Micrometer level porous zirconium dioxide spherical granules

A zirconia, micron-scale technology, applied in zirconia and other directions, can solve problems such as unsatisfactory repeatability, and achieve the effect of narrow particle size distribution and adjustable pore size

Inactive Publication Date: 2002-03-27
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the key raw materials (zirconium hydrosol) used in these two patents are all purchased from outside, and the repeatability

Method used

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  • Micrometer level porous zirconium dioxide spherical granules
  • Micrometer level porous zirconium dioxide spherical granules
  • Micrometer level porous zirconium dioxide spherical granules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 100g of zirconium oxychloride to a 500mL three-necked round-bottomed flask, add 280mL of deionized water and 3mL of acetylacetone, stir well, add dropwise 25% ammonia water and heat the reactant from room temperature to 85°C, maintaining the pH of the solution at 1- 2. Continue stirring for 10h to obtain ZrO 2 Hydrosol. The hydrosol concentration is 20% (w / w), and its average colloidal particle diameter measured by photon correlation spectrometer is 79.8nm (see Figure 1)

Embodiment 2

[0024] Get the ZrO that embodiment 1 prepares 2 Add 200mL of hydrosol to a 500mL three-necked round-bottom flask, adjust pH=1.2, add 20g of urea, stir to dissolve completely, add 25mL of 38% formaldehyde solution at 15°C, stir rapidly for 2min, stop stirring, and react at 15°C for 12h, Add 1% NaOH solution to pH = 8, terminate the reaction, ZrO 2 -The resin composite ball sinks to the bottom of the reactor, the appearance is white, and the particle size is 12-15μm. Filter, wash the product with water, then transfer it to a four-neck flask, add isoamyl acetate to remove water azeotropically, and the white composite ball turns light yellow at this time. Then put the product in a vacuum drying oven, maintain a vacuum degree of 0.06MPa, dry at 120°C for 12 hours, and dry at 200°C for 24 hours. In a high-temperature furnace with a thickness of ≤5mm, the temperature rises from room temperature to 200°C at 4°C / min, then from 200°C to 300°C at 1°C / min, from 300°C to 700°C at 2°C / min...

Embodiment 3

[0026] Soak the micron-sized porous zirconia spheres prepared in Example 2 in 6mol / L hydrochloric acid for 24h, then wash with distilled water until neutral; then soak in 1mol / L sodium hydroxide solution for 24h and wash with distilled water until neutral properties; finally put it in a high-pressure axe and add an appropriate amount of water, heat treatment at 200 ° C for 8 hours. The zirconium colloidal microspheres treated above can be directly used in normal phase chromatography, especially suitable for the separation of basic compounds, and can be suitable for mobile phases in the range of pH=1-13. Figure 4 is an example of normal phase chromatographic separation of zirconium gel stationary phase.

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Abstract

The present invention relates to a technique for preparing micrometer-level porous zirconium dioxide spherulites, the grain size of more than 90% of them is 1-10 plus or minus 0.1 micrometer, and pore size is 1-150 nm. Said invented technique includes the following steps: using zirconium salt to prepare nanometer-level ZrO2 hydrosol, under the condition of pH=0.5-3 utilizing polymerization induced colloid coagulation method to make ZrOz hydrosol and urea-formaldehyde resin form composite spherulites, removing water content and organic substance from composite spherulite, and adopting programmed heating, sintering and fortifying process of obtain the invented micrometer-level porous zirconium dioxide spherulites. Said invention features narrow grain size distribution, adjustable pore size,enough rigidity and high chemical stability, can be used as packing material of HPLC column.

Description

technical field [0001] The present invention relates to the preparation of zirconium dioxide, in particular to the preparation of micron-scale porous zirconium dioxide pellets used as high-performance liquid chromatography column packing. Background technique [0002] High-performance liquid chromatography (HPLC) is widely used in the fields of science and production, such as petroleum, chemical, pharmaceutical, environmental protection and other industries, most of which can be completed by HPLC; and in the purification process of downstream products of biotechnology, Membrane separation is often used as the primary treatment first, and then HPLC is used as high-resolution separation; the current preparative column with a column diameter of tens of centimeters has replaced the classic separation operation in many high-tech enterprises, and its efficiency is as high as that of the classic method. comparable. [0003] Column packing is always one of the k...

Claims

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Application Information

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IPC IPC(8): C01G25/02
Inventor 左育民杨俊佼
Owner NANKAI UNIV
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