CN108452813B - MoS2/SrFe12O19Preparation method of composite magnetic photocatalyst - Google Patents
MoS2/SrFe12O19Preparation method of composite magnetic photocatalyst Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 49
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 47
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title abstract description 15
- 229910002402 SrFe12O19 Inorganic materials 0.000 claims abstract description 65
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 13
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000001699 photocatalysis Effects 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 6
- 229940043267 rhodamine b Drugs 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 229910052724 xenon Inorganic materials 0.000 abstract description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 229910052712 strontium Inorganic materials 0.000 description 6
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910000859 α-Fe Inorganic materials 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005493 condensed matter Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002060 nanoflake Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- -1 transition metal sulfide Chemical class 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- PTISTKLWEJDJID-UHFFFAOYSA-N sulfanylidenemolybdenum Chemical compound [Mo]=S PTISTKLWEJDJID-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Images
Classifications
-
- B01J35/33—
-
- 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
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
MoS2/SrFe12O19A preparation method of a composite magnetic photocatalyst belongs to the field of nano inorganic catalytic materials. The invention adopts a hydrothermal method, firstly prepares a magnetic matrix SrFe12O19Then MoS is prepared2/SrFe12O19A composite magnetic photocatalyst. MoS2/SrFe12O19The composite magnetic photocatalyst has good crystallinity and better magnetic property. Under the irradiation of a xenon lamp simulating sunlight, 100mL of 10mg/L rhodamine B solution is degraded by 50mg of the prepared composite magnetic photocatalyst, the degradation rate within 90min is 95.2%, and the average recovery rate of the catalyst is 67%. The preparation method is simple and convenient in preparation process, easy to control, high in production efficiency, low in cost, green and environment-friendly in use process, and has outstanding advantages for treating industrial organic dye wastewater.
Description
Technical Field
The invention relates to a MoS2/SrFe12O19A preparation method of a composite magnetic photocatalyst belongs to the technical field of inorganic environment-friendly catalytic materials.
Background
The field of nano material photocatalysis is a new research field covering multidisciplinary intersection, and has become a hot research direction for solving fresh water pollution, industrial wastewater treatment and clean energy production technology. Wherein, molybdenum disulfide (MoS)2) The transition metal sulfide is widely applied to metal lubrication, lithium battery photodiodes, energy storage and conversion and the like by virtue of excellent physicochemical properties of the transition metal sulfide. At the same time, MoS2Has graphite-like layered structure and semiconductor properties, has the characteristics of large specific surface area, strong adsorption capacity and the like, and has MoS with different crystal structures2The forbidden band width is small and is only between 1.29eV and 1.9eV, so that valence band electrons can jump into a conduction band under the irradiation of visible light, holes are left, electron-hole pairs are generated, and the photocatalyst has good potential. Particularly when the particle size scale is reduced to nanometer level, MoS2The chemical stability of the material is not obviously weakened while the reactivity is improved, which shows that the material has excellent performance in photoelectrochemical reaction as a semiconductor materialCorrosion resistance, which is lacking in many semiconductor materials with narrow bandgaps. Thus, MoS2Has become a hot research object for developing novel photocatalysts.
For MoS, as reported in the relevant literature at present2The modification and the compound thereof have been studied more frequently, such as "Enhanced photocatalytic activity of ZnS nanoparticles loaded with MoS2A text of nanofilakes by self-assembly for improving (Physica B: Condensed Matter,2016,502:103-112), which adopts a hydrothermal method to prepare ZnS nano-particles and MoS respectively2Dissolving the nano-flake and the nano-flake in ethanol for mixing, and carrying out high-temperature high-pressure hydrothermal reaction on the mixed solution again to generate two compounds. The main problems of the method are that: (1) the preparation process needs three steps in total to obtain the composite product, and has the advantages of long preparation period, high cost, large energy consumption source and unsuitability for popularization; (2) only suitable for treating low-concentration organic wastewater, the photocatalyst is used for degrading 100mL of 5mg/L rhodamine B aqueous solution under the condition that the adding amount is 0.5g/L, and the degradation rate is about 90% after 90 min; (3) the composite catalyst has the problems of difficult recovery, easy secondary pollution and the like.
