CN113877514A - Lanthanum ferrite composite oxide with wheat-ear-shaped hierarchical structure and preparation method and application thereof - Google Patents
Lanthanum ferrite composite oxide with wheat-ear-shaped hierarchical structure and preparation method and application thereof Download PDFInfo
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- CN113877514A CN113877514A CN202111188174.1A CN202111188174A CN113877514A CN 113877514 A CN113877514 A CN 113877514A CN 202111188174 A CN202111188174 A CN 202111188174A CN 113877514 A CN113877514 A CN 113877514A
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- 229910052746 lanthanum Inorganic materials 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 150000002603 lanthanum Chemical class 0.000 claims abstract description 13
- 239000000276 potassium ferrocyanide Substances 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 13
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 239000004098 Tetracycline Substances 0.000 claims abstract description 7
- 229960002180 tetracycline Drugs 0.000 claims abstract description 7
- 229930101283 tetracycline Natural products 0.000 claims abstract description 7
- 235000019364 tetracycline Nutrition 0.000 claims abstract description 7
- 150000003522 tetracyclines Chemical class 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 3
- 239000000273 veterinary drug Substances 0.000 claims abstract description 3
- 239000002351 wastewater Substances 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims abstract 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- 239000012266 salt solution Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 241000209140 Triticum Species 0.000 abstract description 5
- 235000021307 Triticum Nutrition 0.000 abstract description 5
- 238000007885 magnetic separation Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910017771 LaFeO Inorganic materials 0.000 description 2
- 229910002321 LaFeO3 Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 241000495841 Oenanthe oenanthe Species 0.000 description 1
- 238000001016 Ostwald ripening Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NNLJGFCRHBKPPJ-UHFFFAOYSA-N iron lanthanum Chemical compound [Fe].[La] NNLJGFCRHBKPPJ-UHFFFAOYSA-N 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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Abstract
The invention discloses a lanthanum ferrite composite oxide and a preparation method and application thereof, wherein the composite oxide is a homogeneous phase high-dispersion wheat ear-shaped hierarchical structure material, and the method comprises the following steps: preparing lanthanum salt into aqueous solution; dropwise adding a potassium ferrocyanide solution into a lanthanum salt aqueous solution to form a white precipitate; carrying out centrifugal separation, washing with deionized water and absolute ethyl alcohol on the precipitate, and drying to obtain a pure white precursor; and calcining the obtained precursor at a controlled temperature, and naturally cooling to obtain the lanthanum ferrite composite oxide with the wheat ear-shaped hierarchical structure. The lanthanum ferrite composite oxide has the magnetic separation characteristic and excellent adsorption performance, can be used for photocatalytic degradation of tetracycline veterinary drug wastewater, and has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of inorganic functional materials, and particularly relates to a lanthanum ferrite composite oxide with a wheat ear-shaped hierarchical structure, and a preparation method and application thereof.
Background
Lanthanum ferrite (LaFeO)3) Is a typical perovskite (ABO)3) The structural composite metal oxide has unique electric, magnetic, catalytic and gas sensitive performances due to stable structure, and has wide application prospects in the fields of electricity, magnetism, photocatalysis and the like, thereby becoming a research hotspot at home and abroad. But its properties are greatly influenced by its structure, size, morphology, and this property ultimately depends on the preparation method. For LaFeO3At present, researchers mainly use a hydrothermal method, a sol-gel method, an ultrasonic chemical method and the like, but the defects of complex preparation method, poor dispersibility, small specific surface, poor adsorption performance, difficulty in repeatability and the like of the composite material still exist, so that the application of the composite material in large-scale industrial production is limited.
On the other hand, a hierarchical structure material having a well-controlled morphology has recently received much attention due to its superior adsorption, separation and catalytic properties due to its large specific surface area, appropriate pore size distribution, and numerous active sites, as compared to a bulk material. However, the hierarchical lanthanum ferrite composite oxide has not been reported. Therefore, the development of the novel hierarchical lanthanum ferrite composite material and the improvement of the preparation technology thereof have important significance.
Disclosure of Invention
In view of the above, the invention provides a preparation method and application of a lanthanum ferrite composite oxide with a wheat-ear-shaped hierarchical structure. Under the condition of room temperature, lanthanum nitrate and potassium ferrocyanide are used as a lanthanum source and an iron source, deionized water is used as a solvent, a lanthanum-iron bimetallic complex precursor is obtained at normal temperature and normal pressure, and then the lanthanum ferrite composite oxide with the hierarchical structure is obtained by sintering under the condition of temperature control. The method has the advantages that the reaction conditions are mild, the obtained composite material has a wheat ear-shaped hierarchical structure, the process is simple, and the energy consumption is low; the lanthanum ferrite composite oxide prepared by the invention has better magnetic separation characteristic and adsorption performance, and can be used in the fields of photocatalytic degradation of organic pollutants, sterilization, disinfection and the like.
