure 4 As shown in (b), (d) and (j), it can be deduced from the figure that, under the condition that the sintering time is 60 min, the average grain size of nano-silica increases with the increase of the sintering temperature gradient, and is 130 nm, 170 nm and 300 nm respectively.

[0092] In Examples 1 and 2, the sintering temperature during the preparation of nano-silica was 600℃, and the sintering times were 30 min and 60 min, respectively. The corresponding SEM images are shown below. Figure 4 As shown in (a) and (b), it can be deduced from the figures that, under the condition of a sintering temperature of 600℃, the average grain size of nano-silica increases with increasing sintering time, by 100nm and 130nm respectively. In Examples 3 and 4, the sintering temperature during the preparation of nano-silica was 650℃, and the sintering times were 8min and 60min respectively. The corresponding SEM images are shown below. Figure 4 As shown in (c) and (d), it can be deduced from the figures that, under the condition of a sintering temperature of 650℃, the average grain size of nano-silica increases with increasing sintering time, becoming 50nm and 170nm respectively. In Examples 5 to 10, the sintering temperature during the preparation of nano-silica was 700℃, and the sintering times were 2min, 5min, 8min, 10min, 30min, and 60min, respectively. The corresponding SEM images are shown below. Figure 4 As shown in (e), (f), (g), (h), (i), and (j), it can be deduced from the figure that, under the condition that the sintering temperature is 700℃, the average grain size of nano-silica increases with the sintering time, and is 30nm, 90nm, 120nm, 200nm, 230nm, and 300nm respectively.

[0093] It is evident that, in the process of preparing nano-silica using the method of this application, the grain size of the nano-silica spheres can be effectively controlled by adjusting the sintering time and sintering temperature. As the sintering time increases and the sintering temperature rises, the grain size of the nano-silica spheres gradually increases; conversely, as the sintering time decreases and the sintering temperature decreases, the grain size of the nano-silica spheres gradually decreases. Specifically, by changing the sintering conditions, the grain size of the nano-silica spheres can be controlled within the range of 30 nm to 300 nm.

[0094] (III) Analysis of Element Distribution Results:

[0095] The elemental distribution of the nano-silica spheres prepared in Examples 2 and 6 were tested, and the results were as follows: Figure 5 and Figure 6 The test results are shown in the two figures above. It is clear from these figures that the nano-silica rapidly prepared by the method of this application is composed entirely of silicon and oxygen, with no other elements present. To further prove that the prepared sample is indeed silica, quantitative analysis of the internal elements was performed. The molar ratio of oxygen to silicon in the sample was determined to be 2.4:1. This ratio is close to the molar ratio of silica. The slightly higher oxygen content is likely due to interference from atmospheric oxygen in elemental distribution tests, which is within a reasonable error range. Therefore, this elemental analysis result demonstrates the feasibility of preparing nano-silica using the method of this application.

[0096] In summary, the nano-silica prepared by the method of this application not only ensures high purity but also has the advantages of simple experimental operation, concise steps, and short preparation time, thus enriching the preparation methods of nano-silica materials. At the same time, by adjusting the sintering conditions during the preparation process, nano-silica spheres with adjustable grain size in the range of 30nm to 300nm can be controllably prepared.

[0097] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims

1. A method for rapidly preparing nanosilica, characterized by, The steps are as follows: S1. Coat the glass slide with methyl silicone oil evenly; S2. The glass slide coated with methyl silicone oil is sintered at a high temperature of 400℃~1000℃ for 0.5min~30min. S3. Allow the slide to cool naturally to room temperature, then scrape off the solid adhering to the slide to obtain nano-silica.

2. The method for rapidly preparing nanosilica according to claim 1, characterized in that, The operation method of step S1 is as follows: first, take a small amount of methyl silicone oil and place it in a beaker, then use a dropper to measure some methyl silicone oil and drop it onto the surface of the glass slide, and slowly tilt the glass slide several times to make the surface of the glass slide evenly covered with methyl silicone oil.

3. The method for rapidly preparing nanosilica according to claim 1 or 2, characterized in that, In step S1, methyl silicone oil is uniformly coated on one or both sides of a glass slide.

4. The method for rapid preparation of nano-silica according to claim 1, characterized in that, The operation method of step S2 is as follows: a glass slide uniformly coated with methyl silicone oil is placed at an angle inside a quartz boat so that the methyl silicone oil coated surface of the glass slide does not come into contact with the quartz boat; then, the quartz boat containing the glass slide is placed in a tube furnace for high-temperature sintering.

5. The method for rapid preparation of nano-silica according to claim 1, characterized in that, The viscosity of methyl silicone oil is 30cs~80cs.

Images