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Method for preparing nano aluminum oxide through vacuum freeze drying technology

A vacuum freeze-drying, nano-alumina technology, applied in the preparation of alumina/hydroxide, can solve the problems of large alumina particle size, low particle agglomeration specific surface area, wide particle size distribution, etc. Effects of specific surface area, high homogeneity and stability

Inactive Publication Date: 2010-08-04
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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  • Method for preparing nano aluminum oxide through vacuum freeze drying technology
  • Method for preparing nano aluminum oxide through vacuum freeze drying technology
  • Method for preparing nano aluminum oxide through vacuum freeze drying technology

Examples

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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 polyethylene glycol octylphenyl ether (surfactant) and 100ml n-butanol (co-surfactant), 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 stirring, u...

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 nano aluminum oxide with high specific surface area through vacuum freeze drying technology. The method comprises the following steps that: an organic phase is prepared, inorganic aluminum salt is mixed with the organic phase when agitation is conducted to obtain a micro-emulsion liquid system, and alkaline precipitant is added into the micro-emulsion liquid system for reaction to obtain aluminum hydroxide sediment; and after filtration and washing, vacuum freeze drying is conducted to the aluminum hydroxide sediment under conditions with temperature of negative 30 DEG C to negative 70 DEG C after pre-freezing, the freeze drying time is 2-96h to obtain aluminum hydroxide solid powder, and the aluminum hydroxide solid powder is calcined to finally obtain nano aluminum oxide. The preparation method of the invention combines the vacuum freeze drying technology with the reverse-phase micro-emulsion, the obtained nano aluminum oxide is gamma-aluminum oxide phase, the dispersity is good, the particles are even, the average grain size is 5-20nm, the specific surface area of the obtained nano aluminum oxide reaches 400-600m<2> / g and the pore volume is 1.5-2.5cm<3> / g. The invention has the advantages that the production process of the preparation method is controllable, the repetitiveness is high, the mass production can be realized, the stability is very high and the nano aluminum oxide can be used as the standard substance with high specific surface area.

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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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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