CN111229154A - MgFe2O4/Fe2O3Composite and preparation method and application thereof - Google Patents
MgFe2O4/Fe2O3Composite and preparation method and application thereof Download PDFInfo
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- CN111229154A CN111229154A CN202010098880.6A CN202010098880A CN111229154A CN 111229154 A CN111229154 A CN 111229154A CN 202010098880 A CN202010098880 A CN 202010098880A CN 111229154 A CN111229154 A CN 111229154A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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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
Abstract
The invention discloses MgFe2O4/Fe2O3A method for preparing a composite comprising MgFe and use thereof2O4/Fe2O3Preparation of the compound and application thereof in adsorption removal of tetracycline in water. The preparation method is to use FeCl3·6H2O and MgCl2·6H2O is taken as a raw material, NaOH solution is taken as a solvent, and MgFe is hydrothermally synthesized by adopting a one-pot method2O4/Fe2O3And (c) a complex. Then, magnetic stirring adsorption is combined to remove tetracycline in water, and the experimental conditions are controlled such that the addition amount of the catalyst is 5mg/mL and the tetracycline isThe initial concentration was 20mg/L and the magnetic stirring time was 30 min. MgFe prepared by the method2O4/Fe2O3The removal rate of the compound to tetracycline in water can reach 69.9% -75.2%.
Description
Technical Field
The invention relates to the technical field of environmental pollution remediation, and provides MgFe2O4/Fe2O3A compound, a preparation method thereof and application thereof in adsorbing tetracycline in wastewater.
Technical Field
In recent years, the problem of environmental pollution has been increasing. The tetracycline antibiotics have the defects of low raw material utilization rate and low purity of refined tetracycline in the production process, and a large amount of tetracycline is contained in the wastewater in the production process. Statistically, most rivers worldwide contain genes for resistance to sulfonamides and tetracyclines. In order to avoid the resistance of tetracycline residues in wastewater to human and ecological environments, it is necessary to treat tetracycline in wastewater to improve the quality of wastewater. Compared with other processes, the technology has the advantages of lower equipment requirement, environmental friendliness, relatively simple process, lower energy consumption, recoverability and high utilization rate, and thus, the method is an environmental pollution remediation method with great prospect.
MgFe2O4Is made of rich elements (Mg, Fe, O), is red, is harmless to the environment and is a soft magnetic n-type semiconductor material. MgFe2O4/Fe2O3The compound not only has MgFe2O4Has the advantages of large specific surface area and better adsorption performance.
Thus passing through MgFe2O4/Fe2O3The compound is used for removing tetracycline in organic wastewater by adsorption, and is a promising restoration method for environmental pollution.
Disclosure of Invention
The purpose of the invention isProviding MgFe2O4/Fe2O3A compound and a preparation method and application thereof. The preparation method is to use FeCl3·6H2O and MgCl2·6H2Preparing MgFe by hydrothermal synthesis with O as raw material2O4/Fe2O3Compounding, magnetic stirring and MgFe2O4/Fe2O3A method for removing tetracycline in water by adsorption of the compound.
The invention is realized by the following technical scheme: MgFe2O4/Fe2O3The compound is prepared by the following steps:
1) FeCl is added3·6H2O and MgCl2·6H2Dissolving O in NaOH solution respectively, mixing the two solutions, magnetically stirring and ultrasonically treating;
2) transferring the mixture to a polytetrafluoroethylene reaction kettle for hydrothermal reaction;
3) cooling to room temperature, centrifugally filtering, washing for 3-4 times by using distilled water and absolute ethyl alcohol, drying and grinding to obtain the target product.
Preferably, one kind of MgFe described above2O4/Fe2O3Composite, step 1), in molar ratio, FeCl3·6H2O：MgCl2·6H2O＝1:0.5-5。
Preferably, one kind of MgFe described above2O4/Fe2O3The concentration of the compound and sodium hydroxide is 0.1-5 mol/L.
Preferably, one kind of MgFe described above2O4/Fe2O3The temperature of the hydrothermal reaction in the step 2) is 160-200 ℃, and the reaction time is 20-30 hours.
Preferably, one kind of MgFe described above2O4/Fe2O3And (3) drying the compound at 50-70 ℃ for 2-3 hours.
MgFe described above2O4/Fe2O3The application of the compound in adsorbing organic pollutants in wastewater.
