CN108439420A - The preparation method of monodisperse porous silica ball material - Google Patents
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- CN108439420A CN108439420A CN201810280786.5A CN201810280786A CN108439420A CN 108439420 A CN108439420 A CN 108439420A CN 201810280786 A CN201810280786 A CN 201810280786A CN 108439420 A CN108439420 A CN 108439420A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/14—Pore volume
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Abstract
The present invention proposes a kind of preparation method of monodisperse porous silica ball material, including, surfactant and catalyst are dissolved into water by (1), high-speed stirred to clear solution；Silicon source is dissolved in organic solvent, organic solution is obtained；Organic solution is added in clear solution, grease mixed phase system is formed；(2) grease mixed phase system is reacted in 40 80 DEG C of temperature；Obtain dispersed nano ball；(3) surfactant therein is removed, monodisperse porous silica ball material is obtained.Present invention employs the miscible reaction systems of water-oil phase, and due to the reaming effect of organic phase, the aperture of gained inorganic silicon dioxide ball reaches as high as 70nm.Meanwhile the aperture of inorganic silicon dioxide ball can be regulated and controled, realize its aperture freely regulating and controlling between 15~70nm.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, a kind of monodisperse porous silica ball material is particularly related to
Preparation method.
Background technology
Porous silica spheres have porosity height, large specific surface area, chemical property stable, low cost, hydrophily well,
The features such as nontoxic, therefore be used widely in fields such as absorption, catalysis, filtering, biological medicines, since pore structure is its application
Key, therefore the research in relation to regulation and control porous silica aperture more and more is paid attention to, larger in relation to preparing at present
The research of aperture earth silicon material has very much, but in terms of mostly concentrating on the preparation of block materials, therefore can not be applied to
Microscopic fields.Due to being commercialized the limitation of surfactant, it is generally difficult to prepare the silica ball material of larger aperture, make
Standby monodisperse porous silica spheres of the aperture more than 20nm are still prodigious technological challenge.
Invention content
The present invention proposes a kind of preparation method of monodisperse porous silica ball material, solves the prior art porous two
The problem that the aperture of silicon oxide ball material is smaller, aperture adjustable extent is small.
The technical proposal of the invention is realized in this way：
A kind of preparation method of monodisperse porous silica ball material, including：
(1) surfactant and suitable catalyst are dissolved into water, high-speed stirred to clear solution；The clear solution
A concentration of 1.0-22wt% of middle surfactant；
Silicon source is dissolved in organic solvent, organic solution is obtained；The wherein a concentration of 3-50wt% of silicon source；
The organic solution is added in the clear solution, grease mixed phase system is formed；
Surfactant and the mass ratio of silicon source are 0.25-8.0；
(2) the grease mixed phase system is reacted in 40-80 DEG C of temperature；Obtain dispersed nano ball；
(3) in air atmosphere by above-mentioned monodisperse aperture ball, 400-800 DEG C of temperature is risen to from room temperature, and keeps 1-10h
Surfactant therein is removed, monodisperse porous silica ball material is obtained；
Or
Nanosphere obtained by the grease mixed phase system is placed in hydrochloric acid-ethanol solution, is stirred at room temperature, is removed therein
Surfactant is to get to monodisperse porous silica ball material.
As a preferred technical solution, the surfactant in quaternary cationic surfactant one
Kind is several；The quaternary cationic surfactant；Including but not limited to hexadecyltrimethylammonium chloride, hexadecane
Base trimethylammonium bromide, octadecyltrimethylammonium chloride and Cetyltrimethylammonium bromide etc..
The catalyst is selected from ammonium hydroxide, fatty amine, hydramine, aromatic amine, amide, fragrance as a preferred technical solution,
One or more of amine, aliphatic cyclic amine；Including but not limited to octylame, lauryl amine, triethanolamine, diethanol amine.
A concentration of 0.01-1.0wt% of catalyst described in clear solution as a preferred technical solution,.
The mixing speed of the high-speed stirred is 150-800 revs/min as a preferred technical solution, and time control exists
0.25-5h。
As a preferred technical solution, the silicon source in sodium metasilicate, aerosil, ethyl orthosilicate one
Kind is several.
The organic solvent is selected from dioxane, hexamethylene, n-hexane, decahydronaphthalene, alkene as a preferred technical solution,
One or more of hydrocarbon.
The time reacted in the step (2) as a preferred technical solution, is 2-24h；Heating in the step (3)
Rate is 1 DEG C/min.
