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Method for preparing mica iron oxide by hydrothermal reaction and crystallizing

A mica iron oxide, hydrothermal reaction technology, applied in the direction of iron oxide, iron oxide/iron hydroxide, fibrous filler, etc., can solve the problem of not considering the synergistic effect and regulation effect of boric acid usage, particle size and color of mica iron oxide The control effect is not good, and the difficulty and load of impurity ions are increased, so as to achieve the effect of convenient industrial application, strong brightness and three-dimensional effect, and smooth crystal surface

Inactive Publication Date: 2008-05-28
XIANGTAN UNIV
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  • Abstract
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Problems solved by technology

[0003] In the existing technology of hydrothermal reaction crystallization to produce mica iron oxide, the patents EP0416648, US4289746, GB1333788, and US3987156 do not use crystal growth accelerators, and the control effect on mica iron oxide particle size and color is not good, and the prepared mica iron oxide particles Small diameter (below 100 microns)
Patent US4233283 adopts boric acid (H 3 BO 3 ) or borate (MBO 3 ) as a crystal growth accelerator to prepare mica iron oxide, so that the particle size range of mica iron oxide can be enlarged (up to 150 microns), but only the promotion effect of boric acid crystal growth accelerator on the particle size of mica iron oxide is considered, and boric acid is not considered. The synergistic influence and regulation of usage amount, sodium hydroxide (NaOH) concentration of hydrothermal reaction crystallization medium, hydrothermal reaction crystallization temperature and hydrothermal reaction crystallization time on mica iron oxide particle size and color change, and the oxidant used is chloric acid Sodium (NaClO 3 ) or sodium nitrate (NaNO 3 ), thus bringing in new chlorate or nitrate impurity ions, increasing the difficulty and load of separating these impurity ions in subsequent processes

Method used

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  • Method for preparing mica iron oxide by hydrothermal reaction and crystallizing

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Experimental program
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Embodiment 1

[0026] Dissolve 80g of titanium dioxide by-product ferrous sulfate in 300ml of soft water with a temperature of 60°C, filter, and the filtrate is the once-purified ferrous sulfate solution. Add 1.5g of NaOH precipitant and 2.0g of 20% polyacrylamide flocculant, stir slowly for 0.5h, then let it stand for 3h, the supernatant is the secondary purified ferrous sulfate solution. At a temperature of 60°C, 14g of concentrated sulfuric acid with a concentration of 98% was added to the ferrous sulfate solution for secondary purification, and then 23g of hydrogen peroxide with a concentration of 27.5% was added to make the FeSO 4 Oxidized to Fe 2 (SO 4 ) 3 , cooled to room temperature. In the solution after the above reaction, drip 115g concentration of ammonia water of 25%, while stirring, to make Fe 2 (SO 4 ) 3 Fe(OH) transformed into slurry 3 Precursor, stand for 1h, decant. The resulting slurry was washed to pH 6.0. Transfer the slurry to an autoclave with a volume of 1L, ...

Embodiment 2

[0039] Dissolve 80g of titanium dioxide by-product ferrous sulfate in 300ml of soft water with a temperature of 60°C, filter, and the filtrate is the once-purified ferrous sulfate solution. Add 1.5g of NaOH precipitant and 2.0g of 20% polyacrylamide flocculant, stir slowly for 0.5h, then let it stand for 3h, the supernatant is the secondary purified ferrous sulfate solution. At a temperature of 60°C, 14g of concentrated sulfuric acid with a concentration of 98% was added to the ferrous sulfate solution for secondary purification, and then 23g of hydrogen peroxide with a concentration of 27.5% was added to make the FeSO 4 Oxidized to Fe 2 (SO 4 ) 3 , cooled to room temperature. In the solution after the above reaction, drip 115g concentration of ammonia water of 25%, while stirring, to make Fe 2 (SO 4 ) 3 Fe(OH) transformed into slurry 3 Precursor, stand for 1h, decant. The resulting slurry was washed to pH 6.0. Transfer the slurry to a 1L autoclave, add a NaOH solutio...

Embodiment 3

[0041] Dissolve 80g of titanium dioxide by-product ferrous sulfate in 300ml of soft water with a temperature of 60°C, filter, and the filtrate is the once-purified ferrous sulfate solution. Add 1.5g of NaOH precipitant and 2.0g of 20% polyacrylamide flocculant, stir slowly for 0.5h, then let it stand for 3h, the supernatant is the secondary purified ferrous sulfate solution. At a temperature of 60°C, 14g of concentrated sulfuric acid with a concentration of 98% was added to the ferrous sulfate solution for secondary purification, and then 23g of hydrogen peroxide with a concentration of 27.5% was added to make the FeSO 4 Oxidized to Fe 2 (SO 4 ) 3 , cooled to room temperature. In the solution after the above reaction, drip 115g concentration of ammonia water of 25%, while stirring, to make Fe 2 (SO 4 ) 3 Fe(OH) transformed into slurry 3 Precursor, stand for 1h, decant. The resulting slurry was washed to pH 6.0. Transfer the slurry to a 1L autoclave, add a NaOH solutio...

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Abstract

The present invention provides preparation process of mica iron oxide with controllable particle size and color. Ferrous sulfate as the side product of titanium white powder production is used as the material, and through dissolving and purifying, oxidation, creating precursor, hydrothermal reaction and crystallization in controlled conditions, and post-treatment, mica iron oxide with controllable particle size and color is prepared. The mica iron oxide product is in regular hexagonal sheet shape and has particle size of 40-180 micron and color regulated through altering the crystal growth promoter adding amount, medium concentration, temperature and time in the hydrothermal reaction and crystallization stage.

Description

technical field [0001] The invention relates to a method for preparing mica iron oxide with controllable change in particle size and color by using ferrous sulfate, a by-product of titanium dioxide, as a raw material and adopting hydrothermal reaction crystallization, and belongs to the field of inorganic powder material preparation. Background technique [0002] In the industrial production of titanium dioxide produced by the sulfuric acid method, three tons of polyferrous sulfate (FeSO 4 ·7H 2 O). These by-product ferrous sulfates do not have much economic value of direct utilization, but also bring about the environmental problems of these by-product ferrous sulfates piled up. If it can be processed into high value-added mica iron oxide (α-Fe 2 o 3 ), then not only can produce considerable economic benefits, but also solve the outlet and environmental protection problems of by-product ferrous sulfate. [0003] In the existing technology of hydrothermal reaction cryst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/06C09C1/24
Inventor 刘跃进危自燕李振民李功军莫再勇
Owner XIANGTAN UNIV
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