CN115121265A - Molybdenum disulfide/iron molybdate composite catalyst and preparation method and application thereof - Google Patents
Molybdenum disulfide/iron molybdate composite catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a molybdenum disulfide/iron molybdate composite catalyst, a preparation method and application thereof, wherein the preparation method comprises the following steps: adding ferric chloride hexahydrate and terephthalic acid into dimethylformamide, uniformly stirring by magnetic force, transferring into a hydrothermal kettle for hydrothermal reaction, cooling, and then sequentially washing, centrifuging and drying to obtain MIL-53(Fe) powder; adding MIL-53(Fe) powder into ultrapure water, stirring, adding ammonium molybdate tetrahydrate and thiourea, performing ultrasonic dispersion, transferring to a hydrothermal kettle for hydrothermal reaction, cooling, and then sequentially washing, centrifuging and drying to obtain the molybdenum disulfide/iron molybdate composite catalyst. The invention also comprises the composite catalyst prepared by the method and application thereof. The invention effectively solves the problems of low activation efficiency of iron catalysts, secondary water pollution caused by easy leaching of metal ions in catalysis, high energy consumption of traditional PMS activation, low pollutant degradation efficiency and the like.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a molybdenum disulfide/iron molybdate composite catalyst, and a preparation method and application thereof.
Background
The dye is widely applied to various industries such as textile, printing and dyeing, cosmetics, plastics, pharmacy, photography and the like. The annual global dye production exceeds 70 ten thousand tons. These non-biodegradable dyes are discharged into the water body of the natural stream due to the inefficient dyeing process, whereas the dyes present in industrial waste waters are mainly composed of toxic and carcinogenic substances that pose a serious threat to human beings and marine ecology. Therefore, it is important to treat and degrade the colored sewage before the colored sewage is discharged into natural water.
The PMS advanced oxidation technology has huge application potential in the aspect of removing the environment with difficultly-degradable pollutants. In this technique, activation of PMS due to the difference in catalyst properties can generate radicals and non-radicals, both of which exhibit excellent removal effects, and can oxidatively degrade organic contaminants into water and carbon dioxide. Due to certain chemical stability of PMS, a plurality of methods can be used for rapidly activating PMS, such as thermal activation, ultraviolet activation, microwave activation, transition metal activation and the like, wherein the transition metal activated PMS is considered to be an application method for degrading environmental pollutants with high efficiency and high applicability in operation aspect due to free input of external energy.
The traditional iron catalyst has the problems of low efficiency, easy influence of pH, metal leakage and the like in the field of PMS activation, the low catalytic activity of the traditional iron catalyst is not favorable for application universality, and how to improve the catalytic activity and stability of the traditional iron catalyst is an important problem to be solved at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a molybdenum disulfide/iron molybdate composite catalyst, a preparation method and application thereof, the catalyst has the advantages of simple preparation, high PMS (permanent magnet synchronous motor) activation efficiency and the like, and the problems of low activation efficiency of an iron catalyst, secondary water pollution caused by easy leaching of metal ions in catalysis, high energy consumption of traditional PMS activation, low pollutant degradation efficiency and the like are effectively solved.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the molybdenum disulfide/iron molybdate composite catalyst comprises the following steps:
(1) adding ferric chloride hexahydrate and terephthalic acid into dimethylformamide, uniformly stirring by magnetic force, transferring into a hydrothermal kettle for hydrothermal reaction, cooling, and then sequentially washing, centrifuging and drying to obtain MIL-53(Fe) powder;
(2) adding the MIL-53(Fe) powder obtained in the step (1) into ultrapure water, stirring, then adding ammonium molybdate tetrahydrate and thiourea, performing ultrasonic dispersion, transferring the mixture into a hydrothermal kettle for hydrothermal reaction, cooling, and then sequentially washing, centrifuging and drying to obtain the molybdenum disulfide/iron molybdate composite catalyst.
Further, in the step (1), the molar ratio of ferric chloride hexahydrate and terephthalic acid is 1:1, and the molar volume ratio of ferric chloride hexahydrate and dimethylformamide is 1:60 mol/mL.
Further, in the step (1), the mixture is magnetically stirred at the temperature of 20-25 ℃ and 500r/min at 400-.
Further, in the step (1), washing with ultrapure water and ethanol for 2-4 times respectively, centrifuging for 1-3min under the conditions of 11000 and 13000r/min, and drying at the temperature of 60-65 ℃.
