CN109647444A - A kind of metal organic composite multiphase Fenton catalyst and its preparation method and application - Google Patents
A kind of metal organic composite multiphase Fenton catalyst and its preparation method and application Download PDFInfo
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- 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
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- 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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/30—Organic compounds
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/36—Organic compounds containing halogen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- 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 present invention provides a kind of metal organic composite multiphase Fenton catalyst and its preparation method and application, the method uses improved Hummers method to combine the reproducibility graphene oxide of annealing reduction method synthesis as substrate and polyelectron ligand, two molybdic acid hydrate sodium and thiocarbamide prepare final catalyst by the water-heat process adulterated in situ respectively as molybdenum source and sulphur source.Preparation method of the invention is simple, and the metal organic composite multiphase Fenton catalyst being prepared has the advantage that (1) catalyst under room temperature just has organic pollutant degradation removal effect well in neutrality；(2) active component of catalyst is greatly exposed to catalyst surface, has to pollutant and H2O2Easy contact, do not influenced by space steric effect and capillary phenomenon；(3) catalyst will not generate the solid foreign materials such as iron cement during the reaction, foreign body eliminating apparatus not needed, convenient for being separated from water and having good stability, convenient for recycling.
Description
Technical field
The invention belongs to material preparation and application fields, and in particular to a kind of metal organic composite multiphase Fenton catalyst and
Preparation method and application.
Background technique
The removal by numerous studies and exploitation for the pollutant of difficult for biological degradation in water of iron series fenton catalyst.But
Due to the properties of iron inherently, lead to the presence of electronic circulation rate-limiting step in Fenton's reaction, this is but also more
Active low, hydrogen peroxide utilization rate is difficult to break through the appearance of the bottleneck problems such as 50% phase fenton catalyst in neutral conditions.
Summary of the invention
A kind of metal organic composite multiphase is provided it is an object of the invention to overcome the shortcomings of the prior art place
Fenton catalyst and its preparation method and application.
To achieve the above object, the technical scheme adopted by the invention is as follows: a kind of metal organic composite multiphase Fenton catalyst
The preparation method of (MS-rGO NSs), the described method comprises the following steps:
(1) by Na2MoO4Disperse to mix in deionized water with graphene oxide, obtains mixed system E；
(2) by CH4N2S is added in mixed system E, is ultrasonically treated after stirring and evenly mixing, in 180-220 DEG C of closed container
Hydro-thermal reaction is carried out, the time is 20-30 hours, obtains mixed system F；
(3) it is dried after alternately washing mixed system F deionized water and organic solvent, the metal is obtained after grinding to be had
The compound multiphase Fenton catalyst of machine.
Preferably, the graphene oxide preparation method the following steps are included:
(I) under 0 DEG C of ice bath below, graphite powder is slowly added in the concentrated sulfuric acid, during graphite powder is added, is kept
The state of stirring is uniformly mixed and obtains mixed system A, by NaNO3It is added in mixed system A, is uniformly mixed and obtains mixed system
B, by KMnO4It is slowly added in mixed system B, mixing is warming up to 35-38 DEG C after mixing, stirring obtains mixture in 1-1.5 hours
It is C；
(II) deionized water is added into mixed system C, is warming up to 90-100 DEG C, stirring obtains mixed system in 1-2 hours
D；
(III) by H2O2It is added in mixed system D, until mixed system D becomes the suspension of golden brown, solid-liquid point after cooling
From, solid matter is washed with deionized, until cleaning solution pH be 6-7, solid matter A is obtained, by solid matter A in 50-
Combined polymerization annealing is carried out after drying at 70 DEG C, annealing temperature is 340-360 DEG C, obtains graphene oxide after cooling.
The method is mainly received with the reproducibility graphene oxide of improved Hummers method and annealing reduction treatment synthesis
Rice piece (rGO NSs) makees carrier and polyelectron ligand, two molybdic acid hydrate sodium (Na2MoO4·2H2) and thiocarbamide (CH O4N2S) make respectively
For molybdenum source and sulphur source, metal organic composite multiphase Fenton catalyst is synthesized by solvent heat seal.
