Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Controllable preparation method for silica-gel chromatographic filler

A silica gel chromatography, silica gel technology, applied in chemical instruments and methods, other chemical processes, etc., to avoid the use of organic reagents

Inactive Publication Date: 2016-11-09
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
View PDF2 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far there is no solvent-free method for the preparation of chromatographic stationary phases

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
  • Controllable preparation method for silica-gel chromatographic filler
  • Controllable preparation method for silica-gel chromatographic filler
  • Controllable preparation method for silica-gel chromatographic filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] N - Preparation of Methylimidazole Silica Gel Chromatography Packing (Sil-MIm)

[0029] Steps:

[0030] ① First weigh 0.5 g of silica gel and 0.04 g of CPTMS into a 25 mL round bottom flask, and then add 10 mL of bonded monomer MIm into it;

[0031] ② The mixture of silica gel, silane reagent CPTMS and bonded monomer MIm in a certain proportion was reacted for 48 h at 120 °C under magnetic stirring;

[0032] ③ After the reaction, the prepared chromatographic material was washed several times with a small amount of methanol and then with a large amount of water, and then dried in a vacuum oven for 12 h.

Embodiment 2

[0034] N - Preparation of Methylimidazole Silica Gel Chromatography Packing (Sil-MIm)

[0035] Steps:

[0036] ① First weigh 0.5 g of silica gel and 0.06 g of CPTMS into a 25 mL round bottom flask, and then add 10 mL of bonded monomer MIm into it;

[0037] ② The mixture of silica gel, silane reagent CPTMS and bonded monomer MIm in a certain proportion was reacted under magnetic stirring at 60 °C for 48 h;

[0038] ③ After the reaction, the prepared chromatographic material was washed several times with a small amount of methanol and then with a large amount of water, and then dried in a vacuum oven for 12 h.

Embodiment 3

[0040] N - Preparation of Methylimidazole Silica Gel Chromatography Packing (Sil-MIm)

[0041] Steps:

[0042] ① First weigh 1.0 g of silica gel and 0.04 g of CPTMS into a 25 mL round bottom flask, and then add 10 mL of bonded monomer MIm into it;

[0043] ② The mixture of silica gel, silane reagent CPTMS and bonded monomer MIm in a certain proportion was reacted for 48 h at 120 °C under magnetic stirring;

[0044] ③ After the reaction, the prepared chromatographic material was washed several times with a small amount of methanol and then with a large amount of water, and then dried in a vacuum oven for 6 h.

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 discloses a controllable preparation method for silica-gel chromatographic filler. The method comprises the specific steps: adding an MIm (N-methylimidazole) functional monomer into silica gel (SiO2) and CPTMS (3-chloropropyl trimethoxy silane), carrying out a reaction for 12 to 48 hours at the temperature of 60 DEG C to 150 DEG C with stirring, then, carrying out washing sequentially by methanol and water, and carrying out drying, thereby obtaining N-methylimidazole modified silica-gel chromatographic filler, wherein the mass ratio of the silica gel to the CPTMS is 0.5: (0.02 to 0.5); the mass / volume ratio of the silica gel to the MIm functional monomer is (0.5 to 2.5)g: (10 to 50)mL. According to the method, the amount of bonding of the functional monomer is controlled through strictly controlling the charging rate of the silica gel to the silane reagent; meanwhile, the excessive added functional monomer is a reactant and is also a dispersant, so that additional organic solvent is not required to be added; the functional monomer can be reused, so that the requirements of green chemistry are fully met.

Description

technical field [0001] The invention relates to a method for the controllable preparation of silica gel chromatographic packing, specifically a method for preparing by adding silica gel and silane reagents in the case of far excessive functional monomers N - A solvent-free method of methylimidazole-modified silica gel chromatography media (Sil-MIm). Background technique [0002] There are many solvent-free preparation methods, such as: ultrasonic assistance, microwave radiation, ultra-low temperature synthesis and so on. These methods have been successfully applied to many research fields. However, so far there is no solvent-free method for the preparation of chromatographic stationary phases. Contents of the invention [0003] The object of the present invention is to provide a controllable preparation method of a solvent-free, controllably bonded silica gel chromatographic filler. [0004] A controllable preparation method of silica gel chromatographic packing is cha...

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): B01J20/286B01J20/30
CPCB01J20/286
Inventor 邱洪灯刘后梅
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com