The duct of the monodisperse porous silica ball material is center divergence form as a preferred technical solution,
's.
Monodisperse porous silica ball material obtained above, is by the skeleton of the tightly packed formation of silica.It is logical
The parameter of modulation organic phase is crossed, diameter is 60~500nm, and specific surface area is 600~1600m2/ g, aperture be 15~
0.61~2.8cm of 70nm, Kong Rongwei3/g。
Advantageous effect
(1) present invention employs two miscible reaction systems of oil-water, due to the reaming effect of organic phase, gained inorganic two
Before the aperture ratio of silicon oxide ball (≤18nm) it is much higher, reach as high as 70nm.Meanwhile passing through the parameter of modulation organic phase
(such as the change of organic solvent or concentration etc. of silicon source) can regulate and control the aperture of inorganic silicon dioxide ball, realize its hole
Diameter freely regulating and controlling between 15~70nm.
(2) in preparation method, only simply organic phase and aqueous phase system are blended for miscible reaction system, are not necessarily to
Consider two-phase system layering interfaces holding, therefore it is easy to operate, repetitive rate is high, can be adapted for large-scale industrial production.
Description of the drawings
It, below will be to embodiment in order to illustrate more clearly of embodiment of the present invention or technical solution in the prior art
Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only
It is some embodiments of the present invention, for those of ordinary skill in the art, in the premise of not making the creative labor property
Under, other drawings may also be obtained based on these drawings.
Fig. 1 is monodisperse porous silica spheres material characteristics scanning electron microscope (SEM) figure one of embodiment 1.
Fig. 2 is monodisperse porous silica spheres material characteristics scanning electron microscope (TEM) figure two of embodiment 1.
Fig. 3 is monodisperse porous silica spheres material characteristics transmission electron microscope (TEM) figure of embodiment 1.
Fig. 4 is monodisperse porous silica spheres material characteristics nitrogen adsorption-desorption isotherm of embodiment 1.
Fig. 5 is the monodisperse porous silica spheres material characteristics pore size distribution curve of embodiment 1.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
Substance involved in following embodiments is commercially available.
Embodiment 1
A kind of preparation method of monodisperse porous silica ball material, including：
(1) 2.0g hexadecyltrimethylammonium chlorides and 0.08mL triethanolamines are successively dissolved into 20mL deionized waters
In, high-speed stirred is formed uniformly the solution of water white transparency；By the solution of the water white transparency to entering in reactor；Above-mentioned high-speed stirred
Mixing speed can be selected in 150-800 revs/min, time control is in 0.25-5h；The blender wherein used can
To be turbine agitator, dasher, magnetic stirring apparatus, magnetic force heating stirrer, hinging type blender or mechanical agitation
Device；
Ethyl orthosilicate is dissolved in hexamethylene, 8mL organic solutions are obtained；Wherein ethyl orthosilicate is a concentration of
10wt%；Organic solution is added in clear solution, grease mixed phase system is formed,；
(2) the grease mixed phase system in step (1) is reacted into 8h in the oil bath of temperature 60 C；After reaction, it centrifuges
Precipitation is collected, is washed respectively 3 times with water and ethyl alcohol, obtains dispersed nano ball；
(3) above-mentioned monodisperse aperture ball is placed in Muffle furnace, in air atmosphere, temperature is risen to from room temperature with 1 DEG C/min
550 DEG C of degree, and 3h is kept to remove surfactant therein, obtain monodisperse porous silica ball material.
The above-mentioned duct that monodisperse porous silica ball material is made is center divergence form.
Embodiment 2
(1) 0.2g cetyl trimethylammonium bromides and 0.08mL octylames are successively dissolved into 20mL deionized waters, it is high
Speed stirs evenly the solution to form water white transparency；By the solution of the water white transparency to entering in reactor；Above-mentioned high-speed stirred is stirred
Mixing speed can select in 150-800 revs/min, and time control is in 0.25-5h；The blender wherein used can be
Turbine agitator, dasher, magnetic stirring apparatus, magnetic force heating stirrer, hinging type blender or mechanical agitator；
Ethyl orthosilicate is dissolved in dioxane, 10mL organic solutions are obtained；Wherein ethyl orthosilicate is a concentration of
3wt%；Organic solution is added in clear solution, grease mixed phase system is formed；
(2) the grease mixed phase system in step (1) is reacted for 24 hours in the oil bath of 40 DEG C of temperature；After reaction, it centrifuges
Precipitation is collected, is washed respectively 3 times with water and ethyl alcohol, obtains dispersed nano ball；
(3) above-mentioned monodisperse aperture ball is placed in hydrochloric acid-ethanol solution, is stirred at room temperature, removed surface therein and live
Property agent is to get to monodisperse porous silica ball material.
