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Monodisperse macroporous titanium dioxide microsphere and preparing method thereof

A titanium oxide and microsphere technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of affecting analysis accuracy, rising cost of titanium oxide microspheres, and low resolution.

Inactive Publication Date: 2011-08-03
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The titanium oxide microspheres prepared by the existing sol-gel method and oil emulsification method have a wide particle size distribution of the obtained titanium oxide microspheres (the particle size distribution is about ± 3 μm) and the aperture and diameter of the gained titanium oxide microspheres The specific surface area is small (sol-gel method: the pore diameter is about 87 ; Oil emulsification method: the specific surface area is about 78m 2 / g) and other issues, and when it is used as a chromatographic (including HPLC) stationary phase, it will cause a lower degree of separation and affect the accuracy of analysis.
Existing polymerization-induced colloid method, because its step is loaded down with trivial details, can cause the cost of prepared titanium oxide microsphere to rise (not conducive to commercial application), and the specific surface area of ​​the titanium oxide microsphere that adopts existing polymerization-induced colloid method to make is relatively Small (about 36.7m 2 / g)

Method used

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  • Monodisperse macroporous titanium dioxide microsphere and preparing method thereof
  • Monodisperse macroporous titanium dioxide microsphere and preparing method thereof
  • Monodisperse macroporous titanium dioxide microsphere and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step (1) Add 0.0024mol of dodecylamine, 100ml of absolute ethanol, 0.006mol of acetylacetone, 0.012mol of tetrabutyl titanate into a 200ml round bottom flask, stir well at 20°C, add 0.3mol of deionized water, and the solution After turbidity, stop stirring, let stand for 45 minutes, filter, wash with absolute ethanol 2 to 4 times, and dry at room temperature (25°C to 30°C) to obtain a solid.

[0031] Step (2) Add 1 g of the solid obtained in step (1), 0.2 g of urea, add 16 ml of absolute ethanol, and 4 ml of deionized water, place it in an autoclave lined with polytetrafluoroethylene, let it stand at 130 ° C for 8 hours, and after cooling Filter, wash with acetone and methanol for 2 to 3 times in sequence, dry in vacuum at high temperature for 6 hours, and place in a muffle furnace for sintering at 300°C for 6 hours to obtain the target product.

[0032] Utilize the scanning electron microscope to analyze, the measured particle size average size is 1.8μm, see figure 1 ...

Embodiment 2

[0037] Step (1) Add 0.1mol eicosamine, 1000ml absolute ethanol, 0.2mol acetylacetone, 0.10mol isopropyl titanate to a 2000ml round bottom flask, stir well at 40°C, add 5mol deionized water, and wait for the solution After turbidity, stop stirring, let stand for 60 minutes, filter, wash with absolute ethanol for 2-4, and dry at room temperature (25°C-30°C) to obtain a solid.

[0038] Step (2) Add 4 g of the solid obtained in step (1), 0.35 g of urea, add 54 ml of absolute ethanol, and 36 ml of deionized water, put them in an autoclave lined with polytetrafluoroethylene, let stand at 70 ° C for 36 hours, and cool After filtering, washing with acetone and methanol for 2 to 3 times, vacuum drying at high temperature for 10 hours, and sintering in a muffle furnace at 400° C. for 4 hours, the target product was obtained.

[0039] Using a scanning electron microscope to analyze, the average particle size measured is 2.8 μm, see figure 2 ;

[0040] Use N 2 The adsorption and desor...

Embodiment 3

[0044] In step (1) in Example 1, 0.012mol tetrabutyl titanate was replaced by 0.006mol tetrabutyl titanate, 0.3mol deionized water was replaced by 0.2mol deionized water, and other steps were operated according to Example 1 , also can obtain monodisperse titanium oxide microspheres similar to Example 1. Analyzed by a scanning electron microscope, the average particle size measured was 3.4 μm.

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Abstract

The invention relates to a titanium dioxide microsphere for high performance liquid chromatograph (HPLC) and a preparing method thereof. The titanium dioxide microsphere has a mesopore structure, the particle diameter (diameter) is 0.5-5 mum, and the specific surface area of the pore diameter is 100m<2> / g-130 m<2> / g. The titanium dioxide microsphere is prepared by an improved sol-gel and water thermal crystallisation method. The prepared titanium dioxide microsphere has the advantages of monodisperse property, mesopore structure, uniform particle size, conformance of the surface structure (large pore diameter and large specific surface area) to the chromatograph requirements, no need of grading treatment, and the like. In addition, in the process of the preparation method, the particle diameter of the object (titanium dioxide microspheres) can be controlled (i.e. the microspheres with different particle diameters can be easily obtained through adjusting different titanate concentrations), and the whole preparation process is simple and easy.

Description

technical field [0001] The invention relates to a monodisperse mesoporous titanium oxide microsphere for high performance liquid chromatography (HPLC) and a preparation method thereof. Background technique [0002] Silica gel has been widely used as a stationary phase in chromatography, including HPLC. However, since the chromatographic filler based on silica gel is only relatively stable in the range of pH 2 to 8, when analyzing some strong basic compounds, there will be more serious tailing phenomenon (even irreversible adsorption phenomenon) ), thus affecting the analysis results. [0003] Titanium oxide (TiO 2 ), due to its high mechanical strength, thermal stability, and chemical stability (applicable in the range of pH 1 to 14), it has been used as a method for normal phase chromatography, ion exchange chromatography, and reversed phase chromatography. Stationary Phase. But the usage is not ideal (may be related to the structure of the prepared titanium oxide micro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047
Inventor 粱鑫淼程三艳柯燕雄张永平金郁
Owner EAST CHINA UNIV OF SCI & TECH