Preparation method of nano silica microspheres

A nano-silicon dioxide, silicon dioxide technology, applied in the directions of silicon dioxide, silicon oxide, nanotechnology, etc., can solve the problems of unstable preparation process, difficult to meet the market demand of industrial scale production, etc., and achieve a simple preparation process. Effect

Inactive Publication Date: 2015-02-04
CHINA ACADEMY OF ENG PHYSICS FUNCTION MATERIAL RES INST
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Problems solved by technology

[0005] However, when the sol-gel method is used to prepare nano-silica, there are many factors that affect the particle size, dispersion and surface quality of the pro

Method used

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  • Preparation method of nano silica microspheres

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preparation example Construction

[0028] see figure 1 , figure 1 The flow chart of the steps of the method 100 for preparing nano-silica microspheres provided by the embodiment of the present invention includes:

[0029] Step S110: uniformly mixing the organic solvent and the alkaline solution to form a first mixed solution;

[0030] Preferably, the organic solvent is at least one of ethanol, methanol and propanol.

[0031] Preferably, the alkaline solution is an aqueous ammonia solution. It can be understood that the alkaline solution is an ammonia solution is only a preferred embodiment, and other alkaline solutions can also be used in practice.

[0032] Step S120: adding a polymer dispersant to the first mixed solution, and keeping it at a constant temperature to obtain a second mixed solution;

[0033] Preferably, the polymer dispersant is at least one of polyethylene glycol and ethylene glycol.

[0034] Preferably, the constant temperature is 20-60° C., and the holding time is 0.5-1 h.

[0035] Step...

Embodiment 1

[0045] Quantitatively take 1.5L of ammonia water and 16L of ethanol and add them into a 30L glass reactor, stir and mix evenly to form the first mixed solution; weigh 5g of polyethylene glycol, add it to the above-mentioned first mixture, keep it warm at 20°C for 1 hour, and stir to dissolve to form the first mixed solution. Two mixed solutions; add 1.8L tetramethoxysilane dropwise to the above second mixed solution for about 5 hours until the reaction mixture is milky white; after the reaction is completed, the above emulsion is centrifuged and vacuum-dried to obtain a particle size of 300 - 400nm silica nanospheres.

[0046] see figure 2 , for the nano-silica microspheres prepared in Example 1 of the present invention, from figure 2 It can be seen that the sphericity is good, the uniformity of the average particle size is good, the deviation is less than 10%, and the surface of the microspheres is smooth and free of defects.

Embodiment 2

[0048] In a three-necked flask (250mL) equipped with a stirrer, a syringe, and a thermometer, first add 112mL of a mixed solution of absolute ethanol and ammonia water, stir and mix evenly to form the first mixed solution; then add ethylene glycol dispersant, and keep the temperature at 45°C React in a water bath for 6 hours to obtain a second mixed solution; drop tetraethoxysilane into the second mixed solution until a milky white mixture is obtained; centrifuge and vacuum dry to obtain SiO2 with a particle size of about 500nm. powder.

[0049] see image 3 , for the nano-silica microspheres prepared in Example 2 of the present invention, from figure 2 It can be seen that the sphericity is good, the surface of the microspheres is smooth and free of defects.

[0050] see Figure 4 , which is the surface morphology and particle size distribution diagram of the nano-microspheres prepared by the above method in the present invention, from Figure 4 It can be seen from the fi...

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Abstract

The invention provides a preparation method of nano silica microspheres. Highly monodispersed nano silica microspheres can be obtained by using an organic silicate ester as a raw material and through the steps of hydrolyzation, centrifugal separation and vacuum drying in presence of a polymer dispersant and under an alkaline environment. The preparation process is simple and large-scale production of the nano silica microspheres can be realized.

Description

【Technical field】 [0001] The invention relates to a preparation method of nano silicon dioxide microspheres. 【Background technique】 [0002] Monodisperse nano-silica microspheres have the characteristics of good dispersion, uniform particle size, and smooth surface, and the silanol on the surface is suitable for functionalization as a bridge for modification, so that it can be used on catalyst carriers, monodisperse rheology, etc. Liquid, colloidal crystals, optical effects, medicine and solid fillers are widely used. With the development and application of high-tech materials, it is of great practical significance to prepare high-purity, controllable particle size, monodisperse spherical nano-silica conveniently and economically. Since Stober et al. synthesized monodisperse silica in 1968, nano-silica monodisperse system has been one of the most studied monodisperse systems. [0003] At present, the synthesis methods of silica can be divided into two categories: dry metho...

Claims

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Application Information

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IPC IPC(8): C01B33/18B82Y40/00
Inventor 钟发春刘键杨秀兰郝晓飞白军伟
Owner CHINA ACADEMY OF ENG PHYSICS FUNCTION MATERIAL RES INST
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