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A kind of preparation method of the hollow silicon dioxide particle of a kind of shell

A technology of hollow silicon dioxide and silicon dioxide, applied in the direction of silicon dioxide, silicon oxide, nanotechnology for materials and surface science, etc., can solve the problems of harsh experimental techniques, waste of raw materials, unfavorable amplification applications, etc., to achieve Good monodispersity, simple and effective synthesis method, and controllable distance

Active Publication Date: 2020-02-14
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, their method wastes raw materials. In addition, the regulation of the co-hydrolysis of mixed silicon precursors also requires harsh experimental techniques. These are difficult to guarantee the batch quality of the product, and are not conducive to the scale-up application in large-scale production.

Method used

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  • A kind of preparation method of the hollow silicon dioxide particle of a kind of shell
  • A kind of preparation method of the hollow silicon dioxide particle of a kind of shell
  • A kind of preparation method of the hollow silicon dioxide particle of a kind of shell

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1: Preparation of a shell hollow silica particle

[0026] In the mixed solvent of 46.5mL propanol and water, the volume ratio of water and alcohol is 1:99 (V / V), first add 1mL, 0.2mol / L sodium hydroxide aqueous solution (the final concentration of sodium hydroxide is 4.0mmol / L), at a reaction temperature of 25°C and a stirring speed of 100rpm, add 2.5mL tetraethyl orthosilicate (the final concentration of TEOS is 0.22mol / L) at one time, and continue to stir at 25°C and 100rpm for 3 hours. Afterwards, after centrifuging to remove the supernatant, wash once with water, and then wash twice with propanol to prepare a layer of solid silica particles, the product quality is 0.13g.

[0027] Finally, disperse in 50mL water, the concentration of solid silica particles in water is 2.6mg / mL, heat at 80°C for 1 hour, and then centrifuge and purify the product to prepare a layer of hollow silica particles, such as figure 1 .

Embodiment 2

[0028] Example 2: Preparation of four-shell hollow silica particles

[0029] In the mixed solvent of 43.5mL propanol and water, the volume ratio of water and alcohol is 1:99 (V / V), firstly add 1mL, 0.2mol / L sodium hydroxide aqueous solution, at the reaction temperature of 25°C and the stirring speed of 100rpm 2.5 mL of tetraethyl orthosilicate (the final concentration of TEOS is 0.22 mol / L) was added at one time, and stirring was continued at 25° C. and 100 rpm for 3 hours. Afterwards, every interval reaction 3 hours, add the aqueous sodium hydroxide solution of 1mL, 0.3mol / L respectively again, add altogether 3 times, total reaction time is 12 hours (the final concentration after adding aqueous sodium hydroxide solution four times is 22mmol / L). Afterwards, after centrifuging to remove the supernatant, washing once with water and then twice with propanol, the solid silica particles coated with "layer-by-layer" were prepared, and the product mass was 0.57g.

[0030]Finally, d...

Embodiment 3

[0031] Example 3: Preparation of eight-shell hollow silica particles

[0032] In 34.5mL of mixed solvent of ethanol and water, the volume ratio of water and alcohol is 1:49 (V / V), firstly add 1mL, 0.1mol / L potassium hydroxide aqueous solution, when the reaction temperature is 25°C and the stirring speed is 100rpm , 7.5 mL of tetraethylorthosilicate (final concentration of TEOS: 0.66 mol / L) was added at one time, and stirring was continued at 25° C. and 100 rpm for 3 hours. Afterwards, at intervals of 3 hours, add 1mL, the concentrations are 0.15mol / L, 0.2mol / L, 0.25mol / L, 0.3mol / L, 0.35mol / L, 0.4mol / L and 0.5mol / L L of potassium hydroxide aqueous solution was added 7 times in total, and the total reaction time was 24 hours (the final concentration of potassium hydroxide aqueous solution after adding eight times was 45mmol / L). Afterwards, after centrifuging to remove the supernatant, washing once with water, and then washing twice with ethanol, the solid silica particles coate...

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Abstract

The invention discloses a method for preparing multi-shell hollow silica particles, and belongs to the technical field of preparation of nano-particles. The method comprises the following steps: adding an aqueous solution of a strong alkaline catalyst in a water and alcohol mixed solvent system at temperature of 20-50 DEG C in a speed of 100-500 rpm, and adding alkyl silicate; then adding the aqueous solution of the strong alkaline catalyst in 0-7 times, wherein the time interval between every two times of adding of the aqueous solution of the strong alkaline catalyst is 1 to 6 hours; centrifuging a reaction solution after the reaction is performed for 1 to 30 hours, removing supernatant, washing a centrifuged product first with water for 0 to 2 times, then washing the centrifuged productwith an alcohol solvent same as a used alcohol solvent for 0 to 3 times to prepare 'layer-layer''-coated solid silica particles; and pouring the ''layer-layer''-coated solid silica particles in waterfor heating incubation, centrifuging and purifying to obtain the multi-shell hollow silica particles with an adjustable number of shells and adjustable distance between the shells. The method for preparing the multi-shell hollow silica particles is simple and effective, the monodispersity is better, and the size, the number of the shells and the hollow distance between the shells are adjustable.

Description

technical field [0001] The invention belongs to the technical field of nanoparticle preparation, and in particular relates to a method for preparing hollow silicon dioxide particles with multiple shells. Background technique [0002] Hollow silica particles with multiple shells, because of their greater differential interface structure and multi-chamber environment, exhibit better physical and chemical properties in many fields, such as more controllable drug release effects, stronger Catalytic activity and more efficient energy conversion and storage capabilities, among others. Generally, the preparation method of multi-shell hollow silica particles mostly adopts the hard template method, that is, firstly, a solid structure covered by multi-shell layers is formed by "layer-layer" assembly growth technology, and then the "sacrificial layer" is removed by calcination or dissolution. The hollow structure particles with multiple shells are prepared. However, this type of meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12B82Y30/00
CPCB82Y30/00C01B33/12C01P2004/04C01P2004/34C01P2004/62
Inventor 韩延东杨文胜
Owner JILIN UNIV