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

Chromatographic filler, and preparation method and application thereof

A chromatographic packing and raw material technology, applied in the field of analytical chemistry, can solve the problems of alkali resistance defects and slow mass transfer, and achieve the effects of uniform and controllable pore size, improved alkali resistance, and uniform particle size.

Active Publication Date: 2021-07-23
SUZHOU NANOMICRO TECH CO LTD
View PDF6 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the chromatographic packing provided by the above-mentioned patents has a pore structure that is mainly a disordered pore structure, and the mass transfer rate is relatively slow, or the ordered chromatographic packing of a pure silica matrix is ​​obtained, and its alkali resistance and the like still have advantages. certain defects

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
  • Chromatographic filler, and preparation method and application thereof
  • Chromatographic filler, and preparation method and application thereof
  • Chromatographic filler, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] A chromatographic filler, the preparation method thereof includes the following steps:

[0060] (1) 1 g F127 polyether template agent, 0.16 g of a hexadalkyltrimethylammonium ammonium ammonium dielectric (CTAb template), 30 ml deionized water and 6 ml ethanol were mixed under stirring conditions of 500 rpm, Get clarified solution;

[0061] (2) 1.76 g of orthosilicate (TEOS), 0.85 g 1, 4-di (triethoxyla) benzene (BTEB) and step (1) were subjected to a stirring condition of 500 rpm under a rotational speed. The reaction was mixed for 1 h, at 80 ° C for 5 h, and the reaction was reacted at 130 ° C for 12 h, resulting in an intermediate product;

[0062] (3) The intermediate product obtained by flushing step (2) was dried at 50 ° C for 12 h, and the intermediate product was stirred in anhydrous ethanol at 50 ° C for 24 h, and the chromatogram filled.

[0063] The chromatographic filler obtained by the present embodiment is 3.5 μm, a pore size of 8.9 nm, a specific surface area ...

Embodiment 2

[0065] A chromatographic filler, the preparation method thereof includes the following steps:

[0066] (1) 2G F127 polyether template agent, 0.32 g of CTAb template, 50 ml deionized water and 13 ml of ethanol were mixed under stirring of 600 rpm under stirring conditions of 600 rpm to obtain a clear solution.

[0067] (2) The clarified solution obtained by 3.52 g of TEOS, 1.7G BTEB and step (1) was mixed under stirring conditions of 600 rpm, and at 70 ° C at 70 ° C for 6 h, and at 120 ° C for 14 h, the intermediate product was obtained;

[0068] (3) The intermediate product obtained by flushing step (2) was carried out at 70 ° C for 12 h, and the intermediate product was stirred in anhydrous ethanol at anhydrous ethanol at 60 ° C for 24 h, and the chromatographic filler was obtained.

[0069] The chromatographic filler obtained by this embodiment is 2.8 μm, a pore size of 7.1 nm, a specific surface area of ​​472m. 2 / g, the variation coefficient is 12.5%.

Embodiment 3

[0071] A chromatographic filler, the preparation method thereof includes the following steps:

[0072] (1) 0.5 g of F127 polyether template, 0.08 g of CTAb template, 15 ml deionized water and 2.5 ml of ethanol were mixed under stirring conditions of 400 rpm under a stirring conditions of 400 rpm, resulting in a clear solution;

[0073] (2) The clear solution obtained by 0.88 g of TEOS, 0.42 g of BTEB and step (1) was mixed with 0.5 h, and at 85 ° C for 4 h, at 140 ° C for 10 h, to obtain an intermediate product under stirring conditions of 400 rpm.

[0074](3) The intermediate product obtained by flushing step (2) was carried out at 60 ° C for 12 h, and the intermediate product was stirred in anhydrous ethanol at 60 ° C for 24 h, and the chromatographic filler was dried.

[0075] The chromatographic filler obtained by this embodiment is 3.1 μm, a pore size of 9.6 nm, a specific surface area of ​​450m. 2 / g, the variation coefficient is 10.2%.

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

PropertyMeasurementUnit
The average particle sizeaaaaaaaaaa
Apertureaaaaaaaaaa
Specific surface areaaaaaaaaaaa
Login to View More

Abstract

The invention provides a chromatographic filler, and a preparation method and application thereof. The chromatographic filler is prepared from a polyether template, a hexadecyltrimethylammonium bromide template, tetraethoxysilane and 1, 4-bis (triethoxysilyl)benzene. According to the chromatographic filler, a specific part of the polyether template is selected to be matched with a specific part of the hexadecyltrimethylammonium bromide template to serve as a composite template; the combination of tetraethoxysilane and 1, 4-bis(triethoxysilyl)benzene is selected as a silicon source precursor, so that the prepared chromatographic filler spherical particles are smooth in surface and relatively uniform in particle size, have high specific surface area and highly ordered mesoporous channels, and can accelerate mass transfer when being applied to chromatography; and the chromatographic filler also has excellent alkali resistance and important research value.

Description

Technical field [0001] The present invention belongs to the field of analysis chemistry, and is specifically involved in chromatographic films and preparation methods and applications thereof. Background technique [0002] The filler of silica gel is a normal application in high performance liquid chromatography (HPLC), solid phase extraction, silica gel surface can be chemically modified to form a bond phase of various functional groups. However, the maximum disadvantage of silica gel is that the alkali-resistance is different, and the silica gel is dissolved at high pH, ​​and the silica gel surface contains a plurality of silicosol groups, acidic, and is strongly combined with alkaline solute when separating basic compounds (such as amines). Alkaline compound retains, exhibition and trailing. Therefore, the improvement of alkali-resistant alkali-resistant is always an important topic of chromatographic filing research and improvement. [0003] As the silicon ester containing or...

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): C08G77/04C08G77/06B01J20/285B01J20/282
CPCC08G77/04C08G77/06B01J20/285B01J20/282C08G77/80
Inventor 刘晓艳江必旺刘劲松
Owner SUZHOU NANOMICRO TECH CO LTD
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