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Preparation method of magnetic nano ferroferric oxide modified hollow glass microsphere

A hollow glass microbead, ferric oxide technology, applied in chemical instruments and methods, other chemical processes, dyeing organosilicon compound treatment, etc. Weak problems, to achieve the effect of saving raw materials, easy operation, high saturation magnetization

Active Publication Date: 2013-03-27
JIAXING HENENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved by the present invention is to propose a method for preparing magnetic nano ferric oxide modified hollow glass microspheres which saves raw materials and is easy to operate. It uses a hydrothermal method to modify the surface of the hollow glass microspheres, solving the problem of The hollow glass microspheres in the existing modification methods have problems such as no magnetism, poor coating fastness and weak magnetism

Method used

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preparation example Construction

[0012] The invention discloses a method for preparing magnetic nanometer iron ferric oxide modified hollow glass microspheres, which uses a hydrothermal method to directly modify the surface of the hollow glass microspheres while preparing magnetic nanometer ferric oxide particles, specifically Include the following implementation steps:

[0013] Step 1: Take sodium hydroxide, sodium carbonate and sodium silicate and dissolve them in deionized water to obtain a degreasing solution. The mass-volume concentration of sodium hydroxide, sodium carbonate and sodium silicate in the degreasing solution is 40g / L, 10g / L and 5g / L; heat the degreasing solution to 80-100°C; weigh 5-10g of hollow glass microspheres, add them to the above 1L degreasing solution, and use mechanical stirring to make the hollow microspheres Fully disperse in the degreasing liquid, filter and wash with water after reacting for 40-60 minutes. (Taking 1L degreasing solution as an example, the following preparati...

Embodiment 1

[0019] Take 5g of hollow glass microspheres, add them to 1L of degreasing solution, treat at 80°C for 40min, then filter and wash with water. Treat the hollow microspheres with a hydrofluoric acid solution with a mass concentration of 1% and a volume of 1 L at 40°C for 1 hour, and dry the hollow glass microspheres after washing with water at 120°C for 2 hours. The etched hollow microspheres were immersed in 10 mL / L aminopropyltriethoxysilane absolute ethanol aqueous solution, treated at 10 °C for 2 h, filtered, washed, and dried at 80 °C for 30 min, 110 Bake at ℃ for 5 min. The hollow microspheres after coupling modification were immersed in low molecular weight chitosan solution, treated at 60°C for 30min, filtered, prebaked at 90°C for 20min, and baked at 150°C for 5min, and then used Soak in 1mol / L sodium hydroxide solution for 10 minutes, filter and wash with water. Weigh a certain amount of ferrous chloride and ferric chloride, dissolve them in deionized water, control ...

Embodiment 2

[0021] Take 10g of hollow glass microspheres, add them to 1L of degreasing solution, treat at 100°C for 60min, then filter and wash with water. Treat the hollow microspheres with a hydrofluoric acid solution with a mass concentration of 3% and a volume of 1L at 60°C for 2h, and dry the hollow glass microspheres after washing at 120°C for 4h. The etched hollow microspheres were immersed in 20 mL / L aminopropyltriethoxysilane absolute ethanol aqueous solution, treated at 20 °C for 4 h, filtered, washed, and dried at 80 °C for 60 min, 110 Bake at ℃ for 10 minutes. The hollow microspheres after coupling modification were immersed in low molecular weight chitosan solution, treated at 60°C for 60min, filtered, prebaked at 90°C for 40min, and baked at 150°C for 10min, and then used Soak in 1mol / L sodium hydroxide solution for 30min, filter and wash with water. Weigh a certain amount of ferrous chloride and ferric chloride, dissolve them in deionized water, control the total iron con...

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Abstract

The invention discloses a preparation method of a magnetic nano ferroferric oxide modified hollow glass microsphere. The method comprises the steps of removing oil of a hollow glass microsphere; soaking the hollow glass microsphere with oil removed in a coarsening solution to react, filtering and subsequently washing, and drying; dipping the hollow glass microsphere in a coupling agent solution to react, filtering and subsequently washing, drying and baking; dipping the hollow glass microsphere in a chitosan solution, stirring and filtering, subsequently prebaking and baking; soaking the dried hollow glass microsphere in a sodium hydroxide solution, filtering and then washing; and finally dipping the hollow glass microsphere in a ferrous chloride mixture solution, transferring to a high-pressure reaction kettle, sealing and then carrying out insulation treatment, and filtering the hollow glass microsphere after finishing reacting; and washing respectively by using absolute ethyl alcohol and deionized water and drying. The preparation method saves the raw material and is easy and simple to operate; through the modification on the surface of the hollow glass microsphere, the problems of no magnetism, poor coating fastness, weak magnetism and the like of the hollow glass microsphere are solved.

Description

technical field [0001] The invention belongs to the technical field of functional inorganic non-metallic materials, and relates to a method for modifying hollow glass microspheres, in particular to a method for preparing magnetic nanometer iron tetraoxide-modified hollow glass microspheres. Background technique [0002] Ferric oxide (Fe 3 o 4 ) is an important spinel-like ferrite material, which has many optical, electrical, acoustic, thermal and magnetic properties different from conventional materials, and is one of the most widely used soft magnetic materials, often used as recording materials, Pigments, magnetic fluid materials, catalysts, magnetic polymer microspheres and electronic materials also have good application prospects in the fields of biotechnology and medicine. At present, the methods for preparing magnetic nano-Fe3O4 particles mainly include chemical precipitation method, sol-gel method, microwave radiation method and hydrothermal reaction method. Nano-F...

Claims

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Application Information

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IPC IPC(8): C09C1/28C09C3/06C09C3/12C09C3/10C09K3/00
Inventor 詹建朝张辉
Owner JIAXING HENENG TECH CO LTD
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