The above-mentioned duct that monodisperse porous silica ball material is made is center divergence form.
Embodiment 3
(1) 4.4g Cetyltrimethylammonium bromides and 0.15mL lauryl amines are successively dissolved into 20mL deionized waters,
High-speed stirred is formed uniformly the solution of water white transparency；By the solution of the water white transparency to entering in reactor；Above-mentioned high-speed stirred
Mixing speed can select in 150-800 revs/min, and time control is in 0.25-5h；The blender wherein used can be with
It is turbine agitator, dasher, magnetic stirring apparatus, magnetic force heating stirrer, hinging type blender or mechanical agitation
Device；
Aerosil is dissolved in octadecylene, 10mL organic solutions are obtained；Wherein aerosil is a concentration of
50wt%；Organic solution is added in clear solution, grease mixed phase system is formed；
(2) the grease mixed phase system in step (1) is reacted into 2h in the oil bath of 80 DEG C of temperature；After reaction, it centrifuges
Precipitation is collected, is washed respectively repeatedly with water and ethyl alcohol, obtains dispersed nano ball；
(3) above-mentioned monodisperse aperture ball is placed in hydrochloric acid-ethanol solution, is stirred at room temperature, removed surface therein and live
Property agent is to get to monodisperse porous silica ball material.
The above-mentioned duct that monodisperse porous silica ball material is made is center divergence form.
Embodiment 4
(1) 1.0g octadecyltrimethylammonium chloride and 0.06mL diethanol amine are successively dissolved into 20mL deionized waters
In, high-speed stirred is formed uniformly the solution of water white transparency；By the solution of the water white transparency to entering in reactor；Above-mentioned high-speed stirred
Mixing speed can be selected in 150-800 revs/min, time control is in 0.25-5h；The blender wherein used can
To be turbine agitator, dasher, magnetic stirring apparatus, magnetic force heating stirrer, hinging type blender or mechanical agitation
Device；
Sodium metasilicate is dissolved in n-hexane, 8mL organic solutions are obtained；The wherein a concentration of 20wt% of sodium metasilicate；It will be organic
Solution is added in clear solution, forms grease mixed phase system,；
(2) the grease mixed phase system in step (1) is reacted into 5h in the oil bath of temperature 60 C；After reaction, it centrifuges
Precipitation is collected, is washed respectively 2 times with water and ethyl alcohol, obtains dispersed nano ball；
(3) above-mentioned monodisperse aperture ball is placed in Muffle furnace, in air atmosphere, temperature is risen to from room temperature with 1 DEG C/min
600 DEG C of degree, and 3h is kept to remove surfactant therein, obtain monodisperse porous silica ball material.
The above-mentioned duct that monodisperse porous silica ball material is made is center divergence form.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of preparation method of monodisperse porous silica ball material, which is characterized in that including：
(1) surfactant and catalyst are dissolved into water, high-speed stirred to clear solution；Surface-active in the clear solution
A concentration of 1.0-22wt% of agent；
Silicon source is dissolved in organic solvent, organic solution is obtained；The wherein a concentration of 3-50wt% of silicon source；
The organic solution is added in the clear solution, grease mixed phase system is formed；
Surfactant and the mass ratio of silicon source are 0.25-8.0；
(2) the grease mixed phase system is reacted in 40-80 DEG C of temperature；Obtain dispersed nano ball；
(3) in air atmosphere by above-mentioned dispersed nano ball, 400-800 DEG C of temperature is risen to from room temperature, and 1-10h is kept to remove
Surfactant therein obtains monodisperse porous silica ball material；
Or
Nanosphere obtained by the grease mixed phase system is placed in hydrochloric acid-ethanol solution, stirs at room temperature, removes surface therein
Activating agent is to get to monodisperse porous silica ball material.
2. a kind of preparation method of monodisperse porous silica ball material according to claim 1, which is characterized in that institute
The surfactant stated is selected from one or more of quaternary cationic surfactant；Including but not limited to cetyl
Trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyltrimethylammonium chloride, Cetyltrimethylammonium bromide.