Based on this, it is considered that in the photocatalytic degradation of organic wastewater, particularly, large-scale treatment of wastewater often has a problem of difficult catalyst recovery. In order to prevent the secondary pollution caused by incomplete recovery of the photocatalyst and reduce the use cost, the photocatalyst is magnetized, and the separation and recovery are convenient. According to the related documents, the research work of the magnetic photocatalyst is in a development stage, and the magnetic substance is mainly selected from soft magnetic Fe3O4For magnetic substrates, for example, Chinese patent application CN 201610144309.7 discloses "a layered MoS2-Fe3O4The main preparation method is to combine the sol-gel method and explosion high-temperature impact to prepare MoS2The powder is firstly subjected to a layering reaction, then an oxidant is added for an intercalation reaction, and the generated intercalation MoS2Mixing with sol, and exploding to make Fe3O4Reduction and MoS occurs2And (4) stripping to obtain the magnetic layered composite product. The problems of the method are that: (1) the preparation conditions are harsh and complex, the explosion reaction is required in the preparation process, and the used explosive agent (picric acid) has high risk and is not suitable for large-scale industrial production; (2) the prepared composite magnetic material has low saturation magnetization and small coercive force, is easy to lose magnetism after being magnetized under the action of an external magnetic field, has poor recovery effect, and does not give data of recovery rate. Strontium ferrite (SrFe)12O19) As a hard magnetic material, the N-type semiconductor photocatalyst for a visible light driver has a small forbidden band width (1.8eV), and is similar to the traditional metal soft magnetic material Fe3O4Compared with the prior art, the material has the advantages of high coercive force and strong demagnetization resistance, and most importantly, the strontium reserves in China are sufficient and can be widely utilized. For this purpose, the invention uses SrFe12O19Preparing composite magnetic photocatalyst as magnetic matrix to increase MoS2The photocatalysis effect of the catalyst is endowed with magnetic performance, and the separation and the cyclic utilization are convenient.
Disclosure of Invention
The invention solves the technical problem of providing a MoS2/SrFe12O19The core of the preparation method of the composite magnetic photocatalyst lies in synthesizing the composite magnetic photocatalyst with excellent and stable magnetic performance and improving MoS2The photocatalytic activity is realized, and the problems of difficult recovery and secondary pollution to the environment are effectively solved. The preparation method has the advantages of simple and convenient preparation process, easy control, high production efficiency and low cost, has outstanding advantages on the treatment of industrial organic dye wastewater, and simultaneously expands MoS2And the utilization of the composite material photocatalyst thereof.
MoS of the invention2/SrFe12O19The preparation method of the composite magnetic photocatalyst comprises the following steps:
(1)SrFe12O19preparation of
0.7465g of SrCl were weighed out separately2·6H2O and 6.0545g FeCl3·6H2Dissolving the O reagent in 38mL of deionized water by ultrasonic waves to obtain a mixed solution A; 8.736g of NaOH reagent was weighed out and 20mL was used for the removalUltrasonically dissolving the seed water to obtain a solution B; slowly dripping the solution B into the mixed solution A in a water bath at the constant temperature of 20 ℃ under the magnetic stirring, continuously stirring for 15min, and fully mixing the solution to obtain SrFe12O19Precursor C; pouring the precursor C into a 100mL hydrothermal kettle, reacting at 200 ℃ for 24h, taking out, naturally cooling to room temperature, carrying out suction filtration, washing with deionized water until the filtrate is neutral, placing the filter cake into an oven at 80 ℃ for drying for 12h, taking out, and grinding to obtain SrFe12O19。
(2)MoS2/SrFe12O19Preparation of
0.4319g of MoO was weighed out separately3And 0.8746g of KSCN reagent, adding into 60mL of deionized water, carrying out ultrasonic treatment for 15min, and mechanically stirring for 30min to fully mix to obtain a solution A; SrFe is generated according to theory12O19The mass percentage of the SrFe in the compound is 5 wt% -15 wt%, and the prepared SrFe is weighed12O19Adding the powder into the solution A, continuously mechanically stirring for 1h to obtain a suspension B, putting the suspension B into a 100mL hydrothermal kettle, reacting for 24h at 200 ℃, taking out, cooling to room temperature, performing suction filtration, alternately washing with deionized water and absolute ethyl alcohol for several times, drying the filter cake in an 80 ℃ oven for 12h, and grinding to obtain the MoS2/SrFe12O19。
By adopting the technical scheme, the invention mainly has the following effects:
(1) MoS prepared by the method of the invention2/SrFe12O19The composite magnetic photocatalyst has higher photocatalytic activity, 100mL of rhodamine B solution with the concentration of 10mg/L is degraded by the optimal composite magnetic photocatalyst prepared by 50mg under the irradiation of a simulated sunlight xenon lamp, the degradation rate reaches 95.2 percent at 90min, and is higher than the data reported by' Physica B: Condensed Matter,2016,502:103-2/SrFe12O19The composite magnetic photocatalyst has degradation advantage for high-concentration dyes.
