CN113209963A - Method for preparing ultrathin sodium-based transition metal oxide nanosheet catalyst in large scale - Google Patents

Method for preparing ultrathin sodium-based transition metal oxide nanosheet catalyst in large scale Download PDF

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CN113209963A
CN113209963A CN202110560004.5A CN202110560004A CN113209963A CN 113209963 A CN113209963 A CN 113209963A CN 202110560004 A CN202110560004 A CN 202110560004A CN 113209963 A CN113209963 A CN 113209963A
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heating
transition metal
ultrathin
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metal oxide
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黄凯
雷鸣
毕科
赵泽璧
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Beijing University of Posts and Telecommunications
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Abstract

The invention relates to a method for preparing an ultrathin sodium-based transition metal oxide nanosheet catalyst in a large scale, and belongs to the field of material science, engineering technology and chemistry. The transition metal elements contained in the ultrathin sodium-based transition metal oxide nanosheets prepared by the method are any one or more of manganese (Mn), iron (Fe), cobalt (Co) and nickel (Ni), and the phases of the ultrathin sodium-based transition metal oxide nanosheets are any one or more of P2 type layers, P3 type layers, O2 type layers and O3 type layers. Firstly, preparing a certain amount of saturated sodium carbonate solution A according to the molar ratio of various elements in a finished product, slowly dropwise adding the solution A into the uniformly mixed transition metal oxide, ultrasonically heating until the solution is completely evaporated to obtain powder B, and preparing the multi-component multi-phase sodium-based transition metal oxide catalyst through a series of simple heat treatment steps. The method has the advantages of simple operation, controllable yield, high expansibility and the like, and has the advantages of easy operation, high yield, safety, reliability and the like compared with the traditional method for preparing the sodium-containing ultrathin nanosheet.

