CN111974420B - MnFe 2 O 4 @Mo x Sn 1-x S 2 Magnetic catalytic material and preparation method thereof - Google Patents
MnFe 2 O 4 @Mo x Sn 1-x S 2 Magnetic catalytic material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 92
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 91
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 60
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims abstract description 20
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 20
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 20
- 239000001509 sodium citrate Substances 0.000 claims abstract description 20
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 20
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 20
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 20
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 20
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 20
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 19
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 19
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 19
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 19
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims description 95
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 33
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 28
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- 238000005406 washing Methods 0.000 description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- -1 Transition Metal Sulfides Chemical class 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910008813 Sn—Si Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
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- 230000005389 magnetism Effects 0.000 description 1
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- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- B01J35/33—
-
- B01J35/394—
-
- B01J35/61—
Abstract
The invention relates to the field of magnetic catalytic materials, in particular to MnFe 2 O 4 @Mo x Sn 1‑x S 2 The magnetic catalytic material is prepared by selecting ferric acetate, manganese acetate, trisodium citrate and sodium polyacrylate to obtain MnFe with uniform size and enriched chemical bonds on the surface 2 O 4 And (3) granules. By matching the synergistic effect of sodium molybdate, stannic chloride, thioacetamide, ethanol and acetic acid, the method adopts one step method to prepare MnFe 2 O 4 The composite Mo is obtained on the surface of the particles x Sn 1‑x S 2 A nanosheet structure. The invention has the advantages of cheap and easily obtained raw materials, simple synthesis process, low cost, short reaction period and no pollution to the environment. The prepared MnFe 2 O 4 @Mo x Sn 1‑x S 2 The magnetic catalytic material has the advantages of uniform size, adjustable size, good dispersion, high specific surface area and stable structure, and can be applied to catalysis.
Description
Technical Field
The invention relates to the field of magnetic functional composite materials, in particular to MnFe 2 O 4 @Mo x Sn 1-x S 2 Magnetic catalytic material and its preparation method.
Background
In MoS 2 The material is represented by Transition Metal Sulfides (TMDs) as MX 2 A compound of the type (I) wherein M is a transition metal element of the fourth, fifth or sixth period in the periodic Table of the elements, and X is an chalcogen element selected from the group consisting of S, se and Te. TMDs are direct band gap materials, the forbidden band width can be adjusted along with the layer thickness, and the material has a layered structure, a large specific surface area, good flexibility and high thermal stability. MoS 2 The forbidden bandwidth is adjustable depending on the number of layers between 1.2-1.9 eV, the mobility is higher at room temperature, and the method is widely applied to the fields of photoelectric devices, mechanical lubrication, catalysis, semiconductor materials and the like. However, the band gap width is limited, and the corresponding performance cannot be further improved. SnS 2 The Sn-Si semiconductor material is an n-type semiconductor material with the band gap width of 2.2-2.5eV, each layer of Sn atoms is connected with S atoms through stronger Sn-S covalent bonds, and the layers are connected through weaker van der Waals force. The photocatalyst has the advantages of rich reserves, low price, high photocatalytic efficiency, large energy storage capacity and the like, and has wide application prospects in the fields of photoelectric detection, solar cells and energy storage.
In recent years, the controllable physicochemical properties of the nanocomposite material with the core-shell structure have become a research hotspot in the field of nano research, and have received more and more attention from scientists. 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. Prior art has been on MoS 2 And SnS 2 The preparation method is complex, and the prepared product has uneven appearance, which is not beneficial to improving the photoelectric property and the catalytic property.
Disclosure of Invention
The invention aims to solve the primary technical problem of providing uniform MnFe with simple process, low cost and short reaction period 2 O 4 @Mo x Sn 1-x S 2 A preparation method of a magnetic catalytic material.
