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Method for preparing lamellar ferric oxide by ferreous solution ammonia precipitation method

A technology of ammonia water precipitation and iron oxide, which is applied in the direction of iron oxide, iron oxide/iron hydroxide, etc., can solve the problems of large alkali consumption and high processing cost, and achieve the effects of simple process, lower production cost, and reduced alkali consumption

Inactive Publication Date: 2012-05-23
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to use the iron-containing acid immersion solution obtained by the reaction of waste residue containing ferric iron and sulfuric acid, add ferric oxide crystal seeds after neutralization reaction with ammonia water as a precipitant, and prepare flaky iron oxide through hydrothermal reaction. The process is simple and the production cost is low, which solves the problems of high raw material processing cost and large alkali consumption in the traditional hydrothermal method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] ① Preparation of acid leaching solution: take 3000g of pyrite slag, which contains Fe 2 o 3 : 74.41%, FeO: 8.94%, Al 2 o 3 : 3.24%. Add 5300 mL of 50% sulfuric acid into a 10 L three-necked flask, start stirring, and slowly add the above-mentioned slag. Control the reaction temperature to 115°C. After reacting for 4 hours, add an appropriate amount of water, and filter the obtained iron-containing pickling solution while it is hot. Fe in the pickling solution 3+ 132.46g / L, Fe 2+ 31.28g / L, Al 3+ It is 1.154g / L.

[0018] ②Preparation of flaky iron oxide: Take 2763mL of the above iron-containing acid immersion solution and add it to a 10L autoclave, add 61mL of industrial grade 30% H 2 o 2 Adjust Fe 2+ / Fe 3+ The molar ratio is 0.08, Al 3+ / Fe 3+ The molar ratio is 0.016, then diluted with water to 3L to obtain Fe 3+ After the acid immersion solution with a concentration of 2.5mol / L, add concentrated ammonia water to neutralize Fe 3+ Precipitate completely un...

Embodiment 2

[0020] ① Preparation of acid leaching solution: take 3000g of pyrite slag, which contains Fe 2 o 3 : 74.41%, FeO: 8.94%, Al 2 o 3 : 3.24%. Add 5300 mL of 50% sulfuric acid into a 10 L three-necked flask, start stirring, and slowly add the above-mentioned slag. Control the reaction temperature to 115°C. After reacting for 4 hours, add an appropriate amount of water, and filter the obtained iron-containing pickling solution while it is hot. Fe in the pickling solution 3+ 132.46g / L, Fe 2+ 31.28g / L, Al 3+ It is 1.154g / L.

[0021] ②Preparation of flaky iron oxide: Take 2814mL of the above iron-containing acid leaching solution and add it to a 10L autoclave, add 67mL of industrial grade 30% H 2 o 2 Adjust Fe 2+ / Fe 3+ Molar ratio is 0.1, add 10.2g aluminum sulfate to adjust Al 3+ / Fe 3+ The molar ratio is 0.02, then diluted with water to 3L to obtain Fe 3+ After the acid immersion solution with a concentration of 2.5mol / L, add concentrated ammonia water to neutralize Fe...

Embodiment 3

[0023] ① Preparation of acid leaching solution: take 3000g of pyrite slag, which contains Fe 2 o 3 : 74.41%, FeO: 8.94%, Al 2 o 3 : 3.24%. Add 5300 mL of 50% sulfuric acid into a 10 L three-necked flask, start stirring, and slowly add the above-mentioned slag. Control the reaction temperature to 115°C. After reacting for 4 hours, add an appropriate amount of water, and filter the obtained iron-containing pickling solution while it is hot. Fe in the pickling solution 3+ 132.46g / L, Fe 2+ 31.28g / L, Al 3+ It is 1.154g / L.

[0024] ②Preparation of flaky iron oxide: Take 3650mL of the above iron-containing acid leaching solution and add it to a 10L autoclave, add 83mL of industrial grade 30% H 2 o 2 Adjust Fe 2+ / Fe 3+ The molar ratio is 0.07, add 288.65g of aluminum sulfate to adjust Al 3+ / Fe 3+ The molar ratio is 0.10, then diluted with water to 4L to obtain Fe 3+ After the acid immersion solution with a concentration of 2.5mol / L, add concentrated ammonia water to neu...

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Abstract

The invention relates to a method for preparing lamellar ferric oxide by a ferreous solution ammonia precipitation method, comprising the following steps of: reacting ferriferous waste residues with sulfuric acid to obtain ferreous pickle liquor; adding the pickle liquor to a high-pressure autoclave, and regulating the mole ratio of Fe2+ / Fe3+ contained in the pickle liquor to 0.001-1 and the moleratio of Al3+ / Fe3+ to 0.001-0.5; adding ammonia to carry out neutralization so that the Fe3+ contained in the solution is completely subsided, and then adding 0.001-20 g / L of ferric oxide seed crystals to the solution, wherein control temperature is 100-360 DEG C, and reaction time is 0.05-48 hours; filtering, washing, drying and crushing a product to obtain the lamellar ferric oxide; and evaporating and crystallizing filter liquor to obtain a side product ammonium sulfate or prepare the ammonia through blowing. The invention reduces the production cost of the lamellar ferric oxide, a processfor preparing the ferreous pickle liquor by utilizing the ferriferous waste residues is easy, and resources are utilized; and in addition, the invention has environmental benefit and economic benefit.

Description

technical field [0001] The invention relates to a method for preparing flaky iron oxide. The flaky iron oxide is prepared by an ammonia solution precipitation method containing iron, and belongs to the field of inorganic powder material preparation. Background technique [0002] The chemical composition of flake iron oxide is α-Fe 2 o 3 , a single crystal in the form of fine scales, flat or flakes, is an inorganic non-metallic inert material. Due to its special flaky structure, as a pigment, flaky iron oxide is mixed with a suitable binder and coated on the underlying structure such as the steel structure of the exterior wall, and the flaky iron oxide is self-oriented parallel to the underlying structure Arranged, and partially superimposed on each other, the coating film prevents water penetration and protects the substrate from corrosion. In addition, the directional arrangement can shield the coating medium from degradation caused by ultraviolet rays, and at the same ti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/06
Inventor 郑雅杰刘昭成
Owner CENT SOUTH UNIV
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