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Process method for preparing nano zirconium dioxide by rapid homogeneous nucleation

A technology of nano-zirconia and process method, applied in the direction of zirconia, nanotechnology, nanotechnology, etc., can solve the problems of inorganic ammonium salt recovery pollution, particle agglomeration, loss of industrial utilization value, etc., and achieve particle size and morphology Controllable, narrow particle size distribution range, and the effect of reducing agglomeration

Active Publication Date: 2014-07-30
JIANGSU JIUJIUJIU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the use of surfactants and dispersants pollutes the recovery of by-product inorganic ammonium salts, which loses the value of industrial utilization
CN102249304A adopts this method, but it does not solve the problem of particle agglomeration in the co-precipitation process

Method used

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  • Process method for preparing nano zirconium dioxide by rapid homogeneous nucleation
  • Process method for preparing nano zirconium dioxide by rapid homogeneous nucleation

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Will be equipped with stabilizer cation Y 3+ (0.03mol) zirconium oxychloride (0.97mol) aqueous solution (5L) and 4mol ammonia gas were used to prepare the precursor in a jet reactor. The precursor obtained from the collection tube was washed to 2 . Tetragonal crystal products account for 94%, the product particle size distribution is concentrated around 120nm, and the product surface area is 18.5m 2 / g.

[0020] Described jet reactor comprises injector, and injector communicates with accepting cavity 3, and receiving hopper 4 is arranged below accepting cavity; Described injector comprises shower nozzle 1, injection pipe 2, and nozzle outlet communicates with the injection pipe connected with receiving chamber, The nozzle has two inlets 5 and 6, one of which is fed into zirconium salt solution, and the other is fed into ammonia or the mixed gas of ammonia and nitrogen. The injection pipe is in the form of an involute bell mouth. The length-to-diameter ratio of the r...

Embodiment 2

[0022] Will be equipped with stabilizer cation Y 3+ (0.08mol) zirconium oxychloride (0.92mol) aqueous solution (8L) and 4mol ammonia gas were used to prepare the precursor in a jet reactor. The precursor obtained from the collection tube was washed to 2 . Tetragonal crystal products account for 84%, the product particle size distribution is concentrated around 80nm, and the product surface area is 23.5m 2 / g. The jet reactor is the same as in Example 1.

Embodiment 3

[0024] Prepare pure zirconia nanopowder without adding mineralizers and stabilizer cations, hydrothermal synthesis conditions 250 ° C, pressure 4MPa, reaction time 24h, the rest are the same as in Example 1. The tetragonal phase is 92%, the particle size distribution is 100nm, and the specific surface area is 20.5 m2 / g. The jet reactor is the same as in Example 1.

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Abstract

The invention discloses a process method for preparing nano zirconium dioxide (ZrO2) by rapid homogeneous nucleation. The process method comprises the following steps of: reacting a stabilizer cation-mixed zirconium oxychloride aqueous solution with ammonia water in a jet reactor to prepare a precursor; washing the precursor obtained by a collecting pipe till chlorine ions reach the standard; adding a mineralizer; placing into a reaction kettle for hydro-thermal synthesis; and drying and grinding a precipitate obtained by hydro-thermal synthesis to obtain ZrO2. By using the jet reactor, a homogeneous system in a preparation course of the precursor is effectively maintained, OH<-> and Zr<4+> are bonded at high speed to generate a precursor crystal nucleus Zr(OH)4, the particle aggregation is reduced, and colloid particles with uniform particle size, narrow particle diameter distribution range and controllable particle appearance can be prepared. OH<-> and Zr<4+> react instantly through the jet reactor, the reaction speed is improved by more than 4 times, a dispersing agent does not need to be added, and the dosage of ammonia water is obviously reduced.

Description

technical field [0001] The invention relates to a process method for preparing nano zirconium dioxide by homogeneous rapid nucleation. Background technique [0002] Zirconium dioxide has excellent physical and chemical properties such as high melting point, high strength, and strong corrosion resistance. It is mainly used in the fields of manufacturing structural ceramics and functional materials. At present, the liquid phase co-precipitation method is widely used in the industry to prepare ZrO 2 powder. The basic principle is: use ammonia water to drip or reverse Zr 4+ Mixed salt solution with stabilizer cations to obtain insoluble co-precipitate, the reaction is a heterogeneous reaction, the molar concentration of the reaction solution gradually decreases with the addition of ammonia water, the precipitate is filtered to obtain the precursor, and then Calcination of the precursor to obtain ZrO 2 powder. CN200710052559.9, CN101830506A, CN101074116A, etc. all adopt this...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02B82Y30/00
Inventor 周涛沈同德朱建军周新基赵鑫峰
Owner JIANGSU JIUJIUJIU TECH
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