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Preparation method of magnetic mesoporous zirconium dioxide compound microsphere

A technology of zirconia and composites, which is applied in the field of magnetic nanocomposite microspheres, can solve problems such as complicated procedures, difficult to remove templates, adverse effects of micro-nano structures on magnetic response performance, etc., and achieve good repeatability and stable physical and chemical properties , the effect of good application prospects

Inactive Publication Date: 2014-02-26
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the high-temperature heat treatment and organic extraction process are not only complex procedures, it is difficult to completely remove the template, and it will also adversely affect the magnetic response performance and micro-nano structure.

Method used

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  • Preparation method of magnetic mesoporous zirconium dioxide compound microsphere
  • Preparation method of magnetic mesoporous zirconium dioxide compound microsphere
  • Preparation method of magnetic mesoporous zirconium dioxide compound microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) At room temperature, weigh 0.300g Fe 3 o 4 and 0.300g poly(4-styrene sodium sulfonate), and ultrasonically disperse the two in 100ml deionized water, and ultrasonically disperse for 30min to obtain Fe 3 o 4 Suspension, separated by magnet and washed to obtain polyelectrolyte modified Fe 3 o 4 .

[0029] (2) The polyelectrolyte modified Fe obtained above 3 o 4 and 0.4755g zirconium oxychloride octahydrate were added in 200ml absolute ethanol, and ultrasonic 30min obtained polyelectrolyte modified Fe 3 o 4 suspension. Measure 133ml of absolute ethanol, 27ml of deionized water, and 0.5625ml of ammonia water into a beaker, and stir to form an ethanol solution. Under the conditions of ultrasonic power of 200W and mechanical stirring rate of 150r / h, the above-mentioned ethanol solution was added to the polyelectrolyte modified Fe at a rate of 50ml / h using a syringe pump 3 o 4 in suspension. After reacting for 8 hours, Fe with core-shell structure can be obtain...

Embodiment 2

[0034] (1) At room temperature, weigh 0.415g ZnFe 2 o 4 and 0.600g polyacrylic acid, and ultrasonically disperse the two in 100ml deionized water, and ultrasonically disperse for 30min to obtain ZnFe 2 o 4 Suspension, separated by magnet and washed to obtain polyelectrolyte modified ZnFe 2 o 4 .

[0035] (2) The polyelectrolyte modified ZnFe obtained above 2 o 4and 0.915g zirconium isopropoxide were added in 200ml absolute ethanol, and ultrasonic 30min obtained polyelectrolyte modified ZnFe 2 o 4 suspension. Measure 110ml of absolute ethanol, 60ml of deionized water, and 0.600ml of ammonia water into a beaker, and stir to form an ethanol solution. Under the condition that the ultrasonic power is 150W and the mechanical stirring rate is 100r / h, use a syringe pump to add the above mixed solution to the polyelectrolyte modified ZnFe at a rate of 10ml / h 2 o 4 in suspension. After 10 hours of reaction, ZnFe with core-shell structure can be obtained 2 o 4 ZrO 2 Compos...

Embodiment 3

[0039] (1) At room temperature, weigh 0.220g CoFe 2 o 4 and 0.900g polyethylene sulfonic acid, and ultrasonically disperse the two in 100ml deionized water, and ultrasonically disperse for 30min to obtain CoFe 2 o 4 Suspension, separated by magnet and washed to obtain polyelectrolyte modified CoFe 2 o 4 .

[0040] (2) The polyelectrolyte modified CoFe obtained above 2 o 4 and 0.5250g zirconium n-butoxide were added to 200ml absolute ethanol and ultrasonicated for 30min to obtain polyelectrolyte modified CoFe 2 o 4 suspension. Measure 150ml of absolute ethanol, 10ml of deionized water, and 0.7125ml of ammonia water into a beaker, and stir to form an ethanol solution. Under the conditions of ultrasonic power of 100W and mechanical stirring rate of 75r / h, the above mixed solution was added to the polyelectrolyte modified CoFe at a rate of 10ml / h using a syringe pump. 2 o 4 in suspension. After 12 hours of reaction, the core-shell structure of CoFe 2 o 4 ZrO 2 Compo...

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Abstract

The invention relates to a preparation method of a magnetic mesoporous zirconium dioxide compound microsphere. The preparation method comprises the steps of (1) preparing polyelectrolyte modified magnetic powder; (2) ultrasonically dispersing the polyelectrolyte modified magnetic powder and zircon salt into absolute ethyl alcohol, carrying out ultrasonic treatment to obtain a polyelectrolyte modified magnetic powder suspension liquid, then, adding a deionized water solution of ethanol and ammonium hydroxide, reacting, and then, separating by using a magnet to obtain a magnetic zirconium oxide compound microsphere with a core-shell structure; (3) ultrasonically dispersing the magnetic zirconium oxide compound microsphere into the deionized water solution of ethanol and ammonium hydroxide, carrying out hydrothermal reaction after ultrasonic treatment to obtain a product, separating the product by using the magnet, washing, and carrying out vacuum freeze drying to obtain the magnetic mesoporous zirconium dioxide compound microsphere. The preparation method provided by the invention is simple in operation, controllable in process and good in repeatability; the prepared magnetic mesoporous zirconium dioxide compound microsphere is uniform in size and pore diameter distribution, large in specific surface area, stable in physicochemical property, not easy to agglomerate and good in dispersibility, and can be applied to the fields such as environment control, proteomics and the like.

Description

technical field [0001] The invention belongs to the field of magnetic nanocomposite microspheres, in particular to a preparation method of magnetic mesoporous zirconia composite microspheres. Background technique [0002] In recent years, magnetic nanocomposite microspheres have attracted more and more attention. This is because magnetic nanocomposite microspheres have excellent magnetic response characteristics and are easy to be functionalized and modified. They are widely used in medical diagnosis, drug sustained release, biomolecular separation and purification, and other fields. However, mesoporous materials based on magnetic nanocomposite microspheres have the advantages of high specific surface area, high pore volume, and uniform and controllable pore size distribution, which show great advantages in the fields of environmental pollution control, protein separation and purification, etc. [0003] Zirconium dioxide is an important functional material, which has import...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
Inventor 王宏志赵德王刚李耀刚张青红
Owner DONGHUA UNIV
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