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Preparation method of ultrafine iron boride

A technology of iron boride and boric acid solution, which is applied in the direction of boron/boride, metal boride, etc., can solve the problems of small BET, large particle size of iron boride, and low activity, and achieve large BET, high purity, and environmental protection pressure small effect

Active Publication Date: 2020-07-07
蒋央芳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the iron boride obtained by the conventional preparation method has a large particle size, a small BET, and low activity.

Method used

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  • Preparation method of ultrafine iron boride
  • Preparation method of ultrafine iron boride
  • Preparation method of ultrafine iron boride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A kind of preparation method of superfine ferric boride, it is the following steps:

[0037] (1) after ferrous gluconate solution and boric acid solution are mixed, spray drying, obtain spray-dried material, the mol ratio of ferrous gluconate solution and boric acid is 1:1.01;

[0038] (2) Sintering the spray-dried material in a methane atmosphere, the sintering time is 10h, and the sintering temperature is 1200°C to react to obtain the reduced material;

[0039] (3) continue to feed carbon dioxide into the reducing material, and react at a temperature of 700°C for 4 hours to obtain a sintered material;

[0040] (4) The sintered material is subjected to jet crushing, screening and vacuum packaging to obtain superfine iron boride.

[0041] The concentration of described step (1) ferrous gluconate solution is 1.5mol / L, and the concentration of boric acid solution is 1mol / L, and spray drying adopts centrifugal spray drier, and the rotating speed of centrifugal atomization...

Embodiment 2

[0049] A kind of preparation method of superfine ferric boride, it is the following steps:

[0050](1) after ferrous gluconate solution and boric acid solution are mixed, spray drying, obtain spray-dried material, the mol ratio of ferrous gluconate solution and boric acid is 1:1.02;

[0051] (2) Sintering the spray-dried material in a methane atmosphere, the sintering time is 10h, and the sintering temperature is 1200°C to react to obtain the reduced material;

[0052] (3) Continue to feed carbon dioxide into the reducing material, and react at a temperature of 850° C. for 2 hours to obtain a sintered material;

[0053] (4) The sintered material is subjected to jet crushing, screening and vacuum packaging to obtain superfine iron boride.

[0054] The concentration of described step (1) ferrous gluconate solution is 3mol / L, and the concentration of boric acid solution is 2mol / L, and spray drying adopts centrifugal spray drier, and the rotating speed of centrifugal atomization ...

Embodiment 3

[0062] A kind of preparation method of superfine ferric boride, it is the following steps:

[0063] (1) after ferrous gluconate solution and boric acid solution are mixed, spray drying, obtain spray-dried material, the mol ratio of ferrous gluconate solution and boric acid is 1:1.015;

[0064] (2) Sintering the spray-dried material in a methane atmosphere, the sintering time is 8h, and the sintering temperature is 1000°C to react to obtain the reduced material;

[0065] (3) Continue to feed carbon dioxide into the reducing material, and react at a temperature of 780° C. for 3 hours to obtain a sintered material;

[0066] (4) The sintered material is subjected to jet crushing, screening and vacuum packaging to obtain superfine iron boride.

[0067] The concentration of described step (1) ferrous gluconate solution is 2mol / L, and the concentration of boric acid solution is 1.2mol / L, and spray drying adopts centrifugal spray drier, and the rotating speed of centrifugal atomizati...

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Abstract

The invention discloses a preparation method of ultrafine iron boride. A ferrous gluconate solution is mixed with a boric acid solution, and spray drying is carried out to obtain a spray-dried material, and the molar ratio of the ferrous gluconate solution to boric acid is 1: 1.01-1.02; the spray-dried material is sintered in a methane atmosphere for 5-10 hours at the sintering temperature of 800-1200 DEG C for reaction to obtain a reduced material; carbon dioxide is continuously introduced into the reducedmaterial, and reacting for 2-4 hours at the temperature of 700-850 DEG C is carried outto obtain a sintered material; and jet milling, screening and vacuum packaging are carried out on the sintered material to obtain the ultrafine iron boride. The ultrafine iron boride can be prepared,the particle size is small, BET is large, and the purity is high.

Description

technical field [0001] The invention relates to a method for preparing ultrafine iron boride, belonging to the technical field of powder preparation. Background technique [0002] Iron boride is a boride of iron with a chemical formula of FeB and a molecular weight of 66.66. Iron boride is a gray orthorhombic crystal with a melting point of 1652°C and a density of 7.15g / mL. The iron borides are arranged in a zigzag chain, with iron atoms at the corners of the triangular prism, and boron atoms at the center of the triangular prism, connected in the zigzag chain in the form of covalent bonds. The melting point of iron boride is 1652°C and the density is 7.15g / mL. It is soluble in dilute and concentrated nitric acid, concentrated and 1:1 hydrochloric acid solution, and 1:1 H 2 SO 4 and HClO 4 in, μ eff = 1.1 µB. It exists in α-form at low temperature and in β-form with the same Tc (602K) at high temperature. With the change of magnetic moment, it transforms from α to β. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04
CPCC01B35/04C01P2004/03C01P2004/61C01P2004/62C01P2006/11C01P2006/12C01P2006/80
Inventor 蒋央芳
Owner 蒋央芳
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