CN115350709B - Sepiolite-loaded ferro-manganese bimetallic catalyst and preparation method and application thereof - Google Patents
Sepiolite-loaded ferro-manganese bimetallic catalyst and preparation method and application thereof Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
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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
- 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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- 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
- C02F2101/36—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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- 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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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a sepiolite supported ferro-manganese bimetallic catalyst and a preparation method and application thereof. The preparation method comprises the steps of taking soluble saccharides as a carbon source, preparing carbon modified sepiolite by adopting a hydrothermal carbonization method, taking ferric nitrate as an iron source and manganese nitrate as a manganese source, loading ferromanganese bimetallic on the carbon modified sepiolite by adopting an impregnation method, and calcining in an inert atmosphere to obtain the sepiolite loaded ferromanganese bimetallic catalyst. The sepiolite loaded iron-manganese bimetallic catalyst is used as a catalyst, and the peroxymonosulfate is used for carrying out catalytic degradation treatment on the antibiotic wastewater. According to the invention, a supported ferro-manganese bimetallic catalyst is prepared by adopting an impregnation method, clay mineral sepiolite is selected as a carrier material, and carbon is supported on the surface of the catalyst to improve the stability and high dispersion of the ferro-manganese bimetallic catalyst on the surface of the catalyst, so that the activation of persulfates and the generation of active oxygen species are improved, and the efficient degradation and safe conversion of antibiotics are further improved. In addition, the raw materials are cheap and easy to obtain, and the method is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a sepiolite supported iron-manganese bimetallic catalyst and a preparation method and application thereof.
Background
Aiming at the problem of organic pollution caused by novel pollutants such as antibiotics in water, advanced oxidation technology represented by persulfate activation has attracted more and more attention from researchers due to the characteristics of strong oxidation capability, low cost, convenience in storage and transportation and the like. However, the most studied transition metal-based catalysts at present have the problem of secondary pollution caused by ion elution, and non-metal catalysts such as activated carbon, carbon nanotubes, graphene and the like are effective, but have high preparation cost and complex operation process.
Disclosure of Invention
The invention aims at providing a sepiolite supported iron-manganese bimetallic catalyst, a preparation method and application thereof, aiming at the defects of the prior art.
According to the preparation method of the sepiolite supported ferro-manganese bimetallic catalyst, soluble saccharides are used as carbon sources, a hydrothermal carbonization method is adopted to prepare carbon modified sepiolite, ferric nitrate is used as an iron source, manganese nitrate is used as a manganese source, and a dipping method is used for supporting ferro-manganese bimetallic on the carbon modified sepiolite, so that the sepiolite supported ferro-manganese bimetallic catalyst is obtained after calcination in an inert atmosphere.
Further, the specific steps are as follows:
s1: completely dissolving glucose in ultrapure water, then adding sepiolite SEPs under vigorous stirring, and continuously stirring to form uniform suspension after ultrasonic dispersion for a period of time;
s2, transferring the suspension into a high-pressure reaction kettle with an 80mL polytetrafluoroethylene lining, sealing, and reacting for 24-72 h at 150-180 ℃;
s3, alternately washing the product obtained after the reaction in the step S2 with ethanol and deionized water for a plurality of times, and drying and grinding after filtrate is clarified to obtain SEPs@C samples;
s4, impregnating Fe (NO) 3 ) 3 ·9H 2 O and Mn (NO) 3 ) 2 ·2H 2 O is loaded on SEPs@C according to different molar ratios, and dried;
and S5, annealing the product obtained in the step S4 in a tubular furnace at 500-800 ℃ for 5-10h under inert atmosphere, cooling to room temperature, and grinding to obtain the sepiolite supported ferro-manganese bimetallic catalyst FeMn/SEPs@C.
Further, the drying temperature in step S4 was 60℃for 5 hours.
Further, in step S4, the molar ratio of Fe to Mn is 9-5:1.
Further, the soluble sugars include, but are not limited to, glucose, sucrose, chitosan.
Further, the inert atmosphere comprises nitrogen and argon.
The sepiolite-loaded iron-manganese bimetallic catalyst prepared by adopting the preparation method.
Furthermore, sepiolite loaded iron-manganese bimetallic catalyst is used as a catalyst, and the peroxymonosulfate is used for carrying out catalytic degradation treatment on the antibiotic wastewater.
