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Method for preparing pyrenly bonded silicagel fixed phase

A technology of bonded silica gel and stationary phase, which is applied to instruments, measuring devices, scientific instruments, etc., can solve the problems of complicated and cumbersome preparation and high cost of pyrene-bonded silica gel

Inactive Publication Date: 2005-02-16
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, although pyrenyl bonded silica stationary phases have been widely used due to their special properties, the preparation of pyrenylsilane coupling agents in the preparation of pyrenyl bonded silica stationary phases was complicated and cumbersome.
As a result, the cost of pyrene-bonded silica gel is high, the preparation is complicated, and it is difficult to popularize and use

Method used

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  • Method for preparing pyrenly bonded silicagel fixed phase
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  • Method for preparing pyrenly bonded silicagel fixed phase

Examples

Experimental program
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Effect test

Embodiment 1

[0020] (1) Synthesis of pyrenyl butyryl chloride: take 0.5 g of pyrenyl butyric acid solids dried in vacuum in a 50 ml round bottom flask, add 20 ml of dry thionyl chloride, heat and reflux in an oil bath and stir for 24 hours, then distill under reduced pressure. Thionyl chloride is all distilled off, and the remaining solid is pyrenyl butyryl chloride, which is black in color, because it is a macrocyclic aromatic acid chloride, which is not easy to hydrolyze like ordinary small molecular acid chlorides, and is relatively stable in the air. stand-by.

[0021] (2) Amino coupling agent bonded silica gel reaction: Take 2.5g of vacuum-dried silica gel in a 100ml three-necked flask, add 55ml of treated anhydrous toluene and 1.5g of 3-aminopropyltrimethoxysilane, magnetically After stirring, 3 drops (about 0.5 ml) of triethylamine were added dropwise. at N 2 Heated to reflux in an oil bath at 100-120°C in an atmosphere, reacted for 24 hours, cooled, filtered with suction, washed ...

Embodiment 2

[0024] (1) Synthesis of pyrenyl butyryl chloride: take 0.5 g of pyrenyl butyric acid solids dried in vacuum in a 50 ml round bottom flask, add 20 ml of dry thionyl chloride, heat and reflux in an oil bath and stir for 12 hours, then distill under reduced pressure. All the thionyl chloride was distilled off, and the remaining solid was pyrenyl butyryl chloride. stand-by.

[0025] (2) Pyrenylbutyryl chloride and amino coupling agent to generate amide: add 20ml of dry toluene to the pyrenylbutyryl chloride generated in (1), heat to dissolve it completely, pour it into a 100ml three-necked flask, and pass through dry N 2 , cooled, and added dropwise (0.5ml / min) 1.5g of 3-aminopropyltrimethoxysilane and 0.5g of triethylamine in an ice bath, and reacted at room temperature for 12h after 10min.

[0026] (3) Preparation of pyrenyl butyric acid-bonded silica gel: get 2.5g of vacuum-dried silica gel and directly add in the reaction of (2), in N 2 Heat to reflux in an oil bath at 100-1...

Embodiment 3

[0028] (1) Synthesis of pyrenyl acetyl chloride: take 0.5 g of pyrenyl acetic acid solids dried in vacuum in a 50 ml round bottom flask, add 20 ml of dry thionyl chloride, heat and reflux in an oil bath and stir for 12 hours, distill under reduced pressure, and All the thionyl chloride was distilled off, and the remaining solid was pyrenylacetyl chloride for use.

[0029] (2) Amino coupling agent bonded silica gel reaction: Take 2.5g of vacuum-dried silica gel in a 100ml three-necked flask, add 55ml of treated anhydrous toluene and 1.5g of 3-aminopropyltrimethoxysilane, magnetically Stir and add 1 ml of triethylamine. at N 2 Heated to reflux in an oil bath at 100-120°C in an atmosphere, reacted for 24 hours, cooled, filtered with suction, washed with toluene and acetone in turn, and dried in vacuum at 120°C for 5 hours before use.

[0030](3) Preparation of pyrenylacetic acid-bonded silica gel: Take the amino-bonded silica gel in (2) in a 100ml three-necked flask, add it to ...

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Abstract

The present invention relates to a preparation mthod of pyrenyl bonded silica gel fixed phase. Said method includes the following steps; heating pyrenyl butyric acid and sulfur oxychloride according to the mole ratio of 1:1.2-1.5, making reflux reaction for 8-24 hr., reduced pressure distilling out sulfur oxychloride to obtain pyrenyl butyryl chloride, then using coupling agent 3-aminopropyl trimethoxysilane as intermediate adaptor for connecting pyrenyl butyryl chloride and silica gel, making bonding reaction so as to obtain the invented pyrenyl bonded silica gel fixed phase, in which the weight ratio of pyrenyl butyryl chloride, silica gel and coupling agent is 1:0.15-0.55:0.25-0.85. Said invented product can be used for separating fullerence, perchlorinated aromatic hydrocarbon, nitro-aromatic hydrocarbon and aromatic hydrocarbon with condensed rings.

Description

technical field [0001] The invention relates to a preparation method of a pyrene-bonded silica gel stationary phase. Background technique [0002] High-performance liquid chromatography is one of the most widely used analytical methods and separation methods in contemporary times. It can not only be used for the preparation and separation of various mixtures, but also can be used for qualitative and quantitative analysis at the same time. It is widely used in various departments of scientific research and society all areas of production. In a liquid chromatography system, the core component that determines the analysis results and the degree of separation is the chromatographic column. Therefore, the development of new column packing has always been an important topic of concern to chromatographic workers. Among the stationary phases of modern liquid chromatography, chemically bonded phase fillers based on particulate silica gel account for about 80% of the entire applicat...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 冯钰锜余琼卫达世禄
Owner WUHAN UNIV
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