Tetragonal nano zirconia with high specific surface and high purity, preparation method of nano zirconia as well as application in catalytic conversion of catalytic synthesis gas

A technology of nano-zirconia and tetragonal phase, which is applied in the direction of nanotechnology, zirconia, chemical instruments and methods for materials and surface science, and can solve the problems of crystal phase impurity, small specific surface area, and tetragonal phase zirconia production scale Minor problems, to achieve the effects of not easy sintering, low boiling point, low equipment investment and operating costs

Active Publication Date: 2017-08-11
SYNFUELS CHINA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is to provide a high-specific surface and high-purity tetragonal phase nano-zirconia and its preparation method and its application in the catalytic

Method used

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  • Tetragonal nano zirconia with high specific surface and high purity, preparation method of nano zirconia as well as application in catalytic conversion of catalytic synthesis gas
  • Tetragonal nano zirconia with high specific surface and high purity, preparation method of nano zirconia as well as application in catalytic conversion of catalytic synthesis gas
  • Tetragonal nano zirconia with high specific surface and high purity, preparation method of nano zirconia as well as application in catalytic conversion of catalytic synthesis gas

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Example 1. Preparation of tetragonal phase nano-zirconia powder with high specific surface area and high purity

[0051] 1) Weigh 9.25 g of hydrated zirconyl nitrate and add it into 60 mL of deionized water, stir at 70° C. for 15 min to prepare an aqueous zirconium salt solution with a molar concentration of 0.571 mol / L.

[0052] 2) Take the aqueous zirconium salt solution obtained above, add 80 mL of ethanol and 140 mL of n-hexane in sequence, and stir thoroughly.

[0053] 3) Under the condition of continuous stirring, add 24.36g of sodium oleate, the molar ratio of sodium oleate to zirconyl nitrate (calculated as zirconium atoms) is 2:1, heat to 70°C and boil and reflux, then stir and reflux at 70°C for 4h.

[0054] 4) The obtained reaction mixture was layered while hot, and the supernatant was taken, washed 5 times with 30 mL of deionized water until the upper solution was light yellow and clear, and dried in an oven at 120° C. to obtain a yellow colloidal zirconyl o...

Embodiment 2

[0059] Example 2. Preparation of high specific surface and high purity tetragonal phase nano zirconia powder

[0060] 1) Weigh 9.26 g of hydrated zirconyl nitrate and add it into 60 mL of deionized water, stir at 60° C. for 10 min to prepare an aqueous solution with a molar concentration of 0.571 mol / L.

[0061] 2) Take the aqueous zirconium salt solution obtained above, add 90 mL of ethanol and 130 mL of n-hexane in sequence, and stir thoroughly.

[0062] 3) Under the condition of continuous stirring, add 49g of sodium oleate, the molar ratio of sodium oleate to zirconium oxynitrate (calculated as zirconium atoms) is 4:1, heat to 58°C to boil and reflux, then stir and reflux at 58°C for 24h.

[0063] 4) The obtained reaction mixture was separated into layers while it was hot, and the supernatant was taken, washed 5 times with 30 mL of deionized water until the upper solution was light yellow and clear, and evaporated at 90° C. to obtain zirconyl oleate in yellow colloidal for...

Embodiment 3

[0067] Example 3. Preparation of high specific surface and high purity tetragonal phase nano zirconia powder

[0068] 1) Weigh 18.52 g of zirconyl nitrate and add it into 120 mL of deionized water, stir at 60° C. for 10 min to prepare an aqueous solution with a molar concentration of 0.55 mol / L.

[0069] 2) Take the aqueous zirconium salt solution obtained above, add 160 mL of ethanol and 280 mL of n-hexane in sequence, and stir thoroughly.

[0070] 3) Under the condition of continuous stirring, add 49g of sodium oleate, the molar ratio of sodium oleate to zirconium oxynitrate (calculated as zirconium atoms) is 2:1, heat to 70°C to boil and reflux, then stir and reflux at 70°C for 12h.

[0071] 4) The obtained reaction mixture was separated into layers while it was hot, and the supernatant was taken, washed 5 times with 30 mL of deionized water until the upper solution was light yellow and clear, and evaporated at 90° C. to obtain zirconyl oleate in yellow colloidal form.

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Abstract

The invention discloses tetragonal nano zirconia with high specific surface and high purity, a preparation method of nano zirconia as well as an application in catalytic conversion of catalytic synthesis gas. The preparation method of the tetragonal nano zirconia comprises the steps as follows: (1) water-soluble zirconium salt or an aqueous solution of other hydrates is prepared, and a zirconium salt aqueous solution is obtained; (2) the zirconium salt aqueous solution is mixed with an organic solvent, and a mixed solution is obtained; (3) sodium oleate is added to the mixed solution, and the solution is heated until reflux is produced; (4) the system obtained in step (3) is left to stand for layering, an supernatant liquid is taken and dried, and zirconia oleate or zirconium oleate is obtained; (5) zirconia oleate or zirconium oleate is roasted in an oxygen atmosphere. The used solvent is low in boiling point, low in cost and easy to recycle; equipment is operated under the normal pressure, raw materials are roasted at the low temperature in an air atmosphere, energy consumption is lower, the equipment investment and operation cost are low, and industrial production is facilitated.

Description

technical field [0001] The invention relates to a high-specific surface and high-purity tetragonal phase nano-zirconia, a preparation method thereof and an application in the catalytic conversion of catalytic synthesis gas, belonging to the technical field of catalyst preparation and the technical field of nanometer materials. Background technique [0002] Because the surface of nano-zirconia has both acidity, alkalinity, oxidation and reduction properties, it is widely used in the field of catalytic technology, especially in the direction of catalytic conversion of synthesis gas. And because of its good thermal stability, acid and alkali corrosion resistance, it is also widely used in structural ceramics, functional materials and other fields, especially tetragonal zirconia, which is currently an advanced ceramic material with the highest mechanical properties at room temperature, and is an optical fiber connector for optical fiber networks. The best material for medium cer...

Claims

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Application Information

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IPC IPC(8): C01G25/02B01J21/06C10G2/00B82Y30/00
CPCB01J21/066C01G25/02C01P2002/01C01P2002/72C01P2004/04C01P2004/64C01P2006/12C01P2006/80C10G2/33
Inventor 张成华杨成杨勇李永旺
Owner SYNFUELS CHINA TECH CO LTD
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