Further, in the step (2), the mass-volume ratio of MIL-53(Fe) powder to ultrapure water is 0.1-0.3:50-70g/mL, and the molar ratio of ammonium molybdate tetrahydrate to thiourea is 1: 2-2.5.
Further, in the step (2), stirring for 20-30min at 20-25 ℃ and 500r/min at 400-50 kHz, ultrasonically dispersing for 20-30min at 40-50kHz, and carrying out hydrothermal reaction for 10h at 180 ℃.
Further, in the step (2), washing with ultrapure water and ethanol for 2-4 times respectively, centrifuging for 1-3min under the conditions of 11000 and 13000r/min, and drying at the temperature of 60-65 ℃.
The molybdenum disulfide/iron molybdate composite catalyst is prepared by the preparation method of the molybdenum disulfide/iron molybdate composite catalyst.
The application of the molybdenum disulfide/iron molybdate composite catalyst in degrading dye wastewater.
Further, the dye is at least one of rhodamine B, active black 5, active blue 19 and Congo red.
Further, the adding amount of the molybdenum disulfide/iron molybdate composite catalyst and the peroxymonosulfate is 0.15g/L and 0.5mM respectively, and the reaction is catalyzed and activated for 15-25min by magnetic stirring at the rotating speed of 400-500 r/min.
In summary, the invention has the following advantages:
1. the invention provides a method for forming a molybdenum disulfide/iron molybdate composite catalyst by deriving iron molybdate through iron MOF and simultaneously loading molybdenum disulfide nanosheets, wherein S vacancy of the composite catalyst is compared with MoS 2 The S vacancy of the monomer is enhanced to generate the effect that 1+1 is more than 2, the electron transfer rate of the PMS and molybdenum disulfide/iron molybdate composite catalyst is improved, the PMS can be rapidly activated to generate active species, and the dye wastewater is effectively removed.
2. According to the invention, by utilizing the idea of combining the MOF derivatization technology with the composite material, molybdenum disulfide is formed and loaded on the molybdenum disulfide and S vacancies are generated in the process of deriving iron molybdate from iron MOF, and the effective combination of the molybdenum disulfide and S vacancies obviously promotes the internal electron transfer in the PMS activation process, so that the degradation of pollutants is accelerated.
3. The molybdenum disulfide/iron molybdate composite catalyst prepared by synthesis is heterogeneous. Due to MoS 2 The introduction of the catalyst generates a vacancy, and the S vacancy is enhanced after hydrothermal treatment, so that the adsorption of PMS is easier, the electron transfer between PMS and the catalyst is promoted, and the production of singlet oxygen, sulfate radical and hydroxyl radical for degrading pollutants is accelerated. In addition, the catalyst is suitable for degradation of waste water with various different dyes, has high stability, can be repeatedly recycled, has no secondary pollution, and is an environment-friendly catalyst; extra additional energy is not needed in the catalytic degradation process, the process flow is simple, the cost is low, and the method has a wide prospect in the aspect of dye wastewater degradation.
Drawings
FIG. 1 shows MIL-53(Fe) and molybdenum disulfide/iron molybdate composite catalyst of example 1 and MoS obtained in comparative example 1 2 Scanning electron micrographs of the monomers;
FIG. 2 is an X-ray diffraction pattern of the molybdenum disulfide/iron molybdate composite catalyst obtained in example 1;
FIG. 3 is a graph showing the relationship between time and degradation efficiency of activated PMS for degrading rhodamine B by the molybdenum disulfide/iron molybdate composite catalyst obtained in examples 1 to 4;
FIG. 4 shows the degradation effect of the molybdenum disulfide/iron molybdate composite catalyst obtained in example 1 on different dyes in PMS;
FIG. 5 shows the effect of the molybdenum disulfide/iron molybdate composite catalyst obtained in example 1 on the cyclic treatment of rhodamine B in a PMS activation system.
