CN107285325A - A kind of preparation method of the monodisperse silica nanosphere of novel green - Google Patents

A kind of preparation method of the monodisperse silica nanosphere of novel green Download PDF

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Publication number
CN107285325A
CN107285325A CN201710666272.9A CN201710666272A CN107285325A CN 107285325 A CN107285325 A CN 107285325A CN 201710666272 A CN201710666272 A CN 201710666272A CN 107285325 A CN107285325 A CN 107285325A
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nanosphere
surfactant
microemulsion
ethanol
dichloromethane
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CN201710666272.9A
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柴金岭
孙斌
潘金
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Shandong Normal University
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Shandong Normal University
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Priority to CN201710666272.9A priority Critical patent/CN107285325A/en
Priority to CN201710953405.0A priority patent/CN107879348B/en
Publication of CN107285325A publication Critical patent/CN107285325A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention provides a kind of preparation method of the monodisperse silica nanosphere of novel green, including：Prepare O/W types water/ethanol/dichloromethane surfactant-free microemulsion；By tetraethyl orthosilicate (TEOS) in ball-type " oily core " of the ultrasound with the O/W type surfactant-free microemulsions being completely dissolved under stirring action prepared by the first step, then under ammonia-catalyzed, tetraethyl orthosilicate realizes hydrolytie polycondensation, is centrifuged after completion of the reaction.Solid constituent is washed with polar solvent repeatedly produces single dispersing SiO2Nanosphere, remaining liq component carries out distillation and collects ethanol and dichloromethane.This method is simple to operate, cost is low, environment-friendly, system repeats utilization, efficiency high.The SiO of preparation2Nanosphere yardstick is uniform, is worth with universality and large-scale production.Step is simple and convenient to operate, practical.

