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Method for preparing micaceous iron oxide by molten salt growth method

A technology of mica iron oxide and molten salt method, which is applied in the direction of iron oxide, iron oxide/iron hydroxide, etc., which can solve the requirements of volatile, small particle size of mica iron oxide, high pressure vessel temperature resistance, pressure resistance and corrosion resistance Very strict and other issues, to achieve the effect of shortening the reaction time, lowering the synthesis temperature, and increasing the diffusion speed

Inactive Publication Date: 2010-08-04
FUJIAN KUNCAI MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent US4233283 adopts boric acid (H 3 BO 3 ) or borate (MBO 3 ) was used as a crystal growth accelerator to prepare mica iron oxide, so that the particle size range of mica iron oxide was increased (up to 150 microns), but only the promotion effect of boric acid crystal growth accelerator on the particle size of mica iron oxide was considered, and the use of boric acid was not considered The synergistic influence and regulation of the particle size and color change of micaceous iron oxide particles, the concentration of sodium hydroxide (NaOH) in the hydrothermal reaction crystallization medium, the hydrothermal reaction crystallization temperature and the hydrothermal reaction crystallization time
Patent EP0416648 、 US4289746 、 US3987156 does not use a crystal growth accelerator, which has a poor effect on the particle size and color control of mica iron oxide, and the prepared mica iron oxide particle size is relatively small (below 100 microns)
Chinese patent 0610032440.0, although by adjusting the addition of crystal growth accelerator boric acid, sodium hydroxide medium concentration, hydrothermal reaction crystallization temperature, etc., prepared mica iron oxide with suitable particle size and color change, but this method has high pressure on the main device The temperature and pressure resistance and corrosion resistance of the container are very strict, which brings certain difficulties to the actual industrial production
The method has the advantages of low cost, simple operation, and easy industrialization, but FeCl 2 and FeCl 3 The disadvantage of being volatile, which affects the utilization rate of raw materials

Method used

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  • Method for preparing micaceous iron oxide by molten salt growth method
  • Method for preparing micaceous iron oxide by molten salt growth method
  • Method for preparing micaceous iron oxide by molten salt growth method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 10g iron source ferrous ammonium sulfate (FeSO 4 (NH 4 ) 2 SO 4 ·6H 2 O), 8.80gNa 2 SO 4 , 2.53gK 2 SO 4 Mix and grind evenly, put it into a corundum crucible, put the reaction mixture into a reaction furnace, and the temperature controller will raise the temperature at a rate of 5°C / min, the temperature will reach 800°C, keep the temperature for 30 minutes, preheat treatment; continue to heat up to 950°C and keep warm After 6 hours, the program cools down. After cooling to room temperature, transfer the product to a beaker, add 90ml of deionized water, stir and fully wash in a water bath at about 90°C to dissolve the sintered flux in water, and then wash it with a large amount of deionized water after suction filtration. to remove residual ions. The obtained filter cake was dried in a drying oven at 100 °C for about 1 h. After drying, the structure of the filter cake is loose, and the flaky mica iron oxide product is finally obtained. The obtained micaceous ...

Embodiment 2

[0045] 7g iron source ferrous sulfate FeSO 4 ·7H 2 O, 2.24gNaCl, 2.85gKCl are mixed and ground evenly, put into a porcelain crucible, put the reaction mixture into a reaction furnace, the temperature controller is programmed to heat up at a rate of 5°C / min, the temperature reaches 800°C, and the temperature is maintained for 30 minutes, preheating ;Continue to heat up to 900°C for 6 hours, then program to cool down. After cooling to room temperature, the product appeared as a spatter covering all inner surfaces of the crucible. Transfer the product to a beaker, add 90ml of deionized water, and stir in a water bath at about 90°C to fully wash with water to dissolve the sintered flux in water, and then wash with a large amount of deionized water after suction filtration to remove residual ions. The obtained filter cake was dried in a drying oven at 100 °C for about 1 h. After drying, the structure of the filter cake is loose, and the flaky mica iron oxide product is finally o...

Embodiment 3

[0047] 7g iron source ferrous sulfate (FeSO 4 ·7H 2 O), 8.80gNa 2 SO 4 , 2.53gK 2 SO 4 Mix and grind evenly, put it into a corundum crucible, put the reaction mixture into a reaction furnace, and the temperature controller will raise the temperature at a rate of 5°C / min, the temperature will reach 800°C, keep the temperature for 30 minutes, preheat treatment; continue to heat up to 950°C and keep warm After 6 hours, the program cools down. After cooling to room temperature, transfer the product to a beaker, add 90ml of deionized water, stir and fully wash in a water bath at about 90°C to dissolve the sintered flux in water, and then wash it with a large amount of deionized water after suction filtration. to remove residual ions. The obtained filter cake was dried in a drying oven at 100 °C for about 1 h. After drying, the structure of the filter cake is loose, and the flaky mica iron oxide product is finally obtained. The obtained micaceous iron oxide particles have a ...

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Abstract

The invention provides a method for preparing micaceous iron oxide, which has the advantages of controllable grain size and color change, high purity, complete and reliable production process, easy operation and high resource utilization rate, by a molten salt growth method. In the method, ammonium ferrous sulfate or ferrous sulfate or a mixture of ammonium ferrous sulfate and ferrous sulfate serving as an iron source and sulfates or chlorides or a mixture of sulfates and chlorides serving as a fluxing agent are mixed and melted to form the micaceous iron oxide, wherein the main component of the micaceous iron oxide is a-Fe2O3. The method has the advantages of low cost, easy operation, complete process, no toxicity, high chemical stability, high purity, high crystallinity, high heat resistance, easy realization of industrialization and the like.

Description

technical field [0001] The invention relates to a method for preparing mica iron oxide by using a molten salt method, which uses ammonium ferrous sulfate or ferrous sulfate or a mixture of the two as an iron source, sulfate or chloride as a molten salt flux, and belongs to inorganic powders The field of material preparation. [0002] Background technique [0003] The preparation methods of mica iron oxide mainly include natural mica iron oxide and artificial mica iron oxide. With the development and utilization of natural resources, high-grade natural mica iron oxide deposits are decreasing, and new composite materials have higher and higher quality requirements for mica iron oxide. Synthetic mica iron oxide has the advantages of controllable particle size and color, high chemical stability, high purity, good crystallization and high heat resistance. Synthetic mica iron oxide is gradually replacing natural mica iron oxide and is used in antirust paints, coatings, Pearlesc...

Claims

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Application Information

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IPC IPC(8): C01G49/06
Inventor 袁占辉曾庆新王莉玮谢秉坤
Owner FUJIAN KUNCAI MATERIAL TECH
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