CN109647444B - Metal organic composite multiphase Fenton catalyst, and preparation method and application thereof - Google Patents
Metal organic composite multiphase Fenton catalyst, and preparation method and application thereof Download PDFInfo
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- 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
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The invention provides a metal organic composite multiphase Fenton catalyst and a preparation method and application thereof. The preparation method is simple, and the prepared metal organic composite multiphase Fenton catalyst has the following advantages: (1) the catalyst has good degradation and removal effects on organic pollutants under the condition of neutral room temperature; (2) the active components of the catalyst are greatly exposed on the surface of the catalyst and have the effect of resisting pollutants and H2O2The contact is easy, and the influence of steric hindrance effect and capillary phenomenon is avoided; (3) the catalyst can not produce solid foreign matters such as iron mud and the like in the reaction process, does not need a foreign matter removing device, is convenient to separate water from the catalyst, has good stability, and is convenient to recycle.
Description
Technical Field
The invention belongs to the field of material preparation and application, and particularly relates to a metal organic composite multiphase Fenton catalyst, and a preparation method and application thereof.
Background
Iron-based fenton catalysts have been extensively studied and developed for the removal of difficult biodegradable contaminants in water. However, due to some inherent properties of iron, the existence of an electron circulation rate limiting step in the fenton reaction is caused, which also causes the bottleneck problems that the heterogeneous fenton catalyst has low activity under neutral conditions, and the hydrogen peroxide utilization rate is difficult to break through 50%.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a metal organic composite multiphase Fenton catalyst, and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for preparing a metal organic composite heterogeneous Fenton catalyst (MS-rGO NSs), comprising the steps of:
(1) mixing Na2MoO4And graphene oxide are dispersed and uniformly mixed in deionized water to obtain a mixed system E;
(2) will CH4N2S is added into the mixed system E, is stirred and evenly mixed, is subjected to ultrasonic treatment, and is subjected to hydrothermal reaction in a closed container with the temperature of 180-220 ℃ for 20-30 hours to obtain a mixed system F;
(3) and alternately washing the mixed system F by using deionized water and an organic solvent, drying, and grinding to obtain the metal-organic composite multiphase Fenton catalyst.
Preferably, the preparation method of the graphene oxide comprises the following steps:
under the ice bath below 0 ℃, slowly adding graphite powder into concentrated sulfuric acid, in the process of adding the graphite powder,keeping stirring state, mixing to obtain mixed system A, adding NaNO3Adding into the mixed system A, mixing to obtain mixed system B, adding KMnO4Slowly adding into the mixed system B, mixing, heating to 35-38 deg.C, stirring for 1-1.5 hr to obtain mixed system C;
(II) adding deionized water into the mixed system C, heating to 90-100 ℃, and stirring for 1-2 hours to obtain a mixed system D;
(III) reacting H2O2Adding the mixture into a mixed system D until the mixed system D becomes a golden brown suspension, cooling, performing solid-liquid separation, washing the solid substance with deionized water until the pH value of the washing liquid is 6-7 to obtain a solid substance A, drying the solid substance A at 50-70 ℃, performing copolymerization annealing treatment at the annealing treatment temperature of 340-360 ℃, and cooling to obtain the graphene oxide.
The method mainly uses reduced graphene oxide nano sheets (rGO NSs) synthesized by an improved Hummers method and annealing reduction treatment as a carrier and a multi-electron ligand, and sodium molybdate dihydrate (Na)2MoO4·2H2O) and thiourea (CH)4N2S) respectively serving as a molybdenum source and a sulfur source, and synthesizing the metal organic composite heterogeneous Fenton catalyst by a solvothermal method.
Preferably, Na2MoO4And the dosage of the graphene oxide is as follows by weight: 1000: 44-132, wherein the content of the graphene oxide in the mixed system E is 0.5-1.5 g/L.
More preferably, Na2MoO4And the dosage of the graphene oxide is as follows by weight: 1000: 88, wherein the content of the graphene oxide in the mixed system E is 1 g/L.
Preferably, CH in step (2)4The amount of NS is Na2MoO4And CH4N2The molar ratio of S is 1: 3-6.
More preferably, CH in step (2)4The amount of NS is Na2MoO4And CH4N2The molar ratio of S is 1: 5.
preferably, the closed container in the step (2) is a high-pressure reaction kettle.
Preferably, in the step (3), the organic solvent is absolute ethyl alcohol.
Preferably, in the step (3), the drying temperature is 80-100 ℃, and the drying time is 20-30 hours.
More preferably, in the step (3), the drying temperature is 100 ℃ and the drying time is 24 hours.