Detailed Description
Example 1
A preparation method of the molybdenum disulfide/iron molybdate composite catalyst comprises the following steps:
(1) adding 0.674g of ferric chloride hexahydrate and 0.415g of terephthalic acid into 60mL of dimethylformamide, magnetically stirring uniformly at 20 ℃ and 400r/min, transferring into a hydrothermal kettle, carrying out hydrothermal reaction at 150 ℃ for 15h, cooling, washing with ultrapure water and ethanol for 3 times respectively, centrifuging at 12000r/min for 2min, and drying at 60 ℃ to obtain MIL-53(Fe) powder;
(2) adding 0.1g of MIL-53(Fe) powder obtained in the step (1) into ultrapure water, stirring for 20min at 20 ℃ and 400r/min, then adding 0.033g of ammonium molybdate tetrahydrate and 0.072g of thiourea, performing ultrasonic dispersion for 20min at the frequency of 45kHz, transferring to a hydrothermal kettle, performing hydrothermal reaction for 10h at the temperature of 180 ℃, washing for 3 times by using the ultrapure water and ethanol respectively after cooling, centrifuging for 2min at the condition of 12000r/min, and drying at the temperature of 60 ℃ to obtain the molybdenum disulfide/iron molybdate composite catalyst. MoS in molybdenum disulfide/iron molybdate composite catalyst 2 And FeMoO 4 In a mass ratio of 3: 10.
Example 2
A preparation method of the molybdenum disulfide/iron molybdate composite catalyst comprises the following steps:
(1) adding 0.674g of ferric chloride hexahydrate and 0.415g of terephthalic acid into 60mL of dimethylformamide, magnetically stirring uniformly at 20 ℃ and 450r/min, transferring into a hydrothermal kettle, carrying out hydrothermal reaction at 150 ℃ for 15h, cooling, washing with ultrapure water and ethanol for 3 times respectively, centrifuging at 12000r/min for 2min, and drying at 60 ℃ to obtain MIL-53(Fe) powder;
(2) adding 0.3g of MIL-53(Fe) powder obtained in the step (1) into ultrapure water, stirring for 30min at 20 ℃ and 450r/min, then adding 0.033g of ammonium molybdate tetrahydrate and 0.072g of thiourea, performing ultrasonic dispersion for 20min at the frequency of 45kHz, transferring into a hydrothermal kettle, performing hydrothermal reaction for 10h at the temperature of 180 ℃, washing for 3 times with the ultrapure water and ethanol respectively after cooling, centrifuging for 1-3min at 12000r/min, and drying at the temperature of 60 ℃ to obtain the molybdenum disulfide/iron molybdate composite catalyst. MoS in molybdenum disulfide/iron molybdate composite catalyst 2 And FeMoO 4 The mass ratio of (A) to (B) is 1: 10.
Example 3
A preparation method of the molybdenum disulfide/iron molybdate composite catalyst comprises the following steps:
(1) adding 0.674g of ferric chloride hexahydrate and 0.415g of terephthalic acid into 60mL of dimethylformamide, magnetically stirring uniformly at 25 ℃ and 500r/min, transferring into a hydrothermal kettle, carrying out hydrothermal reaction at 150 ℃ for 15h, cooling, washing with ultrapure water and ethanol for 3 times respectively, centrifuging at 12000r/min for 2min, and drying at 65 ℃ to obtain MIL-53(Fe) powder;
(2) adding 0.15g of MIL-53(Fe) powder obtained in the step (1) into ultrapure water, stirring for 30min at 25 ℃ and 500r/min, then adding 0.033g of ammonium molybdate tetrahydrate and 0.072g of thiourea, ultrasonically dispersing for 30min at the frequency of 50kHz, transferring into a hydrothermal kettle, carrying out hydrothermal reaction for 10h at the temperature of 180 ℃, washing for 3 times by using the ultrapure water and ethanol respectively after cooling, centrifuging for 2min at the condition of 12000r/min, and drying at the temperature of 65 ℃ to obtain the molybdenum disulfide/iron molybdate composite catalyst. MoS in molybdenum disulfide/iron molybdate composite catalyst 2 And FeMoO 4 The mass ratio of (A) to (B) is 1: 5.
