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Method for continuous preparation of nanometer-sized hydrous zirconia sol

A technology of hydrated zirconia and zirconium sol, which is applied in the field of reconciliation, and can solve the problems of not being able to provide hydrated zirconia sol

Inactive Publication Date: 2005-11-02
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
  • Method for continuous preparation of nanometer-sized hydrous zirconia sol
  • Method for continuous preparation of nanometer-sized hydrous zirconia sol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0103] 0.2 mol of zirconium oxychloride and 1 g of hydroxypropylmethylcellulose were dissolved in 1 liter of a solvent mixture of 2-propanol and water (molar ratio 0.94) to prepare a zirconium saline aqueous solution. Such as Figure 5b As shown, two spiral type reaction tubes each having an inner diameter of 9.5 mm and a length of 5 m and composed of Pyrex glass were installed in a stainless steel vessel to form a condenser type tube reactor. The zirconium salt aqueous solution was supplied to the reaction tube at a flow rate of 403 cc / min at a temperature of about 10°C. A vapor-phase heating medium composed of hot water and ethanol (molar ratio 1:1) was supplied to the inside of the reactor (outside of the reaction tube) at a temperature of 98°C, and then condensed there. As a result, the outlet temperature of the reaction tube could be 74°C. The pH value of the suspension discharged from the outlets of the two reaction tubes was controlled to 9.1 by adding 0.8 N ammonia w...

Embodiment 2

[0108] 0.04 mol of zirconium oxychloride and 0.6 g of hydroxypropyl cellulose were dissolved in 1 liter of a solvent mixture of 1-propanol and water (1.7 molar ratio) to prepare a zirconium salt aqueous solution. Such as Figure 7a As shown, a 37 stainless steel reaction tube with an inner diameter of 3.37 mm and a length of 500 mm forms a shell-tube heat exchange type tubular reactor. An aqueous zirconium salt solution was fed to the reaction tube at a total flow rate of 1150 cc / min at a temperature of about 8°C. A vapor-phase heating medium obtained by heating 2-propanol was supplied to the shell (outside of the reaction tube) of the reactor at a temperature of 84° C., and then condensed there. As a result, the outlet temperature of the reaction tube could be 78°C.

[0109] The hydrated zirconia sol was continuously prepared by adding and mixing 2.0N ammonia water in the discharge pipe of the suspension mixer to control the pH to 5.6.

[0110] Five (5) drops of the result...

Embodiment 3

[0112] 0.2 mol of zirconium oxychloride and 7 g of polyvinyl alcohol were dissolved in 1 liter of a solvent mixture of 2-propanol and water (0.94 molar ratio) to prepare a zirconium salt aqueous solution. Such as Figure 4 As shown, the tubular reactor used had three (3) straight stainless steel tubes of concentric annular cross-section, 300 mm in length, and gauges of 1 / 4 inch, 3 / 8 inch, and 3 / 4 inch, respectively. The zirconium salt aqueous solution was fed to the concentric annulus of the 1 / 4 inch and 3 / 8 inch reaction tubes at a temperature of about 8°C at a flow rate of 30 cc / min. The hydrocarbon-based heat carrier oil heated to 95°C is simultaneously fed into the 1 / 4 inch pipe and between the 3 / 8 inch pipe and the 3 / 4 inch pipe against the flow direction of the zirconium salt aqueous solution, so as to have a concentric The temperature of the suspension at the outlet of the reaction tube of circular cross-section may be 82°C. The suspension was contacted with ammonia g...

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Abstract

The present invention relates to a method a method for continuous preparation of a well dispersed spherical hydrous zirconia particles with an average diameter (dp) of 1~1,000 nm in the form of sol solution, which method comprises continuously supplying the aqueous solution of a zirconium salt at a concentration of 0.001~0.5 mole / l to a reactor consisting of one or more than two reaction tubes at a temperature of less than 25 DEG C, heating the said aqueous solution in the reactor(s) in a continuous flow state up to the boiling point, and then discharging the said solution through the outlet of the said reactor(s). Contrary to the method employing a conventional batch-type reactor or semi-continuous stirred-type reactor, the method for continuous preparation of a hydrous zirconia sol according to the present invention can allow various operational parameters to be controlled in a certain range and thus contributes to remarkably improve the quality of a hydrous zirconia sol to be prepared or of the zirconia powder obtainable as a 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: continuous preparation method of hydrated zirconia or zirconia hydrate) sol, the nano-scale spherical hydrated zirconia sol is prepared for functional ceramics such as abrasives, anti-wear materials, solid electrolytes in fuel cells, sensors, coatings, etc. 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 1-1000 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 1000 nm are dispersed in a colloidal state. Hydrated zirconia can be prepared by precipitating a z...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00C01G25/02
CPCC01P2004/32C01P2004/64B82Y30/00C01P2004/03C01P2004/51C01P2004/62C01G25/02C01G25/00B82B3/00
Inventor 金希永朴容起尹卿求林亨燮
Owner KOREA RES INST OF CHEM TECH
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