CN111302381A - Magnetic cerium oxide and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of materials, and relates to magnetic cerium oxide and a preparation method thereof. The magnetic cerium oxide synthesized by the method takes ferrite as a magnetic substrate, has the characteristics of abundant varieties, large specific surface area, high stability, good magnetism and the like, and is expected to have more applications in the aspects of catalysis, adsorption, biochemistry and the like.
Description
Technical Field
The invention belongs to the technical field of materials, and relates to magnetic cerium oxide and a preparation method thereof.
Background
Cerium oxide is one of the most important rare earth oxides, and has been widely used in the fields of catalysts, ultraviolet absorbing materials, oxygen sensitive materials, solid oxide battery materials, polishing materials, and the like because of its excellent optical, electrical, and magnetic properties. The magnetic cerium oxide endows the cerium oxide with magnetic performance, is beneficial to recovery and prevents secondary pollution in the application process of the cerium oxide.
The existing magnetic cerium oxide is mostly Fe3O4The magnetic substrate is prepared by a two-step method or a multi-step method mostly, and the process is complex. Li, etc. (Li K, et al. Magnetic ordered mesopous Fe3O4/CeO2composition with synthesis of adsorption and Fenton catalysis Applied Surface science 2017, 425: 526-3O4/CeO2The adsorption and Fenton catalysis of the composite material are cooperated for the adsorption and catalysis of the dye. Gan et al (Gan G, et al. A novel magnetic nanoscaled Fe3O4/CeO2composite precipitated by oxidation-precipitation process and impregnation for the definition of organic G in aqueous solution as Fenton-like hetereogenous catalyst, Chemospere, 2017, 168: 254-263) by three different preparation methods, namely a coprecipitation method, an impregnation oxidation precipitation method and an impregnation reduction precipitation method, to synthesize the magnetic nano-particles Fe3O4/CeO2. Preparation of high-sensitivity and low-sensitivity magnetic cerium oxide material and application thereof in dye wastewater treatment [ D]Shanghai, university of Shanghai science and technology application, 2019.5) prepared magnetic Fe by sol-gel method3O4/CeO2A composite material. Research on adsorption performance of phosphoric acid salt in water by Ninghong cerium oxide and magnetic nano composite material thereof [ D]Taigen, university of tai-theorem 2017.06) was deposited on Fe using cerous chloride as inorganic cerium source and CTAB as template3O4@SiO2Loading cerium oxide on the surface of the magnetic nano-particles, and finally removing the template agent by adopting acetone to obtain the magnetic nano-composite material Fe with the core-shell structure3O4@SiO2@CeO2. Patent [201310049066.5]A magnetic nano ceria ozone catalyst, the magnetic nano ceria ozone catalyst comprises nano Fe3O4Core, wrapping SiO2An intermediate layer, and a support on SiO2CeO on the intermediate layer2The active component is prepared by preparing nano Fe by hydrolysis3O4The core is wrapped by SiO with a certain thickness2An intermediate layer, and adding CeO2Wrapped in SiO2Encapsulated nano-Fe3O4On the particles. Patent [ 201610410600.4]Relates to a preparation method of magnetic load cerium oxide for treating waste gas, which synthesizes Fe-containing magnetic organic hydrotalcite as a magnetic substrate. Patent [201710616148.1]Discloses a preparation method and application of a cerium dioxide-attapulgite-ferroferric oxide magnetic nano composite material, wherein the preparation steps comprise the following three steps: step one, purifying attapulgite; step two, modifying the attapulgite; and step three, preparing the cerium dioxide-attapulgite-ferroferric oxide magnetic nano-carrier.
Disclosure of Invention
The patent aims to provide the magnetic cerium oxide with excellent performance and simple preparation process so as to solve the problems of single variety, complex preparation process, high cost and the like of the existing magnetic cerium oxide.
