A kind of preparation method of micron superparamagnetic ferric oxide microsphere

A ferric tetroxide, superparamagnetic technology, applied in the direction of iron oxide/iron hydroxide, ferrous oxide, etc., can solve problems such as difficulties, and achieve good dispersion, uniform particle size, and easy-to-obtain raw materials. Effect

Inactive Publication Date: 2016-06-01
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the research on the preparation of Fe3O4 has made great progress, it is still very difficult to prepare spherical superparamagnetic Fe3O4 particles with good dispersion and uniform particle size.

Method used

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  • A kind of preparation method of micron superparamagnetic ferric oxide microsphere
  • A kind of preparation method of micron superparamagnetic ferric oxide microsphere
  • A kind of preparation method of micron superparamagnetic ferric oxide microsphere

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Effect test

Embodiment 1

[0017] A method for preparing micron-sized superparamagnetic ferric oxide microspheres, comprising the following steps: ① adding ferric chloride hexahydrate, sodium formate and 20wt% polyacrylic acid solution into ethylene glycol, and stirring evenly to obtain a mixed solution A , wherein the molar ratio of ferric chloride hexahydrate to sodium formate is 1:9, the molar ratio of ferric chloride hexahydrate to ethylene glycol is 1:500, and the volume ratio of ethylene glycol to 20wt% polyacrylic acid solution is 40 : 1; ② Ferric chloride hexahydrate and sodium acetate are added to ethylene glycol, and stirred evenly to obtain a mixed solution B, wherein the molar ratio of ferric chloride hexahydrate and sodium acetate is 1: 7, trichlorohydrin hexahydrate The molar ratio of iron oxide to ethylene glycol is 1:150; ③ transfer the mixed solution A to a high-pressure reactor with mechanical stirring, the mechanical stirring speed is 200 rpm, and the high-pressure reactor is heated to...

Embodiment 2

[0020] A method for preparing micron-sized superparamagnetic ferric oxide microspheres, comprising the following steps: ① adding ferric chloride hexahydrate, sodium formate and 10wt% polyacrylic acid solution into ethylene glycol, and stirring evenly to obtain a mixed solution A , wherein the molar ratio of ferric chloride hexahydrate to sodium formate is 1:8, the molar ratio of ferric chloride hexahydrate to ethylene glycol is 1:400, and the volume ratio of ethylene glycol to 10wt% polyacrylic acid solution is 30 : 1; ② ferric chloride hexahydrate and sodium acetate are added to ethylene glycol, and stirred evenly to obtain a mixed solution B, wherein the molar ratio of ferric chloride hexahydrate and sodium acetate is 1: 6, and trichlorohydrin hexahydrate The molar ratio of iron oxide to ethylene glycol is 1:100; ③ transfer the mixed solution A to a high-pressure reactor with mechanical stirring, the mechanical stirring speed is 150 rpm, and the high-pressure reactor is heate...

Embodiment 3

[0022] A method for preparing micron-sized superparamagnetic ferric oxide microspheres, comprising the following steps: ① adding ferric chloride hexahydrate, sodium formate and 30wt% polyacrylic acid solution into ethylene glycol, and stirring evenly to obtain a mixed solution A , wherein the molar ratio of ferric chloride hexahydrate to sodium formate is 1:10, the molar ratio of ferric chloride hexahydrate to ethylene glycol is 1:300, and the volume ratio of ethylene glycol to 30wt% polyacrylic acid solution is 50 : 1; ② Ferric chloride hexahydrate and sodium acetate are added to ethylene glycol, and stirred evenly to obtain a mixed solution B, wherein the molar ratio of ferric chloride hexahydrate and sodium acetate is 1: 8, trichlorohydrin hexahydrate The molar ratio of iron oxide to ethylene glycol is 1:50; ③ transfer the mixed solution A to a high-pressure reactor with mechanical stirring, the mechanical stirring speed is 300 rpm, and the high-pressure reactor is heated to...

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Abstract

The invention belongs to a preparation method for micron-sized superparamagnetic ferroferric oxide microspheres. A two-step seed growth method is adopted for controlling synthesis, namely nanometer particles generated by a solution A are used as seeds, a solution B is used as mother liquor for subsequent growth, and the ratio of the nanometer particles to the solution B and the temperatures of the nanometer particles and the solution B are controlled to regulate and control the sizes of the superparamagnetic ferroferric oxide microspheres. The sizes of the prepared micron-sized superparamagnetic ferroferric oxide microspheres are ranged from 500 to 2,500nm, and the prepared ferroferric oxide microspheres are high in dispersibility and uniform in particle size, and have superparamagnetism.

Description

technical field [0001] The invention relates to the field of nanomaterial preparation, in particular to a method for preparing micron-sized superparamagnetic ferric oxide microspheres. Background technique [0002] Ferric oxide (Fe 3 o 4 ) is an important spinel-type ferrite, and it is a new type of high-function inorganic material facing the 21st century. Therefore, it has a very broad application prospect in the fields of national defense, environmental engineering, surface engineering, chemical industry, electronics and semiconductor materials. In the past few decades, various methods for the preparation of Fe3O4 have attracted much attention, and so far, a variety of synthetic methods have been developed, such as chemical co-precipitation, oil / water emulsion, thermal decomposition, solvent Thermal synthesis method, sonochemical method, jet decomposition method, arc discharge method, combustion synthesis method, etc. Although the research on the preparation of Fe3O4 h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/08
Inventor 王永强邹炳芳周少敏郑海红程琳
Owner HENAN UNIVERSITY
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