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Method for producing magnetic hollow silicon dioxide particle

A technology of hollow silica and silica, applied in the direction of microsphere preparation, microcapsule preparation, etc., can solve the problem of affecting the stability of the emulsion, the size of the dispersed phase, the type of emulsion, the magnetic properties of the product that affects the stability of the emulsion, and it is not suitable for magnetic hollow Particles and other problems, it is not easy to achieve magnetic properties, low cost, and avoid changes in magnetic properties

Inactive Publication Date: 2008-06-11
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

This method expands the type and scope of the hollow particle product prepared by the Pickering emulsion method, but it is still not suitable for the preparation of magnetic hollow particles. 1) the nanoparticles used in this method are powdered nanoparticles prepared in advance. Particles, dry magnetic particles are easy to agglomerate and difficult to disperse, and the change of particle size will affect the stability of the emulsion and the magnetic properties of the product; 2) The temperature of the emulsion preparation is low and the reaction temperature is high, and the temperature change will seriously affect the stability of the emulsion 3) In addition, the type of Pickering emulsion (oil-in-water or water-in-oil) is determined by powdery nanoparticles with certain hydrophilic or lipophilic properties, which is not easy to adjust

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  • Method for producing magnetic hollow silicon dioxide particle
  • Method for producing magnetic hollow silicon dioxide particle
  • Method for producing magnetic hollow silicon dioxide particle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Slowly add 80 mL of NaOH solution with a concentration of 0.5 mol / L to 50 mL of FeCl containing 0.1 mol / L 2 and 0.2mol / L FeCl 3 In the mixed aqueous solution, stir vigorously, and the pH is controlled between 10-11 to obtain superparamagnetic nano-Fe 3 o 4 The suspension was stirred at 30°C for 30min. Observation of Fe by TEM 3 o 4 The particle size is 8-10nm, and the dispersion is good. The test results of the vibrating sample magnetometer show that the nano-Fe 3 o 4 The particles are superparamagnetic. Add 10ml of cyclohexane to the suspension, and emulsify with a high-speed mixer for 10 minutes to obtain a black oil-in-water emulsion. Take a drop of the emulsion and drop it on a slide, and observe it with an optical microscope. The size of the emulsion droplet is 0.6-2 μm.

[0022] 2) Mix 18.6g TEOS, 3.45g ethanol and 1.8g deionized water, and stir magnetically at 30°C for 21h to obtain SiO 2 Water sol, adding the water sol to the emulsion prepared in step...

Embodiment 2

[0024] 1) Slowly add 80 mL of NaOH solution with a concentration of 0.5 mol / L to 50 mL of FeCl containing 0.1 mol / L 2 and 0.2mol / LFeCl3 In the mixed aqueous solution, stir vigorously, and the pH is controlled between 10-11 to obtain superparamagnetic nano-Fe 3 o 4 The suspension was stirred at 30°C for 30min. Add 10ml of cyclohexane to the suspension, and emulsify with an ultrasonic cell pulverizer for 5 minutes to obtain a black oil-in-water emulsion. Take a drop of the emulsion and drop it on a slide, and observe it with an optical microscope. The droplet size is 0.3-1.2 μm, and the liquid There is a layer of nano-Fe on the surface of the droplet 3 o 4 Particles form a solid film.

[0025] 2) Same as step 2 of Example 1. Finally, a superparamagnetic Fe with a diameter of 580 nm and a shell thickness of 41 nm was obtained 3 o 4 / SiO 2 Composite hollow microspheres.

Embodiment 3

[0027] 1) Slowly add 80 mL of NaOH solution with a concentration of 0.5 mol / L to 50 mL of FeCl containing 0.1 mol / L 2 and 0.2mol / LFeCl 3 In the mixed aqueous solution, stir vigorously, and the pH is controlled between 10-11 to obtain superparamagnetic nano-Fe 3 o 4 The suspension was stirred at 30°C for 30min. Add 10ml of cyclohexane to the suspension, and emulsify for 5 minutes with a high-gravity rotating bed to obtain a black oil-in-water emulsion. Take a drop of the emulsion and drop it on a slide, and observe it with an optical microscope. The droplet size is 0.1-0.5nm.

[0028] 2) Same as step 2 of Example 1. Finally, a superparamagnetic Fe with a diameter of 380 nm and a shell thickness of 40 nm was obtained 3 o 4 / SiO 2 Composite hollow microsphere particles.

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Abstract

The invention relates to a process for preparing magnetic hollow silicon dioxide particles, wherein alkaline water solution is filled into the mixed solution of divalent ferric salt and trivalent ferric salt, suspending liquid which is generated by the reaction with magnetic ferrite nanometer particles and electrolytic solution is filled with oil dissolvent, the volume ratio of the oil dissolvent and the electrolytic solution is 0.05-50, and stable emulsion of ferrite particles is scattered and mixed and is prepared. Silicon source or silicon dioxide water collosol is directly filled into the emulsion which is prepared, which reacts under the normal temperature, and the PH value is regulated to 3.9, silicon dioxide precursors generates controllable chemical reaction in the system to prepare magnetic hollow silicon dioxide particles. The invention synthesizes magnetic hollow silicon dioxide particles by one step, which avoids changes of agglomeration and magnetic performance of nanometer magnetic particles, the invention utilizes the electrolytic solution which is generated during the process of preparing the magnetic ferrite, and leads the particles to reach hydrophilic-lipophilic balance at oil-water interface, and has the advantages of simple artistic process, low cost and low reacting temperature, and avoids affect to the magnetic performance of the particles.

Description

technical field [0001] The invention relates to a method for preparing magnetic hollow silicon dioxide particles, in particular to a method for preparing magnetic hollow silicon dioxide particles by using an emulsion stabilized by magnetic nanoparticles as a template (Pickering emulsion method). Background technique [0002] Magnetic hollow silica particles are a recognized adsorbent and adsorbent carrier, not only has the characteristics of light weight, high specific surface area and strong adsorption capacity, but also can be easily separated from the suspension under an external magnetic field, and removed When exposed to an external magnetic field, these particles do not show any remanence, and can be widely used in high-tech fields such as cell separation, magnetic enzyme immunoassay, drug controlled release carrier and hydrogen storage materials, so they are highly valued by researchers. The most commonly used method for preparing magnetic hollow microspheres is templ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02C04B35/622C04B35/14
Inventor 毋伟沈淑玲郭锴陈建峰
Owner BEIJING UNIV OF CHEM TECH
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