CN101993086A - Preparation method of mono-disperse silicon dioxide micro-spheres - Google Patents
Preparation method of mono-disperse silicon dioxide micro-spheres Download PDFInfo
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Abstract
The invention discloses a preparation method of mono-disperse silicon dioxide micro-spheres, which comprises the following steps of: (1) synthesizing mono-disperse silicon dioxide micro-sphere seeds by using a Stober method, namely at a reaction temperature of 10 to 60 DEG C, and in a solvent system of alcohol, water and ammonia, adding tetraethoxysilane alcoholic solution of which the concentration is 0.1 to 0.5 mol/L to react so as to obtain the mono-disperse silicon dioxide micro-sphere seeds; and (2) preparing the silicon dioxide micro-spheres from the silicon dioxide micro-sphere seeds by using a seed growth method, namely preparing silicon dioxide seed solution of which the concentration is 1,015 to 1,017 seeds/L by using the silicon dioxide micro-sphere seeds, the ammonia and the alcohol, and at the reaction temperature of 10 to 60 DEG C, adding ammonia-alcohol solution of which the concentration is 0.5 to 5.0 mol/L and tetraethoxy-silicane alkanol solution of which the concentration is 0.1 to 5.0 mol/L to react so as to obtain a suspension of the mono-disperse silicon dioxide micro-spheres.
Description
Technical field
The present invention relates to a kind of preparation method of monodisperse silica microspheres, especially size distribution is the preparation method of 100-800nm monodisperse silica microspheres.
Background technology
Monodisperse silica microspheres (the SiO of shape standard, homogeneous grain diameter
2) owing to have superior stability, reinforcement, thixotropy, and form characteristics such as single and surperficial easily functionalization, all have a very wide range of applications in materialogy fields such as rubber, plastics, coating, pigment, catalyzer, chromatograph packing material, high-performance ceramics; In addition, also, molecular biology be can be widely used in, biomass cells separation and engineering in medicine, makeup, medicine, medical diagnosis and immunoassay etc. comprised because its swelling and be not subject to the bacterium erosion not in organic solvent has good bio-compatibility.What in recent years, cause more that people study interest is to prepare photonic crystal with monodisperse silica microspheres for the raw material self-assembly.
The preparation method of silicon dioxide microsphere is a lot, as microemulsion method, chemical gaseous phase deposition method, Stober method.Microemulsion method needs to use a large amount of organism in preparation process, it reclaims difficult, and cost is high and can pollute environment; And the chemical gaseous phase deposition rule needs specific equipment, and energy consumption is higher.Stober method based on sol-gel processing adopts alcohol to make silicate hydrolytie polycondensation under ammonia-catalyzed as solvent, prepares silicon dioxide microsphere through certain post-processing again, and its technology is simple, and cost is low, and can obtain the monodispersity better products.
In decades, the preparation method of silicon dioxide microsphere has obtained bigger progress.People such as Koble in 1956 have generated monodisperse silica microspheres with the tetraethoxy condensation in ethanolic soln, people such as Stober have carried out comparatively systematic research to this reaction, and nineteen sixty-eight is that solvent has made the silicon dioxide microsphere than small particle size with ethanol.After this, scholars constantly improve this method and are perfect.Wish that the civil rights comparison system studied the influence to silicon dioxide microsphere monodispersity and sphericity of traditional sol-gel processing and multistep growth method.Cao Weixiao etc. are by regulating the ratio between tetraethoxysilane (TEOS)/water/ammoniacal liquor, obtain different-grain diameter (35～750nm), the silicon dioxide colloid particle of monodispersity.Utilization statistical models such as Zhang Hui identification LMAP method has been optimized the preparation technology of monodisperse silica microspheres.In addition, the domestic in recent years preparation about monodisperse silica microspheres also has and relates to.CN1974385 has introduced and has a kind ofly gone out monodisperse silica microspheres with the water prepared in reaction with metallic silicon power under a certain amount of base catalysis, and its gordian technique is that the adding speed of control alkali lye makes newly-generated microballoon precursor concentration be lower than the concentration that new karyomorphism becomes.CN101492164 utilizes seed-growth multistep processes, by selecting the ratio of ethanol, ammoniacal liquor and water suitable in seed preparation and the process of growth, makes the particle diameter deviation and is lower than 3%, has high circularity and monodisperse silica microspheres.
