CN113856612A - Persimmon-shaped magnetically separated LaFeO3/CeO2Composite adsorbent and preparation method thereof - Google Patents
Persimmon-shaped magnetically separated LaFeO3/CeO2Composite adsorbent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a dried persimmon-shaped magnetically separated LaFeO3/CeO2A method of making a composite adsorbent, the method comprising the steps of: preparing a cerium salt and lanthanum salt into a mixed salt solution of cerium and lanthanum, and adding EDTA and hydrochloric acid into the mixed aqueous solution of cerium and lanthanum salt to obtain a light green solution; adding a potassium ferrocyanide solution to form a green precipitate, carrying out centrifugal separation on the precipitate, washing the precipitate with deionized water for three times, washing the precipitate with absolute ethyl alcohol for three times, and drying the precipitate to obtain a green precursor; the obtained precursor is calcined at high temperature by a temperature-controlled muffle furnace,naturally cooling to obtain dried persimmon-like LaFeO3/CeO2A composite adsorbent. The invention relates to a persimmon-shaped magnetic separation LaFeO3/CeO2The compound adsorbent can be used for the field of adsorbing water antibiotics.
Description
Technical Field
The invention belongs to the technical field of inorganic functional materials, and particularly relates to a persimmon-shaped magnetically separated LaFeO3/CeO2A preparation method and application of the composite adsorbent.
Background
Magnetic separation techniques are widely studied in the fields of bioseparation, environmental governance, and the like. Under the condition of a proper external magnetic field, a convenient and effective way is provided for the separation of the magnetic separation material. Annual tetracycline production ranks world-second among antibiotics and is also often found in drinking water, making traditional treatment processes impossible to eliminate due to its long-term stability and low biodegradability. Residual tetracycline in water can harm human health through the food chain. Residual tetracycline in the water body can be effectively removed through the magnetic adsorption material.
Lanthanum ferrite (LaFeO)3) The rare earth composite metal oxide is a typical rare earth composite metal oxide with a perovskite structure, has a stable crystal structure and excellent physicochemical properties, is low in price, and is a hot spot of current research. The metal-organic framework Materials (MOFs) generally use metal ions as connecting points, organic ligands support and form space 3D extension, are another important novel porous material besides zeolite and carbon nanotubes, and are widely applied to catalysis, energy storage and separation. Preparation of LaFeO by using MOFs as precursor3The pore structure can be effectively reserved, the specific surface area is increased, and the adsorption performance is improved. LaFeO3The magnetic adsorbent has magnetism, and can be used for high-efficiency magnetic separation adsorbents. In terms of environmental pollution control, CeO2Can decompose organic substances which are difficult to decompose in the environment into CO2And H2Inorganic substances such as O, andsecondary pollution is generated. LaFeO3/CeO2The magnetic composite material can exert respective advantages to adsorb and degrade residual antibiotics in the water body.
Disclosure of Invention
The invention provides a persimmon-shaped magnetically separated LaFeO3/CeO2The invention discloses a preparation method and application of a compound adsorbent, wherein cerium nitrate, lanthanum nitrate and potassium ferrocyanide are used as cerium, lanthanum source and iron source, EDTA is used as a coordination agent, pH is adjusted by hydrochloric acid to obtain MOFs precursor, and then the MOFs precursor is sintered at high temperature to obtain persimmon cake-shaped magnetically separated LaFeO3/CeO2A composite nanomaterial. The method has the advantages of mild reaction conditions, simple process and short time consumption; the nano material prepared by the invention can be used for the field of water body antibiotic adsorption.
In order to solve the technical problems, the application discloses a persimmon-like magnetically separated LaFeO3/CeO2The preparation method of the composite adsorbent comprises the following steps:
step 1, dissolving cerium nitrate and lanthanum nitrate in water to prepare a cerium-lanthanum mixed aqueous solution;
step 3, adding a potassium ferrocyanide solution into the light green solution prepared in the step 2, and then placing in the air for aging; washing the precipitate with centrifugal separation deionized water for three times, washing with absolute ethyl alcohol for three times, and drying to obtain a green precursor;
step 4, placing the green precursor prepared in the step 3 in a crucible, calcining at high temperature by using a temperature-controlled muffle furnace, and naturally cooling to obtain the persimmon-shaped magnetically separated LaFeO3/CeO2A composite adsorbent.
