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Preparation method for high-activity trimanganese tetraoxide

A manganese tetroxide, high activity technology, applied in manganese oxide/manganese hydroxide and other directions, can solve problems such as fast reaction speed, low specific surface area, environmental pollution, etc., to speed up reaction speed, ensure reaction safety, and reduce production. cost effect

Active Publication Date: 2019-11-08
HUNAN SPECIAL METAL MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activity of manganese tetraoxide obtained by this process is low, and its specific surface area is 6-15m 2 Between / g, and the amount of catalyst added is large, usually 1:0.001, and the reaction time is long. The reaction time of 2 tons of raw materials is about 15 to 20 hours, resulting in high production costs, and due to the large amount of catalyst used, subsequent washing is more difficult. , more lotion, more serious environmental pollution
[0004] The patent application with application number 201310214003.0 uses the electrolytic manganese metal suspension method, but the manganese manganese tetraoxide produced has low activity and high production cost; the patent application with application number 201610671638.7 uses the electrolytic manganese metal suspension method with alcohol-water mixed solution The safety factor is low, the impact on the environment is large, and the reaction time is long; although the patent application No. 201110369430.7 has prepared trimanganese tetroxide with relatively high activity, the specific surface area is still not high, and the use of ammonia water as a catalyst consumes a large amount. The environment has a great impact, ultrasonic oscillation is used at the beginning of the reaction, the ultrasonic intensity is not controlled, the reaction speed is very fast, the reaction is prone to out of control, a large amount of hydrogen gas is produced, and safety accidents occur, so it needs to be further improved

Method used

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  • Preparation method for high-activity trimanganese tetraoxide
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preparation example Construction

[0034] A preparation method of the highly active trimanganese tetraoxide of the present invention, comprising the steps of:

[0035] (1) Electrolytic metal manganese flakes are broken into electrolytic metal manganese powder with a vertical screw mill under nitrogen protection;

[0036] (2) sieving the electrolytic manganese metal powder to classify;

[0037] (3) After fully mixing the electrolytic manganese metal powder under the sieve and the catalyst ammonium chloride in an ammonia atmosphere, add a small amount of deionized water, stir and wet it into a non-agglomerated, flowable slurry, and then add the slurry to Suspension is formed in deionized warm water, oxygen or pure air is continuously introduced into the suspension through the air supply pipe, and stirred, so that the electrolytic metal manganese powder is oxidized into trimanganese tetraoxide under the action of the catalyst;

[0038] (4) After waiting to react for 5 to 30 minutes, turn on the ultrasonic generat...

Embodiment 1

[0055] A kind of preparation method of highly active trimanganese tetraoxide of the present invention, the schematic diagram of reaction tank structure is as figure 1 shown, including the following steps:

[0056] (1) Use a vertical screw mill to crush the electrolytic manganese metal flakes into electrolytic manganese metal powder under nitrogen protection.

[0057] (2) Sieve and classify the electrolytic manganese metal powder to be below 150 mesh.

[0058] (3) After fully mixing the electrolytic manganese metal powder under the sieve and the ammonium chloride catalyst in an ammonia atmosphere, wet it with deionized water to form a slurry, and press the mixture of electrolytic metal manganese powder, catalyst and deionized warm water at 1:30 The mass ratio of the electrolytic metal manganese powder and the catalyst is added to deionized warm water to form a suspension in the reaction tank 2, and oxygen is continuously fed into the suspension through the air supply pipe 3 to...

Embodiment 2

[0067] The difference between this embodiment and the method of Embodiment 1 is that in step (4), the mass ratio of the suspension to the activator is 1:0.0002, and after adding the activator, the required reaction time is 3 hours.

[0068] The index of the obtained product is: Mn: 70.8%-71.2%, the impurity content is low, and the impurity containing Na is 0.002% based on the mass fraction of sodium oxide, and the specific surface area: 75-82m 2 / g.

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Abstract

The invention discloses a preparation method for high-activity trimanganese tetraoxide. The preparation method comprises the following steps: S1, mixing electrolytic manganese metal powder with a catalyst, carrying out wetting to form slurry, adding the slurry into warm deionized water to form a suspension, continuously introducing oxygen or pure air, and carrying out a stirring reaction; S2, starting an ultrasonic generator for treatment, adding a activator, and carrying out a reaction for 1.8-5 h to obtain the suspension slurry of high-activity trimanganese tetraoxide, wherein ultrasonic intensity is adjusted within the range of 20 kHz-40 kHz during the reaction; and S3, performing concentration, washing, dehydrating and drying to obtain the high-activity trimanganese tetraoxide. The method of the invention has the advantages of short production cycle, low cost, small environmental pollution and good safety, and can prepare high-activity trimanganese tetraoxide.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a preparation method of highly active trimanganese tetraoxide. Background technique [0002] Trimanganese tetraoxide (Mn 3 o 4 ) is a brown-red powder, which is relatively stable at normal temperature and pressure. It is an important raw material for the production of soft magnetic manganese-zinc ferrite. It can also be used to produce magnetic cores, transformers, inductors, etc. depending on the purity. With the continuous development of electronic products, there are more and more applications of highly active trimanganese tetraoxide in high-performance magnetic materials and functional materials. [0003] The preparation methods of trimanganese tetraoxide mainly include reduction method, roasting method and suspension oxidation method. At present, the most commonly used method in China is the suspension oxidation method. The raw material is electrolytic manganes...

Claims

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Application Information

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IPC IPC(8): C01G45/02B22F9/04
CPCC01G45/02B22F9/04C01P2006/12
Inventor 许定胜伍宏斌张宏祖国红王慧兰刘革建谢戈杨学燕
Owner HUNAN SPECIAL METAL MATERIALS CO LTD
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