Though people have had the deep understanding of system to the monodisperse silica system, because the forming process of monodisperse system is very responsive to condition, two principal reaction hydrolysis in the process and the speed of condensation relation constantly change along with the variation of reaction conditions, and the growth velocity of microballoon also changes along with hydrolysis and condensation, make the preparation of monodisperse silica microspheres still all be confined to so far also be difficult to reach the scale of batch process in the laboratory.
Summary of the invention
Of the present invention
PurposeProvide the preparation method of the simple and monodisperse silica microspheres that particle diameter is controlled of a kind of experiment condition gentleness, technology.
For achieving the above object, the technical solution used in the present invention is:
A kind of preparation method of monodisperse silica microspheres comprises being prepared as follows step:
(1) utilize the Stober method to synthesize the monodisperse silica microspheres seed: under 10-60 ℃ temperature of reaction, in alcohol, water and aqueous ammonia solvent system, the alcoholic solution reaction that adds the tetraethoxysilane of 0. 1-0.5mol/L concentration obtains the monodisperse silica microspheres seed;
(2) utilize seed mediated growth method, prepare silicon dioxide microsphere with above-mentioned silicon dioxide microsphere seed: being made into concentration with silicon dioxide microsphere seed, ammoniacal liquor and alcohol is 10
15-10
17The silicon-dioxide seed liquor of individual/L, under 10-60 ℃ of temperature of reaction, adding concentration is that the ammoniacal liquor-alcoholic solution of 0.5-5mol/L and the tetraethoxysilane alcoholic solution reaction of 0.1-5mol/L obtain monodisperse silica microspheres suspension.
Alcohol in the described step (1) is Fatty Alcohol(C12-C14 and C12-C18); Described Fatty Alcohol(C12-C14 and C12-C18) is an ethanol; Described Fatty Alcohol(C12-C14 and C12-C18) also can be n-propyl alcohol.
Temperature in the described step (1) is 40-50 ℃.
Beneficial effect: because the employing of technique scheme, compared with prior art, the present invention has following advantage:
(1) technology is difficult to reach the scale of batch process in the past, and this technological experiment mild condition, technology are simple to operation, can reach the scale of batch process, is easy to realize industrialization, because the reaction conditions gentleness, easy handling, scalable scale to feather weight.
(2) can obtain high circularity, narrow distribution and the controlled monodisperse silica microspheres of particle diameter by this technology, by the selection of reaction solvent and the control of temperature of reaction, the silicon dioxide microsphere that obtains is more evenly distributed, and the silicon dioxide microsphere size distribution deviation that obtains is not more than 2%.
Embodiment
Embodiment 1:
(1) utilize the Stober method to synthesize the monodisperse silica microspheres seed: in the four-hole boiling flask of a clean 250ml, to add n-propyl alcohol 120ml, water 10.4ml and ammoniacal liquor 9.5ml, open mechanical stirring, the control rotating speed is 450r/pm, controlled temperature is 10 ℃, slowly drip the TEOS-n-propyl alcohol solution 26ml of 0.23mol/L, 25 minutes, reaction obtained the monodisperse silica microspheres seed;
(2) utilize seed mediated growth method, prepare silicon dioxide microsphere with above-mentioned silicon dioxide microsphere seed: adding in (1) silicon dioxide microsphere seed suspension 20ml, n-propyl alcohol 100ml, water 23ml and ammoniacal liquor 16ml of preparation in the four-hole boiling flask of a clean 500ml, to be made into concentration be 10
15The silicon-dioxide seed liquor of individual/L, opening and stirring the control rotating speed is 450rpm.Under 25 ℃, slowly drip the ammoniacal liquor-n-propyl alcohol solution of 2.0mol/L and the TEOS-n-propyl alcohol solution of 0.23mol/L simultaneously, the silicon-dioxide that the TEOS hydrolysis generates is grown on silicon dioxide microsphere seed outside surface.Consume ammoniacal liquor-n-propyl alcohol solution 43ml and TEOS-n-propyl alcohol solution 234ml respectively and continue reaction 8 hours, through monodisperse silica microspheres centrifugal, that washing obtains 100nm for several times, the size distribution deviation is 1.9%.
