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Preparation method of zirconium dioxide microspheres

A zirconia and microsphere technology, applied in zirconia and other directions, can solve the problems of poor particle size uniformity and poor size controllability of zirconia microspheres, and achieve the effect of uniform particle size and controllable size

Pending Publication Date: 2020-08-07
无锡迈科为生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the zirconia microspheres prepared by the existing technology have poor particle size uniformity and poor size controllability. How to prepare zirconia microspheres with uniform particle size and controllable size is still a difficult point

Method used

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  • Preparation method of zirconium dioxide microspheres
  • Preparation method of zirconium dioxide microspheres

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preparation example Construction

[0022] The embodiment of the present invention provides a preparation method of zirconia microspheres, comprising:

[0023] adding the seed microspheres into the aqueous solution containing the dispersant, fully stirring to form a uniformly dispersed seed mixture, the seed microspheres accounting for less than 60% of the weight of the seed suspension;

[0024] Mix the initiator and dispersant evenly to obtain an initiator solution;

[0025] Mix zirconium n-propoxide, alcohol solvent and ammonia water evenly to obtain a precursor mixture;

[0026] Under ultrasonic conditions, the initiator solution is first dropped into the seed mixed solution, and then the precursor mixed solution is added dropwise to react to obtain polymer / zirconia composite microspheres;

[0027] vacuum drying the polymer / zirconia microspheres;

[0028] The dried polymer / zirconia microspheres are heated step by step, the polymer is removed, and finally the zirconia microspheres are obtained.

[0029] In ...

Embodiment 1

[0040] Add styrene-divinylbenzene copolymer seed microspheres (particle size 855 μm, CV=3%) into the aqueous solution containing dextrin, stir well to form a uniformly dispersed seed mixture, styrene-divinylbenzene copolymer The seed microspheres account for 45% of the seed suspension weight; the dextrin weight is 8% of the seed microspheres weight; the benzoyl peroxide is added into the aqueous solution containing polyvinylpyrrolidone and then emulsified to form an initiator solution for subsequent use; Ionized water, 400mL of isopropanol, 5mL of 28% ammonia water and 50mL of ethanol solution containing 10% n-propoxide zirconium were mixed and ultrasonicated for 2 hours to obtain a precursor mixture.

[0041] At 70°C, add the initiator solution dropwise into the seed mixture within 60 minutes to grow the seed microspheres, and stop adding the initiator solution after reaching the preset microsphere particle size. Then the precursor mixed solution is added dropwise to react to...

Embodiment 2

[0044] Add styrene-divinylbenzene copolymer seed microspheres (particle size 0.5 μm, CV=2.8%) into the aqueous solution containing dextrin, stir well to form a uniformly dispersed seed suspension, and styrene-divinylbenzene copolymerization The seed microspheres account for 52% of the seed suspension weight; the dextrin weight is 8% of the seed microsphere weight; benzoyl peroxide is added to the aqueous solution containing polyvinylpyrrolidone and then emulsified to form an initiator solution for subsequent use; 40mL Deionized water, 400 mL of isopropanol, 5 mL of 28% ammonia water and 50 mL of ethanol solution containing 10% n-propoxide zirconium were mixed and then ultrasonicated for 2 hours to obtain a precursor mixed solution.

[0045] At 70°C, the mixed porogen and initiator solution of polyethylene glycol, urea and ammonium sulfate with potassium chloride and sodium chloride was added to the seed suspension to grow the seed microspheres within 60 minutes to reach the pre...

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Abstract

The invention discloses a preparation method of zirconium dioxide microspheres, which comprises the following steps: adding seed microspheres into an aqueous solution containing a dispersing agent, and sufficiently stirring to form a uniformly dispersed seed mixed solution; uniformly mixing an initiator and a dispersing agent to obtain an initiator solution; the preparation method comprises the following steps: uniformly mixing zirconium n-propoxide, an alcohol solvent and ammonia water to obtain a precursor mixed solution; dropwise adding the initiator solution into the seed mixed solution, then dropwise adding the precursor mixed solution, and reacting to obtain polymer / zirconium dioxide composite microspheres; carrying out vacuum drying on the polymer / zirconium dioxide microspheres; andheating the dried polymer / zirconium dioxide microspheres section by section, and removing the polymer to obtain the zirconium dioxide microspheres. According to the method, an initiator solution anda precursor mixed solution are sequentially added into a seed mixed solution, so that the grain size of the obtained zirconium dioxide microspheres is uniform while the growth size of the seed microspheres is effectively controlled.

Description

technical field [0001] The invention relates to a preparation method of microspheres, belonging to the technical field of preparation of zirconia microspheres. Background technique [0002] Zirconium dioxide has excellent physical and chemical properties such as high mechanical strength, good chemical stability, acid and alkali resistance, high melting point and boiling point, and high specific surface area. It is used in solid fuel cells, chemical sensors, adsorption, separation, chromatographic packing and catalysis. field has a wide range of applications. Taking porous zirconia microspheres as an example, porous zirconia materials have played a prominent role in the field of catalysis in recent years, such as hydrogenation of carbon monoxide, Friedel-Crafts alkylation, esterification, and isomerization of alkanes. Porous zirconia microspheres have broad application prospects in the fields of catalysis, adsorption and separation due to their spherical shape, high specific...

Claims

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Application Information

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IPC IPC(8): C01G25/02
CPCC01G25/02C01P2004/61C01P2006/16C01P2006/12
Inventor 阳承利
Owner 无锡迈科为生物科技有限公司
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