CN112090430A - Fe3O4@MoS2Magnetic composite structure and preparation method thereof - Google Patents

Fe3O4@MoS2Magnetic composite structure and preparation method thereof Download PDF

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CN112090430A
CN112090430A CN202010951519.3A CN202010951519A CN112090430A CN 112090430 A CN112090430 A CN 112090430A CN 202010951519 A CN202010951519 A CN 202010951519A CN 112090430 A CN112090430 A CN 112090430A
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高海淇
楚智良
吴小平
赵光
崔灿
李小云
程琳
王朋
吴泽
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Zhejiang University of Technology ZJUT
Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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Abstract

The invention relates to a magnetic functional composite material, a preparation process technology and the application field thereof, in particular to Fe3O4@MoS2A magnetic composite structure and a method for making the same comprising the steps of: a. dissolving iron acetate and sodium acetate in deionized water to form a mixed solution A; b. adding the mixed solution A intoAdding urea and polyethylene glycol to form a mixed solution B; c. adding the mixed solution B into a reaction kettle, and reacting for several hours at a certain temperature to obtain spherical Fe3O4(ii) a d. Adding sodium molybdate and thiourea into deionized water, and adding spherical Fe3O4Forming a mixed solution C, and heating and ultrasonically treating for a certain time; e. adding the treated mixed solution C into a reaction kettle, and reacting at a certain temperature to obtain Fe3O4@MoS2A magnetic composite structure. The dispersing performance and the uniformity of the sheet structure can be effectively improved, the addition of organic solvents such as dispersing agents and the like is avoided, and the stability of the morphology and the structure is high.

