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Method for preparing nanometer SiO2 by using silica sol

A silica sol and nanotechnology, applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve problems such as difficulty in obtaining nanoparticles with uniform particle size, loss of fluidity, difficulty in stirring, etc., to achieve Uniform particle size distribution, good dispersibility, excellent dispersibility effect

Active Publication Date: 2021-03-19
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particle size distribution is not uniform, and due to the addition of inorganic acids such as hydrochloric acid and sulfuric acid, the local acidity in the sol is too high, and it is easy to agglomerate and deteriorate. On the contrary, the viscosity becomes larger because it loses fluidity. Turned into jelly, making it difficult to mix
Therefore, it is difficult to obtain nanoparticles with uniform particle size and monodispersity.
At the same time, the obtained nano-SiO 2 The particle size of the powder is determined by its production process and raw material ratio, and there is basically no repeatability

Method used

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  • Method for preparing nanometer SiO2 by using silica sol
  • Method for preparing nanometer SiO2 by using silica sol
  • Method for preparing nanometer SiO2 by using silica sol

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Experimental program
Comparison scheme
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Embodiment 1

[0073] This embodiment provides a method to prepare nano-SiO by using silica sol 2 method, which is as follows:

[0074] 1) After adding 50mL of ammonia-stabilized silica sol into a three-necked flask, add 5mL (about 0.05mol) of ethyl acetate and 0.5g (about 2.6mmol) of citric acid, and conduct a reflux reaction at 76°C for 3h (milky white appears during the reaction) , carrying out magnetic stirring during the reaction; wherein, the molar concentration of silicon dioxide in the silica sol is 4.99mol / L;

[0075] 2) The reacted product is centrifuged with a high-speed centrifuge, the centrifuged product is washed with warm water containing cetyltrimethylammonium bromide (CTAB), and 95% ethanol is used for solvent replacement and aging;

[0076] 3) The aged product is vacuum-dried, then put into a muffle furnace and roasted at 550° C. for 2 hours. After the roasting is completed, the roasted product is ground to obtain the nano-SiO 2 .

[0077] The nano-SiO that this embodime...

Embodiment 2

[0083] This embodiment provides a method to prepare nano-SiO by using silica sol 2 The method, the molar concentration of silicon dioxide in the silica sol used in this method is 6.66mol / L, and others are all identical with embodiment 1.

[0084] The nano-SiO that this embodiment prepares 2 The TEM image of Figure 3A As shown, nano-SiO 2 The particles are uniformly dispersed, and the particle size is about 15nm.

[0085] The nano-SiO that this embodiment prepares 2 The particle size analysis test results are shown in Table 2, Figure 3B As shown, from Table 2, Figure 3B It can be seen that nano-SiO 2 The particle size is small, the distribution is relatively uniform, and the average particle size of the secondary particle size is about 16.53nm.

[0086] Table 2

[0087]

[0088] The nano-SiO that this embodiment prepares 2 N 2 Adsorption-desorption curves such as Figure 3C shown by Figure 3C It can be seen that the nano-SiO prepared in this example 2 N 2 T...

Embodiment 3

[0092] This embodiment provides a method to prepare nano-SiO by using silica sol 2 The method, the molar concentration of silicon dioxide in the silica sol used in this method is 8.32mol / L, and others are all identical with embodiment 1.

[0093] The nano-SiO that this embodiment prepares 2 The TEM image of Figure 4A As shown, nano-SiO 2 The particles are uniformly dispersed, and the particle size is about 75nm. The nano-SiO that this embodiment prepares 2 The particle size analysis test results are shown in Table 3, Figure 4B As shown in Table 3, Figure 4B It can be seen that nano-SiO 2 The particle size is small, the distribution is relatively uniform, and the average particle size of the secondary particle size is about 92.42nm.

[0094] table 3

[0095]

[0096] The nano-SiO that this embodiment prepares 2 N 2 Adsorption-desorption curves such as Figure 4C shown by Figure 4C It can be seen that the nano-SiO prepared in this example 2 N 2 The adsorptio...

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Abstract

The invention provides a method for preparing nanometer SiO2 by using silica sol. According to the method, silica sol is used as a silicon source, citric acid is used as a protective agent, an acetatesubstance is used as a latent acid precipitant, and a chemical precipitation method is adopted to prepare the nanometer SiO2, wherein the molar concentration of SiO2 in the silica sol is 4.16-9.97 mol / L, the molar ratio of the acetate substance to silicon in the silica sol is 1: 2.97 to 1: 12.5, and the molar ratio of citric acid to silicon in the silica sol is 1: 40 to 1: 192. According to the method, the nanometer SiO2 with a large specific surface area and uniform dispersion is prepared by slowing down the speed of a direct gel reaction between SiO2 colloidal particles in silica sol and H<+> generated by the latent acid reagent.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for preparing nano-SiO by using silica sol 2 Methods. Background technique [0002] Nano silicon dioxide SiO 2 It is a green and environmentally friendly inorganic non-metallic material, commonly known as ultra-fine white carbon black, referred to as white carbon black, with hydroxyl groups on the surface, and the diameter of the particles is in the range of 1-100nm. It is an amorphous white powder. The microstructure is spherical, and under the transmission electron microscope, it is a network and flocculent quasi-granular structure. nano-SiO 2 It has four unique effects as nanomaterials, and has good special properties such as light, electricity, heat, force, magnetism, absorption, and radiation. It still has high toughness, high strength, and good stability at high temperatures. Therefore nano-SiO 2 Can be widely used in various fields. Optically, the sur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y30/00
CPCC01B33/18B82Y30/00C01P2004/64C01P2004/62C01P2006/12
Inventor 秦利霞杨宇翔张晓萍康诗钊李向清黄艳
Owner PETROCHINA CO LTD