KR19980048898A - Method for producing monodisperse aluminum hydroxide fine particles - Google Patents
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- KR19980048898A KR19980048898A KR1019960067548A KR19960067548A KR19980048898A KR 19980048898 A KR19980048898 A KR 19980048898A KR 1019960067548 A KR1019960067548 A KR 1019960067548A KR 19960067548 A KR19960067548 A KR 19960067548A KR 19980048898 A KR19980048898 A KR 19980048898A
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- C—CHEMISTRY; METALLURGY
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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Abstract
본 발명은 구상의 단분산 수산화알루미늄 미립자의 제조방법에 관한 것으로, 그 목적은 알코올과 아세톤(aceton)을 용매로 하고, 알루미늄 알콕사이드를 가수분해시켜, 구상이면서 입도분포가 좁고 1미크론 이하의 크기를 갖는 단분산 수산화알루미늄 미립자를 제조하는 방법을 제공하고자 하는데 있다.The present invention relates to a method for producing spherical monodisperse aluminum hydroxide fine particles, the purpose of which is to use alcohol and acetone as a solvent, hydrolyze the aluminum alkoxide, so that the spherical and narrow particle size distribution is smaller than 1 micron It is to provide a method for producing monodisperse aluminum hydroxide fine particles having.
상기 목적을 달성하기 위한 본 발명은 고급알코올과 아세톤의 혼합 용매중에서 알루미늄 알콕사이드를 가수분해 시켜 수산화알루미늄 미립자를 제조하는 방법에 있어서, 상기 알코올에 알루미늄 알콕사이드를 0.01-0.15mol/l 용해하여 얻어진 용액 50-70vol%와, 아세톤에 물을 0.02-0.15mol/l 용해하여 얻어진 용액 30-50vol%를 각각 20-50℃로 가열한 상태에서 혼합하여 수산화알루미늄 미립자를 생성시키고, 상기 혼합용액을 교반하면서 생성입자를 성장시키는 과정을 포함하여 구성되는 구상의 단분산 수산화알루미늄 미립자의 제조방법에 관한 것을 그 요지로 한다.In order to achieve the above object, the present invention provides a method for producing aluminum hydroxide fine particles by hydrolyzing aluminum alkoxide in a mixed solvent of higher alcohol and acetone, the solution 50 obtained by dissolving 0.01-0.15 mol / l of aluminum alkoxide in the alcohol. -70 vol% and 30-50 vol% of a solution obtained by dissolving 0.02-0.15 mol / l of water in acetone were mixed in a state of heating to 20-50 ° C. to produce aluminum hydroxide fine particles, while stirring the mixed solution. The gist of the present invention relates to a method for producing spherical monodisperse aluminum hydroxide fine particles comprising a step of growing particles.
Description
본 발명은 수산화알루미늄 미립자의 제조방법에 관한 것으로, 보다 상세하게는 구상이면서 1미크론(㎛) 이하의 크기를 갖는 수산화알루미늄 미립자의 제조방법에 관한 것이다.The present invention relates to a method for producing aluminum hydroxide fine particles, and more particularly, to a method for producing aluminum hydroxide fine particles having a spherical shape and a size of 1 micron or less.
일반적으로 균일한 미세구조를 갖는 고밀도의 세라믹스 제품을 신뢰성 높고 재현성 좋게 말들기 위해서는 (1) 구상일 것 (2) 입도분포가 좁으면서 입자간 응집이 없는 것, 단분산 일 것 (3) 1미크론 이하의 미립자 일 것 (4) 조성이 균일하며 고순도일 것 등의 조건을 갖춘 원료 분말이 필요하다. 이와 같은 조건의 원료분말을 제조하는 수단으로서, 금속알콕사이드(Alkoxide)를 유기용매 중에서 가수분해시키는 방법이 최근 주목되고 있다. 이 방법은 알콕사이드법 혹은 가수분해 제어법이라고 일컬어지는데, 1968년 스퇴버(stober)가 에탄올 중에서 암모니아를 촉매로 사용하면서 실리콘 알콕사이드를 가수분해 시켜 0.5미크론 정도의 크기를 갖는 구상의 수산화알루미늄 미립자를 제조하면서 시작하였다. 그 후 에탄올 용매를 사용하여 수산화티타늄 미립자(일본 공개특허공보 소62-91418호, 평1-33939호)와 수산화 지르코늄 미립자(일본 공개특허공보 소62-91421호)가 제조되었다.In general, in order to roll high-density ceramic products with uniform microstructures with high reliability and reproducibility, they should be (1) spherical (2) narrow in particle size distribution, free of intergranular aggregation, and monodisperse (3) 1 micron (4) Raw material powders having conditions such as uniform and high purity are required. As a means for producing a raw material powder under such conditions, a method of hydrolyzing a metal alkoxide in an organic solvent has recently been noted. This method is called alkoxide method or hydrolysis control method. In 1968, Stober hydrolyzed silicon alkoxide while using ammonia as a catalyst in ethanol to produce spherical aluminum hydroxide particles having a size of about 0.5 micron. Started. After that, titanium hydroxide fine particles (Japanese Patent Laid-Open No. 62-91418, Japanese Patent No. Hei 1-33939) and zirconium hydroxide fine particles (Japanese Patent Laid-Open No. 62-91421) were produced using an ethanol solvent.
