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Method for preparing Zr-based hydrophilic chromatographic packing Zr/Si HILIC

A hydrophilic chromatography, zirconium-based technology, used in chemical instruments and methods, other chemical processes, etc., can solve the problems of poor permeability of fillers, difficult to uniform particles, and unsatisfactory pore structure, and achieve ideal pore structure, uniform particles, and good pore structure. Effects of chemical and mechanical stability

Inactive Publication Date: 2012-10-03
HEBEI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, SiO 2 Packing has two difficult problems in chromatographic applications: one is that the usable pH range is narrow, and it can only be used under the condition of pH=2-8
However, the zirconium spheres prepared by the three methods have disadvantages such as difficult uniformity of particles, small specific surface area, unsatisfactory pore structure, wide pore size distribution, and poor permeability of fillers when used as a chromatographic column matrix.

Method used

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  • Method for preparing Zr-based hydrophilic chromatographic packing Zr/Si HILIC
  • Method for preparing Zr-based hydrophilic chromatographic packing Zr/Si HILIC
  • Method for preparing Zr-based hydrophilic chromatographic packing Zr/Si HILIC

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Embodiment 1

[0019] The carefully screened silica gel microspheres with a particle diameter of 3.49 μm (s=0.302) were placed in 6 mol / L hydrochloric acid and ultrasonicated for 0.5 h for activation pretreatment, suction filtered, washed and dried. The activated pretreated silica gel microspheres were put into 6mmol / L SDS solution, ultrasonicated for 0.5h, and a layer of surfactant SDS molecular film was adsorbed on the surface of the silica gel microspheres. After suction filtration, washing, and drying, a film on the surface of the silica balls was obtained. A layer of surfactant complex (SiO 2 -SDS). Then the composite SiO 2 -SDS was put into 0.1mol / L zirconium solution, and ultrasonic treatment was performed at constant temperature for 1.5 hours in a water bath at 60°C to assemble a layer of nano-zirconium film on the surface of the composite microspheres to obtain SiO 2 -SDS-ZrO 2 Composite microspheres, let stand, filter with suction, and dry. The SDS film and the zirconium film w...

Embodiment 2

[0023] The carefully screened silica gel microspheres with a particle diameter of 3.49 μm (s=0.302) were placed in 6 mol / L hydrochloric acid and ultrasonicated for 0.5 h for activation pretreatment, suction filtered, washed and dried. Put the activated and pretreated silica gel microspheres into a 6mmol / L SDS solution and sonicate for 0.5h, adsorb a layer of surfactant SDS molecular film on the surface of the silica gel microspheres, and filter, wash, and dry to obtain a film on the surface of the silica balls. A layer of surfactant composite SiO 2 -SDS. Then the composite SiO 2 -SDS spheres are put into zirconium sol for self-assembly, and subjected to constant temperature ultrasonic treatment for 1.5 hours under the condition of 60°C water bath, suction filtration, washing and drying, and a layer of nano-zirconia particle film can be assembled on the surface of silica gel spheres. So repeated coating of SDS film and ZrO 2 Film 4 times. After burning at 600°C, the core-sh...

Embodiment 3

[0027] The carefully screened silica gel microspheres with a particle diameter of 3.49 μm (s=0.302) were placed in 6 mol / L hydrochloric acid and ultrasonicated for 0.5 h for activation pretreatment, suction filtered, washed and dried. Put the activated pretreated silica gel microspheres into the zirconium sol and magnetically stir for 1.5h for self-assembly, and obtain a composite SiO with a layer of zirconia nanoparticles assembled on the surface of the silica spheres. 2 -ZrO 2 , suction filtration, washing, and drying; repeat the above operation four times. After burning at 500℃, the core-shell type ZrO can be prepared 2 / SiO 2 microspheres, the ZrO 2 / SiO 2 After further screening of microspheres, Zr / Si HILIC was obtained, and its composition is shown in Table 3.

[0028] The ZrO that table 3 embodiment 3 prepares 2 / SiO 2 Composition of microspheres

[0029]

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Abstract

The invention discloses a method for preparing Zr-based chromatographic packing Zr / Si HILIC. The method comprises the following steps: (1) selecting silica gel micron balls with uniform granules, and carrying out cleaning and activating treatment on the silica gel micron balls; (2), coating a sodium dodecyl sulfate (SDS) surface active agent on the surfaces of the activated silica gel micron balls; (3), assembling a zirconia nano granule coating layer on the surface of each silica gel ball; and (4), conducting drying, scorching and flotation on the assembled product, so as to obtain the product, namely core-shell composite material micron ball Zr / Si HILIC. The micron ball Zr / Si HILIC has the advantages that the granules are regular; the particle size distribution is narrow; the specific surface area is large; the hole structure is ideal; the permeability is good; the pH application range is wide; and the surface is easy to decorate. Therefore, the micron ball Zr / Si HILIC is a comparatively ideal chromatographic packing, can be used in a hydrophilic chromatograph, and also can be widely applied to various chromatographic fractionation modes after decoration.

Description

technical field [0001] The present invention relates to a kind of preparation method of zirconium-based chromatographic filler, especially in silica gel (SiO 2 ) Zirconia (ZrO) mounted on the surface of microspheres 2 The invention discloses a preparation method of zirconium-based hydrophilic chromatographic filler Zr / Si HILIC coated with nanoparticles, belonging to the technical field of chromatographic analysis. Background technique [0002] The chromatographic column is the "heart" of chromatography, and the chromatographic column packing material is the key to achieve effective separation. An ideal chromatographic column matrix should have the following characteristics: uniform particles, high specific surface area, ideal pore structure, pore size in the range of mesopores, and narrow pore size distribution range, good permeability, good mechanical and chemical stability . SiO 2 Almost an ideal material. However, SiO 2 Packing has two difficult problems in chromato...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/30B01J20/283
Inventor 敦惠娟魏雨宋秀芹薛树科谭金标
Owner HEBEI NORMAL UNIV
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