Description

Method for preparing ultrathin sodium-based transition metal oxide nanosheet catalyst in large scale
Technical Field
The invention relates to a method for preparing an ultrathin sodium-based transition metal oxide nanosheet catalyst in a large scale, and belongs to the field of material science, engineering technology and chemistry.
Background
After graphene is prepared by a mechanical stripping method for the first time, the research heat of various countries around the world on nanoscale two-dimensional materials is increasing or decreasing. Until now, scientists have reported various methods for preparing two-dimensional nanomaterials. With MoS prepared by using out-of-plane van der Waals interactions2These materials, MXene two-dimensional materials with atoms selectively etched, and two-dimensional metal oxide nanomaterials made by self-assembly or other wet chemical methods. Although two-dimensional materials are prepared by a variety of methods, the selection of the lattice structure of the raw materials in the preparation is often the most critical. Therefore, it is both an opportunity and a challenge for ultrathin sodium-based transition group metal oxide nanosheets.
The preparation of the ultrathin sodium-based transition metal oxide is expected to be realized not only because the ultrathin sodium-based transition metal oxide is simple to process and easy to popularize, but also more importantly, the ultrathin sodium-based transition metal oxide is an optimal material for an electric contact and plays an irreplaceable role in the fields of semiconductors, sensors, electrocatalysis, electronic devices and the like. And many of the best lithium ion battery solutions are being gradually replaced by sodium ion batteries. On the basis of keeping the performance, the reduction of production cost, green recovery and reuse are always the continuous pursuit targets in the field of new energy, and therefore, the original structures of catalysts of scientists in various countries around the world are adjusted. Therefore, the key issue is how to reduce the amount of noble metal used, and how to make the material possess both strong stability and reversible properties.
According to statistics, the conventional process is mainly based on the conventional process of simply grinding and sintering various materials. The electrochemical performance is greatly reduced after the material is affected by water or (and) carbon dioxide. Therefore, finding a process that is simple to operate, green to recover, and can mass produce ultra-thin sodium-based transition metal oxides remains an interesting challenge.
In the lift-off process, the material has in-plane chemical bonds and out-of-plane van der waals interactions, or the ability to self-assemble into an interlayer structure. Under extreme conditions, Van der Waals interaction is extremely easy to eliminate, and the nanoscale two-dimensional material is formed. Inspired by the exfoliation method, we rapidly thermally anneal ultra-thin sodium-based transition metal oxides that are affected by water or (and) carbon dioxide. The rapid change of the environment causes a great amount of water molecules/carbon dioxide molecules between layers to evaporate, and finally the residual amount is produced into thinner and smaller-sized sodium-based transition metal oxide nanosheets. By using the method, the ultrathin nanometer-scale materials are successfully obtained, and importantly, the ultrathin sodium-based transition metal oxide which can be effectively and massively recovered by the rapid process can be continuously used in the electrochemical field in a novel form. That is, the invention firstly proposes and realizes rapid temperature rise and mass production of the ultrathin sodium-based transition metal oxide nanosheet catalyst.
Disclosure of Invention
1. Objects of the invention
The invention aims to provide a method for preparing an ultrathin sodium-based transition metal oxide nanosheet catalyst in a large scale, which is used for simply, safely and massively preparing ultrathin sodium-based transition metal oxide nanosheets by quickly changing the environmental temperature so as to be suitable for various field requirements and applications, thereby obviously reducing the cost of the commercial application of the ultrathin sodium-based transition metal oxide nanosheets.
2. The invention of the technology
The key points of the invention are as follows:
(1) preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of various elements in the finished product, slowly dropwise adding the solution into the uniformly mixed transition metal oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. The transition metal oxide is manganese oxide (Mn)3O4) Iron oxide (Fe)3O4) Cobalt oxide (Co)3O4) Any one or more of nickel oxide (NiO);
(2) and (2) pressing the powder A prepared in the step (1) into a sheet or a pellet by using the pressure of 16 Mpa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, the optional heat preservation temperature range is 650-1200 ℃, for example 650 ℃, 900 ℃, 1000 ℃ and 1200 ℃, and the corresponding finished product phases are P3, P2, O3 and O2 respectively.
(3) And (3) putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 deg.C, and the heating temperature range is 20min-60min, such as 20min, 40min, and 60 min.
Drawings
FIG. 1 is an ultra-thin Na film prepared by the method of the present invention0.85Ni0.34Mn0.66O2Scanning electron microscopy of two-dimensional nanomaterials.
Detailed Description
The following describes embodiments of the method of the invention:
example 1
P2 type-ultrathin Na0.85MnO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Mn in the finished product of 0.85 to 1, slowly dropwise adding the solution to the manganous-manganic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 2
P3 type-ultrathin Na0.85MnO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Mn in the finished product of 0.85 to 1, slowly dropwise adding the solution to the manganous-manganic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 3
O3 type-ultrathin Na0.85MnO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Mn in the finished product of 0.85 to 1, slowly dropwise adding the solution to the manganous-manganic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 4
O2 type-ultrathin Na0.85MnO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Mn in the finished product of 0.85 to 1, slowly dropwise adding the solution to the manganous-manganic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 5
P2 type-ultrathin Na0.85Ni0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and nickel oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 6
P3 type-ultrathin Na0.85Ni0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and nickel oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 7
O3 type-ultrathin Na0.85Ni0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and nickel oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 8
O2 type-ultrathin Na0.85Ni0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and nickel oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 9
P2 type-ultrathin Na0.85Co0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Co to Mn of 0.85 to 0.34 to 0.66 in the finished product, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 10
P3 type-ultrathin Na0.85Co0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 11
O2 type-ultrathin Na0.85Co0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Co to Mn of 0.85 to 0.34 to 0.66 in the finished product, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 12
O3 type-ultrathin Na0.85Co0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Co to Mn of 0.85 to 0.34 to 0.66 in the finished product, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 13
P2 type-ultrathin Na0.85Fe0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Fe and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and triiron tetroxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 14
P3 type-ultrathin Na0.85Fe0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Fe and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and triiron tetroxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 15
O2 type-ultrathin Na0.85Fe0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Fe and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and triiron tetroxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 16
O3 type-ultrathin Na0.85Fe0.34Mn0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Fe and Mn in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of trimanganese tetroxide and triiron tetroxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 17
P2 type-ultrathin Na0.85FeO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Fe in the finished product of 0.85 to 1, slowly dropwise adding the solution to ferroferric oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 40 min.
Example 18
P3 type-ultrathin Na0.85FeO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Fe in the finished product of 0.85 to 1, slowly dropwise adding the solution to ferroferric oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 40 min.
Example 19
O3 type-ultrathin Na0.85FeO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Fe in the finished product of 0.85 to 1, slowly dropwise adding the solution to ferroferric oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 40 min.
Example 20
O2 type-ultrathin Na0.85FeO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Fe in the finished product of 0.85 to 1, slowly dropwise adding the solution to ferroferric oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 40 min.
Example 21
P2 type-ultrathin Na0.85CoO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Co in the finished product of 0.85 to 1, slowly dropwise adding the solution to cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 deg.C and 60 min.
Example 22
P3 type-ultrathin Na0.85CoO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Co in the finished product of 0.85 to 1, slowly dropwise adding the solution to cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 deg.C and 60 min.
Example 23
O3 type-ultrathin Na0.85CoO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Co in the finished product of 0.85 to 1, slowly dropwise adding the solution to cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 deg.C and 60 min.
Example 24
O2 type-ultrathin Na0.85CoO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Co in the finished product of 0.85 to 1, slowly dropwise adding the solution to cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 deg.C and 60 min.
Example 25
P2 type-ultrathin Na0.85NiO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Ni to 0.85 to 1 in the finished product, slowly dropwise adding the solution to nickel oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 40 min.
Example 26
P3 type-ultrathin Na0.85NiO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Ni to 0.85 to 1 in the finished product, slowly dropwise adding the solution to nickel oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 40 min.
Example 27
O3 type-ultrathin Na0.85NiO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Ni to 0.85 to 1 in the finished product, slowly dropwise adding the solution to nickel oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 40 min.
Example 28
O2 type-ultrathin Na0.85NiO2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na to Ni to 0.85 to 1 in the finished product, slowly dropwise adding the solution to nickel oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 40 min.
Example 29
P2 type-ultrathin Na0.85Ni0.34Co0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Co in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of nickel oxide and cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 30
P3 type-ultrathin Na0.85Ni0.34Co0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Co in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of nickel oxide and cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 31
O3 type-ultrathin Na0.85Ni0.34Co0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Co in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of nickel oxide and cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 32
O2 type-ultrathin Na0.85Ni0.34Co0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Ni and Co in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of nickel oxide and cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 33
P2 type-ultrathin Na0.85Fe0.34Co0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Fe and Co in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of the ferroferric oxide and the cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 900 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 34
P3 type-ultrathin Na0.85Fe0.34Co0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Fe and Co in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of the ferroferric oxide and the cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 650 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 35
O3 type-ultrathin Na0.85Fe0.34Co0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Fe and Co in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of the ferroferric oxide and the cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1000 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.
Example 36
O2 type-ultrathin Na0.85Fe0.34Co0.66O2And (3) preparing a two-dimensional nano material.
Preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of Na, Fe and Co in the finished product of 0.85, 0.34 and 0.66, slowly dropwise adding the solution into the mixture of the ferroferric oxide and the cobaltosic oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. Powder A was pressed into flakes or pellets using a pressure of 16 MPa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, and the heat preservation temperature is 1200 ℃. And then, putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 ℃ and 20 min.