Preferably, Na2MoO4With the weight ratio of the dosage of the graphene oxide are as follows: 1000:44-132, the mixture
The content for being graphene oxide described in E is 0.5-1.5g/L.
It is highly preferred that Na2MoO4With the weight ratio of the dosage of the graphene oxide are as follows: 1000:88, the mixed system E
Described in graphene oxide content be 1g/L.
Preferably, CH in step (2)4The dosage of NS is Na2MoO4And CH4N2The molar ratio of S is 1:3-6.
It is highly preferred that CH in step (2)4The dosage of NS is Na2MoO4And CH4N2The molar ratio of S is 1:5.
Preferably, the closed container in step (2) is autoclave.
Preferably, in the step (3), the organic solvent is dehydrated alcohol.
Preferably, in the step (3), drying temperature is 80-100 DEG C, and drying time is 20-30 hours.
It is highly preferred that drying temperature is 100 DEG C in the step (3), drying time is 24 hours.
Preferably, in the step of preparation method of the graphene oxide (I), the concentrated sulfuric acid, graphite powder, NaNO3、KMnO4's
Usage ratio are as follows: 98% concentrated sulfuric acid of 230-240mL, the graphite powder of 10.0-12.0g, 50.0-52.0g NaNO3With
30.0-32.0g KMnO4。
It is highly preferred that in the step of preparation method of the graphene oxide (I), the concentrated sulfuric acid, graphite powder, NaNO3、KMnO4
Usage ratio are as follows: 98% concentrated sulfuric acid of 230mL, the graphite powder of 10.0g, 50.0g NaNO3With the KMnO of 30.0g4。
Preferably, in the step of preparation method of the graphene oxide (II), deionization is added into mixed system C
Water is warming up to 95 DEG C, and stirring obtains mixed system D in 1-2 hours.
Preferably, H in the step of preparation method of the graphene oxide (III)2O2Dosage are as follows: by institute in step (I)
State graphite powder meter H2O2Dosage be 2.4-3mL H2O2/ g graphite powder.
Preferably, the temperature that combined polymerization makes annealing treatment in the step of preparation method of the graphene oxide (III) is 350
℃。
Preferably, the heating rate of combined polymerization annealing is in the step of preparation method of the graphene oxide (III)
5 DEG C/min, the time is 1-2 hours.
Preferably, the time ultrasonic in the step (2) is 20-40 minutes, more preferably 30 minutes.
Preferably, in the step of preparation method of the graphene oxide (I), mixing time is 5-15 after graphite powder is added
Minute；By NaNO3Mixing time after mixed system A is added is 5-15 minutes；By KMnO4First is carried out after mixed system B is added
Secondary heating reaches 38 DEG C and stirs, and mixing time is 1.0-1.5 hours.
It is highly preferred that mixing time is 10 after graphite powder is added in the step of preparation method of the graphene oxide (I)
Minute；By NaNO3Mixing time after mixed system A is added is 10 minutes；By KMnO4It is carried out for the first time after mixed system B is added
Heating reaches 38 DEG C and stirs, and mixing time is 1 hour.
Preferably, in the step of preparation method of the graphene oxide (II), the time stirred after being warming up to 95 DEG C is 1
Hour.
The present invention also provides a kind of metal organic composite multiphase Fenton catalyst that any of the above-described the method is prepared.
The metal organic composite multiphase Fenton catalyst of the method for the present invention preparation has the typical embedding piece of flower-like nanometer ball
Layer structure, i.e. MoS2The evenly dispersed load of porous nano sphere simultaneously embedding is associated in reproducibility stannic oxide/graphene nano lamella substrate table
Face.The special tectonic of the catalyst make the pi-electron on the graphene-based bottom of catalyst be activated migration formed electronic polarity distribution in
The heart, and active site is greatly exposed to catalyst surface in catalyst, makes pollutant and H2O2It can sufficiently and active site
Contact.