Example 4
A molybdenum disulfide/iron molybdate composite catalyst is prepared by the following steps:
(1) adding 0.674g of ferric chloride hexahydrate and 0.415g of terephthalic acid into 60mL of dimethylformamide, magnetically stirring uniformly at 25 ℃ and 500r/min, transferring into a hydrothermal kettle, carrying out hydrothermal reaction at 150 ℃ for 15h, cooling, washing with ultrapure water and ethanol for 3 times respectively, centrifuging at 12000r/min for 2min, and drying at 65 ℃ to obtain MIL-53(Fe) powder;
(2) adding 0.12g of MIL-53(Fe) powder obtained in the step (1) into ultrapure water, stirring for 30min at 25 ℃ and 500r/min, then adding 0.066g of ammonium molybdate tetrahydrate and 0.143g of thiourea, ultrasonically dispersing for 30min at the frequency of 50kHz, transferring into a hydrothermal kettle, carrying out hydrothermal reaction for 10h at the temperature of 180 ℃, washing for 3 times by using the ultrapure water and ethanol respectively after cooling, centrifuging for 2min at 12000r/min, and drying at the temperature of 65 ℃ to obtain the molybdenum disulfide/iron molybdate composite catalyst. MoS in molybdenum disulfide/iron molybdate composite catalyst 2 And FeMoO 4 The mass ratio of (A) to (B) is 1: 2.
Comparative example 1
Weighing 0.033g of ammonium molybdate tetrahydrate and 0.072g of thiourea, simultaneously mixing the ammonium molybdate tetrahydrate and the thiourea in 60mL of ultrapure water, stirring for 30min under the condition of 500r/min until the ammonium molybdate and the thiourea are uniformly mixed, transferring the mixture into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 10h at 180 ℃, cooling, washing with ethanol, centrifuging to obtain precipitate, and finally drying for 12h in a 65 ℃ oven to obtain MoS 2 A monomer.
Examples of the experiments
MIL-53(Fe) and molybdenum disulfide/iron molybdate composite catalyst of example 1 and MoS obtained in comparative example 1 were obtained 2 The scanning electron micrograph of the monomer is shown in FIG. 1. An X-ray diffraction pattern of the molybdenum disulfide/iron molybdate composite catalyst obtained in example 1 was obtained as shown in fig. 2. Wherein, from left to right in FIG. 1, MIL-53(Fe) and MoS are sequentially 2 Monomer and molybdenum disulfide/iron molybdate composite catalyst.
As can be seen from FIG. 1, FeMoO derived from Fe MOF 4 The surface is covered with MoS 2 Nanosheets.
As can be seen from FIG. 2, FeMoO in the molybdenum disulfide/iron molybdate composite catalyst obtained by the invention 4 The sample has strong and obvious peaks, which indicates that the prepared rod-shaped FeMoO 4 Has good crystallinity and is compatible with standard FeMoO 4 Diffraction was almost identical (PDF #87-2367), with typical diffraction peaks at 23.01 °, 25.08 °, 26.16 °, 26.24 °, 26.97 °, 31.63 °, 33.46 ° and 33.52 ° at 2 θ ═ respectively, and FeMoO 4 The (021), (201), (220), (002), (-221), (112), (-222) and (-312) planes in (1).
The molybdenum disulfide/iron molybdate composite catalyst obtained in the embodiment 1-4 is adopted to degrade rhodamine B, the adding amount of the molybdenum disulfide/iron molybdate composite catalyst and the adding amount of the peroxymonosulfate are respectively 0.15g/L and 0.5mM, and the magnetic stirring is carried out at the rotating speed of 400r/min for catalytic activation reaction for 20 min. And obtaining a time-degradation efficiency relation diagram of the molybdenum disulfide/iron molybdate composite catalyst obtained in the embodiment 1-4 for activating PMS to degrade rhodamine B, wherein the time-degradation efficiency relation diagram is shown in figure 3. Wherein, the most right side in fig. 3 is MoS from top to bottom in sequence 2 、MIL-53、MoS 2 MIL-53-0.2 (example 3), MoS 2 MIL-53-0.1 (example 2), MoS 2 MIL-53-0.5 (example 4) and MoS 2 MIL-53-0.3 (example 1).
As can be seen from FIG. 3, the degradation efficiency of the composite catalysts prepared in examples 1 and 4 to rhodamine B in a PMS system is much higher than that of MIL-53(Fe) and MoS2 monomers; after the catalytic reaction is performed for 20min, the composite catalyst prepared in example 1 has the best effect, reaching 97.7%.
The degradation effect of the molybdenum disulfide/iron molybdate composite catalyst obtained in example 1 on different dyes in PMS is obtained, as shown in FIG. 4. Wherein, on the abscissa for 2min, RhB, RB19, RA5 and CR are arranged from top to bottom.
As can be seen from FIG. 4, the molybdenum disulfide/iron molybdate composite catalyst shows good degradation effect on various wastewater dyes, and is suitable for degradation of various dyes.
