CN111974420A - MnFe2O4@MoxSn1-xS2Magnetic catalytic material and preparation method thereof - Google Patents
MnFe2O4@MoxSn1-xS2Magnetic catalytic material and preparation method thereof Download PDFInfo
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- 229910017163 MnFe2O4 Inorganic materials 0.000 title claims abstract description 54
- 239000000463 material Substances 0.000 title claims abstract description 53
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 91
- 238000006243 chemical reaction Methods 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
- 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
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 18
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 18
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims description 96
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 34
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 28
- 230000035484 reaction time Effects 0.000 claims description 6
- 229910000708 MFe2O4 Inorganic materials 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 8
- 239000002131 composite material Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract description 3
- 239000002135 nanosheet Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 239000008367 deionised water Substances 0.000 description 24
- 229910021641 deionized water Inorganic materials 0.000 description 24
- 238000001035 drying Methods 0.000 description 24
- 238000005406 washing Methods 0.000 description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- 238000001816 cooling Methods 0.000 description 13
- 238000001132 ultrasonic dispersion Methods 0.000 description 13
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910052961 molybdenite Inorganic materials 0.000 description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910008813 Sn—Si Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 229910052798 chalcogen Inorganic materials 0.000 description 1
- 150000001787 chalcogens Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229940083542 sodium Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 description 1
- 150000003624 transition metals Chemical class 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 MnFe2O4@MoxSn1‑xS2The 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 surface2O4And (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 MnFe2O4The composite Mo is obtained on the surface of the particlesxSn1‑xS2A 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 MnFe2O4@MoxSn1‑xS2The magnetic catalytic material has uniform size and adjustable sizeGood dispersion, high specific surface area and stable structure, and can be used for catalysis.
Description
Technical Field
The invention relates to the field of magnetic functional composite materials, in particular to MnFe2O4@MoxSn1-xS2Magnetic catalytic material and its preparation method.
Background
In MoS2The material is a Transition Metal Sulfide (TMDs) which is MX2The compound of type (I) is a transition metal element in the fourth, fifth or sixth period of the periodic table, and X represents 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. MoS2The forbidden band width is adjustable between 1.2 and 1.9e V depending on the number of layers, the mobility is high 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. SnS2The 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. There is prior art on MoS2And SnS2The 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 period2O4@MoxSn1-xS2A preparation method of a magnetic catalytic material.
MnFe2O4@MoxSn1-xS2The 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 MnFe2O4；
Dissolving a certain amount of sodium molybdate, stannic chloride and thioacetamide into the solution of ethanol and acetic acid (according to a certain proportion), and then adding spherical MnFe2O4Forming 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 several hours at a certain temperature to obtain MnFe2O4@MoxSn1-xS2Magnetic propertyA catalytic material.
Further, the amount ratio of the substances of the iron acetate and the manganese acetate in the step one is 1:1-5: 1; stirring for 10-60 min; the concentration of the solution A is 0.02-1 mol/L;
further, the molar ratio of the trisodium citrate to the sodium polyacrylate in the second step is 0:1-5:1 respectively; stirring for 10-60 min; 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 proportions above have poor uniformity;
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 stannic chloride in the step four is 1:2-2: 1; the amount of thioacetamide is 0.01875 g to 1.875 g; the volume ratio of the ethanol to the acetic acid is 30:1-10: 1; spherical MnFe2O4The amount of (B) is 0.05-0.5 g; 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 step five is 160-240 ℃; the reaction time is 12-30 h.
MnFe prepared by the preparation method2O4@MoxSn1-xS2Magnetic catalytic material, MnFe2O4@MoxSn1-xS2The size of the magnetic catalytic material is 1-4 μm, and the MFe2O4@MoxSn1-xS2The 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 10-70 nm.
The invention has the beneficial effects that: MnFe of the invention2O4@MoxSn1-xS2The preparation method of the magnetic catalytic material realizes MnFe through reasonable process control2O4@MoxSn1-xS2And (3) preparing the magnetic catalytic material. By selecting iron acetate, manganese acetate, trisodium citrate, sodium polyacrylateMnFe with uniform size and enriched chemical bonds on the surface is obtained2O4And (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 MnFe2O4The composite Mo is obtained on the surface of the particlesxSn1-xS2A 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 MnFe2O4@MoxSn1-xS2The 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.
Description of the drawings FIG. 1 is MnFe prepared in example 12O4@MoxSn1-xS2Scanning electron micrographs of magnetic catalytic material. FIG. 2 is MnFe prepared in example 12O4@MoxSn1-xS2Scanning electron micrographs of magnetic catalytic material. Detailed description the methods described herein are further illustrated by the following specific examples, but are not intended to be limiting.
Example 1:
MnFe2O4@MoxSn1-xS2The 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 MnFe2O4(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 then addingSpheroidal MnFe2O4Forming 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 ethanol and deionized water for multiple times respectively, and drying to obtain MFe2O4@MoxSn1-xS2A magnetic catalytic material.
