Method for continuous preparation of nanometer-sized hydrous zirconia sol using microwave

A technology of hydrated zirconia and zirconia sol, which is applied in zirconia, chemical instruments and methods, nanotechnology for materials and surface science, etc., and can solve the problems of not being able to provide hydrated zirconia sol

Inactive Publication Date: 2005-07-13
KOREA RES INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] These conventional methods of preparing hydrous zirconia do not provide the means to prepare in large quantities the hydrous zirconia sols required in the preparation of spherical zirconia particles having an average diameter of less than about 250 nm and a small particle size distribution

Method used

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  • Method for continuous preparation of nanometer-sized hydrous zirconia sol using microwave
  • Method for continuous preparation of nanometer-sized hydrous zirconia sol using microwave
  • Method for continuous preparation of nanometer-sized hydrous zirconia sol using microwave

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0118] 0.04 mol of zirconium oxychloride and 1 g of hydroxypropyl cellulose were dissolved in 1 liter of a solvent mixture of 1-propanol and water (1.2 molar ratio) to prepare a zirconium salt aqueous solution. At a temperature of about 10° C., the zirconium salt aqueous solution was continuously fed at a flow rate of 403 cc / min into a quartz glass tube having an inner diameter of 16 mm equipped in a stainless steel reactor. Microwaves of 2,450 MHz were irradiated to the solution to heat the solution so that the outlet temperature of the reaction tube could reach 74°C. The pH value of the suspension discharged from the outlet of the reaction tube was controlled to 7.5 by adding 2N ammonia water in the mixer to continuously prepare the hydrated zirconia sol.

[0119] The hydrated zirconia particles were filtered from the obtained hydrated zirconia sol by means of a 20-nm sized filter, followed by repeated washing with distilled water until no Cl was detected. - The hydrated zi...

Embodiment 2

[0123] 0.06 mol of zirconium oxychloride and 0.4 g of hydroxypropyl cellulose were dissolved in 1 liter of a solvent mixture of 2-propanol and water (molar ratio 0.8) to prepare a zirconium saline aqueous solution. At a temperature of about 7°C, an aqueous zirconium salt solution was continuously fed at a flow rate of 910 cc / min into a quartz glass tube having an inner diameter of 16 mm provided in the first stainless steel reactor zone. Microwaves of 2,450 MHz were irradiated to the solution to heat the solution so that the outlet temperature of the reaction tube could reach 45°C.

[0124] The intermediate product flowing from the reaction tubes was continuously fed to the reaction tubes of the second reaction zone in the form of a shell-and-tube heat exchanger with 8 stainless steel reaction tubes of internal diameter 6 mm. Steam at about 106°C as a heating medium is supplied to the shell side and compressed so that the temperature of the suspension flowing out from the reac...

Embodiment 3

[0128] 0.01 mol of zirconium oxychloride and 0.4 g of hydroxypropyl cellulose were dissolved in 1 liter of a solvent mixture of 2-propanol and water (1.6 molar ratio) to prepare a zirconium saline aqueous solution. At a temperature of about 12°C, an aqueous zirconium salt solution was continuously fed at a flow rate of 362 cc / min into a quartz glass tube having an inner diameter of 12 mm provided in the first stainless steel reactor zone. Microwaves of 2,450 MHz were irradiated to the solution to heat the solution so that the outlet temperature of the reaction tube could reach 53°C.

[0129] The intermediate product flowing out from the outlet of the reaction tube was supplied to a second stainless steel reaction zone having a stirring type vessel and an inner diameter of 120 mm and a height of 600 mm. In the second reaction zone, the liquid height is maintained at 400 mm, and the intermediate product is stirred with a stirrer installed in the axial direction of the reactor. ...

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Abstract

The present invention relates to a method for continuously preparing a hydrated zirconia sol dispersed by nanoscale spherical hydrated zirconia particles having an average diameter (dp) of 1 to 250 nm, the method comprising dissolving a zirconium salt solution with a concentration of 0.001 to 0.2 mol / l in aqueous solution The solution is fed into a reactor consisting of one or more reaction tubes, and then microwaves are irradiated onto the flow of the aqueous solution in the reactor so that the aqueous solution can be heated in a flowing state. Compared with conventional batch reactors or semi-continuous stirred reactors, the method for continuously preparing hydrated zirconia sol according to the present invention can allow various operating parameters to be controlled within a certain range, thereby significantly improving The mass of the hydrous zirconia sol prepared or the zirconia powder obtained as the final product.

Description

technical field [0001] The invention relates to a preparation method of nanoscale hydrated zirconia sol, in particular to a nanoscale spherical hydrated zirconia (ZrO 2 ·nH 2 O) The continuous preparation method of sol, this nano-scale spherical hydrated zirconia sol is prepared as functional ceramics such as abrasives, anti-wear materials, solid electrolytes in fuel cells, sensors, coatings, etc. and structural ceramics such as mechanical parts, optical connections Pure zirconia (ZrO 2 ) or fine particles of zirconia-based composite metal oxides. [0002] The present invention more particularly relates to a process for the continuous preparation of spherical hydrous zirconia in the form of a sol having an average particle size (diameter) of about 1-250 nm and a small particle size distribution. [0003] A hydrated zirconia sol is a solution in which hydrated zirconia particles having a diameter of about 1 to 250 nm are dispersed in a colloidal state. Hydrated zirconia can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00C01G25/02C10G25/00C10G25/02
CPCB01J19/126B01J2219/0877B01J2219/1227B82Y30/00C01G25/02C01P2004/64C01G25/00B82B3/00
Inventor 金希永朴容起尹卿求林亨燮
Owner KOREA RES INST OF CHEM TECH
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