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Preparation method of silicon oxide nanoparticles with uniform particle sizes

A nano-silica, silicon dioxide technology, applied in the direction of silicon oxide, silicon dioxide, nanotechnology, etc., can solve the problem of poor batch repeatability, huge influence of particle size, difficulty in controlling the uniformity and shape of nanoparticles, etc. problems, to achieve the effect of achieving scale and uniformity, reducing the concentration of metal impurities, and achieving batch stability

Inactive Publication Date: 2021-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the microemulsion method uses two phases and its particle size is greatly affected by factors such as the stirring speed and the form of the stirring paddle
Therefore, in the large-scale production process, the amplification effect of this preparation method is large, and it is difficult to scale up
The particle size of the scale-up produced silica spheres is not only unevenly distributed, but also has poor batch repeatability
[0008] Inorganic silicon sources obtain orthosilicic acid monomers by means of ion exchange, and then regulate the particle growth process of silica particles by means of orthosilicic acid polymerization, so that the synthesis of silica nanoparticles can be regulated and controlled. However, the raw materials in this preparation process Silicic acid has the characteristics of high activity, easy agglomeration, and instability. Generally, water glass will inevitably introduce metal impurity ions, resulting in the aggregation of orthosilicic acid to varying degrees, resulting in the size, uniformity, and surface properties of nano-silica particles. There is a big difference, especially in the process of regulating the scale by the seed crystal method, these impurity ions will cause the nucleation and growth of silicon oxide particles to mismatch, making it difficult to control the uniformity and particle morphology of nanoparticles

Method used

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  • Preparation method of silicon oxide nanoparticles with uniform particle sizes
  • Preparation method of silicon oxide nanoparticles with uniform particle sizes
  • Preparation method of silicon oxide nanoparticles with uniform particle sizes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Step 1, weigh the water glass sodium silicate raw material of 50g, wherein the silicon dioxide concentration of sodium silicate is 21wt%, the modulus SiO of sodium silicate 2 :Na 2 O=3.3:1; 160g of deionized water was added to the above sodium silicate solution, and stirred evenly to obtain a diluted inorganic sodium silicate solution.

[0081] The obtained cation exchange resin, model 731, will be purchased. Put the cation exchange resin into water and wash it until the solution does not contain impurities. Then use 4wt% hydrochloric acid to wash, and then use deionized water to wash until the washing water is neutral. Then the above diluted inorganic sodium silicate solution was added to obtain the required 5 wt.% concentration of orthosilicic acid solution.

[0082] Step 2. Mix 27 g of tetramethoxysilane and 5.6 g of methanol, then add to the orthosilicic acid solution obtained in step 1 and mix and stir to obtain an organic-inorganic hybrid solution of silicon so...

Embodiment 2

[0085] Step 1, weigh the water glass sodium silicate raw material of 50g, wherein the silicon dioxide concentration of sodium silicate is 21%, the modulus SiO of sodium silicate 2 :Na 2 O=3.3:1; 160g of deionized water was added to the above sodium silicate solution, and stirred evenly to obtain a diluted inorganic sodium silicate solution.

[0086] The obtained cation exchange resin, model 731, will be purchased. Put the cation exchange resin into water and wash it until the solution does not contain impurities. Then use 4wt% hydrochloric acid to wash, and then use deionized water to wash until the washing water is neutral. The above-mentioned inorganic sodium silicate solution was added to obtain a 5 wt.% concentration of orthosilicic acid solution.

[0087] Step 2. Mix 27 g of tetramethoxysilane and 5.6 g of methanol, then add to the orthosilicic acid solution obtained in step 1 and mix and stir to obtain an organic-inorganic hybrid solution of silicon source;

[0088] ...

Embodiment 3

[0090] The difference between sample 3# and sample 2# is: the primer crystal seed in the step 3 in the embodiment 2 is changed into sample 2#, and others are all identical operating steps, and the nano silicon dioxide mark that obtains is sample 3#.

[0091] The difference between sample 4# and sample 2# is: the base material seed crystal in step 3 in the embodiment 2 is changed into sample 3#, and others are all the same operation steps, and the nano silicon dioxide mark that obtains is sample 4#.

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Abstract

The invention discloses a preparation method of silicon dioxide nanoparticles with uniform particle sizes. The preparation method at least comprises the following steps: a) acquiring an orthosilicic acid solution; b) mixing the orthosilicic acid solution in the step a), an organic silicon source and an alcohol solvent to obtain an organic-inorganic hybrid solution; and c) mixing the organic-inorganic hybrid solution in the step b) with an alkaline solution, and carrying out an aging reaction to obtain the required silicon dioxide nanoparticles with uniform particle sizes. According to the preparation method, the purity of nanometer silicon oxide is improved, scale-controllable and uniformity-controllable preparation of the silicon dioxide nanoparticles is effectively realized, the large-scale preparation of the silicon dioxide nanoparticles can be realized, and the mildness, stability and controllability of the synthesis conditions of the silicon dioxide particles can be realized; and therefore, the batch stability of the silicon dioxide nanoparticles is easy to realize.

Description

technical field [0001] The application relates to a method for preparing nano-silica with uniform particle size, which belongs to the field of preparation of silica nano-materials. Background technique [0002] Nano-silica is amorphous silica with a particle size of nanometer (generally 1-200nm), and is a non-toxic, odorless, and non-polluting non-metallic oxide material. Nano-silica has small particle size, large specific surface area, moderate hardness, and excellent chemical properties. At the same time, nano-silica particles have physical or chemical properties with polymers due to surface defects and many non-pairing atoms. The chemical combination is more likely, so it can also be used to enhance the interfacial combination with the polymer matrix, improve the load-bearing capacity of the polymer, and thus strengthen the toughened polymer. Therefore, nano silicon oxide is widely used in integrated circuit manufacturing, rubber, chemical industry, special coatings, tex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y40/00
CPCC01B33/18B82Y40/00C01P2004/64C01P2004/03
Inventor 王树东苏宏久任高远高云峰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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