CN109761279B - Rapid precipitation preparation of two-dimensional BaMoO4Method (2) - Google Patents

Rapid precipitation preparation of two-dimensional BaMoO4Method (2) Download PDF

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CN109761279B
CN109761279B CN201811533819.9A CN201811533819A CN109761279B CN 109761279 B CN109761279 B CN 109761279B CN 201811533819 A CN201811533819 A CN 201811533819A CN 109761279 B CN109761279 B CN 109761279B
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dimensional
bamoo
mixed solution
rapid precipitation
nano material
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CN109761279A (en
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侴术雷
赖伟鸿
王云晓
李用成
李东祥
李亚书
宫毅涛
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Liaoning Xingkong Sodium Battery Co ltd
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Liaoning Xingkong Sodium Battery Co ltd
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Abstract

The invention relates to the technical field of nano material preparation, and discloses a method for preparing two-dimensional BaMoO by rapid precipitation4The method comprises the following steps: 1) respectively dissolving 0.18M Ba (NO3)2 and 0.14M (NH4)6Mo7O24 & 4H2O in 15mL water at room temperature to obtain mixed solutions,for standby; 2) uniformly stirring the mixed solution by using a stirrer at a rated rotation speed of 300rpm until the mixed solution is mixed to separate out a large amount of visible white precipitates for standby; 3) washing the white precipitate obtained in the step 2 by using water and ethanol, and then drying the white precipitate in an oven at the temperature of 60 ℃ to obtain the high-purity two-dimensional nano material BaMoO4. The rapid precipitation method for preparing two-dimensional BaMoO4Compared with the traditional sol-gel method and the reverse micelle method, the method has the advantages of low cost, high reaction rate, simple operation, mildness, easiness in control, energy conservation, environmental friendliness, high product purity and novel appearance.