The invention is realized by the following technical scheme:
a preparation method of magnetic cerium oxide comprises the following steps:
(1) with M (II) (NO)3)2·6H2O、Fe(NO3)3·9H2O preparing solution A, M2+With Fe3+The molar ratio is 1 (1.5-3); preparing solution B from NaOH, and controlling NO in solution A and B3-Uniformly dropwise adding the solution B into the solution A, magnetically stirring, and reacting to obtain a precursor C, wherein the molar ratio of the solution B to NaOH is 1 (1.5-3);
(2) taking a certain amount of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and D3-The molar ratio was (1.5-3): 1, uniformly dropwise adding the solution B into the solution D, magnetically stirring, and reacting to obtain a precursor E;
(3) pressing the precursor C and the precursor E according to M2+And Ce2+Mixing the components according to the molar ratio of (0.1-1), transferring the mixture into a hydrothermal kettle, reacting at a certain temperature, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
Preferably, in the step (1), M is a divalent metal element selected from Fe, Mg, Zn, Ni, Co, Mn and Cu.
Preferably, the temperature of the magnetic stirring in the step (1) is 60-80 ℃.
Preferably, the reaction time in step (1) is 1-4 h.
Preferably, the temperature of the magnetic stirring in the step (2) is 60-80 ℃.
Preferably, the reaction time in step (2) is 0.5 to 2 hours.
Preferably, the reaction temperature in step (3) is 120-180 ℃.
Preferably, the reaction time in step (3) is 6-24 h.
The invention also protects the magnetic cerium oxide prepared by the preparation method.
The invention has the beneficial effects that:
compared with the prior art, the preparation method adopted by the invention is a double in-situ one-step hydrothermal synthesis method, the process is simple, the process is easy to control, the energy consumption and the production cost are low, the large-scale industrial production can be realized, and the industrial prospect is considerable. The magnetic cerium oxide synthesized by the method takes ferrite as a magnetic substrate, has the characteristics of abundant varieties, large specific surface area, high stability, good magnetism and the like, and is expected to have more applications in the aspects of catalysis, adsorption, biochemistry and the like.
Drawings
FIG. 1 is a SEM photograph of the magnetic ceria of the sample of example 1.
FIG. 2 is a SEM picture of the magnetic ceria of the sample of example 2.
FIG. 3 is a SEM picture of the magnetic ceria of the sample of example 3.
FIG. 4 is an XRD pattern of the magnetic ceria of examples 1-3, with the triangles labeled as characteristic diffraction peaks of cobalt ferrite.
FIG. 5 is a photograph showing the magnetic properties of the samples of examples 1 to 3 under the action of a magnet.
Detailed Description
For a better understanding of the present invention, the present invention will be further described with reference to the following examples and the accompanying drawings, which are illustrative of the present invention and are not to be construed as limiting thereof.
Example 1: (Co)2+And Ce2+The molar ratio is 1/10)
A preparation method of magnetic cerium oxide comprises the following steps:
(1) 0.0005 mol Co(NO3)2·6H2o and 0.001mol Fe (NO)3)3·9H2O preparing a solution A; 0.008mol of NaOH to prepare a solution B, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor C.
(2)0.005mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NO in the D and B solutions3-And uniformly dropwise adding the solution B into the solution D at a molar ratio of 1:2 with NaOH, magnetically stirring at 70 ℃, and reacting for 0.5h to obtain a precursor E.
(3) And transferring the precursor C and the precursor E into a hydrothermal kettle, putting the hydrothermal kettle into an oven, setting the temperature to be 160 ℃, reacting for 12h, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
Example 2: (Co)2+And Ce2+The molar ratio is 1/5)
A preparation method of magnetic cerium oxide comprises the following steps:
(1) 0.0005 mol Co(NO3)2·6H2o and 0.001mol Fe (NO)3)3·9H2O preparing a solution A; 0.008mol of NaOH to prepare a solution B, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor C.
(2)0.0025mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controllingPreparation of NO in D and B solutions3-And uniformly dropwise adding the solution B into the solution D at a molar ratio of 1:2 with NaOH, magnetically stirring at 70 ℃, and reacting for 0.5h to obtain a precursor E.
