Ferrocene bonding chromatographic stationary phase and preparing method thereof

A chromatographic stationary phase and ferrocene technology, applied in the field of liquid chromatography, can solve the problems of high cost and complicated process, and achieve the effects of simple operation, simple preparation process and mild reaction conditions

Inactive Publication Date: 2016-03-30
WUHAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although a variety of synthetic methods of ferrocenyl-bonded silica gel chromatography stationary phases have been reported, they are basically obtained by bonding aminopropyl silica gel to ferrocenyl ligands, and the relevant ligands require varying degrees of synthesis. Synthesis and modification, the process is more complicated and the cost is higher

Method used

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  • Ferrocene bonding chromatographic stationary phase and preparing method thereof
  • Ferrocene bonding chromatographic stationary phase and preparing method thereof
  • Ferrocene bonding chromatographic stationary phase and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 5.0g of activated silica gel (particle size 5um), add 150mL of freshly distilled anhydrous toluene to a 250mL round-bottomed three-neck flask, blow nitrogen for 30min, add 5mL of 3-mercaptopropyltrimethoxysilane under stirring, and add 3 drops of Triethylamine, under the protection of nitrogen, heat up to 110-120°C, stir and reflux for 24 hours, cool to room temperature, filter dry, wash with toluene, ether, acetone, methanol, acetone respectively for 2-3 times, and vacuum-dry at 60°C After 18 hours, 3-mercaptopropyl silica gel was obtained.

[0026] Take 4.5g of 3-mercaptopropylated silica gel and add it to 150mL of anhydrous toluene. Under stirring conditions, add 6.0g of vinyl ferrocene and 0.3g of AIBN respectively. Under the protection of nitrogen, heat the oil bath to 110°C, and reflux for 24h. The obtained product was washed successively with toluene, ethanol and acetone, and vacuum-dried at 80°C to obtain a ferrocene-bonded silica gel chromatography station...

Embodiment 2

[0029] According to the method for synthesizing 3-mercaptopropyl silica gel in Example 1, 5 g of activated titanium oxide microspheres (with a particle diameter of 7.5 μm) were used as a matrix filler to obtain 3-mercaptopropyl titanium oxide microspheres.

[0030] Take 4.5g of 3-mercaptopropylated titanium oxide microspheres and add them to 150mL of anhydrous toluene. Under stirring conditions, add 9.0g of vinylferrocene and 0.3g of AIBN respectively. Under the protection of nitrogen, heat the oil bath to 80°C and react After 36 hours, the obtained product was washed successively with toluene, ethanol and acetone, and dried under vacuum at 80°C to obtain a ferrocene-bonded titanium oxide chromatographic stationary phase. The stationary phase structure is:

[0031]

Embodiment 3

[0033] According to the method for synthesizing 3-mercaptopropyl silica gel in Example 1, take 5g of activated zirconia microspheres (particle size 10.0um) as matrix filler, and replace 3-mercaptopropyl trimethoxysilane with 3-mercaptopropyl triethyl Oxysilane can be used to prepare 3-mercaptopropyl zirconia microspheres.

[0034] Add 4.5g of 3-mercaptopropylated zirconia microspheres into 150mL of anhydrous toluene, add 13.5g of vinyl ferrocene and 0.3g of AIBN respectively under stirring conditions, heat the oil bath to 120°C under the protection of nitrogen, and reflux After 12 hours, the obtained product was washed successively with toluene, ethanol and acetone, and dried under vacuum at 80°C to obtain a ferrocene-bonded zirconia stationary phase for chromatography. The stationary phase structure is:

[0035]

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Abstract

The invention discloses a ferrocene bonding chromatographic stationary phase and a preparing method thereof. The ferrocene bonding chromatographic stationary phase is obtained in the way that under the protection of inert atmosphere in an organic solvent, azodiisobutyronitrile is added dropwise to 3-mercaptopropyl silanized inorganic matrix microspheres and vinylferrocene to serve as the initiator, reaction is conducted for 18-36 h at 80-120 DEG C, and then cooling, filtration, washing and drying are conducted. The preparing process is simple, cost is low, reaction materials are easy to obtain and have wide sources, and the ferrocene bonding chromatographic stationary phase can be directly used without any modification; the prepared ferrocene bonding chromatographic stationary phase is a universal hydrophobic interaction chromatographic stationary phase, has high separation selectivity for most compounds, and has high application value and potential.

Description

technical field [0001] The invention belongs to the technical field of liquid chromatography, and in particular relates to a ferrocene bonded chromatography stationary phase and a preparation method thereof. technical background [0002] High-performance liquid chromatography (HPLC) is the most important component of contemporary chromatographic technology. It is the fastest-growing and most widely used separation and analysis technology in modern analytical chemistry. fields play an increasingly important role. In the high-performance liquid chromatography system, the stationary phase plays an important role, and the development of new stationary phases has always been the most active frontier research field of modern high-performance liquid chromatography. [0003] Ferrocene, also known as dicyclopentadiene iron, is an organic transition metal compound with aromatic properties. It is orange-yellow powder at room temperature, with camphor odor. Insoluble in water, easily...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30
Inventor 胡志雄余小波张维农齐玉堂贺军波
Owner WUHAN POLYTECHNIC UNIVERSITY
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