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Method for one-step controllable synthesis of unimodal poly-dispersive nano and submicron silica particles

A silicon dioxide, monodisperse technology, applied in the field of nanomaterials, can solve the problems of narrow size range, long reaction time, ammonia and water consumption cannot be controlled independently, and achieve the effect of simple equipment and high synthesis efficiency

Active Publication Date: 2017-02-15
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction time of this method is long, especially when synthesizing submicron particles, which requires multiple growths on the seed crystal
CN101891208A discloses a method for preparing submicron silica sphere particles. The obtained silica particles have a size of 100nm to 400nm and a narrow size range. The amount of ammonia and water used in the synthesis process cannot be independently and precisely regulated, and it is difficult to adjust the size of the particles. to control the dispersion of

Method used

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  • Method for one-step controllable synthesis of unimodal poly-dispersive nano and submicron silica particles
  • Method for one-step controllable synthesis of unimodal poly-dispersive nano and submicron silica particles
  • Method for one-step controllable synthesis of unimodal poly-dispersive nano and submicron silica particles

Examples

Experimental program
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Effect test

Embodiment 1

[0036] A one-step controllable synthesis of monodisperse, bidisperse, unimodal polydisperse nanometer and submicron silicon dioxide particles. The steps are as follows:

[0037] (1) Mix 3ml tetraethyl orthosilicate with 18ml acetone, and stir magnetically for 20min;

[0038] (2) Add 0.4850ml of ultrapure water to 18ml of acetone, stir magnetically for 10min, then add 0.7142ml of ammonia in methanol solution (7M), and continue stirring;

[0039] (3) Pour the solution obtained in step (1) into the solution prepared in step (2), stir magnetically for 7 hours at room temperature, and then move to a furnace with a preheating temperature of 60° C. for aging for 12 hours. After filtration, centrifugation, repeated washing with acetone and ethanol, and drying at 60°C, monodisperse silica particles with a particle size of 157nm (100-200nm) were obtained. See the SEM photo figure 1 . From figure 1 It can be seen that the particle size of the prepared material is uniform and the parti...

Embodiment 2

[0041] A one-step controllable synthesis of monodisperse, bidisperse, unimodal polydisperse nanometer and submicron silicon dioxide particles. The steps are as follows:

[0042] (1) Mix 3ml tetraethyl orthosilicate with 6ml acetone, and stir magnetically for 20min;

[0043] (2) Add 1.698ml of ultrapure water to 6ml of acetone, stir magnetically for 10 minutes, then add 2.143ml of ammonia in methanol solution (7M), and continue stirring;

[0044] (3) Pour the solution obtained in step (1) into the solution prepared in step (2), stir magnetically for 12 hours at room temperature, and then move to a furnace with a preheating temperature of 60° C. for aging for 18 hours. After filtration, centrifugation, repeated washing with acetone and ethanol, and drying at 60°C, monodisperse silica particles with a particle peak size of 800nm ​​(700-1000nm) were obtained.

Embodiment 3

[0046] A one-step controllable synthesis of monodisperse, bidisperse, unimodal polydisperse nanometer and submicron silicon dioxide particles. The steps are as follows:

[0047] (1) Mix 3ml tetraethyl orthosilicate with 180ml acetone, and stir magnetically for 20min;

[0048](2) Add 1.940ml of ultrapure water to 180ml of acetone, stir magnetically for 10min, then add 2.143ml of ammonia in methanol solution (7M), and continue stirring;

[0049] (3) Pour the solution obtained in step (1) into the solution prepared in step (2), stir magnetically for 12 hours at room temperature, and then move to a furnace with a preheating temperature of 50° C. for aging for 24 hours. After filtration, centrifugation, repeated washing with acetone and ethanol, and drying at 60°C, monodisperse silica particles with a particle peak size of 900nm (800-1000nm) were obtained.

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Abstract

The invention provides a method for the one-step controllable synthesis of mono-dispersive, bidispersive and unimodal poly-dispersive nano and submicron silica particles. According to the method, tetraethoxysilane, water and organic amine are respectively dissolved in an anhydrous organic solvent. A tetraethoxysilane solution is poured into an organic solution containing water and organic amine to be mixed with the organic solution. Obtained materials are subjected to hydrolysis, nucleation, growth, separation, washing and drying to obtain nano and submicron silica spherical particles high in purity and good in dispersibility. The preparation method is simple in process and equipment, high in synthesis efficiency and suitable for large-scale production. The amount of water and the amount of organic amine are accurately and separately controlled, and mono-dispersive, bidispersive or unimodal poly-dispersive nano and submicron silica particles are prepared through the one-step pot method. The particle sizes of obtained particles are 50 nm to 1000 nm.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and specifically relates to a one-step controllable method for synthesizing unimodal polydisperse (including monodisperse, bidisperse, tridisperse and above) nanometer and submicron silicon dioxide particles. Background technique [0002] Submicron silica is an important inorganic non-metallic material due to its high specific surface area, excellent optics, and chemical stability. It has important applications in the fields of construction, chemical industry, aerospace, and biomedicine. Most of the current research focuses on the preparation, characterization and application of monodisperse particles, but in actual use, polydisperse particles are closer to the real particle size distribution of the sample, especially the unimodal polydisperse system. [0003] With the rapid increase of industrial pollutant emissions in recent years, and people's growing concern about their own health and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/14B82Y40/00
CPCC01B33/14C01P2004/03C01P2004/32C01P2004/52C01P2004/62C01P2004/64
Inventor 陈岚田国兰王友峰葛广路
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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