The method specifically comprises the following steps:
dissolving lanthanum salt in water to prepare a lanthanum salt solution;
step 2, dropwise adding a potassium ferrocyanide solution under the condition of stirring to form white particle precipitates; standing for 10 min, washing the precipitate for three times by centrifugal separation deionized water, washing for three times by absolute ethyl alcohol, and drying to obtain a white precursor;
and 3, placing the white complex precursor prepared in the step 2 in a crucible, calcining the white complex precursor in a temperature-controlled muffle furnace, and naturally cooling to obtain the hierarchical lanthanum ferrite composite oxide.
Further, the concentration of the lanthanum salt solution in the step 1 is 0.01-0.6 mol/L.
Further, the lanthanum salt solution in the step 1 is a lanthanum nitrate aqueous solution.
Further, the temperature in the stirring condition in the step 2 is 20-25 ℃, the rotating speed is 350-800r/min, and the drying temperature is 40-80 ℃.
Further, in the step 2, the concentration of the potassium ferrocyanide solution is 0.5mol/L, and the molar ratio of the lanthanum salt to the potassium ferrocyanide is 1:5-6: 1.
Further, the calcination temperature in step 3 is 400-800 ℃, the calcination time is 0.5-5 hours, and the heating rate is 1-5 ℃/min.
The invention also discloses application of the hierarchical lanthanum ferrite composite oxide prepared by the preparation method in photocatalytic degradation of tetracycline veterinary drug wastewater.
Compared with the prior art, the invention can obtain the following technical effects:
(1) the preparation method is simple in preparation process, and the precursor is obtained through a one-step method and then is sintered at a controlled temperature to obtain the product.
(2) The preparation method is a normal pressure liquid phase method, and complex processes such as hydrothermal and the like are not needed.
(3) The conversion rate of the raw materials of the invention can reach more than 95 percent in terms of lanthanum.
(4) The lanthanum ferrite composite oxide prepared by the invention has a wheat ear-shaped hierarchical structure, and has the characteristics of magnetic separation and excellent adsorption and photocatalytic degradation performances.
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 is an XRD spectrum of a complex oxide of lanthanum ferrite having a hierarchical structure of a wheat ear shape prepared in example 1 of the present invention. Comparing the standard data, it can be seen that the composite material is pure phase LaFeO3A composite oxide.
FIG. 2 is an SEM photograph of a hierarchical lanthanum ferrite composite oxide prepared in example 1 of the present invention, (a) a partially enlarged photograph, and (b) a global morphology. As can be seen, the LaFeO obtained3The composite oxide is lanthanum ferrite oxide with a wheat-ear-shaped hierarchical structure formed by aggregating nano small particles.
FIG. 3 is a photograph of a magnetic suspension of lanthanum ferrite obtained by the present invention, which shows that it has better magnetic properties and can be easily separated from the suspension system under the action of a magnetic field.
FIG. 4 is a graph showing the performance of photocatalytic degradation of tetracycline by lanthanum ferrite oxide with a hierarchical structure prepared in example 1 of the present invention. It can be seen that the lanthanum ferrite composite oxide has excellent adsorption performance and photocatalytic degradation performance on tetracycline, the degradation rate of 20mg/L tetracycline within 100 minutes can reach 91%, and the lanthanum ferrite composite oxide is at a higher level in the field.
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 hierarchical lanthanum ferrite composite oxide, a preparation method and an application thereof, wherein the hierarchical lanthanum ferrite composite oxide comprises the following steps:
step 2, adding a potassium ferrocyanide solution under the condition of stirring to form white particle precipitates; standing for 10 min, washing the precipitate for three times by centrifugal separation deionized water, washing for three times by absolute ethyl alcohol, and drying to obtain a white precursor;
and 3, placing the white precursor prepared in the step 2 in a crucible, calcining at high temperature by using a temperature-controlled muffle furnace, and naturally cooling to obtain the hierarchical lanthanum ferrite composite oxide.
In the preparation method, potassium ferrocyanide and lanthanum ions form a complex, and micron particles with a hierarchical structure are obtained through Ostwald ripening. During the high-temperature calcination process, the ligand is decomposed to finally form the lanthanum ferrite composite material.
