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A kind of polyfluorobenzene ring grafted polysiloxane and its preparation method and application

A technology of polyfluorobenzene ring and polysiloxane, which is applied in the field of polyfluorobenzene ring grafted polysiloxane and its preparation, can solve the problems of poor separation performance and achieve improved separation, easy polarization, and improved separation performance Effect

Inactive Publication Date: 2020-12-29
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, through research by the inventors of the present invention, it has been found that the existing polysiloxane immobilization has poor separation performance relative to these pollutants.

Method used

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  • A kind of polyfluorobenzene ring grafted polysiloxane and its preparation method and application
  • A kind of polyfluorobenzene ring grafted polysiloxane and its preparation method and application
  • A kind of polyfluorobenzene ring grafted polysiloxane and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] The synthesis method of 2,5-bis(4-fluorophenyl)-3,4-bis(3,4,5-trifluorophenyl) graft polysiloxane is as follows:

[0077] (1) Synthesis of 1,3-bis(4-fluorophenyl)-2-propanone

[0078] Into a 250.0mL round bottom flask, add 80.0mL of dry dichloromethane, p-fluorophenylacetic acid (10.0g, 65.0mmol), 4-dimethylaminopyridine (DMAP) (10.4g, 85.0mmol), dicyclohexylcarbon Diimine (DCC) (13.4g, 65.0mmol), stirred at room temperature under nitrogen protection for 18h, filtered to remove insoluble matter after the reaction, the filtrate was washed 3 times with 50.0mL water, and 3 times with 50.0mL 2.5mol / L dilute hydrochloric acid , followed by saturated Na 2 CO 3 Aqueous neutralization, anhydrous MgSO 4 After drying, the solvent was evaporated to give a yellow solid. The crude product was recrystallized from methanol / hexane to obtain 1,3-bis(4-fluorophenyl)-2-propanone (5.7 g, 23.0 mmol) with a yield of 71.9%.

[0079] (2) Synthesis of 1,2-bis(3,4,5-trifluorophenyl)-2-hydro...

Embodiment 2

[0089] The synthesis method of 2,5-bis(4-fluorophenyl)-3,4-bis(3,4,5-trifluorophenyl) graft polysiloxane is as follows:

[0090](1) Synthesis of 1,3-bis(4-fluorophenyl)-2-propanone

[0091] Add dry dichloromethane 160.0mL, p-fluorophenylacetic acid (20.0g, 130mmol), DMAP) (20.8g, 169mmol), DCC (26.8g, 130mmol) successively into a 250.0mL round bottom flask, and stir at room temperature under nitrogen protection Reacted for 18 hours, filtered to remove insoluble matter after the reaction, the filtrate was washed 3 times with 80.0mL water, 3 times with 80.0mL 2.5mol / L dilute hydrochloric acid, and then washed with saturated Na 2 CO 3 Aqueous neutralization, anhydrous MgSO 4 After drying, the solvent was evaporated to give a yellow solid. The crude product was recrystallized from methanol / hexane to obtain 1,3-bis(4-fluorophenyl)-2-propanone (11.8 g, 48.0 mmol) with a yield of 73.6%.

[0092] (2) Synthesis of 1,2-bis(3,4,5-trifluorophenyl)-2-hydroxyethanone

[0093] Take a 10...

Embodiment 3

[0101] The synthesis method of 2,5-bis(4-fluorophenyl)-3,4-bis(3,4,5-trifluorophenyl) graft polysiloxane is as follows:

[0102] (1) Synthesis of 1,3-bis(4-fluorophenyl)-2-propanone

[0103] Add dry dichloromethane 120.0mL, p-fluorophenylacetic acid (15.0g, 97.5mmol), DMAP (15.6g, 126.8mmol), DCC (20.1g, 97.5mmol) successively into a 250.0mL round bottom flask, under nitrogen protection Stir the reaction at room temperature for 18 hours. After the reaction, remove the insoluble matter by filtration, wash the filtrate three times with 100.0 mL of water, three times with 100.0 mL of 2.5 mol / L dilute hydrochloric acid, and then wash with saturated Na 2 CO 3 Aqueous neutralization, anhydrous MgSO 4 After drying, the solvent was evaporated to give a yellow solid. The crude product was recrystallized from methanol / hexane to obtain 1,3-bis(4-fluorophenyl)-2-propanone (8.7 g, 35.3 mmol) with a yield of 72.4%.

[0104] (2) Synthesis of 1,2-bis(3,4,5-trifluorophenyl)-2-hydroxyethano...

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Abstract

The invention discloses polyfluorobenzene ring grafted polysiloxane as well as a preparation method and application thereof. The chemical structural formula of the polyfluorobenzene ring grafted polysiloxane is shown in the specification, wherein Vi is vinyl, and the ratio of m to n to p is 85: (11.5-12.0): (3.5-3.0). The polyfluorobenzene ring grafted polysiloxane provided by the invention has the advantages of high selectivity, high thermal stability, low loss and the like as a stationary phase relative to the analysis of pollutants, so that the separation performance of gas chromatography on the environmental pollutants can be provided.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and relates to a polyfluorobenzene ring-grafted polysiloxane and its preparation method and application. 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] Since the advent of capillary gas chromatography, it has been widely used in petrochemical, environmental protection, biomedicine and other separation and analysis science fields due to its high sensitivity and fast analysis speed. At present, gas chromatography, as a mature analytical technique, is still expanding in its breadth and depth of application (Chemical Reagents, 2006, 28(1): 11-15), especially some with high sele...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/385C07C49/697C07C45/74B01J20/26B01J20/281B01J20/30
CPCB01J20/265B01J20/281B01J20/3085C07C45/29C07C45/48C07C45/72C07C45/74C07C49/697C08G77/385C07C49/813C07C49/83C07C49/233
Inventor 吴波徐丽柏建春杨在孝
Owner SHANDONG UNIV