Preferably, for the above-mentioned use, said organic contaminant is tetracycline.
Preferably, in the application, the concentration of the tetracycline in the wastewater is 10-50 mg/L.
Preferably, the above application, method is as follows, in the waste water containing tetracycline, add MgFe2O4/Fe2O3And (4) magnetically stirring the compound for 30-40 min.
Preferably, the application is that 0.5-5g MgFe is added into each liter of wastewater containing tetracycline2O4/Fe2O3And (c) a complex.
The invention has the advantages and effects that:
domestic MgFe2O4/Fe2O3The complex is used as an adsorbent to adsorb organic pollutants and is only reported in documents. We passed on MgFe2O4/Fe2O3The synthesis of the compound and the adsorption condition of the compound to the antibiotic wastewater are preliminarily explored. And the adsorption method has the advantages of simple and convenient operation, simple facilities, environmental protection, no secondary pollution and the like. Verification shows that MgFe2O4/Fe2O3The compound is used as an adsorbent to adsorb tetracycline in organic wastewater, and is an environment-friendly, energy-saving and environment-friendly restoration method with great prospect.
Drawings
FIG. 1 is a graph of MgFe synthesized with different concentrations of NaOH prepared in example 12O4/Fe2O3An X-ray diffraction (XRD) pattern of the complex;
FIG. 2 is a graph of MgFe synthesized with different concentrations of NaOH prepared in example 12O4/Fe2O3SEM images of the composites;
wherein A: cNaOH＝0.1mol/L；B：CNaOH＝0.8mol/L；C：CNaOH＝1.0mol/L；D：CNaOH＝3.0mol/L；E：CNaOH＝5.0mol/L。
FIG. 3 shows MgFe synthesized from NaOH solutions of different concentrations2O4/Fe2O3The effect graph of tetracycline adsorption of the compound is shown;
FIG. 4 is Mg2+/Fe3+MgFe prepared in different proportions2O4/Fe2O3The effect graph of tetracycline adsorption of the compound is shown;
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1MgFe2O4/Fe2O3Composite material
MgFe2O4/Fe2O3A method of preparing a composite comprising the steps of:
the method comprises the following steps: adding 5mmol of FeCl3·6H2O and 10mmol MgCl2·6H2Dissolving O in 30ml of NaOH solution with the concentration of 1.0mol/L respectively, mixing the two solutions into the same conical flask, magnetically stirring at room temperature for 30min, and then carrying out ultrasonic treatment at 500W for 30 min.
Step two: and (3) transferring the solution prepared in the step one to 100ml of polytetrafluoroethylene, putting the solution into an oven, reacting the solution for 24 hours at 180 ℃, and cooling to room temperature after the reaction is finished.
Step three: washing the product with distilled water and anhydrous ethanol for 3-5 times respectively, and collecting the residue (i.e. MgFe)2O4/Fe2O3Compound) to an oven, and drying for 2 hours at 60 ℃ to obtain the target product.
Example 2 MgFe synthesized in sodium hydroxide solutions of different concentrations2O4/Fe2O3Composite material
The method comprises the following steps: adding 5mmol of FeCl3·6H2O and 10mmol MgCl2·6H2O is respectively dissolved in 30ml of NaOH solution with the concentration of 0.1mol/L, 0.5mol/L, 0.8mol/L, 0.9mol/L, 1mol/L, 3mol/L and 5mol/L, the two solutions are mixed into the same conical flask, magnetic stirring is carried out for 30min at room temperature, and then ultrasonic treatment is carried out for 30min under the ultrasonic power of 500W.
Step two: and (3) transferring the solution prepared in the step one to 100ml of polytetrafluoroethylene, putting the solution into an oven, reacting the solution for 24 hours at 180 ℃, and cooling to room temperature after the reaction is finished.
Step three: washing the product with distilled water and anhydrous ethanol for 3-5 times respectively, and collecting the residue (i.e. MgFe)2O4/Fe2O3Compound) to an oven for drying for 2 hours at 60 ℃ to obtain MgFe synthesized in sodium hydroxide solution with different concentrations2O4/Fe2O3And (c) a complex.
