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Preparation method of nano-alumina seed crystal prepared by sol-gel method

A technology of nano-alumina and sol-gel method, which is applied in the field of preparation of nano-alumina seed crystals by sol-gel method, can solve problems such as unfavorable low-cost large-scale production, difficulty in large-scale popularization and application, and complicated process equipment. Achieve the effects of easy large-scale industrial production, easy control of process parameters, and simple preparation process

Active Publication Date: 2018-09-28
SUZHOU CHUANGYUAN INVESTMENT DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It uses high-cost aluminum salts and uses a large amount of alcohol in the process, so the process is difficult to promote and apply on a large scale
The Chinese invention patent with the application number 200710144871 relates to the preparation method of highly compatible nano-alumina and its microemulsion phase transformation. It first prepares aluminum alkoxide microemulsion, and makes it into a microemulsion state under ultrasonic and strong stirring to maintain microemulsion The region changes from liquid phase to nano-scale solidified phase. Although this method can obtain nano-scale alumina, the process equipment is complicated and a large amount of alcohol is required, so it is not conducive to low-cost large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Take 55 kg of industrial-grade pseudo-boehmite containing impurities such as silicon oxide and sodium oxide with a total mass fraction of 0.4%, and mix them with 100 kg of water at 85° C., add nitric acid to control the pH value to 3, and stir to form a sol evenly;

[0032] 2) Add 4kg of industrial fine-grained α-alumina as the original crystal seed to the sol, then add 0.5kg of sodium hexametaphosphate and 0.5kg of nano-carbon sol, and grind for 6 hours in a high-speed stirring mill to obtain a mixed Sol;

[0033] Among them, the primary particle size of industrial fine-grained α-alumina is 0.45 μm, the median particle size D50 is 0.8 μm, the grinding medium uses zirconia balls with a diameter of 2 mm, and the mass ratio of abrasive, grinding medium and water is 1:1 :10;

[0034] 3) placing the mixed sol in a nitrogen atmosphere at a temperature of 95° C. and controlling the temperature for 6 hours;

[0035] 4) Put the mixed sol left standing in the step 3) under ...

Embodiment 2

[0040] 1) Take 55 kg of industrial-grade pseudoboehmite containing impurities such as silicon oxide and sodium oxide with a total mass fraction of 0.4% and 150 kg of water and mix them at 90° C., add nitric acid to control the pH value to 3.5, and stir to form a sol;

[0041] 2) Add 4kg of industrial fine-grained α-alumina as the original crystal seed to the sol, then add 0.6kg of sodium hexametaphosphate and 0.8kg of nano-carbon sol, and grind for 7 hours in a high-speed stirring mill to obtain a mixed Sol;

[0042] Among them, the primary particle size of industrial fine-grained α-alumina is 0.45 μm, the median particle size D50 is 0.8 μm, the grinding medium uses zirconia balls with a diameter of 2 mm, and the mass ratio of abrasive, grinding medium and water is 1:1 :10;

[0043] 3) placing the mixed sol in a nitrogen atmosphere at a temperature of 98° C. and controlling the temperature for 6 hours;

[0044] 4) Put the mixed sol left standing in the step 3) under a nitrog...

Embodiment 3

[0049]1) Take 55kg of industrial-grade pseudoboehmite containing impurities such as silicon oxide and sodium oxide with a total mass fraction of 0.4%, and mix them with 140kg of water at 90°C, add nitric acid to control the pH value to 2.5, and stir to form a sol;

[0050] 2) Add 4kg of industrial fine-grained α-alumina as the original crystal seed to the sol, then add 0.8kg of sodium hexametaphosphate and 0.6kg of nano-carbon sol, and grind for 8 hours in a high-speed stirring mill to obtain a mixed Sol;

[0051] Among them, the primary particle size of industrial fine-grained α-alumina is 0.45 μm, the median particle size D50 is 0.8 μm, the grinding medium uses zirconia balls with a diameter of 2 mm, and the mass ratio of abrasive, grinding medium and water is 1:1 :10;

[0052] 3) placing the mixed sol in a nitrogen atmosphere at a temperature of 98° C. and controlling the temperature for 6 hours;

[0053] 4) Put the mixed sol left standing in the step 3) under a nitrogen ...

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Abstract

The invention discloses a method for preparing nano-alumina seed crystals by virtue of a sol-gel method. By utilizing low-cost industrial raw materials and fine process control, the raw materials are subjected to high-energy ball milling to break agglomeration, and seed crystals are added, so that the conversion temperature from a gamma-alumina phase to an alpha-alumina phase is decreased; and meanwhile, the dispersion degree of the seed crystals during the sol treatment is controlled, the seed crystals are independently prepared by virtue of a constant iteration method, and therefore, the nano-alumina seed crystals are produced in batches from the low-cost industrial raw materials and can be widely applied to the industries of fine ceramics, grinding materials and grinding tools. By virtue of the method, low-cost industrial alumina is taken as an initial fine-grain seed crystal and is subjected to iteration for several times so as to obtain the alumina seed crystals which have original crystals smaller than 100nm and excellent dispersity; and the iteration process is simple, the scale-up production is easily realized, the raw material cost is low, the preparation process is simple, process parameters are easily controlled, and the large-scale industrial production is easily realized.

Description

technical field [0001] The invention relates to the field of inorganic non-metallic materials, in particular to a method for preparing nano-alumina seeds by a sol-gel method. Background technique [0002] As a raw material for ceramics and abrasives, α-alumina is widely used in the fields of aerospace, energy, biology, metallurgy, electronics, chemistry, and chemical industry. Usually α-alumina is obtained from aluminum hydroxide and industrial-grade γ-alumina through high-temperature calcination phase transformation, but the primary grain size after high-temperature phase transformation is usually greater than 300nm, which cannot be used for fine-grained ceramics and abrasive preparation. If seeds are introduced during the calcination process, since the seeds increase the nucleation density of α-alumina and reduce the nucleation barrier in the phase transformation kinetics, fine-grained α-alumina can be obtained at a lower calcination temperature. aluminum. Therefore, nan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/30B82Y30/00
CPCB82Y30/00C01F7/30C01P2004/64
Inventor 王克力蒋丹宇司文元张涛徐兵夏金峰徐海芳
Owner SUZHOU CHUANGYUAN INVESTMENT DEV
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