CN113150028A - Preparation method of mesoporous organic silicon nanowire and mesoporous organic silicon nanowire - Google Patents
Preparation method of mesoporous organic silicon nanowire and mesoporous organic silicon nanowire Download PDFInfo
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- CN113150028A CN113150028A CN202110381342.2A CN202110381342A CN113150028A CN 113150028 A CN113150028 A CN 113150028A CN 202110381342 A CN202110381342 A CN 202110381342A CN 113150028 A CN113150028 A CN 113150028A
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- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
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Abstract
The invention provides a preparation method of mesoporous organic silicon nanowires and mesoporous organic silicon nanowires, and relates to the technical field of preparation of nano materials. The preparation method of the mesoporous organic silicon nanowire comprises the following steps: adding an alkali catalyst into a solvent in which a surfactant is dissolved, and reacting to obtain a reaction liquid a; adding an organosilane coupling agent into the reaction liquid a at a preset rate, and reacting to obtain an organosilicon nanowire; and (3) extracting the organic silicon nanowire by using an acidic ethanol solution to obtain the mesoporous organic silicon nanowire. The preparation method of the mesoporous organosilicon nanowire can prepare the mesoporous organosilicon nanowire with adjustable length-diameter ratio only under the conditions that the water bath is 25-60 ℃ and the rotating speed in oscillation is 50-200 rpm, and has the advantages of simple preparation process, mild preparation conditions, strong controllability, low reaction difficulty and small danger.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method of a mesoporous organic silicon nanowire and the mesoporous organic silicon nanowire.
Background
The mesoporous organic silicon nano material is a novel organic-inorganic hybrid material on a molecular scale, and has wide application value in the aspects of catalysis, chromatographic separation, sensing, biomedicine and the like due to the combination of the mesoporous channel structural characteristics and the adjustable hydrophilicity and hydrophobicity of the organic silicon material. Researches show that the application of the mesoporous organosilicon nano-material depends on the macroscopic morphology of the mesoporous organosilicon nano-material to a great extent, and how to controllably prepare mesoporous organosilicon nano-materials with different morphologies is an important direction in the field. With the continuous development of nanotechnology, researchers continuously prepare mesoporous organosilicon materials with zero-dimensional spherical, one-dimensional rod-shaped structures and two-dimensional layered structures.
Compared with zero-dimensional and two-dimensional structured nanomaterials, one-dimensional structured nanomaterials are widely used in a plurality of fields in recent years due to unique linear structures: (1) the quantum size effect is remarkable, and the special properties of light absorption, light emission and optical nonlinearity are realized, so that the quantum size effect can be applied to photoelectric devices; (2) the surface area volume ratio is high, the surface adsorption is very sensitive, the change of interface ion transport caused by the change of the external environment can be detected, and the sensor can be used as a sensor; (3) the lithium ion battery has the characteristics of high charge and discharge capacity and good cycle performance, and can play a great role in the research and development of novel batteries; (4) has higher giant magnetoresistance effect and opens up the development path of novel functional materials such as one-dimensional giant magnetoresistance materials.
At present, some work has been done by researchers in the preparation of one-dimensional structured nanowire materials. In the prior art, N-dimethylformamide and trichloroethylene are used as a mixed solvent, polyvinylpyrrolidone, zinc acetate and indium nitrate hydrate are dissolved to prepare a precursor solution, then an electrofluid jet printing device is used for printing a nanowire array, and IZO semiconductor nanowires are prepared after high-temperature annealing. In addition, the prior art also has a preparation method for preparing silver nanowires with different high length-diameter ratios by a one-pot method, so that the simple and efficient preparation of the silver nanowires with high length-diameter ratios can be realized.
Although the method prepares the nanowire material with the one-dimensional structure, the reports about the mesoporous organosilicon nanowire with the one-dimensional structure are less at present. The mesoporous organic silicon nanowire has great potential application value. Therefore, the development of a simple and controllable method for preparing the mesoporous organosilicon nanowire has very challenging and significance, and the preparation route of the mesoporous organosilicon nanowire can be enriched and developed to promote the application of the mesoporous organosilicon nanowire.