The present invention also provides a kind of biodegrading process of organic pollutants, the described method comprises the following steps: Xiang Hanyou
Metal organic composite multiphase Fenton catalyst and hydrogen peroxide described above are added in the water body of organic pollutant, and are mixed equal
It is even.
The metal organic composite multiphase Fenton catalyst and H2O2When being combined in water, hydroxyl radical free radical can be generated and surpassed
Oxygen radical, so that whole system has strong oxidizing property, hydroxyl radical free radical generates with hardly degraded organic substance organic in aqueous solution
Free radical is allowed to structure destruction, final oxygenolysis.
Preferably, the organic pollutant include rhodamine B (RhB), methylene blue (MB), Ciprofloxacin, 2- chlorophenol,
At least one of phenytoinum naticum, acid orange 7 (AO7).
The beneficial effects of the present invention are: the present invention provides a kind of metal organic composite multiphase Fenton catalyst and its systems
Preparation Method and application, preparation method of the invention is simple, the metal organic composite multiphase Fenton catalyst being prepared have with
Lower advantage: (1) metal organic composite multiphase Fenton catalyst of the invention is not needed in reaction process by the pH value (pH of system
Value) 2~3 this harsh conditions are adjusted to, cost of water treatment is advantageously reduced, in neutrality under room temperature for difficult for biological degradation
Organic pollutant just has degradation removal effect well；(2) catalyst of the invention has special MoS2Nanosphere is embedding
In the structure of graphene nano on piece, active component is greatly exposed to catalyst surface, has to pollutant and H2O2Easily connect
Touching property, is not significantly affected by space steric effect and capillary phenomenon；(3) catalyst of the invention will not produce during the reaction
The solid foreign materials such as pig iron mud, do not need foreign body eliminating apparatus；(4) catalyst of the invention has during degradation of contaminant
High H2O2Utilization rate；(5) catalyst of the invention has good stability during removing removal organic polluter；(6) originally
The catalyst of invention belongs to solid catalyst, convenient for being separated from water, convenient for recycling.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure for the MS-rGO NSs that the embodiment of the present invention is prepared.
Fig. 2 is transmission electron microscope (TEM) figure for the MS-rGO NSs that the embodiment of the present invention is prepared.
Fig. 3 is degradation results figure of the MS-rGO NSs that is prepared of the embodiment of the present invention for RhB, MB, AO7.
Fig. 4 is that the MS-rGO NSs degradation RhB that the embodiment of the present invention is prepared repeats active result figure.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Embodiment 1
A kind of preparation side of metal organic composite multiphase Fenton catalyst (MS-rGO NSs) as the embodiment of the present invention
Method the described method comprises the following steps:
(1) by 1.60g Na2MoO4·2H2O and 120mg graphene oxide is added in 120mL deionized water, stirring 10
Minute is uniformly dispersed to obtain mixed system E；
(2) by 2.52g CH4N2S is added in mixed system E, stirs 5 minutes, and ultrasound 30 minutes is uniformly dispersed, moves to height
It presses in kettle, hydro-thermal hair is carried out in 200 DEG C of baking oven and is answered, the time is 24 hours, obtains mixed system F；
(3) mixed system F deionized water and dehydrated alcohol are alternately washed, deionized water washed once, dehydrated alcohol
It washes twice, is then dried 24 hours at 70 DEG C, the metal organic composite multiphase Fenton catalyst is obtained after grinding
(MS-rGO NSs)；
The preparation method of the graphene oxide the following steps are included:
(I) under 0 DEG C of ice bath below, 10.0g graphite powder is slowly added in 98% concentrated sulfuric acid of 230ml, is added
During graphite powder, the state being kept stirring is uniformly mixed and obtains mixed system A, by 50.0g NaNO3Mixed system is added
In A, it is uniformly mixed within stirring 10 minutes and obtains mixed system B, by 30.0g KMnO4It is slowly added in mixed system B, mixing mixes
After be warming up to 38 DEG C, stirring obtains mixed system C in 1 hour；
(II) 500mL deionized water is added into mixed system C, is warming up to 95 DEG C, stirring obtains mixed system D in 1 hour；
(III) by 100ml H2O2(30%) it is added in mixed system D, until mixed system D becomes the suspension of golden brown,
It is separated by solid-liquid separation after cooling, solid matter is washed with deionized, until the pH of cleaning solution is 6, solid matter A is obtained, by solid
After substance A is dried 18 hours at 70 DEG C, the solid matter A after drying is moved into Muffle furnace and carries out combined polymerization annealing, place
Managing temperature is 350 DEG C, and the time is 1 hour, and heating rate is 5 DEG C/min, obtains graphene oxide after cooling.