Further, the concentration of the cerium nitrate and lanthanum nitrate solution in the step 1 is 0.02-0.6 mol/L;
further, the temperature in the stirring condition in the step 2 is 20-28 ℃, and the rotating speed is 180-220 r/min.
Further the molar ratio of cerium, lanthanum salt and EDTA in step 2 is 1:0.5-1: 5.
In a further step 3, the concentration of the potassium ferrocyanide solution is 0.5mol/L, the molar ratio of the cerium salt to the lanthanum salt to the potassium ferrocyanide is 1:1-6:1, and the volume ratio of the potassium ferrocyanide solution to the hydrochloric acid is 100:1-190: 1.
In the step 3, the reaction temperature is 20-28 ℃, and the drying temperature is 40-80 ℃.
Further, the calcination temperature in the step 4 is 350-800 ℃, the calcination time is 1-6 hours, and the heating rate is 1-5 ℃/min.
The invention also discloses a persimmon-shaped magnetically separated LaFeO prepared by the preparation method3/CeO2A composite adsorbent.
Compared with the prior art, the invention can obtain the following technical effects:
(1) the preparation method is simple in preparation process and high in production efficiency, and the precursor is obtained through a one-step method and then sintered at high temperature to obtain the product.
(2) The precursor preparation of the invention is carried out at normal temperature without heating.
(3) The preparation method is a normal pressure liquid phase method, and complex processes such as hydrothermal and the like are not needed.
(4) The conversion rate of the raw materials of the invention can reach more than 90 percent by the cerium and the lanthanum.
(5) The persimmon-shaped magnetically separated LaFeO prepared by the invention3/CeO2Antibiotic adsorption properties of the compound.
(6) The persimmon-shaped magnetically separated LaFeO prepared by the invention3/CeO2The compound can be magnetically recovered after adsorbing antibiotics in water.
Of course, it is not necessary for any one product in which the invention is practiced to achieve all of the above-described technical effects simultaneously.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a persimmon-like magnetically separated LaFeO prepared in example 1 of the present invention3/CeO2SEM photograph of the composite adsorbent;
FIG. 2 shows a persimmon-like magnetically separated LaFeO prepared in example 1 of the present invention3/CeO2XRD spectrum of the composite adsorbent;
FIG. 3 shows a persimmon-like magnetically separated LaFeO prepared in example 1 of the present invention3/CeO2A magnetic separation effect diagram of the composite adsorbent;
FIG. 4 shows a persimmon-like magnetically separated LaFeO prepared in example 1 of the present invention3/CeO2And (3) a composite adsorbent adsorption performance graph.
Detailed Description
The following embodiments are described in detail with reference to the accompanying drawings, so that how to implement the technical features of the present invention to solve the technical problems and achieve the technical effects can be fully understood and implemented.
The application discloses a dried persimmon-like magnetically separated LaFeO3/CeO2The preparation method of the composite adsorbent comprises the following steps:
step 1, dissolving cerium nitrate and lanthanum nitrate in water to prepare a cerium-lanthanum mixed aqueous solution.
And 2, adding EDTA and then adding hydrochloric acid at the stirring speed of 180-220r/min to form a light green solution, wherein the molar ratio of cerium to lanthanum salt to EDTA is 1:0.5-1: 5.
Step 3, adding 0.5mol/L potassium ferrocyanide solution into the light green solution prepared in the step 2, and then placing in the air for aging; washing the precipitate with centrifugal separation deionized water for three times, washing with absolute ethyl alcohol for three times, and drying to obtain a green precursor, wherein the molar ratio of cerium to lanthanum salt to potassium ferrocyanide is 1:1-6:1, the volume ratio of potassium ferrocyanide solution to hydrochloric acid is 100:1-190:1, the reaction temperature is 20-28 ℃, and the drying temperature is 40-80 ℃.
Step 4, placing the green precursor prepared in the step 3 in a crucible, and using a temperature control muffleCalcining the mixture for 1 to 6 hours at the temperature rising rate of 1 to 5 ℃/min under the condition of 350 ℃ and 800 ℃, and naturally cooling to obtain the persimmon-shaped magnetically separated LaFeO3/CeO2A composite adsorbent.