MnFe 2 O 4 @Mo x Sn 1-x S 2 The preparation method of the magnetic catalytic material comprises the following steps:
dissolving iron acetate and manganese acetate in ethylene glycol, and stirring to form a mixed solution A;
adding a certain amount of trisodium citrate and sodium polyacrylate 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 MnFe 2 O 4 ；
Dissolving a certain amount of sodium molybdate, stannic chloride and thioacetamide into a solution of ethanol and acetic acid (according to a certain proportion), and then adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion;
step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, and reacting for a plurality of hours at a certain temperature to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Further, the ratio of the amount of the substances of the iron acetate and the manganese acetate in the first step is 1:1-5:1; stirring for 10-60min; the concentration of the solution A is 0.02-1mol/L;
further, the molar ratio of the trisodium citrate to the sodium polyacrylate in the second step is 0:1-5:1; stirring for 10-60min; by selecting the proportion, the uniformity and the density of adsorption bonds on the surface of the particles at the later stage can be improved; particles prepared in excess of the above ratio have poor uniformity;
further, the reaction temperature of the third step is 120-200 ℃; the reaction time is 8-20h;
further, the molar ratio of the sodium molybdate to the stannic chloride in the step four is 1:2-2:1; the amount of thioacetamide is 0.01875 to 1.875g; the volume ratio of ethanol to acetic acid is 30-10; spherical MnFe 2 O 4 The amount of (B) is 0.05-0.5g; through the selection of the proportion range, the particles which have high dispersity, are not aggregated and have uniform flaky sizes can be obtained in the later period; particles prepared outside the above ratio or range are heavily aggregated, or have uneven flake sizes;
further, the reaction temperature of the fifth step is 160-240 ℃; the reaction time is 12-30h.
MnFe prepared by the preparation method 2 O 4 @Mo x Sn 1-x S 2 Magnetic catalytic material, mnFe 2 O 4 @Mo x Sn 1-x S 2 The size of the magnetic catalytic material is 1-4 mu m, and the MnFe 2 O 4 @Mo x Sn 1-x S 2 The magnetic catalytic material is of a spherical structure, the surface of the spherical structure is of a sheet structure, and the thickness of the sheet structure is 10-70nm.
The invention has the beneficial effects that: mnFe of the invention 2 O 4 @Mo x Sn 1-x S 2 The preparation method of the magnetic catalytic material realizes MnFe through reasonable process control 2 O 4 @Mo x Sn 1-x S 2 And (3) preparing the magnetic catalytic material. MnFe with chemical bonds enriched on the surface and uniform size is obtained by selecting iron acetate, manganese acetate, trisodium citrate and sodium polyacrylate 2 O 4 And (3) granules. By matching the synergistic effect of sodium molybdate, stannic chloride, thioacetamide, ethanol and acetic acid, the method adopts one step method to prepare MnFe 2 O 4 The composite Mo is obtained on the surface of the particles x Sn 1-x S 2 A nanosheet structure. The invention has the advantages of cheap and easily obtained raw materials, simple synthesis process, low cost, short reaction period and no pollution to the environment. The prepared MnFe 2 O 4 @Mo x Sn 1-x S 2 The magnetic catalytic material has the advantages of uniform size, adjustable size, good dispersion, high specific surface area, stable structure, wide composite material bandwidth, and good photoelectric property, and can be applied to catalysis and the like.
Drawings
FIG. 1 is MnFe prepared in example 1 2 O 4 @Mo x Sn 1-x S 2 Scanning electron micrographs of magnetic catalytic materials.
FIG. 2 is MnFe prepared in example 1 2 O 4 @Mo x Sn 1-x S 2 Scanning electrode of magnetic catalytic materialAnd (4) a sub-microscope photograph. Detailed Description
The following examples are presented to further illustrate the methods described herein, but are not intended to limit the invention to these examples.
