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KR100996472B1 - Method for manufacturing high purity aluminium trihydroxide - Google Patents

Method for manufacturing high purity aluminium trihydroxide Download PDF

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KR100996472B1
KR100996472B1 KR1020100035063A KR20100035063A KR100996472B1 KR 100996472 B1 KR100996472 B1 KR 100996472B1 KR 1020100035063 A KR1020100035063 A KR 1020100035063A KR 20100035063 A KR20100035063 A KR 20100035063A KR 100996472 B1 KR100996472 B1 KR 100996472B1
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aluminum hydroxide
mother liquor
precipitation
impurities
aging
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허재훈
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주식회사 해마루에너지
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Priority to JP2013504837A priority patent/JP5622300B2/en
Priority to PCT/KR2011/002715 priority patent/WO2011129657A2/en
Priority to CN2011800193884A priority patent/CN103221343A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/46Purification of aluminium oxide, aluminium hydroxide or aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/04Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/06Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Inorganic Chemistry (AREA)
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  • Geochemistry & Mineralogy (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

PURPOSE: A producing method of high-purity aluminum hydroxide is provided to optimize a weight ratio, the amount of an adsorbent, stirring speed, adhesion time, and the precipitation temperature time of a base liquid for securing high quality. CONSTITUTION: A producing method of high-purity aluminum hydroxide comprises the following steps: forming a base liquid by dissolving aluminum hydroxide in a liquid with a weight ratio of 0.68~0.72(S110); aging impurities inside the base liquid(S120); adsorbing the impurities with an adsorbent formed with a pulp material(S200); separating the pulp material, and firstly filtering the base liquid before transferring the liquid to a precipitation tank(S310); applying an aluminum hydroxide seed to the liquid and segregating the aluminum hydroxide(S320); dividing the outcome by particle size(S330); secondly filtering the base liquid including the segregated material with a big particle size(S340); and washing and drying the result(S350).

Description

고순도 수산화알루미늄 제조방법{Method for manufacturing high purity aluminium trihydroxide}Method for manufacturing high purity aluminum trihydroxide

본 발명은 고순도 수산화알루미늄 제조방법에 관한 것으로서, 보다 상세하게는, 바이엘 공정(Bayer Process) 전, 일반수산화알루미늄을 가성소다(NaOH) 용액에 용해시켜 용해된 액을 숙성시킨 후 소량의 흡착제를 사용하여 숙성된 용액속의 불순물만을 선택적으로 제거하여 순도가 높은 수산화알루미늄을 제조함으로써, 종래의 제조방법인 바이엘 공전 전, 수산화알루미늄을 이용하여 용해된 액에 존재하는 불순물을 수산화알루미늄과 함께 공침시키는 공침공정 동안 발생되는 제품의 과다 손실 및 폐기물의 발생, 비효율성으로 인한 상용화의 어려움을 해소할 수 있으면서도, 비용을 절감하는 한편 친환경적인 방법으로 고 품질의 고순도 수산화알루미늄을 제조할 수 있는 고순도 수산화알루미늄 제조방법에 관한 것이다.
The present invention relates to a method for producing high purity aluminum hydroxide, and more specifically, before the Bayer process, general aluminum hydroxide is dissolved in a caustic soda (NaOH) solution to ripen the dissolved liquid, and then a small amount of adsorbent is used. By selectively removing only the impurities in the aged solution to produce a high purity aluminum hydroxide, the coprecipitation step of co-precipitating the impurities present in the dissolved solution with aluminum hydroxide before using a conventional Bayer revolver, aluminum hydroxide A method of manufacturing high purity aluminum hydroxide that can solve the difficulties of commercialization due to excessive loss of products, waste generation, and inefficiency while reducing costs and producing high quality high purity aluminum hydroxide in an eco-friendly way. It is about.

고순도 수산화알루미늄은, 최근 특수도자기, IC 생산을 위한 고순도 유리, 광학 유리, 고순도 알루미늄 화합물 및 고순도 알루미나 원료 등에 사용된다. 최근, LED TV 등의 LED 제품과 관련하여 각광을 받고 있는 화합물이기도 하다.High purity aluminum hydroxide is recently used in special ceramics, high purity glass for producing IC, optical glass, high purity aluminum compound and high purity alumina raw material. Recently, it is also a compound that is in the spotlight in connection with LED products such as LED TV.