FIG. 1 shows MgFe synthesized in sodium hydroxide solutions of different concentrations2O4/Fe2O3X-ray diffraction pattern of the complex. Contains MgFe2O4Standard card (JCPDS No.89-7746), Fe2O3Standard card (JCPDS No.89-0596) and MgFe synthesized by sodium hydroxide solutions with different concentrations (0.1mol/L, 0.5mol/L, 0.8mol/L, 0.9mol/L, 1mol/L, 3mol/L and 5mol/L)2O4/Fe2O3XRD pattern of the complex.
FIG. 2 shows the preparation of MgFe synthesized by NaOH with different concentrations2O4/Fe2O3SEM image of the composite, visible; when the concentration of the NaOH solution is 0.1mol/L, MgFe2O4/Fe2O3The shape of the compound is a uniform ellipsoid structure with the diameter of about 300-400nm, and when the concentration of NaOH solution is 0.8mol/L, MgFe2O4/Fe2O3The shape diameter of the compound is about 200-300nm, and the MgFe is in a mixed structure of a sheet and a cube, and when the concentration of the NaOH solution is 1.0mol/L2O4/Fe2O3The shape of the compound is an elliptical flaky structure with the diameter of about 50nm-250nm, and when the concentration of NaOH solution is 3.0mol/L, MgFe2O4/Fe2O3The shape of the compound is an elliptical sheet structure with the diameter of about 200-400nm, and when the concentration of NaOH solution is 5.0mol/L, MgFe2O4/Fe2O3The morphology of the composite is an elliptical sheet structure with a diameter of about 250nm to 500 nm.
Example 3 different concentrations of NaOH-synthesized MgFe2O4/Fe2O3Effect of the Compound on adsorbing Tetracycline
Comparison of MgFe synthesized with NaOH of different concentrations2O4/Fe2O3The tetracycline adsorption effect of the compound is as follows:
the method comprises the following steps: seven 10mL tetracycline solutions with the concentration of 20mg/L are taken to be put in a beaker, and 5mg of MgFe synthesized by sodium hydroxide solutions with different concentrations (0.1mol/L, 0.5mol/L, 0.8mol/L, 0.9mol/L, 1mol/L, 3mol/L and 5mol/L) which are accurately weighed are respectively added2O4/Fe2O3The compound was magnetically stirred at 1000rpm for 30 min.
Step two: sampling suspension, centrifuging, collecting supernatant, determining tetracycline concentration, and calculating MgFe2O4/Fe2O3The tetracycline adsorption efficiency of the complex, as shown in FIG. 3, can be seen for MgFe synthesized at NaOH concentrations of 0.1, 0.8, 1.0, 3.0 and 5.0mol/L2O4/Fe2O3The adsorption removal rate of the compound on the tetracycline is 3.06 +/-0.97%, 69.9 +/-3.49%, 75.2 +/-4.51%, 68.1 +/-4.48% and 61.4 +/-6.39% respectively.
When the concentration of the synthesized NaOH solution is 1.0mol/L, the adsorption effect is best, and the adsorption rate can reach 75.2 +/-4.51 percent, mainly because of MgFe under the concentration2O4/Fe2O3The oval sheet-shaped structure with the diameter of the composite between 50nm and 250nm has larger specific surface area, so that the adsorption efficiency is better.
Example 4 different proportions of Mg2+/Fe3+Prepared MgFe2O4/Fe2O3Composite material
The method comprises the following steps: adding 5mmol of FeCl3·6H2O、10mmol MgCl2·6H2And O, respectively dissolving in 30ml of NaOH solution with the concentration of 1.0mol/L, mixing the two solutions into the same conical flask, magnetically stirring at room temperature for 30min, and then carrying out ultrasonic treatment at 500W for 30 min.
Step two: and (3) transferring the solution prepared in the step one to 100ml of polytetrafluoroethylene, putting the solution into an oven, reacting the solution for 24 hours at 180 ℃, and cooling to room temperature after the reaction is finished.
Step (ii) ofThirdly, the method comprises the following steps: washing the product with distilled water and anhydrous ethanol for 3-5 times respectively, and collecting the residue (i.e. MgFe)2O4/Fe2O3Compound) to an oven for drying for 2 hours at 60 ℃ to obtain Mg2+/Fe3+The molar ratio is 2:1 of MgFe2O4/Fe2O3And (c) a complex.
The procedure is as above, FeCl3·6H2O、MgCl2·6H2The dosage of O is respectively 5mmol and 5mmol to prepare Mg2+/Fe3+The molar ratio is 1:1 of MgFe2O4/Fe2O3And (c) a complex.