Disclosure of Invention
An object of the first aspect of the present invention is to provide a method for preparing mesoporous organosilicon nanowires, which solves the problems in the prior art that the preparation process of mesoporous organosilicon nanowires is complicated, and the aspect ratio of the prepared mesoporous organosilicon nanowires is not adjustable.
The second aspect of the invention aims to provide mesoporous organosilicon nanowires with adjustable length-diameter ratio.
Particularly, the invention provides a preparation method of mesoporous organic silicon nanowires, which comprises the following steps:
adding an alkali catalyst into a solvent in which a surfactant is dissolved, and reacting to obtain a reaction liquid a;
adding an organosilane coupling agent into the reaction liquid a at a preset rate, and reacting to obtain an organosilicon nanowire;
and extracting the organic silicon nanowire by using an acidic ethanol solution to obtain the mesoporous organic silicon nanowire.
Optionally, the surfactant is selected from cetyltrimethylammonium p-toluenesulfonate;
the solvent comprises a mixed solvent of water and ethanol, wherein the volume ratio of water to ethanol in the mixed solvent is 20-10: 0 to 10;
the molar ratio of the surfactant to the reaction liquid a is 0.05-0.4: 1.
Optionally, the base catalyst is selected from one or more of ammonia, triethylamine, sodium hydroxide or triethanolamine;
the pH value of the reaction liquid a is 9-11.
Optionally, the organosilane coupling agent is selected from one or more of 1, 4-bis (triethoxysilyl) benzene, 1, 2-bis (triethoxysilyl) ethane, 1, 2-bis (triethoxysilyl) ethylene, or bis- [3- (triethoxy) propylsilicon ] disulfide.
Alternatively, the molar ratio of the organosilane coupling agent to the reaction liquid a is (5.0 × 10)-5～10.0×10-4)：1。
Optionally, the preset rate is: 0.003 mL/min-0.096 mL/min.
Optionally, the reaction time in the reaction step for obtaining the organosilicon nanowire is 24-72 h.
Optionally, all processes before the step of obtaining the organic silicon nanowire through reaction are carried out in a water bath with a preset temperature and under an oscillating condition; wherein the preset temperature is 25-60 ℃, and the rotating speed during oscillation is 50-200 rpm.
Optionally, the acidic ethanol solution is a mixed solution prepared by mixing hydrochloric acid and ethanol or a mixed solution prepared by mixing ammonium nitrate and ethanol, wherein the volume of the hydrochloric acid or the ammonium nitrate in the mixed solution is 1% to 10% of the volume of the ethanol.
In particular, the invention also provides a mesoporous organosilicon nanowire prepared by the preparation method, and the mesoporous organosilicon nanowire has a specific surface area of 500m2/g～1200m2The length of the material is 0.5-3 mu m, the width of the material is 14-120 nm, and the length-diameter ratio of the material is 4-178.
The preparation method of the mesoporous organosilicon nanowire can prepare the mesoporous organosilicon nanowire with adjustable length-diameter ratio only under the conditions that the water bath is 25-60 ℃ and the rotating speed in oscillation is 50-200 rpm, and has the advantages of simple preparation process, mild preparation conditions, strong controllability, low reaction difficulty and small danger.
The raw materials of the surfactant, the solvent, the alkali catalyst, the organic silicon coupling agent and the acidic ethanol solution used in the preparation method are simple and easy to obtain, so that the preparation method is low in cost.
The preparation method of the mesoporous organosilicon nanowire can adjust the length, the width and the final length-diameter ratio of the mesoporous organosilicon nanowire by means of the self-assembly effect of the surfactant and the organic silicon source precursor in the solvent and simply regulating and controlling the reaction conditions such as the dropping speed, the dosage, the solvent proportion of the reaction and the like of the organic silicon source precursor, so that the length of the obtained organosilicon nanowire can reach 0.5-3 mu m, the width can reach 14-120 nm, and the length-diameter ratio is 4-178. In addition, after the organosilicon nanowire is obtained, the mesoporous organosilicon nanowire prepared by removing the surfactant has obvious mesoporous structure, regular shape and good dispersion, and the specific surface area of the mesoporous organosilicon nanowire can reach 500m2/g～1200m2And/g, the preparation technology development of the mesoporous organic silicon nanowire with the adjustable length-diameter ratio is promoted.
