CN109399638A - A kind of preparation method of dendroid silicon nanoparticle - Google Patents
A kind of preparation method of dendroid silicon nanoparticle Download PDFInfo
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Abstract
The invention belongs to the new method fields of pharmaceutical nanometer formulation auxiliary material preparation, and in particular to a kind of preparation method of dendroid silicon nanoparticle.This method synthesizes the dendroid silicon nanoparticle of radial pore structure centered on surface texture using cetyl trimethyl ammonium halide, positive esters of silicon acis, fatty acid salt and deionized water as reaction raw materials.Preparation method mild condition of the invention, environmental protection, is easy to amplify production, and obtained product structure is stablized, favorable dispersibility, and the carrier that can be used as large biological molecule or drug, catalyst molecule etc. uses.
Description
Technical field
The invention belongs to the new method fields of pharmaceutical nanometer formulation auxiliary material preparation, and in particular to a kind of dendroid nano-silicon
The preparation method of particle.
Background technique
Nano-medicament carrier has important application value, it has also become popular research field.Nanometer material (particle
Size is less than 500 nanometers) there is more technological merit, for example (,) it is higher specific surface area and pore volume, good colloid-stabilised
Property, excellent biocompatibility etc..In addition, the size of particle, mesoporous pore size and pattern are adjustable, inside particle surface and hole
It can also make its functionalization by chemical modification, therefore in field of biomedicine (imaging diagnosis, bioprobe, biocatalysis, bone
Reparation, bracket engineering, pharmaceutical carrier etc.) there is extensive and important application prospect.
The good adsorption delivered payload capability of meso-porous nano silicon materials has become the candidate of pharmaceutical carrier.It is common mesoporous
Nano silicon material, such as MCM-41, duct are integrally in parallel structure of hexagonal crystal arrangement, and aperture is only suitable for absorption point less than 3 nanometers
Son measures lesser substance, and the hole wall of depths is also difficult to touch substance, therefore limited sorption capacity and is easily saturated；In addition, hole
Wall is thin, is easy to be destroyed after heating or compression.However dendroid silicon nanoparticle has the branch radiated outward from center
Shape hole configurations, stability is good, surface apertures big (maximum can be to 20 nanometers or more), surface area are big, has good absorption dress
Loading capability (especially to large biological molecule, including nucleic acid, protein and lipid molecule etc.).Therefore in relevant medicine and chemistry
The research of catalytic reaction and application field cause extensive interest.
The method of reported preparation dendroid silicon nanoparticle mainly has two-phase stratification method and weak template etc..But
It is still suffered from using the dendroid silicon nanoparticle that these methods conveniently and freely prepare different-grain diameter or different-shape huge
Big challenge.Some methods use organic solvent in large quantities, not only affect the safety of product, but also return subsequent amplification
Difficulty is manufactured.Therefore, the method for improving the preparation of dendroid nano-silicon becomes project urgently to be resolved at present.
Summary of the invention
In view of the existing technical defect, the purpose of the present invention is to provide a kind of preparations of dendroid silicon nanoparticle
Method, the preparation method use fatty acid salt and cationic surfactant to prepare dendroid as mixed surfactant for the first time
Silicon nanoparticle, the present invention prepared by dendroid silicon nanoparticle be spherical nanoparticle, chemical nature be silica
Polymer, the radial pore structure outside from granular center is contained on surface.
To achieve the goals above, the present invention adopts the following technical scheme that.
A method of the silicon nanoparticle with dendritic structure being prepared, this method utilizes cetyl trimethyl halogenation
Ammonium, positive esters of silicon acis, fatty acid salt and deionized water synthesize radial pore structure centered on surface texture as reaction raw materials
The molar ratio of dendroid silicon nanoparticle, the fatty acid salt and cetyl trimethyl ammonium halide is 0.25:1-2:1.
A method of the silicon nanoparticle with dendritic structure being prepared, specific preparation method is as follows.
Step 1 mixes cetyl trimethyl ammonium halide, fatty acid salt with deionized water in proportion, and heating, constant temperature are permanent
Fast magnetic agitation makes it completely dissolved.
Pasc reaction precursor agent is added in step 2.
Step 3, reaction time are 2-16 hours；It is centrifuged at least 5 minutes for 4000 revs/min or more after reaction, abandons supernatant；
Dispersed again with water or ethyl alcohol, be centrifuged, repeated washing 2-3 times, it is dry, obtain product.
Fatty acid salt (the C of the step 1nH2n-1O2-) it is the single-stranded fatty acid salt that carbon number is six to ten four.
