Novel green single-dispersed silica nanoparticle preparation method

A technology of silica and nanospheres, applied in the field of nanomaterials, can solve the problems of difficulty in obtaining high-quality SiO2 nanospheres, poor controllability and repeatability of silica nanospheres, and difficulty in recycling, and achieve uniform morphology. , The system can be reused and the appearance is good.

Inactive Publication Date: 2017-10-24
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method only utilizes the interaction between solvents and does not contain a preparation template, so the controllability and repeatability of preparing silica nanospheres are poor, and it is difficult to obtain high-quality SiO 2 nanosphere
Another preparation of SiO 2 The commonly used method of nanospheres is the microemulsion method, and the SiO prepared by this method 2 Nanospheres have good monodispersity and adjustable size, but when constructing microemulsion templates, a large amount of surfactants and co-surfactants need to be consumed, and these two components are partially dissolved in addition to entering the interface film of microemulsions. In the water phase and oil phase, it is not easy to recycle, and it will pollute the environment, and the surface active agent loaded on the surface of the material is difficult to wash and remove, which affects its purity. These problems have seriously restricted the microemulsion method in the preparation of silica nanoparticles. Aspects of application

Method used

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  • Novel green single-dispersed silica nanoparticle preparation method
  • Novel green single-dispersed silica nanoparticle preparation method
  • Novel green single-dispersed silica nanoparticle preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Mix 4 g of secondary ultrapure water with 76 g of ethanol, add 20 g of dichloromethane under stirring conditions, and continue stirring for 10 min after the addition is complete.

[0043] (2) 1.3 ml of ethyl orthosilicate was slowly added to the O / W surfactant-free microemulsion system obtained in step (1) under stirring, followed by sonicating for 10 minutes and stirring for 20 minutes after the addition was completed.

[0044] (3) The O / W type surfactant-free microemulsion system containing ethyl orthosilicate obtained in step (2) is moved into an ice-water bath, and under stirring conditions, 3ml of ammonia water (25wt﹪) is slowly added therein, and stirring is continued for 10min Then, the reaction apparatus was moved into a 25°C water bath and allowed to react for 6h.

[0045] (4) After the reaction is completed, a white solid is obtained by centrifugation, and the white solid is washed three times to obtain SiO 2 Nanospheres. The remaining liquid fractions w...

Embodiment 2

[0047] (1) Mix 4g of secondary ultrapure water with 36g of ethanol, add 10g of dichloromethane under stirring conditions, and continue to stir for 10min after the addition is complete.

[0048] (2) 1.3 ml of ethyl orthosilicate was slowly added to the O / W surfactant-free microemulsion system obtained in step (1) under stirring, followed by sonicating for 10 minutes and stirring for 20 minutes after the addition was completed.

[0049] (3) The O / W type surfactant-free microemulsion system containing ethyl orthosilicate obtained in step (2) is moved into an ice-water bath, and under stirring conditions, 3ml of ammonia water (25wt﹪) is slowly added therein, and stirring is continued for 10min Then, the reaction apparatus was moved into a 25°C water bath and allowed to react for 6h.

[0050] (4) After the reaction is completed, a white solid is obtained by centrifugation, and the white solid is washed three times to obtain SiO 2 Nanospheres. The remaining liquid fractions were d...

Embodiment 3

[0052] (1) Mix 4g of secondary ultrapure water with 16g of ethanol, add 5g of dichloromethane under stirring conditions, and continue stirring for 10min after the addition.

[0053] (2) 1.3 ml of ethyl orthosilicate was slowly added to the O / W surfactant-free microemulsion system obtained in step (1) under stirring, followed by sonicating for 10 minutes and stirring for 20 minutes after the addition was completed.

[0054] (3) The O / W type surfactant-free microemulsion system containing ethyl orthosilicate obtained in step (2) is moved into an ice-water bath, and under stirring conditions, 3ml of ammonia water (25wt﹪) is slowly added therein, and stirring is continued for 10min Then, the reaction apparatus was moved into a 25°C water bath and allowed to react for 6h.

[0055] (4) After the reaction is completed, a white solid is obtained by centrifugation, and the white solid is washed three times to obtain SiO 2 Nanospheres. The remaining liquid fractions were distilled, an...

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Abstract

The invention provides a novel green single-dispersed silica nanoparticle preparation method. The method includes: preparing an O / W-type water / ethanol / dichloromethane surfactant-free microemulsion; completely dissolving tetraethoxysilane (TEOS) in a spherical 'oil core' of the O / W-type water / ethanol / dichloromethane surfactant-free microemulsion prepared in the first step under the action of ultrasound and agitation, subjecting the TEOS to hydrolytic polycondensation and performing centrifugal separation after reaction; washing solid components with a polar solvent for multiple times to obtain single-dispersed SiO2 nanoparticles, and distilling remaining liquid components to collect ethanol and dichloromethane. The method is simple in operation, low in cost, environment friendly, reusable in system and high in efficiency; the prepared SiO2 nanoparticles are uniform in size, and universality and scale productive values are achieved; the method is simple in step, convenient in operation and high in practicability.

Description

technical field [0001] The invention belongs to the field of nanomaterials, and in particular relates to a preparation method of a novel green monodisperse silica nanosphere. Background technique [0002] Monodisperse SiO 2 Nanospheres have important application value in biomedicine, catalysis, functional materials, high-performance ceramics, coatings and other fields due to their large specific surface area, good dispersibility, and good optical and mechanical properties. method is currently used to prepare SiO 2 One of the commonly used methods for nanospheres, this method has the advantages of simple operation and clean surface of the prepared silica nanospheres. This method only uses the interaction between solvents and does not contain a preparation template, so the controllability and repeatability of the preparation of silica nanospheres are poor, and it is difficult to obtain high-quality SiO 2 Nanospheres. Another preparation of SiO 2 The commonly used method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2002/85C01P2004/04C01P2004/32C01P2004/62
Inventor 柴金岭孙斌潘金
Owner SHANDONG NORMAL UNIV
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