CN115477306B - Ultrathin silicon dioxide nanotube and preparation method thereof - Google Patents
Ultrathin silicon dioxide nanotube and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of nano material preparation, and discloses an ultrathin silicon dioxide nanotube and a preparation method and application thereof. The method comprises the following steps: (1) Mixing and contacting the carbon nano tube with dimethyl silicone oil to obtain a mixture; (2) Transferring the mixture into sintering equipment to sequentially perform first-stage sintering and second-stage sintering; the weight ratio of the dosage of the simethicone to the dosage of the carbon nano tube is 5-10:1; the conditions of the first stage sintering include: the sintering temperature is 550-600 ℃, and the heat preservation time is 6-8h; the conditions for the second stage sintering include: the sintering temperature is 700-800 ℃, and the heat preservation time is 2-3h. The preparation method is simple, has stable process and is suitable for large-scale production of the silicon dioxide nano tube.
Description
Technical Field
The invention relates to the field of nano material preparation, in particular to an ultrathin silicon dioxide nanotube and a preparation method thereof.
Background
The silica nanotube is a novel functional nonmetallic material with no toxicity, no pollution, high stability, large specific surface area, low thermal expansion coefficient and special morphology. Meanwhile, the biological agent has excellent biological performance and can be widely applied to biomedical fields such as drug delivery systems, tissue regeneration and the like. In addition, the silicon dioxide has good aqueous solution stability, and is nontoxic on a catalyst carrier. The chemical fields such as selective separation and detection of metal ions have received a great deal of attention.
Sun Rong et al (CN 103242684B) uses ethyl orthosilicate as a silicon source and sodium hexadecyl benzenesulfonate as a surfactant, and the reaction process needs to adjust the pH value, heat and stir at constant temperature, and the like, so that the conditions are harsh, the mass production of the silica nanotubes is not facilitated, and the wall thickness of the final finished silica tube is 5-100nm; zheng et al (template method for preparing silica nanotubes and characterization thereof, chemical engineering journal, 2007,58 (10), 2641-2646) used ethyl orthosilicate as the silicon source and D, L-ammonium tartrate as the template, and the impurity peaks in XRD spectra of the finished silica nanotubes indicated that the ammonium tartrate template was not removed completely, and the wall thickness was 100-150nm, and the specific surface area was small. The patent application CN102583398A prepares the silicon dioxide nanotube by taking a metal reducing agent, a carbon nanotube and silicon tetrachloride as raw materials, and the process needs to obtain the silicon dioxide coated carbon nanotube in a reaction kettle in advance and then sinter the silicon dioxide coated carbon nanotube to obtain the silicon dioxide nanotube. The preparation process is complex, a reaction kettle is needed, the large-scale production is not facilitated, and the specific surface area of the prepared product is small.
Therefore, there is an urgent need for a preparation method that can mass-produce silica of high purity and high specific surface area.
Disclosure of Invention
The invention aims to solve the problems of complex preparation process, lower product purity, small specific surface area, harsh preparation conditions and the like of a silicon dioxide nanotube in the prior art, and provides an ultrathin silicon dioxide nanotube and a preparation method thereof.
In order to achieve the above object, the present invention provides a method for preparing ultra-thin silica nanotubes, the method comprising the steps of:
(1) Mixing and contacting the carbon nano tube with dimethyl silicone oil to obtain a mixture;
(2) Transferring the mixture into sintering equipment to sequentially perform first-stage sintering and second-stage sintering;
wherein the weight ratio of the dosage of the simethicone to the dosage of the carbon nano tube is 5-10:1;
the conditions of the first stage sintering include: the sintering temperature is 550-600 ℃, and the heat preservation time is 6-8h;
the conditions for the second stage sintering include: the sintering temperature is 700-800 ℃, and the heat preservation time is 2-3h.
Preferably, the specific process of the step (1) includes: adding dimethyl silicone oil into the carbon nano tube, and then stirring and standing to obtain a mixture;
preferably, the time of the standing is 8-15 hours.
Preferably, in the step (1), the outer tube diameter of the carbon nanotubes is 10-110nm;
preferably, the carbon nanotubes have a length of 5-15 μm.