The fatty acid salt of the step 1 is the salt containing lithium, sodium, potassium, caesium, magnesium, calcium, strontium, barium, manganese, zinc or aluminium.
The cetyl trimethyl ammonium halide of the step 1 is cetyl trimethylammonium bromide (CTAB) or cetyl
Trimethyl ammonium chloride (CTAC).
The pasc reaction precursor agent of the step 2 is ethyl orthosilicate, methyl orthosilicate, 1,2- bis- (triethoxysilicane) ethane
Etc. inorganic or organic silicon source.
The volume ratio (v:v) of the step 2 pasc reaction precursor agent and deionized water is 0.6:10 ~ 1:5.
The reaction temperature is 95 DEG C ± 5 DEG C.
Existing dendroid nanometer silicon preparation method is broadly divided into the two-phase stratification method mixed with water with organic solvent and weak
Template, the former can prepare the dendroid nano-silicon of different-shape and partial size, but must use the technology of microwave heating and a large amount of
Organic solvent (such as hexamethylene etc.), be unfavorable for environmental protection, production cost is higher；The latter must use and cetyl trimethyl halogen
Change ammonium and form the hybrid template molecule of interaction, then so that the pattern of nano-silicon is changed with base catalysis, becomes dendroid.This
Invention has used the hybrid template molecular fat hydrochlorate different from reported method, contains hydrophobic carbon in molecular structure
Chain is in alkalescent in aqueous solution, can adjust simultaneously and be catalyzed generation dendroid nano-silicon.The present invention has following technology excellent
Gesture.
(1) production cost is low, and environmental protection easy to operate, easy expanding production: the present invention is prepared in water phase, and the original used
Material includes that fatty acid salt, cetyl trimethyl ammonium halide, silicon precursor agent etc. are relatively environment-friendly reaction reagent.Prepare item
Part can be amplified in proportion by embodiment.
(2) product has good dispersibility, and particle diameter distribution is uniform, and dendritic structure is uniform.
(3) organic solvent is not used in preparation process, obtained dendritic silicon nanoparticle has the radial macropore in center
Gap structure, the carrier that can be used as large biological molecule or drug, catalyst molecule etc. use.
Detailed description of the invention
Fig. 1 is dendroid nano-silicon transmission electron microscope photo prepared by embodiment 1.
Fig. 2 is dendroid nano-silicon transmission electron microscope photo prepared by embodiment 2.
Fig. 3 is dendroid nano-silicon transmission electron microscope photo prepared by embodiment 3.
Fig. 4 is dendroid nano-silicon transmission electron microscope photo prepared by embodiment 4.
Fig. 5 is dendroid nano-silicon transmission electron microscope photo prepared by embodiment 5.
Fig. 6 is dendroid nano-silicon transmission electron microscope photo prepared by embodiment 6.
Fig. 7 is the dendroid nano-silicon transmission electron microscope photo that reaction temperature is 80 DEG C of preparations.
Fig. 8 is the dendroid nano-silicon transmission electron microscope photo that reaction temperature is 70 DEG C of preparations.
Fig. 9 is the dendroid nano-silicon transmission electron microscope that the molar ratio of Sodium Caprylate and cetyl trimethyl ammonium halide is 2:1
Photo.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples, but following embodiments are not intended to limit right model of the invention
It encloses.
Embodiment 1.
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 0.7 gram of Sodium Caprylate (molar ratio 1:1) and go
In ionized water, stirring and dissolving 30 minutes at 95 DEG C, 10 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, 6000 turns/
Supernatant is abandoned in the separation heart 10 minutes；With 30 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
219 ± 24 nanometers of dendroid silicon nanoparticle (Fig. 1).
Embodiment 2.
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 0.7 gram of Sodium Caprylate (molar ratio 1:1) and go
In ionized water, stirring and dissolving 30 minutes at 95 DEG C, 14 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, 6000 turns/
Supernatant is abandoned in the separation heart 10 minutes；With 30 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
275 ± 20 nanometers of dendroid silicon nanoparticle (Fig. 2).
Embodiment 3.
1.5 grams of cetyl trimethylammonium bromides and 0.35 gram of Sodium Caprylate (molar ratio 1:0.5) be added to 100 milliliters go from
In sub- water, stirring and dissolving 30 minutes at 95 DEG C, 14 milliliters of ethyl orthosilicates, which are added, and are stirred to react 8 hours terminates, and 6000 revs/min
Supernatant is abandoned in centrifugation 10 minutes；With 30 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, obtaining partial size is 220 ± 9
The dendroid silicon nanoparticle (Fig. 3) of nanometer.
