Preparation method of silicon dioxide@porous polymer core-shell microspheres with macroporous structure

A technology of silica and core-shell microspheres, which is applied in the fields of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve problems such as limited application and narrow application range of silanol, and achieve easy Control and amplification, expansion of acid and alkali resistance, easy surface modification and modification

Inactive Publication Date: 2018-07-24
NORTHWEST UNIV(CN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has defects such as a narrow pH application range (2.0-8.0) and residual silanol on the surface, which limits its further application, especially in the separation and analysis of basic proteins.

Method used

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  • Preparation method of silicon dioxide@porous polymer core-shell microspheres with macroporous structure
  • Preparation method of silicon dioxide@porous polymer core-shell microspheres with macroporous structure
  • Preparation method of silicon dioxide@porous polymer core-shell microspheres with macroporous structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation method of silica@porous polymer core-shell microspheres comprises the following steps (such as figure 1 ):

[0027] (1) Preparation of non-porous silica microspheres

[0028] First, add 200-300mL of absolute ethanol, appropriate amount of water, ammonia water, and appropriate amount of electrolyte potassium chloride into a clean three-necked bottle, ultrasonically disperse evenly, and stir at room temperature for 30 minutes. Then add an appropriate amount of TEOS dropwise into the above mixed solution, dilute TEOS with absolute ethanol, and the dilution concentration of TEOS is 5-50%. After the dropwise addition, keep the reaction conditions unchanged and continue the reaction for 3h. After the reaction is over, first centrifuge with a centrifuge, 3000r / min for 5 minutes, and use G 5 filter with a glass sand core funnel, wash with distilled water until neutral, then wash with absolute ethanol, and dry in a vacuum oven at 50°C for 12h.

[0029] (2) Su...

Embodiment 2

[0034] (1) Preparation of solid silica microspheres

[0035] According to reference [H. Nakabayashi, A. Yamada, M. Noba, Y. Kobayashi, M. Konno, D. Nagao, Langmuir 26 (2010) 7512-7515] preparation of micron-sized silica solid microspheres, a typical method For: Preparation of liquid A: Take a clean reagent bottle, add 200-300 mL of absolute ethanol, appropriate amount of water, ammonia water and appropriate amount of electrolyte to make a 300 mL mixed solution, and ultrasonicate for 10 min for later use.

[0036] Preparation of solution B: add an appropriate amount of TEOS and a certain amount of absolute ethanol to make a diluted solution, and ultrasonically for 10 min for later use.

[0037] Add liquid A to a 1000 mL three-necked flask, slowly add liquid B dropwise at a controlled rate within 0.8 mL / min, and react at a certain temperature at a certain stirring speed. After the addition of TEOS is completed, keep the reaction conditions unchanged and continue Reaction 3h.

...

example 2

[0044] Take 0.9 g of modified silica gel microspheres in Example 2, add 60 mL of 0.15% SDS for ultrasonic dispersion for 20 min, then add 30 mL of 5% PVA for ultrasonic dispersion for 10 min, and stir at a medium speed at 30 °C. Next, disperse 0.05 g of BPO, 0.9 mL of GMA, 0.9 mL of EDMA, and 1.8 mL of butyl levulinate into a mixed solution of 20 mL of SDS and 10 mL of PVA, and ultrasonically emulsify until uniformly dispersed. Then add the dispersed monomer mixed solution dropwise into the silica gel suspension solution at low rotational speed. React at 30°C for 6 hours. Then pass nitrogen gas for 30 minutes, raise the temperature to 70°C, and continue the reaction for 12 hours. The obtained product is centrifuged three times at 2000 rpm with deionized water, and then washed with a large amount of hot water until the filtrate has no foam, and finally washed once with absolute ethanol. Dry overnight at 60°C. The morphology and pore size distribution of the microspheres are c...

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Abstract

The invention discloses a novel method for preparing macroporous silicon dioxide@porous polymer core-shell microspheres. Non-porous silica microspheres are used as a core, octadecyltrichlorosilane isused for performing the surface hydrophobic modification, PVA and SDS are used as a dispersing agent, monomers GMA, a cross-linking agent EDMA and a pore forming agent are added to prepare the silicondioxide@porous polymer core-shell microspheres with a macroporous structure through an emulsion polymerization process. The preparation method is simple in preparation process, mild in conditions, and easy in mass production; and the surface of the prepared core-shell microspheres is a porous organic polymer which has higher acid and alkali resistance, the application range of core-shell fillersis enlarged, a larger aperture structure can be obtained, and the prepared core-shell microspheres are particularly suitable for the isolated analysis of biological molecules.

Description

technical field [0001] The invention relates to a method for preparing silica@porous polymer core-shell microspheres with a macroporous structure, and belongs to the technical field of chromatographic medium preparation. Background technique [0002] Core-shell packing is considered to be a real substitute for fully porous silica packing due to its superior performance of high column efficiency, high resolution and low back pressure, especially suitable for high-efficiency and fast chromatographic separation of new samples and complex samples, and is an ideal choice for ultrafast HPLC analysis ideal tool. Chromatographic separation materials are the core of chromatographic development, and the preparation of monodisperse core-shell microspheres with controllable shell thickness and pore size is one of the hotspots in chromatographic work. [0003] The core-shell fillers commonly used in the market are mainly surface porous silica core-shell microspheres. This type of filler...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/28B01J20/30B01D15/08
CPCB01D15/08B01J20/28021B01J20/286
Inventor 白泉夏红军
Owner NORTHWEST UNIV(CN)
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