CN111892037A - Porous nano-wire carbon material and super-assembly preparation method thereof - Google Patents
Porous nano-wire carbon material and super-assembly preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of preparation of carbon materials, and provides a porous nano-wire carbon material and a super-assembly preparation method thereof. The preparation method of the porous nanowire material is environment-friendly, strong in sustainability, wide in raw material source and easy to industrialize, the obtained porous nanowire carbon material has a larger inner cavity structure and better biocompatibility, so that the porous nanowire carbon material can be used as an excellent carrier for releasing drugs under temperature control or becomes an important structural unit in an energy storage system to obtain higher energy density than a conventional porous structure, and the porous nanowire material has chemical inertness and can be widely applied to the fields of catalysis, energy storage, drug storage and release and the like.
Description
Technical Field
The invention belongs to the field of carbon material preparation, and particularly relates to a porous nanowire carbon material and a super-assembly preparation method thereof.
Background
In recent years, the design and synthesis of porous structured nanomaterials (such as silica, metal oxides, organic polymers, and carbon materials) have received much attention in both basic research and practical applications. Because of the advantages of low density, high specific surface area, high porosity and the like, the nano-particles show good application prospects in the fields of catalysis, drug storage and release, energy storage and the like. Among the porous nanoparticles with different morphologies reported in these studies, anisotropic nanoparticles, such as cage-like, bowl-like or other morphologies of non-spherical structures, tend to produce unique application effects due to the combination of porous structures and anisotropic structures. For example, anisotropic nanoparticles can be used as excellent carriers for temperature controlled release of drugs, or as an important building block in energy storage systems to achieve higher energy densities than conventional porous structures. The porous carbon material has been widely studied because of its many excellent characteristics, such as large lumen structure, biocompatibility, chemical inertness, high conductivity, etc.
Although considerable work has been devoted to the development of such materials, there are only a few methods reported in the literature for the preparation of anisotropic porous nanoparticles, such as freeze-drying or freeze-etching, anisotropic coating, and template-etch induction. Moreover, most anisotropic nanomaterials are limited to silica, polymer emulsions, or metal oxides, and the synthetic routes for these materials are often lengthy and require the use of toxic reagents.
Disclosure of Invention
The present invention is made to solve the above problems, and an object of the present invention is to provide a porous nanowire carbon material and a super-assembly preparation method thereof.
The invention provides a super-assembly preparation method of a porous nano-wire carbon material, which is characterized by comprising the following steps: step 1, adding 1.2-1.8 mol/L acid solution, ribose and F127 into a polytetrafluoroethylene container, stirring, adding mesitylene, and continuing to react to generate columnar micelles; step 2, after the stirring in the step 1 is finished, adding PSSMA into a polytetrafluoroethylene container, stirring for a period of time, then carrying out hydrothermal reaction to obtain a nanowire carbon material, and step 3, washing and filtering the nanowire carbon material by using water and ethanol, and removing F127 in the nanowire carbon material to obtain the porous nanowire carbon material, wherein the mass ratio of ribose, F127, PSSMA and mesitylene is 6: 2-4: 0.08-0.25: 0.01-0.25, and the feeding ratio of the acid solution to the ribose is 50ml-70ml:6 g.
In the super-assembly preparation method of the porous nano-wire carbon material provided by the invention, the super-assembly preparation method also has the following characteristics: wherein the concentration of the mesitylene is 0.16g/L-4.17 g/L.
The super-assembly preparation method of the porous nano-wire carbon material provided by the invention also has the following characteristics: wherein the concentration of PSSMA is 1.33g/L-4.17 g/L.
The super-assembly preparation method of the porous nano-wire carbon material provided by the invention also has the following characteristics: wherein the acid solution is sulfuric acid solution or hydrochloric acid solution.
The super-assembly preparation method of the porous nano-wire carbon material provided by the invention also has the following characteristics: among them, the concentration of the sulfuric acid solution is 1.4mol/L to 1.8mol/L, more preferably 1.5mol/L to 1.6 mol/L.
The super-assembly preparation method of the porous nano-wire carbon material provided by the invention also has the following characteristics: among them, the concentration of the hydrochloric acid solution is 1.2mol/L to 1.6mol/L, more preferably 1.3mol/L to 1.5 mol/L.
The super-assembly preparation method of the porous nano-wire carbon material provided by the invention also has the following characteristics: wherein the temperature of the hydrothermal reaction is 130-160 ℃, more preferably 135-145 ℃, and the time is 2-24 h, more preferably 3-5 h.
