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Monodisperse silica nanoparticles and preparation method thereof

A technology of silica and nanoparticles, applied in the field of inorganic porous materials, can solve the problems of increasing cost, unfavorable environment, stirring reaction time and aging time to reduce product production efficiency, etc., to achieve short reaction time and reduce environmental pollution.

Active Publication Date: 2014-07-02
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In the prior art, the preparation method of silica needs to use a large amount of organic additives, which increases the cost and is not conducive to the environment. At the same time, the longer stirring reaction time and aging time in the preparation process will also reduce the production efficiency of the product.

Method used

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  • Monodisperse silica nanoparticles and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Dissolve 24.33g of ethyl orthosilicate (tetraethoxysilane) in 300ml of ethanol to obtain a silicon source; use a high-pressure pump to simultaneously extract the silicon source, a hydrogen peroxide solution with a concentration of 0.1mol / L, and 350°C and 22Mpa Put deionized water into the reactor, and control the pressure at about 22Mpa for reaction, the flow rate of extraction is 10ml / min, 10ml / min and 20ml / min respectively, and the suspension is obtained after 5-6 seconds of reaction; the suspension After pumping into the cooler for cooling, the obtained suspension was subjected to 7000r / min high-speed centrifugation to obtain a solid, and the obtained solid was mixed with ethanol for ultrasonic vibration washing. After repeated washing for 3 times, the solid was placed in a vacuum drying oven at 80°C After drying for 12 hours, monodisperse silica nanoparticles can be obtained.

[0045] The obtained monodisperse silica nanoparticles have good monodispersity, the avera...

Embodiment 2

[0048] Dissolve 24.33g of ethyl orthosilicate (tetraethoxysilane) in 300ml of ethanol to obtain a silicon source; use a high-pressure pump to simultaneously extract the silicon source, a hydrogen peroxide solution with a concentration of 0.3mol / L, and 350°C and 22Mpa Put deionized water into the reactor, and control the pressure at about 22Mpa for reaction, the flow rate of extraction is 10ml / min, 10ml / min and 20ml / min respectively, and the suspension is obtained after 5-6 seconds of reaction; the suspension After pumping into the cooler for cooling, the obtained suspension was subjected to 7000r / min high-speed centrifugation to obtain a solid, and the obtained solid was mixed with ethanol for ultrasonic vibration washing. After repeated washing for 3 times, the solid was placed in a vacuum drying oven at 80°C After drying for 12 hours, monodisperse silica nanoparticles can be obtained.

[0049] The obtained monodisperse silica nanoparticles have good monodispersity, the avera...

Embodiment 3

[0051] Dissolve 24.33g of ethyl orthosilicate (tetraethoxysilane) in 300ml of ethanol to obtain a silicon source; use a high-pressure pump to simultaneously extract the silicon source, a hydrogen peroxide solution with a concentration of 0.5mol / L, and 350°C and 22Mpa Put the deionized water into the reactor, and control the pressure at about 22Mpa to react, the flow rate of extraction is 20ml / min, 10ml / min and 10ml / min, and the suspension is obtained after reacting for 5 to 6 seconds; the suspension After the liquid is pumped into the cooler for cooling, the obtained suspension is subjected to 7000r / min high-speed centrifugation to obtain a solid, and the obtained solid is mixed with ethanol for ultrasonic vibration washing. After repeated washing for 3 times, the solid is placed in a vacuum oven at 80°C Dry in medium for 12 hours to obtain monodisperse silica nanoparticles.

[0052] The obtained monodisperse silica nanoparticles have good monodispersity, the average particle ...

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Abstract

The invention discloses a preparation method of monodisperse silica nanoparticles. The preparation method comprises the following steps: mixing a silicon source containing alkoxy silane with critical water and reacting to obtain suspension, and implementing solid-liquid separation to the suspension to obtain a finished product, wherein a structural formula of the alkoxy silane is represented as R<1>mR<2>nSi(OR<3>)4-m-n, both m and n are integers and m+n is equal to 0, 1, 2 or 3, and R<1>, R<2> and R<3> independently represent alkyl; the critical water is water at temperature of 200-500 DEG C and under pressure of 5-30Mpa; the reaction is implemented at 200-500 DEG C and under 5-30Mpa. The preparation method disclosed by the invention is free from such organic matters such as a surfactant, can relieve environmental pollution and is short in reaction time. Furthermore, the invention discloses the monodisperse silica nanoparticles prepared by the method. The particles are relatively uniform in distribution, have a medium microporous structure, are relatively large in surface area and have a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of inorganic porous materials, and in particular relates to monodisperse silica nanoparticles and a preparation method thereof. Background technique [0002] Monodisperse silica spherical nanoparticles have been widely used in the field of catalyst carriers and drug carriers due to their large specific surface area and pore volume, non-toxic and biocompatible properties. At the same time, photonic crystals composed of monodisperse silicon dioxide also have broad application prospects in the field of optoelectronics. [0003] At present, the preparation methods of monodisperse silica mainly include sol-gel method, microemulsion method and chemical vapor deposition method, etc., but due to the long reaction time and aging time, it is not conducive to application and promotion. [0004] The Chinese patent document with publication number CN103318899 discloses a method for controlling the particle size of monod...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y30/00B82Y40/00
Inventor 翁小乐张竞宜吴忠标刘越王海强
Owner ZHEJIANG UNIV
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