Description

A kind of preparation method of the monodisperse silica nanosphere of novel green
Technical field
The invention belongs to field of nanometer material technology, the system of the monodisperse silica nanosphere of more particularly to a kind of novel green Preparation Method.
Background technology
Monodispersed SiO2Nanosphere, because its specific surface area is big, good dispersion, while having good optics and power again Characteristic is learned, there is important application value in fields such as biomedicine, catalysis, functional material, high-performance ceramic, coating.Method is current preparation SiO2One of conventional method of nanosphere, this method has dioxy simple to operate, prepared The advantages of SiClx nanosphere clean surface.The method does not contain preparation template, therefore prepare dioxy merely with the interaction between solvent The controllability and repeatability of SiClx nanosphere are poor, it is difficult to obtain high-quality SiO2Nanosphere.Another preparation SiO2Nanosphere Conventional method is microemulsion method, SiO prepared by this method2Nanosphere, monodispersity is good, size adjustable, but micro- constructing , it is necessary to consume substantial amounts of surfactant and cosurfactant during emulsion template, both components remove the boundary for entering microemulsion Outside facial mask, part is also soluble in the aqueous phase and oil phase, is not easily recycled utilization, and environment is polluted, and loaded by material surface Surfactant is difficult to washing and removes and influence its purity etc., and these problems seriously constrain microemulsion method and preparing silica Application in terms of nano particle.
The content of the invention
In view of the above-mentioned problems, preparing SiO using O/W type surfactant-frees microemulsion for template we have proposed one kind2 The method of nanosphere.Surfactant-free microemulsion component is simple, only by water, oil and " two solvophilics " composition.It is this new Surfactant-free microemulsion system does not contain surfactant, but with the microstructure and property similar to microemulsion, It can overcome during Preparing Nano-Materials in Microemulsions by the shortcoming brought containing exhibiting high surface activating agent, not only can significantly save About cost, and the nano material purity prepared is higher.
In order to obtain, pattern is homogeneous, the single dispersing SiO of uniform particle sizes2Nanosphere, the application is in different surfactant-frees SiO has been carried out in microemulsion system2The preparation of nanosphere.System research SiO2Nanosphere is in surfactant-free Emulsions Shaping rule in system, finds after being screened through many experiments：Using O/W types ethanol/dichloromethane/water surfactant-free micro emulsion Liquid system has pattern homogeneous as template, the silica nanosphere of preparation, the advantage of uniform particle sizes.And in this system, Ethanol is as " solvent pairs ", and dichloromethane is as oil phase, and both solvents are not only with low cost, and because its boiling point is relatively low, Can be in SiO2After the completion of prepared by nanosphere, it is recyclable by the simple way of distillation, reaches the purpose recycled.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of preparation method of the monodisperse silica nanosphere of novel green, including：
Prepare O/W types water/ethanol/dichloromethane surfactant-free microemulsion；
By tetraethyl orthosilicate (TEOS) under ultrasound or stirring action, it is completely dissolved in prepared O/W types and is lived without surface In the ball-type " oily core " of property agent microemulsion, then under ammonia-catalyzed, tetraethyl orthosilicate realizes hydrolytie polycondensation, leads to after completion of the reaction Cross centrifugation and collect solid constituent, polar solvent washs 3 times to obtain SiO2Nanosphere, liquid component is distilled, and collects ethanol With dichloromethane component.
It is preferred that, in the surfactant-free microemulsion, mass fraction of the fixed dichloromethane in system is 20%, Water is respectively 4-9.5 with ethanol mass ratio：6-0.5.
It is preferred that, the volume ratio of the tetraethyl orthosilicate and ammoniacal liquor (25 ﹪ wt) is 1.3：3.
It is preferred that, it is described tetraethyl orthosilicate is dissolved in above-mentioned surfactant-free microemulsion concretely comprise the following steps：Will Quantitative tetraethyl orthosilicate (TEOS) is added slowly with stirring in the surfactant-free microemulsion, ultrasound or machinery Stir certain time.
It is preferred that, the ammoniacal liquor is slowly added into the O/W dissolved with tetraethyl orthosilicate without surface under ice-water bath, stirring condition In activating agent microemulsion system.
It is preferred that, the condition of the hydrolytie polycondensation is：1-24h is reacted in being stood under 25-35 DEG C of water-bath.
It is preferred that, the separation is concretely comprised the following steps：System after completion of the reaction is carried out solid constituent, pole is collected by centrifugation Property solvent wash 3 times, liquid component is distilled, collection ethanol, dichloromethane component.
