CN106829974A - A kind of preparation method of single dispersing, the Nano particles of silicon dioxide of small size - Google Patents
A kind of preparation method of single dispersing, the Nano particles of silicon dioxide of small size Download PDFInfo
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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
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Abstract
The preparation method of a kind of single dispersing, the Nano particles of silicon dioxide of small size, belongs to nano-particle preparing technical field.It is in alcohol, aqueous solvent, to add alkyl silicate, a hydronium(ion) lithia and other alkali compounds, and lithium hydroxide is 1 with the quality amount ratio of other alkali compounds：0~650；Then under 20~50 DEG C, 100~500rpm stirring conditions, react 1~8 hour；Reaction solution centrifugation is removed supernatant by reaction after terminating, centrifugation product is first washed 1~2 time, washed 2~3 times with the identical alcoholic solvent for above being used again, afterwards dry product at 50~80 DEG C, so as to obtain the silicon dioxide granule of pure single dispersing, small size (3~200nm).The present invention prepares Nano particles of silicon dioxide by a step growth in situ, it is not required to multistep injection silicon source or additionally introduces the methods such as seed, other impurities (such as various surfactants of cation, anion, neutrality) need not more be introduced, therefore, the preparation method is more simple, product is easier purifying.
Description
Technical field
The invention belongs to nano-particle preparing technical field, and in particular to a kind of single dispersing, the silica of small size are received
The preparation method of rice corpuscles.
Background technology
Silicon dioxide granule is in fields such as heterogeneous catalysis, film forming, gel, polishing, high-performance ceramics and chromatogram fillings
It is with a wide range of applications.Traditional silicon dioxide granule is prepared and is widely usedMethod (J.Colloid
Interface Sci.1968,26,62-69).The method is usually in alcohol, water mixed solvent, to be made with the ammoniacal liquor of various concentrations
It is catalyst, spherical silicon dioxide granule is prepared through tetraethyl orthosilicate hydrolysis, condensation.Silica prepared by the method
Particle size range is general at 10~500nm adjustable (J.Colloid Interface Sci.1992,154,481-501), obtains
Arrive large scale particle (>200nm) its particle diameter is more homogeneous, and small size particles (<200nm) monodispersity is poor
(J.Eur.Ceram.Soc.1994,14,205-214).In order to realize single dispersing, the silicon dioxide granule of small size it is easy,
Effectively prepare, researchers have developed various preparation methods.Arriagada et al. utilizes reverse microemulsion process, is prepared for particle diameter
Homogeneous, size is in the adjustable silicon dioxide granules of 30~60nm (J.Colloid Interface Sci.1999,221,210-
220)；Cao is proud it is also proposed that using reverse microemulsion process, preparing size adjustable monodisperse silica grain between 20~200nm
Sub (Chinese invention patent publication number：CN 101913611A).But reverse microemulsion process, needs largely to use the surface for being difficult to removal
Particle properties are often had a negative impact by activating agent.Tsapatsis et al. is proposed with alkaline biomolecule (such as lysine
Or arginine) as catalyst, through hydrolysis, condensation in the two phase emulsion system that tetraethyl orthosilicate and water are constituted, obtain chi
Very little is the silicon dioxide granule (Chem.Mater.2006,18,5814-5816 of 5nm or so；Pub.No.：US 2008/
0213883A1), technology reaction time needs more than 24 hours, and by the unstability of used two-phase system, it is difficult to it is right
The size of particle is regulated and controled.Yokoi et al. is improved the method that lysine catalysis prepares silicon dioxide granule, with pungent
Alkane and water constitute relatively stable two-phase system, and by regulating and controlling pH value, preparing uniform particle diameter, size can between 12~44nm
Silicon dioxide granule (the J.Am.Chem.Soc.2006,128,13664-13665 of tune；Chem.Mater.2009,21,3719-
3729；Pub.No.：US 2008/0311397A1；Pub.No.：US 2011/0151260A1).Due to lysine and silicic acid point
Stronger electrostatic interaction between son, either all cannot be bigger using D types lysine, L-type lysine or its mixture
Particle size is regulated and controled in size range.In order to solve this problem Kitaev et al. proposes to synthesize lysine method two
Silicon oxide particle obtains size in the adjustable silicon dioxide granules of 15~200nm as seed using the method for regrowth
(Langmuir 2008,24,1714-1720), but the method in large-scale production be difficult avoid secondary or multiple nucleation, grain
Sub- polydispersion angle value is higher, will have a negative impact to particle homogeneity.