Experimental result
The metal organic composite multiphase Fenton catalyst (MS-rGO NSs) that the present embodiment is prepared carry out SEM and
The characterization of TEM.
The SEM figure that Fig. 1 is the MS-rGO NSs that the present embodiment is prepared, it can be seen from the figure that a large amount of diameter is
The MoS of 400 nanometers to 800 nanometers of rule2The flower-shaped ball of nanofiber is uniformly embedded on the graphene nanoplatelets of fluctuating, shape
At MS-rGO NSs composite catalyst.
Fig. 2 is the TEM image of MS-rGO NSs, can be further observed that its subtle appearance structure, embedding on the surface rGO
MoS2Nanosphere shows 3D flower shape biomimetic features, and petal fiber uniformly rolls up pleat towards surrounding and scatters, and every valve is by with a thickness of 5
The curling nanometer sheet of~20nm forms, and forms a large amount of hole between lamella, shows biggish specific surface area and active component
Degrees of exposure.High-resolution-ration transmission electric-lens figure shows the gem-pure lattice fringe of nanosphere body petal, and interplanar distance is
0.625nm is MoS2(002) crystal face shown, further prove MoS2Nanosphere is in the generation on the surface rGO and embedding
Structure.
Embodiment 2
A kind of application method of metal organic composite multiphase Fenton catalyst as the embodiment of the present invention, the method packet
Include following steps:
(1) the MS-rGO NSs for preparing 0.01g embodiment 1 puts into 25mL 10mg L-1Rhodamine liquor in, keep
PH value is 7.0,35 DEG C of constant temperature；
(2) the addition 10mM H after reaching adsorption equilibrium between pollutant and catalyst is continuously stirred2O2It is uniformly mixed；
(3) it after reacting 90 minutes, is separated by solid-liquid separation, collects MS-rGO NSs, and put into 25mL 10mg L-1Luo Dan
In bright solution, step (1), (2) are repeated.
The dyestuff organic matter is respectively RhB, AO7 and MB.
Experimental result
The concentration of sample detection pollutant is put in different times.As a result as shown in Figure 3.From the figure 3, it may be seen that at 120 minutes
The degradation rate of AO7 and MB has reached 85.7% and 97%, and the degradation rate of RhB just reached 100% at 15 minutes.
Embodiment 3
As the biodegrading process of dyestuff organic matter in a kind of water of the embodiment of the present invention, the described method comprises the following steps:
(1) the MS-rGO NSs for preparing 0.01g embodiment 1 puts into 25mL 10mg L-1Dyestuff organic solution in,
Keeping pH value is about 7.0, and 35 DEG C of constant temperature；
(2) the addition 10mM H after reaching adsorption equilibrium between pollutant and catalyst is continuously stirred2O2It is uniformly mixed.