Example 1:
MnFe 2 O 4 @Mo x Sn 1-x S 2 The preparation method of the magnetic catalytic material comprises the following steps: step one, dissolving 2.25mmol of ferric acetate and 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
FIGS. 1 and 2 are each MnFe prepared in this example 2 O 4 @Mo x Sn 1-x S 2 SEM image of magnetic catalytic material, and MnFe prepared from the SEM image 2 O 4 @Mo x Sn 1-x S 2 The magnetic catalytic material has good dispersibility and uniform size, the size is 1-4 mu m, and the MnFe 2 O 4 @Mo x Sn 1-x S 2 The magnetic catalytic material is of a spherical structure, the surface of the spherical structure is of a sheet structure, and the thickness of the sheet structure is 10-70nm.
MnFe obtained by the present invention 2 O 4 @Mo x Sn 1-x S 2 The magnetic catalytic material realizes MnFe through reasonable process control 2 O 4 @Mo x Sn 1-x S 2 And (3) preparing the magnetic catalytic material. MnFe with enriched chemical bonds on the surface and uniform size is obtained by selecting iron acetate, manganese acetate, trisodium citrate and sodium polyacrylate in specific proportion 2 O 4 And (3) granules. Through the synergistic effect of sodium molybdate, stannic chloride, thioacetamide, ethanol and acetic acid in a specific ratio, the MnFe is processed by a one-step method 2 O 4 The composite Mo is obtained on the surface of the particles x Sn 1-x S 2 The nano-sheet structure does not need the traditional fractional step method for respective preparation or the preparation of a surfactant. The invention has the advantages of cheap and easily obtained raw materials, simple synthesis process, low cost, short reaction period and no pollution to the environment. The prepared MnFe 2 O 4 @Mo x Sn 1-x S 2 The magnetic catalytic material has the advantages of uniform size, adjustable size, good dispersion, high specific surface area and stable structure, and is beneficial to the application of catalytic performance.
Example 2:
this example differs from example 1 in that the amounts of iron acetate and manganese acetate were changed to 1.5 and 3mmol in step one, otherwise the same as example 1, specifically as follows: step one, dissolving 1.5mmol of ferric acetate and 3mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic treatmentDispersing; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 3:
the difference between this example and example 1 is that the amount of ethylene glycol in step one was changed to 30ml, and the other steps are the same as in example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 4.5mmol of manganese acetate in 30ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 4:
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 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 30min to form a mixed solution A; step two, adding 4.5mmol trisodium citrate and 0.45g sodium polyacrylate into the mixed solution A, stirring for 20min,forming 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 5:
this example differs from example 1 in that the amounts of trisodium citrate and sodium polyacrylate in step two were changed to 3mmol and 0.3g, and the other steps are the same as in example 1, as follows: step one, dissolving 2.25mmol of ferric acetate and 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 3mmol of trisodium citrate and 0.3g of sodium polyacrylate 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 200 ℃, centrifuging after the reaction kettle is naturally cooled to room temperature, washing the reaction kettle with ethanol and deionized water for multiple times respectively, and dryingTo obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 6:
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 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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, 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 7:
this example differs from example 1 in that the reaction temperature was changed to 160 ℃ 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 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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 washing with ethanol and deionized water respectivelyWashing for multiple times and drying to obtain spherical MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 8:
the difference between this example and example 1 is that the reaction time in step three was changed to 16h, and the rest is the same as example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 9:
this example differs from example 1 in the amount of sodium molybdate in step fourThe reaction solution was changed to 1mmol, which was the same as example 1, as follows: step one, dissolving 2.25mmol of ferric acetate and 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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 MnFe 2 O 4 (ii) a Step four, dissolving 1mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 10:
this example differs from example 1 in that ethanol and acetic acid were changed to 67ml and 3ml in step four, and the rest is the same as example 1, specifically as follows: step one, dissolving 2.25mmol of ferric acetate and 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 67ml of ethanol and 3ml of acetic acid, and then adding spherical MnFe 2 O 4 Form aMixing the solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at the temperature of 200 ℃, centrifuging after the reaction kettle is naturally cooled to the room temperature, respectively washing ethanol and deionized water for multiple times, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 11:
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 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; adding 4.5mmol of trisodium citrate and 0.45g of sodium polyacrylate 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 24 hours at 180 ℃, centrifuging after the reaction kettle is naturally cooled to room temperature, washing ethanol and deionized water for multiple times respectively, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Example 12:
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 4.5mmol of manganese acetate in 45ml of ethylene glycol, and stirring for 20min to form a mixed solution A; step two, adding 4.5mmol of trisodium citrate and 0.45g of polypropylene into the mixed solution AStirring sodium salt 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 MnFe 2 O 4 (ii) a Step four, dissolving 1.5mmol of sodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and adding spherical MnFe 2 O 4 Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, reacting for 18 hours at 180 ℃, centrifuging after the reaction kettle is naturally cooled to room temperature, washing ethanol and deionized water for multiple times respectively, and drying to obtain MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material.
