CN115744880A - Method for preparing carbon nano tube based on bifidobacterium lactis - Google Patents
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- CN115744880A CN115744880A CN202211435614.3A CN202211435614A CN115744880A CN 115744880 A CN115744880 A CN 115744880A CN 202211435614 A CN202211435614 A CN 202211435614A CN 115744880 A CN115744880 A CN 115744880A
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Abstract
The invention provides a method for preparing a carbon nano tube based on bifidobacterium lactis. The method comprises the following steps: putting the bifidobacterium lactis freeze-dried powder matched with the carrier into a tube furnace, heating to 750-900 ℃ at a preset heating rate under protective gas, preserving heat for a preset time, and naturally cooling to prepare the carbon nano tube. The invention is prepared by a one-step annealing method, has simple process and low cost, replaces the traditional complex and high-cost preparation process, and is more suitable for large-scale commercial application.
Description
Technical Field
The invention relates to the technical field of carbon nanotube preparation, in particular to a method for preparing a carbon nanotube based on bifidobacterium lactis.
Background
Carbon nanotubes, also known as buckytubes, are one-dimensional quantum materials with a special structure (radial dimension is nanometer magnitude, axial dimension is micrometer magnitude, both ends of the tube are basically sealed). The current methods for preparing carbon nanotubes mainly include arc discharge methods, laser evaporation methods and chemical vapor deposition methods.
The arc discharge method has the advantages of high carbon nanotube production rate, simple process parameter setting required in the experimental process, straight carbon nanotube obtained by growth, good crystallinity and the like, but has the following defects: the temperature requirement of the growing carbon nano tube is high, the equipment required for growing the carbon nano tube is very complex, and the grown carbon nano tube has obvious defects; the catalyst is easy to sinter with the by-products generated in the growth process, such as amorphous carbon, graphite particles, fullerene and other impurities, and is not beneficial to separation and purification; the preparation cost is high, and the large-scale and industrial production is not facilitated.
The laser evaporation method is to place the target material made of metal catalyst/graphite powder in a quartz tube reactor, and the quartz tube is placed in a horizontal heating furnace. When the furnace temperature was raised to 1473K, inert gas was charged into the tube and a laser was focused on the graphite target. The graphite target generates gaseous carbon under the laser irradiation, and the gaseous carbon grows single-walled carbon nanotubes under the action of the catalyst. The yield of the carbon nano tube is increased along with the shortening of the time interval of the laser pulse, and the tube diameter of the carbon nano tube can also be controlled by adjusting the power of the laser pulse. However, there are disadvantages in that the purity of the prepared carbon nanotubes is low, the production efficiency is low, the product is easily tangled, and the production cost is expensive.
The chemical vapor deposition method has the advantages of low cost, high purity, large yield, easy control of experimental conditions and the like, and the size of the carbon nano tube is controlled by the size of catalyst particles, so the production cost is low and the applicability is strong. Is the most promising method for preparing high-quality carbon nanotubes in large quantities. Therefore, this method has received high attention and is widely used. However, the carbon nanotubes prepared by the chemical vapor deposition method also have the disadvantages of long length, non-uniform diameter and low graphitization degree.
In addition to the above methods, shijian Hua team uses some natural biomass as a catalyst precursor, natural gas as a carbon source, and a CVD process to prepare carbon nanotubes. Most of the methods can obtain carbon nanotube arrays with uniform tube diameter distribution, but the natural substances need to be treated for not less than six hours before firing. Natural gas as a carbon source does not fundamentally solve the problem of carbon nanotube production. However, the method has a disadvantage of a long operation time, and the problem is not solved from the aspect of carbon source.
The thermal cracking-catalytic modification method (two-stage method) adopted by Lanmeichen team can obtain high-value product carbon nano tube while processing waste plastics, and has the characteristics of cheap and easily available raw materials, economy and environmental protection, but the existing reactor can not process waste plastics in large batch and continuously produce carbon nano tube; waste plastics generated in life are various in types and complex in composition, and can have great influence on the appearance and quality of the carbon nano tube, so that the practical application of the method is hindered; the excessive interaction between the active components of the catalyst and the carrier can cause the sintering agglomeration of the catalyst, so that the diameter of the carbon nano tube is too large, and the weak interaction can influence the catalytic effect to reduce the yield of the carbon nano tube; the carbon nano tube prepared by cracking the plastic is not practically applied because of difficult separation from the catalyst, other carbon impurities contained in the product and the like.
Disclosure of Invention
In view of the above-mentioned technical problems, a method for preparing carbon nanotubes based on bifidobacterium lactis is provided. The technical means adopted by the invention are as follows:
a preparation method of carbon nano-tubes based on bifidobacterium lactis comprises the following steps:
putting the bifidobacterium lactis freeze-dried powder matched with the carrier into a tube furnace, heating to 750-900 ℃ at a preset heating rate under protective gas, preserving heat for a preset time, and naturally cooling to prepare the carbon nano tube.