그러나 상기의 종래 방법으로는 구상의 단분산 수산화알루미늄 입자는 만들어지지 않는다. 그 가장 큰 이유는 출발물질(Precursor)인 알루미늄 알콕사이드의 가수분해 속도가 매우 빠르기 때문이다. 즉, 종래의 방법에서 사용하고 있는 에탄올 등의 저급 알코올 용매로서는 매우 빠른 알루미늄 복합알콕사이드의 가수분해 속도를 적절히 제어할 수 없기 때문에, 구상의 단분산미립자를 얻을 수 없었다.However, spherical monodisperse aluminum hydroxide particles are not produced by the above conventional method. The main reason is that the hydrolysis rate of aluminum alkoxide, which is a precursor, is very fast. That is, spherical monodisperse fine particles could not be obtained because the hydrolysis speed of a very fast aluminum composite alkoxide cannot be properly controlled as a lower alcohol solvent such as ethanol used in the conventional method.
이에 본 발명자들은 상기와 같은 문제점을 해결하기 위해 연구와 실험을 거듭하고, 그 결과에 근거하여 본 발명은 제안하게 된 것으로, 본 발명은 알코올과 아세톤(aceton)을 용매로 하고, 알루미늄 알콕사이드를 가수분해시켜, 구상이면서 입도분포가 좁고 1미크론 이하의 크기를 갖는 단분산 수산화알루미늄 미립자를 제조하는 방법을 제공하고자 하는데 그 목적이 있다.In order to solve the above problems, the present inventors have repeatedly conducted research and experiments, and based on the results, the present invention has been proposed. The present invention uses alcohol and acetone as a solvent, and alkoxide is used as a valence. It is an object of the present invention to provide a method for producing monodisperse aluminum hydroxide fine particles having a spherical shape, a narrow particle size distribution, and a size of 1 micron or less.
제1도는 본 발명의 방법에 의해 제조된 구상의 단분산 수산화알루미늄 미립자의 주사전자현미경(SEM) 사진이다.1 is a scanning electron microscope (SEM) photograph of spherical monodisperse aluminum hydroxide fine particles produced by the method of the present invention.
제2도는 비교방법에 의해 제조된 응집체 형태의 수산화알루미늄 미립자의 주사전자현미경(SEM) 사진이다.FIG. 2 is a scanning electron microscope (SEM) photograph of aluminum hydroxide fine particles in aggregate form prepared by a comparative method.
상기 목적을 달성하기 위한 본 발명은 고급알코올과 아세톤의 혼합 용매중에서 알루미늄 알콕사이드를 가수분해 시켜 수산화알루미늄 미립자를 제조하는 방법에 있어서, 상기 알코올에 알루미늄 알콕사이드를 0.01-0.15mol/l 용해하여 얻어진 용액 50-70vol%와, 아세톤에 물을 0.02-0.15mol/l 용해하여 얻어진 용액 30-50vol%를 각각 20-50℃로 가열한 상태에서 혼합하여 수산화알루미늄 미립자를 생성시키고, 상기 혼합용액을 교반하면서 생성입자를 성장시키는 과정을 포함하여 구성되는 구상의 단분산 수산화알루미늄 미립자의 제조방법에 관한 것이다.In order to achieve the above object, the present invention provides a method for producing aluminum hydroxide fine particles by hydrolyzing aluminum alkoxide in a mixed solvent of higher alcohol and acetone, the solution 50 obtained by dissolving 0.01-0.15 mol / l of aluminum alkoxide in the alcohol. -70 vol% and 30-50 vol% of a solution obtained by dissolving 0.02-0.15 mol / l of water in acetone were mixed in a state of heating to 20-50 ° C. to produce aluminum hydroxide fine particles, while stirring the mixed solution. A method for producing spherical monodisperse aluminum hydroxide fine particles comprising a step of growing particles.