Description

Fe3O4@MoS2Magnetic composite structure and preparation method thereof
Technical Field
The invention relates to a magnetic photocatalytic composite structure and the field of preparation technology and application thereof, in particular to a magnetic photocatalytic composite structure
Fe3O4@MoS2Magnetic composite structures and methods of making the same.
Background
MoS2The material has a layered structure, a large specific surface area, good flexibility and high thermal stability. The larger light absorption coefficient enables the material to have stronger light-material interaction, the intrinsic response time is fast due to the short exciton service life, and the inherent spin orbit coupling effect opens a way for researching valley physics and devices thereof. The forbidden bandwidth of the material is adjustable depending on the number of layers between 1.2 and 1.9e V, the mobility is high at room temperature, and other excellent photoelectric characteristics, so that MoS is obtained2Has important application prospect in the fields of catalysis, batteries, electronic transistors, flexible electronics, biomedicine and the like. However, simple MoS2The single performance limits the application rangeAt present, the nanocomposite material with the core-shell structure becomes a research hotspot in the field of nano research due to the controllable physicochemical properties of the nanocomposite material, and is paid more and more attention by scientists. In general, a nano-structured material formed by coating one material with another nano-material through chemical bonds or physical adhesion is called a core-shell type nano-composite material. After being compounded, the nano-composite has more excellent properties in the aspects of electricity, optics, magnetism and the like than single particles, so that the synthesis of the nano-composite is widely concerned. Although the prior art has a few on MoS2The research on the composite structure, however, the prepared material has serious adhesion, poor dispersibility and complex preparation method, and the preparation method still needs to be improved. Especially for preparing Fe with good dispersity and uniform size3O4@MoS2Magnetic composite structures are still very difficult. In view of this, the present invention is intended to prepare an Fe by a liquid phase method3O4@MoS2The material has a magnetic composite structure and has high photocatalytic and photoelectric properties.
Disclosure of Invention
The invention aims to solve the primary technical problem of providing uniform Fe with simple process, low cost and short reaction period3O4@MoS2A method for preparing a magnetic composite structure.
Fe3O4@MoS2A method of making a magnetic composite structure comprising the steps of:
dissolving iron acetate and sodium acetate in deionized water, and stirring to form a mixed solution A;
adding a certain amount of urea and polyethylene glycol (PEG) into the mixed solution A, and stirring for a certain time to form a mixed solution B;
step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for several hours at a certain temperature to obtain spherical Fe3O4；
Step four, adding a certain amount of sodium molybdate and thiourea into deionized waterThen adding spherical Fe3O4Forming a mixed solution C, and heating and ultrasonically treating for a certain time;
step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, and reacting for several hours at a certain temperature to obtain Fe3O4@MoS2A magnetic composite structure.
Further, in the first step, the mass ratio of the ferric acetate to the sodium acetate is 1:1-5: 1; stirring for 10-60 min; the concentration of the solution A is 0.02-1 mol/L;
further, the amount of the urea in the step two is 1-5 mmol; the amount of PEG is 1-5 ml; stirring for 10-60 min;
further, the reaction temperature of the third step is 120-200 ℃; the reaction time is 8-20 h;
further, the molar ratio of the sodium molybdate to the thiourea in the fourth step is 1:2-2: 1; spherical Fe3O4The amount of (B) is 0.05-0.5 g; only in the above proportion range, particles with complete coating and good dispersibility can be obtained;
further, the heating temperature of the fourth step is 50-65 ℃, and the ultrasonic time is 1-3 h;
further, the reaction temperature of the step five is 160-240 ℃; the reaction time is 12-30 h.
Fe prepared by the preparation method3O4@MoS2Magnetic composite structure, Fe3O4@MoS2The size of the magnetic composite structure is 300nm-2 μm.
The invention has the beneficial effects that: fe of the invention3O4@MoS2The preparation method of the magnetic composite structure does not need expensive instruments and equipment, and realizes Fe through reasonable process control3O4@MoS2And (4) preparing a magnetic composite structure. The invention particularly adopts the method that the solution C is firstly heated and ultrasonically treated for a certain time before being placed in a reaction kettle so as to lead Fe3O4Surface adsorption and formation of uniformly dispersed MoS2Seed layer to facilitate later formation of monodisperse uniform Fe3O4@MoS2Compared with the traditional method, the method can effectively improve the dispersion performance and the uniformity of the sheet structure, avoids the addition of organic solvents such as dispersing agents and the like, and has high stability of the morphology and structure. And selecting Fe3O4In order to facilitate magnetic separation of particles, sizing of size and shape and the like, the invention has the advantages of cheap and easily available raw materials, simple synthesis process, low cost, short reaction period and no pollution to the environment. The prepared Fe3O4@MoS2The magnetic composite structure has uniform size, adjustable size and good dispersion, and the surface of the magnetic composite structure is composed of MoS2The porous structure formed by the nano sheets effectively improves the specific surface area, and can be applied to the fields of catalysis, photoelectricity, biomedical treatment and the like.
Drawings
FIG. 1 is Fe prepared in example 13O4@MoS2Scanning Electron Microscope (SEM) photographs of the magnetic composite structure.
FIG. 2 is Fe prepared in example 13O4@MoS2Scanning Electron Microscope (SEM) photographs of the magnetic composite structure.
Detailed Description
The following examples are presented to further illustrate the methods of the present invention and are not intended to limit the invention to these examples.
Example 1:
fe3O4@MoS2The preparation method of the magnetic composite structure comprises the following steps: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Form aMixing the solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
FIGS. 1 and 2 are Fe prepared in this example3O4@MoS2SEM image of magnetic composite structure, from which Fe prepared can be seen3O4@MoS2The magnetic composite structure has better dispersity and more uniform size.
Comparative example 1:
the difference between this example and example 1 is that in step four, the heating temperature is normal temperature, the ultrasonic dispersion time is 2h, and other steps are the same as example 1, and the results show that the particles are aggregated to some extent, the dispersion is not uniform, and the flake composition is not uniform.
Comparative example 2:
this example differs from example 1 in that in step four, the heating temperature was 80 ℃ and the ultrasonic dispersion time was 2 hours, and otherwise the same as example 1, the results showed good dispersion but the flake composition was not uniform.
Comparative example 3:
this example differs from example 1 in that in step four, the heating temperature was 60 ℃ and the ultrasonic dispersion time was 20min, and otherwise, the same as example 1, the results showed that aggregation was severe, dispersion was not uniform, and the flake composition was not uniform.
Comparative example 4:
this example differs from example 1 in that in step four, the heating temperature was 60 ℃ and the ultrasonic dispersion time was 4 hours, and otherwise the same as example 1, the results showed that the dispersibility was better but the flake composition was not uniform.
The results show that the dispersion is good, the aggregation is avoided, and the thickness of the flaky component is uniform within the temperature and ultrasonic time range of the application. If the temperature is higher or lower than the range of the present application, the particles may be aggregated at a lower temperature, and if the temperature is higher than the range of the present application, the particles may be non-uniformly flaky; similarly, the ultrasonic time has certain influence on the shape of the product, for example, the ultrasonic time is shorter, the dispersibility is not good, and the ultrasonic time is higher than the time of the application, so that the sheet shape is not uniform.
Example 2:
fe3O4@MoS2The preparation method of the magnetic composite structure comprises the following steps: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 50 ℃, and the ultrasonic dispersion time is 3 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing the reaction kettle with ethanol and deionized water for multiple times respectively, and drying to obtain Fe with good dispersibility3O4@MoS2A magnetic composite structure.
Example 3:
fe3O4@MoS2The preparation method of the magnetic composite structure comprises the following steps: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, and using ethanolWashing with deionized water for several times, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 65 ℃, and the ultrasonic dispersion time is 1 h; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing the reaction kettle with ethanol and deionized water for multiple times respectively, and drying to obtain Fe with good dispersibility3O4@MoS2A magnetic composite structure.
Example 4:
this example differs from example 1 in that the amounts of iron acetate and sodium acetate were changed to 1.5 and 4mmol in step one, otherwise the same as example 1, specifically as follows: step one, dissolving 1.5mmol of ferric acetate and 4mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 5:
this example differs from example 1 in that the amount of deionized water was changed in the first step30ml, otherwise the same as example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 30ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 6:
the difference between this example and example 1 is that the stirring time is changed to 30min in the first step, and the rest is the same as example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 30min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, mixing the mixed solution treated in the step fourC, adding the mixture into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 7:
this example differs from example 1 in that the amount of urea and polyethylene glycol was changed to 3mmol and 4ml in step two, and the other steps are the same as in example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 3mmol of urea and 4ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 8:
the difference between this example and example 1 is that the stirring time in step two is changed to 30min, and the rest is the same as example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 30min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, and placing the reaction kettle at a constant temperatureReacting for 12h at 160 ℃ in a box, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing the reaction kettle with ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 9:
this example differs from example 1 in that the reaction temperature was changed to 180 ℃ in the third step, and the other steps are the same as in example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 180 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 10:
this example is the same as example 1Except that the reaction time was changed to 16h in the third step, which was otherwise the same as in example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 16 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 11:
this example differs from example 1 in that the amounts of sodium molybdate and thiourea were changed to 1.5mmol and 1.5mmol, respectively, in step four, and otherwise the same as example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 1.5mmol of sodium molybdate and 1.5mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature in the fourth step is 60 ℃,the ultrasonic dispersion time is 2 h; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 12:
this example differs from example 1 in that the amount of deionized water in step four was changed to 45ml, and the other steps are the same as in example 1, as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 45ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 13:
this example differs from example 1 in that the reaction temperature was changed to 180 ℃ in step five, and the other steps are the same as in example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, mixing the mixed solution BAdding into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12h at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 180 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 14:
the difference between this example and example 1 is that the reaction time in step five was changed to 18h, and the rest is the same as example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 60ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 45ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 18 hours at 200 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.
Example 15:
this example differs from example 1 in that the reaction temperature was changed to 160 ℃ in step five, and the other steps are the same as in example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 6mmol of sodium acetate in 45ml of deionized water, and stirring for 20min to form a mixed solution A; adding 4.5mmol of urea and 6ml of polyethylene glycol into the mixed solution A, and stirring for 20min to form a mixed solution B; step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 12 hours at 160 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical Fe3O4(ii) a Step four, adding 2.25mmol of sodium molybdate and 2.25mmol of thiourea into 60ml of deionized water, and then adding spherical Fe3O4Forming a mixed solution C; the heating temperature of the step four is 60 ℃, and the ultrasonic dispersion time is 2 hours; step five, adding the mixed solution C treated in the step four into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 160 ℃, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Fe3O4@MoS2A magnetic composite structure.

