Ridge-free fused mass structure manganese trifluoride material and preparation method thereof

Abstract

The invention discloses a preparation method of a manganese trifluoride material with a non-edge fused solid structure. Manganese trifluoride is produced by adopting a high-energy ball milling-freezing heating type pre-fluorination-high-temperature cooling type fluorination process, and the method comprises the following steps: gradually heating and pre-fluorinating raw materials including manganese oxide and manganese-containing fluoride which are dried in vacuum in a frozen anhydrous hydrogen fluoride solution, gradually cooling and fluorinating at high temperature, cooling and sieving, and drying to obtain the manganese trifluoride. The manganese trifluoride material with the edge-free fused body structure is obtained. The particle size of the prepared manganese trifluoride is 0.1-10 [mu] m, and the prepared manganese trifluoride is of an edge-free fused solid structure. The method is simple in preparation flow, controllable in process, good in stability, capable of achieving batch production and suitable for macro preparation.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and in particular relates to a manganese trifluoride material with an edgeless fused body structure and a preparation method. Background technique [0002] Manganese trifluoride is a monoclinic material with high melting point and excellent thermal stability, and is a widely used fluorination reagent. With the development of aerospace technology, especially the demand for cathode materials for high-voltage thermal batteries, manganese trifluoride is becoming the primary raw material for many electrode materials, and high-purity manganese trifluoride has great application prospects. [0003] At present, the preparation methods of manganese trifluoride are mainly liquid phase method and high temperature fluorination method. Among them, the liquid phase method is complex and requires high production equipment. Since manganese trifluoride is very easy to absorb water, water is often int...

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Problems solved by technology

Mazej (Z.Mazej.Room temperature syntheses of MnF 3 ,MnF 4 andhexafluoromanganate(IV) salts of alkaline cations[J].Journal of FluorineChemistry,2002,114(1),75-80.) Treat manganese difluoride with low-temperature anhydrous hydrogen fluoride (temperature -196°C) and carry out long-term Manganese trifluoride is obtained by fluorination. Although the introduction of water is avoided, the working temperature is low, the equipment requirements are high, and the working time is long, at least 9 days of reaction time, which limits the large-scale production of manganese trifluoride raw materials. synthesis

Ehlert et al. (T.C.Ehlert, M.Hsia.Mass spectrometric and thermochemical studies of themanganese fluorides[J].Journal of Fluorine Chemistry,1972,2(1), 33-51.) fluorinated at high temperature and short time with fluorine gas to obtain Manganese trifluoride has been produced, but due to the short fluorination time, it is difficult to completely transform it. In addition, the valence of manganese is high, the manganese-containing fluoride is thermodynamically unstable, and there are many kinds of manganese-containing fluoride coexistence phenomenon, which is not conducive to the formation of stable single-phase fluoride.

[0004] In the preparation method of manganese trifluoride, in addition to the synthesis process of the above-mentioned raw materials, there is no report on the preparation of manganese trifluoride with a fused body structure by freezing and heating type pre-fluorination-high temperature cooling type fluoridation treatment, nor See the introduction of other manganese trifluoride functional materials with special morphology

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