CN112553651B - Preparation method of selenide coated carbon nanotube material - Google Patents
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- CN112553651B CN112553651B CN202011209942.2A CN202011209942A CN112553651B CN 112553651 B CN112553651 B CN 112553651B CN 202011209942 A CN202011209942 A CN 202011209942A CN 112553651 B CN112553651 B CN 112553651B
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Abstract
The invention discloses a method for preparing a selenide coated carbon nanotube material, which prepares a nanoflower-shaped selenide coated carbon nanotube in one step by the synergistic action of microwave and high pressure. The selenide coated carbon nano tube disclosed by the invention is prepared by mixing a molybdenum source, a selenium source and an organic solvent ethylenediamine, and greatly improving the heating efficiency through the combined action of energy and high pressure provided by microwave radiation, promoting the motion and collision probability of molybdenum source, selenium source and plasma, reducing the boiling point required by the reaction and saving a large amount of time. The selenide coated carbon nanotube material is efficiently and controllably prepared. The selenide coated carbon nano material provided by the invention has higher specific surface area and more active sites, and the preparation method has the advantages of easily available raw materials, simple process, low cost and high yield, and is expected to obtain a remarkable achievement in the field of electrocatalysis.
Description
Technical Field
The invention belongs to the technical field of electrolyzed water, and particularly relates to a preparation method of a selenide coated carbon nanotube material.
Background
In recent years, with the problems of large consumption of fossil fuels and consequent shortage of energy, environmental pollution and greenhouse effect, development of green sustainable energy based on energy conversion devices and technologies has gradually become a common subject of global social development. At present, hydrogen is the most promising clean renewable energy source, and the electrocatalytic water decomposition method is one of the best available technologies for preparing hydrogen. Among the catalyst choices, platinum (Pt) is the most effective catalyst for electrocatalytic hydrogen production, however, its high cost and limited global reserves limit its large-scale use. Therefore, the development of a high-efficiency and stable non-noble metal catalyst is one of the keys of the hydrogen production by water electrolysis.
Transition metal selenides are of great interest due to their excellent physicochemical properties, and there are many metals that can react with selenium dioxide, which is a selenium source, to form selenides, and molybdenum, tungsten, nickel, cobalt, iron, cerium, etc. are common. Molybdenum selenide is one of typical transition metal chalcogenide compounds, is a typical representative of transition metal compound nano materials, has the characteristics of large specific surface area and high surface activity, but has poor conductivity and easy agglomeration, and is limited in application in the field of hydrogen production by electrolyzing water.
Aiming at the defects of the product and the technology, the invention provides a new method for synthesizing a selenide coated carbon nanotube material by using microwave high-pressure stirring synergy and application thereof. The high pressure, the microwave and the stirring are carried out simultaneously, the synergistic effect is achieved, the carbon nano tube is used as a lead, the defect of pure molybdenum selenide is overcome, and the prepared selenide coated carbon nano tube material has high specific surface area and high catalytic activity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a selenide coated carbon nanotube material comprises the following steps:
the microwave, the high pressure and the stirring are simultaneously carried out, the carbon nanotube material coated with the selenide is prepared by one step through the synergistic reaction, the defects of long time consumption and easy agglomeration of common water are improved, and the method comprises the following steps:
(1) placing a molybdenum-based element source, a selenium source and the oxidized carbon nano tube into water, violently stirring, adding a reducing agent polyethylene glycol and an organic solvent ethylenediamine with a coordination effect, and continuously violently stirring to obtain a uniformly dispersed suspension;
(2) putting the suspension obtained in the step (1) into a reaction kettle, carrying out solvothermal reaction, controlling the pressure in the reaction kettle to be at least 1 MPa in the whole reaction process, carrying out stirring in the whole reaction process, controlling the reaction temperature to be 100-220 ℃ through microwave heating, and cooling to room temperature after the reaction is finished to obtain a solution containing a product;
(3) and (3) centrifuging the solution containing the product obtained in the step (2), collecting the precipitate, drying the precipitate in vacuum, and calcining the dried precipitate in a nitrogen atmosphere to obtain the selenide-coated carbon nanotube material.
Further, the molybdenum-based element source in the step (1) is any one or more of ammonium molybdate tetrahydrate, sodium molybdate and phosphomolybdic acid, and the selenium source is any one of selenium dioxide or ammonium selenide.
Further, the molar ratio of the molybdenum-based element source to the selenium source in the step (1) is 1: 1-1: 6.
Further, the molar ratio of the molybdenum-based element source to the selenium source in the step (1) is 1: 4.
Further, in the step (2), the microwave power is 300-1000W, the reaction kettle is magnetically stirred, and the rotating speed of the stirring magnetons is 100-1200 r/min.
Further, the hydrothermal reaction time in the step (2) is 1-14 hours.