Result such as Fig. 4 institute of the repeated application for the metal organic composite multiphase Fenton catalyst that embodiment 1 is prepared
Show, degraded rhodamine 90 minutes using MS-rGO NSs, and after being repeated 8 times, 98% or more is up to the degradation rate of RhB,
Illustrate that metal organic composite multiphase Fenton catalyst has good catalytic activity and stability.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of preparation method of metal organic composite multiphase Fenton catalyst, which is characterized in that the method includes following steps
It is rapid:
(1) by Na2MoO4Disperse to mix in deionized water with graphene oxide, obtains mixed system E；
(2) by CH4N2S is added in mixed system E, is ultrasonically treated after stirring and evenly mixing, carries out in 180-220 DEG C of closed container
Hydro-thermal reaction, time are 20-30 hours, obtain mixed system F；
(3) it is dried after alternately washing mixed system F deionized water and organic solvent, it is organic multiple that the metal is obtained after grinding
Close multiphase Fenton catalyst.
2. preparation method according to claim 1, which is characterized in that the preparation method of the graphene oxide includes following
Step:
(I) under 0 DEG C of ice bath below, graphite powder is slowly added in the concentrated sulfuric acid, during graphite powder is added, is kept stirring
State, be uniformly mixed obtain mixed system A, by NaNO3It is added in mixed system A, is uniformly mixed and obtains mixed system B, it will
KMnO4It is slowly added in mixed system B, mixing is warming up to 35-38 DEG C after mixing, stirring obtains mixed system C in 1-1.5 hours；
(II) deionized water is added into mixed system C, is warming up to 90-100 DEG C, stirring obtains mixed system D in 1-2 hours；
(III) by H2O2It is added in mixed system D, until mixed system D becomes the suspension of golden brown, is separated by solid-liquid separation after cooling,
Solid matter is washed with deionized, until the pH of cleaning solution is 6-7, solid matter A is obtained, by solid matter A at 50-70 DEG C
Combined polymerization annealing is carried out after lower drying, annealing temperature is 340-360 DEG C, obtains graphene oxide after cooling.
3. preparation method according to claim 1 or 2, which is characterized in that Na2MoO4With the dosage of the graphene oxide
Weight ratio are as follows: 1000:44-132, the content of graphene oxide described in the mixed system E are 0.5-1.5g/L.
4. preparation method according to claim 1 or 2, which is characterized in that CH in step (2)4N2The dosage of S is Na2MoO4
And CH4N2The molar ratio of S is 1:3-6.
5. preparation method according to claim 2, which is characterized in that the step of the preparation method of the graphene oxide
(I) in, the concentrated sulfuric acid, graphite powder, NaNO3、KMnO4Usage ratio are as follows: 98% concentrated sulfuric acid, the 10.0-12.0g of 230-240mL
Graphite powder, 50.0-52.0g NaNO3With the KMnO of 30.0-32.0g4。
6. preparation method according to claim 2, which is characterized in that the step of the preparation method of the graphene oxide
(III) H in2O2Dosage are as follows: by graphite powder meter H described in step (I)2O2Dosage be 2.4-3mL H2O2/ g graphite powder.
7. preparation method according to claim 2, which is characterized in that the step of the preparation method of the graphene oxide
(III) heating rate that combined polymerization makes annealing treatment in is 5 DEG C/min, and the time is 1-2 hours.
8. a kind of metal organic composite multiphase Fenton catalyst being prepared such as any the method for claim 1-7.
9. a kind of biodegrading process of organic pollutants, which is characterized in that the described method comprises the following steps: to containing organic
Catalyst and hydrogen peroxide as claimed in claim 8 are added in the water body of pollutant, and are uniformly mixed.
10. according to the method described in claim 9, it is characterized in that, the organic pollutant include rhodamine B, methylene blue,
At least one of Ciprofloxacin, 2- chlorophenol, phenytoinum naticum, acid orange 7.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110142051A (en) * | 2019-05-28 | 2019-08-20 | 广州大学 | A kind of zinc sulphide load molybdenum sulfide catalyst and its preparation method and application |
| CN113649000A (en) * | 2021-06-29 | 2021-11-16 | 福建师范大学 | Honeycomb porous Fe/Mg (OH)2Catalytic material and preparation method thereof |
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