Claims (8)

1. Fe3O4@MoS2The preparation method of the magnetic composite structure is characterized by comprising the following steps of:
dissolving iron acetate and sodium acetate in deionized water, and stirring to form a mixed solution A;
adding a certain amount of urea and polyethylene glycol (PEG) into the mixed solution A, and stirring for a certain time to form a mixed solution B;
step three, adding the mixed solution B into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for several hours at a certain temperature to obtain spherical Fe3O4；
Step four, adding a certain amount of sodium molybdate and thiourea into deionized water, and then adding spherical Fe3O4Forming a mixed solution C, and heating and ultrasonically treating for a certain time;
step five, adding the treated mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, and reacting for several hours at a certain temperature to obtain Fe3O4@MoS2A magnetic composite structure.
2. Fe as claimed in claim 13O4@MoS2The preparation method of the magnetic composite structure is characterized by comprising the following steps: the method is characterized in that: step one, the mass ratio of the ferric acetate to the sodium acetate is 1:1-5: 1; stirring for 10-60 min; the concentration of the solution A is 0.02-1 mol/L.
3. Fe as claimed in claim 13O4@MoS2The preparation method of the magnetic composite structure is characterized by comprising the following steps: the amount of the urea in the second step is 1-5 mmol; the amount of PEG is 1-5 ml; the stirring time is 10-60 min.
4. Fe as claimed in claim 13O4@MoS2The preparation method of the magnetic composite structure is characterized by comprising the following steps: the reaction temperature of the third step is 120-200 ℃; the reaction time is 8-20 h.
5. Fe as claimed in claim 13O4@MoS2The preparation method of the magnetic composite structure is characterized by comprising the following steps: the molar ratio of the sodium molybdate to the thiourea in the step four is 1:2-2: 1; spherical Fe3O4The amount of (B) is 0.05-0.5 g.
6. Fe as claimed in claim 13O4@MoS2The preparation method of the magnetic composite structure is characterized by comprising the following steps: the heating temperature of the fourth step is 50-65 ℃; the ultrasonic time is 1-3 h.
7. Fe as claimed in claim 13O4@MoS2A method for the preparation of a magnetic composite structure,the method is characterized in that: the reaction temperature of the step five is 160-240 ℃; the reaction time is 12-30 h.
8. Fe prepared by the preparation method according to any one of claims 1 to 73O4@MoS2Magnetic composite structure, its characterized in that: fe3O4@MoS2The size of the magnetic composite structure is 300nm-2 μm.
CN202010951519.3A 2020-09-11 2020-09-11 Fe3O4@MoS2Magnetic composite structure and preparation method thereof Pending CN112090430A (en)

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