It is preferred that, the polar solvent is ethanol, methanol, Huo Zheshui.
Present invention also offers monodisperse silica nanosphere prepared by any above-mentioned method.
It is preferred that, the particle diameter of the silica nanosphere is 275~785mm.
Biomedical material, catalysis material are being prepared present invention also offers any above-mentioned monodisperse silica nanosphere Application in material, functional material, high-performance ceramic or coating.
" green " in the present invention refers to：A kind of green synthesis method.
Beneficial effects of the present invention
(1) SiO is prepared compared to traditional w/o type microemulsion method2Nanosphere, the present invention is using O/W types without surface-active Agent microemulsion is template to prepare SiO2Nanosphere, significantly reduces the consumption of oil phase, has saved cost.Utilize O/W types water/second Alcohol/dichloromethane surfactant-free microemulsion is that template prepares SiO2Nanosphere, this method is simple to operate, cost is low, environment The silica nanosphere pattern that friendly, system repeats utilizations, efficiency high, prepare is homogeneous, uniform particle sizes, with universality with Large-scale production is worth.
(2) silica nanosphere prepared by the present invention, pattern is good, and yardstick is homogeneous, and particle diameter adjustable extent is big, and surface is clean Only, subsequent treatment is simple.Surfactant-free microemulsion system component is simple, and recoverable does not contain surfactant energy It is enough a large amount of cost-effective.
(3) preparation method of the present invention is simple, preparation efficiency is high, practical, it is easy to promote.
Brief description of the drawings
The Figure of description for constituting the part of the present invention is used for providing further understanding of the present application, and the application's shows Meaning property embodiment and its illustrate be used for explain the application, do not constitute the improper restriction to the application.
Fig. 1 is to change the silica nanosphere that the mass ratio of water and ethanol is obtained in the timing of dichloromethane content one TEM schemes；
Fig. 2 is when water alcohol ratio is 0.5:When 9.5, the EDS figures of the silica nanosphere of preparation；
Fig. 3 is the TEM figures of silica nanosphere prepared by comparative example 1.
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field The identical meanings of understanding.
A kind of utilization surfactant-free microemulsion is the method that template prepares silica nanosphere, including step as follows Suddenly：
(1) preparation of O/W types surfactant-free microemulsion template：Under agitation, by appropriate water, ethanol and Dichloromethane is well mixed, and mixing persistently stirs certain time after finishing.
(2) by quantitative tetraethyl orthosilicate (TEOS), be added slowly with stirring O/W types prepared by step (1) without In surfactant microemulsion system, certain time is persistently stirred, tetraethyl orthosilicate is completely dissolved in O/W surfactant-frees micro- Among emulsion " oily core ".
(3) under ice-water bath stirring condition, quantitative ammoniacal liquor (25 ﹪ wt) is slowly added into the system obtained by step (2) In, addition continues ice-water bath after finishing and stirred several minutes, then moves into 25 DEG C of water-baths and stands reaction 1-24 hours.
(4) it is centrifuged, gained white solid, is washed with water 3 times, remaining liq is distilled after completion of the reaction, Reclaim ethanol and dichloromethane.
The present invention principle be：First with water, ethanol and dichloromethane prepare O/W surfactant-free microemulsion moulds Reactant tetraethyl orthosilicate, is then added in system by plate, and tetraethyl orthosilicate is completely dissolved in by ultrasound or mechanical agitation Among " the oily core " of O/W surfactant-free microemulsion systems.Ammonia spirit is slowly added under the conditions of ice-water bath, it is ensured that ammoniacal liquor It is soluble in the aqueous phase, reaction unit is moved into 25 DEG C of water-baths, reaction is proceeded by.
The reaction mechanism mechanism of reaction of silica nanosphere prepared by the method is as follows：
Hydrolysis：
Polycondensation：
After tetraethyl orthosilicate (TEOS) is added to O/W without in the microemulsion of surface, it is completely into O/W types without surface-active Among " the oily core " of agent microemulsion, because the interfacial film of O/W drops is made up of a large amount of ethanol molecules and hydrone, hydrone can It is hydrolyzed into " oily core " with TEOS and condensation reaction, by monohydroxy silicate monomer to polyhydroxy esters of silicon acis until being formed Nucleus.Finally in " the oily core " of O/W surfactant-free microemulsion systems, spherical silicon dioxide nano particle is formed.
Embodiment 1：
(1) bis- ultra-pure waters of 4g are mixed with 76g ethanol, 20g dichloromethane is added under agitation, after addition is finished Persistently stir 10min.