(2) The composite magnetic photocatalyst MoS prepared by the method2/SrFe12O19Can be used under the action of external magnetic fieldAnd secondary recovery and reuse.
(3) The method adopts a hydrothermal method, is simple and convenient to operate, safe and environment-friendly, high in production efficiency and suitable for popularization.
Drawings
FIG. 1 shows SrFe12O19、MoS2/SrFe12O19And MoS2X-ray diffraction patterns of (a);
FIG. 2 shows MoS2/SrFe12O19SEM image of field emission scanning electron microscope;
FIG. 3 shows MoS2、MoS2/SrFe12O19And SrFe12O19An infrared spectrum of (1);
FIG. 4 shows SrFe12O19And MoS2/SrFe12O19Magnetic hysteresis loop diagram of (1).
Detailed Description
The present invention will be further described with reference to the following specific embodiments.
Example 1
MoS2/SrFe12O19The preparation method of the composite magnetic photocatalyst comprises the following specific steps:
(1)SrFe12O19preparation of
0.7465g of SrCl were weighed out separately2·6H2O and 6.0545g FeCl3·6H2Dissolving the O reagent in 38mL of deionized water by ultrasonic waves to obtain a mixed solution A; 8.736g of NaOH reagent is weighed and dissolved by 20mL of deionized water through ultrasound to obtain solution B; slowly dripping the solution B into the mixed solution A under the action of constant-temperature 20 ℃ water bath and magnetic stirring, and continuously stirring for 15min until the solution is fully mixed to obtain SrFe12O19Precursor C; pouring the precursor C into a 100mL hydrothermal kettle, reacting at 200 ℃ for 24h, taking out, naturally cooling to room temperature, carrying out suction filtration, washing with deionized water until the filtrate is neutral, placing the filter cake into an oven at 80 ℃ for drying for 12h, taking out, and grinding to obtain SrFe12O19。
(2)MoS2/SrFe12O19Preparation of
0.4319g of MoO was weighed out separately3And 0.8746g of KSCN reagent, adding into 60mL of deionized water, carrying out ultrasonic treatment for 15min, and mechanically stirring for 30min to fully mix to obtain a solution A; SrFe is generated according to theory12O19The prepared SrFe is weighed according to the mass percent of 5 wt% in the compound12O19Adding the powder into the solution A, continuously mechanically stirring for 1h to obtain a suspension B, putting the suspension B into a 100mL hydrothermal kettle, reacting for 24h at 200 ℃, taking out, cooling to room temperature, performing suction filtration, alternately washing with deionized water and absolute ethyl alcohol for several times, drying the filter cake in an 80 ℃ oven for 12h, and grinding to obtain the MoS2/SrFe12O19。
Example 2
MoS2/SrFe12O19The preparation method of the composite magnetic photocatalyst comprises the following specific steps:
(1) same as in step (1) of example 1.
(2)MoS2/SrFe12O19Preparation of
0.4319g of MoO was weighed out separately3And 0.8746g of KSCN reagent, adding into 60mL of deionized water, carrying out ultrasonic treatment for 15min, and mechanically stirring for 30min to fully mix to obtain a solution A; SrFe is generated according to theory12O19The prepared SrFe is weighed up according to the mass percentage of 10 wt% in the compound12O19Adding the powder into the solution A, continuously mechanically stirring for 1h to obtain a suspension B, putting the suspension B into a 100mL hydrothermal kettle, reacting for 24h at 200 ℃, taking out, cooling to room temperature, performing suction filtration, alternately washing with deionized water and absolute ethyl alcohol for several times, drying the filter cake in an 80 ℃ oven for 12h, and grinding to obtain the MoS2/SrFe12O19。
Example 3
MoS2/SrFe12O19The preparation method of the composite magnetic photocatalyst comprises the following specific steps:
(1) same as in step (1) of example 1.
