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Two-step preparation method of hollow silica particles

A silicon dioxide and particle technology, applied in the field of preparation of hollow silicon dioxide particles, can solve the problems of affecting the application performance of hollow silicon dioxide particles, environmental pollution, increase production costs, etc., to simplify the post-processing process and reduce production costs. , the effect of reducing the impact

Inactive Publication Date: 2011-08-31
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above examples, emulsifiers and template micelles play a key role in the formation of hollow silica particles, but their presence will affect the application performance of hollow silica particles
At the same time, specific emulsifier selection or preparation of functional micellar materials will also increase the production cost accordingly
Secondly, the organic solvent as the continuous phase in the water / oil emulsion system will also cause serious pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 5 parts of 25% ammonia water and 90 parts of distilled water into the flask, and heat the above solution to 25° C. in a water bath. Under stirring, slowly add the first batch of 0.06 parts of tetraethyl orthosilicate dropwise to the flask, finish adding within 30 minutes, continue to react for 5 minutes, then add the remaining 2.94 parts of tetraethyl orthosilicate to the above system, Keep the temperature constant, and react under stirring for 7 hours. The product was washed by centrifugation with distilled water, and dried under vacuum at 60°C to obtain hollow silica particles. Observed under a transmission electron microscope, it is a hollow particle with a particle size of 200-800nm ​​and a shell thickness of about 18nm.

Embodiment 2

[0019] Add 5 parts of 25% ammonia water and 90 parts of distilled water into the flask, and heat the above solution to 50° C. in a water bath. Under stirring, slowly add the first batch of 0.1 parts of ethyl orthosilicate dropwise to the flask, and finish adding within 50 minutes, and continue to react for 10 minutes, then, add the remaining 2.9 parts of ethyl orthosilicate to the above system, Keep the temperature constant, and react under stirring for 5 hours. The product was washed by centrifugation with distilled water, and dried under vacuum at 60°C to obtain hollow silica particles. Observed under a transmission electron microscope, it is a hollow particle with a particle size of 200-800nm ​​and a shell thickness of about 33nm.

Embodiment 3

[0021] Add 5 parts of 25% ammonia water and 90 parts of distilled water into the flask, and heat the above solution to 75° C. in a water bath. Under stirring, slowly add the first batch of 0.6 parts of ethyl orthosilicate dropwise to the flask, and finish adding within 30 minutes, and continue to react for 5 minutes, then, add the remaining 2.4 parts of ethyl orthosilicate to the above system, Keep the temperature constant, and react under stirring for 5 hours. The product was washed by centrifugation with distilled water, and dried under vacuum at 60°C to obtain hollow silica particles. Observed under a transmission electron microscope, it is a hollow particle with a particle size of 200-800nm ​​and a shell thickness of about 50nm.

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Abstract

The invention relates to a two-step preparation method of hollow silica particles, comprising the following steps of: heating ammonia-water to 25-75 DEG C; slowly dripping a part of silica precursor in the ammonia-water for reaction for 5-10 minutes; then adding rest silica precursor at constant temperature; stirring for reaction for a couple of hours; and centrifuging, washing, and drying in vacuum to obtain hollow silica particles. In the system, the weight percentage: water and ammonia-water (25 percent) is 15-150: 1; and the weight percentage of water and silica precursor is 10-30: 1. The silica precursor which is firstly added accounts for 2-20 percent of total amount of silica precursor; and the reaction temperature is 25-75 DEG C.

Description

(1) Technical field [0001] The invention belongs to the technical field of nanometer functional materials, and in particular relates to a preparation method of silicon dioxide hollow particles. (2) Technical background [0002] Hollow particle materials have attracted great attention because of their special structure, morphology and surface and interface properties. Compared with hollow organic particles, hollow inorganic particles have very superior thermal, optical, electrical, mechanical properties, and acid and alkali stability. Therefore, they are widely used as microcapsule materials in the controlled delivery and release systems of drugs, dyes, cosmetics, sensitive reagents (enzymes and proteins), and can also be used as lightweight fillers, highly selective catalysts or catalyst supports . In addition, they are also extremely valuable in artificial cells, disease diagnosis, etc. [0003] Silica hollow microspheres are one of the most important and widely concerne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12
Inventor 王昭群李云兴顾昊薛奇
Owner NANJING UNIV
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