Embodiment 4.
1.5 grams of cetyl trimethylammonium bromides and 1.15 grams of sodium n-caproates (molar ratio 1:2) are added to 100 milliliters of deionizations
In water, stirring and dissolving 30 minutes at 95 DEG C, 10 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, 6000 revs/min from
The heart 10 minutes, abandon supernatant；With 30 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, obtains partial size and received for 218 ± 14
The dendroid silicon nanoparticle (Fig. 4) of rice.
Embodiment 5.
1.5 grams of cetyl trimethylammonium bromides and 0.4 gram of sodium caprate (molar ratio 1:0.5) be added to 100 milliliters go from
In sub- water, stirring and dissolving 30 minutes at 95 DEG C, 10 milliliters of ethyl orthosilicates, which are added, and are stirred to react 4 hours terminates, and 6000 revs/min
Supernatant is abandoned in centrifugation 10 minutes；With 30 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
149 ± 15 nanometers of dendroid silicon nanoparticle (Fig. 5).
Embodiment 6.
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 0.46 gram of sodium laurate (molar ratio 1:0.5) and go
In ionized water, stirring and dissolving 30 minutes at 95 DEG C, 10 milliliters of ethyl orthosilicates, which are added, and are stirred to react 4 hours terminates, 6000 turns/
Supernatant is abandoned in the separation heart 10 minutes；With 30 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
133 ± 11 nanometers of dendroid silicon nanoparticle (Fig. 6).
The screening experiment of reaction condition.
1) screening of reaction temperature.
Differential responses temperature has a significant impact the dispersibility of nano-particle product, and ideal temperature is 95 DEG C ± 5 DEG C, reduces
Temperature can lead to product dispersibility variation, be the product electromicroscopic photograph (Fig. 7, Fig. 8) respectively at 80 DEG C and 70 DEG C below.
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 0.7 gram of Sodium Caprylate (molar ratio 1:1) and go
In ionized water, stirring and dissolving 30 minutes at 80 DEG C, 14 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates.Crude product
It is dry with ethyl alcohol eccentric cleaning 2-3 times, obtain the poor dendroid silicon nanoparticle (Fig. 7) of dispersibility.
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 0.7 gram of Sodium Caprylate (molar ratio 1:1) and go
In ionized water, stirring and dissolving 30 minutes at 70 DEG C, 14 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates.Crude product
It is dry with ethyl alcohol eccentric cleaning 2-3 times, obtain the poor dendroid silicon nanoparticle (Fig. 8) of dispersibility.
It can be seen from Fig. 7 and Fig. 8 when reaction temperature is reduced to 80 DEG C (Fig. 7) or 70 DEG C (Fig. 8), nano-silicon
Grain produces more adhesion each other, and the dispersibility of particle is obviously identical not as good as 2 other conditions of embodiment, and temperature is 95 DEG C
Preparation result (Fig. 2).
2) screening of sodium soap and cetyl trimethylammonium bromide molar ratio.
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 1.4 grams of Sodium Caprylates (molar ratio 1:2) and go
In ionized water, stirring and dissolving 30 minutes at 95 DEG C, 14 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates.Crude product
With ethyl alcohol eccentric cleaning 2-3 times, the poor dendroid silicon nanoparticle (Fig. 9) of dispersibility is obtained.
The molar ratio of fatty acid salt and cetyl trimethyl ammonium halide is 0.25:1 ~ 2:1.This range is to dendroid
The dispersibility and pattern of silicon nanoparticle all have an impact.Fatty acid salt has alkalescent, while having and adjusting product and catalysis instead
The function of answering, dosage is too low to will lead to reaction not exclusively (such as ratio is lower than 0.25:1).As shown in figure 9, with embodiment 2 and in fact
It applies example 3 and compares that (molar ratio of 2 result figure 2 of embodiment, Sodium Caprylate and cetyl trimethyl ammonium halide is respectively 1:1 together；It is real
3 result figure 3 of example is applied, the molar ratio of Sodium Caprylate and cetyl trimethyl ammonium halide is respectively 0.5:1) as can be seen that fixing it
His reaction condition as the molar ratio of Sodium Caprylate and cetyl trimethyl ammonium halide changes to 1:1 from 0.5:1, then arrives 2:1
When, the partial size of product nano silicon increases, and dispersibility reduces.
3) screening of silicon precursor agent dosage.