(2)MoS2/SrFe12O19Preparation of
0.4319g of MoO was weighed out separately3And 0.8746g of KSCN reagent, adding into 60mL of deionized water, carrying out ultrasonic treatment for 15min, and mechanically stirring for 30min to fully mix to obtain a solution A; SrFe is generated according to theory12O19The prepared SrFe is weighed according to the mass percent of 15 wt% in the compound12O19Adding the powder into the solution A, continuously mechanically stirring for 1h to obtain a suspension B, putting the suspension B into a 100mL hydrothermal kettle, reacting for 24h at 200 ℃, taking out, cooling to room temperature, performing suction filtration, alternately washing with deionized water and absolute ethyl alcohol for several times, drying the filter cake in an 80 ℃ oven for 12h, and grinding to obtain the MoS2/SrFe12O19。
Results of the experiment
MoS prepared in example 22/SrFe12O19The catalytic degradation activity is optimal. For ease of comparison, MoS was prepared2And (3) sampling. MoS2The preparation method is that in the step (2) of the example 2, SrFe is not added12O19。
SrFe prepared by the invention12O19、MoS2/SrFe12O19And MoS2The XRD characterization of (A) is as shown in figure 1, wherein (a) is SrFe12O19The characteristic peaks of 2-Theta at 23.19 degrees, 30.39 degrees, 31.02 degrees, 32.36 degrees, 34.22 degrees, 37.18 degrees, 40.43 degrees, 42.53 degrees, 55.18 degrees, 55.82 degrees, 57.46 degrees and 63.12 degrees are respectively assigned to the M-type strontium ferrite SrFe12O19(JCPDS card No.33-1340) (006), (110), (008), (107), (114), (203), (205), (206), (217), (0014), (218), and (220) crystal planes; in the figure, (c) represents MoS22-Theta at 14.37 DEG, 29.02 DEG, 32.67 DEG and 58.33 DEG, respectively corresponding to the MoS form 2H molybdenum sulphide in standard cards2(JCPDS card No.37-1492) crystal planes of (002), (004), (100) and (110); by way of comparison, FIG. (b) is a MoS prepared by the method of the invention2/SrFe12O19A composite magnetic photocatalyst having a characteristic X-ray diffraction peak associated with the above SrFe12O19And MoS2Characteristic peaks ofCorrespondingly, each peak shape is obvious, sharp and symmetrical, which indicates that the product is completely crystallized, the arrangement of mass points in the crystal is regular, and SrFe exists in a spectrogram12O19Has a diffraction peak of MoS2Diffraction peak of (2) indicating MoS2/SrFe12O19The composite magnetic photocatalysis is composed of hexagonal phase crystal system 2H type molybdenum sulfide and M type strontium ferrite, and has the relevant characteristics and stable structure.
The characterization result of SEM is shown in FIG. 2, which is MoS from left to right2、SrFe12O19And MoS2/SrFe12O19. It can be seen that the MoS prepared by the hydrothermal method2The shape of the SEM selected area is in a flower ball cluster shape, the SEM selected area is formed by stacking flower balls formed by ultrathin flocculent layers one by one, and a thin layer can be clearly seen in the figure under the visible condition that the magnification is 1 mu m; in the figure, SrFe12O19The SEM appearance is regular hexagon sheet layer, the thickness of each sheet layer is about 0.196-0.332 mu M, the appearance is complete, no impurity is generated, and the appearance characteristic is consistent with the appearance characteristic of the M-type strontium ferrite corresponding to the XRD representation result; MoS in the figure2/SrFe12O19SEM selective area morphology of the composite magnetic photocatalyst shows that in MoS2SrFe is mixed in the ball cluster12O19The regular hexagon lamella can be seen in the figure, the composite sample simultaneously meets the characteristic appearance of molybdenum disulfide and strontium ferrite, and the MoS prepared by the method is proved to be successfully prepared2/SrFe12O19The magnetic photocatalyst is compounded, and the product has obvious appearance characteristics.
MoS prepared by the method of the invention2、MoS2/SrFe12O19And SrFe12O19The infrared spectrum of the sample is characterized as shown in FIG. 3, and the wave number in the characteristic region is 3447.4cm-1、1639.5cm-1The strong absorption peak is an absorption vibration peak formed by the stretching vibration and bending vibration of hydroxyl O-H of the composite oxide on the surface of the tested sample for absorbing water; at 2913.7cm-1The left and right absorption peaks are caused by the stretching vibration of the C-H bond; and 2347cm-1Left and right weak absorption peaksSupposedly CO2Due to antisymmetric telescoping; wherein MoS can be seen from the characteristic absorption peak displayed by the fingerprint area2/SrFe12O19The composite magnetic photocatalyst is 435.5cm-1、 548.4cm-1And 586.8cm-1The absorption peak is attributed to SrFe12O19Characteristic absorption peak of (a); at 418.9cm-1Has an absorption peak of Mo-S bond which is close to 457.2cm-1All absorption peaks are attributed to MoS2Other miscellaneous peaks are not shown in the spectrogram, the characterization result is consistent with the literature, and the MoS is proved to be in the invention2/SrFe12O19The preparation method of the composite magnetic photocatalyst is practical and effective.
