CN104326478A - Preparation method of nano silica microspheres - Google Patents
Preparation method of nano silica microspheres Download PDFInfo
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- CN104326478A CN104326478A CN201410015493.6A CN201410015493A CN104326478A CN 104326478 A CN104326478 A CN 104326478A CN 201410015493 A CN201410015493 A CN 201410015493A CN 104326478 A CN104326478 A CN 104326478A
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Abstract
The invention provides a preparation method of nano silica microspheres. Highly monodispersed nano silica microspheres can be obtained by using an organic silicate ester as a raw material and through the steps of hydrolyzation, centrifugal separation and vacuum drying in presence of a polymer dispersant and under an alkaline environment. The preparation process is simple and large-scale production of the nano silica microspheres can be realized.
Description
[technical field]
The present invention relates to a kind of preparation method of nano silica microsphere.
[background technology]
Monodisperse nano silicon dioxide microballoon has the characteristics such as good dispersity, uniform particle sizes, any surface finish, and the bridge that the silicone hydroxyl on its surface is suitable as modification makes its functionalization, thus it is made to become liquid, colloidal crystal, optical effect, medicine and solid packing field be widely used at support of the catalyst, single dispersing stream.Along with the development and application of new high-tech material, convenient, prepare high-purity, size tunable, monodisperse spherical nano silicon-dioxide economically and have very important practical significance.Since the synthesis monodisperse silicas such as nineteen sixty-eight Stober, nano silicon monodisperse system is one of monodisperse system of people's most study always.
At present, the synthetic method of silicon-dioxide can be divided into dry method and wet method two class, and wherein dry method comprises vapor phase process and arc process, and wet method has the precipitator method, sol-gel method, microemulsion method, hypergravity reaction method and hydrothermal synthesis method etc.
From the result of study of lot of documents report, the nano silicon purity of dry process is high, but equipment cost is high, complex process, and energy consumption is high.Current nano silica microsphere preparation all adopts wet processing.Wherein sol-gel method is prepared silicon-dioxide comparatively additive method cost is low, and can form metastable compound, have granularity controlled, and uniform particle degree is high, purity is high, and reaction process is easy to control, and side reaction is few, point equal advantage.From same raw material, change technological process and can obtain different products.
But when sol-gel method prepares nano silicon, affect the many factors of product cut size size, dispersiveness and surface quality, preparation process is unstable, is laboratory preparation substantially, is difficult to the market requirement meeting industrial large-scale production.
[summary of the invention]
The object of the present invention is to provide a kind of preparation method of nano silica microsphere, preparation method's process of this nano silica microsphere is easy, can realize the extensive preparation of nano silica microsphere.
For achieving the above object, the present invention adopts following technical proposals:
A preparation method for nano silica microsphere, comprises the steps:
By organic solvent with mix formation first mixing solutions in basic solution;
Macromolecule dispersing agent is added in described first mixing solutions, and constant temperature insulation, obtain the second mixing solutions;
Organosilicon acid esters is instilled, until obtain opalescent mixture in described second mixing solutions; And
Opalescent mixture described in centrifugation vacuum-drying obtains described silicon dioxide microsphere.
In certain embodiments, described organic solvent is at least one in ethanol, methyl alcohol, propyl alcohol.
In certain embodiments, described basic solution is ammonia soln.
In certain embodiments, described macromolecule dispersing agent is at least one in polyoxyethylene glycol, ethylene glycol.
In certain embodiments, described organosilicon acid esters is at least one in tetramethoxy-silicane, tetraethoxysilane.
In certain embodiments, the mass range of described organosilicon acid esters and described organic solvent is 10-60%.
In certain embodiments, the temperature of described constant temperature is 20-60 DEG C, and the time of described insulation is 0.5-1h.
In certain embodiments, the temperature of described drying is 50-80 DEG C, and time of drying is 5-8h.
In certain embodiments, the particle diameter of described silicon dioxide microsphere is between 100-900nm.
Adopt technique scheme, beneficial effect of the present invention is:
The preparation method of nano silica microsphere provided by the invention with organosilicon acid esters for raw material, under macromolecule dispersing agent and alkaline environment, height mono-dispersed nano silicon dioxide microsphere can be obtained through operations such as hydrolysis, centrifugation and vacuum-dryings, its preparation process is simple, can realize the extensive preparation of nano silica microsphere.
[accompanying drawing explanation]
Fig. 1 is the flow chart of steps of the preparation method of nano silica microsphere provided by the invention;
The SEM scintigram of the nano silica microsphere that Fig. 2 provides for the embodiment of the present invention;
The SEM scintigram of the nano silica microsphere that Fig. 3 provides for another embodiment of the present invention;
Fig. 4 is surface topography and the grain size distribution of Nano microsphere provided by the invention.