(3) And transferring the precursor C and the precursor E into a hydrothermal kettle, putting the hydrothermal kettle into an oven, setting the temperature to be 160 ℃, reacting for 12h, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
Example 3: (Co)2+And Ce2+The molar ratio is 1/3)
A preparation method of magnetic cerium oxide comprises the following steps:
(1) 0.0005 mol Co(NO3)2·6H2o and 0.001mol Fe (NO)3)3·9H2O preparing a solution A; 0.008mol of NaOH to prepare a solution B, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor C.
(2)0.0015mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NO in the D and B solutions3-And uniformly dropwise adding the solution B into the solution D at a molar ratio of 1:2 with NaOH, magnetically stirring at 70 ℃, and reacting for 0.5h to obtain a precursor E.
(3) And transferring the precursor C and the precursor E into a hydrothermal kettle, putting the hydrothermal kettle into an oven, setting the temperature to be 160 ℃, reacting for 12h, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
Example 4: (Zn)2+And Ce2+The molar ratio is 1/1)
A preparation method of magnetic cerium oxide comprises the following steps:
(1) 0.0005 mol Zn(NO3)2·6H2o and 0.001mol Fe (NO)3)3·9H2O preparing a solution A; 0.008mol of NaOH to prepare a solution B, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 80 ℃, and reacting for 1h to obtain a precursor C.
(2)0.0005mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NO in the D and B solutions3-Uniformly dripping the solution B into the solution D at 60 ℃ with the molar ratio of NaOH being 1:2And magnetically stirring, and reacting for 1h to obtain a precursor E.
(3) And transferring the precursor C and the precursor E into a hydrothermal kettle, putting the hydrothermal kettle into an oven, setting the temperature to be 180 ℃, reacting for 6h, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
Example 5: (Zn)2+And Ce2+The molar ratio is 1/8)
A preparation method of magnetic cerium oxide comprises the following steps:
(1) 0.0005 mol Zn(NO3)2·6H2o and 0.001mol Fe (NO)3)3·9H2O preparing a solution A; 0.008mol of NaOH to prepare a solution B, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 80 ℃, and reacting for 1h to obtain a precursor C.
(2)0.004mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NO in the D and B solutions3-And uniformly dripping the solution B into the solution D at a molar ratio of 1:3 with NaOH, magnetically stirring at 60 ℃, and reacting for 1h to obtain a precursor E.
(3) And transferring the precursor C and the precursor E into a hydrothermal kettle, putting the hydrothermal kettle into an oven, setting the temperature to be 120 ℃, reacting for 24h, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
Example 6: (Mn)2+And Ce2+The molar ratio is 1/6)
A preparation method of magnetic cerium oxide comprises the following steps:
(1) 0.0005 mol Mn(NO3)2·6H2o and 0.00125mol Fe (NO)3)3·9H2O preparing a solution A; 0.008mol of NaOH to prepare a solution B, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 80 ℃, and reacting for 1h to obtain a precursor C.
(2)0.003mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NO in the D and B solutions3-And uniformly dropwise adding the solution B into the solution D at a molar ratio of 1:1.5, magnetically stirring at 70 ℃, and reacting for 1h to obtain a precursor E.
(3) And transferring the precursor C and the precursor E into a hydrothermal kettle, putting the hydrothermal kettle into an oven, setting the temperature to be 140 ℃, reacting for 10h, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
Example 7: (Mn)2+And Ce2+The molar ratio is 1/6)
A preparation method of magnetic cerium oxide comprises the following steps:
(1) 0.0005 mol Mn(NO3)2·6H2o and 0.0075mol Fe (NO)3)3·9H2O preparing a solution A; 0.008mol of NaOH to prepare a solution B, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 80 ℃, and reacting for 1h to obtain a precursor C.
(2)0.003mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NO in the D and B solutions3-And uniformly dropwise adding the solution B into the solution D with the molar ratio of 1:2.5, magnetically stirring at 80 ℃, and reacting for 0.5h to obtain a precursor E.
(3) And transferring the precursor C and the precursor E into a hydrothermal kettle, putting the hydrothermal kettle into an oven, setting the temperature to be 150 ℃, reacting for 9h, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
Example 8: (Mg)2+And Ce2+The molar ratio is 1/2)
A preparation method of magnetic cerium oxide comprises the following steps:
(1) 0.0005 mol Mg(NO3)2·6H2o and 0.0015mol Fe (NO)3)3·9H2O preparing a solution A; 0.008mol of NaOH to prepare a solution B, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 60 ℃, and reacting for 2 hours to obtain a precursor C.