Claims (1)

1. A method for preparing ultrathin sodium-based transition metal oxide nanosheet catalysts in a large scale is characterized by comprising the following steps:
(1) preparing a certain amount of saturated sodium carbonate solution according to the molar ratio of various elements in the finished product, slowly dropwise adding the solution into the uniformly mixed transition metal oxide, and ultrasonically heating until the solution is completely evaporated to obtain powder A. The transition metal oxide is manganese oxide (Mn)3O4) Iron oxide (Fe)3O4) Cobalt oxide (Co)3O4) Any one or more of nickel oxide (NiO);
(2) and (2) pressing the powder A prepared in the step (1) into a sheet or a pellet by using the pressure of 16 Mpa. Then placed in a muffle furnace to be heated for 24 hours, and finally cooled to room temperature to obtain an intermediate B. The reaction atmosphere is air, the temperature rise rate of the muffle furnace is 5 ℃/min, the optional heat preservation temperature range is 650-1200 ℃, for example 650 ℃, 900 ℃, 1000 ℃ and 1200 ℃, and the corresponding finished product phases are P3, P2, O3 and O2 respectively.
(3) And (3) putting the intermediate B into 50ml of ultrapure water, heating and stirring to 100 ℃, quickly putting the intermediate B into a preheated muffle furnace when water is evaporated until the intermediate is in a mud shape, heating for a certain time, and taking out a reaction sample to obtain the ultrathin sodium-based transition metal oxide nanosheet catalyst. The reaction atmosphere is air. The heating temperature is 500 deg.C, and the heating temperature range is 20min-60min, such as 20min, 40min, and 60 min.
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