Further, antibiotics include, but are not limited to ofloxacin, sulfamethoxazole, tetracycline hydrochloride.
Further, the antibiotic is ofloxacin, every 5-50 mg FeMn/SEPs@C catalyst is dispersed into 100mL 10ppm ofloxacin solution, and after 60min, 0.1M NaOH or H is used for achieving adsorption-desorption balance 2 SO 4 The solution adjusts the initial pH value of the system, and then 0.3-0.7g/L of Peroxymonosulfate (PMS) is added to start degradation reaction.
Compared with the prior art, the invention has at least the following advantages:
(1) According to the invention, a supported ferro-manganese bimetallic catalyst is prepared by adopting an impregnation method, clay mineral sepiolite is selected as a carrier material, and carbon is supported on the surface of the catalyst to improve the stability and high dispersion of the ferro-manganese bimetallic catalyst on the surface of the catalyst, so that the activation of persulfates and the generation of active oxygen species are improved, and the efficient degradation and safe conversion of antibiotics are further improved. In addition, the raw materials are cheap and easy to obtain, and the method is suitable for large-scale industrial production;
(2) The catalyst prepared by the invention has excellent catalytic activity in an activated persulfate degradation ofloxacin system, and can be recycled for multiple times.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of a sample prepared in example 2;
FIG. 2 is a Transmission Electron Microscope (TEM) image of the sample prepared in example 2;
FIG. 3 is a graph of the catalytic performance kinetics of the samples obtained in example 3;
FIG. 4 is a graph showing the degradation curves and kinetics of the different catalysts to ofloxacin;
FIG. 5 is a graph of 5 cycles degradation of ofloxacin by FeMn/SEPs@C catalyst.
Detailed Description
The following are specific embodiments of the present invention and the technical solutions of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
The technical scheme of the present invention will be further explained in connection with several preferred embodiments. The experimental methods used in the following examples are conventional methods unless otherwise specified, and materials, reagents and instruments used therein are commercially available. The reagents used were all analytically pure. Milli-Q high purity water (18.2 mΩ) was used during the experiment.
Example 1: preparation of carbon-supported sepiolite Carrier
3.75g of glucose was completely dissolved in 57mL of ultra pure water, then 0.75g of Sepiolite (SEPs) was added under vigorous stirring, and the dispersion was carried out for 30min by ultrasonic, and stirring was continued for 24h to form a uniform solution; subsequently, transferring the suspension into an 80mL polytetrafluoroethylene-lined high-pressure reaction kettle, and reacting for 48 hours at 160 ℃ after sealing; alternately washing the reacted product with ethanol and deionized water for several times, standing at 60 ℃ for drying overnight after the filtrate is clarified, and finally grinding the dried sample to obtain a carrier material (marked as SEPs@C);
example 2: preparation of sepiolite-loaded iron-manganese bimetallic catalyst
Fe (NO) is impregnated with 3 ) 3 ·9H 2 O and Mn (NO) 3 ) 2 ·2H 2 O is loaded on SEPs@C according to different molar ratios (1:0, 9:1, 7:1,5:1, 0:1), and is placed in a 60 ℃ oven for drying for 5 hours; calcining for 8 hours in a tube furnace at 650 ℃ under nitrogen atmosphere, cooling to room temperature, and grinding to obtain a sepiolite-supported ferro-manganese bimetallic catalyst (marked as FeMn/SEPs@C);
fig. 1 is an X-ray diffraction (XRD) pattern of the sepiolite-supported ferro-manganese bimetallic catalyst, and it can be seen from the figure that products with different ferro-manganese ratios all retain characteristic diffraction peaks of sepiolite, that wide characteristic diffraction peaks occurring at 20 ° to 30 ° of 2θ are amorphous carbon, and that no other diffraction peaks exist.
Fig. 2 is a Transmission Electron Microscope (TEM) image of the above-mentioned 7:1 iron-manganese molar ratio supported catalyst, from which it can be seen that the prepared FeMn/seps@c catalyst maintains the fibrous structure of sepiolite and that no significant agglomeration of the supported iron-manganese bimetallic active component occurs.
