25,27-di(3-methyl-thio-ethoxy thiadiazole) calix[4]arene stationary phase, preparation method and application thereof

A methylthiadiazolyl thioethoxy, stationary phase technology, applied in the separation field, can solve the problems of few chromatographic theoretical research and application examples, poor solubility, and few research reports, etc., and achieves a simple and easy synthesis method. , The effect of stable bonding layer and high bonding amount

Active Publication Date: 2011-06-15
ZHENGZHOU UNIV
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Problems solved by technology

Due to the poor solubility of calixarene and the steric hindrance effect of macrocycles, its preparation technology is much more difficult than ODS and other general stationary phases. Although there are some commercial products, there are not many research reports on the preparation methods, and most of them are patent documents.
Compared with macrocyclic compounds such as crown ethers and cyclodextrins, the variety of stationary phases of calixarene is limited, and there are few related chromatographic theoretical studies and application examples. Therefore, the basic and application research on calixarene in chromatographic separation needs to be further deepened.

Method used

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  • 25,27-di(3-methyl-thio-ethoxy thiadiazole) calix[4]arene stationary phase, preparation method and application thereof
  • 25,27-di(3-methyl-thio-ethoxy thiadiazole) calix[4]arene stationary phase, preparation method and application thereof
  • 25,27-di(3-methyl-thio-ethoxy thiadiazole) calix[4]arene stationary phase, preparation method and application thereof

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Embodiment Construction

[0022] The structural formula of the 25,27-two (3-methylthiadiazolylthioethoxy) calix [4] arene stationary phase (TBS-4) of the present invention is as follows: (as figure 1 )

[0023]

[0024] Its synthetic route is as follows figure 2 :

[0025] .

[0026] 1. Preparation of activated silica gel

[0027] Weigh a certain amount of silica gel into a round bottom flask, add 25% (volume ratio) hydrochloric acid, the mass of porous silica gel (g): hydrochloric acid (ml) = 1: 15 ~ 1: 20. Soak for 24 hours, stir and reflux for 12 hours to remove metal ions, filter while hot with G5 sand core funnel, wash twice with double-distilled water until neutral, then wash with acetone three times, and vacuum-dry at 160 °C for 12 hours to obtain activated silica gel .

[0028] 2. Preparation of γ-glycidyl etheroxypropyl bonded silica gel

[0029] Add 200 ml of freshly steamed toluene, add 20 ml of silylating reagent KH-560 and stir in a 500 ml three-neck flask for 10 min, add 16 g ...

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Abstract

The invention discloses a 25,27-di(3-methyl-thio-ethoxy thiadiazole) calix[4]arene stationary phase which is low in cost, high in content of compounded calixarene bonded stationary phase bonded amount, and stable in stability bonding layer, and is prepared by the following steps of: under the action of phase transfer catalyst ammonium tetrabutyl bromide, carrying out nitrogen protection to gamma-glycidol ether bonded silica gel and calixarene derivative sodium phenolate, and preparing the object calixarene stationary phase at 80 DEG C. The calixarene stationary phase compounded by the method in the invention is high in bonded amount, stable in boned layer, simple and easy in compounding method, low in cost, free of pollution in the compounding process and the like. The stationary phase not only has traditional ODS (Octadecylsilyl) reversion phase chromatography performance, and has containing complexing action, pi-pi action, hydrogen bonding action and dipole-dipole action because of many action sites; in a certain degree, the stationary phase in the invention has special separation performance comparing with the traditional ODS column.

Description

technical field [0001] The invention relates to separation technology, in particular to a 25,27-bis(3-methylthiadiazolylthioethoxy) calix[4]arene stationary phase with low cost and high bonding content. It also relates to the preparation method and application of the stationary phase. Background technique [0002] With the development of separation science, liquid chromatography, especially high performance liquid chromatography, is widely used in petroleum, chemical industry, environmental protection, food, medicine, legal inspection, In clinical and natural product analysis, it plays a very important role and becomes an important technique for separating complex samples. With the development of science and technology, the separation system is becoming more and more complex, especially the separation of positional isomers and optical isomers with similar structures and properties, as well as the separation and analysis of actual samples put forward higher requirements for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01D15/08
Inventor 张书胜胡锴闻付勇丁呈华赵文杰陈康康冶保献
Owner ZHENGZHOU UNIV
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