Preparation method of nanoscale hercynite

A kind of iron-aluminum spinel and nano-scale technology, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of high thermal conductivity of iron-aluminum spinel, uneven particle size, and high energy consumption of electric melting method problem, achieve the effect of reducing the synthesis temperature and operation difficulty, reducing the calcination temperature and simplifying the synthesis process

Active Publication Date: 2015-07-29
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The sintering method uses metallic iron and alumina as starting materials. Iron can only form ferrous oxide in a weakly reducing atmosphere, and then react with alumina to form iron-aluminum spinel. The key to the synthesis is to strictly control the reaction atmosphere to be weakly reducing. The reaction conditions are not easy to control during the specific implementation of this method (patent publication number: CN102583462A), and in order to be applicable to high-temperature tunnel kilns, rotary kilns and shaft kilns commonly used in industrial production, etc. cannot guarantee good sealing, the obtained iron-aluminum The yield of spinel products is not high, and the particle size is not uniform
The iron-aluminum spinel synthesized by

Method used

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Experimental program
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Effect test

Embodiment 1

[0021] A preparation method of nano-scale iron-aluminum spinel, the method comprises the steps of:

[0022] (1) Preparation of Fe-Al spinel precursor

[0023] Measure N,N-dimethylformamide and water to make a mixed solution with a volume ratio of 20:55 for subsequent use; weigh 4.22g aluminum nitrate nonahydrate, 1.245g terephthalic acid and 0.795g iron acetylacetonate and dissolve in 75mL of the mixed solution, heated and stirred until completely dissolved to obtain a reactant solution; put the prepared reactant solution in a closed container for aging at a temperature of 130°C for 48 hours, then lower it to room temperature, centrifuge to obtain a precipitate, add The precursor product was obtained after washing the precipitate three times with an appropriate amount of N,N-dimethylformamide.

[0024] (2) Preparation of nano-scale iron-aluminum spinel

[0025] Put the precursor product obtained in step (1) into a high-temperature furnace protected by nitrogen flow, raise th...

Embodiment 2

[0028] A preparation method of nano-scale iron-aluminum spinel, the method comprises the steps of:

[0029] (1) Preparation of Fe-Al spinel precursor

[0030] Measure N,N-dimethylformamide and water to make a mixed solvent with a volume ratio of 20:55, and set aside; weigh 2.11g aluminum nitrate nonahydrate and 0.29g aluminum oxide, 1.245g terephthalic acid and 0.795g Dissolve iron acetylacetonate in 75mL of the mixed solution, heat and stir until completely dissolved to obtain a reactant solution; put the prepared reactant solution in a closed container for aging at a temperature of 130°C for 48h, then cool down to room temperature, and centrifuge The precipitate was obtained, and an appropriate amount of N,N-dimethylformamide was added to wash the precipitate three times to obtain a precursor product.

[0031] (2) Preparation of nano-scale iron-aluminum spinel

[0032] Put the precursor product obtained in step (1) into a high-temperature furnace protected by nitrogen flow...

Embodiment 3

[0034] A preparation method of nano-scale iron-aluminum spinel, the method comprises the steps of:

[0035] (1) Preparation of Fe-Al spinel precursor

[0036] Measure N,N-dimethylformamide and water to make a mixed solution with a volume ratio of 20:55 for subsequent use; weigh 2.11g aluminum nitrate nonahydrate and 0.44g aluminum hydroxide, 1.245g terephthalic acid and 0.795 Dissolve 1 g of iron acetylacetonate in 75 mL of mixed solution, heat and stir until completely dissolved to obtain a reactant solution; put the prepared reactant solution in a closed container for aging at a temperature of 130°C for 48 hours, and then lower it to room temperature, The precipitate was obtained by centrifugation, and an appropriate amount of N,N-dimethylformamide was added to wash the precipitate three times to obtain the precursor product.

[0037] (2) Preparation of nano-scale iron-aluminum spinel

[0038] Put the precursor product obtained in step (1) into a high-temperature furnace p...

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Abstract

The invention relates to a preparation method of nanoscale hercynite. The method comprises steps as follows: (1) a mixed solution of N,N-dimethyl formamide and water is prepared, wherein the volume fraction of the N,N-dimethyl formamide ranges from 65% to 85%; (2) an aluminum-containing compound, terephthalic acid and ferric acetylacetonate with the molar ratio being 15:10:3 are added to the solution prepared in Step (1) and evenly stirred, and a reactant solution is prepared; (3) the reactant solution prepared in Step (2) is aged in an airtight manner, then cooled to the room temperature and subjected to solid-liquid separation, and a hercynite precursor product is obtained; (4) the hercynite precursor product is placed in a high-temperature furnace for calcination and then cooled to the room temperature, and the nanoscale hercynite is obtained. Compared with the prior art, the preparation method has the advantages that the synthesis process is simple, the method is convenient to operate, the cost is low, the energy consumption is low and the like.

Description

technical field [0001] The invention relates to a preparation method of nanometer materials, in particular to a preparation method of nanoscale iron-aluminum spinel. Background technique [0002] There are many kinds of spinel-type composite oxides and they are widely used. Different cations entering the spinel structure can have many different charge combinations. The distribution of cations in the spinel structure is not only related to the chemical composition, but also related to the charge of the constituent cations, crystal chemistry and the physicochemical environment during formation. Spinel composite oxides can be used as pigments, catalytic materials, magnetic materials and other applications. With the continuous deepening of people's understanding and research, its application range in practice is also becoming more and more extensive. Recent studies have shown that oxygen-deficient spinel ferrite has a good prospect in the control of air pollution, which can b...

Claims

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Application Information

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IPC IPC(8): C01G49/00B82Y30/00
Inventor 吴一楠李风亭卢慧宫
Owner TONGJI UNIV
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