Example 3: catalytic performance of sepiolite supported iron-manganese bimetallic catalyst
The method for detecting the catalytic performance comprises the following steps: dispersing the obtained 5-50 mg FeMn/SEPs@C catalyst into 100mL 10ppm Ofloxacin (OFX) solution, and after 60min to reach adsorption-desorption equilibrium, using 0.1M NaOH or H 2 SO 4 The initial pH value of the solution regulating system is regulated, and then 0.3-0.7. 0.7g/L of Peroxymonosulfate (PMS) is added to start degradation reaction, and at each given time interval, a certain volume of solution is taken, 2.5mL of filtrate is collected by a 0.22 μm filter, and then 0.1M Na is added 2 S 2 O 3 Quenching the oxidation reaction. The OFX concentration was analyzed by high performance liquid chromatography (HPLC, thermo Fisher Scientific, ultiMate 3000) equipped with a UV/vis detector. The separation was carried out on a C-18 column, the mobile phase consisting of 76% aqueous phosphoric acid (ph=2.6) and 24% acetonitrile, the flow rate being 0.8mL/min, the injection quantity being 20 μl, the column temperature being maintained at 25 ℃ and the detection wavelength being 288nm.
In this embodiment:
dispersing the obtained FeMn/SEPs@C catalyst with different iron-manganese molar ratios into 100mL 10ppm Ofloxacin (OFX) solution, and after 60min to reach adsorption-desorption equilibrium, dispersing with 0.1M H 2 SO 4 The initial pH of the solution was adjusted to 3, 0.3g/L PMS was added to initiate degradation, 2mL of solution was taken at each given time interval and 1.5mL of filtrate was collected with a 0.22 μm filter, followed by 0.1M Na 2 S 2 O 3 Quenching the oxidation reaction. The other steps are the same as comparative experiments with no catalyst added in the examples.
As known from the Lamber-Beer law, the concentration of ofloxacin solution is in direct proportion to the absorption peak area of characteristic absorption wavelength, so that the catalytic degradation rate can be quantitatively analyzed by detecting the change of the absorption peak area of the solution in the degradation process, and then the catalytic effect of the catalyst is measured by the degradation rate (R).
R＝[(A 0 -A)/A 0 ]×100％
In which A 0 The absorption peak area before persulfate is added; a is the absorption peak area at the time t of degradation.
Fig. 3 is a graph showing degradation kinetics of the catalyst to ofloxacin with different iron-manganese molar ratios, and it can be seen from the graph that after the adsorption-desorption equilibrium is reached in 60min, when n (Fe): n (Mn) =0:1 or 1:0, after PMS is added, the degradation of ofloxacin by the catalyst is not significantly improved, which indicates that the single metal loaded seps@c does not play a role in catalytic oxidation of ofloxacin. When the ferro-manganese bimetal exists at the same time, the removal efficiency of ofloxacin is optimal when n (Fe): n (Mn) =7:1, and the degradation efficiency of ofloxacin reaches more than 90% within 30 min. From this, n (Fe): n (Mn) =7:1 supported catalyst FeMn/SEPs@C has the best effect on PMS activation degradation of ofloxacin.
Example 4: catalytic Properties of FeMn/SEPs@C catalyst
Dispersing the obtained catalyst of 10mg FeMn/SEPs@C, fe/SEPs@C, mn/SEPs@C, SEPs@C into 100mL 10ppm Ofloxacin (OFX) solution, standing for 60min to reach adsorption-desorption equilibrium, and adding 0.1M NaOH or H 2 SO 4 The initial pH of the solution was adjusted to 6.5 and 0.5g/L PMS was added to initiate degradation, 2mL of solution was taken at each given time interval and 1.5mL of filtrate was collected with a 0.22 μm filter followed by 0.1M Na 2 S 2 O 3 Quenching the oxidation reaction. The other steps are the same as comparative experiments with no catalyst added in the examples.
At the end of each experiment, the catalyst was dried in an oven at 60 ℃ after filtration and washing, and then stability and repeatability experiments were performed under the same catalytic conditions.
FIG. 4 is a graph showing the degradation curves and kinetics of the different catalysts to ofloxacin, and it can be seen from FIG. 4a that the degradation efficiency to ofloxacin is within 20minThe rate reaches more than 90 percent. Whereas single metal supported catalysts, PMS alone and seps@c had little removal effect on ofloxacin. As can be seen from FIG. 4b, the degradation curves of the three catalysts Fe/SEPs@C, mn/SEPs@C and FeMn/SEPs@C for ofloxacin conform to the quasi-first order kinetics, and the rate constant k is from 0.009min -1 ，0.012min -1 Increase to 0.142min -1 . Thus, compared with a single metal supported catalyst, the ferro-manganese bimetallic support can indeed improve the degradation of ofloxacin.