Preferably, in step (i) of the preparation method of graphene oxide, concentrated sulfuric acid, graphite powder, and NaNO3、KMnO4The dosage proportion is as follows: 230-240mL 98% concentrated sulfuric acid, 10.0-12.0g graphite powder, 50.0-52.0g NaNO3And 30.0-32.0g of KMnO4。
More preferably, in step (i) of the preparation method of graphene oxide, concentrated sulfuric acid, graphite powder and NaNO3、KMnO4The dosage proportion is as follows: 230mL of 98% concentrated sulfuric acid, 10.0g of graphite powder, and 50.0g of NaNO3And 30.0g of KMnO4。
Preferably, in the step (ii) of the preparation method of graphene oxide, deionized water is added to the mixed system C, the temperature is raised to 95 ℃, and the mixed system D is obtained by stirring for 1 to 2 hours.
Preferably, H in step (iii) of the method for preparing graphene oxide2O2The dosage of the composition is as follows: according to the amount of the graphite powder used in the step (I), H2O2The dosage of the (B) is 2.4-3mL of H2O2Per gram of graphite powder.
Preferably, the temperature of the copolymerization annealing treatment in step (iii) of the method for preparing graphene oxide is 350 ℃.
Preferably, the temperature rise rate of the copolymerization annealing treatment in step (iii) of the graphene oxide preparation method is 5 ℃/min, and the time is 1-2 hours.
Preferably, the time for the sonication in step (2) is 20 to 40 minutes, more preferably 30 minutes.
Preferably, in the step (i) of the preparation method of graphene oxide, graphite powder is added and stirred for 5-15 minutes; adding NaNO3When the mixture is stirred after being added into the mixed system AThe time is 5-15 minutes; mixing KMnO4Adding the mixed system B, heating to 38 ℃ for the first time, and stirring for 1.0-1.5 hours.
More preferably, in the step (i) of the preparation method of graphene oxide, graphite powder is added and then stirred for 10 minutes; adding NaNO3The stirring time after the addition of the mixed system A is 10 minutes; mixing KMnO4Adding the mixed system B, heating to 38 ℃ for the first time, and stirring for 1 hour.
Preferably, in step (ii) of the preparation method of graphene oxide, the time for stirring after the temperature is raised to 95 ℃ is 1 hour.
The invention also provides the metal-organic composite heterogeneous Fenton catalyst prepared by any one of the methods.
The metal organic composite heterogeneous Fenton catalyst prepared by the method has a typical flower-shaped nanosphere embedded lamellar structure, namely MoS2The porous nanospheres are uniformly dispersed, loaded and embedded on the surface of the substrate of the reducing graphene oxide nanosheet layer. The special structure of the catalyst enables pi electrons on a graphene substrate of the catalyst to be activated and migrated to form an electron polarity distribution center, and active sites in the catalyst are greatly exposed on the surface of the catalyst, so that pollutants and H are generated2O2Can be sufficiently contacted with the active site.
The invention also provides a method for degrading organic pollutants in water, which comprises the following steps: adding the metal-organic composite multiphase Fenton catalyst and hydrogen peroxide into a water body containing organic pollutants, and uniformly mixing.
The metal-organic composite heterogeneous Fenton catalyst and H2O2When the hydroxyl radical and the superoxide radical are used together in water, hydroxyl radicals and superoxide radicals can be generated, so that the whole system has strong oxidizing property, and the hydroxyl radicals and refractory organic matters generate organic radicals in aqueous solution to destroy the structure of the organic radicals, and finally, the organic radicals are oxidized and decomposed.
Preferably, the organic contaminants include at least one of rhodamine b (rhb), Methylene Blue (MB), ciprofloxacin, 2-chlorophenol, phenytoin, acid orange 7(AO 7).
The invention has the beneficial effects that: the invention provides a metal organic composite multiphase Fenton catalyst and a preparation method and application thereof, the preparation method is simple, and the prepared metal organic composite multiphase Fenton catalyst has the following advantages: (1) the metal organic composite multiphase Fenton catalyst does not need to adjust the pH value (pH value) of a system to 2-3 in the reaction process, is favorable for reducing the water treatment cost, and has good degradation and removal effects on organic pollutants difficult to biodegrade under the condition of neutral room temperature; (2) the catalyst of the invention has a special MoS2The nanosphere is embedded and linked on the graphene nanosheet, the active component of the nanosphere is greatly exposed on the surface of the catalyst, and the nanosphere has the functions of resisting pollutants and H2O2The contact is easy, and the obvious influence of steric hindrance effect and capillary phenomenon is avoided; (3) the catalyst of the invention does not produce solid foreign matters such as iron mud and the like in the reaction process, and does not need a foreign matter removing device; (4) the catalyst of the invention has high H in the process of degrading pollutants2O2Utilization rate; (5) the catalyst has good stability in the process of removing organic pollutants; (6) the catalyst of the invention belongs to a solid catalyst, is convenient to separate from water and is convenient to recycle.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of MS-rGO NSs prepared by the embodiment of the invention.