The invention also provides the dried persimmon-shaped magnetically separated LaFeO prepared by the preparation method3/CeO2Composite adsorbent material
In the present preparation method
1. The hydrochloric acid has the function of adjusting the pH, and the EDTA (ethylene diamine tetraacetic acid) disodium salt has 6 coordination atoms for coordination, four oxygen atoms on four carboxyl groups and two nitrogen atoms on two amino groups, has strong coordination capacity and forms a 1:1 complex with cerium and lanthanum.
2. EDTA as ligand forms complex with cerium and lanthanum ions, and potassium ferrocyanide can coordinate with cerium and lanthanum ions. If EDTA is not added, the persimmon cake-shaped appearance can not be obtained. If potassium ferrocyanide is not added, MOFs precursors cannot be obtained.
3. Competitive coordination of potassium ferrocyanide and EDTA provides structure-oriented action for formation of dried persimmon-like precursor, lanthanide ions and compounds are paramagnetic, and during high-temperature calcination, ligand is decomposed to finally form magnetically separated LaFeO3/CeO2The composite adsorbent material.
Example 1
Dissolving cerium nitrate and lanthanum nitrate in deionized water, preparing 20 mL of mixed aqueous solution of 0.05mol/L cerium nitrate and 0.05mol/L lanthanum nitrate, adding 5 mL of 0.2 mol/L EDTA solution and 0.05 mL of hydrochloric acid under the stirring condition of the rotation speed of 200r/min and the temperature of 25 ℃, and adding 6 mL of 0.5mol/L potassium ferrocyanide solution after a light green solution appears. Potassium ferrocyanide needs to be added after hydrochloric acid and EDTA; and carrying out centrifugal separation, washing with deionized water for three times, washing with absolute ethyl alcohol for three times, and drying at 60 ℃ to obtain a green precursor. And transferring the dried precursor sample into a crucible, sintering the precursor sample at high temperature by using a temperature-controlled muffle furnace, wherein the heating rate is 2 ℃/min, and keeping the temperature for 2 hours at 500 ℃ to obtain a product. The scanning electron micrograph of the obtained product is shown in figure 1, the original morphology can be maintained after high-temperature calcination, the XRD spectrogram is shown in figure 2, and each XRD spectrogramDiffraction peak and LaFeO3/CeO2Diffraction peaks of a standard spectrogram of the compound correspond to one another, and other miscellaneous peaks are not found, which indicates that the prepared magnetically separated LaFeO3/CeO2The purity of the compound is higher. As shown in FIG. 3, LaFeO was magnetically separated3/CeO2Magnetic phenomenon of the complex, the complex adsorbent can be magnetically recycled, and the prepared dried persimmon-like magnetic separation LaFeO is used3/CeO2The performance of the composite adsorbent for adsorbing tetracycline is shown in fig. 4. In 150-300 ppm tetracycline solution, the adsorption amount is 53 mg/g-72 mg/g after 2 hours of adsorption.
Example 2
Dissolving cerium nitrate and lanthanum nitrate in deionized water, preparing 20 mL of mixed aqueous solution of 0.05mol/L cerium nitrate and 0.05mol/L lanthanum nitrate, adding 4 mL of 0.2 mol/L EDTA solution and 0.05 mL of hydrochloric acid under the stirring condition of the rotation speed of 200r/min and the temperature of 25 ℃, and adding 4 mL of 0.5mol/L potassium ferrocyanide solution after a light green solution appears. Potassium ferrocyanide needs to be added after hydrochloric acid and EDTA; and carrying out centrifugal separation, washing with deionized water for three times, washing with absolute ethyl alcohol for three times, and drying at 60 ℃ to obtain a green precursor. And transferring the dried precursor sample into a crucible, sintering the precursor sample at high temperature by using a temperature-controlled muffle furnace, wherein the heating rate is 2 ℃/min, and keeping the temperature for 2 hours at 600 ℃ to obtain a product.
