Preparation method of high-purity nano aluminum oxide

A nano-alumina, high-purity technology, applied in the preparation of aluminum hydroxide, chemical instruments and methods, inorganic chemistry, etc., can solve the difficulties in the preparation of nano-alpha alumina, narrow and ultra-fine α-alumina, and lack of particle size distribution and other problems to achieve the effect of avoiding excessive grain growth, avoiding agglomeration, and narrowing the particle size distribution range

Pending Publication Date: 2020-08-11
河北铭万精细化工有限公司
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  • Application Information

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Problems solved by technology

[0004] However, the preparation of nano-α-alumina is very difficult, because the α-phase transition temperature is above 1000°C, and nano-precursors (including nano-γ-alumina, nano-ammonium aluminum carbonate, nano-aluminum hydroxide, etc.) High-temperature calcination, and during this process, the nanoparticles will be severely agglomerated and sintered. If the ultra-fine α-alumina is directly ground from the large-grained α-alumina, the abrasive loss will be large due to the high hardness of the α-alumina, which will also cause The particle size distribution is wide, and ultra-fine α-alumina with a narrow particle size distribution cannot be obtained. Therefore, it is necessary to find a simple and efficient method for preparing monodisperse, high-purity, low-sodium nano-α-alumina

Method used

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  • Preparation method of high-purity nano aluminum oxide
  • Preparation method of high-purity nano aluminum oxide
  • Preparation method of high-purity nano aluminum oxide

Examples

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Effect test

Embodiment 1

[0072] This embodiment provides a kind of high-purity nano-alumina, and its preparation method specifically includes the following steps:

[0073] 1) Al(NO 3 ) 3 9H 2 O and tartaric acid are dissolved in deionized water to obtain solution A;

[0074] 2) Take polyvinyl alcohol and dissolve it in 10 times the weight of deionized water, heat and stir until the polyvinyl alcohol is completely dissolved and becomes a uniform sol B;

[0075] 3) Under stirring, slowly add the solution A of step 1) into the sol B dropwise, continue heating and stirring in a water bath for 60 minutes to obtain a mixed solution C;

[0076] 4) Add ammonia water to solution C under stirring to adjust pH=10.0 to obtain viscous wet gel D;

[0077] 5) Wet gel D was firstly incubated at 128°C for 45 minutes, and then at 155°C for 90 minutes to obtain dry gel, which was ground into powder;

[0078] 6) The dry gel powder obtained in step 5) is obtained by heat-preserving and calcining at 1125° C. for 5 hou...

experiment example 1

[0094] The morphological characteristics of the composite samples were observed with a Japanese Hitachi SU-1500 scanning electron microscope, and the observation voltage was 15kV; the powder X-ray diffraction test was carried out with a D / max-r A X-ray powder diffractometer of Rigaku Corporation, Cu target , the target voltage is 40kV, the target current is 30mA, Kα rays, the scanning speed is 7° / min, the scattering slit is 1°, and the receiving groove is 0.15nm. From its SEM image ( figure 1 ) It can be seen that the alumina particles are small spherical particles with a uniform particle size and an average particle size of D 50 Around 200nm. By its XRD image ( figure 2 ) shows that the position of each diffraction peak is related to that of α-Al 2 o 3 The XRD standard card (JCPDS NO.46-1212) is consistent, and the diffraction peaks are sharp and free of impurity peaks, indicating that the prepared α-Al 2 o 3 Higher purity and higher crystallinity. The final product h...

Embodiment 2

[0096] This embodiment provides another kind of nano-alumina, its preparation method and formula components are basically similar to the embodiment, the difference is that in this embodiment, glycine is used instead of tartaric acid and Al(NO 3 ) 3 9H 2 O was co-dissolved in deionized water to obtain solution A, and nano-alumina was prepared according to the same subsequent steps as in Example 1.

[0097] In addition, this embodiment also provides another heat insulating material, which is prepared through the following steps:

[0098] 1) The high-purity nano-alumina powder described in this embodiment, the opacifying agent silicon carbide, and the reinforcing fiber high-strength glass fiber are stirred and dispersed evenly according to the weight ratio of 20:14:1 to obtain a mixture;

[0099] 2) Mix the mixture described in step 1) at 330T / m 2 The pressure is pressed into aluminum oxide nano heat insulation board.

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Abstract

The invention relates to a preparation method of high-purity nano aluminum oxide. The preparation method is characterized by comprising the following steps: slowly dropwise adding a mixed solution ofAl (NO3) 3 and tartaric acid into polyvinyl alcohol sol, adding ammonia water into the mixed solution until the mixed solution is alkaline, dehydrating to obtain xerogel, and calcining at the temperature not lower than 1100 DEG C to obtain the high-purity nano aluminum oxide. The preparation method is controllable and mild without generating oxygen in the traditional alumina preparation process, and avoids the erosion of oxygen to equipment; and agglomeration of aluminum oxide molecules in the calcining process is greatly avoided, and the nano aluminum oxide is high in uniformity, narrow in particle size distribution range, relatively high in purity and extremely low in sodium content and can meet the special application in multiple fields.

Description

technical field [0001] The invention relates to the technical field of nanometer metal oxide materials, in particular to a preparation method of high-purity nanometer alumina. Background technique [0002] The molecular formula of aluminum oxide is Al 2 o 3 According to its crystal structure, it can be divided into α, γ, β, ρ, κ, δ, θ and other crystal forms, among which α-Al 2 o 3 It is a high-temperature stable crystal form with a series of excellent properties such as high melting point, high hardness and high strength, especially its excellent electrical insulation, radiation resistance, high temperature resistance and corrosion resistance, and its very good chemical stability. This makes it an important functional material with military and civilian value. Among them, alumina polycrystalline material is an ideal high-temperature window material, infrared dome material, and watch mirror material due to its excellent optical and mechanical properties. Since the 1960s...

Claims

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Application Information

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IPC IPC(8): C01F7/34C01F7/44C04B35/10C04B35/626C04B30/02C04B14/36
CPCC01F7/34C01F7/441C04B35/10C04B35/626C04B30/02C04B14/303C01P2004/32C01P2004/62C01P2004/51C04B2201/32
Inventor 闫德利魏雨林玉龙姚春毅
Owner 河北铭万精细化工有限公司
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