CN112480410A - Preparation method of raspberry-shaped periodic mesoporous organic hollow silicon spheres - Google Patents
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Abstract
The invention discloses a preparation method of raspberry-shaped periodic mesoporous organic hollow silicon spheres, belonging to the technical field of material science. The method comprises the steps of raw material mixing, standing, washing, heating and centrifuging; the raw materials comprise a surfactant, a catalyst, silsesquioxane and a solvent. The preparation method of the raspberry-shaped periodic mesoporous organic hollow silicon spheres provided by the invention is a method for preparing the raspberry-shaped periodic mesoporous organic hollow silicon spheres at normal temperature in one step, has a simple formula and a simplified process flow, and is beneficial to realizing industrial production.
Description
Technical Field
The invention belongs to the technical field of material science, and particularly relates to a preparation method of raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Background
Periodic mesoporous organosilicon material (PMO) is a novel material which is discovered and proposed by the three scientific communities at the end of the last century. Its advantages are regular periodic mesoporous channel structure, high specific surface area, low density and easy preparing. In the next two decades, this material was extensively studied and developed by scientists. Scientists have prepared PMO particle materials with various shapes and structures, such as virus-shaped, feather-shaped and Janus-shaped PMO particles, by changing preparation conditions, designing a preparation method and the like. However, the preparation of PMO particles with complex morphology often requires a large number of preparation steps and harsh preparation conditions.
Disclosure of Invention
The invention aims to provide a preparation method of raspberry-shaped periodic mesoporous organic hollow silicon spheres and a product prepared by the preparation method.
The invention provides a preparation method of raspberry-shaped periodic mesoporous organic hollow silicon spheres, which comprises the following steps: (a) mixing the raw materials; (b) standing; (c) washing; (d) heating; (e) and (4) centrifuging.
In any of the above embodiments of the first aspect of the present invention, the feedstock in step (a) comprises a surfactant, a catalyst, a silsesquioxane, and a solvent.
In any of the above embodiments of the first aspect of the present invention, the raw material surfactant in step (a) is cetyltrimethylammonium bromide (CTAB), cetyltrimethylammonium chloride (CTAC), dodecyltrimethylammonium bromide (C)12TAB) or more; and/or the catalyst is one or more of ammonia water, dilute hydrochloric acid and sodium hydroxide aqueous solution; and/or the silsesquioxane is one or two of 1, 2-bis (triethoxysilyl) ethane (BTSE) and 1, 4-bis (triethoxysilyl) benzene (BTEB); and/or the solvent is water and/or ethanol.
In any of the above embodiments of the first aspect of the present invention, step (b) comprises: (b1) standing for 10-30 min at 20-30 ℃; (b2) standing for 4-48 h at 5-20 ℃.
In any one of the above embodiments of the first aspect of the present invention, step (d) is to dissolve the washed product in ethanol, heat at 60-80 ℃ for 4-6 h, and repeat 3 times.
The invention provides raspberry-shaped periodic mesoporous organic hollow silicon spheres prepared by the method provided by the first aspect of the invention.
The invention has the beneficial effects that:
(1) the preparation method of the raspberry-shaped periodic mesoporous organic hollow silicon spheres provided by the invention is a method for preparing the raspberry-shaped periodic mesoporous organic hollow silicon spheres at normal temperature in one step in a large scale, has a simple formula, greatly simplifies the process flow compared with the traditional preparation method of mesoporous silicon dioxide materials and other raspberry-shaped particles containing organic components, and is beneficial to realizing industrial production.
(2) The surfactant in the raw materials also serves as a template agent, and raspberry-shaped periodic mesoporous organic hollow silicon sphere nanoparticles with complex shapes can be prepared without adding a template agent additionally.
(3) The raspberry-shaped periodic mesoporous organic hollow silicon spheres prepared by the invention have a hollow structure and a high specific surface area (which can reach 1600 m)2More than g) can play an important role in the technical fields of super-hydrophobic coatings, high-specific-surface-area adsorption materials, composite material fillers and the like.
Drawings
FIG. 1 is a transmission electron microscope photograph of raspberry-like periodic mesoporous hollow organosilicon spheres obtained in example 1 of the present invention;
FIG. 2 is a photograph of a distribution diagram of the particle size of the raspberry-like periodic mesoporous hollow organosilicon spheres obtained in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantageous technical effects of the present invention more clear, the present invention is further described in detail with reference to the following embodiments. It should be understood that the embodiments described in this specification are only for the purpose of explaining the present invention and are not intended to limit the present invention.
For the sake of brevity, only some numerical ranges are explicitly disclosed herein. However, any lower limit may be combined with any upper limit to form ranges not explicitly recited; and any lower limit may be combined with any other lower limit to form a range not explicitly recited, and similarly any upper limit may be combined with any other upper limit to form a range not explicitly recited. Also, although not explicitly recited, each point or individual value between endpoints of a range is encompassed within the range. Thus, each point or individual value can form a range not explicitly recited as its own lower or upper limit in combination with any other point or individual value or in combination with other lower or upper limits.
