Preparation method of carbon-titanium dioxide chromatography stationary phase with shell-core structure and application

A chromatographic stationary phase and core-shell structure technology, applied in the field of stationary phase preparation, can solve the problems of high column efficiency, high density of metal oxide microspheres, etc., and achieve strong repeatability, good synthesis effect, and good separation effect Effect

Inactive Publication Date: 2010-10-27
HEILONGJIANG UNIV
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Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that the metal oxide-based chromatographic stationary phase is difficult to fill out a high-efficiency chromatographic column through the homogenization method due to the high density of metal oxide microspheres, and provides a carbon shell-core structure -Preparation method and application of titanium dioxide chromatographic stationary phase

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  • Preparation method of carbon-titanium dioxide chromatography stationary phase with shell-core structure and application
  • Preparation method of carbon-titanium dioxide chromatography stationary phase with shell-core structure and application
  • Preparation method of carbon-titanium dioxide chromatography stationary phase with shell-core structure and application

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specific Embodiment approach 1

[0013] Specific embodiment one: the preparation method of the carbon-titanium dioxide chromatographic stationary phase of core-shell structure in the present embodiment is as follows: one, soluble ferrous salt and carbohydrate carbohydrate are dissolved in water, the soluble ferrous salt and carbohydrate carbohydrate The mass ratio is 1:2, seal with a plastic film, and then ultrasonic for 20-40 minutes, until the solution is completely clear and transparent, put it into a hydrothermal kettle, react with water at 155-165°C for 7-9 hours, and then follow the centrifugation and ultrasonic washing , centrifugation, ultrasonic alcohol washing and centrifugation for 2 to 4 times until the supernatant is clear, and dry at room temperature to obtain carbon spheres; 2. Add carbon spheres to TiO 2 In the sol, ultrasonic 20 ~ 40min, let stand for 10min, centrifuge; 3. Put the carbon spheres treated in step 2 in a tube furnace in N 2 Under protected conditions, the temperature is raised t...

specific Embodiment approach 2

[0015] Embodiment 2: This embodiment differs from Embodiment 1 in that the soluble ferrous salt described in step 1 is ferrous gluconate, ammonium ferrous sulfate or lithium ferrous phosphate. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0016] Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that the sugar carbohydrates described in step 1 are glucose, fructose, starch or oligosaccharides. Others are the same as those in the first or second embodiment.

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Abstract

The invention discloses a preparation method of a carbon-titanium dioxide chromatography stationary phase with a shell-core structure and an application, relating to the preparation method of the stationary phase and the application. The preparation method can solve the problems that as the density of metal oxide microspheres is higher, the chromatography stationary phase taking a metal oxide as a matrix is very difficult to fill out a chromatographic column with high column efficiency through the homogenization method. The method comprises the following steps: adding prepared carbon spheres into TiO2 sol, carrying out ultrasonic treatment, standing, carrying out centrifugation, and then obtaining the carbon-titanium dioxide chromatography stationary phase with the shell-core structure which is used in capillary electrochromatography and high-performance liquid chromatography under the condition of N2 protection. The carbon spheres are taken as the matrix, and the carbon spheres have uniform particle size distribution, good appearance, large specific surface area and high strength. TiO2 high-performance particles are enriched on the surface of the obtained carbon-titanium dioxide chromatography stationary phase with the shell-core structure, and the carbon-titanium dioxide chromatography stationary phase has high surface activity and is resistant to high temperature and extreme pH; and the carbon-titanium dioxide chromatography stationary phase is used in the high-temperature high-performance liquid chromatography separation technology, and has good separation effect, high efficiency and strong repeatability.

Description

technical field [0001] The invention relates to a preparation method and application of a stationary phase. Background technique [0002] With the development of production and the improvement of science and technology, people put forward higher requirements for analysis and testing technology. Compared with gas chromatography, the application of liquid chromatography is far from commensurate with its actual potential. High temperature liquid chromatography (HTLC) combines many advantages of gas chromatography and liquid chromatography. It is a new type of chromatographic separation mode newly developed in recent years. However, the application of HTLC is not very extensive. Among the many reasons, the main point is that It is the lack of its chromatographic packing material. Conventional chromatographic stationary phases are mostly based on silica gel, and the groups bound to the surface will lose a large amount under high temperature conditions, making them lose their se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30G01N30/60
Inventor 付宏刚张权青刘洋王瑞红张维冰
Owner HEILONGJIANG UNIV
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