The above and other objects, advantages and features of the present invention will become more apparent to those skilled in the art from the following detailed description of specific embodiments thereof, taken in conjunction with the accompanying drawings.
Drawings
Some specific embodiments of the invention will be described in detail hereinafter, by way of illustration and not limitation, with reference to the accompanying drawings. The same reference numbers in the drawings identify the same or similar elements or components. Those skilled in the art will appreciate that the drawings are not necessarily drawn to scale. In the drawings:
fig. 1 is a schematic flow diagram of a method of preparing mesoporous silicone nanowires according to one embodiment of the invention;
FIG. 2 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 1;
FIG. 3 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 2;
FIG. 4 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 3;
FIG. 5 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 4;
FIG. 6 is a distribution diagram of the specific surface area and the pore diameter of the mesoporous organosilicon nanowire prepared according to example 4;
FIG. 7 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 5;
FIG. 8 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 6;
FIG. 9 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 7;
fig. 10 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 8;
fig. 11 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 9;
FIG. 12 is a transmission electron micrograph of nanoparticles prepared according to example 10;
fig. 13 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 11;
fig. 14 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 12;
fig. 15 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 13;
fig. 16 is a transmission electron microscope image of mesoporous organosilicon nanowires prepared according to example 14.
Detailed Description
Fig. 1 is a schematic flow diagram of a method for preparing mesoporous organosilicon nanowires according to one embodiment of the invention. As shown in fig. 1, the preparation method of the mesoporous organosilicon nanowire of the present embodiment may include the following steps:
step S100, adding an alkali catalyst into a solvent in which a surfactant is dissolved, and reacting to obtain a reaction liquid a;
step S200, adding an organosilane coupling agent into the reaction liquid a according to a preset rate, and reacting to obtain an organic silicon nanowire;
and step S300, extracting the organic silicon nanowire by using an acidic ethanol solution to obtain the mesoporous organic silicon nanowire.
In this embodiment, in step S100, the step of obtaining the reaction solution a includes: and placing the solvent dissolved with the surfactant and the alkali catalyst in a water bath at a preset temperature for oscillation to obtain the reaction liquid a, wherein the preset temperature is 25-60 ℃, and the rotation speed during oscillation is 50-200 rpm.
The preset temperature in this embodiment may be 25 ℃ to 60 ℃, for example, the preset temperature may be 25 ℃, 30 ℃, 50 ℃ or 60 ℃. In this embodiment, the oscillating rotation speed may be 50rpm to 200 rpm. For example, the rotational speed of the oscillation may be 50rpm, 80rpm, 100rpm, or 200 rpm.
In step S100, the surfactant is first added to the solvent to be dissolved. Specifically, after the surfactant is added into the solvent, the surfactant containing the solvent is placed in a water bath at 25-60 ℃, and oscillation is carried out at the rotating speed of 50-200 rpm, so that the dissolving speed of the surfactant in the solvent can be accelerated, and the surfactant can be more uniformly dissolved. The surfactant can self-assemble to form a stable surfactant micelle only when dissolved uniformly. In addition, in step S100, if the temperature of the water bath is too low, the solubility of the surfactant is poor, and the surfactant cannot be dissolved and self-assembled well to form surfactant micelles, and the interaction force between the organosilicon source precursor (i.e., the organosilicon coupling agent) and the surfactant micelles is poor, so that linear organosilicon nanowires cannot be assembled together. If the temperature of the water bath is too high, the kinetics of the hydrolysis condensation reaction of the organic silicon source precursor is increased, and the organic silicon source precursor cannot react with the surfactant micelle, so that the organic silicon source precursor forms independent floccule through self-nucleation in the solvent.
In this example, the surfactant is selected from cetyltrimethyl-p-toluenesulfonammonium. The hexadecyl trimethyl p-toluene ammonium sulfonate contains benzene rings, can be self-assembled into a rod-shaped micelle in a solvent, and can enable an organosilane coupling agent precursor in the subsequent step S200 to linearly grow along the rod-shaped micelle to form a one-dimensional nanowire structure.