Particle polydispersity is one of particle size distribution width and measures that can be represented with particle size deviation, its is normal
Rule computational methods are the particles that selection is more than 200 from transmission electron microscope photo, and its grain size is measured respectively, are then calculated
Its dimensional discrepancy (J.Colloid Interface Sci.2000,232,102-110).Deviation is smaller, shows particle size point
Cloth is narrower, and particle diameter is more homogeneous, and corresponding particle polydispersion angle value is lower.When particle polydispersion angle value<When 5%, grain is considered as
Son is monodispersed (Langmuir 2008,24,1714-1720.).
The content of the invention
The technical problem to be solved in the present invention is the problem for overcoming background technology to exist, there is provided a kind of easy, effective list
Dispersion, the preparation method of the silicon dioxide granule of small size (3~200nm).Small size and uniform particle diameter prepared by the present invention
Nano particles of silicon dioxide has structure homogeneous and polydispersion angle value can be controlled in less than 5%.
In the technical program, the introducing of lithium hydroxide is in regulation and control silicon dioxide granule size and improvement silicon dioxide granule
Homogeneity aspect serves key effect.It can accelerate the hydrolysis rate of alkyl silicate, promote silicate monomer fast nucleation,
More primary particles are formed, while promoting efficiently separating for particle nucleation and growth course again, enables particle according to warp
" nucleation-growth pattern " of allusion quotation is carried out, the adverse effect for preventing the secondary or multiple nucleation after nucleation from being produced to particle homogeneity.
Additionally, in alkyl silicate initial reaction stage, if being individually added into a small amount of lithium hydroxide, it can promote silicon source faster to hydrolyze,
Condensation and nucleation.Because lithium hydroxide consumption is less, quickly consumed in initial reaction stage, particle grew after fast nucleation
Journey becomes more slow, and the particle size for ultimately forming is smaller and more homogeneous.
The preparation method of a kind of small size of the present invention and the silicon dioxide granule of uniform particle diameter, it is characterised in that：
(water and alcohol volume ratio are 1 in alcohol, aqueous solvent：4~99), add alkyl silicate, its final concentration of 1~300g/
L；Add a hydronium(ion) lithia, the final concentration of 0.002~0.2g/L of lithium hydroxide；Other alkali compounds are added, its end
Concentration is 0~20g/L, and lithium hydroxide and the quality amount ratio of other alkali compounds are 1：0~650；Then 20~50
DEG C, under 100~500rpm (rev/min) stirring condition, react 1~8 hour；Reaction goes reaction solution centrifugation after terminating
Clearly, centrifugation product is first washed 1~2 time, then is washed 2~3 times with the identical alcoholic solvent for above being used, afterwards at 50~80 DEG C
Product is dried, so as to obtain the silicon dioxide granule of pure single dispersing, small size (3~200nm).
Described alcoholic solvent, refers to methyl alcohol, ethanol, propyl alcohol or their mixture.The alkyl silicate, its structure can
With Si (R ')m(OR)nTo represent, wherein m, n is integer, and m+n=4, m=0~3, n=1~4, R and R ' be methyl, ethyl,
Propyl group or butyl, R and R ' both can be the same or different；Described alkyl silicate is specifically referred to：When m=0, n=4, R points
Wei not methyl, ethyl, propyl group and butyl；M=1, n=3, when m=2, n=2 or m=3, n=1, R ' and R can be methyl, second
Base, propyl group and butyl；What is added in reaction can be the mixture of one or more in abovementioned alkyl esters of silicon acis.
