CN102815712A - Preparation method of nanometer SiO2 particles - Google Patents
Preparation method of nanometer SiO2 particles Download PDFInfo
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- CN102815712A CN102815712A CN2012101798452A CN201210179845A CN102815712A CN 102815712 A CN102815712 A CN 102815712A CN 2012101798452 A CN2012101798452 A CN 2012101798452A CN 201210179845 A CN201210179845 A CN 201210179845A CN 102815712 A CN102815712 A CN 102815712A
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- sio
- solution
- ethanol
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- volume ratio
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Abstract
The invention provides a preparation method of SiO2. The preparation method comprises the following steps: 1, mixing ethanol and ethyl orthosilicate with a volume ratio of the ethanol to the ethyl orthosilicate of 1:2 to prepare a solution A; 2, mixing the ethanol and 13.4mol/L ammonia water with a volume ratio of the ethanol to the 13.4mol/L ammonia water of 1:2-2:1 to prepare a solution B; 3, respectively pouring the solution A and the solution B to two separating funnels, and adjusting the dropping rates of solution drops and the rotation speed of an electronic stirrer; 4, transferring an SiO2 precipitate; 5, repeatedly carrying out ultrasonic washing and centrifuging of the SiO2 obtained in step 4; and 6, drying the SiO2 obtained in step 5 under infrared rays.
Description
Technical field
The invention belongs to the nanometer particle field, particularly a kind of nanometer SiO
2The preparation method of particle.
Background technology
There is rheological phenomena in the liquid of known highly concentrated nano level particle preparation, when receiving the external force collision is, can be used for cushioning the extraneous shearing force of a part, when liquid changes near the solid state, recurs and keeps out effect completely.And the flowability of liquid can solve the thick and heavy shortcoming that can't nimble use of traditional protector well.
Summary of the invention
The present invention provides a kind of nanometer SiO that prepared
2The preparation method of particle, this method prepare SiO with tetraethoxy
2The chemical principle of particle:
Hydrolysis reaction: Si (OC
2H
5)
4+ 4H
2O → Si (OH)
4+ 4OC
2H
5OH
Condensation reaction: Si (OH)
4→ SiO
2+ 2H
2O
Total reaction: Si (OC
2H
5)
4+ 2H
2O → SiO
2+ 4OC
2H
5OH
SiO of the present invention
2The preparation method comprises the following steps:
With volume ratio is ethanol and the tetraethoxy mixing wiring solution-forming A of 1:2;
Be the ammoniacal liquor wiring solution-forming B of the ratio of 1:2-2:1 again with the volume ratio with ethanol and 13.4mol/L;
Respectively solution A, B are poured in 2 separating funnels, reconcile the rotating speed that following speed of drop and electronics stir appearance;
Shift SiO
2Deposition;
SiO to step 4)
2Carry out supersound washing and centrifugal repeatedly;
At infrared down baking step 5) SiO
2
The preferred embodiment of the invention, solvent for use is selected from absolute ethyl alcohol, zero(ppm) water, absolute ethyl alcohol during the step 5) washing, or its mixture.
The silicon dioxide granule of the present invention's preparation of the present invention has SiO
2" solid-liquid conversion " reciprocal characteristics.
The silicon-dioxide stable in properties of the present invention's preparation of the present invention, nontoxic basically, centralized particle diameter, nanometer scale, hardness is high, SiO
2Can be used for as disperse phase.
Description of drawings
Accompanying drawing 1: the SiO of medicine ratio and system
2The parameter map of particle diameter.
Accompanying drawing 2: sample one particle diameter test result.
Can be seen that by test result the nano silica powder particle diameter of experiment gained is very even, radius is about 110nm.
Embodiment
Following examples are used to specify the present invention, yet can not the present invention be interpreted as and only comprise following examples.
Material and instrument:
Three drop bottles, electronics stirs appearance, 2 of separating funnels, glass stick, 2 in beaker; Glue head dropper, each one in 100ml, 250ml graduated cylinder, tetraethoxy 500ml*3,25% ammoniacal liquor 500ml, absolute ethyl alcohol 500ml*2; The ultrasonic washing agent, ultra red ray drying appearance, whizzer, 6 of reagent pipes; Mortar, 2 of watch-glasss, foam beads, plastics poly-bag.
Drug parameter is set
Concrete steps
1, assembling three drop bottles, separating funnel, electronics stir appearance, and whether the position of opening power post debugging three drop bottles can balance.
2, with ethanol mixing tetraethoxy wiring solution-forming A, use ethanol mixing water and ammoniacal liquor wiring solution-forming B again,
Respectively solution A, B are poured in 2 separating funnels, reconcile the rotating speed that following speed of drop and electronics stir appearance.
3, shift SiO
2Deposition is carried out supersound washing and centrifugal repeatedly.Solvent is respectively absolute ethyl alcohol, zero(ppm) water, absolute ethyl alcohol during washing.
4, shift SiO
2, oven dry under the ultra red ray drying appearance.
Nanometer SiO
2The test of particle diameter
Claims (2)
1. SiO
2The preparation method comprises the following steps:
1) with volume ratio is ethanol and the tetraethoxy mixing wiring solution-forming A of 1:2;
2) with the volume ratio be the ammoniacal liquor wiring solution-forming B of the ratio of 1:2-2:1 again with ethanol and 13.4mol/L;
3) respectively solution A, B are poured in 2 separating funnels, reconcile the rotating speed that following speed of drop and electronics stir appearance;
4) shift SiO
2Deposition;
5) to the SiO of step 4)
2Carry out supersound washing and centrifugal repeatedly;
6) at infrared down baking step 5) SiO
2
2. the described method of claim 1 is characterized in that, solvent for use is selected from absolute ethyl alcohol, zero(ppm) water, absolute ethyl alcohol during the step 5) washing, or its mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101798452A CN102815712A (en) | 2012-06-01 | 2012-06-01 | Preparation method of nanometer SiO2 particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101798452A CN102815712A (en) | 2012-06-01 | 2012-06-01 | Preparation method of nanometer SiO2 particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102815712A true CN102815712A (en) | 2012-12-12 |
Family
ID=47300224
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101798452A Pending CN102815712A (en) | 2012-06-01 | 2012-06-01 | Preparation method of nanometer SiO2 particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102815712A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120585A (en) * | 2011-01-26 | 2011-07-13 | 深圳航天科技创新研究院 | Preparation method of SiO2 micro-nanosphere and micro-reaction system |
| CN102234118A (en) * | 2010-05-05 | 2011-11-09 | 张永昶 | Method for preparing nano silicon oxide by dispersion of surfactant |
-
2012
- 2012-06-01 CN CN2012101798452A patent/CN102815712A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234118A (en) * | 2010-05-05 | 2011-11-09 | 张永昶 | Method for preparing nano silicon oxide by dispersion of surfactant |
| CN102120585A (en) * | 2011-01-26 | 2011-07-13 | 深圳航天科技创新研究院 | Preparation method of SiO2 micro-nanosphere and micro-reaction system |
Non-Patent Citations (3)
| Title |
|---|
| 中国材料研究学会: "《纳米材料与技术应用进展-第四届全国纳米材料会议论文集》", 31 December 2005, 冶金工业出版社 * |
| 段涛等: "二氧化硅微球的制备与形成机理", 《中国粉体技术》 * |
| 聂鲁美等: "单分散二氧化硅微球的制备及反应机理", 《陶瓷学报》 * |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20121212 |