CN115744880B - Carbon nanotube preparation method based on bifidobacterium lactis - Google Patents
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- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 58
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- 229940009289 bifidobacterium lactis Drugs 0.000 title claims abstract description 27
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Abstract
The invention provides a method for preparing carbon nanotubes based on bifidobacterium lactis. The method of the invention comprises the following steps: and (3) placing the bifidobacterium lactis freeze-dried powder matched with the carrier into a tube furnace, heating to 750-900 ℃ at a preset heating rate under the protection gas, preserving heat for a preset time, and naturally cooling to obtain the carbon nanotube. The method provided by the invention is prepared by a one-step annealing method, has the advantages of 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 carbon nanotube preparation method based on bifidobacterium lactis.
Background
The carbon nanotube, also called bucky tube, is a one-dimensional quantum material with a special structure (the radial dimension is in the order of nanometers, the axial dimension is in the order of micrometers, and both ends of the tube are basically sealed). The current methods for preparing carbon nanotubes mainly comprise an arc discharge method, a laser evaporation method and a chemical vapor deposition method.
The arc discharge method has the advantages of high carbon nanotube production rate, simple technological parameter setting required in the experimental process, good straightness and crystallinity of the grown carbon nanotubes, and the like, but has the following disadvantages: the temperature requirement of the grown 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 method is easy to sinter byproducts 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 put a target material made of metal catalyst/graphite powder into a quartz tube reactor, and the quartz tube is put into a horizontal heating furnace. When the furnace temperature was raised to 1473K, an inert gas was filled into the tube and a laser was focused onto the graphite target. The graphite target generates gaseous carbon under the irradiation of laser, and single-wall carbon nano-tubes are grown under the action of a catalyst. The yield of the carbon nanotubes increases with the shortening of the time interval of the laser pulse, and the tube diameter of the carbon nanotubes 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, entanglement of products is easy to occur, 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 the catalyst particles, so that the production cost is low, and the applicability is strong. Is the most promising method for preparing high-quality carbon nano-tubes in large quantity. Therefore, this method is highly paid attention to and widely used. However, the carbon nanotubes prepared by the chemical vapor deposition method have the defects of long length, uneven diameter and low graphitization degree.
In addition to the above method, shi Jian waffle uses some natural biomass as a catalyst precursor, uses natural gas as a carbon source, and adopts 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 fabrication. But has a disadvantage of a long operation time and does not solve the problem in terms of the carbon source.
The lanmei morning team adopts a thermal cracking-catalytic modification method (two-stage method) to treat waste plastics and obtain high-value product carbon nanotubes, so that the method has the characteristics of low-cost and easily obtained raw materials, economy and environmental protection, but the existing reactor can not treat the waste plastics in a large scale and continuously produce the carbon nanotubes; the waste plastics generated in life are various and complex in composition, and have great influence on the shape and quality of the carbon nano tube, so that the practical application of the method is hindered; too strong interaction between the active components of the catalyst and the carrier can cause sintering and agglomeration of the catalyst so as to lead the diameter of the carbon nano tube to be too large, and too weak interaction can influence the catalytic effect so as to lead the yield of the carbon nano tube to be reduced; the carbon nanotubes prepared by plastic pyrolysis have not been practically used because of the difficulty in separation from the catalyst, the product contains other carbon impurities, and the like.
Disclosure of Invention
According to the technical problem presented above, a method for preparing carbon nanotubes based on bifidobacterium lactis is provided. The invention adopts the following technical means:
a method for preparing carbon nanotubes based on bifidobacterium lactis comprises the following steps:
and (3) placing the bifidobacterium lactis freeze-dried powder matched with the carrier into a tube furnace, heating to 750-900 ℃ at a preset heating rate under the protection gas, preserving heat for a preset time, and naturally cooling to obtain the carbon nanotube.
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 temperature rising rate is 9.5-10.5 ℃/min.
Further, the heat preservation time is 2-2.5 h.
Further, the shielding gas is nitrogen.
Further, the gas flow rate is 55 to 60ml/min.
The invention has the following advantages:
1. the invention firstly utilizes bifidobacterium lactis as a precursor to prepare the multiwall carbon nanotube and is applied to material science. Based on the intrinsic characteristics of bifidobacterium lactis serving as procaryotic cells (without complex organelles), a foundation is provided for a hollow structure. The cell wall of bifidobacterium lactis consists 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 green and environment-friendly development trend, and has lower cost and wide source.
3. The method for preparing the aluminum alloy by the one-step annealing method has the advantages of simple process and low cost, 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 that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort to a person skilled in the art.