(2)0.001mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NO in the D and B solutions3-And uniformly dripping the solution B into the solution D at a molar ratio of 1:2 with NaOH, magnetically stirring at 60 ℃, and reacting for 1h to obtain a precursor E.
(3) And transferring the precursor C and the precursor E into a hydrothermal kettle, putting the hydrothermal kettle into an oven, setting the temperature to be 170 ℃, reacting for 8h, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
The magnetic cerium oxides prepared in examples 1 to 3 were identified. FIGS. 1-3 are SEM pictures of the magnetic ceria of the samples of examples 1-3. As can be seen from FIGS. 1-3, the samples of examples 1-3 were all spheroidal particles, loose in texture, slightly agglomerated, and found by comparison to be approximately 100nm and uniform in size.
FIG. 4 is an XRD pattern of the magnetic ceria of examples 1-3, with the triangles labeled as characteristic diffraction peaks of cobalt ferrite. By comparing fig. 4 with the ceria standard XRD standard card, the magnetic ceria sample was compared with ceria, in which characteristic diffraction peaks of (111), (200), (311), (222), (400), (331), and (412) of ceria were appeared and were clearly and sharper, indicating that the magnetic ceria synthesized in examples 1 to 3 all had the ceria structure and good crystallinity. Sample and CoFe2O4In comparison with the XRD standard card of (1), the magnetic cerium dioxide still has CoFe2O4Shows that the sample still has the magnetic matrix CoFe2O4。
FIG. 5 is a photograph showing the magnetic properties of the samples of examples 1 to 3 under the action of a magnet, and it can be seen from the photographs that the samples are attracted by the magnet.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (9)
1. A preparation method of magnetic cerium oxide is characterized by comprising the following preparation steps:
(1) with M (II) (NO)3)2·6H2O、Fe(NO3)3·9H2O preparing solution A, M2+With Fe3+The molar ratio is 1 (1.5-3); preparing solution B from NaOH, and controlling NO in solution A and B3-The mol ratio of NaOH to NaOH is 1 (1.5-3),uniformly dropwise adding the solution B into the solution A, magnetically stirring, and reacting to obtain a precursor C;
(2) taking a certain amount of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution D, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and D3-The molar ratio is (1.5-3): 1, uniformly dropwise adding the solution B into the solution D, magnetically stirring, and reacting to obtain a precursor E;
(3) pressing the precursor C and the precursor E according to M2+And Ce2+Mixing the components according to the molar ratio of (0.1-1), transferring the mixture into a hydrothermal reaction kettle, reacting at a certain temperature, cooling, taking out, washing with water, performing magnetic separation to neutrality, and drying to obtain a magnetic cerium oxide sample.
2. The method according to claim 1, wherein the magnetic cerium oxide is prepared by: in the step (1), M is one of divalent metal elements in Fe, Mg, Zn, Ni, Co, Mn and Cu.
3. The method according to claim 1, wherein the magnetic cerium oxide is prepared by: the temperature of the magnetic stirring in the step (1) is 60-80 ℃.
4. The method according to claim 1, wherein the magnetic cerium oxide is prepared by: the reaction time in the step (1) is 1-4 h.
5. The method according to claim 1, wherein the magnetic cerium oxide is prepared by: the temperature of the magnetic stirring in the step (2) is 60-80 ℃.
6. The method according to claim 1, wherein the magnetic cerium oxide is prepared by: the reaction time in the step (2) is 0.5-2 h.
7. The method according to claim 1, wherein the magnetic cerium oxide is prepared by: the reaction temperature in the step (3) is 120-180 ℃.
8. The method according to claim 1, wherein the magnetic cerium oxide is prepared by: the reaction time in the step (3) is 6-24 h.
9. A magnetic cerium oxide prepared by the preparation method according to any one of claims 1 to 8.
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