Preferably, the temperature rising rate of the first-stage sintering is 0.5-2 ℃/min.
Preferably, the temperature rising rate of the second-stage sintering is 0.5-2 ℃/min.
Preferably, in step (2), the sintering atmosphere for the first stage sintering is air;
preferably, the sintering atmosphere of the second stage sintering is air.
Preferably, in step (2), the sintering apparatus is a muffle furnace.
In a second aspect, the invention provides ultra-thin silica nanotubes prepared by the method described above.
Preferably, the outer pipe diameter of the silica nano-tube is 10-70nm;
preferably, the thickness of the tube wall of the ultrathin silicon dioxide nanotube is 3-5nm;
preferably, the specific surface area of the ultrathin silica nanotubes is 200-500m 2 /g。
In a third aspect the present invention provides the use of ultra-thin silica nanotubes as hereinbefore described as a drug carrier.
The invention discloses a simple preparation method of an ultrathin silicon dioxide nanotube, which takes dimethyl silicone oil as a silicon source, takes a carbon nanotube as a template, and is completed through simple stirring, mixing and infiltration and one-step sintering, thereby greatly simplifying the preparation process and conditions. And no auxiliary agents such as a surfactant are needed, so that the residual harm of the auxiliary agents is reduced. The prepared silicon dioxide tube has thinner tube wall, larger inner pore canal and large specific surface area, and can effectively load various medicines.
Drawings
FIG. 1 is a TEM image of the product of example 1;
FIG. 2 is a TEM image of the product of comparative example 2;
FIG. 3 is an XRD pattern for the feedstock carbon nanotubes, the product of example 1, and the product prepared in comparative example 4;
FIG. 4 is a TG plot of the product prepared in example 1.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The inventor of the invention discovers that the silicon dioxide nanotube with excellent performance can be prepared by selecting the carbon nanotube as a template and matching with the simethicone as a silicon source through simple stirring, mixing, infiltration and one-step sintering. Based on this, the present invention has been completed.
In one aspect, the present invention provides a method for preparing ultra-thin silica nanotubes, comprising the steps of:
(1) Mixing and contacting the carbon nano tube with dimethyl silicone oil to obtain a mixture;
(2) Transferring the mixture into sintering equipment to sequentially perform first-stage sintering and second-stage sintering;
wherein the weight ratio of the dosage of the simethicone to the dosage of the carbon nano tube is 5-10:1;
the conditions of the first stage sintering include: the sintering temperature is 550-600 ℃, and the heat preservation time is 6-8h;
the conditions for the second stage sintering include: the sintering temperature is 700-800 ℃, and the heat preservation time is 2-3h.
In a preferred embodiment, the weight ratio of the simethicone to the carbon nanotubes may be in the range of 6-8:1. Specifically, the ratio may be 6:1, 7:1 or 8:1.
Preferably, the specific process of the step (1) includes: adding the simethicone into the carbon nano tube, and then stirring and standing to obtain the mixture.
In the method, the dimethyl silicone oil is added into the carbon nano tube, and then stirring is carried out, so that the carbon nano tube is wrapped in the dimethyl silicone oil for contact, and in order to ensure that the dimethyl silicone oil and the carbon nano tube are in full contact, the stirred material can be still placed.
Further preferably, the time of the standing is 8 to 15 hours. Specifically, it may be 8h, 9h, 10h, 11h, 12h, 13h, 14h or 15h.
In the method of the present invention, in order to further obtain silica nanotubes having a thin wall, a large specific surface area and a uniform particle diameter, preferably, in the step (1), the outer diameter of the carbon nanotubes is 10-110nm; preferably, the carbon nanotubes have a length of 5-15 μm. Further preferably, the outer pipe diameter of the carbon nano-tube is 10-70nm; further preferably, the carbon nanotubes have a length of 7-12 μm.
In the method of the present invention, a sintering method of continuously performing two-stage sintering is preferably used in order to promote the formation of silica nanotubes and to reduce the residual template.
In particular embodiments, the sintering temperature of the first stage sintering may be 550 ℃, 560 ℃, 570 ℃, 580 ℃, 590 ℃, or 600 ℃; the heat preservation time of the sintering in the first stage can be 6 hours, 7 hours or 8 hours.
