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High-specific-surface area pure-monoclinic-phase zirconia preparation method

A high specific surface area, zirconia technology, applied in zirconia, chemical instruments and methods, chemical/physical processes, etc.

Active Publication Date: 2014-01-22
CHNA ENERGY INVESTMENT CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, limited by the specific surface area and impurity content, it is not suitable for use in the field of catalysts with high requirements for specific surface area and purity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 32.22 g of ZrOCl 2 ·8H 2 O was dissolved in 100 g of deionized water to form an acidic solution, which was then placed in a three-necked flask.

[0024] Put the three-necked flask into a 120°C oil bath and heat it while stirring, and reflux the water in the solution. After 24 hours, the solution becomes a slurry. Take out the slurry from the oil bath and adjust its pH value to 5.

[0025] The resulting slurry was filtered, and the filter cake was repeatedly washed with deionized water until no chloride ions were detected in the silver nitrate solution, and then dried in a drying oven at 120° C. for 12 hours to obtain a dry powder.

[0026] Put the dried powder above into a muffle furnace at 500° C. for 2 hours and calcinate to obtain pure monoclinic zirconia with high specific surface area.

Embodiment 2

[0028] 16 g of Zr(OH) 4 Put it into a three-necked flask, and then add 100 grams of nitric acid solution with a concentration of 20% by weight and 3 grams of polyvinyl alcohol (molecular weight: 1000-2000) to form an acidic solution.

[0029] Put the three-necked flask into a 110°C water bath to heat, while stirring, and reflux the water in the solution. After 48 hours, the solution becomes a slurry. Take out the slurry from the water bath, and adjust its pH value to 7 with ammonia water.

[0030] The resulting slurry was filtered, the filter cake was repeatedly washed with deionized water, and then dried in a drying oven at 120° C. for 6 hours to obtain a dry powder.

[0031] The above dried powder is placed in a muffle furnace at 500° C. for 1 hour and calcined to obtain pure monoclinic zirconia with a high specific surface area.

Embodiment 3

[0033] 26.73 g of ZrO(NO 3 ) 2 2H 2 O was dissolved in 100 g of deionized water to form an acidic solution, which was then placed in a three-necked flask.

[0034] Put the three-necked flask into an 80°C oil bath to heat, while stirring, and reflux the water in the solution. After 24 hours, the solution becomes a slurry. Take out the slurry from the oil bath, and adjust its pH value to 10.

[0035] The resulting slurry was filtered, the filter cake was repeatedly washed with deionized water, and then dried in a drying oven at 120° C. for 12 hours to obtain a dry powder.

[0036] Put the above dried powder into a muffle furnace at 500° C. for 4 hours and calcinate to obtain pure monoclinic zirconia with high specific surface area.

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Abstract

The invention discloses a high-specific-surface area pure-monoclinic-phase zirconia preparation method. The method sequentially comprises the steps that: (1) an acidic solution comprising zirconium ions and with a pH value lower than 5 is formed; (2) the solution is heated for 3-120h under a temperature of 80-300 DEG C, such that the solution forms monoclinic-phase zirconia colloidal particles or tiny solid particles comprising crystal water, wherein the zirconium concentration in the acidic solution is maintained unchanged. (3) the pH value of the solution is regulated to 5-11, such that the monoclinic-phase zirconia colloidal particles or tiny solid particles are deposited; (4) the solution is filtered; an obtained filter cake is washed until no impurity ion is left; and drying is carried out; and (5) the washed and dried filter cake is roasted, such that crystal water is removed, and high-specific-surface area pure-monoclinic-phase zirconia is obtained. The prepared pure-monoclinic-phase zirconia can be used as a carrier for various catalysts.

Description

technical field [0001] The invention relates to a preparation method of pure monoclinic zirconia with high specific surface area. Background technique [0002] Zirconium dioxide is an important basic industrial raw material, which is widely used in many fields, such as chemical industry, fine materials and catalysts, [0003] Zirconium dioxide has various phases such as amorphous, monoclinic, tetragonal and cubic, and the physical and chemical properties of different phases of zirconium dioxide are different. In various catalytic reactions of synthesis gas, it often shows higher Catalytic reactivity and product selectivity. Therefore, the application of pure monoclinic zirconia with high specific surface area will bring a qualitative leap in the catalyst efficiency of many catalytic reactions. [0004] However, it is very difficult to prepare pure monoclinic zirconia with high specific surface area. Up to now, no report has been made on a really simple and practical method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B01J21/06
Inventor 汪国高杨霞田大勇孙守理孙琦
Owner CHNA ENERGY INVESTMENT CORP LTD
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