Further, the carrier is maltose.
Further, the mass of the bifidobacterium lactis freeze-dried powder is 10g.
Further, the maximum temperature of the temperature rise was 850 ℃.
Further, the heating rate is 9.5-10.5 ℃/min.
Further, the heat preservation time is 2-2.5 h.
Further, the protective gas is nitrogen.
Further, the gas flow rate is 55-60 ml/min.
The invention has the following advantages:
1. the invention uses the bifidobacterium lactis as a precursor for preparing the multi-wall carbon nano tube for the first time and is applied to material science. Based on the intrinsic characteristics of the bifidobacterium lactis as prokaryotic cells (no complex organelles), the method provides a basis for a hollow structure. The bifidobacterium lactis cell wall is composed of hexagonal cyclic peptidoglycan (similar to a graphene structure), and provides a basis for graphitization. The prepared bifidobacterium lactis derived carbon nano tube has rich intrinsic defects and nitrogen atom doping, and can effectively improve the electrocatalytic activity.
2. The bifidobacterium lactis is taken as a biomass material, accords with the development trend of environmental protection, and has lower cost and wide source.
3. The preparation method has the advantages of simple process and low cost by adopting a one-step annealing method, replaces the traditional complex and high-cost preparation process, and is more suitable for large-scale commercial application.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the description of the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a scanning electron microscope image of annealed Bifidobacterium lactis carbon nanotubes of the present invention, and (a) to (d) are respectively 100nm, 400nm, 1 μm and 600 nm.
FIG. 2 is a high resolution-projection electron microscope test chart of the present invention.
FIG. 3 is an X-ray diffraction test chart of the present invention.
FIG. 4 is a Raman spectrum test chart of the present invention.
FIG. 5 is an X-ray photoelectron spectroscopy (XPS) of the present invention, wherein (a) (B) are X-ray photoelectron spectroscopy (XPS) of conventional NS-850 and B-850 prepared according to the present invention, respectively.
FIG. 6 is a diagram of the energy spectrum analysis of the present invention, in which a) is a diagram of the analysis of the composition and content of carbon nanotubes prepared by a normal route, and b) is a diagram of the analysis of the composition and content of biomass carbon nanotubes prepared by the present invention.
FIG. 7 is an electrochemical test chart of the present invention, wherein (a) is a cyclic voltammogram test; and (b) linear voltammetry scanning test.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The embodiment provides a method for preparing carbon nanotubes based on bifidobacterium lactis, which comprises the following steps:
and (3) putting the bifidobacterium lactis freeze-dried powder into a tube furnace, heating to 750-900 ℃ at a preset heating rate under protective gas, preserving heat for a preset time, and naturally cooling to obtain the carbon nano tube. In this embodiment, maltose is used as the carrier, which is beneficial for the fungi to maintain morphological and structural features. Through a plurality of experiments, only maltose can realize the function in the invention. During the heating process, a proper amount of maltose is placed first, and then the bifidobacterium lactis freeze-dried powder is placed.
The highest annealing temperature, the heating rate, the heat preservation time and the cooling rate in the annealing process have important influences on the characteristics of the carbon nano tube such as appearance, intrinsic defects, heteroatom doping and the like, and further the physical, chemical, mechanical, thermodynamic and other properties of the carbon nano tube can be influenced. The specific influence of the four factors on the performance is one of the difficulties in preparing efficient CNTs. Therefore, the invention obtains that the heating rate is 9.5-10.5 ℃/min, the heat preservation time is 2-2.5 h, the gas flow rate is 55-60 ml/min as an optional range through a plurality of experiments, and the optimal annealing maximum temperature in the preparation process is 850 ℃. The heating rate was 10 ℃/min. The heat preservation time is 2h. The protective gas is nitrogen, and the nitrogen is beneficial to doping nitrogen atoms of the product, so that the electrocatalytic activity can be effectively improved. The gas flow rate was 60ml/min.
As shown in FIG. 1, which is a picture obtained after the field emission scanning electron microscope test, it can be seen from the graph (a) that the carbon nanotubes are successfully prepared, and the diameter thereof is about 30 to 50nm. In the graphs (b), (c) and (d), it is clear that the carbon nanotubes are uniform.
Fig. 2 is a picture obtained after the high resolution-projection electron microscope test, and the observation of the hollow structure proves that the carbon nanotube is formed, the fracture is sealed, the total length is 30.7nm, the clear lattice fringes are known, the graphitization degree is higher, and the high conductivity is shown.
FIG. 3 is an X-ray diffraction test chart of the present invention. XRD characterization shows that the prepared carbon nanotube material has (002) and (100) crystal faces, is amorphous carbon and further proves to be partially graphitized. Meanwhile, the prepared carbon nanotube has a negative shift of (002) peak position compared with NS-850, indicating that the degree of graphitization is weak, which may cause a change in lattice spacing due to heteroatom doping and defects.
