Preparation method of monodisperse porous inorganic microsphere

A monodisperse, microsphere technology, applied in the field of monodisperse porous inorganic microspheres and their preparation, can solve problems such as wide particle size distribution, and achieve the effects of controllable pore size, low price and simple preparation process

Inactive Publication Date: 2011-07-27
PEKING UNIV SHENZHEN GRADUATE SCHOOL +1
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Problems solved by technology

[0004] Chinese patent (CN1124715) discloses a method for preparing porous silica microspheres, that is, using the cell wall or cell membrane of biological cells as a template, adding silicate compounds and porogens, and dispersing them in the aqueous phase system In this process, porous silica microspheres with a particle size of 1-200 microns are prepared through two-stage hydrolysis condensation and gelation reactions, but the particle size distribution is wide
However, the size of the porous inorganic microspheres finally obtained by this method is 20-50% smaller than that of the original template microspheres, and the yield is only about 40%.

Method used

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  • Preparation method of monodisperse porous inorganic microsphere
  • Preparation method of monodisperse porous inorganic microsphere
  • Preparation method of monodisperse porous inorganic microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 3.68g of porous polyglycidyl methacrylate / ethylene glycol dimethacrylate [P(GMA / EGDMA)] copolymerized microspheres (5μm) in a 250mL three-necked bottle, add 120mL of water, and ultrasonicate for 20min to make the balls completely Spread out. Then 4g of ethylenediamine (EDA) was added, and the reaction was heated at 80°C for 12h. The obtained microspheres were repeatedly washed with water, and then washed with ethanol several times, and dried in a vacuum oven at 50°C.

Embodiment 2

[0037] Take 4.0g of porous P(GMA / EGDMA) microspheres (10μm) in a 250mL three-necked bottle, add 120mL of water, and disperse the balls completely by ultrasonication for 20min. Then 5g of ammonia water was added, and the reaction was heated at 80°C for 12h. The obtained microspheres were repeatedly washed with water, and then washed with ethanol several times, and dried in a vacuum oven at 50°C.

[0038] 2. Synthesis of porous silica microspheres:

Embodiment 3

[0040] Take 0.2 g of the porous microspheres of Example 1 in a 500 mL three-neck flask, add 40 mL of deionized water, 200 mL of isopropanol, 0.5 mL of tetrabutylammonium bromide and 1 mL of 28% ammonia water, and then sonicate for 10 min. 5 mL of isopropanol solution containing 10% tetraethyl orthosilicate (TEOS) was added dropwise into the reaction system within 1 h, and reacted at room temperature for 24 h. The obtained polymer / silica composite microspheres were repeatedly washed with ethanol and acetone, and then dried in a vacuum oven at 50°C. The dried polymer / silica composite microspheres were placed in a muffle furnace, and the temperature was raised to 600°C step by step, and kept at this temperature for 6 hours to burn, and finally 5 μm porous silica microspheres were obtained.

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PUM

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Abstract

The invention provides a preparation method of a monodisperse porous inorganic microsphere. Functionalized porous polymer microspheres are used as templates; the hydrolysis condensation reaction of an inorganic precursor is controlled to perform in the pores of the microspheres so as to prepare polymer / inorganic substance composite microspheres; and the templates are removed to obtain porous inorganic microspheres. The porous inorganic microspheres provided by the invention has the same size as the templates with no size reduction phenomenon, and the yield is up to above 98%; the inorganic microspheres have stable chemical properties and high mechanical strength, and have potential application value to the fields of chromatography, bioseparation, wastewater treatment, catalyst carrier, immobilized enzyme, etc.

Description

technical field [0001] The invention relates to the technical field of inorganic microsphere materials, in particular to a monodisperse porous inorganic microsphere and a preparation method thereof. Background technique [0002] Due to their high mechanical strength, heat resistance, solvent resistance, easy surface functional modification and biocompatibility, porous inorganic microspheres have been used in catalyst carriers, immobilized enzymes, wastewater treatment, high performance liquid chromatography, etc. There are attractive application prospects in the application field. In order to meet the application requirements in the above fields, the size of the inorganic microspheres is required to be controlled between 1 and 10 microns, and the particle size distribution is uniform, and the microspheres are also required to have a controllable pore size distribution. At present, monodisperse inorganic microspheres with tens to hundreds of nanometers can be prepared by tra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
Inventor 阳承利何洁张以梅吴俊成江必旺陈荣姬
Owner PEKING UNIV SHENZHEN GRADUATE SCHOOL
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