Embodiment 2:
(1) utilize the Stober method to synthesize the monodisperse silica microspheres seed: in the four-hole boiling flask of a clean 250ml, to add ethanol 130ml, water 11.6ml and ammoniacal liquor 9.8ml, open mechanical stirring, the control rotating speed is 450r/pm, controlled temperature is 20 ℃, slowly drip the TEOS-ethanolic soln 31ml of 0.21mol/L, 25 minutes, reaction obtained the monodisperse silica microspheres seed;
(2) utilize seed mediated growth method, prepare silicon dioxide microsphere with above-mentioned silicon dioxide microsphere seed: adding in (1) silicon dioxide microsphere seed suspension 20ml, ethanol 120ml, water 20ml and ammoniacal liquor 15ml of preparation in the four-hole boiling flask of a clean 500ml, to be made into concentration be 10
15The silicon-dioxide seed liquor of individual/L, opening and stirring the control rotating speed is 450rpm.Under 35 ℃, slowly drip the ammoniacal liquor-ethanolic soln of 0.5mol/L and the TEOS-ethanolic soln of 0.1mol/L simultaneously, the silicon-dioxide that the TEOS hydrolysis generates is grown on silicon dioxide microsphere seed outside surface.Consume ammoniacal liquor-ethanolic soln 46ml and TEOS-ethanolic soln 209ml respectively and continue reaction 7 hours, through monodisperse silica microspheres centrifugal, that washing obtains 200nm for several times, the size distribution deviation is 1.7%.
Embodiment 3:
(1) utilize the Stober method to synthesize the monodisperse silica microspheres seed: in the four-hole boiling flask of a clean 250ml, to add ethanol 125ml, water 10.6ml and ammoniacal liquor 8.8ml, open mechanical stirring, the control rotating speed is 450r/pm, controlled temperature is 40 ℃, slowly drip the TEOS-ethanolic soln 27ml of 0.31mol/L, 25 minutes, reaction obtained the monodisperse silica microspheres seed;
(2) utilize seed mediated growth method, prepare silicon dioxide microsphere with above-mentioned silicon dioxide microsphere seed: adding in (1) silicon dioxide microsphere seed suspension 20ml, ethanol 140ml, water 30ml and ammoniacal liquor 21ml of preparation in the four-hole boiling flask of a clean 500ml, to be made into concentration be 10
15The silicon-dioxide seed liquor of individual/L, opening and stirring the control rotating speed is 450rpm.Under 40 ℃, slowly drip the ammoniacal liquor-ethanolic soln of 4mol/L and the TEOS-ethanolic soln of 3mol/L simultaneously, the silicon-dioxide that the TEOS hydrolysis generates is grown on silicon dioxide microsphere seed outside surface.Consume ammoniacal liquor-ethanolic soln 49ml and TEOS-ethanolic soln 256ml respectively and continue reaction 5 hours, through monodisperse silica microspheres centrifugal, that washing obtains 400nm for several times, the size distribution deviation is 1.4%.
Embodiment 4:
(1) utilize the Stober method to synthesize the monodisperse silica microspheres seed: in the four-hole boiling flask of a clean 250ml, to add n-propyl alcohol 135ml, water 10.8ml and ammoniacal liquor 10.1ml, open mechanical stirring, the control rotating speed is 450r/pm, controlled temperature is 45 ℃, slowly drip the TEOS-n-propyl alcohol solution 27ml of 0.50mol/L, 25 minutes, reaction obtained the monodisperse silica microspheres seed;
(2) utilize seed mediated growth method, prepare silicon dioxide microsphere with above-mentioned silicon dioxide microsphere seed: adding in (1) silicon dioxide microsphere seed suspension 20ml, n-propyl alcohol 136ml, water 27ml and ammoniacal liquor 20ml of preparation in the four-hole boiling flask of a clean 500ml, to be made into concentration be 10
15The silicon-dioxide seed liquor of individual/L, opening and stirring the control rotating speed is 450rpm.Under 40 ℃, slowly drip the ammoniacal liquor-n-propyl alcohol solution of 3.2mol/L and the TEOS-n-propyl alcohol solution of 0.50mol/L simultaneously, the silicon-dioxide that the TEOS hydrolysis generates is grown on silicon dioxide microsphere seed outside surface.Consume ammoniacal liquor-n-propyl alcohol solution 51ml and TEOS-n-propyl alcohol solution 263ml respectively and continue reaction 5.5 hours, through monodisperse silica microspheres centrifugal, that washing obtains 300nm for several times, the size distribution deviation is 1.3%.