Other described alkali compounds, refer to NaOH, potassium hydroxide, TMAH, tetraethyl hydrogen-oxygen
Change the mixing of one or more in ammonium, TPAOH, TBAH, choline, basic amino acid, ammoniacal liquor
Thing.
Beneficial effects of the present invention：
Because the method for the present invention is used with alkyl silicate and lithium hydroxide or lithium hydroxide and other alkalizations
The mix reagent reaction of compound, via a step growth in situ, is not required to multistep injection and silicon source or additionally introduces the methods such as seed, more without
Other impurities (such as various surfactants of cation, anion, neutrality) need to be introduced, therefore, the preparation method is more simple,
Product is easier purifying.Additionally, tune of the synthetic method of the Nano particles of silicon dioxide of the single dispersing, small size to particle size
Control has more preferable effect, particle size can be regulated and controled in 3~200nm scopes.
Brief description of the drawings
Fig. 1 is the transmission electron microscope of the 3nm silicon dioxide granules of size uniformity obtained in the embodiment of the present invention 1
(TEM) image, 3nm particles are shown in image particle in black circles.
Fig. 2 is the transmission electron microscope of the 6nm silicon dioxide granules of size uniformity obtained in the embodiment of the present invention 2
(TEM) image.
Fig. 3 is the transmission electron microscope of the 15nm silicon dioxide granules of size uniformity obtained in the embodiment of the present invention 3
(TEM) image.
Fig. 4 is the transmission electron microscope of the 40nm silicon dioxide granules of size uniformity obtained in the embodiment of the present invention 4
(TEM) image.
Fig. 5 is the transmission electron microscope of the 60nm silicon dioxide granules of size uniformity obtained in the embodiment of the present invention 5
(TEM) image.
Fig. 6 is the transmission electron microscope of the 90nm silicon dioxide granules of size uniformity obtained in the embodiment of the present invention 6
(TEM) image.
Fig. 7 is the transmission electron microscope of the 160nm silicon dioxide granules of size uniformity obtained in the embodiment of the present invention 7
(TEM) image.
Fig. 8 is the transmission electron microscope of the 200nm silicon dioxide granules of size uniformity obtained in the embodiment of the present invention 8
(TEM) image.
Specific embodiment
The following is the primary condition of specific embodiment of the invention, but the scope that the present invention can be implemented is not limited to these
Condition, is also not necessarily limited to these embodiments：
20 DEG C of environment temperature, 1 atmospheric pressure；
One hydronium(ion) lithia (LiOHH2O), every gram contains 0.57 gram of LiOH.
TMAH (TMAOH) aqueous solution, mass fraction 25%, density 1.02g/mL, every milliliter contains 0.26
Gram TMAOH.
Ammoniacal liquor, mass fraction 25%, density 0.91g/mL, every milliliter contains 0.23 gram of NH3。
Choline (C5H15NO2) aqueous solution, mass fraction 48.50%, density 1.09g/mL, every milliliter contains 0.53 gram
C5H15NO2。
Embodiment 1：The preparation of 3nm silicon dioxide granules
In the mixed solvent of 50mL propyl alcohol and water, water, alcohol volume ratio are 1：99 (V/V), are firstly added 0.18mg mono-
Hydronium(ion) lithia (the whole mass concentration 0.002g/L of lithium hydroxide), in 20 DEG C of reaction temperature, mixing speed 100rpm, plus
Enter 0.05g MTESs (whole mass concentration 1g/L), continue to be stirred 1 hour under the conditions of 20 DEG C of temperature, 100rpm,
Reaction terminate after after centrifugation removes supernatant, first wash one time, then after washing twice with propyl alcohol, 60 DEG C dry particle, obtain pure
The 3nm silicon dioxide granules of uniform particle diameter, such as Fig. 1.Particle polydispersity is 4.8%, and yield is 52%.