The solvent in the embodiment comprises a mixed solvent of water and ethanol, wherein the volume ratio of water to ethanol in the mixed solvent is 20-10: 0 to 10. For example, the volume ratio of water to ethanol in the mixed solvent may be 20:1, 20:5, 20:10, 10:1, 10:5, or 10: 10.
In this embodiment, a proper amount of ethanol is added to the solvent, so that the solubility of the organosilane coupling agent in the subsequent step S200 is enhanced, which is beneficial to the width improvement of the mesoporous organosilicon nanowire. However, if the amount of ethanol is too high, the solubility of the surfactant is increased, the formed micelle is distorted, the acting force with the organic silicon source precursor is weakened, the uniformity of the formed product is poor, and even agglomeration occurs.
In this example, the molar ratio of the surfactant to the reaction solution a was (0.05-0.4): 1. For example, the molar ratio of surfactant to reaction solution a may be 0.05:1, 0.1:1, 0.2:1, or 0.4: 1.
In this embodiment, the alkali catalyst is selected from one or more of ammonia water, triethylamine, sodium hydroxide, and triethanolamine, and after the alkali catalyst is added, the pH value of the reaction solution a obtained by the reaction may be 9 to 11. For example, the pH of the reaction solution a may be 9, 10 or 11. In the embodiment, the alkali catalyst is preferably ammonia water, the ammonia water is weakly alkaline, the hydrolysis-condensation reaction rate of the organosilane coupling agent is relatively slow, and the rate of the generated organosilicon nanowires is controllable. When the dosage of the ammonia water is too small, the hydrolysis condensation speed of the organic silicon source precursor is slow, and the organic silicon nanowires are not easy to generate. When the using amount of the ammonia water is too large, the hydrolysis condensation rate of the organic silicon source precursor is too high due to the too strong base catalysis, and the organic silicon source precursor can be nucleated in a homogeneous phase to form free organic silicon small particles, so that a solution with the pH value within the range of 9-11 is obtained after the ammonia water is preferably added.
In step S200, the organosilane coupling agent is selected from one or more of 1, 4-bis (triethoxysilyl) benzene, 1, 2-bis (triethoxysilyl) ethane, 1, 2-bis (triethoxysilyl) ethylene, or bis- [3- (triethoxy) propylsilicon ] disulfide. In this embodiment, all of the organosilane coupling agents described above can be reacted with the reaction solution a to obtain the organosilicon nanowires. In this embodiment, 1, 4-bis (triethoxysilyl) benzene (BTEB) is preferable as the organosilane coupling agent in the embodiment, because the BTEB contains a benzene ring in the molecular structure, the compatibility with the surfactant cetyl trimethyl ammonium p-toluenesulfonate (CTATos) is better, a stable composite system can be better formed, the obtained organosilicon nanowire is more uniform, and the aspect ratio can be more easily adjusted.
In step S200, the molar ratio of the organosilane coupling agent to the reaction liquid a is (5 × 10)-5～10×10-4): 1. for example, the molar ratio of the organosilane coupling agent to the reaction liquid a may be 5 × 10-5：1、6×10-5：1、1×10-4:1 or 10X 10-4: 1. the organic silicon nanowires can be formed in the range, but when the dosage of the organic silane coupling agent is less, the formed organic silicon nanowires are less, the form is unstable, and the yield is low; when the dosage of the organosilane coupling agent is more, the formed organosilicon nanowires are disordered and the length-diameter ratio is difficult to regulate. Therefore, the amount of the organosilane coupling agent in the range is preferable.
As a specific embodiment of the present invention, in this embodiment, the preset rate is: 0.003 mL/min-0.096 mL/min. Preferably, the predetermined rate of the dropping is 0.006mL/min to 0.048 mL/min. If the preset dropping rate of the organosilane coupling agent is too low, the concentration of the initial siloxane oligomer generated by the organosilane coupling agent in the solvent is low, and the initial siloxane oligomer and the surfactant micelle are difficult to assemble together to form the organosilicon nanowire. When the preset dropping rate of the organosilane coupling agent is too high, a large amount of siloxane oligomer can be generated in a short time under the alkaline reaction condition, the homogeneous nucleation barrier can be overcome, and free organosilicon small particles are formed through homogeneous nucleation in a system.