Embodiment 5:
(1) utilize the Stober method to synthesize the monodisperse silica microspheres seed: in the four-hole boiling flask of a clean 250ml, to add ethanol 115ml, water 9.3ml and ammoniacal liquor 8.6ml, open mechanical stirring, the control rotating speed is 450r/pm, controlled temperature is 50 ℃, slowly drip the TEOS-ethanolic soln 24ml of 0.15mol/L, 25 minutes, reaction obtained the monodisperse silica microspheres seed;
(2) utilize seed mediated growth method, prepare silicon dioxide microsphere with above-mentioned silicon dioxide microsphere seed: adding in (1) silicon dioxide microsphere seed suspension 20ml, ethanol 100ml, water 24ml and ammoniacal liquor 17ml of preparation in the four-hole boiling flask of a clean 500ml, to be made into concentration be 10
17The silicon-dioxide seed liquor of individual/L, opening and stirring the control rotating speed is 450rpm.Under 50 ℃, the ammoniacal liquor-ethanolic soln of simultaneously slow Dropwise 5 mol/L and the TEOS-ethanolic soln of 5mol/L, the silicon-dioxide that the TEOS hydrolysis generates is grown on silicon dioxide microsphere seed outside surface.Consume ammoniacal liquor-ethanolic soln 38ml and TEOS-ethanolic soln 206ml respectively and continue reaction 5 hours, through monodisperse silica microspheres centrifugal, that washing obtains 500nm for several times, the size distribution deviation is 1.2%.
Embodiment 6:
(1) utilize the Stober method to synthesize the monodisperse silica microspheres seed: in the four-hole boiling flask of a clean 250ml, to add n-propyl alcohol 135ml, water 10.8ml and ammoniacal liquor 10.1ml, open mechanical stirring, the control rotating speed is 450r/pm, controlled temperature is 60 ℃, slowly drip the TEOS-n-propyl alcohol solution 27ml of 0.10mol/L, 25 minutes, reaction obtained the monodisperse silica microspheres seed;
(2) utilize seed mediated growth method, prepare silicon dioxide microsphere with above-mentioned silicon dioxide microsphere seed: adding in (1) silicon dioxide microsphere seed suspension 20ml, n-propyl alcohol 130ml, water 29ml and ammoniacal liquor 23ml of preparation in the four-hole boiling flask of a clean 500ml, to be made into concentration be 10
17The silicon-dioxide seed liquor of individual/L, opening and stirring the control rotating speed is 450rpm.Under 60 ℃, slowly drip the ammoniacal liquor-n-propyl alcohol solution of 0.8mol/L and the TEOS-n-propyl alcohol solution of 3.2mol/L simultaneously, the silicon-dioxide that the TEOS hydrolysis generates is grown on silicon dioxide microsphere seed outside surface.Consume ammoniacal liquor-n-propyl alcohol solution 42ml and TEOS-ethanolic soln 233ml respectively and continue reaction 4.5 hours, through monodisperse silica microspheres centrifugal, that washing obtains 800nm for several times, the size distribution deviation is 1.9%.
Claims (5)
1. the preparation method of a monodisperse silica microspheres is characterized in that, comprises being prepared as follows step:
(1) utilize the Stober method to synthesize the monodisperse silica microspheres seed: under 10-60 ℃ temperature of reaction, in alcohol, water and aqueous ammonia solvent system, the alcoholic solution reaction that adds the tetraethoxysilane of 0.1-0.5mol/L concentration obtains the monodisperse silica microspheres seed;
(2) utilize seed mediated growth method, prepare silicon dioxide microsphere with above-mentioned silicon dioxide microsphere seed: being made into concentration with silicon dioxide microsphere seed, ammoniacal liquor and alcohol is 10
15-10
17The silicon-dioxide seed liquor of individual/L, under 10-60 ℃ temperature of reaction, adding concentration is that the ammoniacal liquor-alcoholic solution of 0.5-5.0mol/L and the tetraethoxysilane alcoholic solution reaction of 0.1-5mol/L obtain monodisperse silica microspheres suspension.
