Method of producing iron oxide red through iron sulfate hydrothermal process

A technology of ferrous sulfate and red iron oxide, applied in the directions of iron oxide, iron oxide/iron hydroxide, etc., can solve the problems of high raw material cost, large alkali consumption and high production cost, and achieve lower production cost and lower alkali The effect of stable consumption and quality

Inactive Publication Date: 2015-12-09
CENT SOUTH UNIV
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Problems solved by technology

The Chinese patent with the publication number CN1903735A discloses a method for producing iron oxide red by ferrous sulfate hydrothermal method, which is a hydrothermal reaction under oxygen pressure, and the process reaction pressure is high (1.2-2.2MPa), requiring excessive Ammonia water has large alkali consumpt

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Fe(OH) 3 The preparation of colloid: get ferrous sulfate (main component FeSO 4 4H 2 O) 106.8?g, the preparation of Fe 2+ 700?mL of ferrous sulfate solution with a concentration of 0.6?mol / L was placed in a 1000?mL three-neck flask, and concentrated ammonia water was slowly added dropwise under sufficient stirring conditions to adjust the initial pH value of the reaction solution to 9.5. The oxygen flow rate was 0.4?L / min, the stirring speed was 450?r / min, and after 1.5?h of reaction at room temperature, the aeration was stopped. Fully washed, vacuum filtered to obtain Fe(OH) 3 colloid.

[0019] Preparation of iron oxide red: take 288.6?g of the above-mentioned Fe(OH) 3 Prepare 300 mL of colloidal solution with a total iron concentration of 1.25 2+ ) / n(Fe 3+ ) at a ratio of 0.08 to 0.08, add 7.784?g, and add 1.5?g iron oxide red (Hunan Sanhuan Pigment Co., Ltd., superfine iron oxide red H130M) at a concentration of 5?g / L. Transfer the prepared colloidal solu...

Embodiment 2

[0021] Fe(OH) 3 Preparation of colloid: Take 600?g of titanium dioxide by-products, dry ferrous sulfate and 2.3?g of reduced iron powder, dissolve in saturation at 64?°C, slowly cool to 10?°C for recrystallization, and obtain 1 refined sulfurous acid Iron 634.6?g, crystallization yield 89.46%. Take 126.3 g of refined ferrous sulfate once to prepare Fe 2+ 700?mL of ferrous sulfate solution with a concentration of 0.6?mol / L was placed in a 1000?mL three-neck flask, and concentrated ammonia water was slowly added dropwise under sufficient stirring conditions to adjust the initial pH value of the reaction solution to 9.5. The oxygen flow rate was 0.3?L / min, the stirring speed was 400?r / min, and after 2.5?h of reaction at room temperature, the aeration was stopped. Fully washed, vacuum filtered to obtain Fe(OH) 3 colloid.

[0022] Preparation of iron oxide red: take 273.7?g of the above-mentioned Fe(OH) 3 Prepare 300?mL colloidal solution with a total iron concentration of...

Embodiment 3

[0024] Fe(OH) 3 Preparation of colloid: Take 600?g of titanium dioxide by-products, dry ferrous sulfate and 2.3?g of reduced iron powder, dissolve in saturation at 64?°C, slowly cool to 10?°C for recrystallization, and obtain 1 refined sulfurous acid Iron 634.6?g, crystallization yield 89.46%. Take 400?g of refined ferrous sulfate for the first time, dissolve it in saturation at 64?°C, slowly cool to 10?°C for recrystallization, and obtain 307.3?g of refined ferrous sulfate for the second time, with a crystallization yield of 78.74%. Take 102.6 g of refined ferrous sulfate twice to prepare Fe 2+ 700?mL of ferrous sulfate solution with a concentration of 0.5?mol / L was placed in a 1000?mL three-neck flask, and concentrated ammonia water was slowly added dropwise under sufficient stirring conditions to adjust the initial pH value of the reaction solution to 9. The air flow rate was 1.5?L / min, the stirring speed was 200?r / min, and after 12?h of reaction at room temperature, th...

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Abstract

The invention relates to a method of producing iron oxide red through an iron sulfate hydrothermal process. The method of producing iron oxide red through the iron sulfate hydrothermal process comprises the steps of dissolving iron sulfate in water to prepare an Fe<2+> solution with the concentration of 0.1 to 1 mol/L, slowly dripping ammonia water under the condition of full agitation, regulating the pH value of the solution to 8 to 10, feeding oxygen or air, performing room-temperature reaction for 1 to 24h under agitation to obtain Fe(OH)3 colloids and filtrate, preparing the Fe(OH)3 colloids into a colloid solution with the total iron concentration being 0.5 to 2 mol/L, adding iron oxide red crystal seeds and heptahydrate iron sulfate, performing hydrothermal reaction for 0.5 to 3h at 200 to 300 DEG C in a high-pressure kettle, then performing filtration, washing, drying and crushing to obtain the iron oxide red, performing ammonia precipitation, and then recovering ammonium sulfate through evaporative crystallization of filtrate or preparing ammonia water through stripping. By preparing the iron oxide red by using the iron sulfate hydrothermal process, the process is simple, and the production cost of the iron oxide red is reduced and the environmental and economic benefits are great.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic powder materials, and in particular relates to a method for producing iron oxide red by using ferrous sulfate. Background technique [0002] Ferrous sulfate mainly comes from the production of titanium dioxide. Titanium dioxide (commonly known as titanium dioxide) is currently the most important white pigment in the world. Its production processes mainly include sulfuric acid method and chlorination method. China's titanium dioxide output reached 2.466 million tons in 2014, and most of China's titanium dioxide production uses the sulfuric acid method. The sulfuric acid method is used to produce titanium dioxide. For every ton of titanium dioxide produced, 3.5 to 4 tons of ferrous sulfate must be discharged. China discharged about 9 million tons of ferrous sulfate in 2014. Such a large amount of ferrous sulfate (FeSO 4 ·7H 2 O) If it is not comprehensively utilized, it will pollute the env...

Claims

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Application Information

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IPC IPC(8): C01G49/06
Inventor 郑雅杰余旺
Owner CENT SOUTH UNIV
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