Embodiment 2：The preparation of 6nm silicon dioxide granules
In the mixed solvent of 10mL propyl alcohol and water, water, alcohol volume ratio are 1：49 (V/V), are firstly added 0.18mg mono-
Hydronium(ion) lithia (the whole mass concentration 0.01g/L of lithium hydroxide), reaction temperature regulation is stabilized to 25 DEG C, mixing speed
During 200rpm, the positive quanmethyl silicates of 0.5g (whole mass concentration 50g/L) is added, continued in 25 DEG C of temperature, mixing speed 200rpm
Under the conditions of stir 3 hours, supernatant is removed in centrifugation after reaction terminates, and is first washed one time, then after washing twice with propyl alcohol, 60 DEG C are dried particle
It is dry, obtain the 6nm silicon dioxide granules of pure uniform particle diameter, such as Fig. 2.Particle polydispersity is 4.5%, and yield is 56%.
Embodiment 3：The preparation of 15nm silicon dioxide granules
In the mixed solvent of 100mL ethanol and water, water, alcohol volume ratio are 1：24 (V/V), are firstly added 3.51mg mono-
Hydronium(ion) lithia (the whole mass concentration 0.02g/L of lithium hydroxide) and the ammonia spirit (NH that 2mL mass fractions are 25%3's
Whole mass concentration 4.60g/L), lithium hydroxide is 1 with the quality amount ratio of ammonia：230, reaction temperature regulation to 30 DEG C, stirring speed
When degree is stabilized to 300rpm, 10g tetraethyl orthosilicates (whole mass concentration 100g/L) is added, continued in 30 DEG C of temperature, 300rpm
Under the conditions of stir 6 hours, after reaction terminates, supernatant is removed in centrifugation, is first washed one time, then after washing twice with ethanol, and 60 DEG C by particle
Drying, obtains the 15nm silicon dioxide granules of pure uniform particle diameter, such as Fig. 3.Particle polydispersity is 4.2%, and yield is
62%.
Embodiment 4：The preparation of 40nm silicon dioxide granules
In the mixed solvent of 200mL ethanol and water, water, alcohol volume ratio are 1：79 (V/V), are firstly added 17.55mg
One hydronium(ion) lithia (the whole mass concentration 0.05g/L of lithium hydroxide), 0.25g NaOH (whole mass concentration 1.25g/L)
With 1g 1Bs (whole mass concentration 5g/L), quality consumption (NaOH and the 1B of lithium hydroxide and other alkali
Gross mass) than being 1：125, when reaction temperature regulation to 40 DEG C, mixing speed is stabilized to 400rpm, add the ethoxy of 40g ethyls three
Base silane (whole mass concentration 200g/L), continues to be stirred 8 hours under the conditions of 40 DEG C of temperature, 400rpm, after reaction terminates, centrifugation
Supernatant is removed, is first washed one time, then after washing twice with ethanol, 60 DEG C dry particle, obtain the 40nm bis- of pure uniform particle diameter
Silicon oxide particle, such as Fig. 4.Particle polydispersity is 4.5%, and yield is 70%.
Embodiment 5：The preparation of 60nm silicon dioxide granules
In the mixed solvent of 500mL methyl alcohol and water, water, alcohol volume ratio are 1：19 (V/V), are firstly added 175.44mg
One hydronium(ion) lithia (the whole mass concentration 0.20g/L of lithium hydroxide) and the ammonia spirit (NH that 40mL mass fractions are 25%3
Whole mass concentration 18.40g/L), the quality amount ratio of lithium hydroxide and ammonia is 1：91, reaction temperature regulation to 50 DEG C, stirring
When velocity-stabilization is to 500rpm, add the positive butyl esters of silicic acid four of 135g (whole mass concentration 270g/L), continue 50 DEG C of temperature,
Stirred 6 hours under the conditions of 500rpm, after reaction terminates, supernatant is removed in centrifugation, is first washed one time, after again with methanol washes twice, 50 DEG C
Particle is dried, the 60nm silicon dioxide granules of pure uniform particle diameter, such as Fig. 5 is obtained.Particle polydispersity is 4.0%, is produced
Rate is 76%.