In particular embodiments, the sintering temperature of the second stage sintering may be 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, or 800 ℃; the heat preservation time of the second-stage sintering can be 2 hours, 2.5 hours or 3 hours.
Further preferably, the temperature rise rate of the first stage sintering is 0.5-2 ℃/min. Specifically, it may be 0.5℃per minute, 1℃per minute, 1.5℃per minute or 2℃per minute.
Further preferably, the rate of temperature rise of the second stage sintering is 0.5-2 ℃/min. Specifically, it may be 0.5℃per minute, 1℃per minute, 1.5℃per minute or 2℃per minute.
Still more preferably, the first stage sintering and the second stage sintering have the same rate of temperature rise.
In a preferred embodiment, in step (2), the sintering atmosphere of the first stage sintering is air.
In a preferred embodiment, the sintering atmosphere for the second stage sintering is air.
Preferably, in step (2), the sintering apparatus is a muffle furnace.
In a second aspect, the invention provides ultra-thin silica nanotubes prepared by the method described above.
Preferably, the outer pipe diameter of the silica nano-tube is 10-70nm;
preferably, the thickness of the tube wall of the ultrathin silicon dioxide nanotube is 3-5nm;
preferably, the specific surface area of the ultrathin silica nanotubes is 200-500m 2 /g。
In a third aspect the present invention provides the use of ultra-thin silica nanotubes as hereinbefore described as a drug carrier.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
The reagents used in the following examples and comparative examples were commercially available products unless otherwise specified.
Example 1
(1) Adding 60g of simethicone into 10g of carbon nano tube (the outer diameter of the tube is 10-50nm, the length is 7-10 mu m), then using a glass cup to gently stir, and then standing for 10h to obtain a mixture;
(2) Pouring the mixture obtained in the step (1) into a corundum boat, and placing the corundum boat in a muffle furnace to sinter in the air atmosphere, wherein the sintering procedure is as follows: heating to 600 ℃ at 1 ℃/min, preserving heat for 6 hours, heating to 800 ℃ at 1 ℃/min, preserving heat for 2 hours, and naturally cooling to obtain the silica nanotube.
Example 2
(1) 70g of simethicone is added into 10g of carbon nano tube (the outer diameter of the tube is 10-70nm, the length is 7-10 mu m), and then the mixture is obtained after the mixture is gently stirred by a glass cup and then is stood for 12 hours;
(2) Pouring the mixture obtained in the step (1) into a corundum boat, and placing the corundum boat in a muffle furnace to sinter in the air atmosphere, wherein the sintering procedure is as follows: heating to 600 ℃ at 2 ℃/min, preserving heat for 8 hours, heating to 750 ℃ at 1 ℃/min, preserving heat for 2 hours, and naturally cooling to obtain the silica nanotube.
Example 3
(1) Adding 80g of simethicone into 10g of carbon nano tube (the outer diameter of the tube is 10-70nm, the length is 7-12 mu m), then using a glass cup to gently stir, and then standing for 12h to obtain a mixture;
(2) Pouring the mixture obtained in the step (1) into a corundum boat, and placing the corundum boat in a muffle furnace to sinter in the air atmosphere, wherein the sintering procedure is as follows: heating to 550 ℃ at a speed of 1 ℃/min, preserving heat for 6 hours, heating to 800 ℃ at a speed of 1 ℃/min, preserving heat for 2 hours, and naturally cooling to obtain the silica nanotube.
Comparative example 1
The procedure described in example 1 was followed, except that in step (1), the same weight of tetraethyl orthosilicate was used instead of simethicone.
Comparative example 2
The procedure described in example 1 was followed, except that in step (1), the amount of simethicone was 40g.
Comparative example 3
The procedure described in example 1 was followed, except that in step (1), the amount of simethicone was 120g.
Comparative example 4
The procedure was followed as described in example 1, except that the sintering procedure was as follows: heating to 600 ℃ at 2 ℃/min, preserving heat for 10 hours, and naturally cooling to obtain the silica nanotube.
