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Method for preparing zirconium oxide nano ball stack blank by carbon nano-tube auxiliary double liquid phase precipitation

A technology of carbon nanotubes and zirconia, applied in zirconia, chemical instruments and methods, catalyst activation/preparation, etc. The size of the diameter cannot reach the nanometer level, etc., and achieve the effects of wide range of formula changes, low cost, and good monodispersity

Inactive Publication Date: 2003-06-25
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The preparation of catalysts with large specific surface area and suitable pore structure has always been one of the key topics in the research of catalytic technology. ZrO 2 It can be used in the gas-phase synthesis process of various organic substances, and can also be used as a carrier for various catalysts and adsorbents, but due to ZrO 2 The thermal stability itself is poor, and it is difficult to obtain a catalyst with a high specific surface area by conventional preparation methods
[0003] In the patent application number 88106688.1 [Preparation of zirconia powder by microemulsion method], the particle size of the zirconia powder prepared by the microemulsion method cannot reach the nanometer level; The method of nano-zirconia with controllable diameter is the research work of preparing zirconia nano-powder by microemulsion method and micro-emulsion method to prepare zirconia nano-particles [see journal Acta.Phys.Chim.Sin., 2002, 18 (1): 5-9] said microemulsion method adopts Triton 100 to make surfactant, n-hexanol is made cosurfactant, forms microemulsion, can obtain particle size controllable from several nanometers to tens of nanometers. Zirconia particles of a few nanometers have the problems of complex process, large amount of surfactant, and low utilization rate of raw materials. At the same time, there is a problem of powder agglomeration during the sintering process, and the microscopic morphology of nanoparticles cannot be well maintained.

Method used

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  • Method for preparing zirconium oxide nano ball stack blank by carbon nano-tube auxiliary double liquid phase precipitation
  • Method for preparing zirconium oxide nano ball stack blank by carbon nano-tube auxiliary double liquid phase precipitation
  • Method for preparing zirconium oxide nano ball stack blank by carbon nano-tube auxiliary double liquid phase precipitation

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example 2

[0021] Example 2: 100ml toluene, add 0.3g AOT, stir for 10min; and 0.1mol / l ZrOCl 2 Mix 50ml of the solution, stir vigorously for one hour, drop 10ml of 1.5mol / l ammonia water, and slowly drop, the whole titration process takes 1 hour, stir vigorously for 2 hours; centrifugal sedimentation, liquid phase separation, the upper layer is toluene organic phase , the lower layer is the aqueous phase (containing NH 4 Cl), the middle layer is a zirconium hydroxide precipitated gel wrapped by AOT reverse micelles, the gel is dried at 110°C, and fired at 500°C for 4 hours to obtain a powder.

example 3

[0022] Example 3: 100ml cyclohexane, add 0.5g AOT, stir for 10min; add 0.3g CNTs, ultrasonic 20min; and 0.1mol / l ZrOCl 2 Mix 20ml of the solution, stir vigorously for 30min, drip 5ml of 1.5mol / l ammonia water, slowly drip, and vigorously stir for 2 hours; centrifuge and settle, and the liquid phases are separated. The upper layer is an organic phase of cyclohexane, and the lower layer is an aqueous phase (containing NH 4Cl), the middle layer is a zirconium hydroxide precipitation gel wrapped by AOT reverse micelles containing CNTs, the gel is dried at 110°C, and fired at 500°C for 4 hours in an Ar atmosphere to obtain a powder.

[0023] In the above examples, zirconia nanospheres with a diameter of about 20 nm were obtained, and the size was monodisperse. Its microstructure is as figure 1 and figure 2 .

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Abstract

The present invention relates to preparation of catalyst. In the double liquid phase precipitation process, carbon nanotube is added into organic solvent with water insoluble AOT in the same volume to obtain nano zirconia grains coated by double liquid phase counter-colloid ball and without agglomeration through supersonic dispersion and deposition; and stacked blank of nano zirconia balls with great specific surface area is then obtained. The said process can obtain dispersed nano zirconija grains in high material utilization. The produced powder has size of several nano to decade nano, similar to that obtained through microemulsion process. The presnt invention may be used in catalyst industry, information ceramic and structural ceramic fields.

Description

technical field [0001] The invention belongs to the scope of catalyst preparation, in particular to zirconia nanoparticles capable of forming monodisperse, which is applied in the fields of catalysis industry, information functional ceramics and structural ceramics to prepare zirconia by carbon nanotubes (CNTs) assisted two-liquid phase precipitation Method for stacking green bodies of nanospheres Background technique [0002] The preparation of catalysts with large specific surface area and suitable pore structure has always been one of the key topics in the research of catalytic technology. ZrO 2 It can be used in the gas-phase synthesis process of various organic substances, and can also be used as a carrier for various catalysts and adsorbents, but due to ZrO 2 The thermal stability itself is poor, and it is difficult to obtain a catalyst with a high specific surface area by conventional preparation methods. [0003] In the patent application number 88106688.1 [Prepara...

Claims

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Application Information

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IPC IPC(8): B01J37/03C01G25/02
Inventor 罗天勇梁彤祥李辰砂
Owner TSINGHUA UNIV