[embodiment]
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and the specific embodiments, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Refer to Fig. 1, the flow chart of steps of the preparation method 100 of the nano silica microsphere that Fig. 1 provides for the embodiment of the present invention, comprising:
Step S110: by organic solvent with mix formation first mixing solutions in basic solution;
Preferably, organic solvent is at least one in ethanol, methyl alcohol, propyl alcohol.
Preferably, basic solution is ammonia soln.Be appreciated that basic solution is ammonia soln just preferably a kind of embodiment, other basic solution in reality, can also be adopted.
Step S120: add macromolecule dispersing agent in the first mixing solutions, and constant temperature insulation, obtain the second mixing solutions;
Preferably, macromolecule dispersing agent is at least one in polyoxyethylene glycol, ethylene glycol.
Preferably, the temperature of constant temperature is 20-60 DEG C, and the time of insulation is 0.5-1h.
Step S130: instill organosilicon acid esters in the second mixing solutions, until obtain opalescent mixture;
Preferably, organosilicon acid esters is at least one in tetramethoxy-silicane, tetraethoxysilane.
Particularly, by certain feed rate by the instillation to above-mentioned second mixing solutions of organosilicon acid esters, wherein, organosilicon acid esters adds for ensureing by feed rate in 4-8h, add as continued reaction 2h after organic silicon ester, until obtain uniform and stable opalescent mixture.
Preferably, the mass range of organosilicon acid esters and organic solvent is 10-60%.Being appreciated that by changing proportioning between reaction product (organosilicon acid esters, macromolecule dispersing agent, ammoniacal liquor, organic solvent etc.) or rate of addition, preparing that particle diameter is adjustable, the nano-silicon dioxide particle of uniform particle diameter.
Step S140: centrifugation opalescent mixture vacuum-drying obtains silicon dioxide microsphere.
Preferably, dry temperature is 50-80 DEG C, and time of drying is 5-8h.
Preferably, the particle diameter of silicon dioxide microsphere is between 100-900nm.
The preparation method of nano silica microsphere provided by the invention with organosilicon acid esters for raw material, under macromolecule dispersing agent and alkaline environment, height mono-dispersed nano silicon dioxide microsphere can be obtained through operations such as hydrolysis, centrifugation and vacuum-dryings, its preparation process is simple, can realize the extensive preparation of nano silica microsphere.
Set forth the present invention further by the following examples, these embodiments are only presented for purposes of illustration, do not limit the scope of the invention.Except the actual conditions indicated, the test method in embodiment all conveniently condition is carried out.
Embodiment 1
Quantitative 1.5L ammoniacal liquor and 16L ethanol add in 30L glass reaction still and are uniformly mixed formation first mixing solutions; Take 5g polyoxyethylene glycol, join in above-mentioned first mixing, in 20 DEG C of insulation 1h, and stirring and dissolving forms the second mixing solutions; Drip 1.8L tetramethoxy-silicane at above-mentioned second mixing solutions, within about 5 hours, add, until reaction mixture is creamy white; By above-mentioned emulsion centrifugation after completion of the reaction and vacuum-drying, the silicon dioxide nanosphere of particle diameter 300-400nm can be obtained.
Referring to Fig. 2, is the nano silica microsphere prepared by the embodiment of the present invention 1, and as can be seen from Figure 2, good sphericity, median size homogeneity is good, and deviation is less than 10%, and microsphere surface is bright and clean, zero defect.
Embodiment 2
In the there-necked flask (250mL) that agitator, syringe, thermometer are housed, first add the mixing solutions 112mL of dehydrated alcohol and ammoniacal liquor, be uniformly mixed formation first mixing solutions; Add ethylene glycol dispersion agent again, react 6 hours in 45 DEG C of waters bath with thermostatic control, obtain the second mixing solutions; Tetraethoxysilane is instilled, until obtain opalescent mixture in described second mixing solutions; Be separated through centrifuge, vacuum-drying obtains the SiO2 white powder of particle diameter about 500nm.
Referring to Fig. 3, is the nano silica microsphere prepared by the embodiment of the present invention 2, and as can be seen from Figure 2, good sphericity, microsphere surface is bright and clean, zero defect.
