A kind of preparation method of single crystal trimanganese tetraoxide

A technology of manganese tetroxide and manganese tetroxide seed crystal, applied in chemical instruments and methods, single crystal growth, single crystal growth and other directions, can solve the problem of easy agglomeration of particles, and achieve the effect of complete crystal shape and regular morphology

Active Publication Date: 2016-08-03
BYD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention solves the problem of preparing Mn in the prior art 3 o 4 It is difficult to form single crystal Mn with regular octahedral structure in the process 3 o 4 And the technical problem that the particles are easy to agglomerate

Method used

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  • A kind of preparation method of single crystal trimanganese tetraoxide
  • A kind of preparation method of single crystal trimanganese tetraoxide
  • A kind of preparation method of single crystal trimanganese tetraoxide

Examples

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preparation example Construction

[0017] The invention provides a single crystal Mn 3 o 4 The preparation method comprises the following steps:

[0018] S1. Add the water-soluble manganese compound to the basic compound to react to obtain manganese hydroxide; the OH in the basic compound - and Mn in water-soluble manganese compounds 2+ The molar ratio is 2-7;

[0019] S2, the manganese hydroxide obtained in step S1 is oxidized to Mn 3 o 4 ;

[0020] S3, the Mn that step S2 obtains under the inert atmosphere 3 o 4 Ripe to get Mn 3 o 4 seed crystal;

[0021] S4, Mn obtained in S3 3 o 4 In the presence of seed crystals, oxidation proceeds simultaneously with the reaction of water-soluble manganese compounds with basic compounds, Mn 3 o 4 The seed crystal grows up to obtain the single crystal Mn 3 o 4 .

[0022] Single crystal Mn provided by the invention 3 o 4 In the preparation method, in OH - Manganese hydroxide obtained under excess conditions (that is, adding water-soluble manganese compou...

Embodiment 1

[0038] (1) Synthesis of manganese hydroxide

[0039] In a three-necked flask, add 14g of NaOH solution and 70ml of water, stir to dissolve, and vent the air with nitrogen for 15min; put 8.45g of MnSO 4 ·H 2 O was dissolved in 30ml of water, configured as a manganese sulfate solution, and added dropwise to the above NaOH solution under stirring conditions, and the dripping was completed in 30 minutes (OH - with Mn 2+ The molar ratio is 7); the solution was heated to 90°C and kept for 1h.

[0040] (2) Mn 3 o 4 Synthesis

[0041] Under stirring conditions, air was introduced into the product system of step (1), and oxidized at 90°C for 8 hours to obtain Mn 3 o 4 The product system is denoted as sample A.

[0042] (3) Mn 3 o 4 maturation (i.e. synthesis of seed crystals)

[0043] Mn to step (2) 3 o 4 Nitrogen was introduced into the product system, and kept at 90°C for 8 hours to obtain Mn 3 o 4 Seed system.

[0044] (4) Growth of seed crystal

[0045] Keep the Mn...

Embodiment 2

[0047] Using the same steps as in Example 1 to prepare the single crystal Mn of this example 3 o 4 Sample S20, the difference is: after completing step (4), continue to repeat step (4) to obtain the single crystal Mn 3 o 4 Sample, denoted as S20.

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Abstract

The invention provides a method for preparing monocrystal manganese tetroxide (Mn3O4). The method comprises the following steps of: (1) adding a water-soluble manganese compound into an alkaline compound, and reacting so as to obtain manganese hydroxide, wherein the mole ratio of OH- in the alkaline compound to Mn<2+> in the water-soluble manganese compound is 2-7; (2) oxidizing the manganese hydroxide obtained in the step (1) into Mn3O4; (3) aging Mn3O4 obtained in the step (2) in an inert atmosphere so as to obtain Mn3O4 seed crystals; and (4) oxidizing while the water-soluble manganese compound reacts with the alkaline compound in the presence of the Mn3O4 seed crystals obtained in the step (3), and growing the Mn3O4 seed crystals, thereby obtaining the monocrystal Mn3O4. The method provided by the invention has the advantages that the monocrystal Mn3O4 with complete crystal forms and regular morphologies can be prepared, and the grain size of the monocrystal Mn3O4 can be appropriately selected according to actual needs.

Description

technical field [0001] The invention belongs to the technical field of manganese compound synthesis, and in particular relates to a preparation method of single crystal trimanganese tetraoxide. Background technique [0002] mn 3 o 4 with LiMn 2 o 4 The same spinel structure, hence the use of Mn 3 o 4 Preparation of LiMn by Sintering as Precursor 2 o 4 It can reduce the time of crystal transformation and greatly shorten the time of solid phase sintering. According to the bulk density of the powder increases with the increase of its particle diameter, it is very necessary to have a large particle size of LiMn 2 o 4 . Although the precursor mixed raw materials can make the crystal grains grow during the high-temperature calcination process, the desired large particles are often not obtained. Therefore, by first preparing the precursor Mn with large particle size 3 o 4 particles, then large particles of LiMn were produced in a short sintering time 2 o 4 . [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/16C30B7/14
Inventor 陈小芳苗伟峰
Owner BYD CO LTD
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