In the description herein, it is to be noted that, unless otherwise specified, "above" and "below" are inclusive, and "several" of "one or several" means two or more.
The above summary of the present invention is not intended to describe each disclosed embodiment or every implementation of the present invention. The following description more particularly exemplifies illustrative embodiments. At various points throughout this application, guidance is provided through a list of embodiments that can be used in various combinations. In each instance, the list is merely a representative group and should not be construed as exhaustive.
The embodiment of the invention provides a preparation method of raspberry-shaped periodic mesoporous organic hollow silicon spheres, which comprises the following steps: s10, mixing the raw materials; s20, standing; s30, washing; s40, heating; and S50, centrifuging.
At S10, the feedstock includes a surfactant, a catalyst, a silsesquioxane, and a solvent.
In some preferred embodiments, at S10, the surfactant is weighed and then the solvent, catalyst, and silsesquioxane are added sequentially. At S10, the silsesquioxane is added last. In a more preferred embodiment, S10 includes: s11, dissolving a surfactant in a solvent to obtain a system A; s12, adding a catalyst into the system A, and uniformly mixing to obtain a system B; s13, dissolving silsesquioxane in ethanol to obtain a system C; and S14, mixing the system C with the system B to obtain a system D.
At S10, the raw material components are added in proportion. The raw materials comprise, by mass, 0.01-0.1% of a surfactant, 1-10% of a catalyst, 0.1-1% of silsesquioxane and the balance of a solvent.
Preferably, in S10, 0.01-0.1% of surfactant is weighed, and 95-99% of solvent, 1-10% of catalyst and 0.1-1% of silsesquioxane are sequentially added. Wherein the mass fraction of the solvent is preferably 95-98.89% and 95-98%.
More preferred example, S10 includes: s11, dissolving 0.01-0.1% of surfactant in a solvent to obtain a system A; s12, adding 1-10% of catalyst into the system A, and uniformly mixing to obtain a system B; s13, dissolving 0.1-1% silsesquioxane in ethanol to obtain a mixed solution C; and S14, mixing the mixed solution C with the system B to obtain a system D. Wherein the sum of the amounts of the solvents used in S11 and S13 is 95-99%, 95-98.89% or 95-98% of the solvent.
At S10, the surfactant is Cetyl Trimethyl Ammonium Bromide (CTAB), Cetyl Trimethyl Ammonium Chloride (CTAC), dodecyl trimethyl ammonium bromide (C)12TAB) is selected from one or more of the following. And/or the catalyst is one or more of ammonia water, dilute hydrochloric acid and sodium hydroxide aqueous solution. And/or the silsesquioxane is one or two of 1, 2-bis (triethoxysilyl) ethane (BTSE) and 1, 4-bis (triethoxysilyl) benzene (BTEB); and/or the solvent is water and/or ethanol.
Preferably, the solvent is a mixed solvent of water and ethanol, 60-80% of water and 20-40% of ethanol in mass fraction.
At S20, the mixture is allowed to stand at room temperature and then cooled and allowed to stand. Further, standing for 10-30 min at 20-30 ℃, and then standing for 4-48 h at 5-20 ℃. More preferably, the mixture is firstly kept stand at 25 ℃ for 10-30 min, 15-30 min or 15-20 min; and then standing for 10-48 h or 10-24 h at 15 ℃.
At S30, the product obtained at S20 is washed three times by centrifugation with ethanol and water, respectively, to wash out unreacted raw materials and catalyst, and finally a centrifuged solid material is obtained.
At S40, the solid material obtained at S30 is dissolved in excess fatty alcohol, preferably in excess ethanol, to sufficiently wash off the template molecules inside the particles; and then heating for 4-6 h at 60-80 ℃. Preferably, heating is carried out at 80 ℃ for 6 h.
And repeating S40 for three times, centrifuging S50, and drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Examples
The present disclosure is more particularly described in the following examples that are intended as illustrations only, since various modifications and changes within the scope of the present disclosure will be apparent to those skilled in the art. Unless otherwise indicated, all parts, percentages, and ratios reported in the following examples are on a weight basis, and all reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further treatment, and the equipment used in the examples is commercially available.
Example 1
Weighing 0.05g CTAB molecule, dissolving in a mixed solvent of 10ml ethanol and 30ml water, adding 0.2ml ammonia water with mass fraction of 28%, and shaking up. 0.08g of the powder with the density of 0.958g/cm3The BTSE molecule (2) was dissolved in 1ml of ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 30min, and allowed to stand at 15 ℃ for 10 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Fig. 1 is a transmission electron micrograph of the obtained raspberry-like periodic mesoporous hollow organosilicon spheres, fig. 2 is a photograph of a particle size distribution diagram of the obtained raspberry-like periodic mesoporous hollow organosilicon spheres, and it can be seen from fig. 2 that the particle size distribution of the particles prepared in example 1 is narrow, i.e., uniform.