The invention also provides a porous nano-wire carbon material, which is prepared by the super-assembly preparation method of the porous nano-wire carbon material provided by the invention and has the following characteristics: the porous nanocarbon material is linear, and the outer surface and the inner part of the porous nanocarbon material are provided with mesoporous pore canals parallel to the axis of the porous nanocarbon material.
The porous nano-wire carbon material provided by the invention also has the following characteristics: wherein, the length of the porous nano-wire carbon material is 600nm-5 μm, the ratio of the length to the diameter is 3-50, and the aperture of the mesoporous pore canal is 3nm-5 nm.
Action and Effect of the invention
According to the super-assembly preparation method of the porous nano carbon material, acid solution with the concentration of 1.2-1.8 mol/L, ribose and F127 are added into a polytetrafluoroethylene container to be stirred, mesitylene is added to be continuously stirred to generate columnar micelles, poly (4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA) is added into the polytetrafluoroethylene container to be continuously stirred, the polytetrafluoroethylene container is placed into a hydrothermal kettle to carry out hydrothermal reaction, the nano carbon material is obtained through super-assembly, the nano carbon material is fully washed with water and ethanol, and is subjected to suction filtration to remove the F127, so that the porous nano carbon material is obtained.
The added poly (4-styrenesulfonic acid-copolymerization-maleic acid) sodium salt (PSSMA) is adsorbed on the surface of the columnar micelle, so that the surface energy of the columnar micelle is effectively reduced, and the micelle is easy to assemble into a longer nanowire.
In addition, the mass ratio of ribose, F127, poly (4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA), and mesitylene was 6: 2-4: 0.08-0.25: 0.01-0.25, so that the obtained porous nano-wire carbon material has ordered mesopores.
In addition, the feeding ratio of the acid solution to the ribose is 50ml-70ml:6g, so that the porous nanowire carbon material with a good appearance is obtained.
The porous nano-wire carbon material obtained by the invention is linear, the outer surface and the inner part of the porous nano-wire carbon material are provided with pore channels parallel to the axis of the porous nano-carbon material, so that the material has more cavities to improve the loading capacity, has good biocompatibility, and can be used as an excellent carrier for controlling and releasing drugs by temperature or an important structural unit in an energy storage system to obtain higher energy density than a conventional porous structure.
In conclusion, the super-assembly preparation method of the porous nanowire carbon material provided by the invention has the advantages of wide raw material source, environmental friendliness, strong sustainability and easiness in industrialization, the outer surface and the inner part of the obtained porous nanowire carbon material are provided with pore channels parallel to the axis of the porous nanowire carbon material, and the material has chemical inertness and has wide application prospects in the fields of catalysis, energy storage, drug storage and release and the like.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a porous nanowire carbon material obtained in example 1 of the present invention;
FIG. 2 is a high magnification SEM image of the porous nanowire carbon material obtained in example 1 of the present invention;
FIG. 3 is a higher magnification SEM image of the porous nanowire carbon material obtained in example 1 of the present invention;
FIG. 4 is a Transmission Electron Microscope (TEM) image of the porous nanowire carbon material obtained in example 1 of the present invention;
FIG. 5 is a high magnification TEM image of the porous nanowire carbon material obtained in example 1 of the present invention;
fig. 6 is a nitrogen adsorption and desorption curve of the porous nanowire carbon material obtained in example 1 of the present invention;
FIG. 7 is a pore size distribution diagram of the porous nanowire carbon material obtained in example 1 of the present invention;
FIG. 8 is a small angle X-ray scattering plot of the porous nanowire carbon material obtained in example 1 of the present invention;
FIG. 9 is an SEM image of a porous nanowire carbon material obtained in example 2 of the present invention;
FIG. 10 is an SEM image of a porous nanowire carbon material obtained in example 3 of the present invention;
FIG. 11 is an SEM image of a porous nanowire carbon material obtained in example 4 of the present invention;
fig. 12 is an SEM image of the porous nanowire carbon material obtained in example 5 of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the porous nano-wire carbon material and the super-assembly preparation method thereof of the invention are specifically described below with reference to the embodiments and the accompanying drawings.
In the examples of the present invention, the reagents and raw materials were purchased from commercial sources except the materials which were prepared in the laboratory.
F127 was purchased from Sigma-Aldrich under the trade designation P2443-250 g; polymer poly (4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA) was purchased from Aladdin, Inc. under the designation P107093-25g, with a 1:1 molar ratio of 4-styrenesulfonic acid to maleic acid; ribose was purchased from Aladdin under a trade designation of R104820-500g, and 1,3, 5-mesitylene was purchased from Aladdin under a trade designation of T105015-100 ml.
