Preparation method of continuous controllable monodispersed silica microspheres

A technology of monodisperse silica microspheres and silica, applied in the direction of silica, silica, nanotechnology for materials and surface science, etc., can solve problems such as low efficiency and long reaction time, and achieve improvement Productivity, short reaction time, effect of solving agglomeration problems

Inactive Publication Date: 2014-08-27
NANJING DONGJIAN BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yoki et al. found a method to prepare nano-scale monodisperse silica with amino acids, but the reaction time is too long and the efficiency is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A method for preparing continuous and controllable monodisperse silica microspheres, comprising the following steps:

[0033](1) Nucleation step: add a certain amount of water, ethanol, and ammonia water in the three-necked glass bottle of the reaction kettle in sequence, turn on the agitator, and the stirring speed is 230~300rpm, heat up slowly, and wait until the mixed solution in the reaction kettle is completely boiled for 4~ After 10 minutes, add the ethanol solution of ethyl orthosilicate, the concentration of ethanol in the system is 0.014M, the concentration of ammonia water is 0.2M, V (tetraethyl orthosilicate): V (ammonia water) = 1:1, boiling reaction 0.5 hour, turn off the heater, stop the reflux of condensed water, but continue to stir and cool naturally, half an hour later, bottle the seed solution to obtain a 20-100nm monodisperse silica seed solution.

[0034] (2) Growth step: prepare a certain proportion of water-ethanol-ammonia water mixed solution and...

Embodiment 2

[0040] A method for preparing continuous and controllable monodisperse silica microspheres, comprising the following steps:

[0041] (1) Nucleation step: Add a certain amount of water, ethanol, and ammonia water in the three-necked glass bottle of the reaction kettle in sequence, turn on the agitator, heat up slowly, wait until the mixed solution in the reaction kettle boils completely for 4 to 10 minutes, then add orthosilicic acid Ethanol solution of ethyl ester, the concentration of ethanol in the system is 0.010M, the concentration of ammonia water is 0.5M, V (tetraethyl orthosilicate): V (ammonia water) = 1:1, boiling reaction for 1.5 hours, turn off the heater, stop Reflux the condensed water, but continue to stir and cool naturally. After half an hour, bottle the seed liquid to obtain a 20-100nm monodisperse silica seed liquid, or directly use the monodisperse silica obtained in Example 1 The microsphere suspension was used as seed.

[0042] (2) Growth step: Preparing ...

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PUM

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Abstract

The invention discloses a preparation method of continuous controllable monodispersed silica microspheres, and the process includes the steps of nucleation, growth and separation. The process can achieve batching preparation of the monodispersed silica microspheres with high degree of sphericity and narrow particle size distribution; according to the method, in the nucleation step of silica microsphere seeds, a reaction system is a boiling system, heat transfer and mass transfer are good in a strong convective state, the silica microsphere seeds can homogeneously and rapidly nucleate, the agglomeration problem in the prior art can be solved, the reaction time is shortened, and monodispersed microsphere seeds with narrower particle size distribution can be obtained. The monodispersed silica microspheres with high degree of sphericity and controllable particle size distribution can be obtained by one step growth or multi step growth to separate the steps of nucleation and growth, the particle size distribution deviation is less than 2%, and the performance is better. According to the actual need, monodispersed silica microspheres with various particle sizes from 20 to 10000nm can be obtained, and various problems of the prior art can be overcome.

Description

technical field [0001] The invention relates to a preparation method of silica microspheres, in particular to a continuous controllable preparation method of monodisperse silica microspheres with a particle size distribution of 20-10000nm. Background technique [0002] Monodisperse silica microspheres are non-toxic, odorless, non-polluting non-metallic materials with surface effect, small size, effect quantum size effect and macroscopic quantum tunnel effect, and produce singular mechanics, electricity, magnetism, Special properties such as optics, heat and chemistry have special significance in the field of science and technology, and have broad application prospects in many scientific fields such as standardization, information and information, analytical chemistry, medicine and biochemistry, electronic packaging materials, and polymer composite materials. [0003] In recent years, the preparation methods of monodisperse spherical nano-silica include gas phase method, prec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y30/00B82Y40/00
Inventor 顾忠泽张文冬徐永智杨子学孙小爱陈阳
Owner NANJING DONGJIAN BIOLOGICAL TECH
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