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Monodisperse porous zirconium dioxide-cerium dioxide composite microsphere and preparation method thereof

A ceria and zirconia technology, which is applied in the field of monodisperse porous zirconia-ceria composite microspheres and the preparation thereof, can solve the problem that it is only suitable for chromatographic separation of small molecular compounds, and achieves high mechanical strength and size. And the effect of controllable pore size and uniform particle size

Inactive Publication Date: 2017-05-10
PEKING UNIV SHENZHEN GRADUATE SCHOOL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the report used the porous ZrO prepared by the microemulsion method 2 / CeO 2 The particle size distribution of composite microspheres is wide, and the pore size is only 6.3nm, which is only suitable for chromatographic separation of small molecular compounds

Method used

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  • Monodisperse porous zirconium dioxide-cerium dioxide composite microsphere and preparation method thereof
  • Monodisperse porous zirconium dioxide-cerium dioxide composite microsphere and preparation method thereof
  • Monodisperse porous zirconium dioxide-cerium dioxide composite microsphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] In this example, the commercially available porous PGMA / EGDMA microspheres with a particle size of 5 μm were used as a template to prepare the monodisperse porous zirconia-ceria composite microspheres of this example. The specific preparation method is as follows:

[0036] Weigh 1g of porous PGMA / EGDMA microspheres with a particle size of 5μm in a beaker, and weigh 2g of zirconium oxychloride ZrOCl 2 ·8H 2 O was fully dissolved in 3mL of water, weighed 0.5g of cerium ammonium nitrate and dissolved in 2mL of water to fully dissolve, then poured the solution of zirconium source and cerium source into the beaker containing porous PGMA / EGDMA microspheres, added 3mL of ethanol, and ultrasonically dispersed into the solution There are no obvious large particles in the. Then put it into an oven at 90° C. for 10 h to form zirconia-ceria-polymer composite microspheres. In order to remove the polymer template of the zirconia-ceria-polymer composite microsphere, the dried zircon...

Embodiment 2

[0041] The template of this example is the same as that of Example 1, except that in this example, the porous PGMA / EGDMA microsphere template has been modified with EDA to prepare the monodisperse porous zirconia-ceria composite microspheres of this example . Among them, the purpose of EDA modification is to make the surface of the polymer microspheres have amino groups. Using the coordination between amino groups and zirconium and cerium, the polymer microspheres can better interact with the zirconium and cerium sources to regulate the prepared The pore size of the porous zirconia-ceria composite microspheres and the method of EDA modification can be carried out with reference to conventional experiments. The specific preparation method of the monodisperse porous zirconia-ceria composite microspheres of this example is as follows:

[0042] Ultrasonic disperse 3g of monodisperse porous PGMA / EGDMA microspheres with a particle size of 5μm in 200mL of water, then add 6g of EDA, ...

Embodiment 3

[0048] In this example, the same template as in Example 1 was used to prepare monodisperse porous zirconia-ceria composite microspheres. The difference is that in this example, 1 g of cerium ammonium nitrate was dissolved in 2 mL of water as the cerium source solution. The remaining steps and parameters And condition is all identical with embodiment one.

[0049] Similarly, the monodisperse porous zirconia-ceria composite microspheres prepared in this example were observed by scanning electron microscopy, and the results showed that the porous zirconia-ceria composite microspheres prepared in this example had good monodispersity and particle size The diameter is uniform.

[0050] The monodisperse porous zirconia-ceria composite microspheres prepared in this example were subjected to statistical analysis of the pore size distribution using the same method as in Example 1. The results showed that the porous zirconia-ceria composite microspheres of this example had a pore diamete...

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Abstract

The invention discloses a monodisperse porous zirconium dioxide-cerium dioxide composite microsphere and a preparation method thereof. The preparation method of the monodisperse porous zirconium dioxide-cerium dioxide composite microsphere comprises the following steps of using porous polymer microspheres as templates; using a solution containing a zirconium source and a cerium source for performing infiltration on the porous polymer microspheres; meanwhile, performing sol-gel conversion to form a zirconium dioxide-cerium dioxide polymer composite microsphere; then, performing high-temperature calcination on the zirconium dioxide-cerium dioxide polymer composite microsphere; removing the porous polymer; obtaining the monodisperse porous zirconium dioxide-cerium dioxide composite microsphere. The preparation method provided by the invention has the advantages that the operation is simple; the repeatability is good; the prepared porous zirconium dioxide-cerium dioxide composite microsphere has the uniform particle diameter; the dimension and the bore diameter are controllable; the mechanical intensity is high; the use requirements of a chromatography filling material can be met. The preparation method provided by the invention provides a novel method and path for preparing a high-quality chromatography filling material.

Description

technical field [0001] The present application relates to the field of liquid chromatography separation fillers, in particular to a monodisperse porous zirconia-ceria composite microsphere and a preparation method thereof. Background technique [0002] The chromatographic column is the heart of chromatographic separation, and the quality of the chromatographic column is determined by the material filled in the column, which we call the stationary phase of chromatography, that is, filler or medium. Currently, liquid chromatography is widely used, especially in the chromatographic separation of proteins. As an ideal liquid chromatography separation filler, the following conditions must be met (Nawrocki, J. et al. J. Chromatogr. A 2004, 1028, 1-30. Schomburg, G. et al. Anal. Chem. 1991, 10, 163-169. ): (1) Variable comparison, such as retention and sample capacity; (2) Long-term chemical stability, acid and alkali resistance and high temperature resistance; (3) High mechanical...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/30
CPCB01J20/285B01J20/3028B01J2220/54
Inventor 何洁陈继伟任连兵滕超王勇
Owner PEKING UNIV SHENZHEN GRADUATE SCHOOL
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