Core-shell SiO2@rosin-based polymer microspheres and preparation method thereof

A technology of polymer microspheres and core-shell type, which is applied in the field of high performance liquid chromatography, can solve the problems of low theoretical plate number of chromatographic columns, narrow range of mobile phase selection, wide particle size distribution of microspheres, etc., and achieve pore structure Rich, good separation performance, high solvent tolerance effect

Inactive Publication Date: 2019-04-26
GUANGXI UNIV FOR NATITIES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are many studies on chromatographic fillers. For example, the invention patent application with application number 201710710292.1 discloses a weakly polar rosin-based polymer microsphere and its preparation method and application. It uses methyl methacrylate as a monomer, Using the rosin derivative propylene pimaric acid ethylene glycol acrylate as a cross-linking agent to prepare weakly polar rosin-based polymer microspheres and fill the chromatographic column with it, a good separation of gastrodin and its derivatives was achieved, but , the chromatographic column filled with the above-mentioned weakly polar rosin-based polymer microspheres has a narrow range of mobile phase selection, especially high sensitivity to water, which limits the further development of its excellent performance; such as Qin Feng, Chen Xiaoming, Liu Yueqi, etc. The cellulose-three (tetramethylbenzoate) derivat...

Method used

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  • Core-shell SiO2@rosin-based polymer microspheres and preparation method thereof
  • Core-shell SiO2@rosin-based polymer microspheres and preparation method thereof
  • Core-shell SiO2@rosin-based polymer microspheres and preparation method thereof

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Experimental program
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preparation Embodiment 1

[0034] First 1.0g maleopimaric acid ethylene glycol acrylate, 1.0g methacrylic acid and 0.1g azobisisobutyronitrile are mixed uniformly to obtain the material for coating, and then the material for coating is evenly coated to 20.0 g silica gel surface, and then placed in 100 mL of 1% sodium lauryl sulfate aqueous solution for free radical polymerization for 6 hours, then Soxhlet extracted the product with absolute ethanol, and then vacuum dried to obtain the core-shell Type SiO 2 @ Rosin-based polymer microspheres.

[0035] After detection and analysis, the core-shell type SiO obtained in this embodiment 2 The particle size distribution of @rosin-based polymer microspheres is concentrated in the range of 80-120μm, the average pore size is 6.5nm, and the specific surface area is 350m 2 / g.

preparation Embodiment 2

[0037] First 50g maleopimaric acid ethylene glycol acrylate, 200g acrylic acid and 5g azobisisoheptanonitrile are mixed uniformly to obtain the material for coating, then the material for coating is evenly coated on the surface of 250g silica gel, and then placed Carry out radical polymerization reaction in 1000mL of 5% sodium dodecyl sulfate aqueous solution for 7h, then Soxhlet extract the product with absolute ethanol, and then vacuum dry to obtain core-shell SiO 2 @ Rosin-based polymer microspheres.

[0038] After detection and analysis, the core-shell type SiO obtained in this embodiment 2 The particle size distribution of @rosin-based polymer microspheres is concentrated in the range of 200-250μm, the average pore size is 0.5nm, and the specific surface area is 293m 2 / g.

preparation Embodiment 3

[0040]First mix 10g ethylene glycol maleopimarate, 50g methyl methacrylate and 1.5g azobisisobutyronitrile evenly to obtain a coating material, and then evenly coat the coating material to 2000g Silica gel surface, and then placed in 1000mL of 15% sodium lauryl sulfate aqueous solution for free radical polymerization reaction for 9h, then Soxhlet extraction of the product with absolute ethanol, and then vacuum drying to obtain the core-shell SiO 2 @ Rosin-based polymer microspheres.

[0041] After detection and analysis, the core-shell type SiO obtained in this embodiment 2 The particle size distribution of @rosin-based polymer microspheres is concentrated in the range of 2-14μm, the average pore size is 26.01nm, and the specific surface area is 312m 2 / g.

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Abstract

The invention discloses core-shell SiO2@rosin-based polymer microspheres and a preparation method thereof. A rosin-based crosslinking agent, an acrylic monomer and a radical initiator are uniformly mixed, the mixture is uniformly applied to the surface of silica gel, the silica gel is placed in an aqueous phase for radical polymerization, and the core-shell SiO2@rosin-based polymer microspheres are obtained. The core-shell SiO2@rosin-based polymer microspheres have particle size distribution centralized in the range of 2-900 mu m, the mean pore size of 0.5-100 nm and the specific surface areaof 50-350 m<2>/g and have the characteristics of excellent degree of sphericity, uniform particle size, rich pore structure, high mechanical strength and high solvent tolerant degree, and a chromatographic column filled with the core-shell SiO2@rosin-based polymer microspheres as chromatographic packing especially has good separation effect on alkaloids, gastrodin and derivatives thereof.

Description

technical field [0001] The invention belongs to the technical field of high performance liquid chromatography, and in particular relates to a core-shell type SiO 2 @Rosin-based polymer microspheres and their preparation methods. Background technique [0002] As a separation method and technology, high-performance liquid chromatography has become more and more mature in recent years due to its advantages of high separation efficiency, high selectivity, high detection sensitivity, and fast analysis speed, and its application fields have gradually developed to the separation of pesticide residues and drugs. , food testing and other fields. As a place and tool for separation, a chromatographic column is the core of the entire HPLC system, and its performance directly determines the separation effect. The development of chromatographic packing determines the development of chromatographic columns. At present, according to the different matrix materials, chromatographic packing ...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/28C08F289/00C08F220/06C08F220/14
CPCB01J20/28021B01J20/286C08F289/00C08F220/06C08F220/14
Inventor 雷福厚孙耀李文申利群邓杰谢文博易冯梅丁猛胡锦烘
Owner GUANGXI UNIV FOR NATITIES
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