Further, in the step (3), the calcining temperature is 300-600 ℃, the temperature is too low, the crystal form is not good, the material is decomposed when the temperature is too high (preferably 500 ℃), and the calcining time is 1-6 hours.
Compared with the prior art, the invention has the advantages that:
(1) the microwave, high pressure and stirring are cooperated, so that the boiling point of the solution is reduced, the activity of reactants is improved, the dispersibility and the reaction degree of the reactants are improved, and the reaction time is shortened;
(2) the defects of pure selenide agglomeration and poor conductivity are overcome;
(3) this scheme demonstrates the lower overpotential of selenide coated carbon nanotubes in acidic and alkaline electrolytes;
(4) the scheme has low cost, is simple and feasible, and can realize large-scale industrial application.
Drawings
FIG. 1 is a scanning electron micrograph of a selenide coated carbon nanotube material prepared in example 1 by using a combination of high pressure of 4MPa, a microwave power of 800W and stirring at a speed of 800 rmp.
FIG. 2 scanning electron micrograph of selenide coated carbon nanotubes prepared in accordance with stirring at a high pressure of 4MPa and a rate of 800rmp in comparative example 2.
FIG. 3 scanning electron micrograph of selenide coated carbon nanotubes prepared by microwave synergy at high pressure of 4MPa and power of 800W in comparative example 3.
FIG. 4 is a scanning electron micrograph of molybdenum selenide coated carbon nanotubes prepared by the synergy of stirring at a power of 800W microwaves and a speed of 800rmp in comparative example 1.
FIG. 5 shows a selenide coated carbon nanotube material (MoSe) prepared by high pressure microwave stirring under acidic electrolyte2/CNT-1) and microwave high voltage synergistically prepared selenide coated carbon nanotube material (MoSe)2/CNT-4), microwave stirring, and selenide coated carbon nanotube material (MoSe) prepared by the cooperation of the two2/CNT-2), high-pressure stirring, and preparing selenide coated carbon nanotube material (MoSe) in pairs2/CNT-3) comparative graph of hydrogen evolution performance.
FIG. 6 shows a selenide coated carbon nanotube material (MoSe) prepared by high pressure microwave stirring under alkaline electrolyte2/CNT-1) and microwave high voltage synergistically prepared selenide coated carbon nanotube material (MoSe)2/CNT-4), microwave stirring, and selenide coated carbon nanotube material (MoSe) prepared by the cooperation of the two2/CNT-2), high-pressure stirring, and preparing selenide coated carbon nanotube material (MoSe) in pairs2/CNT-3) comparative graph of hydrogen evolution performance.
FIG. 7 MoSe in example 12Temperature time profile and pressure time profile during the preparation of/CNT-1.
Detailed Description
In order to make the technical purpose, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention are further described with reference to specific examples, which are intended to explain the present invention and are not to be construed as limiting the present invention, and those who do not specify a specific technique or condition in the examples follow the techniques or conditions described in the literature in the art or follow the product specification.
The method for preparing the selenide coated carbon nanotube material by adopting a microwave high-pressure stirring synergistic method comprises the following steps:
example 1
Step (1), selenium source selenium dioxide and molybdenum source ammonium molybdate tetrahydrate in a ratio of 4:1 are prepared into an aqueous solution, 0.2g/L of carbon nano tube and 0.2g/L of reducing agent polyethylene glycol are added, vigorous stirring is carried out until the mixture is uniform, then 30mL of organic solvent ethylene diamine is added, and vigorous stirring is carried out at a constant temperature until the solution is uniformly mixed.
And (2) putting the solution in the step (1) into a reaction kettle, and reacting for 7 hours at the temperature of 200 ℃ by the cooperation of high pressure of 4MPa, microwave of 800W and stirring speed of 800 rmp.
Step (3) is the same as step (3) in example 1 and is denoted as MoSe2/CNT-1。
Referring to fig. 1, a large amount of uniform and dense flower-like molybdenum selenide is loaded on a carbon nanotube.
Comparative example 1
Step (1) is the same as step (1) in example 1.
And (2) putting the solution obtained in the step (1) into a reaction kettle, and reacting for 7 hours at the temperature of 200 ℃ by the aid of microwaves of 800W and the stirring speed of 800rmp in a coordinated manner.
And (3) centrifugally collecting the precipitate obtained in the step (2), drying the precipitate at 140 ℃ in vacuum to obtain black powder solid of the molybdenum selenide coated carbon nano tube, then placing the solid in a crucible, calcining the solid at the high temperature of 500 ℃ in nitrogen by using a tube furnace, and then grinding the calcined solid to obtain a selenide material of the tubular carbon nano tube coated by the nano flower-shaped molybdenum selenide, wherein the selenide material is recorded as MoSe2/CNT-2. Compared with the example 1, the difference is that the microwave stirring and the reaction are synergistic, and high pressure is not added, and as is apparent from fig. 2, the carbon nanotube prepared by the comparative example 1 has a small and sparse molybdenum selenide loading on the surface.
