Method for preparing floriform metal fluoride nano material

Abstract

The invention discloses a method for preparing a floriform metal fluoride nano material. The method comprises the following steps: 1) calcining a carbon nitride compound so as to obtain g-C3N4; 2) performing ultrasonic dispersion on g-C3N4 into an alcohol solvent so as to obtain a g-C3N4 dispersion; 3) adding a metal salt into the g-C3N4 dispersion, performing uniform mixing, further adding hydrofluoric acid, and performing uniform mixing so as to obtain a mixed solution; and 4) adding the mixed solution into a reaction kettle, performing a solvothermal reaction, further filtering the reactionliquid, and performing washing and drying on a solid obtained through filtration. The method disclosed by the invention can be adopted to prepare the floriform metal fluoride nano material and is cheap in raw material, easy in raw material obtaining, short in synthesis route, short in time, simple in operation and low in production cost, and in addition, the prepared floriform metal fluoride nanomaterial is small in particle size and thus is large in specific surface area, rich in active site and good in electrochemical activity and catalysis activity.

Description

technical field [0001] The invention relates to a preparation method of a flower-shaped metal fluoride nanometer material, which belongs to the technical field of nanomaterials. Background technique [0002] Metal fluorides have many important physical and chemical properties, and have good application prospects in solar cells, lithium secondary batteries, aromatization and dealkylation catalysis, and photocatalysis. [0003] At present, the preparation methods of metal fluoride nanomaterials that have been reported (taking iron fluoride as an example) mainly include the following: CN 103855389A discloses a preparation method of iron trifluoride / carbon composite materials. Ferric fluoride is obtained by fluorination in a hydrogen fluoride atmosphere, and then ball milled with carbon nanotubes or graphene to obtain composite materials, but carbon nanotubes and graphene are expensive and difficult to obtain, and the ball milling process consumes a lot of energy, making it diff...

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Problems solved by technology

[0003] At present, the preparation methods of metal fluoride nanomaterials that have been reported (taking iron fluoride as an example) mainly include the following: CN 103855389A discloses a preparation method of iron trifluoride / carbon composite materials. Ferric fluoride is obtained by fluorination in a hydrogen fluoride atmosphere, and then ball milled with carbon nanotubes or graphene to obtain composite materials, but carbon nanotubes and graphene are expensive and difficult to obtain, and the ball milling process consumes a lot of energy, making it difficult for industrial production ; CN 105336946A discloses a preparation method of ferric fluoride positive electrode material for lithium ion batteries. Anhydrous ferric fluoride is obtained through an acid-thermal reaction between a highly active fluorine source and an iron salt for more than 48 hours, but the preparation process takes a long time and the fluorine The source must be high-concentration hydrofluoric acid or anhydrous hydrogen fluoride gas, the conditions are harsh, and it is also difficult to industrialize production; CN 105680043A discloses a preparation method of nano-ferric fluoride, which comprises ferric salt alcohol solution and NH 4 HF 2 Aqueous solutions were mixed to obtain (NH 4 ) 3 FeF 6 White precipitate, and then high-temperature calcination to obtain ferric fluoride, but the fluorinating reagent NH 4 HF 2 The price is high, it is difficult to produce on a large scale, and due to the use of NH 4 HF 2 Aqueous solution, it is easy to cause ferric fluoride to decompose into iron oxide impurities due to residual water during high-temperature calcination in the later stage; Bai et al [BaiY, et al. Nano Energy, 2017, 32, 10-18.] Prepared by liquid phase precipitation Nanoflower-like ferric fluoride materials are produced. The tiny nanosheets provide a large specific surface area, which is conducive to the infiltration of the electrolyte and can improve the rate performance of the material. However, the preparation process needs to be left for more than 12 hours, which takes a long time. Difficult to industrial production; Li et al. [Li Y, et al.ACS Applied Materials & Interfaces, 2017, 9, 19852-19860.] prepared ferric fluoride materials decorated with nanosheet flower-shaped metal silver by hydrothermal method and ladder calcination method, but The preparation process is relatively complicated and the cost is high; Zhang et al [QiZhang, et al, Chemical Engineering Journal, 2019, 371, 245-251.] prepared ferric fluoride nanosheets by growing ferric fluoride on titanium foil by hydrothermal method , but the surface treatment of titanium foil is required, the process is cumbersome, and the loading of ferric fluoride on the titanium foil cannot be controlled, so it is difficult to industrialize production

[0004] Therefore, in general, the existing methods for preparing metal fluoride nanomaterials mainly have the following problems: 1) the substrate used in the material is expensive, not easy to obtain, and the production cost is high; 2) the preparation method is complicated, the synthesis path is long, and the production cycle is long; 3 ) prepared metal fluoride nanomaterials have large particle size, small specific surface area, poor electrochemical and catalytic activity, and it is difficult to fully meet the actual needs.

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