(2) 1.3ml tetraethyl orthosilicates are slowly added into the O/W types obtained by step (1) under stirring to live without surface Property agent microemulsion system in, ultrasound 10min successively after addition is finished, stirring 20min.
(3) the O/W type surfactant-frees microemulsion system containing tetraethyl orthosilicate obtained by step (2) is moved into frozen water Bath, under agitation, 3ml ammoniacal liquor (25wt ﹪) is slowly added thereto, and is persistently stirred reaction unit immigration 25 after 10min DEG C water-bath stands reaction 6h.
(4) after reaction terminates, by being centrifugally separating to obtain white solid, white solid is washed 3 times and obtains SiO2Nanometer Ball.Remaining liq component is distilled, and collects ethanol and dichloromethane component.By SiO2Nanosphere is scattered in ethanol again, Its TEM is shown in that figure (1) d, EDS figure is shown in figure (2).
Embodiment 2：
(1) bis- ultra-pure waters of 4g are mixed with 36g ethanol, 10g dichloromethane is added under agitation, after addition is finished Persistently stir 10min.
(2) 1.3ml tetraethyl orthosilicates are slowly added into the O/W types obtained by step (1) under stirring to live without surface Property agent microemulsion system in, ultrasound 10min successively after addition is finished, stirring 20min.
(3) the O/W type surfactant-frees microemulsion system containing tetraethyl orthosilicate obtained by step (2) is moved into frozen water Bath, under agitation, 3ml ammoniacal liquor (25wt ﹪) is slowly added thereto, and is persistently stirred reaction unit immigration 25 after 10min DEG C water-bath stands reaction 6h.
(4) after reaction terminates, by being centrifugally separating to obtain white solid, white solid is washed 3 times and obtains SiO2Nanometer Ball.Remaining liq component is distilled, ethanol and dichloromethane component is collected.By SiO2Nanosphere is scattered in ethanol again In, its TEM is as shown in figure (1) c.
Embodiment 3：
(1) bis- ultra-pure waters of 4g are mixed with 16g ethanol, 5g dichloromethane is added under agitation, after addition is finished Persistently stir 10min.
(2) 1.3ml tetraethyl orthosilicates are slowly added into the O/W types obtained by step (1) under stirring to live without surface Property agent microemulsion system in, ultrasound 10min successively after addition is finished, stirring 20min.
(3) the O/W type surfactant-frees microemulsion system containing tetraethyl orthosilicate obtained by step (2) is moved into frozen water Bath, under agitation, 3ml ammoniacal liquor (25wt ﹪) is slowly added thereto, and is persistently stirred reaction unit immigration 25 after 10min DEG C water-bath stands reaction 6h.
(4) after reaction terminates, by being centrifugally separating to obtain white solid, white solid is washed 3 times and obtains SiO2Nanometer Ball.Remaining liq component is distilled, and collects ethanol and dichloromethane component.By SiO2Nanosphere is scattered in ethanol again, TEM is as shown in figure (1) b.
Embodiment 4：
(1) bis- ultra-pure waters of 4g are mixed with 16g ethanol, 5g dichloromethane is added under agitation, after addition is finished Persistently stir 10min.
(2) 1.3ml tetraethyl orthosilicates are slowly added into the O/W types obtained by step (1) under stirring to live without surface Property agent microemulsion system in, ultrasound 10min successively after addition is finished, stirring 20min.
(3) the O/W type surfactant-frees microemulsion system containing tetraethyl orthosilicate obtained by step (2) is moved into frozen water Bath, under agitation, 3ml ammoniacal liquor (25wt ﹪) is slowly added thereto, and is persistently stirred reaction unit immigration 25 after 10min DEG C water-bath stands reaction 6h.
(4) after reaction terminates, by being centrifugally separating to obtain white solid, white solid is washed 3 times and obtains SiO2Nanometer Ball.Remaining liq component is distilled, and collects ethanol and dichloromethane component.By SiO2Nanosphere is scattered in ethanol again, TEM is as shown in figure (1) a.
The different water alcohol ratio (R of table 1.w/e) under the conditions of the obtained particle diameter of silica nanosphere
Comparative example 1：
(1) bis- ultra-pure waters of 5g are mixed with 45g ethanol.
(2) 1.3ml tetraethyl orthosilicates are slowly added under stirring in the mixed system of ethanol and water, lasting stirring 20min。
(3) under agitation, 2.0ml ammoniacal liquor (25wt ﹪) is slowly added to contain tetraethyl orthosilicate obtained by step (2) Ethanol and water mixed system in, persistently stir and reaction unit is moved into 25 DEG C of water-baths after 30min stand reaction 12h.
(4) after reaction terminates, it is centrifuged collection white solid, ethanol is washed 3 times, water washing obtains dioxy 1 time SiClx nano particle.Nano SiO 2 particle is scattered in ethanol again, TEM is as schemed shown in (3).
The preferred embodiment of the application is the foregoing is only, the application is not limited to, for the skill of this area For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.

