CN107915230A - A kind of preparation method of nanometer particle - Google Patents

A kind of preparation method of nanometer particle Download PDF

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Publication number
CN107915230A
CN107915230A CN201711239863.4A CN201711239863A CN107915230A CN 107915230 A CN107915230 A CN 107915230A CN 201711239863 A CN201711239863 A CN 201711239863A CN 107915230 A CN107915230 A CN 107915230A
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China
Prior art keywords
small
nanometer particle
dropwise
preparation
6mol
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CN201711239863.4A
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Chinese (zh)
Inventor
程桂平
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Individual
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Individual
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Priority to CN201711239863.4A priority Critical patent/CN107915230A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/021Preparation

Abstract

A kind of preparation method of nanometer particle, step are as follows:Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, 80 °C are heated to after stirring the lower 2mol/L sodium hydroxide solutions for adding 7.0mL;Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.

Description

A kind of preparation method of nanometer particle
Technical field
A kind of preparation method of nanometer particle.
Background technology
In the prior art, the preparation method process of nanometer particle is cumbersome, and yield rate is low.
The content of the invention
The present invention provides a kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.0mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Simple technological process is used, process environmental protection is easy to operate, easy to spread.
Embodiment
Embodiment 1
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.1mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 2
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.2mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 3
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.3mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 4
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.4mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 5
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.5mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 5
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.5mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 6
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.6mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 7
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.7mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 8
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.8mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 9
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.9mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
Embodiment 10
A kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L sodium hydroxides for adding 8mL 80 °C are heated to after solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.

Claims (2)

1. a kind of preparation method of nanometer particle, step are as follows:
Step 1:2g cetyl trimethylammonium bromides are added in 720mL water, stir the lower 2mol/L hydroxides for adding 7.0mL 80 °C are heated to after sodium solution;
Step 2:Dropwise instill 15.0mL ethyl orthosilicates, continue stirring 2 it is small when;
Step 3:Positive four butyl esters of silicic acid of 5.0mL are instilled dropwise, when ultrasonic disperse 1 is small;
Step 4:It is cooled to room temperature, after filtering white precipitate, is washed 5 times with 2L deionized waters;
Step 5:1L is used again, and the ethanol of 6mol/L washs 5 times, 60 °C of dryings;
Step 6:White powder roasted under 550 °C 3 it is small when remove surfactant, you can obtain nanometer particle.
2. having used simple technological process, process environmental protection is easy to operate, easy to spread.
CN201711239863.4A 2017-11-30 2017-11-30 A kind of preparation method of nanometer particle Withdrawn CN107915230A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114010845A (en) * 2021-11-01 2022-02-08 淮阴工学院 Near-infrared light response antibacterial coating and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101214962A (en) * 2008-01-11 2008-07-09 东南大学 Method for preparing mesoporous silicon dioxide micro-sphere by combined template method
CN101475183A (en) * 2009-01-15 2009-07-08 北京航空航天大学 Preparation of hollow mesoporous silicon dioxide sphere with continuously variable cavity diameter
CN101559952A (en) * 2009-05-13 2009-10-21 南京工业大学 Method for preparing nanoscale mesoporous silica spheres
CN103738969A (en) * 2013-12-25 2014-04-23 上海纳米技术及应用国家工程研究中心有限公司 Mesoporous silica and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101214962A (en) * 2008-01-11 2008-07-09 东南大学 Method for preparing mesoporous silicon dioxide micro-sphere by combined template method
CN101475183A (en) * 2009-01-15 2009-07-08 北京航空航天大学 Preparation of hollow mesoporous silicon dioxide sphere with continuously variable cavity diameter
CN101559952A (en) * 2009-05-13 2009-10-21 南京工业大学 Method for preparing nanoscale mesoporous silica spheres
CN103738969A (en) * 2013-12-25 2014-04-23 上海纳米技术及应用国家工程研究中心有限公司 Mesoporous silica and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114010845A (en) * 2021-11-01 2022-02-08 淮阴工学院 Near-infrared light response antibacterial coating and preparation method thereof

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