FIGS. 1 and 2 are each MnFe prepared in this example2O4@MoxSn1-xS2SEM image of magnetic catalytic material, from which the MFe prepared can be seen2O4@MoxSn1-xS2The magnetic catalytic material has good dispersibility and relatively uniform size, the size is 1-4 mu m, and the MFe2O4@MoxSn1-xS2The 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 10-70 nm.
MnFe obtained by the present invention2O4@MoxSn1-xS2The magnetic catalytic material realizes MnFe through reasonable process control2O4@MoxSn1-xS2And (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 proportion2O4And (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 method2O4The composite Mo is obtained on the surface of the particlesxSn1-xS2The 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 MnFe2O4@MoxSn1-xS2The 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 MnFe2O4(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 MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2A magnetic catalytic material.
Example 3:
this example differs from example 1 in that the amount of ethylene glycol was changed to 30ml in step one, 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 MnFe2O4(ii) a Step four, 1.5mmol ofSodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide were dissolved in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and spherical MnFe was added2O4Forming 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 MnFe2O4@MoxSn1-xS2A 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; 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 MnFe2O4(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 MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2A magnetic catalytic material.
Example 5:
this example differs from example 1 in that the amounts of trisodium citrate and sodium polyacrylate were changed to 3mmol and 0.3g in step two, otherwise the same as example 1, as follows: step oneDissolving 2.25mmol of iron 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 MnFe2O4(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 MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2A 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 MnFe2O4(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 MnFe2O4Forming a mixed solution C, and performing ultrasonic dispersion; step five, adding the prepared mixed solution C intoPutting the reaction kettle in a tetrafluoroethylene reaction kettle, reacting for 24 hours at 200 ℃ in a constant temperature box, naturally cooling the reaction kettle to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain MnFe2O4@MoxSn1-xS2A 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, washing ethanol and deionized water for multiple times respectively, and drying to obtain spherical MnFe2O4(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 MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2A 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 intoPutting the reaction kettle into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, reacting for 16h 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 MnFe2O4(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 MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2A magnetic catalytic material.
Example 9:
this example is different from example 1 in that the amount of sodium molybdate in step four was changed to 1mmol, respectively, and the other steps are 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 MnFe2O4(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 MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2Magnetic propertyA 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 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 MnFe2O4(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 adding spherical MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2A 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 MnFe2O4(ii) a Step four, 1.5mmol ofSodium molybdate, 1.5mmol of stannic chloride and 0.1875g of thioacetamide were dissolved in a mixed solution of 33.5ml of ethanol and 1.5ml of acetic acid, and spherical MnFe was added2O4Forming 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 MnFe2O4@MoxSn1-xS2A 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; 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 MnFe2O4(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 MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2A magnetic catalytic material.
Claims (7)
1. MnFe2O4@MoxSn1-xS2The magnetic catalytic material and the preparation method thereof are characterized by comprising 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 MnFe2O4；
Dissolving a certain amount of sodium molybdate, stannic chloride and thioacetamide into the ethanol and acetic acid solution, and adding spherical MnFe2O4Forming 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 MnFe2O4@MoxSn1-xS2A magnetic catalytic material.
2. MnFe of claim 12O4@MoxSn1-xS2The preparation method of the magnetic catalytic material is characterized by comprising the following steps: the mass ratio of the iron acetate to the manganese acetate in the first step is 1:1-5: 1; stirring for 10-60 min; the concentration of the solution A is 0.02-1 mol/L.
3. MnFe of claim 12O4@MoxSn1-xS2The preparation method of the magnetic catalytic material is characterized by comprising the following steps: in the second step, the molar ratio of the trisodium citrate to the sodium polyacrylate is 0:1-5:1 respectively; the stirring time is 10-60 min.
4. MnFe of claim 12O4@MoxSn1-xS2The preparation method of the magnetic catalytic material 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. MnFe of claim 12O4@MoxSn1-xS2The preparation method of the magnetic catalytic material is characterized by comprising the following steps: the molar ratio of the sodium molybdate to the stannic chloride in the step IV is 1:2-2: 1; the amount of thioacetamide is 0.01875 g to 1.875 g; the volume ratio of the ethanol to the acetic acid is 30:1-10: 1; spherical MnFe2O4The amount of (B) is 0.05-0.5 g.
6. MnFe of claim 12O4@MoxSn1-xS2The preparation method of the magnetic catalytic material is characterized by comprising the following steps: the reaction temperature of the step five is 160-240 ℃; the reaction time is 12-30 h.
7. MnFe prepared by the preparation method according to any one of claims 1 to 62O4@MoxSn1-xS2Magnetic catalytic material, characterized in that: MFe2O4@MoxSn1-xS2The size of the magnetic catalytic material is 1-4 μm, and the MFe2O4@MoxSn1-xS2The 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 10-70 nm.
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