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Chemically-bonded cellulose-type chiral stationary phase and preparation method thereof

A chiral stationary phase and cellulose-based technology, applied in chemical instruments and methods, and other chemical processes, can solve the problems of high pressure resistance, short service life, etc., and achieve good reproducibility, wide application range, and application range wide effect

Inactive Publication Date: 2015-11-25
HUAIAN CHEM NEW MATERIAL RES CENT DALIAN INST OF CHEM PHYSICS CHINESE ACADEMYOF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Therefore, we have prepared a chemically bonded cellulose-based chiral chromatography stationary phase with excellent chromatographic performance, which overcomes the shortcomings of coated chiral stationary phases such as swelling or dissolving in some solvents, short service life, and high pressure resistance.

Method used

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  • Chemically-bonded cellulose-type chiral stationary phase and preparation method thereof
  • Chemically-bonded cellulose-type chiral stationary phase and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Activate 3g of silica gel and dry it overnight at 120°C, put it in a 100ml three-necked round-bottomed flask, add 30ml of dry toluene and 5ml of triethoxyaminopropylsilane in sequence, and heat it under nitrogen protection at 110°C for 24h. Filtrate while hot, wash, and dry overnight at 80°C to obtain aminopropyl silica gel.

[0021] (2) Preparation of cellulose derivatives

[0022] Put 1g of cellulose in a three-necked round-bottomed flask filled with 40ml of pyridine, add 3g of triphenylchloromethane and react at 100°C for 24h, then add 3g of 4-chloromethylphenyl isocyanate and continue to react at 100°C for 24h, cool Afterwards, the product was poured into 100 ml of methanol solution of hydrochloric acid, stirred at room temperature for 24 hours, filtered, washed with methanol, and dried in vacuum to obtain cellulose derivatives.

[0023] (3) chemical bonding

[0024] Dissolve 0.5g of cellulose derivatives in a beaker containing 30ml of tetrahydrofuran, add 2g ...

Embodiment 2

[0026] (1) Activate 15g of silica gel and dry it overnight at 120°C, place it in a 250ml three-neck round-bottomed flask, add 150ml of dry toluene, 25ml of triethoxyaminopropylsilane in turn, and reflux at 110°C for 24 hours under nitrogen protection. Filtrate while hot, wash, and dry overnight at 80°C to obtain aminopropyl silica gel.

[0027] (2) Preparation of cellulose derivatives

[0028] Put 3g of cellulose in a three-necked round-bottom flask filled with 100ml of pyridine, add 10g of triphenylchloromethane and react at 100°C for 24h, then add 10g of 4-chloromethylphenylisocyanate and continue to react at 100°C for 24h, cool Finally, the product was poured into 300ml of methanol solution of hydrochloric acid, and reacted for 24 hours, filtered, washed with methanol, and dried in vacuum to obtain cellulose derivatives.

[0029] (3) chemical bonding

[0030] Take 3g of cellulose derivatives and dissolve them in a beaker containing 180ml of tetrahydrofuran, add 12g of ami...

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Abstract

The invention discloses a chemically-bonded cellulose-type chiral stationary phase and a preparation method thereof. The preparation method comprises the following steps: (1) adding cellulose derivatives, which are obtained by reactions between cellulose and derivatives thereof, into a reaction container containing an organic solvent, washing and drying the cellulose derivatives, and saving cellulose derivatives for later use; (2) painting the prepared cellulose derivatives on the surface of aminopropyl silica gel, evaporating the solvent, adding a new solvent and a joint arm reagent to carry out reactions, cooling, then washing the reaction products by methanol and tetrahydrofuran, and drying the reaction products in vacuum so as to obtain the chemically-bonded cellulose-type chiral stationary phase. The prepared chiral stationary phase has the advantages of wide application range, good chromatographic performance, and high chemical stability, and can be applied to commercial production.

Description

technical field [0001] The present invention relates to the preparation of chromatographic fillers, specifically using 4-chloromethylbenzoate cellulose derivatives as chiral selectors, 1,6-hexamethylene diisocyanate as connecting arms, and modifying them by chemical bonding On the carrier, a chemically stable bonded cellulose (4-chloromethyl benzoate) chiral chromatographic stationary phase is prepared. Background technique [0002] Among a large number of chiral stationary phases, polysaccharide chiral stationary phases have been proven to have a wide range of uses. The chiral stationary phase prepared with polysaccharide derivatives such as cellulose and starch is the most widely used chiral stationary phase in chiral resolution of high performance liquid chromatography, and has good resolution ability. Since Hesse and Hagel first used microcrystalline cellulose triacetate directly as a chiral stationary phase in liquid chromatography in 1973, the research on chiral stati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/29B01J20/30
Inventor 韩海峰周利娟朱建生汪青王涛
Owner HUAIAN CHEM NEW MATERIAL RES CENT DALIAN INST OF CHEM PHYSICS CHINESE ACADEMYOF SCI
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