FIG. 2 is a Transmission Electron Microscope (TEM) image of MS-rGO NSs prepared by the present invention.
FIG. 3 is a graph of the degradation results of MS-rGO NSs prepared according to the example of the present invention with respect to RhB, MB, AO 7.
FIG. 4 is a graph of the results of the activity of MS-rGO NSs degrading RhB repeat activity prepared in the examples of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The preparation method of the metal organic composite heterogeneous Fenton catalyst (MS-rGO NSs) provided by the embodiment of the invention comprises the following steps:
(1) 1.60g of Na2MoO4·2H2Adding O and 120mg of graphene oxide into 120mL of deionized water, stirring for 10 minutes, and uniformly dispersing to obtain a mixed system E;
(2) 2.52g of CH4N2S, adding the mixture into the mixed system E, stirring for 5 minutes, performing ultrasonic treatment for 30 minutes, uniformly dispersing, transferring the mixture into a high-pressure kettle, and performing hydrothermal reaction in an oven at the temperature of 200 ℃ for 24 hours to obtain a mixed system F;
(3) alternately washing the mixed system F with deionized water and absolute ethyl alcohol, washing with deionized water once and washing with absolute ethyl alcohol twice, then drying for 24 hours at 70 ℃, and grinding to obtain the metal organic composite multiphase Fenton catalyst (MS-rGO NSs);
the preparation method of the graphene oxide comprises the following steps:
under ice bath below 0 ℃, slowly adding 10.0g of graphite powder into 230ml of 98% concentrated sulfuric acid, keeping the stirring state in the process of adding the graphite powder, uniformly mixing to obtain a mixed system A, and adding 50.0g of NaNO3Adding into the mixed system A, stirring for 10 min, mixing to obtain mixed system B, adding 30.0g KMnO4Slowly adding the mixture into the mixed system B, uniformly mixing, heating to 38 ℃, and stirring for 1 hour to obtain a mixed system C;
(II) adding 500mL of deionized water into the mixed system C, heating to 95 ℃, and stirring for 1 hour to obtain a mixed system D;
(III) 100ml of H2O2(30%) adding the mixture into a mixed system D until the mixed system D becomes a golden brown suspension, cooling, performing solid-liquid separation, washing the solid substance with deionized water until the pH value of the washing liquid is 6 to obtain a solid substance A, drying the solid substance A at 70 ℃ for 18 hours, transferring the dried solid substance A to a muffle furnace for copolymerization annealing treatment at the treatment temperature of 350 ℃ for 1 hour, and cooling to obtain the graphene oxide.
Results of the experiment
SEM and TEM characterization is carried out on the metal organic composite heterogeneous Fenton catalyst (MS-rGO NSs) prepared in the embodiment.
FIG. 1 is an SEM image of the MS-rGO NSs prepared in this example, from which it can be seen that a large number of regular MoS with diameters of 400 nm to 800 nm2The nanofiber flower-like spheres are uniformly embedded on the fluctuant graphene nano-sheet to form the MS-rGO NSs composite catalyst.
FIG. 2 is a TEM image of MS-rGO NSs, which can further observe the fine morphology structure of the MS-rGO NSs, i.e. MoS embedded on the surface of rGO2The nanosphere presents a 3D flower-shaped bionic structure, petal fibers of the nanosphere are evenly crimped and scattered all around, each petal is composed of crimped nanosheets with the thickness of 5-20 nm, a large number of pores are formed between the sheet layers, and the nanosphere shows a large specific surface area and an active component exposure degree. The high-resolution transmission electron microscope image shows very clear lattice stripes of the nano-sphere petals, the interplanar spacing is 0.625nm, and the crystal surface spacing is MoS2Further demonstrates MoS as exhibited by (002) crystal plane2Generation and mosaic structure of nanospheres on the surface of rGO.
Example 2
The application method of the metal-organic composite heterogeneous Fenton catalyst provided by the embodiment of the invention comprises the following steps of:
(1) 0.01g of the MS-rGO NSs prepared in example 1 was dosed into 25mL of 10mg L-1In the rhodamine solution, the pH value is kept at 7.0, and the constant temperature is kept at 35 ℃;
(2) continuously stirring until the adsorption equilibrium between the pollutant and the catalyst is reached, and adding 10mM H2O2Mixing uniformly;
(3) after 90 minutes of reaction, solid-liquid separation is carried out, MS-rGO NSs are collected and put into 25mL of 10mg L-1Repeating the steps (1) and (2) in the rhodamine solution.
The dye organics are RhB, AO7 and MB respectively.
