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Hercynite synthesis method

A technology of iron-aluminum spinel and synthesis method, applied in chemical instruments and methods, iron compounds, inorganic chemistry, etc., can solve the problems of reduced thermal efficiency, unstable system, etc., and achieves low cost, simple preparation process, and high yield. Effect

Active Publication Date: 2015-05-06
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for synthesizing iron-aluminum spinel, which overcomes the defects of the thermal efficiency reduction caused by the addition of water in the combustion synthesis method and the instability of the system due to evaporation as the temperature rises

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] Prepare iron-aluminum spinel according to the following steps:

[0018] ① Mix 0.01 mol ferric nitrate, 0.02 mol aluminum nitrate, 0.05 mol urea, 0.015 mol diethylamine hydrochloride, and heat to 100°C to form a liquid;

[0019] ②Continue to heat the liquid mentioned in step ① to 200°C to burn the liquid, which will produce a large amount of smoke and open flame, releasing a large amount of heat;

[0020] ③ Collect the solid produced after complete combustion in step ②, cool and grind to obtain a gray-black powder. XRD results show that the powder is pure iron-aluminum spinel, which is designated as sample A.

[0021] Carry out XRD and HRTEM, FESEM and N to above-mentioned white powder respectively 2 Adsorption and desorption test, the test spectrum is as follows Figure 1 to Figure 4 shown. Depend on figure 1 It can be seen that the 2θ angles at 30.92°, 36.22°, 44.30°, 55.06°, 58.26°, and 64.28° in the XRD pattern correspond to (220), (311), (400), (422), (511), (4...

Embodiment 2

[0023] Prepare iron-aluminum spinel according to the following steps:

[0024] ① Mix 0.01 mol ferric nitrate, 0.02 mol aluminum nitrate, 0.05 mol urea, 0.01 mol diethylamine hydrochloride, and heat to 150°C to form a liquid;

[0025] ②Continue to heat the liquid mentioned in step ① to 200°C to burn the liquid, which will produce a large amount of smoke and open flame, releasing a large amount of heat;

[0026] ③ Collect the solid produced after complete combustion in step ②, cool and grind to obtain a gray-black powder. XRD results show that the powder is pure iron-aluminum spinel, which is designated as sample B.

[0027] Carry out XRD and N to the above-mentioned white powder respectively 2 Adsorption and desorption test, XRD pattern as figure 1 As shown in sample B, it presents a pure iron-aluminum spinel structure; N 2 Adsorption and desorption tests show that the specific surface area of ​​the powder is 116.07 m 2 / g, the average pore diameter is 3.81nm, and the total...

Embodiment 3

[0029] Prepare iron-aluminum spinel according to the following steps:

[0030] ① Mix 0.01 mol ferric nitrate, 0.02 mol aluminum nitrate, 0.05 mol urea, 0.008 mol diethylamine hydrochloride, heat to 160°C to form a liquid;

[0031] ②Continue to heat the liquid mentioned in step ① to 240°C, the liquid will burn, and the combustion will produce a large amount of smoke, and produce an open flame, releasing a large amount of heat;

[0032] ③ Collect the solid produced after complete combustion in step ②, cool and grind to obtain a gray-black powder. XRD results show that the powder is pure iron-aluminum spinel, which is designated as sample C.

[0033] Carry out XRD and N to the above-mentioned white powder respectively 2 Adsorption and desorption test, XRD pattern as figure 1 As shown in sample C, it presents a pure iron-aluminum spinel structure; N 2 Adsorption and desorption tests show that the specific surface area of ​​the powder is 143.59 m 2 / g, the average pore diameter...

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Abstract

The present invention discloses a method for synthesizing high specific surface area hercynite through rapid combustion. According to the method, ferric nitrate, aluminum nitrate, urea and one or a plurality of materials selected from trimethylamine hydrochloride, triethylamine hydrochloride, diethylamine hydrochloride and dimethylamine hydrochloride are adopted as raw materials, mixing is performed according to an amount ratio of 1:2:(2-8):(0.1-3), the mixture is heated to achieve a liquid state, heating is continuously performed until the liquid combusts, and the obtained solid is grinded to obtain the hercynite material. According to the invention, the urea and the ammonium salt are adopted as the mixed fuel, and are subjected to the oxidation reduction reaction with the nitrate, the heat released from the combustion reaction is utilized to ensure the formation of the spinel, the large amounts of the gases released by the reaction make the material have the porous structure and the high specific surface area, and the preparation method has characteristics of simpleness, no requirement of sophisticated equipment, short time and high product purity, and is suitable for industrial mass production.

Description

technical field [0001] The invention relates to a method for synthesizing a high specific surface iron-aluminum spinel material with a porous structure, belonging to the field of material preparation. Background technique [0002] with AB 2 o 4 FeAl with spinel structure 2 o 4 (Fe-aluminum spinel) has been used as refractory and magnetic materials due to its excellent physical and chemical properties, such as high strength, high melting point, and good magnetism, and has received more and more attention. In the prior art, synthetic iron-aluminum spinel is generally made of Al 2 o 3 Fe and Fe are used as raw materials by electromelting (Journal of Magnetism and Magnetic Materials, 2003, 264, 264-274), but the process is complicated, the reaction is difficult to control and insufficient, the power consumption is high, and the cost is high. Shock wave synthesis (Glass and Ceramics, 1998; 55:283–284), microwave reaction (Journal of The Asian Ceramic Society, 2013, 1, 41–45...

Claims

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Application Information

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IPC IPC(8): C01G49/00
Inventor 李发堂柴美娟赵叶刘瑞红郝影娟王晓静
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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