3. a kind of preparation method of monodisperse porous silica ball material according to claim 1, which is characterized in that institute
The catalyst stated is selected from one or more of ammonium hydroxide, fatty amine, hydramine, aromatic amine, amide, aromatic amine, aliphatic cyclic amine；Including but
It is not limited to octylame, lauryl amine, triethanolamine, diethanol amine.
4. a kind of preparation method of monodisperse porous silica ball material according to claim 1 or 3, feature exist
In a concentration of 0.01-1.0wt% of catalyst described in clear solution.
5. a kind of preparation method of monodisperse porous silica ball material according to claim 1, which is characterized in that institute
The mixing speed for stating high-speed stirred is 150-800 revs/min, and time control is in 0.25-5h.
6. a kind of preparation method of monodisperse porous silica ball material according to claim 1, which is characterized in that institute
The silicon source stated is selected from one or more of sodium metasilicate, aerosil, ethyl orthosilicate.
7. a kind of preparation method of monodisperse porous silica ball material according to claim 1, which is characterized in that institute
The organic solvent stated is selected from one or more of dioxane, hexamethylene, n-hexane, decahydronaphthalene, alkene.
8. a kind of preparation method of monodisperse porous silica ball material according to claim 1, which is characterized in that institute
It is 2-24h to state the time reacted in step (2)；Heating rate in the step (3) is 1 DEG C/min.
9. a kind of preparation method of monodisperse porous silica ball material according to claim 1, which is characterized in that institute
The duct for the monodisperse porous silica ball material stated is center divergence form.
10. a kind of preparation method of monodisperse porous silica ball material according to claim 1, which is characterized in that
Monodisperse porous silica ball material obtained is by the skeleton of the tightly packed formation of silica, diameter 60
~500nm, specific surface area are 600~1600m2/ g, aperture are 15~70nm, 0.61~2.8cm of Kong Rongwei3/g。
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| CN201810280786.5A CN108439420B (en) | 2018-04-02 | 2018-04-02 | Preparation method of monodisperse porous silicon dioxide sphere material |
| CN201911105579.7A CN110627075A (en) | 2018-04-02 | 2018-04-02 | Preparation method of monodisperse porous silicon dioxide sphere material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109368648A (en) * | 2018-12-14 | 2019-02-22 | 深圳元颉新材料科技有限公司 | The preparation method of monodisperse mesoporous silica nanometer sheet material |
| CN110371992A (en) * | 2019-07-19 | 2019-10-25 | 国家纳米科学中心 | It is a kind of regulate and control microemulsion reaction methods monodisperse silica sphere particle method and products thereof and purposes |
| CN110963495A (en) * | 2019-12-26 | 2020-04-07 | 沃克福德环境科技(深圳)有限责任公司 | Preparation method of silicon dioxide nano material with various loaded mesopores |
| WO2020078029A1 (en) * | 2018-10-19 | 2020-04-23 | 广州市飞雪材料科技有限公司 | High-dispersion silica and preparation method therefor |
| CN115849440A (en) * | 2023-01-29 | 2023-03-28 | 宁波卿甬新材料科技有限公司 | Preparation method of porous zirconia |
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| CN112210841A (en) * | 2020-08-24 | 2021-01-12 | 百事基材料（青岛）股份有限公司 | Method for nest loading of plant active molecules by porous silicon dioxide slow-release molecules |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020078029A1 (en) * | 2018-10-19 | 2020-04-23 | 广州市飞雪材料科技有限公司 | High-dispersion silica and preparation method therefor |
| CN109368648A (en) * | 2018-12-14 | 2019-02-22 | 深圳元颉新材料科技有限公司 | The preparation method of monodisperse mesoporous silica nanometer sheet material |
| CN110371992A (en) * | 2019-07-19 | 2019-10-25 | 国家纳米科学中心 | It is a kind of regulate and control microemulsion reaction methods monodisperse silica sphere particle method and products thereof and purposes |
| CN110963495A (en) * | 2019-12-26 | 2020-04-07 | 沃克福德环境科技(深圳)有限责任公司 | Preparation method of silicon dioxide nano material with various loaded mesopores |
| CN115849440A (en) * | 2023-01-29 | 2023-03-28 | 宁波卿甬新材料科技有限公司 | Preparation method of porous zirconia |
| CN115849440B (en) * | 2023-01-29 | 2023-06-23 | 宁波卿甬新材料科技有限公司 | Preparation method of porous zirconia |
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| Publication number | Publication date |
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| CN110627075A (en) | 2019-12-31 |
| CN108439420B (en) | 2020-09-01 |
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