Description

Rapid precipitation preparation of two-dimensional BaMoO4Method (2)
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a method for preparing two-dimensional BaMoO by rapid precipitation4The method of (1).
Background
BaMoO4Belongs to metal molybdate, and has wide potential application in the fields of optics, energy storage and the like due to the special crystal structure of the metal molybdate. The preparation of the electrode material and the synthesis of the ion conductor material in large scale can be rapidly carried out, and the method has wide application. Particularly, the special two-dimensional structure is a sheet structure material with atomic thickness, and the unique electronic, optical and mechanical properties of the sheet structure material are considered to be important nanometer material branches.
Through the summary of reference, the two-dimensional BaMoO is prepared4The method of the nano material mainly utilizes a hydrothermal method (Z.Luo, H.Li, H.Shu, K.Wang, J.Xia, Y.Yan, Crystal Growth and Design 2008, 8, 2275-. However, the above method is long in time consumption, high in cost, and needs to be carried out at high temperature and high pressure, and the reaction needs to be carried out by adding a large amount of auxiliary surfactant, so that the large-scale production is difficult。
Therefore, the invention can simply and quickly prepare the two-dimensional BaMoO4The method of the nanometer material is particularly important for future industrialization and mass application production. The precipitation method has various excellent characteristics of high efficiency, rapidness, simplicity and the like in preparing materials. At the same time, however, the rapid crystallization of the precipitation reaction allows the preparation, regulation and control of nanomaterials along specific dimensions: such as two-dimensional nanomaterials, are very challenging.
Therefore, in order to overcome the defects of the prior art, the two-dimensional nano material BaMoO is prepared4The invention provides a BaMoO with excellent performance4The shape and phase control method of the nano-sheet utilizes ammonium tert-molybdate ((NH)4)6Mo7O24·4H2O) is a precipitant to rapidly precipitate out the target material.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for preparing two-dimensional BaMoO by rapid precipitation4The method has the advantages of low cost, high reaction rate, mild and easily-controlled reaction, energy conservation, environmental protection, high product purity, novel appearance and the like, and solves the problem of the existing preparation of two-dimensional BaMoO4The method of the nano material mainly utilizes a hydrothermal method or a microwave heating method; however, the method has the problems of long time consumption, high cost, high temperature and high pressure, addition of a large amount of auxiliary surfactant for reaction and difficulty in large-scale production.
(II) technical scheme
In order to realize the purposes of low cost, high reaction rate, mild and easily-controlled reaction, energy conservation, environmental protection, high product purity, novel appearance and the like, the invention provides the following technical scheme: rapid precipitation preparation of two-dimensional BaMoO4The method comprises the following steps:
1) under the condition of room temperature, 0.18MBa (NO)3)2And 0.14M (NH)4)6Mo7O24·4H2Dissolving O in 15mL of water respectively to prepare a mixed solution for later use;
2) uniformly stirring the mixed solution by using a stirrer at a rated rotation speed of 300rpm until the mixed solution is mixed to separate out a large amount of visible white precipitates for standby;
3) washing the white precipitate obtained in the step 2 by using water and ethanol, and then drying the white precipitate in an oven at the temperature of 60 ℃ to obtain the high-purity two-dimensional nano material BaMoO4
(III) advantageous effects
Compared with the prior art, the invention provides a method for preparing two-dimensional BaMoO by rapid precipitation4The method has the following beneficial effects:
1. the rapid precipitation method for preparing two-dimensional BaMoO4The process of (1), using ammonium tert-molybdate ((NH)4)6Mo7O24·4H2O) is a precipitant to rapidly precipitate the target material; (NH)4)6Mo7O24·4H2O has low dissociation coefficient and can slowly release MoO4 -The ions balance the growth speed and the diffusion speed of the material, so that the material can directionally grow according to two-dimensional directions in the growth process.
2. The rapid precipitation method for preparing two-dimensional BaMoO4Compared with the traditional sol-gel method and the reverse micelle method, the method has the advantages of low cost, high reaction rate, simple operation, mildness, easiness in control, energy conservation, environmental protection, high product purity and novel appearance; and the prepared product is of a two-dimensional nanosheet structure, and the nanosheet is large in length-diameter ratio, stable in quality, high in purity, low in manufacturing cost and remarkably increased in specific surface area.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of BaMoO4 nanosheets in the examples;
fig. 2 is a scanning electron microscope (TEM) test image of BaMoO4 nanosheets in the examples.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example (b): rapid precipitation preparation of two-dimensional BaMoO4The method comprises the following steps:
1) under the condition of room temperature, 0.18MBa (NO)3)2And 0.14M (NH)4)6Mo7O24·4H2Dissolving O in 15mL of water respectively to prepare a mixed solution for later use;
2) uniformly stirring the mixed solution by using a stirrer at a rated rotation speed of 300rpm until the mixed solution is mixed to separate out a large amount of visible white precipitates for standby;
3) washing the white precipitate obtained in the step 2 by using water and ethanol, and then drying the white precipitate in an oven at the temperature of 60 ℃ to obtain the high-purity two-dimensional nano material BaMoO4(see FIGS. 1-2).
The method has various excellent characteristics of high efficiency, rapidness, simplicity and the like in preparing the material, overcomes the great challenge of regulating and controlling the two-dimensional nano material caused by rapid crystallization of precipitation reaction, and prepares the two-dimensional nano material BaMoO4Using ammonium tert-molybdate ((NH)4)6Mo7O24·4H2O) is a precipitant to rapidly precipitate the target material; (NH)4)6Mo7O24·4H2O has low dissociation coefficient and can slowly release MoO4 -The ions balance the growth speed and the diffusion speed of the material, so that the material can directionally grow according to two-dimensional directions in the growth process.
The method has the advantages of low cost, high reaction rate, mild and easily-controlled reaction, energy conservation, environmental protection, high product purity, novel appearance and the like, and solves the problem of the existing preparation of two-dimensional BaMoO4The method of the nano material mainly utilizes a hydrothermal method or a microwave heating method, but the method has the problems of long time consumption, high cost, high temperature and high pressure, addition of a large amount of auxiliary surfactant for reaction and difficulty in large-scale production。
Having described embodiments of the present invention, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in the embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (1)

1. Rapid precipitation preparation of two-dimensional BaMoO4The method is characterized by comprising the following steps:
1) 0.18M Ba (NO) at room temperature3)2And 0.14M (NH)4)6Mo7O24·4H2Dissolving O in 15mL of water respectively to prepare a mixed solution for later use;
2) uniformly stirring the mixed solution by using a stirrer at a rated rotation speed of 300rpm until the mixed solution is mixed to separate out a large amount of visible white precipitates for standby;
3) washing the white precipitate obtained in the step 2 by using water and ethanol, and then drying the white precipitate in an oven at the temperature of 60 ℃ to obtain the high-purity two-dimensional nano material BaMoO4
CN201811533819.9A 2018-12-14 2018-12-14 Rapid precipitation preparation of two-dimensional BaMoO4Method (2) Active CN109761279B (en)

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CN110540242A (en) * 2019-09-06 2019-12-06 辽宁星空新能源发展有限公司 method for preparing two-dimensional basic manganese oxide nanosheet through rapid precipitation
CN111792673B (en) * 2020-07-07 2021-05-14 中国科学院广州地球化学研究所 Hexagonal structure BaMoO4And method for preparing the same

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