CN112194104B - Preparation method of flower-ball-shaped ZIF-67-molybdenum selenide nano particles - Google Patents
Preparation method of flower-ball-shaped ZIF-67-molybdenum selenide nano particles Download PDFInfo
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Abstract
The invention discloses a preparation method of a flower-ball-shaped ZIF-67-molybdenum selenide nano particle, which comprises the following steps: dissolving cobalt nitrate in a methanol solution, uniformly dispersing by ultrasonic to obtain a solution A, and dissolving 2-methylimidazole in the methanol solution, and uniformly dispersing by ultrasonic to obtain a solution B. And slowly dripping the solution B into the solution A, standing, centrifuging, and washing with methanol to obtain ZIF. Weighing a proper amount of ZIF-67, dispersing in a proper amount of water to obtain a solution a, weighing a proper amount of selenium powder, dissolving in a hydrazine hydrate solution to obtain a solution b, filling the ab solution into a three-necked bottle, adding a magnet, carrying out oil bath, weighing a proper amount of sodium molybdate dihydrate, dissolving in water, adding into the three-necked bottle, continuing to react, centrifuging the obtained solution, and washing to obtain a finished product. The prepared nano composite ions are in a flower ball shape, have uniform size, good dispersibility and low toxicity, can show high-efficiency photothermal conversion performance under the irradiation of near infrared light, and can be applied to the biomedical fields of photothermal treatment of tumors and the like. In addition, the method has the advantages of simple process, low energy consumption, small equipment quantity and convenient popularization.
Description
Technical Field
The invention relates to the technical field of nano composite materials, in particular to a preparation method of a flower-ball-shaped ZIF-67-molybdenum selenide nano particle.
Background
The transition metal chalcogenide has a narrower band gap and a more suitable Fermi level compared with an oxide due to the fact that the transition metal chalcogenide has a special electronic structure, most of the transition metal chalcogenide has a special layered structure similar to graphene, the transition metal chalcogenide has a larger interlayer spacing, and ions can be easily inserted between layers, so that the materials have excellent performances in the aspects of light, catalysis, material modification and the like. Molybdenum selenide is taken as one of transition metal chalcogenide compounds, belongs to a hexagonal crystal system, very strong Se-Mo-Se covalent bonds are arranged in layers, weak van der Waals force is arranged among the layers, and the thickness of a single layer is about 0.65 nm. Each molybdenum atom in the molybdenum selenide is surrounded by six selenium atoms and is arranged in a triangular prism, the number of the edge surfaces of Mo to Se is quite large, and compared with the titanium dioxide material which is researched for pyrogenic, the forbidden bandwidth of the molybdenum selenide is narrower and is about 1.4eV, so that the molybdenum selenide nano particles have the characteristics of large specific surface area, high surface activity and the like, and can well absorb light in a visible light region and a near infrared light region.
However, pure molybdenum selenide is easy to agglomerate, an inert inner layer structure is preferentially grown on the pure molybdenum selenide, the active edge is not exposed due to a large number of agglomerates, and the excellent performance of the molybdenum selenide cannot be fully utilized. Therefore, the molybdenum selenide is of great significance to be compounded with other substrate materials.
The existing methods for preparing molybdenum selenide nanoparticles mainly comprise a solid-phase method, a gas-phase method and a liquid-phase method, wherein the solid-phase method is simple in synthesis process, high in conversion rate, uniform in particle size, harsh in reaction conditions and high in equipment requirement, the liquid-phase method does not need high temperature and pressure, but is easy to cause hard agglomeration in the preparation process and long in process flow, the gas-phase method is high in equipment requirement, and the purity of the obtained product is not enough, so that the cost, the environment and other factors are considered, and the development of a simple and efficient synthesis method is necessary.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a flower-ball-shaped ZIF-67-molybdenum selenide nano particle, and aims to provide a method for preparing a molybdenum selenide nano particle with simple preparation process, low energy consumption, small equipment quantity and short process flow.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a flower-ball-shaped ZIF-67-molybdenum selenide nano particle comprises the following steps:
preparation of zif precursor:
(1) dissolving 3mmol of cobalt nitrate in 10-100 ml of methanol solution, and performing ultrasonic dispersion uniformly to obtain a solution A;
(2) dissolving 12mmol of 2-methylimidazole in 2-30 ml of methanol solution, and uniformly dispersing by ultrasonic to obtain a solution B;
(3) slowly dripping the solution B into the solution A, standing for 12h, centrifuging for 5min at 3000-16000 r/min, and washing with methanol for 1-2 times to obtain ZIF blue nanoparticles;
II, preparing the molybdenum selenide nano particles:
(1) weighing 0.3mmol of ZIF-67, and dispersing in 10-100 ml of water to obtain a solution a;
(2) weighing 1mmol of selenium powder, and dissolving the selenium powder in 1-10 ml of hydrazine hydrate to obtain a solution b;
(3) putting the solution a and the solution b into a 50ml three-necked bottle, adding a magnet, and reacting for 2-12 h in a constant-temperature oil bath kettle at 40-190 ℃;
(4) then weighing 0.5mmol of sodium molybdate dihydrate, dissolving in 2-20 ml of water, adding into the three-necked bottle, and continuing to react for 2-8 h;
(5) and after the reaction is finished, centrifuging the obtained solution for 5min at 5000-12000 r/min, and washing with water for 1-2 times to obtain the needed ZIF-67-molybdenum selenide nano particles.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the technology has the advantages that: the invention aims to provide a method for preparing molybdenum selenide nano particles, which has the advantages of simple preparation process, low energy consumption, small equipment quantity and short process flow. The prepared molybdenum selenide nano particles have a flower ball shape and uniform size. Under the irradiation of near infrared light, the temperature can be raised to 80 ℃ within 5min, and the nano-silver nano-particles have good near infrared absorption capacity and high-efficiency photothermal conversion capacity and can be widely applied to the fields of seawater desalination, tumor treatment, sewage treatment and the like.