< example 1>
Transferring 5.0mL of concentrated sulfuric acid into 55mL of deionized water to obtain an acid solution with the concentration of 1.53M, adding the obtained acid solution into a 100mL polytetrafluoroethylene lining (hereinafter referred to as lining), adding 6.0g of ribose and 3.0g of F127 into the lining, stirring for 4 hours, adding 200 mu L of mesitylene into the lining, stirring for 8 hours, adding 170mg of PSSMA into the lining, and stirring for 12 hours. The lining is then placed in a stainless steel hydrothermal kettle and reacted in an oven at 140 ℃ for 4 hours. And taking the nanowire carbon material obtained by the reaction out of the lining, washing with water and ethanol respectively, carrying out suction filtration, removing F127, and drying to obtain the porous nanowire carbon material.
The porous nanowire carbon material obtained in the present example was tested, and the test results are shown in fig. 1-8.
FIG. 1 is a Scanning Electron Microscope (SEM) image of the porous nanowire carbon material obtained in the present example; FIG. 2 is a high magnification SEM image of the porous nanowire carbon material obtained in the present example; FIG. 3 is a higher magnification SEM image of the porous nanowire carbon material obtained in the present example; FIG. 4 is a Transmission Electron Microscope (TEM) image of the porous nanowire carbon material obtained in the present example; fig. 5 is a high magnification TEM image of the porous nanowire carbon material obtained in this example.
As shown in fig. 1-5, the prepared porous nanowire carbon material has a linear structure, and has rich pore channels on the outer surface and inside, the average length of the porous nanowire carbon material is 4182 nm, the diameter of the porous nanowire carbon material is 114 nm, and the ratio of the length to the diameter of the porous nanowire carbon material is 36.7.
Fig. 6 is a nitrogen adsorption and desorption curve of the porous nanowire carbon material obtained in the present embodiment; fig. 7 is a pore size distribution graph of the porous nanowire carbon material calculated from the data of fig. 6.
As shown in fig. 6 and 7, the nitrogen adsorption and desorption curves of the porous nanowire carbon material have obvious hysteresis loops, which indicate the existence of mesoporous channels, and the diameter of the mesoporous channels calculated by a Barrett-Joyner-halenda (bjh) model is about 3.8 nm.
Fig. 8 is a small-angle X-ray scattering diagram of the porous nanowire carbon material obtained in the present example.
As shown in fig. 8, a sharp peak appears on the small-angle X-ray scattering diagram, indicating that the mesoporous channels on the porous nanowire carbon material are ordered.
< example 2>
Transferring 5.0mL of concentrated sulfuric acid into 55mL of deionized water to obtain an acid solution with the concentration of 1.53M, adding the obtained acid solution into a 100mL polytetrafluoroethylene lining (hereinafter referred to as lining), adding 6.0g of ribose and 3.0g of F127 into the lining, stirring for 4 hours, adding 80 mu L of mesitylene into the lining, stirring for 8 hours, adding 100mg of PSSMA into the lining, and stirring for 12 hours. The lining is then placed in a stainless steel hydrothermal kettle and reacted in an oven at 140 ℃ for 4 hours. And taking the nanowire carbon material obtained by the reaction out of the lining, washing with water and ethanol respectively, carrying out suction filtration, removing F127, and drying to obtain the porous nanowire carbon material.
The porous nanowire carbon material obtained in this example was tested, and the test results are shown in fig. 9.
Fig. 9 is an SEM image of the porous nanowire carbon material obtained in the present example.
As shown in fig. 9, the porous nanowire carbon material prepared in this embodiment has a linear structure, the average length of the porous nanowire carbon material is 924 nm, the diameter of the porous nanowire carbon material is 209 nm, the ratio of the length to the diameter of the porous nanowire carbon material is 4.4, and the diameter of a pore channel calculated by a Barrett-Joyner-halenda (bjh) model is about 3.8 nm.
< example 3>
Transferring 5.0mL of concentrated sulfuric acid into 55mL of deionized water to obtain an acid solution with the concentration of 1.53M, adding the obtained acid solution into a 100mL polytetrafluoroethylene lining (hereinafter referred to as lining), adding 6.0g of ribose and 3.0g of F127 into the lining, stirring for 4 hours, adding 150 mu L of mesitylene into the lining, stirring for 8 hours, adding 100mg of PSSMA into the lining, and stirring for 12 hours. The lining is then placed in a stainless steel hydrothermal kettle and reacted in an oven at 140 ℃ for 4 hours. And taking the nanowire carbon material obtained by the reaction out of the lining, washing with water and ethanol respectively, carrying out suction filtration, removing F127, and drying to obtain the porous nanowire carbon material.
