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Preparation method of iron nitride based on metal organic framework material

A metal organic framework, iron nitride technology, applied in the direction of nitrogen-metal/silicon/boron binary compounds, etc., can solve the problem of small specific surface area of ​​iron nitride particles, low specific surface area of ​​iron nitride powder, and unfavorable safe operation of devices and other problems, to achieve the effect of improving heat resistance stability, improving yield and quality, and high practical application value

Active Publication Date: 2017-11-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The methods for preparing iron nitride in the prior art mostly use inorganic iron salts or oxides as the iron source, and prepare iron nitride by methods such as reduction nitriding method, vapor deposition method, sol-gel method, high-temperature thermal method, etc., but the above-mentioned The specific surface area of ​​the iron nitride particles synthesized by this method is small, which limits its application in the fields of catalysis and magnetic materials
[0004] Patent CN103145106 provides a method for preparing iron nitride nanopowder, which uses ferric hydroxide as iron source, and prepares and synthesizes iron nitride powder under high pressure in an ammonia atmosphere, but the operating pressure of this method is relatively high. It is not conducive to the safe operation of the device. In addition, the specific surface area of ​​the iron nitride powder prepared by this method is low

Method used

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  • Preparation method of iron nitride based on metal organic framework material
  • Preparation method of iron nitride based on metal organic framework material
  • Preparation method of iron nitride based on metal organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put ferric chloride, terephthalic acid, N,N-dimethylformamide, and copper chloride into a stainless steel reactor lined with polytetrafluoroethylene in a molar ratio of 0.5:0.5:200:0.05. The reaction solution was reacted at 100°C for 10 hours to obtain an iron-containing MOF material with a relative crystallinity of 87% and a BET specific surface area of ​​1045m2. 2 / g.

Embodiment 2

[0031] Put ferric chloride, terephthalic acid, N,N-dimethylformamide, and copper chloride into a stainless steel reactor lined with polytetrafluoroethylene in a molar ratio of 2:2:350:0.2, The reaction solution was reacted at 200°C for 30 hours to obtain an iron-containing MOF material with a relative crystallinity of 90% and a specific surface area of ​​1186m2 by BET test. 2 / g.

Embodiment 3

[0033] Put ferric chloride, terephthalic acid, N,N-dimethylformamide, and copper chloride into a stainless steel reactor lined with polytetrafluoroethylene in a molar ratio of 1:0.8:280:0.07. The reaction solution was reacted at 150°C for 24 hours to obtain an iron-containing MOF material with a relative crystallinity of 98% and a specific surface area of ​​1268m2 by BET test. 2 / g, SEM photos such as image 3 .

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Abstract

The invention provides a preparation method of iron nitride based on a metal organic framework material, and is characterized in that the preparation method comprises the steps: placing a metal organic framework material in a tubular heating furnace, carrying out program heating at a speed of 1-20 DEG C / min to a nitridation temperature of 300-600 DEG C, keeping for 10-24 h under the condition, and thus obtaining an iron nitride material through a nitridation reaction; and after completion of the nitridation reaction, cooling to room temperature, and introducing inert gas to prevent oxidation of iron nitride, wherein the nitrogen-source gas is ammonia and / or nitrogen gas. According to the method, the metal organic framework material or a molding body thereof is used as an iron source, and higher specific surface area, pore volume and metal content of the metal organic framework material or the molding body thereof can well control performance of the iron nitride material; the metal organic framework material or the molding body thereof provides a rich pore system, and the nitrogen-source gas can fully make contact with metal atoms, so as to be conducive to transformation of the nano iron nitride material and improve the yield and quality of the iron nitride.

Description

technical field [0001] The invention belongs to the field of magnetic material preparation, and in particular relates to a method for preparing a magnetic material containing iron. Background technique [0002] Metal nitrides have the properties of covalent compounds, ionic crystals and metals. They have special physical and chemical properties, especially metal nitrides with high specific surface area. The strong catalytic properties of noble metals in this catalytic reaction have attracted extensive attention. Iron nitride is a good magnetic material and has a good application prospect in magnetic fluid. It is also a good catalytic material and has good catalytic activity in Fischer-Tropsch synthesis and ammonia synthesis. [0003] The methods for preparing iron nitride in the prior art mostly use inorganic iron salts or oxides as the iron source, and prepare iron nitride by methods such as reduction nitriding method, vapor deposition method, sol-gel method, high-temperat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/06
Inventor 王海洋马蕊英赵亮张英王刚
Owner CHINA PETROLEUM & CHEM CORP
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