이하, 본 발명은 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명에서 사용되는 알루미늄 알콕사이드로서는 예를 들면, 알루미늄 메톡사이드 알루미늄 에톡사이드, 알루미늄 프로폭사이드, 알루미늄 부톡사이드 등을 들 수 있다. 이러한 종래의 알루미늄 알콕사이드를 사용할 수 있는 본 발명에서는 우선 알루미늄 알콕사이드를 알코올에 용해하는데, 이때 사용되는 알코올로서는 펜탄올, 헥산올, 헵탄올, 옥탄올 등의 고급알코올이 바람직하며, 상온에서 잘 녹지 않는 경우는 약 50℃ 정도로 가열하면서 교반하면 용이하게 용해시킬 수 있다.As an aluminum alkoxide used by this invention, aluminum methoxide aluminum ethoxide, aluminum propoxide, aluminum butoxide, etc. are mentioned, for example. In the present invention in which such conventional aluminum alkoxide can be used, first, aluminum alkoxide is dissolved in alcohol, and as the alcohol to be used, higher alcohols such as pentanol, hexanol, heptanol, and octanol are preferable, and they are not easily dissolved at room temperature. In that case, it can melt | dissolve easily, stirring, heating at about 50 degreeC.
상기 알루미늄 알콕사이드를 알코올에 용해함에 있어, 그 농도로서는 0.01-0.15mol/l로 제어할 필요가 있다. 농도가 0.01mol/l 미만에서는 가수분해 생성물의 농도가 낮아 수산화알루미늄 미립자의 전단계 물질인 핵생성이 일어나지 않으며, 0.15mol/l을 넘으면 오히려 용액중에 과다한 핵이 생성되어 입성장 과정에서 서로 달라붙어 응집체가 생성하기 때문이다.In dissolving the said aluminum alkoxide in alcohol, it is necessary to control to 0.01-0.15 mol / l as the density | concentration. When the concentration is less than 0.01 mol / l, the concentration of the hydrolyzate is low, so that nucleation, which is a preliminary material of the aluminum hydroxide fine particles, does not occur. When the concentration exceeds 0.15 mol / l, excessive nuclei are generated in the solution and adhere to each other during particle growth. Because it generates.
또한, 본 발명에서는 아세톤에 물을 용해시킴에 있어, 물의 농도는 0.02-0.15mol/l가 되도록 제어해야 한다. 물의 농도가 0.02mol/l 미만에서는 용액중에서 수산화알루미늄이 콜로이드(Colloid) 입자가 석출하기까지 시간이 많이 걸려 실용성이 없으며 0.15mol/l이 넘으면 수산화알루미늄 미립자의 입도분포가 넓게 되어 소위 다분산으로 되거나 구상의 미립자가 아닌 응집체가 생성되기 때문이다.In addition, in the present invention, in dissolving water in acetone, the concentration of water should be controlled to be 0.02-0.15 mol / l. When the concentration of water is less than 0.02 mol / l, aluminum hydroxide takes a long time to precipitate colloidal particles in solution, and if it is more than 0.15 mol / l, the particle size distribution of the aluminum hydroxide fine particles becomes wide so that it becomes polydispersion or This is because aggregates which are not spherical fine particles are formed.
상기 알루미늄 알콕사이드를 용해한 알코올 용액과 상기 물을 용해한 아세톤 용액을 혼합하면, 곧 가수분해 반응이 일어나 핵이 생성되고 연이어 입성장이 일어나는데, 이 핵성성과 입성장이 용액 전체에서 균일하게 일어나게 하기 위해서는 알코올 용액과 아세톤 용액의 혼합성이 좋아야 한다. 이를 달성하기 위하여는 혼합전 두 용액을 각각 20-50℃로 가열할 필요가 있다. 가열온도가 20℃ 미만에서 알코올 용액과 아세톤 용액은 전혀 혼합되지 않으며, 50℃를 넘으면 혼합 후 가수분해 반응이 너무 빨리 진행되어 구상의 미립자는 얻어지지 않고 응집체만 생성되기 때문이다.When the alcohol solution in which the aluminum alkoxide is dissolved and the acetone solution in which the water is dissolved are mixed, a hydrolysis reaction occurs immediately to generate nuclei and subsequent grain growth. In order for the nucleus and grain growth to occur uniformly throughout the solution, The acetone solution should be well mixed. To achieve this it is necessary to heat each of the two solutions before mixing to 20-50 ° C. This is because the alcohol solution and the acetone solution are not mixed at all when the heating temperature is less than 20 ° C., and when the temperature exceeds 50 ° C., the hydrolysis reaction proceeds too fast after mixing, and spherical fine particles are not obtained but only aggregates are formed.