The porous nanowire carbon material obtained in this example was tested, and the test results are shown in fig. 10.
Fig. 10 is an SEM image of the porous nanowire carbon material obtained in the present example.
As shown in fig. 10, the porous nanowire carbon material prepared in this example has a linear structure, the average length of the porous nanowire carbon material is 1478 nm, the diameter of the porous nanowire carbon material is 217 nm, the ratio of the length to the diameter of the porous nanowire carbon material is 6.8, and the diameter of a pore channel calculated by a Barrett-Joyner-halenda (bjh) model is about 3.8 nm.
< example 4>
Transferring 5.0mL of concentrated sulfuric acid into 55mL of deionized water to obtain an acid solution with the concentration of 1.53M, adding the obtained acid solution into a 100mL polytetrafluoroethylene lining (hereinafter referred to as lining), adding 6.0g of ribose and 3.0g of F127 into the lining, stirring for 4 hours, adding 200 mu L of mesitylene into the lining, stirring for 8 hours, adding 120mg of PSSMA into the lining, and stirring for 12 hours. The lining is then placed in a stainless steel hydrothermal kettle and reacted in an oven at 140 ℃ for 4 hours. And taking the nanowire carbon material obtained by the reaction out of the lining, washing with water and ethanol respectively, carrying out suction filtration, removing F127, and drying to obtain the porous nanowire carbon material.
The porous nanowire carbon material obtained in this example was tested, and the test result is shown in fig. 11.
Fig. 11 is an SEM image of the porous nanowire carbon material obtained in example 4 of the present invention.
As shown in fig. 11, the porous nanowire carbon material prepared in this example has a linear structure, the average length of the porous nanowire carbon material is 1729 nm, the diameter of the porous nanowire carbon material is 217 nm, the ratio of the length to the diameter of the porous nanowire carbon material is 11.1, and the diameter of a pore channel calculated by a Barrett-Joyner-halenda (bjh) model is about 3.8 nm.
< example 5>
Transferring 5.0mL of concentrated sulfuric acid into 55mL of deionized water to obtain an acid solution with the concentration of 1.53M, adding the obtained acid solution into a 100mL polytetrafluoroethylene lining (hereinafter referred to as lining), adding 6.0g of ribose and 3.0g of F127 into the lining, stirring for 4 hours, adding 200 mu L of mesitylene into the lining, stirring for 8 hours, adding 200mg of PSSMA into the lining, and stirring for 12 hours. The lining is then placed in a stainless steel hydrothermal kettle and reacted in an oven at 140 ℃ for 4 hours. And taking the nanowire carbon material obtained by the reaction out of the lining, washing with water and ethanol respectively, carrying out suction filtration, removing F127, and drying to obtain the porous nanowire carbon material.
The porous nanowire carbon material obtained in this example was tested, and the test results are shown in fig. 12.
Fig. 12 is an SEM image of the porous nanowire carbon material obtained in example 5 of the present invention.
As shown in fig. 12, the porous nanowire carbon material prepared in this example has a linear structure, the average length of the porous nanowire carbon material is 4239 nm, the diameter of the porous nanowire carbon material is 109 nm, the ratio of the length to the diameter of the porous nanowire carbon material is 38.9, and the diameter of a pore passage calculated by a Barrett-Joyner-halenda (bjh) model is about 3.8 nm.
Effects and effects of the embodiments
According to the super-assembly preparation method of the porous nano carbon material, acid solution with the concentration of 1.2-1.8 mol/L, ribose and F127 are added into a polytetrafluoroethylene container to be stirred, and then mesitylene is added to be continuously stirred, so that columnar micelles are generated. After the reaction is finished, adding poly (4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA) into a polytetrafluoroethylene container, stirring for a period of time, then putting the polytetrafluoroethylene container into a hydrothermal kettle for hydrothermal reaction, performing super-assembly to obtain a nanowire carbon material, fully washing and leaching the nanowire carbon material with water and ethanol, and removing F127 to obtain the porous nanowire carbon material.
The added poly (4-styrenesulfonic acid-copolymerization-maleic acid) sodium salt (PSSMA) is adsorbed on the surface of the columnar micelle, so that the surface energy of the columnar micelle is effectively reduced, and the micelle is easy to assemble into a longer nanowire.
In addition, the mass ratio of ribose, F127, poly (4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA), and mesitylene was 6: 2-4: 0.08-0.25: 0.01-0.25, and the obtained porous nanowire carbon material has ordered mesopores.
