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Fe3O4/TiO2 nano magnetic compound and preparation method thereof

A nano-magnetism and composite technology, which is applied in the fields of inorganic material magnetism, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of complex operation process, weakened magnetic properties, and difficult to achieve separation effect, and achieves simple process, Easy to operate effect

Inactive Publication Date: 2012-10-03
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Domestic magnetic nano TiO 2 / Fe 3 o 4 The complex has done a lot of research, such as the Chinese invention patent CN1562464 using the sol-gel method to prepare Fe 3 o 4 As the core, SiO 2 As the isolation layer, TiO 2 It is a double-coated magnetic nanocomposite with an outer coating layer. This method has a complicated operation process and will weaken the Fe 3 o 4 magnetic properties
[0006] Sun Ming and others used an improved sol-gel method to prepare TiO in "Chemical Industry and Engineering", Volume 25, Phase 2, Page 104-106, 2008 2 / SiO 2 / Fe 3 o 4 Coated compound has better effect, but it complicates the preparation process. If the conditions are not well controlled, the effect of the prepared compound is not good
[0007] Bao Shujuan et al. reported in "Molecular Catalysis" 2003, Volume 17, Issue 2, Page 96-99 that the reaction of Fe with polyethylene glycol 3 o 4 The surface was modified to prepare TiO by sol-gel method 2 / Fe 3 o 4 Magnetic composites, this method uses surfactants in the preparation process, it is difficult to achieve the effect of separation, and it will cause inconvenience to the subsequent processing process

Method used

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  • Fe3O4/TiO2 nano magnetic compound and preparation method thereof
  • Fe3O4/TiO2 nano magnetic compound and preparation method thereof
  • Fe3O4/TiO2 nano magnetic compound and preparation method thereof

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Embodiment 1

[0034] (1) Weigh 5.96g FeCl 2 4H 2 O and 16.22 g FeCl 3 ·6H 2 O, add 30ml of distilled water, heat in a water bath at 50°C, stir at 450rpm to dissolve, add ammonia water dropwise until pH = 11, react for 1h, and obtain Fe 3 o 4 Liquid, adjust pH=5, let it stand for later use;

[0035] (2) Preparation of Fe 3 o 4 The mass of 6.96g, according to TiO 2 / Fe 3 o 4 The mass ratio is 3, and the nano-TiO with a solid content of 30% mass fraction is weighed 2 Colloidal solution (Hunan Titang Nano Technology Co., Ltd.) 69.6g, primary particle size 5nm, surface potential +39.7mV, dilute it into a 10% mass fraction solution, heat it in a water bath to 80°C, and prepare in step (1) Slowly add the liquid into it, stir at 350rpm, and the stirring time is 1h, then centrifuge at 3500rpm, put it into a vacuum oven with a vacuum degree of -0.09MPa to dry at 80°C, and grind to obtain a magnetic Fe 3 o 4 / TiO 2 Composite samples.

Embodiment 2

[0037] (1) Weigh 5.96g FeCl 2 4H 2 O and 16.22 g FeCl 3 ·6H 2 O, add 30ml of distilled water, heat in a water bath at 50°C, stir at 450rpm to dissolve, add ammonia water dropwise until pH = 11, react for 1h, and obtain Fe 3 o 4 Liquid, adjust pH=5, let it stand for later use;

[0038] (2) Fe produced 3 o 4 The mass of 6.96g, according to TiO 2 / Fe 3 o 4The mass ratio of = 3, weigh the nano-TiO with a solid content of 30% mass fraction 2 Colloidal solution (Hunan Titang Nano Technology Co., Ltd.) 69.6g, primary particle size 5nm, surface potential +39.7mV, dilute it into a 10% mass fraction solution, heat it in a water bath to 80°C, and prepare in step (1) Slowly add the liquid into it, stir at 350rpm for 2h, then centrifuge at 3500rpm, dry at 80°C in a vacuum oven with a vacuum of -0.1MPa, and grind to obtain magnetic Fe 3 o 4 / TiO 2 Composite samples.

Embodiment 3

[0040] (1) Weigh 5.96g FeCl 2 4H 2 O and 16.22 g FeCl 3 ·6H 2 O, add 30ml of distilled water, heat in a water bath at 50°C, stir at 450rpm to dissolve, add ammonia water dropwise until pH = 11, react for 1h, and obtain Fe 3 o 4 Liquid, adjust pH=6, let it stand for later use;

[0041] (2) Fe produced 3 o 4 The mass of 6.96g, according to TiO 2 / Fe 3 o 4 The mass ratio of = 3, weigh the nano-TiO with a solid content of 30% mass fraction 2 Colloidal solution (Hunan Titang Nano Technology Co., Ltd.) 69.6g, the primary particle size is 5nm, the surface potential is +38.6mV, dilute it into a 10% solution by mass fraction, heat the water bath to 80°C, and prepare in step (1) Slowly add the liquid into it, stir at 350rpm, and the stirring time is 3h, then centrifuge at 3500rpm, put it into a vacuum oven with a vacuum degree of -0.09MPa to dry at 80°C, and grind to obtain a magnetic Fe 3 o 4 / TiO 2 Composite samples.

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Abstract

The invention provides a Fe3O4 / TiO2 nano magnetic compound and a preparation method thereof. The preparation method comprises the following steps: (1), weighing ferric chloride hexahydrate and ferrous chloride tetrahydrate according to the molar ratio of (1.5 to 2.5) to 1 between ferric ions and ferrous ions, adding water, carrying out water bath at 50 to 60 DEG C; stirring for dissolving, and dripping ammonia water till the pH value of the liquid reactant is 10 to 11, so as to obtain Fe3O4 liquid; and (2) carrying out water bath on nano TiO2 colloidal solution till the temperature reaches 50 to 60 DEG C, adding the prepared Fe3O4 liquid into the nano TiO2 colloidal solution, stirring, carrying out centrifugal separation and vacuum drying, and grinding to obtain the Fe3O4 / TiO2 nano compound, wherein the solid mass ratio of TiO2 to Fe3O4 is (3 to 5) to 1. The method has the advantages that the process is concise; the operation is feasible; suitability for industrial production is obtained; a certain magnetic property is reserved; and requirements of practical application can be met.

Description

technical field [0001] The invention relates to a nano-magnetic composite body and a preparation method thereof, which belong to the technical field of magnetic nano-materials and also belong to the field of magnetic photocatalyst materials. Background technique [0002] Nanomagnetic iron oxide (also known as iron tetraoxide Fe 3 o 4 ) has a relatively high saturation magnetization, the prepared magnetic liquid has both the strong magnetism of a solid and the rheology of a liquid, and the fluidity and distribution can be oriented and positioned by an external magnetic field. Therefore, in printing, magnetic paper and anti-counterfeiting paper and other fields have potential applications. However, the appearance color of magnetic iron oxide is black, which limits its application range and application method to a certain extent. [0003] Nano-TiO 2 It has a huge specific surface area and positive charge, and the abundant hydroxyl groups on its surface make it easy to adsor...

Claims

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Application Information

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IPC IPC(8): B01J23/745H01F1/34
Inventor 陈小泉张洪鑫邓雪燕
Owner SOUTH CHINA UNIV OF TECH