Method and special device for synthesizing liquid chromatogram stationary phase by catalysis of gas-solid phase

A technology of chromatographic stationary phase and special device, which is applied in the field of synthetic liquid chromatographic stationary phase, can solve the problems of uneven distribution and agglomeration, reduce the bonding density of stationary phase, reduce the reproducibility of bonding reaction, etc., and achieve Good heat transfer performance, reducing high boiling point impurities to participate in the reaction, and solving the effect of uneven mixing

Inactive Publication Date: 2014-04-23
北京迪马欧泰科技发展中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of the liquid-phase bonding reaction is that the reaction site of the organosilane molecule can be solvated by the solvent molecule, which prevents the silane from reacting with the silanol on the surface of the silica gel, thereby inhibiting the bonding reaction and reducing the bonding density of the stationary phase; The uneven distribution and bonding in the phase reduce the reproducibility of the bonding reaction, and the inhomogeneity of the preparation process of the bonded phase also leads to a decrease in the separation performance of the stationary phase; unreacted silane, Removal of catalysts and salts and isolation of pure products from reaction mixtures is a waste of time and effort

Method used

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  • Method and special device for synthesizing liquid chromatogram stationary phase by catalysis of gas-solid phase
  • Method and special device for synthesizing liquid chromatogram stationary phase by catalysis of gas-solid phase
  • Method and special device for synthesizing liquid chromatogram stationary phase by catalysis of gas-solid phase

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Example 1 Preparation of C18 chromatographic stationary phase by gas-solid catalytic method

[0040] 100 g of silica gel (3) (AGC Si-Tech Co. Ltd., 5 mm, 100 ?, 440 m 2 / g) into the reactor (0), open the valve B (9), dry nitrogen into the reactor (0) through the flow meter (10) and preheater (6), silica gel (3) through the heater (4) Heat to 170 0 C dry for 24 hours. Add 600 grams of octadecyldimethylchlorosilane into the silane vaporizer (12) and heat it to boiling. The vaporized silane enters the preheater (6) through the valve C (11), and passes into the reactor after further heating In (0), ammonia gas is passed through the catalyst vaporizer (8), valve A (7) and preheater (6) into the reactor (0) to react with the silica gel (3) at the same time. Maintain reaction temperature at 340 with heater (4) o C or so. After the unreacted octadecyldimethylchlorosilane is condensed by the condenser (15), it returns to the Soxhlet extractor (14), and then returns to the s...

Embodiment 2

[0041] Example 2 Preparation of C8 chromatographic stationary phase by gas-solid catalytic method

[0042] 100 g of silica gel (3) (AGC Si-Tech Co. Ltd., 5 mm, 100 ?, 440 m 2 / g) is filled into the reactor (0), and the silica gel (3) is heated to 170 0 C dry for 24 hours, add 150-200 ml of pyridine into the catalyst vaporizer (8), and heat to boiling, the vaporized catalyst enters the preheater (6) through valve A (7), and after further heating, enters the reactor (0). At the same time, 500 milliliters of C8dimethylmethoxysilane is added to the silane vaporizer (12), and heated to boiling, the vaporized silane enters the preheater (6) through valve C (11), and after further heating, enters React with silica gel (3) in reactor (0), maintain reaction temperature at 200 with heating system (4) 0 C or so. After the unreacted eight-carbon dimethylmethoxysilane is condensed by the condenser (15), it returns to the Soxhlet extractor (14), and then returns to the silane vaporizer ...

Embodiment 3

[0043] Example 3 Preparation of C18 stationary phase by liquid phase bonding (for comparison)

[0044] Add 10 g of spherical silica gel (AGC Si-Tech Co. Ltd., 5 mm, 100 ?, 440 m 2 / g), at 170 0 C for 24 hours. After the silica gel was cooled under an argon atmosphere, xylene (100 ml), octadecyldimethylchlorosilane (18 g) and pyridine (5 ml) were added, mechanically stirred and heated to reflux under argon, reaction 16 Hour. Stop the reaction, vacuum filter, wash with toluene, dichloromethane, tetrahydrofuran, acetone, methanol-water (1:1, v / v), methanol, 80 0 C dry for 24 hours. Bonded silica gel was put into a reactor, xylene (100 ml) and hexamethyldisilazane (10 ml) were added, stirred mechanically and heated to reflux under an argon atmosphere, and reacted for 16 hours. Stop the reaction, vacuum filter, wash with toluene, dichloromethane, tetrahydrofuran, acetone, methanol-water (1:1, v / v), methanol, 80 0 C dried for 24 hours to obtain the stationary phase.

[0045] ...

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Abstract

The invention discloses a method for synthesizing a liquid chromatogram stationary phase. The method comprises the following steps: firstly, performing heating pretreatment on a carrier; then, bonding a gasified catalyst and gasified silane to the carrier; finally, reacting the bonded carrier with a gasified silane capping reagent to obtain the liquid chromatogram stationary phase. A gas-solid phase catalytic fluidized bed synthesis reaction device is established on the basis of a principle that gas molecules have high diffusion speed and facilitate participation in a reaction with solid in each part of particles. The method and the device are easy and convenient to operate and have high reproducibility; the carbon loading amount and the bonding intensity of the chromatographic stationary phase can be greatly improved. A chromatographic filler prepared by the method and the device can be effectively used for the separation and the analysis of acidic, neutral and basic compounds.

Description

technical field [0001] The invention relates to a new method for synthesizing liquid chromatography stationary phase, which belongs to the technical field of preparation of liquid chromatography separation materials. Background technique [0002] High-performance liquid chromatography (HPLC) is a widely used analytical chromatographic technique, the basic principle of which is to use the difference in the partition coefficient of sample molecules between the stationary phase and the mobile phase to achieve separation. High-performance liquid chromatography technology has become the core of many fields such as environmental monitoring, medicine and health, food safety, life science, petrochemical industry, geological exploration, national security, etc. analysis techniques. It can be said that chromatographic separation and analysis technology is pervasive and has penetrated into all aspects of the national economy. The essence of liquid chromatography is to improve the abi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01J8/18
Inventor 李广庆孙晓莉
Owner 北京迪马欧泰科技发展中心
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