The volume ratio (v:v) of pasc reaction precursor agent and deionized water is 0.6:10 ~ 1:5.Increase the ratio of silicon precursor solution
Can have an impact to the dispersibility and partial size of silicon nanoparticle, it can from the corresponding Electronic Speculum result figure 1 of Examples 1 and 2 and Fig. 2
Out, fixed other conditions, the dosage for increasing silicon precursor agent make the partial size of dendroid silicon nanoparticle increase (about 50 nanometers), point
Scattered property decreases.
4) screening of the fatty acid salt of different carbon chain lengths.
The fatty acid salt of different carbon chain lengths has larger impact to the pattern of dendroid nano-silicon, and carbochain increases, will lead to
The increase of dendroid silicon nanoparticle hole, partial size reduce, and dispersibility reduces.Such as 3 and of Electronic Speculum result figure of embodiment 3 and 5,6
Shown in Fig. 5, Fig. 6, the pattern of silicon nanoparticle is produced bigger effect using Sodium Caprylate and sodium caprate, sodium laurate respectively, the last of the ten Heavenly stems
Sour sodium and the silicon nanoparticle hole of sodium laurate preparation are bigger, partial size reduction (220 ± 9 nanometers of Sodium Caprylate, sodium caprate 149 ±
15 nanometers, 133 ± 11 nanometers of sodium laurate), dispersibility reduces.
5) investigation of speed of agitator and centrifugal rotational speed time.
Experiments have shown that speed of agitator influences less the property of product, the constant range of speeds can from 100 revs/min to
700 revs/min.The magnetic agitation rotating speed of the reaction influences less product characteristics, appropriate.
Centrifugation step system after the reaction precipitates solid product from liquid, and the revolving speed time is not hard
Property require.
Claims (8)
1. a kind of preparation method of the silicon nanoparticle with dendritic structure, which is characterized in that this method utilizes cetyl
Trimethyl-ammonium halide, positive esters of silicon acis, fatty acid salt and deionized water synthesize and radiate centered on surface texture as reaction raw materials
The molar ratio of the dendroid silicon nanoparticle of shape pore structure, the fatty acid salt and cetyl trimethyl ammonium halide is 0.25:1
-2:1。
2. a kind of preparation method of the silicon nanoparticle with dendritic structure, which is characterized in that the preparation method include with
Lower step:
Step 1 mixes cetyl trimethyl ammonium halide, fatty acid salt with deionized water in proportion, heating, constant temperature constant speed magnetic
Power stirring makes it completely dissolved；
Pasc reaction precursor agent is added in step 2；
Step 3, reaction time are 2-16 hours；4000 revs/min or more are centrifuged at least 5 minutes, abandon supernatant；Again with water or ethyl alcohol
Dispersion, centrifugation, repeated washing 2-3 times is dry, obtains product.
3. a kind of preparation method of silicon nanoparticle with dendritic structure according to claim 2, feature exist
In the fatty acid salt (C of the step 1nH2n-1O2-) it is the single-stranded fatty acid salt that carbon number is six to ten four.
4. a kind of preparation method of silicon nanoparticle with dendritic structure according to claim 2, feature exist
In the fatty acid salt of the step 1 is the salt containing lithium, sodium, potassium, caesium, magnesium, calcium, strontium, barium, manganese, zinc or aluminium.
5. a kind of preparation method of silicon nanoparticle with dendritic structure according to claim 2, which is characterized in that
The cetyl trimethyl bromine ammonium halide of the step 1 is cetyl trimethylammonium bromide CTAB or cetyl trimethyl chlorine
Change ammonium CTAC.
6. a kind of preparation method of silicon nanoparticle with dendritic structure according to claim 2, feature exist
In the pasc reaction precursor agent of the step 2 is ethyl orthosilicate, methyl orthosilicate, 1,2- bis- (triethoxysilicane) second
Alkane etc. is inorganic or organic silicon source.
7. a kind of preparation method of silicon nanoparticle with dendritic structure according to claim 2, which is characterized in that
The volume ratio of the step 2 pasc reaction precursor agent and deionized water is 0.6:10- 1:5.
8. a kind of preparation method of silicon nanoparticle with dendritic structure according to claim 2, which is characterized in that
It is 95 DEG C ± 5 DEG C that reaction temperature is heated in the step 1.
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| CN112259740A (en) * | 2020-10-28 | 2021-01-22 | 成都新柯力化工科技有限公司 | Dendritic silicon-carbon composite negative electrode material of lithium battery and preparation method |
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| CN113526515A (en) * | 2021-08-29 | 2021-10-22 | 浙江华飞电子基材有限公司 | Nano spherical silicon micro powder separation and extraction method |
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