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Metal-doped hollow silicon dioxide microsphere and preparation method and application thereof

A hollow silica, metal-doped technology, applied in the preparation of microspheres, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc. High-level problems, to achieve the effect of maintaining uniformity, uniform particle size distribution, and ensuring the uniformity of particle size distribution

Active Publication Date: 2020-04-17
NANJING UNIV YANCHENG ENVIRONMENTAL PROTECTION TECH & ENG RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problems of easy collapse and uneven particle size in the preparation process of existing hollow silica microspheres, the present invention provides a metal-doped hollow silica microsphere with uniform particle size and a preparation method thereof. By adjusting the order of adding raw materials and Control the synthesis conditions to ensure that metal-doped hollow silica microspheres with firm skeleton and uniform particle size are obtained;
[0008] Aiming at the problem of low catalytic efficiency of existing ozone heterogeneous catalysts, the present invention provides a metal-doped hollow silica microsphere with a micro-nano size, which can increase organic molecules and catalyst active sites in its confinement cavity. Effective collision probability between points and ozone molecules, thus greatly improving the efficiency of ozone catalytic oxidation

Method used

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  • Metal-doped hollow silicon dioxide microsphere and preparation method and application thereof
  • Metal-doped hollow silicon dioxide microsphere and preparation method and application thereof
  • Metal-doped hollow silicon dioxide microsphere and preparation method and application thereof

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Embodiment 1

[0042] Its preparation method of metal-doped hollow silica microspheres in the present embodiment comprises the following steps:

[0043](1) Prepare an inverse microemulsion system: Mix cyclohexane, Triton X-100, n-hexanol and deionized water and stir vigorously at a speed of 600rpm for 1.5h;

[0044] (2) Add tetraethyl orthosilicate and an ethanol solution of 3-aminopropyltrimethoxysilane (APTMS) with a concentration of 0.5 μmol / L to the inverse microemulsion system, and then vigorously stir at a speed of 600 rpm for 3 h; Add concentrated ammonia water (mass concentration is 28%) subsequently and react 10h with the rotating speed of 150rpm, obtain such as figure 1 Undoped silica microspheres with uniform particle size distribution shown;

[0045] Ensure that the volume ratio of cyclohexane, Triton X-100, n-hexanol, deionized water, tetraethylorthosilicate, 3-aminopropyltrimethoxysilane (APTMS) in ethanol and concentrated ammonia water is 125:30: 5:5:1:0.25:2.5.

[0046] (3...

Embodiment 2

[0057] Its preparation method of metal-doped hollow silica microspheres in the present embodiment comprises the following steps:

[0058] (1) Prepare an inverse microemulsion system: Mix cyclohexane, Triton X-100, n-hexanol and deionized water and stir vigorously at a speed of 700rpm for 3h;

[0059] (2) Add tetraethyl orthosilicate and an ethanol solution of 3-aminopropyltrimethoxysilane (APTMS) with a concentration of 0.6 μmol / L to the inverse microemulsion system, and then vigorously stir at a speed of 700 rpm for 5 h; Then add concentrated ammonia water (mass concentration: 29%) and stir at a speed of 200 rpm for 15 hours to obtain undoped silica microspheres with uniform particle size distribution;

[0060] Ensure that the volume ratio of cyclohexane, Triton X-100, n-hexanol, deionized water, tetraethylorthosilicate, 3-aminopropyltrimethoxysilane (APTMS) in ethanol and concentrated ammonia water is 125:30: 5:15:5:0.25:2.5.

[0061] (3) Centrifuge after mixing undoped si...

Embodiment 3

[0072] Its preparation method of metal-doped hollow silica microspheres in the present embodiment comprises the following steps:

[0073] (1) Prepare an inverse microemulsion system: Mix cyclohexane, Triton X-100, n-hexanol and deionized water and stir vigorously at a speed of 800 rpm for 3 hours;

[0074] (2) Add tetraethyl orthosilicate and the ethanol solution of 3-aminopropyltrimethoxysilane (APTMS) with a concentration of 1 μmol / L to the inverse microemulsion system, then vigorously stir at a speed of 800 rpm for 5 h; then Add concentrated ammonia water (mass concentration: 30%) and stir at a speed of 250 rpm for 15 hours to obtain undoped silica microspheres with uniform particle size distribution;

[0075] Ensure that the volume ratio of cyclohexane, Triton X-100, n-hexanol, deionized water, tetraethylorthosilicate, 3-aminopropyltrimethoxysilane (APTMS) in ethanol and concentrated ammonia water is 125:30: 5:15:5:0.25:2.5.

[0076] (3) Centrifuge after mixing undoped s...

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Abstract

The invention discloses a metal-doped hollow silicon dioxide microsphere and a preparation method and application thereof, belonging to the technical field of material preparation. The preparation method comprises the following steps: firstly, preparing undoped silicon dioxide microspheres by adopting a reversed-phase microemulsion method; then, adding the undoped silicon dioxide microspheres intoa mixed solution of an inorganic salt containing Mn, Cu and Ce, and conducting hydrothermal treatment so as to obtain a metal doped silicon dioxide microsphere; and finally, carrying out water bath treatment on the metal-doped silicon dioxide microsphere to obtain the metal-doped hollow silicon dioxide microsphere. According to the invention, the metal-doped hollow silicon dioxide microsphere with a firm skeleton and uniform granularity are obtained by adjusting the adding sequence of raw materials and controlling the synthesis conditions.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and more specifically relates to a metal-doped hollow silica microsphere and its preparation method and application. Background technique [0002] Ozone has the advantages of high treatment efficiency, complete oxidation and no secondary pollution in water treatment, and has been widely concerned in the treatment of industrial wastewater. Single ozone oxidation wastewater has low ozone utilization rate and limited treatment effect, while ozone catalytic oxidation technology can significantly improve ozone utilization rate and wastewater treatment effect. It is an efficient and green sewage treatment technology. In recent years, ozone catalytic oxidation has become the field of industrial sewage treatment research hotspots. The catalyst is added to make the conditions of ozone oxidation no longer tend to be strict, and can accelerate the decomposition of ozone and improve the efficie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02B01J23/889B01J35/02B01J35/08B01J35/10C02F1/72B01J35/00
CPCB01J13/02B01J23/8892B01J21/08C02F1/78C02F1/725B01J35/40B01J35/51B01J35/61
Inventor 赵选英刘君君杨峰程夫苓王智宁巫先坤戴建军
Owner NANJING UNIV YANCHENG ENVIRONMENTAL PROTECTION TECH & ENG RES INST
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