Example 2
Weighing 0.02g CTAB molecule, dissolving in a mixed solvent of 10ml ethanol and 30ml water, adding 0.6ml ammonia water with mass fraction of 28%, and shaking up. 0.08g of the powder with the density of 0.958g/cm3The BTSE molecule (2) was dissolved in 1ml of ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 30min, and allowed to stand at 15 ℃ for 10 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Example 3
0.05g of CTAB molecule is weighed and dissolved in a mixed solvent of 10ml of ethanol and 30ml of water, 0.2ml of ammonia water with the mass fraction of 28 percent is added, and the mixture is shaken up. 0.08g of the powder with the density of 0.958g/cm3The BTSE molecule (2) was dissolved in 1ml of ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 30min, and allowed to stand at 15 ℃ for 10 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Example 4
0.04g CTAB molecule is weighed and dissolved in a mixed solvent of 10ml ethanol and 30ml water, 0.8ml hydrochloric acid with the mass fraction of 37 percent is added, and the mixture is shaken up. 0.08g of the powder with the density of 0.958g/cm3The BTSE molecule (2) was dissolved in 1ml of ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 30min, and allowed to stand at 15 ℃ for 10 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Example 5
0.01g of C was weighed12Dissolving TAB molecule in a mixed solvent of 10ml ethanol and 30ml water, adding 0.9ml ammonia water with mass fraction of 37%, and shaking up. 0.08g of the powder with the density of 0.958g/cm3The BTSE molecule (2) was dissolved in 1ml of ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 30min, and allowed to stand at 15 ℃ for 10 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Example 6
0.06g of C are weighed12Dissolving TAB molecule in mixed solvent of 10ml ethanol and 30ml water, adding 0.2ml hydrochloric acid with mass fraction of 37%, and shaking. 0.1g of a resin having a density of 0.958g/cm3The BTSE molecule (2) was dissolved in 1ml of ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 15min, and allowed to stand at 15 ℃ for 48 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Example 7
0.027g CTAB molecule is weighed and dissolved in a mixed solvent of 10ml ethanol and 30ml water, 0.2ml ammonia water with the mass fraction of 28% is added, and the mixture is shaken up. 0.1g of a resin having a density of 1.015g/cm3The BTEB molecule of (1 ml) was dissolved in ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 30min, and at 15 ℃ for 48 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Example 8
0.027g of CTAC molecule is weighed and dissolved in a mixed solvent of 10ml of ethanol and 30ml of water, 0.2ml of ammonia water with the mass fraction of 28% is added, and the mixture is shaken up. 0.2g of a density of 1.015g/cm3The BTEB molecule of (1 ml) was dissolved in ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 30min and at 10 ℃ for 24 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
Example 9
0.027g of CTAC molecule is weighed and dissolved in a mixed solvent of 10ml of ethanol and 30ml of water, 0.2ml of ammonia water with the mass fraction of 28% is added, and the mixture is shaken up. 0.2g of a density of 1.015g/cm3The BTEB molecule of (1 ml) was dissolved in ethanol, and this solution was added dropwise to the previous system, allowed to stand at 25 ℃ for 30min and at 10 ℃ for 24 hours. The resulting product was washed three times with ethanol and water by centrifugation, respectively. The product was dissolved in 100ml ethanol, heated at 80 ℃ for 6h, and this heating step was repeated three times. Finally, the product was isolated by centrifugation. And drying the obtained solid substance in a vacuum oven at room temperature for 48 hours to obtain the raspberry-shaped periodic mesoporous organic hollow silicon spheres.
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and various equivalent modifications and substitutions can be easily made by those skilled in the art within the technical scope of the invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A preparation method of raspberry-shaped periodic mesoporous organic hollow silicon spheres is characterized by comprising the steps of raw material mixing, standing, washing, heating and centrifuging; the raw materials comprise a surfactant, a catalyst, silsesquioxane and a solvent.
2. The preparation method according to claim 1, characterized in that the raw materials comprise 0.01-0.1% of surfactant, 1-10% of catalyst, 0.1-1% of silsesquioxane and the balance of solvent by mass fraction.
3. The preparation method according to claim 1 or 2, characterized in that the surfactant is one or more of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride and dodecyl trimethyl ammonium bromide; and/or the presence of a gas in the gas,
the catalyst is one or more of ammonia water, dilute hydrochloric acid and sodium hydroxide aqueous solution; and/or the presence of a gas in the gas,
the silsesquioxane is one or two of 1, 2-bis (triethoxysilyl) ethane and 1, 4-bis (triethoxysilyl) benzene; and/or the presence of a gas in the gas,
the solvent is water and/or ethanol.
4. The method of manufacturing according to claim 1, wherein the resting comprises:
(b1) standing for 10-30 min at 20-30 ℃;
(b2) standing for 4-48 h at 5-20 ℃.
5. The method of claim 1, wherein the washing reagent is water and/or ethanol; the number of washing times was 3 or more.
6. The preparation method according to claim 1, wherein the heating is carried out by dissolving the washed product in fatty alcohol and heating at 60-80 ℃ for 4-6 h.
7. The method of claim 6, wherein the heating step is repeated 3 times.
8. A raspberry-shaped periodic mesoporous organic hollow silicon sphere, which is prepared by the preparation method of any one of claims 1 to 7.
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