Embodiment 6：The preparation of 90nm silicon dioxide granules
In the mixed solvent of 1.0L methyl alcohol and water, water, alcohol volume ratio are 1：9 (V/V), are firstly added 58.77mg mono-
Hydronium(ion) lithia (the whole mass concentration 0.03g/L of lithium hydroxide), 90.0mg potassium hydroxide (whole mass concentration 0.09g/L) and
84mL mass fractions are 25% ammonia spirit (NH3Whole mass concentration 19.32g/L), the quality of lithium hydroxide and other alkali
Consumption (gross mass of NaOH and ammonia) is than being 1：647, reaction temperature regulation is stabilized to 200rpm to 25 DEG C, mixing speed
When, the positive silicic acid orthocarbonates of 300g (whole mass concentration 300g/L) is added, continue the stirring 6 under the conditions of 25 DEG C of temperature, 200rpm small
When, after reaction terminates, supernatant is removed in centrifugation, is first washed one time, and after again with methanol washes twice, 70 DEG C dry particle, obtain pure
Uniform particle diameter 90nm silicon dioxide granules, such as Fig. 6.Particle polydispersity is 3.5%, and yield is 81%.
Embodiment 7：The preparation of 160nm silicon dioxide granules
In the mixed solvent of 5.0L ethanol and water, water, alcohol volume ratio are 1：4 (V/V), are firstly added the water of 0.44g mono-
Lithium hydroxide (the whole mass concentration 0.05g/L of lithium hydroxide) is closed, 0.57mL mass fractions are 48.5% aqueous choline base solution (courage
The whole mass concentration 0.06g/L of alkali) and ammonia spirit (NH that 50mL mass fractions are 25%3Whole mass concentration 2.30g/L),
Lithium hydroxide is 1 with quality consumption (gross mass of choline and ammonia) ratio of other alkali：47, reaction temperature is adjusted to 25 DEG C, stirring
When velocity-stabilization is to 200rpm, 90g tetraethyl orthosilicates (whole mass concentration 18g/L) is added, continued in 25 DEG C of temperature, 200rpm
Under the conditions of stir 3 hours, after reaction terminates, supernatant is removed in centrifugation, is first washed one time, and after again with methanol washes twice, 80 DEG C by particle
Drying, obtains the 160nm silicon dioxide granules of pure uniform particle diameter, such as Fig. 7.Particle polydispersity is 3.8%, and yield is
86%.
Embodiment 8：The preparation of 200nm silicon dioxide granules
In the mixed solvent of 5.0L ethanol and water, water, alcohol volume ratio are 1：9 (V/V), are firstly added the water of 1.48g mono-
Lithium hydroxide (the whole mass concentration 0.17g/L of lithium hydroxide) is closed, 67.3mL mass fractions are 25% TMAH
The aqueous solution (the whole mass concentration 3.50g/L of TMAH) and 60g 1Bs (whole mass concentration 12g/L), hydrogen-oxygen
Change lithium with the quality consumption (gross mass of TMAH and 1B) of other alkali than being 1：91, reaction temperature regulation
When being stabilized to 250rpm to 30 DEG C, mixing speed, 75g tetraethyl orthosilicates (whole mass concentration 15g/L) is added, continued at 30 DEG C
Stirred 3 hours under the conditions of temperature, 250rpm, after reaction terminates, supernatant is removed in centrifugation, is first washed one time, then after washing twice with ethanol,
50 DEG C dry particle, obtain the 200nm silicon dioxide granules of pure uniform particle diameter, such as Fig. 8.Particle polydispersity is
2.7%, yield is 90%.
