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Method for preparing nano zirconium oxide by using spray granulator

Active Publication Date: 2020-10-27
宁德三祥纳米新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a method for preparing nano-zirconia by using a spray granulator to solve the problem of agglomeration of nano-zirconia in the drying process in the method for preparing nano-zirconia by a spray granulator in the prior art. question

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  • Method for preparing nano zirconium oxide by using spray granulator

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Effect test

Embodiment 1

[0037] At room temperature, weigh 17kg of zirconium oxychloride (containing crystal water) and 1.1kg of yttrium nitrate hexahydrate according to the ratio of 3Y, dissolve them in 25L of deionized water, and record it as solution A; mix 5kg of acrylamide (AM), 200g of N,N'-methylenebisacrylamide (MBAM) was dissolved in solution A, and 2ml of tetramethylethylenediamine (TEMED) was added dropwise, which was recorded as solution B; 5g of ammonium persulfate was weighed and added to the solution Stir in B, then immediately introduce the solution into the granulator for thermal reaction; obtain zirconium source gel particles; soak it in excess ammonia water (25% concentration, 60L) for 2 hours; at this time, the particles have changed from transparent to White, wash and filter the particles several times until the chloride ion is less than 20ppm, then dry them in an oven (90-110°C) to obtain micron-sized zirconia precursor gel particles with a certain strength; put the particles at 8...

Embodiment 2

[0039] At room temperature, weigh 17kg of zirconium oxychloride (containing crystal water) and 0.56kg of yttrium chloride according to the ratio of 3Y, dissolve them in 25L of deionized water, and record it as solution A; mix 5kg of acrylamide (AM), 200g of N , N'-methylenebisacrylamide (MBAM) was dissolved in solution A, and 2ml of tetramethylethylenediamine (TEMED) was added dropwise, which was recorded as solution B; 5g of ammonium persulfate was weighed and added to solution B Stir in medium, then immediately introduce the solution into the granulator for thermal reaction; obtain zirconium source gel particles; soak it in excess ammonia water (25% concentration, 60L) for 2 hours; at this time, the particles have changed from transparent to white , wash and filter the particles several times until the Cl- ions are less than 20ppm, and then dry them in an oven (90-110°C) to obtain micron-sized zirconia precursor gel particles with a certain strength; the particles are heated ...

Embodiment 3

[0041] A kind of method utilizing spray granulator to prepare nano zirconia, comprises the following steps:

[0042] Step 1: Mix soluble zirconium source and soluble yttrium source, mix with deionized water, prepare solution A of 0.5mol / L, the total weight of zirconium source and yttrium source is M1; zirconium element and yttrium element in the reaction solution A The molar ratio is 97:6; the soluble zirconium source is any one of zirconium oxychloride and zirconium acetate or a combination of both; the soluble yttrium source is yttrium chloride, yttrium oxalate, yttrium nitrate, and yttrium acetate Any one or two combinations of them;

[0043]Step 2: Cool solution A to 0°C, weigh acrylamide with a weight of M2 and N,N'-methylenebisacrylamide with a weight of M3, put them into solution A to dissolve, and drop into tetramethyldiethyl Amine, to obtain solution B, and keep cooling at a temperature of 0°C, wherein M2:M1 is 1:3, M3:M2 is 1:15;

[0044] Step 3: Add ammonium persu...

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Abstract

The invention discloses a method for preparing nano zirconium oxide by using a spray granulator, and provides a method for preparing monodisperse nano zirconium oxide. The method comprises the following steps: preparing a gel system and a zirconium source solution according to the heating and drying characteristics of a spray granulator to form micron-sized micro-particle gel, soaking gel particles in ammonia water, drying the gel after the gel is completely discolored, and calcining at 800 DEG C for 4 hours to obtain the nano zirconium powder with favorable properties. Compared with a traditional gel method process, chemical gel is adopted, the method has the advantages of being small in colloidal particle, easy to react, clean, load and transport and the like, and in the process, the problem of nano-powder agglomeration is solved from the source after the gel is firstly subjected to the reaction.

Description

technical field [0001] The invention relates to the technical field of material science, in particular to a method for preparing nano zirconia by using a spray granulator. Background technique [0002] Nano zirconia powder helps to optimize the performance of zirconia ceramics, and the preparation of nano zirconia powder has always been a research hotspot. The manufacture of high-performance ceramic materials has high requirements for the powder used. In addition to the requirements for accurate, uniform chemical composition and phase composition of the powder, and low impurity content, there are strict requirements for the shape and size of the particles in the powder. It can be roughly summarized as follows: [0003] 1) The particle size is small; [0004] 2) The particle size distribution range is narrow; [0005] 3) The particle shape is preferably spherical or equiaxed; [0006] 4) There is no agglomeration or a small degree of agglomeration among the particles. ...

Claims

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Application Information

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IPC IPC(8): C04B35/626C04B35/48
CPCC04B35/62695C04B35/62675C04B35/48
Inventor 姜波骆兵周志永
Owner 宁德三祥纳米新材料有限公司
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