Preparation method of highly dispersed silicon dioxide microsphere with controllable particle size

A silicon dioxide, high dispersion technology, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of long time, poor dispersion of silicon dioxide microspheres, etc., to achieve simple equipment, low external environment requirements, good dispersibility. Effect

Inactive Publication Date: 2017-10-24
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In view of the poor dispersibility of silica microspheres in the prior art, the need to modify the silica microspheres to improve their dispersibility, and the shortcomings of time-consuming preparation of controllable silica microspheres, the present invention provides a preparation of high A method for dispersing silica microspheres with controllable particle size, the method comprising the steps of:

Method used

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  • Preparation method of highly dispersed silicon dioxide microsphere with controllable particle size
  • Preparation method of highly dispersed silicon dioxide microsphere with controllable particle size
  • Preparation method of highly dispersed silicon dioxide microsphere with controllable particle size

Examples

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Effect test

Embodiment 1

[0033] (1) Take 4.5mL tetraethyl orthosilicate and 45mL absolute ethanol and mix well;

[0034] (2) Take 20mL ammonia water, 16mL ethanol and 25mL deionized water and mix well;

[0035] (3) Put the solution obtained in the above step (2) into a constant temperature magnetic stirrer, set the temperature at 25°C, and the rotation speed at 1800rpm, then quickly add the solution obtained in step (1) into it, and reduce the rotation speed to 1000rpm after 1min. Then continue to react for 2h;

[0036] (4) After the reaction is completed, centrifuge and wash with deionized water for 3 times at a rotational speed of 3500 rpm for 8 min.

[0037] (5) Put the washed silica microspheres into a drying oven for drying at a temperature of 60°C.

[0038] (6) The dried silica microspheres were crushed with a glass rod, dissolved in DMF solution and ultrasonicated for 3 h.

[0039] The particle diameter measured by laser particle size analyzer is 293nm, see figure 1.

Embodiment 2

[0041] (1) Take 4.5mL tetraethyl orthosilicate and 45mL absolute ethanol and mix well;

[0042] (2) Take 20mL ammonia water, 16mL ethanol and 25mL deionized water and mix well, then add 0.01gKCl;

[0043] (3) Put the solution obtained in the above step (2) into a constant temperature magnetic stirrer, set the temperature at 25°C, and the rotation speed at 1800rpm, then quickly add the solution obtained in step (1) into it, and reduce the rotation speed to 1000rpm after 1min. Then continue to react for 2h;

[0044] (4) After the reaction is completed, centrifuge and wash with deionized water for 3 times at a rotational speed of 3500 rpm for 8 min.

[0045] (5) Put the washed silica microspheres into a drying oven for drying at a temperature of 60°C.

[0046] (6) The dried silica microspheres were crushed with a glass rod, dissolved in DMF solution and ultrasonicated for 3 h.

[0047] The particle diameter measured by laser particle size analyzer is 354nm, see figure 2 .

Embodiment 3

[0049] (1) Take 4.5mL tetraethyl orthosilicate and 45mL absolute ethanol and mix well;

[0050] (2) Take 20mL ammonia water, 16mL ethanol and 25mL deionized water and mix well, then add 0.02g KCl;

[0051] (3) Put the solution obtained in the above step (2) into a constant temperature magnetic stirrer, set the temperature at 25°C, and the rotation speed at 1800rpm, then quickly add the solution obtained in step (1) into it, and reduce the rotation speed to 1000rpm after 1min. Then continue to react for 2h;

[0052] (4) After the reaction is completed, centrifuge and wash with deionized water for 3 times at a rotational speed of 3500 rpm for 8 min.

[0053] (5) Put the washed silica microspheres into a drying oven for drying at a temperature of 60°C.

[0054] (6) The dried silica microspheres were crushed with a glass rod, dissolved in DMF solution and ultrasonicated for 3 h.

[0055] The particle size measured with a laser particle size analyzer is 459nm, see image 3 .

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Abstract

The invention relates to a preparation method of a highly dispersed silicon dioxide microsphere with a controllable particle size. The preparation method comprises the following steps: (1) evenly mixing ethyl ortho-silicate and anhydrous ethanol; (2) dissolving inorganic salts into a mixed solution of ammonia water, anhydrous ethanol, and deionized water, wherein silicon dioxide microspheres with different particle sizes can be obtained according to the species and addition amounts of inorganic salts; and (3) stirring the solution obtained in the step (2) at a high speed, adding the solution obtained in the step (1) into the solution obtained in the step (2), reducing the stirring speed after the solutions are evenly mixed; two hours after reactions, carrying out centrifugal separation, and drying to obtain the silicon dioxide microsphere. The adopted equipment is simple, the operation is convenient, the repeatability is high, and the requirements on external environment are low. The particle size of the microsphere can be precisely controlled, during the preparation process of highly dispersed silicon dioxide microsphere. The reaction time is not changed. The prepared silicon dioxide microsphere has good dispersibility without grafting modification.

Description

technical field [0001] The invention relates to the field of non-metallic compounds, in particular to a method for preparing silica microspheres with high dispersion and controllable particle size. Background technique [0002] In recent years, silica microspheres have been widely used in chromatographic column fillers, coatings, catalysts, etc. due to their high mechanical strength, good stability, and easy dispersion in solvents. At the same time, silica microspheres also have the advantages of non-toxicity, high biological activity, hydrophilicity, and easy functionalization of surface silicon hydroxyl groups, and have potential application values ​​in the fields of biological detection and medicine. Remarkable results have been achieved in shear thickening fluids, two-dimensional ordered nanoparticle self-assembled arrays, and three-dimensional photonic crystals. Applications in these fields require that silica microspheres must have the characteristics of high roundnes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/32C01P2004/51C01P2004/62
Inventor 李玉芳金磊唐群涛沈鸿烈
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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