Example 3
Dissolving cerium nitrate and lanthanum nitrate in deionized water, preparing 25 mL of mixed aqueous solution of 0.05mol/L cerium nitrate and 0.05mol/L lanthanum nitrate, adding 5 mL of 0.2 mol/L EDTA solution and 0.05 mL of hydrochloric acid under the stirring condition of the rotation speed of 200r/min and the temperature of 25 ℃, and adding 6 mL of 0.5mol/L potassium ferrocyanide solution after a light green solution appears. Potassium ferrocyanide needs to be added after hydrochloric acid and EDTA; and carrying out centrifugal separation, washing with deionized water for three times, washing with absolute ethyl alcohol for three times, and drying at 60 ℃ to obtain a green precursor. And transferring the dried precursor sample into a crucible, sintering the precursor sample at high temperature by using a temperature-controlled muffle furnace, and keeping the temperature for 2 hours at 550 ℃ at the heating rate of 5 ℃/min to obtain a product.
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. Persimmon-shaped magnetically separated LaFeO3/CeO2The preparation method of the composite adsorbent is characterized by comprising the following steps:
step 1, dissolving cerium nitrate and lanthanum nitrate in water to prepare a cerium-lanthanum mixed aqueous solution;
step 2, adding EDTA and then adding hydrochloric acid under the condition of stirring;
step 3, adding a potassium ferrocyanide solution into the light green solution prepared in the step 2, and then placing in the air for aging; carrying out centrifugal separation on the precipitate, washing the precipitate with deionized water for three times, washing the precipitate with absolute ethyl alcohol for three times, and drying the precipitate to obtain a green precursor;
step 4, placing the green precursor prepared in the step 3 in a crucible, calcining at high temperature by using a temperature-controlled muffle furnace, and naturally cooling to obtain the persimmon-shaped magnetically separated LaFeO3/CeO2A composite adsorbent.
2. The persimmon-like magnetically separated LaFeO according to claim 13/CeO2The preparation method of the composite adsorbent is characterized in that the concentrations of cerium nitrate and lanthanum nitrate in the step 1 are both 0.02-0.6 mol/L.
3. The persimmon-like magnetically separated LaFeO according to claim 13/CeO2The preparation method of the composite adsorbent is characterized in that the temperature in the stirring condition in the step 2 is 20-28 ℃, and the rotating speed is 180-220 r/min.
4. The persimmon-like magnetically separated LaFeO according to claim 13/CeO2The preparation method of the composite adsorbent is characterized in that the molar ratio of the cerium salt to the lanthanum salt is 1:4-2: 1.
5. The persimmon-like magnetically separated LaFeO according to claim 13/CeO2The preparation method of the compound adsorbent is characterized in that the molar ratio of the cerium-lanthanum mixed salt to the EDTA is 1:0.5-1: 5.
6. The persimmon-like magnetically separated LaFeO according to claim 13/CeO2The preparation method of the composite adsorbent is characterized in that the concentration of the potassium ferrocyanide solution is 0.5mol/L, the molar ratio of cerium to lanthanum salt to potassium ferrocyanide is 1:1-6:1, and the volume ratio of the potassium ferrocyanide solution to hydrochloric acid is 100:1-190: 1.
7. The persimmon-like magnetically separated LaFeO according to claim 13/CeO2The preparation method of the composite adsorbent is characterized in that the reaction temperature in the step 1-3 is 20-28 ℃, and the drying temperature is 40-80 ℃.
8. The persimmon-like magnetically separated LaFeO according to claim 13/CeO2The preparation method of the composite adsorbent is characterized in that the calcination temperature in the step 4 is 350-800 ℃, the calcination time is 1-6 hours, and the heating rate is 1-5 ℃/min.
9. Persimmon-shaped magnetically separated LaFeO3/CeO2Composite adsorbent, characterized in that it is prepared by the process according to any one of claims 1 to 8.
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| CN113856610A (en) * | 2021-09-28 | 2021-12-31 | 淮阴师范学院 | Orange-shaped magnetic lanthanum ferrite adsorbent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113856610A (en) * | 2021-09-28 | 2021-12-31 | 淮阴师范学院 | Orange-shaped magnetic lanthanum ferrite adsorbent and preparation method thereof |
| CN113856610B (en) * | 2021-09-28 | 2023-08-15 | 淮阴师范学院 | Orange-shaped magnetic lanthanum ferrite adsorbent and preparation method thereof |
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Application publication date: 20211231 |