FIG. 1 is a scanning electron microscope image of annealed bifidobacterium lactis carbon nanotubes according to the present invention, wherein (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 test chart (XPS) of the present invention, wherein (a) and (B) are respectively the existing NS-850 and B-850 prepared by the present invention.
Fig. 6 is an energy spectrum analysis chart of the present invention, wherein a) is an analysis chart of components and contents of carbon nanotubes prepared by a normal route, and b) is an analysis chart of components and contents 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; (b) is a linear voltammetric scan test.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the 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, and naturally cooling after preserving heat for a preset time to obtain the carbon nanotube. In this example, maltose is selected as the carrier, which is advantageous for maintaining morphological and structural characteristics of the fungus. Experiments show that only maltose can realize the function. During the heating process, a proper amount of maltose is firstly placed, 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 morphology, intrinsic defects, heteroatom doping and the like, and further influence the physical, chemical, mechanical, thermodynamic and other performances of the carbon nano tube. Grasping the specific impact of the four factors on their performance is one of the difficulties in preparing CNTs with high efficiency. Therefore, the invention obtains the optimal value annealing maximum temperature of 850 ℃ in the preparation process by multiple experiments, wherein 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 and is in an optional range. The temperature rising rate is 10 ℃/min. The incubation time was 2h. The protective gas is nitrogen, and the nitrogen is favorable for 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 fig. (a) that the carbon nanotubes were successfully prepared, which have diameters of about 30-50nm. The carbon nanotubes were uniform as shown in the figures (b), (c) and (d).
Fig. 2 is a graph obtained after high resolution-projection electron microscope test, and the hollow structure is observed, which proves that the carbon nano tube is a seal at the fracture, the total length is 30.7nm, and the graphitization degree is higher, so that the high conductivity is shown.
Fig. 3 is an X-ray diffraction test chart of the present invention. XRD characterization revealed that the prepared carbon nanotube material had both (002) and (100) crystal planes, amorphous carbon, further demonstrated partial graphitization. Meanwhile, the prepared carbon nanotube has negative shift of (002) peak position compared with NS-850, which indicates weaker graphitization degree, which may cause lattice spacing change due to heteroatom doping and defects.
Fig. 4 is a raman spectrum test chart of the present invention. Raman tests showed both D and G peaks, indicating that the prepared carbon nanotubes had graphitization and defect sites. The graphitization degree of the prepared carbon nano tube is higher than that of NS-850, which is derived from graphitization of the carbon nano tube, and further proves the existence of the carbon nano tube. Furthermore, as the annealing temperature increases, the value of ID/IG decreases, indicating that graphitization is promoted.
FIG. 5 is a graph of an X-ray photoelectron spectroscopy test according to the present invention. As compared to NS-850, CNTs are prepared that contain nitrogen atom doping, which contributes to electrocatalytic activity.
FIG. 6 is a graph of the energy spectrum analysis of the present invention. Further tests show that the prepared biomass carbon nanotubes have nitrogen atom doping and stronger electrocatalytic activity compared with normal carbon nanotubes.
FIG. 7 is a graph of electrochemical testing of the present invention, showing that CNTs are all prepared with corresponding ORR activity compared to NS-850, wherein B-850 activity is highest and half-wave potential is only 16mV worse than commercial 20% Pt/C.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (7)
1. A method for preparing carbon nanotubes based on bifidobacterium lactis, which is characterized by comprising the following steps: placing the bifidobacterium lactis freeze-dried powder matched with the carrier into a tube furnace, heating to 750-900 ℃ at a preset heating rate under the protection gas, preserving heat for a preset time, and naturally cooling to obtain the carbon nano tube;
the carrier is maltose.
2. The method for preparing carbon nanotubes based on bifidobacterium lactis according to claim 1, wherein the mass of the bifidobacterium lactis freeze-dried powder is 10g.
3. The method for preparing a carbon nanotube based on bifidobacterium lactis according to claim 1, wherein the highest temperature of temperature rise is 850 ℃.
4. A method for preparing carbon nanotubes based on bifidobacterium lactis according to claim 1 or 3, wherein the heating rate is 9.5-10.5 ℃/min.
5. The method for preparing carbon nanotubes based on bifidobacterium lactis according to claim 4, wherein the incubation time is 2 to 2.5 hours.
6. The method for preparing carbon nanotubes based on bifidobacterium lactis according to claim 1, wherein the shielding gas is nitrogen.
7. The method for preparing carbon nanotubes based on bifidobacterium lactis according to claim 1 or 6, wherein the gas flow rate is 55-60 ml/min.
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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 |
| 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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