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 description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIGS. 1 and 2 are scanning electron micrographs of ZIF-67-molybdenum selenide nanoparticles.
FIG. 3 is a graph of temperature versus time for different concentrations of ZIF-67-molybdenum selenide nanoparticles under 808nm near infrared irradiation at 2-5W for 5 min.
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 embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of a flower-ball-shaped ZIF-67-molybdenum selenide nano particle comprises the following steps:
preparation of zif precursor:
(1) dissolving 3mmol of cobalt nitrate in 10ml of methanol solution, and performing ultrasonic dispersion uniformly to obtain a solution A;
(2) dissolving 12mmol of 2-methylimidazole in 2ml of methanol solution, and uniformly dispersing by ultrasonic to obtain a solution B;
(3) slowly dripping the solution B into the solution A, standing for 12h, centrifuging at 3000r/min for 5min, and washing with methanol for 1 time to obtain ZIF blue nanoparticles;
II, preparing the molybdenum selenide nano particles:
(1) weighing about 0.3mmol of ZIF-67, and dispersing in 10ml of water to obtain a solution a;
(2) weighing about 1mmol of selenium powder, and dissolving the selenium powder in 1ml of hydrazine hydrate to obtain a solution b;
(3) putting the solution a and the solution b into a 50ml three-necked bottle, adding a magnet, and reacting for 12 hours in a constant-temperature oil bath kettle at 40 ℃;
(4) then 0.5mmol of sodium molybdate dihydrate is weighed and dissolved in 2ml of water, and the mixture is added into the three-necked bottle and continuously reacted for 2 hours;
(5) and after the reaction is finished, centrifuging the obtained solution for 5min at 5000r/min, and washing the solution for 1 time by using water to obtain the needed ZIF-67-molybdenum selenide nano particle.
Example 2:
a preparation method of a flower-ball-shaped ZIF-67-molybdenum selenide nano particle comprises the following steps:
preparation of zif precursor:
(1) dissolving 3mmol of cobalt nitrate in 100ml of methanol solution, and performing ultrasonic dispersion uniformly to obtain a solution A;
(2) dissolving 12mmol of 2-methylimidazole in 30ml of methanol solution, and uniformly dispersing by ultrasonic to obtain a solution B;
(3) slowly dripping the solution B into the solution A, standing for 12h, centrifuging for 5min at 16000r/min, and washing with methanol for 1 time to obtain ZIF blue nanoparticles;
II, preparing the molybdenum selenide nano particles:
(1) weighing about 0.3mmol of ZIF-67, and dispersing in 100ml of water to obtain a solution a;
(2) weighing about 1mmol of selenium powder and dissolving the selenium powder in 10ml of hydrazine hydrate to obtain a solution b;
(3) putting the solution a and the solution b into a 50ml three-necked bottle, adding a magnet, and reacting for 2 hours in a constant-temperature oil bath kettle at 190 ℃;
(4) then 0.5mmol of sodium molybdate dihydrate is weighed and dissolved in 20ml of water, and the mixture is added into the three-necked bottle and continuously reacted for 8 hours;
(5) and after the reaction is finished, centrifuging the obtained solution at 12000r/min for 5min, and washing the solution for 1 time by using water to obtain the needed ZIF-67-molybdenum selenide nano particles.