Comparative example 2
Step (1) is the same as step (1) in example 1.
And (2) putting the solution obtained in the step (1) into a reaction kettle, and reacting for 7 hours at the temperature of 200 ℃ through the cooperation of the high pressure of 4MPa and the stirring speed of 800 rmp.
Step (3) is the same as step (3) in example 1 and is denoted as MoSe2[ CNT-3 ]. Compared with the example 1, the difference is that the two are synergistically reacted under high-pressure stirring, and microwaves are not added, and as is apparent from fig. 3, the carbon nanotube prepared in the comparative example 2 has a small and sparse molybdenum selenide loading on the surface.
Comparative example 3
Step (1) is the same as step (1) in example 1.
And (2) putting the solution obtained in the step (1) into a reaction kettle, and reacting for 7 hours at the temperature of 200 ℃ by the cooperation of high pressure of 4MPa and microwaves of 800W.
Step (3) is the same as step (3) in example 1 and is denoted as MoSe2/CNT-4。
Compared with example 1, the difference is that the microwave high-pressure synergistic reaction is not accompanied by stirring in the whole process, and as is apparent from fig. 4, the carbon nanotube prepared in comparative example 3 has a small and sparse loading of molybdenum selenide on the surface.
Adding MoSe2/CNT-1、MoSe2/CNT-2，MoSe2[ CNT-3 ] and MoSe2The hydrogen evolution performance test of the/CNT-4 shows that the molybdenum selenide coated carbon nano tube prepared by the microwave high-pressure stirring three synergistic modes has better hydrogen evolution performance than the microwave high-pressure two-by-two synergy, the microwave stirring two-by-two synergy and the high-pressure stirring two-by-two synergy under the acid electrolyte condition from figure 5. As is apparent from FIG. 6, under alkaline electrolyte conditions, MoSe2The hydrogen evolution law of the/CNT is consistent with that of the acidic electrolyte.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and their concepts should be equivalent or changed within the technical scope of the present invention.
The present invention is not limited to the above embodiments, and those skilled in the art can implement the present invention in other embodiments according to the disclosure of the present invention, or make simple changes or modifications on the design structure and idea of the present invention, and fall into the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Claims (6)
1. A preparation method of a selenide coated carbon nanotube material is characterized by comprising the following steps: the method comprises the following steps:
the microwave, the high pressure and the stirring are simultaneously carried out, the carbon nanotube material coated with the selenide is prepared by one step through the synergistic reaction, the defects of long time consumption and easy agglomeration of common water are improved, and the method comprises the following steps:
(1) placing a molybdenum-based element source, a selenium source and the oxidized carbon nano tube into water, violently stirring, adding a reducing agent polyethylene glycol and an organic solvent ethylenediamine with a coordination effect, and continuously violently stirring to obtain a uniformly dispersed suspension;
(2) putting the suspension obtained in the step (1) into a reaction kettle, carrying out solvothermal reaction, controlling the pressure in the reaction kettle to be at least 1 MPa in the whole reaction process, carrying out stirring in the whole reaction process, controlling the reaction temperature to be 100-220 ℃ through microwave heating, and cooling to room temperature after the reaction is finished to obtain a solution containing a product;
(3) centrifuging the solution containing the product obtained in the step (2), collecting the precipitate, drying the precipitate in vacuum, and calcining the dried precipitate in nitrogen atmosphere to obtain a selenide-coated carbon nanotube material;
in the step (2), the microwave power is 300-1000W, the reaction kettle is magnetically stirred, and the rotating speed of the stirring magnetons is 100-1200 rpm.
2. The method of preparing a selenide coated carbon nanotube material of claim 1, wherein: the molybdenum-based element source in the step (1) is any one or more of ammonium molybdate tetrahydrate, sodium molybdate and phosphomolybdic acid, and the selenium source is any one of selenium dioxide or ammonium selenide.
3. The method of preparing a selenide coated carbon nanotube material of claim 1, wherein: the molar ratio of the molybdenum-based element source to the selenium source in the step (1) is 1: 1-1: 6.
4. The method of preparing a selenide coated carbon nanotube material of claim 1, wherein: the hydrothermal reaction time in the step (2) is 1-14 hours.
5. The method of preparing a selenide coated carbon nanotube material of claim 1, wherein: in the step (3), the calcining temperature is 300-600 ℃, and the calcining time is 1-6 hours.
6. The method of preparing a selenide coated carbon nanotube material of claim 1, wherein: the calcination temperature in step (3) was 500 ℃.
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| CN115101762B (en) * | 2022-07-05 | 2023-05-16 | 青岛科技大学 | Preparation method of carbon nano tube/metal selenide material |
| CN116119626B (en) * | 2022-11-22 | 2024-07-02 | 湖南大学 | Synthesis method of PEG-200-2-C@MoSe2@NMWCNT nanocomposite heterojunction material based on N-doped CNT |
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