A kind of method for preparing nano-alumina by vacuum freeze-drying

A vacuum freeze-drying and nano-alumina technology, which is applied in the preparation of alumina/hydroxide, etc., can solve the problems of wide particle size distribution, low specific surface area of ​​particle agglomeration, and large alumina particle size, so as to increase pore volume and improve Effect of specific surface area, height uniformity and stability

Inactive Publication Date: 2012-02-15
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to prepare alumina powder with high specific surface area and large pore volume by adopting vacuum freeze-drying technology combined with microemulsion method; Generally low problem; used as a standard material, it provides uniform data at home and abroad for the basic physical properties of various high specific surface area nanopowders (including alumina), and provides traceability for the calibration of specific surface area analyzers; thus providing a Preparation method of nano-alumina material with controllable process and good repeatability and high specific surface area

Method used

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  • A kind of method for preparing nano-alumina by vacuum freeze-drying
  • A kind of method for preparing nano-alumina by vacuum freeze-drying
  • A kind of method for preparing nano-alumina by vacuum freeze-drying

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Embodiment 1

[0035] Adopt the method for preparing nano-alumina material of the present invention, the specific preparation steps of the gamma-alumina material obtained are as follows:

[0036] 1) According to surfactant: co-surfactant=1.2: 1 (volume ratio), oil phase: (surfactant+co-surfactant)=1.3: 1 (volume ratio) batching, take by weighing 290ml cyclohexane ( oil phase), 120ml of polyethylene glycol octylphenyl ether (surfactant) and 100ml of n-butanol (cosurfactant), and sequentially added dropwise to the reaction vessel, mixed and electrically stirred evenly;

[0037] 2) Add dropwise 100ml of 1.0M aluminum nitrate aqueous solution to the above-mentioned organic phase at a rate of 2ml / min, stir while adding dropwise and control the mol ratio of water and surfactant to be 15 to form an aluminum nitrate inverse microemulsion;

[0038] 3) At 25°C, add 100ml of 2.0M ammonium carbonate aqueous solution dropwise at a rate of 2ml / min to the aluminum nitrate inverse microemulsion under stirri...

Embodiment 2

[0044] The preparation method is the same as that of Example 1, except that the pre-freezing temperature is -40° C., and the obtained product is the high specific surface area nano-alumina material prepared in this example.

Embodiment 3

[0046] The preparation method is the same as that of Example 1, except that the pre-freezing temperature is -50° C., and the obtained product is the high specific surface area nano-alumina material prepared in this example.

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Abstract

The invention relates to a method for preparing a nano-alumina material with a high specific surface area by vacuum freeze-drying. The method comprises the following steps: preparing an organic phase, mixing the inorganic aluminum salt solution with the organic phase while stirring to obtain a microemulsion system, adding an alkaline precipitating agent into the microemulsion system for reaction, and obtaining aluminum hydroxide precipitation; filtering, After washing, it is pre-frozen and then vacuum freeze-dried at a temperature of -30°C to -70°C for 2-96 hours to obtain solid aluminum hydroxide powder, which is then calcined to finally form nano-alumina. The preparation method of the present invention combines the vacuum freeze-drying technology with the reverse-phase microemulsion method, and the obtained nano-alumina is a γ-alumina phase, with good dispersion and uniform particles, and the average particle size is 5-20nm. The obtained nano-alumina The specific surface area of ​​aluminum is as high as 400-600m2 / g, and the pore volume is 1.5-2.5cm3 / g. The production process of the preparation method is controllable, has strong repeatability, can be mass-produced, has extremely high stability, and can be used as a high specific surface area standard substance.

Description

technical field [0001] The invention relates to a method for preparing nano-alumina by vacuum freeze-drying, in particular to a method for preparing nano-alumina by combining vacuum freeze-drying technology and microemulsion method. Background technique [0002] Alumina powder material is a widely used industrial product. Because alumina powder material has the characteristics of high temperature resistance, oxidation resistance, wear resistance, good insulation and large surface area, it has been used as a catalyst or catalyst carrier material for many years It is used in many hydrogenation reaction catalyst carriers in the petrochemical industry, surface coating of automobile exhaust purification catalyst carriers and other fields. In recent years, with the rapid development of my country's petrochemical and nanomaterials industries, nano-Al with high specific surface area 2 0 3 research and development has become increasingly active. Among them, how to use stable and c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/30
Inventor 朴玲钰刘祥志王琛
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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