Refer to Fig. 4, the surface topography of the Nano microsphere adopting aforesaid method to prepare for the present invention and grain size distribution, as can be seen from Figure 4, by changing proportioning between reaction product (organosilicon acid esters, macromolecule dispersing agent, ammoniacal liquor, organic solvent etc.) or rate of addition, prepare that particle diameter is adjustable between 100-900nm, the nano-silicon dioxide particle of uniform particle diameter.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be do not depart from technical solution of the present invention content, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (9)
1. a preparation method for nano silica microsphere, is characterized in that, comprises the steps:
By organic solvent with mix formation first mixing solutions in basic solution;
Macromolecule dispersing agent is added in described first mixing solutions, and constant temperature insulation, obtain the second mixing solutions;
Organosilicon acid esters is instilled, until obtain opalescent mixture in described second mixing solutions; And
Opalescent mixture described in centrifugation vacuum-drying obtains described silicon dioxide microsphere.
2. the preparation method of nano silica microsphere according to claim 1, is characterized in that, described organic solvent is at least one in ethanol, methyl alcohol, propyl alcohol.
3. the preparation method of nano silica microsphere according to claim 1, is characterized in that, described basic solution is ammonia soln.
4. the preparation method of nano silica microsphere according to claim 1, is characterized in that, described macromolecule dispersing agent is at least one in polyoxyethylene glycol, ethylene glycol.
5. the preparation method of nano silica microsphere according to claim 1, is characterized in that, described organosilicon acid esters is at least one in tetramethoxy-silicane, tetraethoxysilane.
6. the preparation method of nano silica microsphere according to claim 1, is characterized in that, the mass range of described organosilicon acid esters and described organic solvent is 10-60%.
7. the preparation method of nano silica microsphere according to claim 1, is characterized in that, the temperature of described constant temperature is 20-60 DEG C, and the time of described insulation is 0.5-1h.
8. the preparation method of nano silica microsphere according to claim 1, is characterized in that, the temperature of described drying is 50-80 DEG C, and time of drying is 5-8h.
9. the preparation method of nano silica microsphere according to claim 1, is characterized in that, the particle diameter of described silicon dioxide microsphere is between 100-900nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104860320A (en) * | 2015-05-06 | 2015-08-26 | 杭州云界生物科技有限公司 | Method for preparing modified nanosilicon dioxide |
| CN107970934A (en) * | 2016-10-21 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of furfural hydrogenation 2- methylfurans method for preparing catalyst and catalyst |
| CN108341414A (en) * | 2017-01-22 | 2018-07-31 | 华东师范大学 | A kind of uniform silicon dioxide microsphere and its preparation method and application |
| CN109336120A (en) * | 2018-10-12 | 2019-02-15 | 安庆北化大科技园有限公司 | Nano-meter SiO_2 with surface migration2The preparation method and Nano-meter SiO_2 of microballoon2 |
| CN110683552A (en) * | 2019-10-17 | 2020-01-14 | 蚌埠市万科硅材料科技有限公司 | Preparation method of nano silicon dioxide microspheres with particle size of 10-20nm |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860320A (en) * | 2015-05-06 | 2015-08-26 | 杭州云界生物科技有限公司 | Method for preparing modified nanosilicon dioxide |
| CN104860320B (en) * | 2015-05-06 | 2017-07-04 | 杭州云界生物科技有限公司 | A kind of preparation method of modified manometer silicon dioxide |
| CN107970934A (en) * | 2016-10-21 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of furfural hydrogenation 2- methylfurans method for preparing catalyst and catalyst |
| CN108341414A (en) * | 2017-01-22 | 2018-07-31 | 华东师范大学 | A kind of uniform silicon dioxide microsphere and its preparation method and application |
| CN108341414B (en) * | 2017-01-22 | 2020-08-04 | 华东师范大学 | Uniform silicon dioxide microsphere and preparation method and application thereof |
| CN109336120A (en) * | 2018-10-12 | 2019-02-15 | 安庆北化大科技园有限公司 | Nano-meter SiO_2 with surface migration2The preparation method and Nano-meter SiO_2 of microballoon2 |
| CN109336120B (en) * | 2018-10-12 | 2022-09-09 | 安庆北化大科技园有限公司 | Nano SiO with surface migration 2 Preparation method of microsphere and nano SiO 2 |
| CN110683552A (en) * | 2019-10-17 | 2020-01-14 | 蚌埠市万科硅材料科技有限公司 | Preparation method of nano silicon dioxide microspheres with particle size of 10-20nm |
| CN110683552B (en) * | 2019-10-17 | 2022-05-03 | 蚌埠市万科硅材料科技有限公司 | Preparation method of nano silicon dioxide microspheres with particle size of 10-20nm |
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