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Method for preparing functional multi-particle size monodisperse silicon dioxide spherical material

A silicon dioxide, monodisperse technology, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of large pore size variation of silicon dioxide microspheres, difficult to control batch stability, and high technical requirements, to reduce the calcination process, The effect of good shape and strong controllability of pore size

Active Publication Date: 2018-11-27
南京亘闪生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high technical requirements and cumbersome process. Firstly, porous polymer microspheres with monodisperse particle size must be prepared as a template to prepare silica spherical fillers; and the controllability of the calcination process is poor. If the polymer calcination is not Complete or insufficient, the pore size of silica microspheres varies greatly, and batch stability is difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Seed Preparation: Preparation of Monodisperse Polymer Seeds by Suspension Polymerization

[0028] Weigh 160mL of ethanol and 20mL of ultrapure water and add them to a 500 ml round-bottomed flask. The reaction bottle is equipped with a reflux condenser, mechanical stirring, and N 2 Ventilation duct and thermometer, add 2.5g of seeds, add 2.0g of dispersant PVP and 1.0g of auxiliary dispersant lauryl alcohol, stir evenly at a speed of 250 rpm, feed nitrogen for 10-20min, and raise the temperature of the system to 60°C; Get 1.0g of dodecanethiol, 0.14g of azobisisobutyronitrile (AIBN) dissolved in 20g of styrene, and join in the above-mentioned round bottom flask; after insulation reaction for 20h, monodisperse polymer seed liquid is obtained, After cleaning, test the molecular weight of the seeds Mn=3284, and the particle size is 3.1 μm.

Embodiment 2

[0030] Seed Preparation: Preparation of Monodisperse Polymer Seeds by Suspension Polymerization

[0031] Weigh 160mL of ethanol and 20mL of ultrapure water and add them to a 500 ml round-bottomed flask. The reaction bottle is equipped with a reflux condenser, mechanical stirring, and N 2 Ventilation duct and thermometer, add 2.5g of seeds, add 2.0g of dispersant PVP and 1.0g of auxiliary dispersant dodecyl alcohol, stir evenly at a speed of 160 rpm, feed nitrogen for 10-20min, and heat up the system to 60°C; Get 0.6g of dodecyl mercaptan, 0.05g of azobisisobutyronitrile (AIBN) dissolved in 20g of styrene, and join in the above-mentioned round bottom flask; after insulation reaction for 20h, monodisperse polymer seed liquid is obtained, After cleaning, test the molecular weight of the seeds Mn=18391, and the particle size is 5.0 μm.

Embodiment 3

[0033] Seed Preparation: Preparation of Monodisperse Polymer Seeds by Swelling Method

[0034] Weigh 2.5g of seeds in a 250 mL round bottom flask; weigh 0.11g of AIBN, 20g of styrene, 0.4g of dodecanethiol, 0.1g of SDS, and 20mL of ultrapure water in a 100mL beaker, emulsify to particle size Add an emulsion of about 10 μm into the above-mentioned round bottom flask, heat up to 60°C, and keep it warm for 3 hours; add 0.5g PEG4000 / 40g ultrapure aqueous solution, and react at 80°C for 20 hours to obtain a monodisperse polymer seed solution. After cleaning, test The molecular weight of the seed is Mn=10448, and the particle size is 10.3 μm.

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Abstract

The invention relates to a method for preparing a functional multi-particle size monodisperse silicon dioxide spherical material. The method specifically comprises the following steps: (1) preparing seeds, namely preparing monodisperse polymer seeds; (2) swelling, namely mixing silicate ester M1, silicate ester M2 and an emulsifier, uniformly emulsifying, adding the monodisperse polymer seeds after reactions in the step (1), and carrying out swelling; (3) polymerizing, namely putting a polymerization agent into the solution obtained after reactions in the step (2), and heating to carry out polymerization; and (4) cleaning, namely removing the excessive solution after the reactions are completed, and cleaning with a detergent, thereby obtaining the monodisperse silicon dioxide spherical material. By adopting the method, the swellable particle-size monodisperse polymer seeds are adopted as a template, the preparation process is simple, the prepared porous silicon dioxide spherical material is good in morphology and has a monodisperse particle size, and compared with a conventional reported process, a calcining process is reduced, and the prepared monodisperse silicon dioxide spherical material is good in porosity controllability.

Description

technical field [0001] The invention belongs to the field of liquid chromatography packing preparation technology and application thereof, and in particular relates to a preparation method of a functionalized porous particle size monodisperse silica spherical material. Background technique [0002] Chromatography packings can be divided into organic matrix packings, inorganic matrix packings and polysaccharide matrix packings according to different matrices. Among them, silica gel packing in inorganic matrix packings has high mechanical strength, heat resistance, organic solvent resistance, stable performance and easy surface Modification and other characteristics make it one of the most widely used chromatographic packing materials. [0003] In 1956, G.Kolber (G.Kolbe, The complex chemical behavior of silica[D].Thesis, Friedrich schillr Universitat Jena, 1965) and others used the method of hydrolysis and condensation of tetraethyl orthosilicate in ethanol solution to obtain...

Claims

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Application Information

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IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/32C01P2004/52C01P2004/61C01P2006/80
Inventor 仲玉任连兵
Owner 南京亘闪生物科技有限公司
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