Claims (2)
1. MnFe 2 O 4 @Mo x Sn 1-x S 2 The preparation method of the magnetic catalytic material is characterized by comprising the following steps of:
dissolving iron acetate and manganese acetate in ethylene glycol, and stirring to form a mixed solution A;
adding a certain amount of trisodium citrate and sodium polyacrylate 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 MnFe 2 O 4 ；
Dissolving a certain amount of sodium molybdate, stannic chloride and thioacetamide into the ethanol and acetic acid solution, and adding spherical MnFe 2 O 4 Forming a mixed solution C; ultrasonically dispersing for a certain time;
step five, adding the prepared mixed solution C into a tetrafluoroethylene reaction kettle, placing the reaction kettle in a thermostat, and reacting for a certain time at a certain temperature to obtain the tetrafluoroethylene-tetrafluoroethylene copolymerTo MnFe 2 O 4 @Mo x Sn 1-x S 2 A magnetic catalytic material;
the mass ratio of the iron acetate to the manganese acetate in the first step is 1:1-5:1; stirring for 10-60min; the concentration of the solution A is 0.02-1mol/L;
the molar ratio of the trisodium citrate to the sodium polyacrylate in the second step is 0:1-5:1 respectively; stirring for 10-60min;
the reaction temperature of the third step is 120-200 ℃; the reaction time is 8-20h;
the molar ratio of the sodium molybdate to the stannic chloride in the step four is 1:2-2:1; the amount of thioacetamide is 0.01875 to 1.875g; the volume ratio of ethanol to acetic acid is 30-10; spherical MnFe 2 O 4 The amount of (B) is 0.05-0.5g;
the reaction temperature of the fifth step is 160-240 ℃; the reaction time is 12-30h.
2. MnFe prepared by the preparation method of claim 1 2 O 4 @Mo x Sn 1-x S 2 Magnetic catalytic material, characterized in that: mnFe 2 O 4 @Mo x Sn 1-x S 2 The size of the magnetic catalytic material is 1-4 mu m, and the MnFe 2 O 4 @Mo x Sn 1-x S 2 The magnetic catalytic material is of a spherical structure, the surface of the spherical structure is of a sheet structure, and the thickness of the sheet structure is 10-70nm.
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Effective date of registration: 20231226 Address after: 315000 No. 55, Nandu Road, private science and Technology Park, Jiangkou street, Fenghua District, Ningbo City, Zhejiang Province Patentee after: Ningbo Roche Magnetic Industry Co.,Ltd. Address before: Room 713, Comprehensive Building, No. 586 West Ring Road, Keqiao Economic Development Zone, Qixian Street, Keqiao District, Shaoxing City, Zhejiang Province, 312000 (commitment declaration) Patentee before: SHAOXING YINCHUANG TECHNOLOGY Co.,Ltd. Effective date of registration: 20231226 Address after: Room 713, Comprehensive Building, No. 586 West Ring Road, Keqiao Economic Development Zone, Qixian Street, Keqiao District, Shaoxing City, Zhejiang Province, 312000 (commitment declaration) Patentee after: SHAOXING YINCHUANG TECHNOLOGY Co.,Ltd. Address before: 310000 no.928, No.2 street, Baiyang street, Hangzhou Economic and Technological Development Zone, Zhejiang Province Patentee before: ZHEJIANG SCI-TECH University |