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Preparation method of ultrafine nano silicon dioxide spheres

Inactive Publication Date: 2021-01-12
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

How to obtain lower size nano-silica is still a big challenge

Method used

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  • Preparation method of ultrafine nano silicon dioxide spheres
  • Preparation method of ultrafine nano silicon dioxide spheres
  • Preparation method of ultrafine nano silicon dioxide spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Weigh 1.46g of lysine, dissolve it in 139ml of water, add 8.7ml of cyclohexane, stir and dissolve in a water bath at 40°C. After lysine, water, and cyclohexane are completely miscible, adjust the rotation speed to 500r / min, add a total of 112ml tetraethyl orthosilicate at a rate of 2-3ml / min, and maintain a constant temperature water bath at 40°C and a 500r / min The stirring speed was 24h to obtain a silica suspension.

[0031] (2) Wash and centrifuge the silica suspension for 3 times, the washing solution is deionized water, the centrifugal rate is 5000r / min, dry at 120°C, grind the obtained precipitate into powder, and place it in a muffle furnace for 600 ℃ roasting 4h. A white powder of nano-silica spheres was obtained.

[0032] figure 1 The transmission electron micrograph and particle size distribution diagram of the nano-silica spheres prepared in this example show that the average diameter of the silica spheres is 9.5 nm. Figure 6 The XRD diffraction spec...

Embodiment 2

[0034] (1) Weigh 1.46g of lysine, dissolve it in 139ml of water, add 8.7ml of cyclohexane, stir and dissolve in a water bath at 40°C. After lysine, water, and cyclohexane are completely miscible, adjust the rotation speed to 500r / min, add a total of 112ml tetraethyl orthosilicate at a rate of 2 to 3ml / min, and maintain a constant temperature water bath at 60°C and a 500r / min The stirring speed was 24h to obtain a silica suspension.

[0035] (2) Wash and centrifuge the silica suspension for 3 times, the washing solution is deionized water, the centrifugal rate is 5000r / min, dry at 120°C, grind the obtained precipitate into powder, and place it in a muffle furnace for 600 ℃ roasting 4h. A white powder of nano-silica spheres was obtained.

[0036] figure 2 The transmission electron microscope images and particle size distribution diagrams of the nano silica spheres prepared in this example show that the average diameter of the silica spheres is 17.8nm.

Embodiment 3

[0038] (1) Weigh 1.46g of lysine, dissolve it in 139ml of water, add 8.7ml of cyclohexane, stir and dissolve in a water bath at 40°C. After lysine, water, and cyclohexane are completely miscible, adjust the rotation speed to 500r / min, add a total of 112ml tetraethyl orthosilicate at a rate of 2 to 3ml / min, and maintain a constant temperature water bath at 80°C and a 500r / min The stirring speed was 24h to obtain a silica suspension.

[0039] (2) Wash and centrifuge the silica suspension for 3 times, the washing solution is deionized water, the centrifugal rate is 5000r / min, dry at 120°C, grind the obtained precipitate into powder, and place it in a muffle furnace for 600 ℃ roasting 4h. A white powder of nano-silica spheres was obtained.

[0040] image 3 The transmission electron micrograph and particle size distribution diagram of the nano-silica spheres prepared in this example show that the average diameter of the silica spheres is 26.5 nm.

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Abstract

The invention relates to a preparation method of ultrafine nano silicon dioxide spheres. The preparation method specifically comprises the following steps: (1) dissolving a certain amount of alkalineamino acid in water, adding a proper amount of a non-polar organic solvent, stirring in a constant-temperature water bath, adding an organic silicon raw material after complete mixing and dissolving,and stirring by using a mechanical stirrer to obtain a silicon dioxide suspension; and (2) centrifugally washing the silicon dioxide turbid liquid obtained in the step (1) for 2-3 times, drying to obtain precipitates, grinding the precipitates into powder, and roasting the powder in a muffle furnace to obtain the ultrafine nano silicon dioxide spheres. The nano silicon dioxide spheres prepared bythe method are relatively small in particle size, and the minimum particle size can reach 10nm. The particle size of the silicon dioxide spheres can be controlled by adjusting the rotating speed, temperature, concentration and the like, the manufacturing process is simple, and yield is high. The low-nano silicon dioxide spheres prepared by the method can be widely applied to industries such as biological medicines, cosmetics, rubber and pigments, and have a wide application prospect.

Description

technical field [0001] The invention belongs to the field of nanometer materials, and relates to a method for preparing ultrafine nanometer silicon dioxide spheres. Background technique [0002] Nano-silica is an inorganic chemical material that plays an important role in the industrial and scientific fields. Due to its good optical properties, mechanical strength, heat resistance and chemical resistance, etc., it is widely used in paint pigments, glass ceramics, plastic rubber, pharmaceuticals and medical industries. Depending on the method used, the requirements for the particle size of silica are also different. At present, the common methods for producing nano-silica mainly include hydrolysis precipitation method, sol-gel method and gas-phase method, etc., and the size of the obtained nano-silica spheres is between 20-100nm, even reaching 0.9 μm (CN 110589841 A). Due to its larger size, silica typically has a smaller specific surface area. How to obtain nano-silica wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y40/00
CPCB82Y40/00C01B33/18C01P2004/32C01P2004/64
Inventor 王发根韩凯航张林佳汪炎
Owner JIANGSU UNIV