Results of the experiment
Samples were taken at different time points to measure the concentration of the contaminant. The results are shown in FIG. 3. As can be seen from FIG. 3, the AO7 and MB degradation rates reached 85.7% and 97% at 120 minutes, and the RhB degradation rate reached 100% at 15 minutes.
Example 3
The method for degrading the dye organic matters in the water, provided by the embodiment of the invention, comprises the following steps of:
(1) 0.01g of the MS-rGO NSs prepared in example 1 was dosed into 25mL of 10mg L-1Keeping the pH value to be about 7.0 in the dye organic solution, and keeping the temperature to be 35 ℃;
(2) continuously stirring until the adsorption equilibrium between the pollutant and the catalyst is reached, and adding 10mM H2O2And (4) uniformly mixing.
The result of repeated application of the metal-organic composite heterogeneous fenton catalyst prepared in example 1 is shown in fig. 4, where the MS-rGO NSs are used to degrade rhodamine for 90 minutes, and after repeating for 8 times, the degradation rate of RhB is as high as 98% or more, which indicates that the metal-organic composite heterogeneous fenton catalyst has good catalytic activity and stability.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A preparation method of a metal-organic composite heterogeneous Fenton catalyst is characterized by comprising the following steps of:
(1) mixing Na2MoO4And graphene oxide are dispersed and uniformly mixed in deionized water to obtain a mixed system E;
(2) will CH4N2S is added into the mixed system E, is stirred and evenly mixed, is subjected to ultrasonic treatment, and is subjected to hydrothermal reaction in a closed container with the temperature of 180-220 ℃ for 20-30 hours to obtain a mixed system F;
(3) alternately washing the mixed system F by using deionized water and an organic solvent, drying, and grinding to obtain the metal-organic composite multiphase Fenton catalyst;
the preparation method of the graphene oxide comprises the following steps:
slowly adding graphite powder into concentrated sulfuric acid in an ice bath at the temperature of below 0 ℃, keeping the stirring state in the process of adding the graphite powder, uniformly mixing to obtain a mixed system A, and adding NaNO into the mixed system A3Adding into the mixed system A, mixing to obtain mixed system B, adding KMnO4Slowly adding into the mixed system B, mixing, heating to 35-38 deg.C, stirring for 1-1.5 hr to obtain mixed system C;
(II) adding deionized water into the mixed system C, heating to 90-100 ℃, and stirring for 1-2 hours to obtain a mixed system D;
(III) reacting H2O2Adding the mixture into a mixed system D until the mixed system D becomes a golden brown suspension, cooling, performing solid-liquid separation, washing the solid substance with deionized water until the pH value of the washing liquid is 6-7 to obtain a solid substance A, drying the solid substance A at 50-70 ℃, performing copolymerization annealing treatment at the annealing treatment temperature of 340-360 ℃, and cooling to obtain the graphene oxide.
2. The method according to claim 1, wherein Na is2MoO4And the dosage of the graphene oxide is as follows by weight: 1000: 44-132, wherein the content of the graphene oxide in the mixed system E is 0.5-1.5 g/L.
3. The method according to claim 1, wherein CH in the step (2)4N2The dosage of S is Na2MoO4And CH4N2The molar ratio of S is 1: 3-6.
4. The method according to claim 1, wherein in step (I) of the graphene oxide preparation method, concentrated sulfuric acid, graphite powder, NaNO3、KMnO4The dosage proportion is as follows: 230-240mL 98% concentrated sulfuric acid, 10.0-12.0g graphite powder, 50.0-52.0g NaNO3And 30.0-32.0g of KMnO4。
5. The production method according to claim 1, wherein H is used in step (III) of the production method for graphene oxide2O2The dosage of the composition is as follows: according to the amount of the graphite powder used in the step (I), H2O2The dosage of the (B) is 2.4-3mL of H2O2Per gram of graphite powder.
6. The method according to claim 1, wherein the temperature increase rate of the copolymerization annealing treatment in step (III) of the method for producing graphene oxide is 5 ℃/min for 1 to 2 hours.
7. A metal-organic composite heterogeneous Fenton's catalyst prepared according to any one of claims 1 to 6, wherein MoS has a diameter of 400 nm to 800 nm2The nanofiber flower-like balls are embedded on the graphene nanosheets.
8. A method for degrading organic contaminants in water, the method comprising the steps of: adding the catalyst of claim 7 and hydrogen peroxide to a body of water containing organic contaminants and mixing well.
9. The method of claim 8, wherein the organic contaminants comprise at least one of rhodamine B, methylene blue, ciprofloxacin, 2-chlorophenol, phenytoin, and acid orange 7.
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| 3D二硫化钼/石墨烯组装体的制备及其催化脱硫性能;王旭珍，等;《新型炭材料》;20140430;第29卷(第2期);第82-87页 * |
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