Claims (8)
1. a kind of single dispersing, the preparation method of the Nano particles of silicon dioxide of small size, it is characterised in that：In alcohol, aqueous solvent body
In system, alkyl silicate, its final concentration of 1~300g/L are added；Add a hydronium(ion) lithia, lithium hydroxide it is final concentration of
0.002~0.2g/L；Other alkali compounds are added, its final concentration of 0~20g/L, and lithium hydroxide and other alkaline chemical combination
The quality amount ratio of thing is 1：0~650；Then under 20~50 DEG C, 100~500rpm stirring conditions, react 1~8 hour；Instead
Supernatant is removed into reaction solution centrifugation after should terminating, centrifugation product is first washed 1~2 time, then with molten with the identical alcohol for above being used
Agent is washed 2~3 times, afterwards dries product at 50~80 DEG C, so as to obtain the titanium dioxide silicon grain of pure single dispersing, small size
Son.
2. as claimed in claim 1 a kind of single dispersing, the preparation method of the Nano particles of silicon dioxide of small size, its feature exist
In：The size range of the Nano particles of silicon dioxide for preparing is 3~200nm.
3. as claimed in claim 1 a kind of single dispersing, the preparation method of the Nano particles of silicon dioxide of small size, its feature exist
In：The polydispersity of the Nano particles of silicon dioxide for preparing is less than 5%.
4. as claimed in claim 1 a kind of single dispersing, the preparation method of the Nano particles of silicon dioxide of small size, its feature exist
In：Water is 1 with the volume ratio of alcohol：4~99.
5. as claimed in claim 1 a kind of single dispersing, the preparation method of the Nano particles of silicon dioxide of small size, its feature exist
In：Alcoholic solvent is methyl alcohol, ethanol, propyl alcohol or their mixture.
6. as claimed in claim 1 a kind of single dispersing, the preparation method of the Nano particles of silicon dioxide of small size, its feature exist
In：The structural formula of alkyl silicate is Si (R ')m(OR)n, wherein m, n is integer, and m+n=4, m=0~3, n=1~4, R and
R ' is methyl, ethyl, propyl group or butyl, and R and R ' are identical or different；The one kind or several in abovementioned alkyl esters of silicon acis is added in reaction
The mixture planted.
7. as claimed in claim 6 a kind of single dispersing, the preparation method of the Nano particles of silicon dioxide of small size, its feature exist
In：When m=0, n=4, R is methyl, ethyl, propyl group or butyl；M=1, n=3, when m=2, n=2 or m=3, n=1, R ' and R
It is methyl, ethyl, propyl group or butyl.
8. as claimed in claim 1 a kind of single dispersing, the preparation method of the Nano particles of silicon dioxide of small size, its feature exist
In：Other alkali compounds are NaOH, potassium hydroxide, TMAH, tetraethyl ammonium hydroxide, tetrapropyl hydrogen-oxygen
Change the mixture of one or more in ammonium, TBAH, choline, basic amino acid, ammoniacal liquor.
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| CN107381579A (en) * | 2017-06-28 | 2017-11-24 | 华东师范大学 | A kind of preparation method of mesoporous spherical nano Sio 2 particle |
| CN107673361A (en) * | 2017-11-03 | 2018-02-09 | 吉林大学 | A kind of preparation method of the hollow silicon dioxide particle of more shells |
| CN112209386A (en) * | 2020-09-29 | 2021-01-12 | 天津大学 | Preparation method of small-size hollow mesoporous silica nanoparticles |
| CN112226221A (en) * | 2020-10-19 | 2021-01-15 | 河南大学 | Nano silicon dioxide oil displacement agent and preparation method and application thereof |
| CN112226221B (en) * | 2020-10-19 | 2022-03-01 | 河南大学 | Nano silicon dioxide oil displacement agent and preparation method and application thereof |
| CN113184863A (en) * | 2021-05-11 | 2021-07-30 | 北京工业大学 | Preparation method of sphere-like porous silicon dioxide powder |
| CN113772681A (en) * | 2021-09-24 | 2021-12-10 | 吉林大学 | Regulation and control method of mercapto-silicon dioxide particle microstructure |
| CN115180627A (en) * | 2022-07-11 | 2022-10-14 | 吉林大学 | Preparation method of silicon dioxide particles with branch structures on surfaces |
| CN115180627B (en) * | 2022-07-11 | 2023-09-15 | 吉林大学 | Preparation method of silica particles with branch structure on surface |
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