Example 3:
a preparation method of a flower-ball-shaped ZIF-67-molybdenum selenide nano particle comprises the following steps:
preparation of zif precursor:
(1) dissolving 3mmol of cobalt nitrate in 50ml of methanol solution, and performing ultrasonic dispersion uniformly to obtain a solution A;
(2) dissolving 12mmol of 2-methylimidazole in 20ml of methanol solution, and uniformly dispersing by ultrasonic to obtain a solution B;
(3) slowly dripping the solution B into the solution A, standing for 12h, centrifuging at 12000r/min for 5min, and washing with methanol for 2 times to obtain ZIF blue nanoparticles;
II, preparing the molybdenum selenide nano particles:
(1) weighing about 0.3mmol of ZIF-67, and dispersing in 50ml of water to obtain a solution a;
(2) weighing about 1mmol of selenium powder and dissolving the selenium powder in 5ml of hydrazine hydrate to obtain a solution b;
(3) putting the solution a and the solution b into a 50ml three-necked bottle, adding a magnet, and reacting for 6 hours in a constant-temperature oil bath kettle at 120 ℃;
(4) then 0.5mmol of sodium molybdate dihydrate is weighed and dissolved in 10ml of water, and the mixture is added into the three-necked bottle and continuously reacted for 5 hours;
(5) and after the reaction is finished, centrifuging the obtained solution at 6000r/min for 5min, and washing with water for 2 times to obtain the needed ZIF-67-molybdenum selenide nano particles.
Example 4:
the prepared molybdenum selenide nano particles are observed under a scanning electron microscope (figures 1 and 2), and the molybdenum selenide nano particles are in a flower ball shape and uniform in size;
example 5:
irradiating the prepared ZIF-67-molybdenum selenide nano particles with different concentrations for 5min by using near infrared with the wavelength of 808nm of 5W cm-2, and exploring the change conditions of different temperatures and time to obtain a graph 2, wherein the temperature can reach about 80 ℃ at most under the laser irradiation of 5min, and the ZIF-67-molybdenum selenide nano particles can show high-efficiency photothermal conversion performance.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present 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 solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (1)
1. A preparation method of a flower-ball-shaped ZIF-67-molybdenum selenide nano particle is characterized by comprising the following steps:
preparation of zif precursor:
(1) dissolving 3mmol of cobalt nitrate in 10-100 ml of methanol solution, and performing ultrasonic dispersion uniformly to obtain a solution A;
(2) dissolving 12mmol of 2-methylimidazole in 2-30 ml of methanol solution, and uniformly dispersing by ultrasonic to obtain a solution B;
(2) slowly dripping the solution B into the solution A, standing for 12h, centrifuging for 5min at 3000-16000 r/min, and washing with methanol for 1-2 times to obtain ZIF blue nanoparticles;
II, preparing the molybdenum selenide nano particles:
(1) weighing 0.3mmol of ZIF-67, and dispersing in 10-100 ml of water to obtain a solution a;
(2) weighing 1mmol of selenium powder, and dissolving the selenium powder in 1-10 ml of hydrazine hydrate to obtain a solution b;
(3) putting the solution a and the solution b into a 50ml three-necked bottle, adding a magnet, and reacting for 2-12 h in a constant-temperature oil bath kettle at 40-190 ℃;
(4) then weighing 0.5mmol of sodium molybdate dihydrate, dissolving in 2-20 ml of water, adding into the three-necked bottle, and continuing to react for 2-8 h;
(5) and after the reaction is finished, centrifuging the obtained solution for 5min at 5000-12000 r/min, and washing with water for 1-2 times to obtain the needed ZIF-67-molybdenum selenide nano particles.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105460921A (en) * | 2015-11-20 | 2016-04-06 | 复旦大学 | Molybdenum selenide nanosheets/graphene nanoribbons composite material and preparation method thereof |
| CN106099053A (en) * | 2016-06-03 | 2016-11-09 | 东华大学 | A kind of molybdenum sulfide/selenizing molybdenum composite material and preparation thereof and application |
| WO2018197715A1 (en) * | 2017-04-28 | 2018-11-01 | Cambridge Enterprise Limited | Composite metal organic framework materials, processes for their manufacture and uses thereof |
| CN108975416A (en) * | 2018-08-23 | 2018-12-11 | 大连理工大学 | A kind of preparation method of transient metal sulfide composite nano materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105460921A (en) * | 2015-11-20 | 2016-04-06 | 复旦大学 | Molybdenum selenide nanosheets/graphene nanoribbons composite material and preparation method thereof |
| CN106099053A (en) * | 2016-06-03 | 2016-11-09 | 东华大学 | A kind of molybdenum sulfide/selenizing molybdenum composite material and preparation thereof and application |
| WO2018197715A1 (en) * | 2017-04-28 | 2018-11-01 | Cambridge Enterprise Limited | Composite metal organic framework materials, processes for their manufacture and uses thereof |
| CN108975416A (en) * | 2018-08-23 | 2018-12-11 | 大连理工大学 | A kind of preparation method of transient metal sulfide composite nano materials |
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