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

Ethyl propionate grafted polysiloxane, preparation method and application thereof

A technology of polysiloxane and ethyl propionate, applied in chemical instruments and methods, other chemical processes, ion exchange, etc., can solve problems such as temperature range limitation, chromatographic peak tailing, etc., to achieve enhanced separation selectivity, Increased grafting rate and excellent temperature resistance

Inactive Publication Date: 2020-11-06
SHANDONG UNIV
View PDF4 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Based on this feature, polysiloxane commercial stationary phases have been developed rapidly, but polysiloxane stationary phases used in the analysis of trace components of Chinese liquor are rarely reported, and polyethylene glycol stationary phases (such as PEG- 20M, FFAP) occupy a dominant position, but this type of stationary phase cannot well solve the separation problem of volatile main aroma components, and the chromatographic problems caused by adsorption of semi-volatile aldehydes, ketones, acids, esters, and alcohols. Due to the problem of peak tailing, the temperature range is also limited, so it is necessary to develop a new type of polysiloxane gas chromatographic stationary phase for liquor analysis, in order to use a wider temperature range and realize the detection of organic alcohols, esters, and fatty acids. The effective separation of gas chromatography has opened up a new field for the research of gas chromatography stationary phase

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
  • Ethyl propionate grafted polysiloxane, preparation method and application thereof
  • Ethyl propionate grafted polysiloxane, preparation method and application thereof
  • Ethyl propionate grafted polysiloxane, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Ethyl propionate graft polysiloxane, the preparation method is as follows:

[0050] (1) Preparation of methyl hydrogen-containing silicone oil with a Si-H chain link content of 25%: according to m:n=3:1 feeding, 26.57g D 4 (0.09mol), 7.2g D 4 H (0.03mol) was added into a 250mL four-neck flask, 0.02mL trifluoromethanesulfonic acid was added, and the reaction was stirred at room temperature for 24h. When the molecular weight of the reactant gradually increased and became viscous, 0.025 g of hexamethyldisiloxane was added as an end-capping agent. After 4 hours of reaction, a slight excess of ammonia water was added to remove trifluoromethanesulfonic acid, and the reaction was stopped after 1 hour. During the reaction, it can be seen that the substance in the reaction bottle gradually changes from a colorless and transparent liquid to a viscous polymer. Dissolve the product with 30mL of n-hexane, filter out the insoluble matter, then wash with distilled water until neutr...

Embodiment 2

[0057] Ethyl propionate graft polysiloxane, the preparation method is as follows:

[0058] (1) Preparation of methyl hydrogen-containing silicone oil with a Si-H chain link content of 25%: according to m:n=3:1 feeding, 26.57g D 4 (0.09mol), 7.2g D 4 H (0.03mol) was added into a 250mL four-neck flask, 0.02mL trifluoromethanesulfonic acid was added, and the reaction was stirred at room temperature for 24h. When the molecular weight of the reactant gradually increased and became viscous, 0.025 g of hexamethyldisiloxane was added as an end-capping agent. After 4 hours of reaction, a slight excess of ammonia water was added to remove trifluoromethanesulfonic acid, and the reaction was stopped after 1 hour. During the reaction, it can be seen that the substance in the reaction bottle gradually changes from a colorless and transparent liquid to a viscous polymer. Dissolve the product with 30mL of n-hexane, filter out the insoluble matter, then wash with distilled water until neutr...

Embodiment 3

[0063] Ethyl propionate graft polysiloxane, the preparation method is as follows:

[0064] (1) Preparation of methyl hydrogen-containing silicone oil with a Si-H chain link content of 25%: according to m:n=3:1 feeding, 26.57g D 4 (0.09mol), 7.2g D 4 H (0.03mol) was added into a 250mL four-neck flask, 0.02mL trifluoromethanesulfonic acid was added, and the reaction was stirred at room temperature for 24h. When the molecular weight of the reactant gradually increased and became viscous, 0.025 g of hexamethyldisiloxane was added as an end-capping agent. After 4 hours of reaction, a slight excess of ammonia water was added to remove trifluoromethanesulfonic acid, and the reaction was stopped after 1 hour. During the reaction, it can be seen that the substance in the reaction bottle gradually changes from a colorless and transparent liquid to a viscous polymer. Dissolve the product with 30mL of n-hexane, filter out the insoluble matter, then wash with distilled water until neutr...

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
Column lengthaaaaaaaaaa
The inside diameter ofaaaaaaaaaa
Column lengthaaaaaaaaaa
Login to View More

Abstract

The invention relates to the technical field of gas chromatography stationary phases, particularly to ethyl propionate grafted polysiloxane and a preparation method thereof, and application of the ethyl propionate grafted polysiloxane as a gas chromatography stationary phase. According to the invention, the ethyl propionate grafted polysiloxane is prepared by grafting ethyl acrylate onto long-chain methyl hydrogen-containing silicone oil through a hydrosilylation reaction; by using the ethyl propionate grafted polysiloxane polymer as a gas chromatography stationary phase, the ethyl propionategrafted polysiloxane polymer has the temperature resistance of a polysiloxane main chain, and the temperature resistance of the ethyl propionate grafted polysiloxane polymer is superior to that of a common polyethylene glycol commodity stationary phase; a side chain is grafted with a special selective group, so that the separation selectivity is improved; and a capillary column coated with the stationary phase is an acid column, and the stationary phase is a novel gas chromatography stationary phase suitable for analyzing substances such as organic alcohol, ester, fatty acid and the like in Chinese white spirit.

Description

technical field [0001] The invention relates to the technical field of gas chromatographic stationary phases, in particular to ethyl propionate grafted polysiloxane, a preparation method thereof and an application as a gas chromatographic stationary phase. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Polysiloxane has been widely used in the field of gas chromatography stationary phase due to its advantages of high and low temperature resistance, weather resistance, aging resistance, physiological inertness, and good film-forming properties. By modifying the polysiloxane main chain or side chain and introducing functional groups with special selectivity, a series of pol...

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): C08G77/38C08G77/12B01J20/285B01J20/30B01D15/08
CPCB01D15/08B01J20/285C08G77/12C08G77/38
Inventor 吴波柏建春杜爱琴杨在孝
Owner SHANDONG UNIV
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