The effect of the molybdenum disulfide/iron molybdate composite catalyst obtained in example 1 on the cyclic treatment of rhodamine B in a PMS activation system is obtained, as shown in fig. 5.
As can be seen from fig. 5, after four cycles, the degradation effect of the molybdenum disulfide/iron molybdate composite catalyst on rhodamine B in the PMS activation system can still have 67.5% removal efficiency, which indicates that the molybdenum disulfide/iron molybdate composite catalyst has good catalytic stability and reusability in the PMS activation system.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (10)
1. A preparation method of a molybdenum disulfide/iron molybdate composite catalyst is characterized by comprising the following steps:
(1) adding ferric chloride hexahydrate and terephthalic acid into dimethylformamide, uniformly stirring by magnetic force, transferring into a hydrothermal kettle for hydrothermal reaction, cooling, and then sequentially washing, centrifuging and drying to obtain MIL-53(Fe) powder;
(2) adding the MIL-53(Fe) powder obtained in the step (1) into ultrapure water, stirring, then adding ammonium molybdate tetrahydrate and thiourea, performing ultrasonic dispersion, transferring the mixture into a hydrothermal kettle to perform hydrothermal reaction, cooling, and then sequentially washing, centrifuging and drying to obtain the molybdenum disulfide/iron molybdate composite catalyst.
2. The method for preparing a molybdenum disulfide/iron molybdate composite catalyst according to claim 1, wherein in the step (1), the molar ratio of the ferric chloride hexahydrate to the terephthalic acid is 1:1, and the molar volume ratio of the ferric chloride hexahydrate to the dimethylformamide is 1:60 mol/mL.
3. The method for preparing the molybdenum disulfide/iron molybdate composite catalyst as claimed in claim 1, wherein in the step (1), the mixture is magnetically stirred at the temperature of 20-25 ℃ and 500r/min 400-.
4. The method for preparing the molybdenum disulfide/iron molybdate composite catalyst as claimed in claim 1, wherein in the step (1), the catalyst is respectively washed by ultrapure water and ethanol for 2 to 4 times, centrifuged for 1 to 3min under the conditions of 11000 and 13000r/min, and dried at the temperature of 60 to 65 ℃.
5. The method for preparing the molybdenum disulfide/iron molybdate composite catalyst according to claim 1, wherein in the step (2), the mass-to-volume ratio of MIL-53(Fe) powder to ultrapure water is 0.1-0.3:50-70g/mL, and the molar ratio of ammonium molybdate tetrahydrate to thiourea is 1: 2-2.5.
6. The method for preparing the molybdenum disulfide/iron molybdate composite catalyst as claimed in claim 1, wherein in the step (2), the mixture is stirred for 20-30min at 20-25 ℃ and 500r/min 400-.
7. The method for preparing the molybdenum disulfide/iron molybdate composite catalyst as claimed in claim 1, wherein in the step (2), absolute ethyl alcohol is adopted for washing, centrifugation is carried out for 1-3min under the conditions of 11000-13000r/min, and drying is carried out at the temperature of 60-65 ℃.
8. A molybdenum disulfide/iron molybdate composite catalyst produced by the method of preparing a molybdenum disulfide/iron molybdate composite catalyst as set forth in any one of claims 1 to 7.
9. Use of the molybdenum disulfide/iron molybdate composite catalyst of claim 8 for degrading dye wastewater.
10. The method for preparing the catalyst comprises the steps of 9, wherein the adding amount of the molybdenum disulfide/iron molybdate composite catalyst and the adding amount of the peroxymonosulfate are respectively 0.15g/L and 0.5mM, and the magnetic stirring catalytic activation reaction is carried out for 15-25min at the rotating speed of 400-500 r/min.
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| CN116037163A (en) * | 2023-02-17 | 2023-05-02 | 江苏科技大学 | Iron-loaded molybdenum disulfide nanosphere catalytic material and preparation method thereof |
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| CN116375095A (en) * | 2023-04-13 | 2023-07-04 | 浙江新光药业股份有限公司 | Preparation method of ferric molybdate and application of ferric molybdate in photocatalytic degradation of pollutants in water |
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Cited By (3)
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| CN116173988A (en) * | 2022-11-21 | 2023-05-30 | 中国科学院生态环境研究中心 | Preparation and application of molybdenum disulfide-activated carbon piezoelectric catalyst |
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