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Preparation method of monodisperse porous silicon dioxide microspheres

A technology of porous silicon dioxide and silicon dioxide, applied in the direction of silicon dioxide, silicon oxide, nanotechnology for materials and surface science, etc., can solve the problems of many reactants, high biological toxicity, and complicated preparation process, etc. Achieve the effect of pure product, mild reaction conditions and simple preparation method

Active Publication Date: 2015-09-16
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, DechaoNiu et al. used the block copolymer PS-b-PAA and cetyltrimethylammonium bromide (CTAB) dual templates to prepare macroporous silica and used it in the field of drug delivery (Niu D, Liu Z , Li Y, et al.[J].Advanced Materials, 2014), but this method uses the traditional template agent CTAB, CTAB is a quaternary ammonium salt cationic surfactant, which has high biological toxicity, which limits the use of this surfactant Applications of Synthetic Porous Materials
[0004] In the Chinese patent literature, Chen Tiehong et al. (CN1923684A) used a less toxic anionic surfactant (sodium lauryl sarcosinate) as a template to prepare mesoporous silica, but the particle size of the prepared mesoporous silica Inhomogeneous, and can only be mesoporous with a pore size of ~3nm, and, due to the use of structure-directing agents such as (3-aminopropyl)trimethoxysilane, many reactants are used, and the preparation process is complicated, which greatly limits the The preparation and application of the material
Dai Zhao et al. (CN 102351200A) used organic polymer microspheres of small particle size as pore-forming agents, and finally used solvent or calcination to remove internal organic templates to prepare macroporous silica microspheres; due to the use of organic polymer microspheres The ball is used as a template, so it is necessary to use solvent or calcination to remove this template, which leads to the toxicity of this method, which is not environmentally friendly, and consumes a lot of energy. It is difficult to show the value of this method in practical applications.

Method used

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  • Preparation method of monodisperse porous silicon dioxide microspheres
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  • Preparation method of monodisperse porous silicon dioxide microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 5mL of ammonia water and 96mL of absolute ethanol into a single-necked flask, stir and mix evenly, and place in a 30°C water bath. After the temperature stabilizes, take 4mL of tetraethyl orthosilicate (TEOS) and 4mL of absolute ethanol, mix evenly, and then add dropwise , stirred at room temperature for 24h, the product was centrifuged and washed several times with absolute ethanol, and finally dried to obtain monodisperse solid silica microspheres, and its transmission electron microscope photo is as follows figure 1 As shown, it can be seen that the prepared solid silica microspheres have a complete structure, uniform size, and a particle size of about 70nm.

[0027] Take 0.5 g of the above-mentioned solid silica microspheres and 20 mL of deionized water and put them into a polytetrafluoroethylene-lined hydrothermal reaction kettle, and place them in a thermostat at 130°C for 12 hours. The product was taken out and centrifuged and washed several times with absolu...

Embodiment 2

[0030] Take the mixed solution of 0.5g of solid silica microspheres obtained in step 1 of Example 1 and 20mL of deionized water and absolute ethanol, and add it to a hydrothermal reaction kettle with a polytetrafluoroethylene liner, and place it in a 120°C Stand in the incubator for 18h. The product was taken out and centrifuged, washed several times with absolute ethanol, and dried to obtain a monodisperse porous silica microsphere material. Wherein the volume ratio of deionized water and absolute ethanol is 2:1. The micropores on the prepared porous silicon dioxide microspheres are evenly distributed, and the pore size is about 12 nm.

[0031] In this example, absolute ethanol was added during the hydrothermal reaction, because ethanol has a better dissolving effect on silicon dioxide, so the dual effects of ethanol and water in the high temperature and high pressure reaction environment lead to the final formation of porous The pores of silica become larger.

Embodiment 3

[0033] The aqueous solution of 0.5 g of solid silica microspheres and 20 mL of water-soluble polymer obtained in step 1 in Example 1 was added to a hydrothermal reaction kettle lined with polytetrafluoroethylene, and placed in a constant temperature box at 100 ° C. Set 20h. The product was taken out and centrifuged, washed several times with absolute ethanol, and dried to obtain a monodisperse porous silica microsphere material. The aqueous solution of the water-soluble polymer is prepared by mixing 0.05 g of polyvinylpyrrolidone (PVP) with deionized water.

[0034] The prepared porous silica microsphere transmission electron microscope photograph is as follows image 3 As shown, it can be seen that the distribution of micropores is uniform, and the pore size is about 20 nm. In this embodiment, since the addition of PVP can penetrate into the interior of the silica during hydrolysis, more nanoparticles are removed, resulting in further enlargement of the pores of the final p...

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Abstract

The invention discloses a preparation method of monodisperse porous silicon dioxide microspheres, which comprises the following steps: hydrolyzing ethyl orthosilicate under alkaline conditions to generate nano solid silicon dioxide microspheres, and carrying out hydrothermal treatment to implement solid-to-porous transition, thereby obtaining the monodisperse porous silicon dioxide microsphere material with controllable microsphere diameter / pore size and favorable biocompatibility. The preparation method is simple, and has the advantages of mild reaction conditions and no harm to the environment. The prepared porous silicon dioxide microspheres have favorable monodispersity and biocompatibility, and can be widely used in the fields of biomedicine, catalytic carriers and the like.

Description

technical field [0001] The invention relates to material synthesis and preparation technology, in particular to a preparation method of monodisperse porous silica microspheres. Background technique [0002] Since Kresge and other scientists of Mobil Corporation successfully synthesized the M41S series of ordered mesoporous silica materials using cationic surfactants as templates in 1992, due to their advantages such as high specific surface area and ordered pore distribution, they have been widely used in biomedicine. And catalytic materials and other fields have extremely broad application prospects, and porous materials represented by it have rapidly become a research hotspot in the field of materials at home and abroad. [0003] Generally, porous silica materials use surfactant molecular aggregates as templates, and tetraethyl orthosilicate as a silicon source. In aqueous solution, surfactant self-assembled micelles and tetraethyl orthosilicate interfaces are assembled in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y30/00
Inventor 戴李宗余世荣袁丛辉罗伟昂毛杰许一婷陈国荣曾碧榕
Owner XIAMEN UNIV
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