Claims (10)

1. a kind of preparation method of the monodisperse silica nanosphere of novel green, it is characterised in that including：
Prepare O/W types water/ethanol/dichloromethane surfactant-free microemulsion；
Tetraethyl orthosilicate TEOS is dissolved in the ball-type " oily core " of above-mentioned O/W types surfactant-free microemulsion, existed in ammoniacal liquor Under the conditions of, teos hydrolysis polycondensation, separation, washing produce single dispersing SiO2Nanosphere.
2. the method as described in claim 1, it is characterised in that in the surfactant-free microemulsion, fixed dichloromethane Mass fraction is 20%, and the mass ratio of water and ethanol is 6-9.5:4-0.5.
3. the method as described in claim 1, it is characterised in that the volume ratio of the tetraethyl orthosilicate and the ﹪ wt of ammoniacal liquor 25 is 1.3：3.
4. the method as described in claim 1, it is characterised in that described that tetraethyl orthosilicate is dissolved in above-mentioned surfactant-free Concretely comprising the following steps in microemulsion：By quantitative tetraethyl orthosilicate TEOS, it is added slowly with stirring the O/W and is lived without surface Property agent microemulsion system in, 8~10min of ultrasound successively after addition is finished, 8~10min of stirring.
5. the method as described in claim 1, it is characterised in that the ammoniacal liquor is slowly added under ice-water bath, stirring condition Dissolved with the O/W type surfactant-free microemulsion systems of silester.
6. the method as described in claim 1, it is characterised in that the condition of the hydrolytie polycondensation is：In quiet under 25-35 DEG C of water-bath Put reaction 1-24h.
7. the method as described in claim 1, it is characterised in that the separation is concretely comprised the following steps：By body after completion of the reaction System is centrifuged, and solid constituent washs 3 times with polar solvent and distills to obtain silica nanosphere, and remaining liq component is carried out Ethanol is collected in distillation, and dichloromethane is recycled.
8. monodisperse silica nanosphere prepared by the method described in claim any one of 1-7.
9. monodisperse silica nanosphere as claimed in claim 8, it is characterised in that the grain of the silica nanosphere Footpath is 275~785mm.
10. the monodisperse silica nanosphere described in any one of claim 8 or 9 is preparing biomedical material, catalysis material Application in material, functional material, high-performance ceramic or coating.
CN201710666272.9A 2017-08-07 2017-08-07 A kind of preparation method of the monodisperse silica nanosphere of novel green Withdrawn CN107285325A (en)

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CN108751208A (en) * 2018-06-05 2018-11-06 山东师范大学 A kind of monodisperse silica nanosphere and preparation method thereof prepared by surfactant-free microemulsion
RU2758782C1 (en) * 2020-12-11 2021-11-01 Автономная некоммерческая образовательная организация высшего образования "Сколковский институт науки и технологий" (Сколковский институт науки и технологий) Environmentally sustainable method for processing bulk silicon into silicon dioxide nanoparticles in an aqueous solution

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CN112969526A (en) * 2018-11-13 2021-06-15 硅循环股份有限公司 Hydrophobic/hydrophilic adjustable organic siloxane nanosphere/microsphere and preparation method thereof
CN110371991B (en) * 2019-07-05 2021-06-25 山东师范大学 Preparation method of core-shell structure silicon dioxide spherical nano-particles
CN110760298B (en) * 2019-10-23 2022-02-11 中国海洋石油集团有限公司 Surfactant-free microemulsion and preparation method thereof
CN115725081B (en) * 2022-11-18 2023-11-14 齐鲁师范学院 Preparation method of monodisperse organic silicon microsphere

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CN108751208A (en) * 2018-06-05 2018-11-06 山东师范大学 A kind of monodisperse silica nanosphere and preparation method thereof prepared by surfactant-free microemulsion
RU2758782C1 (en) * 2020-12-11 2021-11-01 Автономная некоммерческая образовательная организация высшего образования "Сколковский институт науки и технологий" (Сколковский институт науки и технологий) Environmentally sustainable method for processing bulk silicon into silicon dioxide nanoparticles in an aqueous solution
WO2022124948A1 (en) * 2020-12-11 2022-06-16 Autonomous Non-Profit Organization For Higher Education “Skolkovo Institute Of Science And Technology” Method of silicon recycling: synthesis of silica nanoparticles in an aqueous solution

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