Fig. 5 is a graph of 5 times of cyclic degradation of ofloxacin by the FeMn/seps@c catalyst, and it can be seen from the graph that the degradation efficiency of ofloxacin by the catalyst after 5 times of cyclic degradation can still reach more than 80%, and good reusability is shown.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of example, it will be appreciated by those skilled in the art that the foregoing examples are provided for the purpose of illustration only and are not intended to limit the scope of the invention, and that various modifications or additions and substitutions to the described specific embodiments may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the invention as defined in the accompanying claims. It should be understood by those skilled in the art that any modification, equivalent substitution, improvement, etc. made to the above embodiments according to the technical substance of the present invention should be included in the scope of protection of the present invention.
Claims (7)
1. The application of sepiolite supported ferro-manganese bimetallic catalyst is characterized in that: preparing carbon-modified sepiolite by using soluble saccharides as a carbon source and adopting a hydrothermal carbonization method, then taking ferric nitrate as an iron source and manganese nitrate as a manganese source, loading ferromanganese bimetallic on the carbon-modified sepiolite by using an impregnation method, and calcining in an inert atmosphere to obtain a sepiolite-loaded ferromanganese bimetallic catalyst;
wherein, the specific operation of calcination is: annealing in a tube furnace at 500-800 ℃ for 5-10 h;
the sepiolite loaded iron-manganese bimetallic catalyst is used as a catalyst, and the peroxymonosulfate is used for carrying out catalytic degradation treatment on the antibiotic wastewater;
the molar ratio of Fe to Mn is 9-7:1.
2. The use of a sepiolite supported iron manganese bimetallic catalyst as claimed in claim 1, wherein: the preparation method of the sepiolite supported iron-manganese bimetallic catalyst comprises the following specific steps:
s1: completely dissolving glucose in ultrapure water, then adding sepiolite SEPs under vigorous stirring, and continuously stirring to form uniform suspension after ultrasonic dispersion for a period of time;
s2, transferring the suspension into a high-pressure reaction kettle with an 80mL polytetrafluoroethylene lining, and reacting for 24-72 hours at 150-180 ℃ after sealing;
s3, alternately washing the product obtained after the reaction in the step S2 with ethanol and deionized water for a plurality of times, and drying and grinding after filtrate is clarified to obtain SEPs@C samples;
s4, impregnating Fe (NO) 3 ) 3 ·9H 2 O and Mn (NO) 3 ) 2 ·2H 2 O is loaded on SEPs@C according to different molar ratios, and dried;
and S5, annealing the product obtained in the step S4 in a tubular furnace at 500-800 ℃ for 5-10h under inert atmosphere, cooling to room temperature, and grinding to obtain the sepiolite supported ferro-manganese bimetallic catalyst FeMn/SEPs@C.
3. The use of a sepiolite supported iron manganese bimetallic catalyst as claimed in claim 2, wherein: the drying temperature in step S4 was 60 ℃ and the time was 5h.
4. The use of a sepiolite supported iron manganese bimetallic catalyst as claimed in claim 1, wherein: the soluble saccharide comprises glucose, sucrose and chitosan.
5. The use of a sepiolite supported iron manganese bimetallic catalyst as claimed in claim 1, wherein: the inert atmosphere comprises nitrogen and argon.
6. The use of a sepiolite supported iron manganese bimetallic catalyst as claimed in claim 1, wherein: antibiotics include ofloxacin, sulfamethoxazole, and tetracycline hydrochloride.
7. The use of a sepiolite supported iron manganese bimetallic catalyst as claimed in claim 1, wherein: the antibiotic is ofloxacin, every 5-50 mg of FeMn/SEPs@C catalyst is dispersed into 100mL of 10ppm ofloxacin solution, and after 60min to reach adsorption-desorption equilibrium, 0.1M NaOH or H is used for preparing the antibiotic 2 SO 4 The solution adjusts the initial pH value of the system, and then 0.3-0.7. 0.7g/L of peroxymonosulfate is added to start degradation reaction.
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