또한 본 발명에서는 알코올 용액과 아세톤 용액의 혼합시 적절한 혼합비를 갖는다. 즉, 두 용매를 혼합한 후의 부피양을 100vol%로 할 때, 이중 아세톤이 차지하는 부피가 30-50vol%가 되도록 할 필요가 있다. 아세톤이 차지하는 부피비가 30vol% 미만 혹은 50vol%가 넘는 범위에서는 혼합성이 나쁘게 되어 구상의 미립자가 아닌 응집체가 얻어지게 되기 때문이다.In addition, the present invention has an appropriate mixing ratio when mixing the alcohol solution and acetone solution. That is, when the volume amount after mixing two solvents is 100 vol%, the volume occupied by double acetone needs to be 30-50 vol%. This is because in the range where the volume ratio of acetone occupies less than 30 vol% or more than 50 vol%, the miscibility becomes poor, thereby obtaining aggregates that are not spherical fine particles.
또한, 본 발명에서는 용액의 균일한 혼합과 입성장이 용액 전체에서 균일하게 얼어나게 하기 위하여 용액을 교반하는 것이 발마직하다. 교반 방법으로서는, 예를 들면, 마그네틱 스터러(Magnetic Stirrer)에 의한 교반, 프로펠라형 교반기에 의한 교반, 초음파를 이용한 교반 등을 들 수 있는데, 특별히 교반방법이나 장치를 제한하지는 않는다.Further, in the present invention, it is desirable to stir the solution so that the uniform mixing and grain growth of the solution are uniformly frozen throughout the solution. As a stirring method, stirring with a magnetic stirrer, stirring with a propeller type stirrer, stirring using an ultrasonic wave, etc. are mentioned, for example, A stirring method and an apparatus are not specifically limited.
상기와 바와 같은 본 발명에 의하면 일정량의 수산화알루미늄 미립자의 핵이 생성한 후에는 이들을 핵으로 하는 입성장 과정만 진행되어 즉, 후속적인 핵생성이 억제되기 때문에 단분산성이 높은 수산화알루미늄 미립자가 얻어진다.According to the present invention as described above, after a certain amount of nuclei of aluminum hydroxide fine particles are generated, only a particle growth process using these as nuclei proceeds, that is, subsequent nucleation is suppressed, so that aluminum hydroxide fine particles having high monodispersity are obtained. .
본 발명에서의 수산화알루미늄 미립자의 성장속도는 알코올 용액과 아세톤 용액 혼합 후 약 5분 정도까지는 대단히 빠르지만, 입자의 성장과 함께 완만하게 되는데, 이와 같은 입자 성장은 혼합 후 약 1시간까지 지속되며 10분 경과 후의 입자크기는 최종입경의 약 90%에 달한다. 따라서, 입성장 시간을 적당히 선택하는 것에 의해 입경이 다른 수산화알루미늄 입자를 얻을 수 있다. 예를 들어, 30분 입성장 시킨 후 얻어진 미립자의 크기는 약 0.47미크론이다.The growth rate of the aluminum hydroxide fine particles in the present invention is very fast up to about 5 minutes after mixing the alcohol solution and the acetone solution, but becomes gentle with the growth of the particles. Such growth of the particles lasts up to about 1 hour after mixing. The particle size after the passage reaches about 90% of the final particle size. Therefore, aluminum hydroxide particles having different particle diameters can be obtained by appropriately selecting the grain growth time. For example, the particle size obtained after 30 minutes of grain growth is about 0.47 microns.
