Process for preparing electronic grade manganous-manganic oxide and byproduct nano-iron oxide red from pyrolusite

A technology of trimanganese tetraoxide and red iron oxide, applied in the field of manganese hydrometallurgy, can solve the problems of low manganese leaching rate, environmental pollution, low metal recovery rate, etc.

Active Publication Date: 2014-09-03
JISHOU UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The process for preparing electronic-grade manganese tetraoxide by-product nano-iron oxide red by wet reduction of pyrolusite provided by the present invention aims to solve the problem of low manganese leach

Method used

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  • Process for preparing electronic grade manganous-manganic oxide and byproduct nano-iron oxide red from pyrolusite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Ball-mill the pyrolusite to 80 mesh and then sieve it. Add iron filings as a reducing agent to the sifted material and stir evenly. The amount of iron filings added makes the molar ratio of manganese and iron in the pyrolusite 1.5:1. . The obtained mixed mineral powder is metered into an acid leaching tank, and sulfuric acid with a concentration of 80wt% equivalent to 60% of the mixed mineral powder weight is added. Then, add water, and control the addition of the amount of water according to the solid-to-liquid ratio of 1:6. Stirring and leaching at 80° C. for 5 h, and then separating by filtration to obtain a filtrate. At first the pH of gained filtrate is adjusted to 2.0 and temperature is kept on 38-40 ℃, then this filtrate is adsorbed (reaching equilibrium in 100 minutes) with the adsorption resin A of absorbing iron (Ⅲ), and aqueous phase and adsorption resin phase are separated, obtain Tail water containing manganese and adsorption resin phase containing iron (...

Embodiment 2

[0052] Example 1 was repeated. Other conditions are as follows:

[0053] According to the above steps of ball mill sieving, batching, acid leaching, ion exchange, impurity removal, manganese precipitation, oxidation, washing, drying and other steps, in the batching process, choose pyrolusite with a manganese grade of 35.8% and iron-containing 95.6% scrap iron scrap is used as raw material, and the molar ratio of manganese substance in pyrolusite to iron substance in reducing agent is 1.4:1. The leaching rate of manganese reaches 98.6%, and the comprehensive recovery rate of manganese is 92.5%, the manganese content in the trimanganese tetraoxide product is 71.5%, and the specific surface area is 23.6m 2 / g, selenium-free, silicon dioxide content is 0.005%, sulfur content is 0.032%, the content of ferric oxide in the nano-iron red product is 98.0%, and the particle size is 80nm.

Embodiment 3

[0055] Repeat embodiment 1, wherein use propylene glycol to replace xylitol, other conditions are as follows:

[0056] According to the above steps of ball mill sieving, batching, acid leaching, ion exchange, impurity removal, manganese precipitation, oxidation, washing, drying and other steps, in the batching process, choose pyrolusite with a manganese grade of 27.5% and iron-containing 93.6% of waste iron chips are used as raw materials, and the molar ratio of the amount of manganese in the pyrolusite to the amount of iron in the reducing agent is 1.5:1. The leaching rate of manganese is 98.5%, and the comprehensive recovery rate of manganese is 91.8%, the manganese content in the manganese tetraoxide product is 71.6%, and the specific surface is 22.8m 2 / g, no selenium, silicon dioxide content of 0.006%, sulfur content of 0.038%, iron oxide content of 98.6% in the nano-iron red product, particle size of 90nm.

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Abstract

The invention belongs to the technical field of wet metallurgy of manganese, and provides a process for preparing electronic grade manganous-manganic oxide and byproduct nano-iron oxide red from pyrolusite by means of wet reduction. The process is used for preparing an electronic grade manganous-manganic oxide product by steps of ball-mill screening, preparing (adding a reducing agent), acid pickling, ion exchanging by chelate resin, impurity removing, manganese precipitation, oxidizing, washing, baking and the like, wherein an ion exchange eluent is subjected to iron neutralizing precipitation, filtering, washing and drying, calcining and the like to produce a byproduct nano-iron oxide red; the leaching rate of manganese is over 98 percent, the comprehensive recycling rate is more than 90 percent, the content of manganese in the manganous-manganic oxide is 71 percent, the specific surface area is more than 20m<2>/g, the byproduct nano-iron oxide red product can be prepared, the purity of the nano iron red product is more than 95 percent, and the grain diameter of the nano iron red product is less than 100nm. Compared with the prior art, the purity of the manganous-manganic oxide product is increased, the product quality is more stable, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of manganese hydrometallurgy, and in particular relates to a process for preparing electronic-grade manganese tetraoxide by-product nano-iron oxide red through wet reduction of pyrolusite. Background technique [0002] Electronic grade manganese tetroxide is a high-performance structural material, mainly used in the electronics industry, and is one of the important raw materials required for the production of soft ferrite. Especially in recent years, with the rapid development of the electronic information industry, the output of my country's soft ferrite has been increasing. For the manganese tetraoxide as its raw material, more and more demands have been proposed not only in quantity but also in quality and performance. high demands. The preparation method of trimanganese tetroxide can be divided into five classes according to the difference of manganese raw materials used: (1) metal manganese method; (2) ...

Claims

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Application Information

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IPC IPC(8): C01G49/08C01G49/06B82Y30/00
Inventor 颜文斌方玉刘阳文高峰石爱华华骏
Owner JISHOU UNIVERSITY
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