As a specific example of the present invention, in this example, the reaction time in the reaction step of obtaining the organosilicon nanowire is 24h to 72 h. For example, the reaction time may be 24h, 30h or 72 h. If the reaction time is too short, part of the organosilicon floc which is not completely reacted appears in the system, and the increase of the reaction time does not affect the shape of the final nanowire, but increases the energy consumption of the reaction.
In this embodiment, in step S100 and step S200, all processes are obtained by reaction under the condition of oscillation in a water bath at a preset temperature. The preset temperature may be 25 ℃ to 60 ℃, for example, the preset temperature may be 25 ℃, 30 ℃, 50 ℃ or 60 ℃. If the temperature is too low, the solubility of the surfactant is poor, the surfactant micelle cannot be well dissolved and self-assembled, the action force between the organic silicon source precursor and the surfactant micelle is poor, and the linear organic silicon nanowire cannot be formed by co-assembly. If the temperature is too high, the hydrolysis condensation reaction kinetics of the organic silicon source precursor is increased, and the organic silicon source precursor cannot react with the surfactant micelle, so that the organic silicon source precursor forms independent floccules through self-nucleation in the solvent.
In this embodiment, in step S100 and step S200, the rotation speed of all the processes during oscillation may be 50rpm to 200 rpm. For example, the rotational speed of the oscillation may be 50rpm, 80rpm, 100rpm, or 200 rpm. If the oscillation speed is low, the surfactant micelle obtained by dissolving the surfactant is uneven, so that the acting force between the organic silicon source precursor and the surfactant micelle is poor, and the organic silicon nanowire is difficult to form. If the oscillation speed is high, the surfactant is easy to foam, a uniform and stable surfactant micelle is difficult to form, and the organosilicon nanowire is difficult to obtain.
As a specific example of the present invention, in this example, in step S300, the acidic ethanol solution is a mixed solution prepared by mixing hydrochloric acid and ethanol or a mixed solution prepared by mixing ammonium nitrate and ethanol, wherein a volume of the hydrochloric acid and/or the ammonium nitrate in the mixed solution is 1% to 10% of a volume of the ethanol.
In the preparation method of the mesoporous organosilicon nanowire in the embodiment, the length, the width and the final length-diameter ratio of the mesoporous organosilicon nanowire can be adjusted by simply regulating and controlling the dropping speed, the dosage, the solvent ratio and the like of the organic silicon source precursor only by virtue of the self-assembly effect of the surfactant and the organic silicon source precursor in the solvent.
In addition, the preparation method in the embodiment can prepare the mesoporous organosilicon nanowire with adjustable length-diameter ratio only under the conditions that the water bath is 25-60 ℃ and the oscillation speed is 50-200 rpm, and has the advantages of mild condition, strong controllability, low reaction difficulty and small danger.
In addition, the raw materials of the surfactant, the solvent, the alkali catalyst, the organosilicon coupling agent and the acidic ethanol solution used in the whole preparation method are simple and easy to obtain, so that the preparation method of the embodiment has low cost.
As another specific example of the present invention, in this embodiment, a mesoporous organosilicon nanowire is prepared by the above preparation method. Specifically, the specific surface area of the mesoporous organosilicon nanowire is 500m2/g～1200m2The length of the material is 0.5-3 mu m, the width of the material is 14-120 nm, and the length-diameter ratio of the material is 4-178.
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1:
(1) 1 molar part of deionized water was weighed and added to 1.0X 10-4Adding surfactant CTATos into oscillator with oscillation rate of 80rpm, placing the oscillator in water bath at 30 deg.C, oscillating for 0.5 hr to dissolve surfactant, and adding 6.0 × 10-3And (4) obtaining reaction liquid a by using ammonia water in molar parts.
(2) After 5min, 1, 4-bis (triethoxysilyl) benzene (BTEB) was added dropwise to the reaction solution a prepared in step (1) so that the molar ratio of the surfactant, the organosilane coupling agent and the aqueous ammonia was 1.0: 1.1: and 60, after oscillating reaction for 36 hours, centrifugally cleaning the obtained product for 3 times by using ethanol and deionized water, and then extracting by using an acidic ethanol solution to remove the surfactant to obtain the mesoporous organic silicon nanowire. A transmission electron microscope image of the mesoporous organosilicon nanowire prepared in this example is shown in fig. 2. As can be seen from the transmission electron microscope image, the length of the mesoporous organosilicon nanowire obtained in the embodiment is about 2.5 μm, the width is about 14nm, and the aspect ratio is 178.
