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Core-shell type porous zirconium dioxide material and preparation method thereof

A technology of zirconia and nano-zirconia, which is applied in zirconia, chemical instruments and methods, and other chemical processes, and can solve the problems of limited pressure range of full-pore packing, mass transfer process and long separation time, etc.

Active Publication Date: 2015-12-02
天津博纳艾杰尔科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Patent CN01142023.5 uses zirconium salt to prepare zirconia hydrosol, and then uses polymerization-induced colloid coagulation method to make zirconia hydrosol and urea-aldehyde resin to produce composite microspheres. After removing moisture and organic matter, it is calcined at high temperature to obtain a micron-scale porous Zirconium dioxide spheres have sufficient rigidity and high chemical stability and can be used as HPLC column packing. However, the obtained porous zirconia microspheres are used as full-pore separation packing. Due to the axial diffusion of the sample in the packing, mass transfer is difficult. The process and separation time are longer, and the mechanical strength is affected by the pores, so that the pressure range that the full-pore packing can withstand is limited

Method used

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  • Core-shell type porous zirconium dioxide material and preparation method thereof
  • Core-shell type porous zirconium dioxide material and preparation method thereof
  • Core-shell type porous zirconium dioxide material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Dissolve 200 g of zirconium n-propoxide in a mixed solution of 2500 mL of ethanol and 1000 mL of deionized water. 20 mL of 30% ammonia solution was added, mechanically stirred at 600 rpm for 30 seconds at 35° C., and then the mixture was slowly magnetically stirred at room temperature for 3 hours to generate nano-sized zirconia particles. Distill to reduce the volume of the mixture to 800mL, and filter to obtain a colorless, clear high-purity zirconia sol, and add a small amount of ammonia to adjust the pH to about 7-8. The content of nano zirconium dioxide particles in the zirconium dioxide sol is 6.5%, and the particle diameter is 25nm.

Embodiment 2

[0042] Dissolve 150 g of zirconium isopropoxide in a mixed solution of 2000 mL of ethanol and 500 mL of deionized water. 5 mL of 30% ammonia solution was added, mechanically stirred at 600 rpm for 30 seconds at 25° C., and then the mixture was slowly magnetically stirred at room temperature for 3 hours to generate nano-sized zirconia particles. Distill to reduce the volume of the mixture to 500mL, and filter to obtain a colorless, clear high-purity zirconia sol, and add a small amount of ammonia to adjust the pH to about 8-9. The content of nano zirconium dioxide particles in the zirconium dioxide sol is 7.1%, and the particle diameter is 15nm.

Embodiment 3

[0044] Add 1240 mL of deionized water, 37 g of urea, 60 g of 37% formaldehyde solution, and the zirconium sol prepared in Example 1 into a 5000 mL beaker in sequence, and stir until the urea dissolves.

[0045] Add 2 mL of nitric acid under rapid stirring and continue rapid stirring for 15 seconds. After standing for 30 minutes, a white precipitate, that is, zirconium dioxide-urea-formaldehyde resin composite microspheres, was precipitated.

[0046] Filtration, washing, drying, and microscopic examination revealed that the particle size of the zirconia composite microspheres was 2.5 μm, and the spherical shape was uniform.

[0047] The above-mentioned zirconia composite microspheres were calcined at a high temperature of 1100° C. for 15 hours. 50 g of zirconia solid spheres were obtained.

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Abstract

The invention discloses a preparation method of a core-shell type porous zirconium dioxide material. The method includes the steps of preparing a zirconium dioxide solid core through the combination of a sol-gel process and a calcination process with zirconium alkoxide as precursors, forming a porous shell layer by alternately wrapping the surface of the solid core by polyester electrolyte and nanometer zirconium dioxide particles, obtaining a core-shell type porous zirconium dioxide microballoon sphere, conducitng high-temperature roasting and acid treatment to obtain the core-shell type porous zirconium dioxide material. The invention further discloses the core-shell type porous zirconium dioxide material prepared according to the preparation method. The core-shell type porous zirconium dioxide material comprises the solid core and the porous shell layer, wherein zirconium dioxide serves as a matrix. The core-shell type porous zirconium dioxide material is uniform in spherical shape and controllable in particle size, and the core-shell type porous zirconium dioxide material has the advantages of being wide in suitable pH range, suitable for sample separation and analysis under the alkaline mobile phase, capable of being rapidly separated out, capable of bearing high pressure, and the like when used as HPLC chromatography filler.

Description

technical field [0001] The invention belongs to the technical field of fillers, in particular to a core-shell porous zirconia material and a preparation method thereof. Background technique [0002] High performance liquid chromatography (HPLC) is widely used in the fields of science and production, such as petroleum, chemical industry, medicine, environmental protection, food and biotechnology downstream analysis and separation tasks, most of which can be completed by HPLC, and has It has the advantages of fast separation speed, high resolution, high sensitivity, reusable chromatographic column, less sample consumption and easy recovery. The key technology to realize HPLC separation lies in chromatographic packing, which determines the application range, separation efficiency, separation mechanism, mobile phase composition, and even detection methods of HPLC, which are important factors in HPLC separation. At present, the most widely used chromatographic column filler is s...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/285B01J20/30C01G25/02C04B35/628
Inventor 周丽李海涛
Owner 天津博纳艾杰尔科技有限公司
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