Preparation method of hollow mesoporous silica nano microspheres

A technology of mesoporous silica and nano-microspheres, applied in the directions of silica, silica, nanotechnology, etc., can solve the problems of complex preparation method and serious agglomeration of hollow mesoporous nanospheres, and achieve simple and heavy-duty preparation methods. Good performance and good dispersion effect

Active Publication Date: 2020-06-05
NORTHWESTERN POLYTECHNICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

He (Guangdong Chemical Industry, Preparation of Hollow Mesoporous Silica Nanoparticles with Rough Surfaces for The hollow mesoporous nanospheres sy

Method used

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  • Preparation method of hollow mesoporous silica nano microspheres
  • Preparation method of hollow mesoporous silica nano microspheres
  • Preparation method of hollow mesoporous silica nano microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Add 10g of styrene and 1.5g of polypyrrolidone into 100mL of aqueous solution and stir thoroughly, then add 0.26g of 2,2'-azobis(2-methylpropylimidium) dihydrochloride to the above mixed solution , the process was protected by nitrogen and stirred at room temperature for 60 minutes, then the reaction temperature was raised to 70 ° C, and PS balls were obtained after 24 hours of reaction; the stirring rate was 100-200 r / min; the PS balls were washed three times with water and ethanol , dried under vacuum at 45°C.

[0028] (2) Add 0.3335 g of PS spheres to 45 mL of ethanol solution, and disperse by ultrasonic for 5-10 min, then transfer the mixed solution of PS spheres to a magnetic stirring device and start stirring; the ultrasonic power is 60W.

[0029] (3) Add 2g TEOs to the solution (2), and immediately add 2.4mL ammonia water, and heat in a water bath at 50°C for 3h to obtain PS@SiO 2 nanospheres; resulting PS@SiO 2 The nano-microspheres are washed three times ...

Embodiment 2

[0033] (1) Add 10g styrene and 1.5g polypyrrolidone into 100mL aqueous solution and stir thoroughly, then add 0.26g of 2,2'-azobis(2-methylpropylimidium) dihydrochloride to the above mixed solution , the process was protected by nitrogen and stirred at room temperature for 60 minutes, then the reaction temperature was raised to 70 ° C, and PS balls were obtained after 24 hours of reaction; the stirring rate was 100-200 r / min; the PS balls were washed three times with water and ethanol , dried under vacuum at 45°C.

[0034] (2) Add 0.3335 g of PS spheres to 45 mL of ethanol solution, and disperse by ultrasonic for 5-10 min, then transfer the mixed solution of PS spheres to a magnetic stirring device and start stirring; the ultrasonic power is 60W.

[0035] (3) Add 1.2g of TEOs to (2) solution, and immediately add 5.6mL of ammonia water, and heat in a water bath at 50°C for 1.5h to obtain PS@SiO 2 nanospheres; resulting PS@SiO 2 The nano-microspheres are washed three times wit...

Embodiment 3

[0039] (1) Add 10g styrene and 1.5g polypyrrolidone into 100mL aqueous solution and stir thoroughly, then add 0.26g of 2,2'-azobis(2-methylpropylimidium) dihydrochloride to the above mixed solution , the process was protected by nitrogen and stirred at room temperature for 60 minutes, then the reaction temperature was raised to 70 ° C, and PS balls were obtained after 24 hours of reaction; the stirring rate was 100-200 r / min; the PS balls were washed three times with water and ethanol , dried under vacuum at 45°C.

[0040] (2) Add 0.3335 g of PS spheres to 45 mL of ethanol solution, and disperse by ultrasonic for 5-10 min, then transfer the mixed solution of PS spheres to a magnetic stirring device and start stirring; the ultrasonic power is 60W.

[0041] (3) Add 1 g of TEOs to the solution (2), and immediately add 2.24 mL of ammonia water, and heat in a water bath at 50 °C for 1.5 h to obtain PS@SiO 2 nanospheres; resulting PS@SiO 2 The nano-microspheres are washed three ti...

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Abstract

The invention relates to a preparation method of hollow mesoporous silica nano microspheres, which comprises the following steps: by using polystyrene microspheres (PS microspheres) with positive cations on the surfaces as a template and tetraethoxysilane (TEOs) as a silicon source, reacting in an alkaline environment to obtain silica-coated polystyrene microspheres (PS@SiO2); and calcining the obtained PS@SiO2 nano-microsphere to obtain the hollow silicon dioxide nano-microsphere with the mesoporous structure. According to the preparation method disclosed by the invention, the hollow mesoporous silicon dioxide spheres with the shell thickness of 8-40 nm can be obtained by only adjusting the addition amount of tetraethoxysilane (TEOs) without adding a surfactant and other pore-foaming agents. The method has the advantages of simple preparation method, good reproducibility (repeated experiments for at least 50 times), low cost (low drug price) and the like. The obtained hollow mesoporous silica nanospheres have the characteristics of good dispersibility, large specific surface area, small shell thickness, uniform size and the like.

Description

technical field [0001] The invention belongs to the technical field of controllable synthesis of nanomaterials, and relates to a method for preparing hollow mesoporous silicon dioxide nanometer microspheres. Background technique [0002] Hollow mesoporous materials have attracted widespread attention of researchers because of their high specific surface area, large pore volume, uniform and orderly mesoporous structure, and abundant synthetic raw materials. In recent years, a hollow mesoporous silica nanomaterial has been developed. In addition to the main characteristics of the hollow and mesoporous structure, the material also has good biocompatibility, easy chemical modification of the surface, low synthesis cost, and high immobilization capacity. Many advantages. Hollow mesoporous silica nanospheres have extremely important application value in biological drug loading, adsorption separation and energy catalysis. [0003] In recent years, due to the broad application pro...

Claims

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Application Information

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IPC IPC(8): C01B33/18B82Y30/00B82Y40/00
CPCC01B33/18B82Y40/00B82Y30/00C01P2004/03C01P2004/04C01P2004/62C01P2004/64C01P2006/16C01P2006/12C01P2004/34
Inventor 胡小玲闫超仁管萍舒琪牛辉哲丁敏玲黄彤彤侯彤彤
Owner NORTHWESTERN POLYTECHNICAL UNIV
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