Example 2:
compared with the embodiment 1, the dosage of the organosilane coupling agent is only changed, and the molar ratio of the surfactant, the organosilane coupling agent and the ammonia water is 1.0: 2.2: and 60, obtaining the mesoporous organic silicon nanowire by the same other steps. A transmission electron microscope image of the mesoporous organosilicon nanowire prepared in this example is shown in fig. 3. As can be seen from the transmission electron microscope image, the length of the mesoporous organosilicon nanowire obtained in the present embodiment is about 1.5 μm, the width is about 20nm, and the aspect ratio is 70.
Example 3:
compared with the embodiment 1, the dosage of the organosilane coupling agent is only changed, and the molar ratio of the surfactant, the organosilane coupling agent and the ammonia water is 1.0: 4.4: and 60, obtaining the mesoporous organic silicon nanowire by the same other steps. A transmission electron microscope image of the mesoporous organosilicon nanowire prepared in this example is shown in fig. 4. As can be seen from the transmission electron microscope image, the length of the mesoporous organosilicon nanowire obtained in the present embodiment is about 1.2 μm, the width is about 34nm, and the aspect ratio is 35.
Example 4:
compared with the embodiment 1, the dosage of the organosilane coupling agent is only changed, and the molar ratio of the surfactant, the organosilane coupling agent and the ammonia water is 1.0: 9.0: and 60, obtaining the mesoporous organic silicon nanowire by the same other steps. A transmission electron microscope image of the mesoporous organosilicon nanowire prepared in this example is shown in fig. 5. As can be seen from the transmission electron microscope image, the length of the mesoporous organosilicon nanowire obtained in the present embodiment is about 1.0 μm, the width is about 40nm, and the aspect ratio is 25.
Fig. 6 is a distribution diagram of the specific surface area and the pore diameter of the mesoporous organosilicon nanowire prepared in embodiment 4. As can be seen from FIG. 6, the mesoporous organosilicon nanowire has a specific surface area of 990m2Per g, pore size 4.73 nm.
As can be seen from the experimental procedures and results of the above examples 1 to 4, the amount of 1, 4-bis (triethoxysilyl) benzene (BTEB) in the examples 1 to 4 is continuously increased, and as can be seen from the transmission electron microscope image, the length of the finally prepared mesoporous organosilicon nanowire is gradually reduced from 2.5 μm to 1.0 μm, the width is gradually increased from 14nm to 40nm, and the length-diameter ratio range is 25 to 178. That is, the length of the mesoporous organosilicon nanowire decreases as the amount of the organosilane coupling agent increases, and the width of the mesoporous organosilicon nanowire increases as the amount of the organosilane coupling agent increases, according to the method of the present application.
Example 5:
in comparison with example 1, only the proportion of solvent was varied, deionized water was chosen: the volume ratio of ethanol is 18: and 2, obtaining the mesoporous organic silicon nanowire by the same other steps. A transmission electron microscope image of the mesoporous organosilicon nanowire prepared in this example is shown in fig. 7. As can be seen from the transmission electron microscope image, the mesoporous organosilicon nanowire obtained in the present embodiment has a length of about 3.0 μm, a width of about 60nm, and an aspect ratio of 50.
Example 6:
in comparison with example 1, only the proportion of solvent was varied, deionized water was chosen: the volume ratio of ethanol is 17: and 3, obtaining the mesoporous organic silicon nanowire by the same other steps. A transmission electron microscope image of the mesoporous organosilicon nanowire prepared in this example is shown in fig. 8. As can be seen from the transmission electron micrograph, the length is about 1.5 μm, the width is about 100nm, and the aspect ratio is 15.
