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Preparation process of hollow silica ball

A technology of silica and hollow spheres, which is applied in the direction of silica and silica, can solve the problems of agglomerated particle size of silica hollow spheres, complex preparation process, and unevenness, so as to shorten the synthesis time and simplify the preparation The effect of gentle steps and processes

Inactive Publication Date: 2009-06-03
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to propose a method for preparing hollow silica spheres without the use of organic sacrificial templates and surfactants, and the prepared hollow silica spheres have better monodispersity and are suitable for industrial production; There are technologies that need to prepare templates or use surfactants in advance, the preparation process is complicated, time-consuming, and the obtained silica hollow spheres will be agglomerated and have different particle sizes

Method used

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  • Preparation process of hollow silica ball
  • Preparation process of hollow silica ball
  • Preparation process of hollow silica ball

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Example 1: Preparation of hollow silicon dioxide spheres with an inner diameter of 40 nanometers and a wall thickness of 10 to 20 nanometers with polyacrylic acid

[0019] In this embodiment, the polyelectrolyte is polyacrylic acid as an example, the alcohol solvent is ethanol as an example, and the silicon source precursor is tetraethyl orthosilicate as an example; take 0.08 grams of polyacrylic acid and put it in a 50 ml conical flask with a stopper, add 1. 50 ml of 25% ammonia water was slightly stirred until it was completely dissolved, then 30 ml of ethanol was quickly added, and vigorously stirred for 30 minutes, 0.50 ml of 4.4 mol / L tetraethyl orthosilicate was added dropwise at a rate of 0.05 ml / hour, and the stirring was continued after the addition 4 hours. After the reaction, the product obtained was centrifuged and washed at least three times with distilled water and absolute ethanol respectively, so as to remove impurities. Finally, the product was dried i...

Embodiment 2

[0031] Example 2: Preparation of hollow silicon dioxide spheres with an inner diameter of 50 to 60 nanometers and a wall thickness of 40 nanometers with sodium polyacrylate

[0032] In this embodiment, the polyelectrolyte is sodium polyacrylate as an example, the alcohol solvent is ethanol as an example, and the silicon source precursor is tetraethyl orthosilicate as an example; take 0.1 g of sodium polyacrylate and place it in a 50 ml stoppered Erlenmeyer flask , add 2.50 ml of 20% ammonia water and stir gently until completely dissolved, quickly add 30 ml of ethanol, stir vigorously for 30 minutes, add 2.00 ml of 2.2 mol / liter tetraethyl orthosilicate dropwise at a rate of 0.2 ml / hour, and the addition is complete Stirring was continued for 10 hours. After the reaction, the product obtained was centrifuged and washed at least three times with distilled water and absolute ethanol respectively, so as to remove impurities. Finally, the product was dried in a vacuum oven at 60°...

Embodiment 3

[0040] Example 3: Preparation of hollow silicon dioxide spheres with an inner diameter of 20 nanometers and a wall thickness of 42 nanometers with sodium polymethacrylate

[0041] In this embodiment, the polyelectrolyte takes sodium polymethacrylate as an example, the alcohol solvent takes ethanol and isopropanol as an example, and the silicon source precursor takes tetraethyl orthosilicate as an example; take 0.03 grams of sodium polymethacrylate in Add 2.00 ml of 25% ammonia water to a 50 ml conical flask with a stopper and stir slightly until it is completely dissolved, then quickly add 30 ml of a mixed alcohol solution with a volume ratio of ethanol and isopropanol of 1:1, stir vigorously for 30 minutes, and dissolve 1.80 ml of 4.4 mol / liter tetraethyl orthosilicate was added dropwise at a rate of 0.15 ml / hour, and stirring was continued for 8 hours after the addition was completed. After the reaction, the product obtained was centrifuged and washed at least three times wi...

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Abstract

The preparation process of hollow silica ball includes the following steps: adding alcohol solvent into ammonia water solution of polymer electrolyte in 3-500 g / L concentration, dropping silicon source precursor solution of 1.1-4.4 mol / L concentration in the speed of 0.05-0.2 ml and silicon source precursor / ammonia water volume ratio of 1 / 15 to 2, reaction in a sealed container at 10-40 deg.c for 2-24 hr, and washing and drying the product, with the ammonia water having concentration of 10-25 wt% and the volume ratio between alcohol solvent and ammonia water being 3 to 25. The preparation process of the present invention is simple and suitable for industrial production, and has mild reaction condition, no environmental pollution and high yield, and the obtained hollow silica ball is loose, has inner diameter of 10-250 nm and water thickness of 10-40 nm, and may be used as medicine carrier and catalyst carrier.

Description

Technical field: [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for preparing hollow silicon dioxide spheres by using a sol-gel method. Background technique: [0002] The existing common methods for preparing silica hollow spheres include organic template method, surfactant vesicle template method, layer-by-layer self-assembly method, etc. For example: the United States "Langmuir" (Langmuir, 2005, volume 21, pages 6572-6575) reported the use of organic sacrificial templates to prepare hollow silica spheres. In order to remove the templates, the product needs to be subjected to 660 ° C. Calcination treatment. The hollow spheres obtained by this traditional template method are seriously agglomerated and not suitable for further use. [0003] American "Langmuir" (Langmuir, 2003, volume 19, pages 1069-1074), British "Journal of Materials Chemistry" (Journal of Materials Chemistry, 2001, volume 11, pages 19...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18
Inventor 俞书宏万勇
Owner UNIV OF SCI & TECH OF CHINA
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