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Porous silicon dioxide microspheres as well as preparation method and application thereof

A technology of porous silicon dioxide and silicon dioxide, applied in the direction of silicon dioxide, silicon oxide, chemical instruments and methods, etc., to achieve the effect of good reproducibility, simple process and easy operation

Active Publication Date: 2020-07-21
JIANGSU JICUI INTELLIGENT LCD TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the size of microspheres used in chromatographic packing is generally required to be 3-10 μm, and it is difficult to obtain such large spheres by the traditional sol-gel method.

Method used

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  • Porous silicon dioxide microspheres as well as preparation method and application thereof
  • Porous silicon dioxide microspheres as well as preparation method and application thereof
  • Porous silicon dioxide microspheres as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Preparation contains the liquid crystal mixture of 1.5g reactive liquid crystal RM257, 8.5g non-reactive liquid crystal 5CB, 0.1g photoinitiator DMPAP and 0.332g comonomer glycidyl methacrylate (the mass percent of reactive liquid crystal accounting for liquid crystal mixture is 14.4 %, the molar ratio of comonomer and reactive liquid crystal is about 1:1), it is made into polymer microspheres according to the above steps, wherein the SPG film micropore diameter is 10 microns, the continuous phase is water, and the liquid crystal conformation changes The molar concentration of SDS in water is 2mM. Such as image 3 As shown, the average particle size of the polymer microspheres in ethanol is 27 μm ( image 3 (a)), and shows a ray-type optical anisotropy (Maltese black cross) ( image 3 (b)). Keeping other conditions unchanged, changing the amount of comonomer so that the molar ratio of the comonomer to the reactive liquid crystal is 2:1 and 1:2, functional polymer mic...

Embodiment 2

[0060] Prepare liquid crystal mixtures containing 1g reactive liquid crystal RM257, 9g non-reactive liquid crystal 5CB, 0.221g comonomer glycidyl methacrylate and 0.1g photoinitiator DMPAP, and 2g reactive liquid crystal RM257, 8g non-reactive liquid crystal The liquid crystal mixture of 5CB, 0.443g comonomer glycidyl methacrylate and 0.1g photoinitiator DMPAP (wherein the mass percentage that reactive liquid crystal accounts for liquid crystal mixture is respectively 9.7% and 19%, comonomer and reactive liquid crystal The molar ratio is about 1:1). It was made into polymer microspheres according to the above steps, wherein the micropore diameter of the SPG membrane was 20 microns, the continuous phase was water, and the molar concentration of the liquid crystal conformation changing agent SDS in water was 2 mM.

[0061] Next, 0.5 g of the above-prepared polymer microspheres were dispersed in 20 mL of tetrahydrofuran, and 560 μL of ethylenediamine was added with stirring, and ...

Embodiment 3

[0066] Preparation contains the liquid crystal mixture of 1.5g reactive liquid crystal RM257, 8.5g non-reactive liquid crystal 5CB, 0.1g photoinitiator DMPAP and 0.332g comonomer glycidyl methacrylate (the mass percent of reactive liquid crystal accounting for liquid crystal mixture is 14.4 %, the molar ratio of comonomer and reactive liquid crystal is about 1:1), it is made into polymer microspheres according to the above steps, wherein the SPG membrane micropore diameter is 2.8 microns, the continuous phase is water, and the liquid crystal conformation changes The molar concentration of SDS in water is 2mM.

[0067] Next, 0.5 g of the above-prepared polymer microspheres were dispersed in 20 mL of tetrahydrofuran, 560 μL of ethylenediamine was added under stirring, and the mixture was refluxed at 80° C. for 24 hours. Filter, wash with ethanol and distilled water alternately for 3 times, and dry to obtain aminated polymer microspheres.

[0068] Finally, 0.5 g of aminated poly...

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Abstract

The invention discloses porous silicon dioxide microspheres, which have a radial conformation internal structure and pore passage arrangement, and which have a particle size of 3-300 microns. The invention also discloses a method for preparing the porous silicon dioxide microspheres, which comprises the following steps: preparing porous aminated polymer microspheres with a radial conformation internal structure and pore passage arrangement; adding a silicon dioxide precursor, and carrying out hydrolysis reaction to obtain silicon dioxide / polymer composite microspheres; calcining the silicon dioxide / polymer composite microspheres to obtain the porous silicon dioxide microspheres. The invention also discloses an application of the porous silicon dioxide microspheres in chromatographic separation. The method is simple in process, easy to operate, good in reproducibility and capable of achieving large-scale production. The porous silicon dioxide microspheres prepared by the method are controllable in particle size and orderly in internal structure and pore passage arrangement, and can be widely applied to the fields of chromatographic separation, catalytic carriers, drug controlled release and the like.

Description

technical field [0001] The invention relates to the field of inorganic porous materials, in particular to porous silica microspheres, a preparation method and application thereof. Background technique [0002] High performance liquid chromatography (HPLC) is an efficient and rapid new analysis and separation technology developed since the 1970s. monitoring and many other fields. The liquid chromatography packing is the key basis for the establishment and development of high performance liquid chromatography technology. Among them, silica has become one of the most ideal liquid chromatography packing matrices because of its excellent mechanical strength, easy-to-control pore structure and specific surface area, good stability, and easy chemical bonding or modification. , has a broad market application prospect. [0003] At present, more than 90% of the HPLC fillers on the market are based on silica gel, and most of them are porous spherical silica gel (porous silica micros...

Claims

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Application Information

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IPC IPC(8): C01B33/12B01J20/283
CPCC01B33/12B01J20/282C01P2004/61C01P2004/60C01P2006/12C01P2006/16C01P2004/02C01P2002/82C01P2004/03B01J20/283C01B33/18B01J20/103
Inventor 李昂陆嘉伟N·L·阿伯特
Owner JIANGSU JICUI INTELLIGENT LCD TECH CO LTD
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