Example 7:
in comparison with example 1, only the proportion of solvent was varied, deionized water was chosen: the volume ratio of ethanol is 16: and 4, obtaining the mesoporous organic silicon nanowire by the same other steps. A transmission electron microscope image of the mesoporous organosilicon nanowire prepared in this example is shown in fig. 9. As can be seen from the transmission electron micrograph, the length is about 0.5 μm, the width is about 120nm, and the aspect ratio is 4.
As can be seen from the experimental processes and results of the above examples 5 to 7, the ethanol content in the examples 5 to 7 is increased, and with the increase of the ethanol content in the system, the length of the obtained organic silicon nanowire is gradually reduced from 3.0 μm to 0.5 μm, the width is gradually increased from 60nm to 120nm, and the length-diameter ratio is in the range of 4 to 50.
The conditions and results of examples 8 to 14 are shown in the following table:
in examples 8 to 14, the results obtained by changing one of the variables based on example 1 were obtained, and transmission electron micrographs of the mesoporous organosilicon nanowires obtained in examples 8 to 14 are shown in fig. 10 to 16.
Example 8 the reaction temperature was increased compared to example 1, and the transmission electron micrograph of the result obtained in example 8 is shown in fig. 10. Wherein, the length-diameter ratio of the prepared mesoporous organic silicon nanowire is reduced along with the increase of the temperature. In addition, in example 9, when the reaction temperature was further increased to 80 ℃, the nano-silicone particles having a spherical-flocculent result were prepared, as shown in fig. 11. The experiment further shows that the reaction temperature is not too high, and the mesoporous organosilicon nanowire can be obtained under a mild condition.
Transmission electron micrographs of the results obtained in example 1, example 10 and example 11 correspond to fig. 2, fig. 12 and fig. 13, respectively. As can be seen from the experimental processes and results of the above examples 1, 10 and 11, the amount of ammonia water used in the examples 1, 10 and 11 is continuously increased, and as can be seen from the transmission electron microscope images of FIG. 2, FIG. 12 and FIG. 13, the length of the finally prepared mesoporous organosilicon nanowire is gradually increased from 0.5 μm to 2.5 μm, the width is gradually increased from 10nm to 60nm, and the aspect ratio is in the range of 25-178. That is, the aspect ratio of the mesoporous organosilicon nanowire prepared according to the method of the present application increases with the amount of ammonia water.
The transmission electron micrographs of the results of example 12 and example 13 correspond to fig. 14 and fig. 15, respectively. From the experimental processes and results of the above examples 1, 12 and 13, it can be seen that the amount of the surfactant (CTATos) in the examples 1, 12 and 13 is continuously increased, as can be seen from the transmission electron microscope images of fig. 2, 14 and 15, the length of the finally prepared mesoporous organosilicon nanowire is gradually increased from 0.6 μm to 2.5 μm and then decreased to 0.8 μm, the width is gradually increased from 12nm to 25nm, and the aspect ratio range is 32-178. That is, the aspect ratio of the mesoporous organosilicon nanowire prepared according to the method of the present application increases with the increase of the amount of the surfactant (CTATos) but gradually decreases to a certain value.
Example 14 the dropping rate of the silane coupling agent was increased as compared with example 1. The transmission electron micrograph of the result prepared in example 14 is shown in fig. 16. From the results of example 14, it is known that increasing the dropping speed of the silane coupling agent can reduce the aspect ratio of the prepared mesoporous organosilicon nanowire.
As can be seen from the above examples 1 to 14, in the reaction system of the present embodiment, with the difference in the content of the organosilicon coupling agent, the difference in the content of ethanol in the solvent, the difference in the reaction temperature, the difference in the amount of ammonia water or the difference in the dropping speed of the silane coupling agent, the finally obtained organosilicon nanowires have different lengths, widths, aspect ratios and specific surface areas. The length-diameter ratio can be adjusted and changed according to the content of the organosilicon coupling agent, the content of ethanol in the solvent, the amount of ammonia water, the dropping speed of the silane coupling agent, and the reaction temperature, so that the mesoporous organosilicon nanowires with different length-diameter ratios can be easily obtained according to the preparation method of the embodiment.