Example 1
Lanthanum nitrate is dissolved in 20mL of deionized water to obtain 0.05mol/L lanthanum nitrate solution, and 6mL of 0.5mol/L potassium ferrocyanide solution is slowly added under the stirring condition of the rotating speed of 220 r/min and the temperature of 20 ℃. 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 white 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 the temperature of 500 ℃ at the temperature rise rate of 5 ℃/min to obtain a product. The scanning electron micrograph of the obtained product is shown in figure 1, and the XRD spectrum is shown in figure 2. The adsorption and photocatalytic degradation performances of the prepared lanthanum ferrite composite oxide on tetracycline are shown in fig. 4, and it can be seen that the lanthanum ferrite composite oxide has excellent adsorption performance, the adsorption removal rate reaches more than 60% within 30 minutes, the lanthanum ferrite composite oxide is continuously degraded under the condition of visible light, and the degradation rate reaches 91% after 100 minutes.
Example 2
Lanthanum nitrate is dissolved in 10mL of deionized water to obtain 0.1mol/L lanthanum nitrate solution, and 10mL of 0.5mol/L potassium ferrocyanide solution is slowly added under the stirring condition of the rotation speed of 200 r/min and the temperature of 25 ℃. 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 white 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 5 ℃/min, and keeping the temperature for 0.5 hour at 600 ℃ to obtain a product.
Example 3
Lanthanum nitrate is dissolved in 10mL of deionized water to obtain 0.30mol/L lanthanum nitrate solution, and 10mL of 0.30mol/L potassium ferrocyanide solution is slowly added under the stirring condition that the rotation speed is 520 r/min and the temperature is 20 ℃. 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 white 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 5 ℃/min, and keeping the temperature for 1 hour at 400 ℃ to obtain a product.
Example 4
Lanthanum nitrate is dissolved in 10mL of deionized water to obtain 0.6mol/L lanthanum nitrate solution, and 2mL of 0.5mol/L potassium ferrocyanide solution is slowly added under the stirring condition that the rotating speed is 320 r/min and the temperature is 20 ℃. 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 white 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 5 ℃/min, and keeping the temperature for 1 hour at 400 ℃ 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 (8)
1. A preparation method of a wheat-ear-shaped lanthanum ferrite composite oxide is characterized in that the obtained wheat-ear-shaped lanthanum ferrite composite oxide is a homogeneous phase high-dispersion wheat-ear-shaped hierarchical structure material, and the preparation method comprises the following steps:
dissolving lanthanum salt in water to prepare a lanthanum salt solution;
step 2, dropwise adding a potassium ferrocyanide solution under the condition of stirring to form white particle precipitates; standing for 10 min, washing the precipitate for three times by centrifugal separation deionized water, washing for three times by absolute ethyl alcohol, and drying to obtain a white precursor;
and 3, placing the white precursor prepared in the step 2 in a crucible, calcining the white precursor in a temperature-controlled muffle furnace, and naturally cooling to obtain the wheat-ear-shaped hierarchical lanthanum ferrite composite oxide.
2. The method of claim 1, wherein the concentration of the lanthanum salt solution in step 1 is 0.01-0.6 mol/L.
3. The method of claim 1, wherein the lanthanum salt solution in step 1 is an aqueous solution of lanthanum nitrate.
4. The method for preparing a complex oxide of lanthanum ferrite in the form of ear as claimed in claim 1, wherein the temperature of the stirring condition in step 2 is 20-25 ℃, the rotation speed is 180-220 r/min, and the drying temperature is 40-80 ℃.
5. The method of claim 1, wherein the molar ratio of lanthanum salt to potassium ferrocyanide is 1:5 to 6: 1.
6. The method for preparing a pseudowheat-like lanthanum ferrite composite oxide as claimed in claim 1, wherein the calcination temperature in step 3 is 400-700 ℃, the calcination time is 0.5-5 hours, and the temperature rise rate is 1-5 ℃/min.
7. A pseudomorphic lanthanum ferrite composite oxide, which is prepared by the preparation method according to any one of claims 1 to 6.
8. The use of the pseudomorphic lanthanum ferrite composite oxide of claim 7 in photocatalytic degradation of tetracycline veterinary drug wastewater.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115501853A (en) * | 2022-09-20 | 2022-12-23 | 北京师范大学珠海校区 | Hierarchical pore structure lanthanum-based hydroxide adsorbing material, and preparation method and application thereof |
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2021
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115501853A (en) * | 2022-09-20 | 2022-12-23 | 北京师范大学珠海校区 | Hierarchical pore structure lanthanum-based hydroxide adsorbing material, and preparation method and application thereof |
| CN115501853B (en) * | 2022-09-20 | 2023-11-14 | 北京师范大学珠海校区 | Multistage pore structure lanthanum-based hydroxide adsorption material, preparation method and application |
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