The photocatalytic experiment carried out by combining the characterization results shows that the MoS prepared by the method disclosed by the invention2/SrFe12O19Composite magnetic photocatalyst SrFe12O19When the mass percent of the compound is 10 wt%, under the irradiation of a simulated sunlight xenon lamp, 100mL of 10mg/L rhodamine B solution is degraded by using 50mg of prepared composite magnetic photocatalyst, and the degradation rate of rhodamine B in 90min reaches 95.2%, which shows that the MoS prepared by the method is adopted2/SrFe12O19The composite magnetic photocatalyst has higher photocatalytic activity, has stronger utilization, conversion and absorption effects on simulated sunlight, can accelerate the generation of electron-hole pairs, enables the holes to react with water to generate OH free radicals with better reaction activity, degrades dyes into inorganic ions and organic micromolecules, and keeps the degradation rate of rhodamine B above 70 percent after being recycled for many times.
SrFe12O19And MoS2/SrFe12O19The results of the magnetic property parameter test are shown in FIG. 4, SrFe12O19A saturation magnetization (Ms) of 58.08emu/g and a coercivity (Hci) of 793.4 Oe; MoS2/SrFe12O19The saturation magnetization is 10.14emu/g, and the coercive force is 1407.7 Oe; the product prepared by the method has stronger magnetic performance advantages, particularly the prepared composite sample has obviously improved coercive force, is beneficial to recycling of the photocatalyst, is green and environment-friendly, and hasEffectively solves the problem of secondary pollution to the environment after the catalyst is used.
The above examples describe the preparation process, the main features and the advantages of the present invention. The present invention is not limited to the above-described embodiments, and the present invention can be continuously modified without departing from the scope of the principle and method of the present invention, which falls within the protection scope of the present invention.
Claims (2)
1. MoS2/SrFe12O19The preparation method of the composite magnetic photocatalyst is characterized by comprising the following steps:
(1)SrFe12O19preparation of
0.7465g of SrCl were weighed out separately2·6H2O and 6.0545g FeCl3·6H2Dissolving the O reagent in 38mL of deionized water by ultrasonic waves to obtain a mixed solution A; 8.736g of NaOH reagent is weighed and dissolved by 20mL of deionized water through ultrasound to obtain solution B; slowly dripping the solution B into the mixed solution A in a water bath at the constant temperature of 20 ℃ under the magnetic stirring, continuously stirring for 15min, and fully mixing the solution to obtain SrFe12O19Precursor C; pouring the precursor C into a 100mL hydrothermal kettle, reacting at 200 ℃ for 24h, taking out, naturally cooling to room temperature, carrying out suction filtration, washing with deionized water until the filtrate is neutral, placing the filter cake into an oven at 80 ℃ for drying for 12h, taking out, and grinding to obtain SrFe12O19；
(2)MoS2/SrFe12O19Preparation of
0.4319g of MoO was weighed out separately3And 0.8746g of KSCN reagent, adding into 60mL of deionized water, carrying out ultrasonic treatment for 15min, and mechanically stirring for 30min to fully mix to obtain a solution A; SrFe is generated according to theory12O19The mass percentage of the SrFe in the compound is 5 wt% -15 wt%, and the prepared SrFe is weighed12O19Adding the powder into the solution A, continuously mechanically stirring for 1h to obtain a suspension B, putting the suspension B into a 100mL hydrothermal kettle, reacting for 24h at 200 ℃, taking out, cooling to room temperature, performing suction filtration, alternately washing with deionized water and absolute ethyl alcohol for several times, drying the filter cake in an oven at 80 ℃ for 12h, and grinding to obtain the final productObtaining MoS2/SrFe12O19。
2. The MoS of claim 12/SrFe12O19The preparation method of the composite magnetic photocatalyst is characterized in that the composite magnetic photocatalyst is prepared by a hydrothermal method, has high photocatalytic activity and can be recovered by a magnetic medium.
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