상기의 제조방법에 의해 얻고자 하는 크기로 성장시킨 수산화알루미늄 미립자를 원심분리에 의해 회수하고, 이를 오븐 및 진공건조기 등에서 건조시킴으로써 구상의 단분산 수산화알루미늄 미립자를 얻을 수 있다. 생성된 수산화알루미늄 미립자의 입도분포는 정규분포를 하고 있으며 평균입경의 ±10% 이내에 전체입자의 68% 이상이 포함되어 단분산성이 매우 높은 미립자가 얻어진다.Spherical monodisperse aluminum hydroxide fine particles can be obtained by centrifuging the aluminum hydroxide fine particles grown to the size desired by the above-described production method, and drying them in an oven or a vacuum dryer. The particle size distribution of the produced aluminum hydroxide fine particles is normally distributed, and 68% or more of all the particles are contained within ± 10% of the average particle diameter, thereby obtaining highly monodisperse fine particles.
이하, 실시예를 통하여 본 발명은 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.
[실시예]EXAMPLE
실시예 1Example 1
알루미늄 알콕사이드(0.05mol/l)를 60vol%의 옥탄올에 50℃의 열을 가하면서 용해한 용액에 40vol%의 아세톤에 용해한 재증류수(0.05mol/l)를 혼합하여 교반하면서 가수분해를 행하였다. 이때 용액의 혼합은 30℃에서 행하였다. 그 후 상온에서 1시간 입성장시킨 다음 원심분리기로 생성된 미립자와 용매를 분리하고, 분리된 침전물을 200℃의 진공건조기에서 6시간 건조하였다. 이와 같이하여 얻어진 수산화알루미늄 미립자의 주사전자현미경(SEM) 사진을 제1도에 나타내었다. 제1도에 나타난 바와 같이, 얻어진 수산화알루미늄 미립자는 구상이면서 평균입경 0.5 미크론이고 응집이 전혀 없는 단분산 미립자임을 알 수 있다.The aluminum alkoxide (0.05 mol / l) was dissolved in 60 vol% octanol while heating at 50 ° C., and distilled water (0.05 mol / l) dissolved in 40 vol% acetone was mixed and hydrolyzed while stirring. At this time, the solution was mixed at 30 ° C. After granulation at room temperature for 1 hour, the fine particles and the solvent were separated by a centrifuge, and the separated precipitate was dried for 6 hours in a vacuum dryer at 200 ° C. A scanning electron microscope (SEM) photograph of the aluminum hydroxide fine particles thus obtained is shown in FIG. As shown in FIG. 1, it can be seen that the obtained aluminum hydroxide fine particles are spherical, monodisperse fine particles having an average particle diameter of 0.5 micron and no aggregation at all.
실시예 2Example 2
알루미늄 알콕사이드(0.15mol/l)를 50vol%의 옥탄올에 50℃의 열을 가하면서 용해한 용액에, 50vol%의 아세톤에 용해한 재증류수(0.1mol/l)를 혼합하여 교반하면서 가수분해를 행하였다. 이때 용액의 혼합은 50℃에서 행하였다. 그 후 상온에서 1시간 입성장시킨 다음 원심분리기로 생성된 미립자와 용매를 분리하고, 분리된 침전물을 200℃의 진공건조기에서 6시간 건조하였다. 본 실시예에서 얻어진 수산화알루미늄 미립자도 실시예 1에서 얻어진 수산화알루미늄 미립자와 같이 구상이면서 평균 입경이 1미크론 이하이고 응집이 전혀 없는 단분산 미립자였다.Hydrolysis was carried out while mixing aluminum alkoxide (0.15 mol / l) with 50 vol% octanol while heating at 50 ° C. with distilled water (0.1 mol / l) dissolved in 50 vol% acetone. . At this time, the solution was mixed at 50 ° C. After granulation at room temperature for 1 hour, the fine particles and the solvent were separated by a centrifuge, and the separated precipitate was dried for 6 hours in a vacuum dryer at 200 ° C. The aluminum hydroxide fine particles obtained in this example were also monodisperse fine particles having a spherical shape and an average particle diameter of 1 micron or less and no aggregation at all, like the aluminum hydroxide fine particles obtained in Example 1.