The length-diameter ratio of the mesoporous organosilicon nanowire prepared by the method can be regulated, and a desired length-diameter ratio range can be obtained by changing experimental conditions, so that the mesoporous organosilicon nanowire can be applied to different fields, such as lithium batteries. The longer the length or the larger the length-diameter ratio of the obtained mesoporous organic silicon nanowire is, the better the electron transmission capability is, and the better the performance of the lithium battery is. The test conditions of the present application can be adjusted to obtain the mesoporous organosilicon nanowire with a high long-diameter ratio.
In addition, the specific surface area of the mesoporous organosilicon nanowire in the application is different along with different reaction conditions, and the specific surface area of the mesoporous organosilicon nanowire has a relatively obvious influence on the adsorption capacity of the organosilicon nanowire. When the specific surface area of the prepared mesoporous organosilicon nanowire is larger, the adsorption capacity of the mesoporous organosilicon nanowire is better. The preparation method can prepare mesoporous structures with different specific surface areas under mild conditions, and increases the application range of the nanowire.
Thus, it should be appreciated by those skilled in the art that while a number of exemplary embodiments of the invention have been illustrated and described in detail herein, many other variations or modifications consistent with the principles of the invention may be directly determined or derived from the disclosure of the present invention without departing from the spirit and scope of the invention. Accordingly, the scope of the invention should be understood and interpreted to cover all such other variations or modifications.
Claims (10)
1. The preparation method of the mesoporous organic silicon nanowire is characterized by comprising the following steps:
adding an alkali catalyst into a solvent in which a surfactant is dissolved, and reacting to obtain a reaction liquid a;
adding an organosilane coupling agent into the reaction liquid a at a preset rate, and reacting to obtain an organosilicon nanowire;
and extracting the organic silicon nanowire by using an acidic ethanol solution to obtain the mesoporous organic silicon nanowire.
2. The method for preparing mesoporous organosilicon nanowires according to claim 1,
the surfactant is selected from hexadecyl trimethyl ammonium p-toluenesulfonate;
the solvent comprises a mixed solvent of water and ethanol, wherein the volume ratio of water to ethanol in the mixed solvent is 20-10: 0 to 10;
the molar ratio of the surfactant to the reaction liquid a is 0.05-0.4: 1.
3. The method for preparing mesoporous organosilicon nanowires according to claim 1,
the alkali catalyst is selected from one or more of ammonia water, triethylamine, sodium hydroxide or triethanolamine;
the pH value of the reaction liquid a is 9-11.
4. The method for preparing mesoporous organosilicon nanowires according to claim 1,
the organosilane coupling agent is selected from one or more of 1, 4-bis (triethoxysilyl) benzene, 1, 2-bis (triethoxysilyl) ethane, 1, 2-bis (triethoxysilyl) ethylene or bis- [3- (triethoxy) propylsilicon ] disulfide.
5. The method for preparing mesoporous organosilicon nanowires according to claim 1,
the molar ratio of the organosilane coupling agent to the reaction solution a was 5.0X 10-5～10.0×10-4：1。
6. The method for preparing mesoporous organosilicon nanowires according to claim 1, wherein,
the preset rate is as follows: 0.003 mL/min-0.096 mL/min.
7. The method for preparing mesoporous organosilicon nanowires according to claim 1, wherein,
the reaction time in the reaction step of obtaining the organic silicon nanowire is 24-72 h.
8. The method for preparing mesoporous organosilicon nanowires according to claim 1, wherein,
all processes before the step of obtaining the organic silicon nanowire through reaction are carried out in a water bath with a preset temperature and under an oscillating condition; wherein the preset temperature is 25-60 ℃, and the rotating speed during oscillation is 50-200 rpm.
9. The method for preparing mesoporous organosilicon nanowires according to claim 1, wherein,
the acidic ethanol solution is a mixed solution prepared by mixing hydrochloric acid and ethanol or a mixed solution prepared by mixing ammonium nitrate and ethanol, wherein the volume of the hydrochloric acid or the ammonium nitrate in the mixed solution is 1-10% of that of the ethanol.
10. The mesoporous organosilicon nanowire prepared by the preparation method according to any one of claims 1 to 9, wherein the mesoporous organosilicon nanowire has a specific surface area of 500m2/g～1200m2The length of the material is 0.5-3 mu m, the width of the material is 14-120 nm, and the length-diameter ratio of the material is 4-178.
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