2. the preparation method of monodisperse silica microspheres according to claim 1, it is characterized in that: the alcohol in the described step (1) is Fatty Alcohol(C12-C14 and C12-C18).
3. the preparation method of monodisperse silica microspheres according to claim 2, it is characterized in that: described Fatty Alcohol(C12-C14 and C12-C18) is an ethanol.
4. the preparation method of monodisperse silica microspheres according to claim 2, it is characterized in that: described Fatty Alcohol(C12-C14 and C12-C18) is a n-propyl alcohol.
5. the preparation method of monodisperse silica microspheres according to claim 1, it is characterized in that: the temperature of reaction in the described step (1) is 40-50 ℃.
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| CN102390926A (en) * | 2011-07-28 | 2012-03-28 | 东华大学 | Method for preparing glass fibre with structural colors |
| CN102662050A (en) * | 2012-05-24 | 2012-09-12 | 东北师范大学 | Immunoassay method based on infrared absorption property of silicon dioxide nanoparticle |
| CN102795630A (en) * | 2011-05-24 | 2012-11-28 | 山西博亮硅业有限公司 | Method for preparing silicon dioxide by using reverse micro-emulsion method |
| CN102808317A (en) * | 2012-08-23 | 2012-12-05 | 东华大学 | Method for preparing silicon dioxide nanosphere assembled polymer fiber |
| CN102951648A (en) * | 2011-08-31 | 2013-03-06 | 中国石油化工股份有限公司 | Preparation method of nano silicon dioxide |
| CN103318899A (en) * | 2013-06-24 | 2013-09-25 | 哈尔滨工业大学 | Control method of grain sizes of monodisperse silicon dioxide pellets |
| CN103359740A (en) * | 2012-03-27 | 2013-10-23 | 浩华科技实业有限公司 | Preparation method of silica shear thickening liquid |
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| CN101492164A (en) * | 2009-03-09 | 2009-07-29 | 东南大学 | Method of manufacturing monodisperse silicon dioxide microsphere |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101492164A (en) * | 2009-03-09 | 2009-07-29 | 东南大学 | Method of manufacturing monodisperse silicon dioxide microsphere |
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| CN102390926B (en) * | 2011-07-28 | 2014-05-28 | 东华大学 | Method for preparing glass fibre with structural colors |
| CN102390926A (en) * | 2011-07-28 | 2012-03-28 | 东华大学 | Method for preparing glass fibre with structural colors |
| CN102951648A (en) * | 2011-08-31 | 2013-03-06 | 中国石油化工股份有限公司 | Preparation method of nano silicon dioxide |
| CN102951648B (en) * | 2011-08-31 | 2014-11-26 | 中国石油化工股份有限公司 | Preparation method of nano silicon dioxide |
| CN103359740A (en) * | 2012-03-27 | 2013-10-23 | 浩华科技实业有限公司 | Preparation method of silica shear thickening liquid |
| CN102662050A (en) * | 2012-05-24 | 2012-09-12 | 东北师范大学 | Immunoassay method based on infrared absorption property of silicon dioxide nanoparticle |
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| CN104003408A (en) * | 2014-05-16 | 2014-08-27 | 南京东检生物科技有限公司 | Preparation method of continuous controllable monodispersed silica microspheres |
| WO2015196092A1 (en) * | 2014-06-20 | 2015-12-23 | Wei Wang | Porous silicon nanostructured electrode and method |
| US10756330B2 (en) | 2014-06-20 | 2020-08-25 | The Regents Of The University Of California | Porous silicon nanostructured electrode and method |
| CN104556071A (en) * | 2014-12-29 | 2015-04-29 | 上海新安纳电子科技有限公司 | Porous silica preparation method and application of porous silica |
| CN107848811A (en) * | 2015-07-31 | 2018-03-27 | 福吉米株式会社 | The manufacture method of silicon dioxide gel |
| CN107848811B (en) * | 2015-07-31 | 2021-11-05 | 福吉米株式会社 | Method for producing silica sol |
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Application publication date: 20110330 |