Preparation method of macroporous silica microsphere based on template method and applications thereof

A technology of macroporous silica gel and template method, which is applied in the field of macroporous silica gel microspheres and spherical silica gel particles, which can solve problems such as poor uniformity and insufficient pore size of silica gel microspheres, and achieve the effect of promoting development

Inactive Publication Date: 2017-07-14
UNIV OF SHANGHAI FOR SCI & TECH
View PDF2 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a method for preparing macroporous silica gel microspheres based on the template method, and the method for preparing macroporous silica gel microspheres based on the template method should solve the problems in the prior art. Technical problems of insufficient pore size and poor uniformity of prepared silica gel microspheres for high performance liquid chromatography

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of macroporous silica microsphere based on template method and applications thereof
  • Preparation method of macroporous silica microsphere based on template method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 Preparation of macroporous silica microspheres

[0028] In a 500 ml Erlenmeyer flask, add 15 g of a commercially available cation exchange polymer microsphere (Zhengzhou Inno Biotechnology Co., Ltd. WCX), 25 ml of 50% TMSPTMA methanol solution, 25 ml of triethanolamine, 200 ml of deionized water and 125 ml ethanol, sonicated for 1 h; then placed in a constant temperature water bath at 30°C for 10 min with magnetic stirring, and then, under stirring, added a mixed solution of 25 ml TEOS and 75 ml ethanol drop by drop with a dropping funnel to control the rate of addition. The dropwise addition was completed within 30 min; continue to stir for 24 h; after the reaction was completed, take out the triangular flask and let it stand until the particles naturally settled, filter to remove the clear liquid, and wash the solid particles with ethanol centrifugation three times, dry them at 80°C for 12 h, and place them in the air Calcined at 600 °C for 10 h in the at...

Embodiment 2

[0029] Example 2 Surface bonding

[0030] Take 2 g of the obtained SiO 2The microspheres were soaked and stirred in 1 mol / L hydrochloric acid for 2 h, and the hydrochloric acid was washed away by centrifugation with water and ethanol, respectively, and dried at 80 °C; the acidified and dried SiO 2 Add 1.5 g of microspheres to a 250 ml three-neck round bottom flask after grinding, add 100 ml of dry toluene, stir magnetically in an oil bath, raise the temperature to 120°C to reflux the toluene for 10 min to remove water, then add 0.6 g of imidazole, After stirring for 10 min, add a mixed solution of 1.3 g octadecyldimethylsilyl chloride and 50 ml toluene with a dropping funnel within 15 min, and continue to reflux and stir the suspension for 8 h. Cool to room temperature, and after settling, remove the clear liquid by filtration, add 150 ml of fresh toluene to wash the solid particles, and then use methanol, methanol / water mixture and ethanol to wash by centrifugation, respecti...

Embodiment 3

[0031] Embodiment 3 packing and testing

[0032] Prepare 200ml of a mixture of isopropanol and chloroform with a volume ratio of 1:1, as a homogenate for later use; take 1.2 g of the above-mentioned bonded silica gel, add an appropriate amount of homogenate, ultrasonicate for 3 minutes, and then load it under a hydraulic pressure of 5000psi into a 4.6 × 50mm chromatographic column, and the protein separation test.

[0033] Standard protein chromatographic separation conditions: mobile phase A: 90% water, 10% acetonitrile, 0.1% trifluoroacetic acid; B phase: 90% acetonitrile, 10% water, 0.1% trifluoroacetic acid; flow rate: 0.8 ml / min; Detection wavelength 220 nm; Gradient elution program: 0→15.0min, 5%→65%B; 15→30min, keep 65%B. The test chromatogram is as figure 2 shown.

[0034] The invention prepares macroporous silica gel microspheres of about 2 micrometers, which can be used for the separation of proteins by high-performance liquid chromatography. figure 2 are the c...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a preparation method of a macroporous silica microsphere based on a template method. The preparation method comprises the following steps: mixing a polymer microsphere template with a structure-directing agent, a silica gel precursor, and an alkaline catalyst, carrying out hydrolytic condensation to form composite microspheres of organic polymer and silica, and burning the composite microspheres at a temperature of 400 to 700 DEG C to obtain the macroporous silica microsphere. The prepared macroporous silica microsphere has the characteristics of mono-dispersion and macroporous structure. The prepared macroporous silica microsphere can be subjected to surface modification to prepare the stationary phase of HPLC (high performance liquid chromatography) such as C18 bonding modification (chlorodimethyloctadecylsilane), and can be applied to fields such as separation and analysis in biomedicine, environment detection, food detection, and the like.

Description

technical field [0001] The invention belongs to the field of inorganic materials and relates to a macroporous silica gel microsphere, in particular to a method for preparing spherical silica gel microparticles with monodisperse and macroporous structures based on a template method and an application thereof. Background technique [0002] High performance liquid chromatography (HPLC) has developed into one of the most commonly used separation and analysis methods in the fields of biomedicine, chemical engineering, food hygiene, and environmental protection. Chromatographic columns and column packings are often considered the core of HPLC, which determine the final effect of chromatographic separation. The stationary phase based on silica gel is currently the most widely used HPLC packing, mainly because silica gel has good mechanical strength, stable morphology, pore structure and specific surface area, and its surface contains abundant silanol groups that can Features suc...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): B01J20/283B01J20/291C01B33/12B01J20/30
CPCB01J20/283B01J20/291C01B33/12
Inventor 黄明贤牛梦娜马红彦胡飞王世革刘璐常海洲
Owner UNIV OF SHANGHAI FOR SCI & TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap