Synthesis method of core-shell type liquid chromatogram filler

Abstract

The invention discloses a synthesis method of a core-shell type liquid chromatogram filler, which is characterized by comprising the following steps of: 1, mixing and stirring silane and an alcoholic mixture, and synthesizing non-porous spherical silicon gel to be used as a core part of the core-shell type filler; 2, carrying out calcination and acid treatment on the core part obtained from the step 1, and then coating a layer of cationic polymer electrolyte on the surface of the core part; and 3, modifying a layer of nano particles on the surface of a product obtained from the step 2 to obtain the core-shell type filler, wherein the alcoholic mixture comprises the following components in weight: 9.5-14.5 percent of alcohol, 60-80 percent of water and 6.5-13 percent of ammonia water. By adopting the preparation method disclosed by the invention, the core grain size of the obtained core-shell type filler and the modifying thickness of the nano particles can be controlled, and the surface functional groups can be freely selected, so that demands on different separation modes are met; and a filler detection column efficiency reaches 180,000 theoretical pedals / m which is over 2 times that of the conventional chromatograph filler.

Description

technical field [0001] The invention relates to a chromatographic filler, in particular to a method for synthesizing a core-shell type liquid chromatography filler. Background technique [0002] With the continuous development of chromatographic technology, the separation medium is constantly updated and improved. The chromatographic column is the core of the entire chromatographic system. How to obtain higher column efficiency has always been a concern of people. For traditional packed chromatographic columns, people use smaller and smaller fillers in pursuit of high column efficiency. Reducing the particle diameter of spherical packing media will reduce multipath effects and accelerate mass transfer, thereby improving column efficiency. However, the ensuing problem is that the reduction of particle diameter will cause a sharp increase in operating pressure, which undoubtedly puts forward more stringent requirements for equipment performance and technical operation. In fac...

AI Technical Summary

Problems solved by technology

In U.S. Patent No. 4,477,492, a filler is disclosed, which is spray-dried. The silica gel core is prepared by the sol-gel method, and then spray-dried at high temperature (about 200°C) and high pressure. However, this preparation method synthesizes Particles have defects of inhomogeneity and incomplete classification, so that the final core-shell packing is inconsistent

In addition, the use of expensive spray drying equipment increases the cost of production

[0004] US Patent No. 3,505,785 uses a multi-layer thin-layer method, but this method is time-consuming and often requires multi-stage processing procedures, and this method is not suitable for the preparation of particles below 5 μm

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