[비교예 1]Comparative Example 1
알루미늄 알콕사이드(0.3mol/l)를 90vol%의 옥탄올에 50℃의 열을 가하면서 용해한 용액에 10vol%의 아세톤에 용해한 재증류수(0.2mol/l)를 혼합하여 교반하면서 가수분해를 행하였다. 이때 용액의 혼합은 상온에서 행하였다. 그 후 상온에서 1시간 입성장시킨 다음 원심분리기로 생성된 미립자와 용매를 분리하고, 분리된 침전물을 200℃의 진공건조기에서 6시간 건조하였다. 얻어진 수산화알루미늄 미립자의 주사전자현미경(SEM) 사진을 제2도에 나타내었다. 제2도에 나타낸 바와 같이, 본 발명의 범위를 벗어난 조건에서 얻어진 수산화알루미늄 미립자는 구상의 미립자가 아닌 응집체임을 알 수 있다.Hydrolysis was carried out while mixing aluminum alkoxide (0.3 mol / l) with distilled water (0.2 mol / l) dissolved in 10 vol% acetone in a solution dissolved in 90 vol% octanol by applying 50 ° C. heat. At this time, the solution was mixed at room temperature. After granulation at room temperature for 1 hour, the fine particles and the solvent were separated by a centrifuge, and the separated precipitate was dried for 6 hours in a vacuum dryer at 200 ° C. A scanning electron microscope (SEM) photograph of the obtained aluminum hydroxide fine particles is shown in FIG. As shown in FIG. 2, it can be seen that the aluminum hydroxide fine particles obtained under conditions outside the scope of the present invention are aggregates, not spherical fine particles.
상술한 바와 같은 본 발명의 방법에 의하면 구상이면서 평균입경이 1미크론 이하이고 응집이 없는 구상의 단분산 수산화알루미늄 미립자를 얻을 수 있고 또한 얻어진 수산화알루미늄 미립자는 균일입경을 갖는다. 따라서 세라믹스 소결체의 원료분말로서 최적이기 때문에 전자재료, 안료, 화장품, 보성, 충진재 등의 여러가지 용도로도 이용될 수 있는 것이다.According to the method of the present invention as described above, spherical monodisperse aluminum hydroxide fine particles having a spherical shape and an average particle diameter of 1 micron or less and without aggregation can be obtained, and the obtained aluminum hydroxide fine particles have a uniform particle size. Therefore, since it is optimal as a raw material powder of the ceramic sintered body, it can be used for various uses such as electronic materials, pigments, cosmetics, complementary materials, fillers, and the like.
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KR100383089B1 (en) * | 1998-12-29 | 2003-07-22 | 재단법인 포항산업과학연구원 | Alumina single-dispersion particulate synthesis method |
KR100467795B1 (en) * | 2000-08-24 | 2005-01-24 | 재단법인 포항산업과학연구원 | Preparation method of monosized alumina particles |
KR100732455B1 (en) * | 2001-08-31 | 2007-06-27 | 주식회사 포스코 | Fabrication method of spherical aluminum hydroxide |
KR20220033639A (en) * | 2020-09-09 | 2022-03-17 | 한국생산기술연구원 | Porous alumina composition and method for manufacturing dye adsorbent comprising the same |
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US4010247A (en) * | 1974-02-21 | 1977-03-01 | Condea Petrochemie-Gesellschaft M.B.H. | Method for making water dispersible aluminum hydroxide |
JPS61183108A (en) * | 1985-02-09 | 1986-08-15 | Natl Inst For Res In Inorg Mater | Preparation of fine powder of aluminium nitride |
KR910000294B1 (en) * | 1988-07-20 | 1991-01-24 | 한국과학기술원 | Process for synthesis of alumina-gol |
JPH02248356A (en) * | 1989-03-18 | 1990-10-04 | Mitsubishi Mining & Cement Co Ltd | Method for controlling rate of hydrolysis of metal alkoxide |
US5409683A (en) * | 1990-08-23 | 1995-04-25 | Regents Of The University Of California | Method for producing metal oxide aerogels |
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KR100383089B1 (en) * | 1998-12-29 | 2003-07-22 | 재단법인 포항산업과학연구원 | Alumina single-dispersion particulate synthesis method |
KR100467795B1 (en) * | 2000-08-24 | 2005-01-24 | 재단법인 포항산업과학연구원 | Preparation method of monosized alumina particles |
KR100732455B1 (en) * | 2001-08-31 | 2007-06-27 | 주식회사 포스코 | Fabrication method of spherical aluminum hydroxide |
KR20220033639A (en) * | 2020-09-09 | 2022-03-17 | 한국생산기술연구원 | Porous alumina composition and method for manufacturing dye adsorbent comprising the same |
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