FIG. 4 is a Raman spectrum test chart of the present invention. Raman tests show that the carbon nano-tubes have D and G peaks, and the prepared carbon nano-tubes have graphitization and defect sites. The carbon nanotubes produced were more graphitized than NS-850, which resulted from the graphitization of the carbon nanotubes, further demonstrating the presence of carbon nanotubes. Furthermore, as the annealing temperature increased, the value of ID/IG decreased, indicating that graphitization was promoted.
FIG. 5 is a test chart of X-ray photoelectron spectroscopy according to the present invention. Compared with NS-850, CNTs prepared contain nitrogen atom doping, which contributes to electrocatalytic activity.
FIG. 6 is a diagram of the spectral analysis of the present invention. Further tests show that the percentage and the distribution condition of nitrogen atoms are obtained, and the prepared biomass carbon nano tube has nitrogen atom doping and stronger electrocatalytic activity than a normal carbon nano tube.
FIG. 7 is a graph showing electrochemical tests of the present invention, which shows that CNTs prepared have corresponding ORR activity compared to NS-850, wherein B-850 has the highest activity, and the half-wave potential is only 16mV different from commercial 20% Pt/C.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for preparing carbon nanotubes based on Bifidobacterium lactis is characterized by comprising the following steps: and (3) putting the bifidobacterium lactis freeze-dried powder matched with the carrier into a tube furnace, heating to 750-900 ℃ at a preset heating rate under protective gas, preserving heat for a preset time, and naturally cooling to obtain the carbon nano tube.
2. The method for preparing carbon nanotubes based on Bifidobacterium lactis according to claim 1, wherein the carrier is maltose.
3. The method for preparing carbon nanotubes on the basis of bifidobacterium lactis as claimed in claim 1, wherein the mass of the bifidobacterium lactis lyophilized powder is 10g.
4. The method for preparing bifidobacterium lactis-based carbon nanotubes as claimed in claim 1, wherein the maximum temperature of the elevated temperature is 850 ℃.
5. The method for preparing carbon nanotubes based on Bifidobacterium lactis according to claim 1 or 4, wherein the temperature increase rate is 9.5 to 10.5 ℃/min.
6. The method for preparing carbon nanotubes based on Bifidobacterium lactis according to claim 5, wherein the incubation time is 2 to 2.5 hours.
7. The method for preparing carbon nanotubes based on bifidobacterium lactis according to claim 1, wherein the protective gas is nitrogen.
8. The method for preparing carbon nanotubes based on Bifidobacterium lactis according to claim 1 or 7, wherein the gas flow rate is 55 to 60ml/min.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US20140193323A1 (en) * | 2011-11-04 | 2014-07-10 | Cheil Industries Inc. | Double Wall Carbon Nanotubes and Method for Manufacturing Same |
CN109097059A (en) * | 2018-07-24 | 2018-12-28 | 湘潭大学 | A kind of bacterial origin mesoporous carbon material and preparation method thereof and the application in heavy metal pollution water system or soil remediation |
US20190270677A1 (en) * | 2016-07-22 | 2019-09-05 | The Regents Of The University Of Colorado, A Body Corporate | Filamentous organism-derived carbon-based materials, and methods of making and using same |
US20200277193A1 (en) * | 2019-03-02 | 2020-09-03 | Qatar University | Carbon nanotubes decorated with carbon nanospheres |
WO2022085771A1 (en) * | 2020-10-22 | 2022-04-28 | 株式会社Nextコロイド分散凝集技術研究所 | Method for separating between metal-type carbon nanotube and semiconductor-type carbon nanotube and purifying said carbon nanotubes |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20140193323A1 (en) * | 2011-11-04 | 2014-07-10 | Cheil Industries Inc. | Double Wall Carbon Nanotubes and Method for Manufacturing Same |
US20190270677A1 (en) * | 2016-07-22 | 2019-09-05 | The Regents Of The University Of Colorado, A Body Corporate | Filamentous organism-derived carbon-based materials, and methods of making and using same |
CN109097059A (en) * | 2018-07-24 | 2018-12-28 | 湘潭大学 | A kind of bacterial origin mesoporous carbon material and preparation method thereof and the application in heavy metal pollution water system or soil remediation |
US20200277193A1 (en) * | 2019-03-02 | 2020-09-03 | Qatar University | Carbon nanotubes decorated with carbon nanospheres |
WO2022085771A1 (en) * | 2020-10-22 | 2022-04-28 | 株式会社Nextコロイド分散凝集技術研究所 | Method for separating between metal-type carbon nanotube and semiconductor-type carbon nanotube and purifying said carbon nanotubes |
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