The procedure is as above, FeCl3·6H2O、MgCl2·6H2The dosage of O is respectively 10mmol and 5mmol, and Mg is prepared2+/Fe3+The molar ratio is 1:2 MgFe2O4/Fe2O3And (c) a complex.
EXAMPLE 5 different proportions of Mg2+/Fe3+Prepared MgFe2O4/Fe2O3Effect of the Compound on adsorbing Tetracycline
Comparing Mg at different proportions2+/Fe3+Prepared MgFe2O4/Fe2O3The tetracycline adsorption effect of the compound is as follows:
the method comprises the following steps: taking 10mL of tetracycline solution with the concentration of 20Mg/L into a beaker, and adding accurately weighed 5Mg of Mg2+/Fe3+The molar ratio is 2: 1. 1: 1. 1:2 MgFe2O4/Fe2O3The compound was magnetically stirred at 1000rpm for 30 min.
Step two: sampling suspension, centrifuging, collecting supernatant, determining tetracycline concentration, and calculating MgFe2O4/Fe2O3The tetracycline adsorption efficiency of the complex is shown in FIG. 4, and Mg can be seen2+/Fe3+The ratio of (A) to (B) is 1: 2; MgFe prepared at 1:1 and 2:12O4/Fe2O3The adsorption removal rate of the compound to the tetracycline is 52.3 +/-2.23%, 56.5 +/-3.30% and 75.2 +/-4.51% respectively. Wherein Mg2+/Fe3+In a ratio of2:1, MgFe2O4/Fe2O3The compound has larger specific surface area and thus has the best adsorption removal efficiency on the tetracycline in the water.
Claims (10)
1. MgFe2O4/Fe2O3The compound is characterized by comprising the following preparation methods:
1) FeCl is added3·6H2O and MgCl2·6H2Dissolving O in NaOH solution respectively, mixing the two solutions, magnetically stirring and ultrasonically treating;
2) transferring the mixture to a polytetrafluoroethylene reaction kettle for hydrothermal reaction;
3) cooling to room temperature, centrifugally filtering, washing for 3-4 times by using distilled water and absolute ethyl alcohol, drying and grinding to obtain the target product.
2. MgFe according to claim 12O4/Fe2O3The compound is characterized in that in the step 1), FeCl is used according to the molar ratio3·6H2O：MgCl2·6H2O＝1:0.5-2。
3. MgFe according to claim 12O4/Fe2O3The compound is characterized in that the concentration of the sodium hydroxide is 0.1-5 mol/L.
4. MgFe according to claim 12O4/Fe2O3The compound is characterized in that in the step 2), the temperature of the hydrothermal reaction is 160-200 ℃, and the reaction time is 20-30 hours.
5. MgFe according to claim 12O4/Fe2O3The compound is characterized in that in the step 3), the drying temperature is 50-70 ℃, and the drying time is 2-3 hours.
6. MgFe of claim 12O4/Fe2O3The application of the compound in adsorbing organic pollutants in wastewater.
7. The use according to claim 6, wherein said organic contaminant is tetracycline.
8. The use according to claim 7, wherein the concentration of tetracycline in the wastewater is 10-50 mg/L.
9. Use according to claim 8, characterized in that MgFe is added to the waste water containing tetracycline2O4/Fe2O3And (4) magnetically stirring the compound for 30-40 min.
10. Use according to claim 9, characterized in that 0.5-5g MgFe per liter of wastewater containing tetracycline is added2O4/Fe2O3And (c) a complex.
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Cited By (3)
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| CN112047568A (en) * | 2020-08-27 | 2020-12-08 | 盐城师范学院 | Aquaculture wastewater sterilization treatment system and method |
| CN113318740A (en) * | 2021-06-29 | 2021-08-31 | 辽宁大学 | Cu2O/MgFe2O4Catalyst, preparation method and application thereof |
| CN113351218A (en) * | 2021-06-29 | 2021-09-07 | 辽宁大学 | Cu2O/BiFeO3Composite material and preparation method and application thereof |
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| CN113318740A (en) * | 2021-06-29 | 2021-08-31 | 辽宁大学 | Cu2O/MgFe2O4Catalyst, preparation method and application thereof |
| CN113351218A (en) * | 2021-06-29 | 2021-09-07 | 辽宁大学 | Cu2O/BiFeO3Composite material and preparation method and application thereof |
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