In addition, the feeding ratio of the acid solution to the ribose is 50ml-70ml:6g, so that the porous nanowire carbon material with a good appearance is obtained.
As can be seen from examples 1, 4 and 5, the higher the concentration of PSSMA in the reaction system, the longer the length of the porous nanowire carbon material, for example, the amount of PSSMA used in example 1 was 170mg, the length of the porous nanowire carbon material was 4182 nm, the amount of PSSMA used in example 4 was 120mg, the length of the porous nanowire carbon material was 1729 nm, the amount of PSSMA used in example 5 was 200mg, and the length of the porous nanowire carbon material was 4239 nm.
It can be seen from examples 2 and 3 that the length of the porous nanowire material is longer as the concentration of mesitylene in the reaction system is higher, for example, 80. mu.L of mesitylene is used in example 2, 924 nm of the porous nanowire carbon material is used in example 3, 150. mu.L of mesitylene is used in example 3, and 1478 nm of the porous nanowire carbon material is used.
The porous nano-wire carbon material obtained in the embodiment is linear, and the outer surface and the inner part of the porous nano-wire carbon material are provided with pore channels parallel to the axis of the porous nano-carbon material, so that the material has more cavities to improve the loading capacity, has good biocompatibility, can be used as an excellent carrier for controlling and releasing drugs by temperature, or can be used as an important structural unit in an energy storage system to obtain higher energy density than a conventional porous structure.
In summary, the super-assembly preparation method of the porous nanowire carbon material provided by the embodiment has the advantages of wide raw material source, environmental friendliness, strong sustainability and easiness in industrialization, the outer surface and the inner part of the obtained porous nanowire carbon material are provided with pore channels parallel to the axis of the porous nanowire carbon material, and the material has chemical inertness and can be widely applied to the fields of catalysis, energy storage, drug storage and release and the like.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (9)
1. A super-assembly preparation method of a porous nanowire carbon material is characterized by comprising the following steps:
step 1, adding 1.2mol/L-1.8mol/L acid solution, ribose and F127 into a polytetrafluoroethylene container for stirring, adding mesitylene for continuous stirring to generate columnar micelles,
step 2, after the stirring in the step 1 is finished, adding PSSMA into the polytetrafluoroethylene container for stirring for a period of time, then carrying out hydrothermal reaction to obtain the nano-wire carbon material,
step 3, washing and filtering the nanowire carbon material with water and ethanol to remove the F127 in the nanowire carbon material to obtain a porous nanowire carbon material,
wherein the mass ratio of the ribose, the F127, the PSSMA and the mesitylene is 6: 2-4: 0.08-0.25: 0.01-0.25,
the feeding ratio of the acid solution to the ribose is 50ml-70ml:6 g.
2. The method for preparing the porous nanowire carbon material in a super-assembly manner according to claim 1, wherein the method comprises the following steps:
wherein the concentration of the mesitylene is 0.16g/L-4.17 g/L.
3. The method for preparing the porous nanowire carbon material in a super-assembly manner according to claim 1, wherein the method comprises the following steps:
wherein the concentration of the PSSMA is 1.33g/L-4.17 g/L.
4. The method for preparing the porous nanowire carbon material in a super-assembly manner according to claim 1, wherein the method comprises the following steps:
wherein the acid solution is a sulfuric acid solution or a hydrochloric acid solution.
5. The method for preparing the porous nanowire carbon material in a super-assembly manner according to claim 4, wherein the method comprises the following steps:
wherein the concentration of the sulfuric acid solution is 1.4-1.8 mol/L.
6. The method for preparing the porous nanowire carbon material in a super-assembly manner according to claim 4, wherein the method comprises the following steps:
wherein the concentration of the hydrochloric acid solution is 1.2-1.6 mol/L.
7. The method for preparing the porous nanowire carbon material in a super-assembly manner according to claim 1, wherein the method comprises the following steps:
wherein the temperature of the hydrothermal reaction is 130-160 ℃, and the time is 2-24 h.
8. A porous nanowire carbon material, characterized in that the porous nanocarbon material is prepared by the super-assembly preparation method of the porous nanowire carbon material according to any one of claims 1 to 7,
the porous nanocarbon material is linear, and mesoporous pore channels parallel to the axis of the porous nanocarbon material are formed in the outer surface and the inner portion of the porous nanocarbon material.
9. The porous nanowire carbon material of claim 8, wherein:
the length of the porous nanowire carbon material is 600nm-5 mu m, the ratio of the length to the diameter is 3-50, and the pore diameter of the mesoporous pore channel is 3nm-5 nm.
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