Test example 1
The products prepared in examples 1-3 and comparative example 2 were characterized by TEM, wherein the characterization of the product prepared in example 1 is shown in fig. 1 and the characterization of the product prepared in comparative example 2 is shown in fig. 2.
From the figure, the product prepared in example 1 has a clear tubular morphology and is uniformly dispersed. And combining with Nano Measure software to obtain the silica nanotube with the outer diameter of 10-70nm and the wall thickness of 3-5nm. The TEM characterization results of examples 2-3 are similar to those of example 1, and thus are not described in detail.
In comparative example 2, because the addition amount of the methyl silicone oil is small, the methyl silicone oil does not completely infiltrate the surface of the carbon nanotube in the same infiltration time, and the morphology defect of the finally formed silicon dioxide nanotube is not obvious in a tubular structure.
Test example 2
XRD was used to characterize the starting carbon nanotubes, the product of example 1, and the product prepared in comparative example 4, the results are shown in fig. 3.
As can be seen from FIG. 3 (a), the (002) peak at 26℃2. Theta. Is a characteristic peak of MCNTs; in fig. 3 (b) is the XRD spectrum peak of the product prepared in comparative example 4, and the characteristic peak (002) of MCNTs is still present in the product obtained by performing the first stage sintering (i.e. comparative example 4), which indicates that the MCNTs template sintering still remains after the one-step combustion. In fig. 3 (c) is the XRD spectrum peak of the product of example 1, it can be seen that the prepared silica nanotube has an amorphous structure.
Test example 3
The product prepared in example 1 was characterized using a thermogravimetric analyzer and the results are shown in figure 4.
From the graph, the TG curve is divided into three temperature gradients in the air atmosphere, the first being in the range 20-265 ℃, the second being in the range 504-644 ℃, and the third being in the range 724-1000 ℃. It can be seen that the MCNTs have constant quality after three sintering stages and two weight loss stages. It is stated that the carbon nanotubes can be completely removed after continuous high temperature sintering.
Test example 4
The products obtained in examples 1 to 3 and comparative examples 1 to 4 were examined by BET, and as a result, it was found that the products prepared in examples had a mainly mesoporous pore structure, and the specific surface data are shown in Table 1.
TABLE 1
| Numbering device | Specific surface area m 2 /g |
| Example 1 | 440.43 |
| Example 2 | 430.72 |
| Example 3 | 428.60 |
| Comparative example 1 | 219.09 |
| Comparative example 2 | 221.03 |
| Comparative example 3 | 330.32 |
| Comparative example 4 | 340.27 |
As can be seen from Table 1, the mesoporous silica nanotubes with larger specific surface area can be prepared by the method of the present invention.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (6)
1. A method for preparing ultra-thin silica nanotubes, the method comprising the steps of:
(1) Mixing and contacting the carbon nano tube with dimethyl silicone oil to obtain a mixture;
(2) Transferring the mixture into sintering equipment to sequentially perform first-stage sintering and second-stage sintering;
wherein the weight ratio of the dosage of the simethicone to the dosage of the carbon nano tube is 5-10:1;
the conditions of the first stage sintering include: the sintering temperature is 550-600 ℃, and the heat preservation time is 6-8h;
the conditions for the second stage sintering include: sintering at 700-800 deg.c for 2-3 hr;
the specific process of the step (1) comprises the following steps: adding dimethyl silicone oil into the carbon nano tube, and then stirring and standing to obtain a mixture;
the standing time is 8-15h;
in the step (1), the outer pipe diameter of the carbon nano-tube is 10-110nm;
the length of the carbon nano tube is 5-15 mu m.
2. The method of claim 1, wherein the first stage sintering has a ramp rate of 0.5-2 ℃/min.
3. The method of claim 1, wherein the second stage sintering has a ramp rate of 0.5-2 ℃/min.
4. The method of preparing ultra-thin silica nanotubes according to claim 1, wherein in step (2), the sintering atmosphere of the first stage sintering is air.
5. The method of preparing ultra-thin silica nanotubes according to claim 4, wherein the sintering atmosphere of the second stage sintering is air.
6. The method of preparing ultra-thin silica nanotubes according to claim 1 or 2, wherein in step (2), the sintering equipment is a muffle furnace.
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