이와 같은 고순도 수산화알루미늄을 제조하기 위해서는 화합물의 제조 공정 중 바이엘 공정(Bayer Process)을 필수적으로 거쳐야 하는데, 이 바이엘 공정은 보오크싸이트(Bauxite) 광석에 존재하는 수산화알루미늄을 추출하기 위해 가성소다(NaOH) 용액에 보오크싸이트를 넣고 가열하여 수산화알루미늄을 용출시킨 후(용해공정) 슬러지는 버리고 상기 가성소다에 의하여 용해된 수산화알루미늄을 석출시키는 공법(석출공정)이다.In order to manufacture such high-purity aluminum hydroxide, a Bayer process is essential in the process of preparing a compound, which is a caustic soda (NaOH) to extract aluminum hydroxide present in the bauxite ore. A method of depositing aluminum hydroxide dissolved in the caustic soda after dissolving aluminum hydroxide by dissolving aluminum hydroxide by heating the bauxite in a solution (dissolution step).

이와 같은 바이엘 공정으로 생산된 수산화알루미늄은 용해공정에서 투입되는 보오크싸이트에서 유입된 불순물과 상기 바이엘 공정 시 사용되는 부원료의 잔유물에 의해 다량의 불순물을 함유하게 된다.The aluminum hydroxide produced by the Bayer process contains a large amount of impurities by the impurities introduced from the bauxite introduced in the melting process and the residues of the subsidiary materials used in the Bayer process.

그러므로, 일반적인 바이엘 공정만으로는 일정 순도 이상의 고순도 수산화알루미늄을 제조할 수는 없었다. 따라서, 종래에는 불순물을 제거하기 위해 수산화알루미늄을 산(Acid)에 용해시킨 후 Isodecanol, Kerosene 등의 유기용매를 이용하여 금속이온을 제거하는 일부 방법이 동원되었다. 그러나, 이러한 불순물 제거방법은 조작이 어렵고, 고가의 용매 추출제를 사용하여야 함은 물론 환경오염 등의 문제가 대두되었다.Therefore, the general Bayer process alone could not produce high purity aluminum hydroxide above a certain purity. Accordingly, some methods of removing metal ions using an organic solvent such as Isodecanol and Kerosene after dissolving aluminum hydroxide in acid to remove impurities have been mobilized. However, such an impurity removal method is difficult to operate, and expensive solvent extractants have to be used as well as problems such as environmental pollution.

또한, 알루미늄(Al) 금속을 이용하여 제조하는 방법들이 사용되기도 하나 이 역시 제조비용이 높아 상용화 여부가 불투명하고, 실질적으로 고순도 수산화알루미늄 제조방법은 비공개 노하우로써 전세계적으로 1∼2개의 기업에서만 상품화되어 있는 처지이다.
In addition, the manufacturing method using aluminum (Al) metal is also used, but also because of the high manufacturing cost, it is not clear whether to commercialize. In practice, high-purity aluminum hydroxide manufacturing method is a private know-how, commercialized only by one or two companies worldwide. It is a situation.

본 발명은 상술한 바와 같은 기술적 과제를 해결하기 위하여 안출된 것으로서, 일반수산화알루미늄을 가성소다(NaOH) 용액을 이용하여 용해시킨 후, 그 용해된 액을 숙성(여기서 사용되는 용어 중, "숙성"이라 함은 용해된 상태에서 입자를 키우는 것을 말함)시켜 불순물들을 활성화시킨 후 펄프 재질의 흡착제를 이용하여 용해된 액에 존재하는 불순물을 흡착시킨 후 여과하여 용해된 액을 효과적으로 정제하고, 그 정제된 액을 바이어 공정(Bayer Process)을 이용하여 고순도 수산화알루미늄을 석출시킴으로써, 저비용, 친환경적인 방법으로 고순도 수산화알루미늄을 양산할 수 있는 고순도 수산화알루미늄 제조방법을 제공하는 것을 그 목적으로 한다.The present invention has been made to solve the above technical problem, and after dissolving the general aluminum hydroxide using a caustic soda (NaOH) solution, the dissolved liquid is aged (in the term used herein, "maturation" This refers to growing particles in a dissolved state) to activate impurities and to adsorb impurities present in the dissolved liquid using an adsorbent made of pulp material, and then to purify the dissolved liquid effectively by filtering. It is an object of the present invention to provide a high purity aluminum hydroxide production method capable of mass-producing high purity aluminum hydroxide in a low cost and environmentally friendly manner by depositing a high purity aluminum hydroxide using a Bayer process.

또한, 본 발명은 고순도 수산화알루미늄 제조시 요구되는 중요한 조건인 공정모액의 중량비, 숙성시간, 흡착제의 양, 교반속도, 흡착시간, 석출온도 및 석출시간 등 최적의 조건을 개발하여 99.9 이상의 순도를 가진 고순도 수산화알루미늄 제조방법을 제공하는 것을 그 목적으로 한다.In addition, the present invention has developed the optimum conditions such as the weight ratio of the process mother liquor, the maturation time, the amount of the adsorbent, the stirring speed, the adsorption time, the precipitation temperature and the precipitation time, which is an important condition required for the production of high purity aluminum hydroxide, having a purity of 99.9 or more. It is an object of the present invention to provide a method for producing high purity aluminum hydroxide.

본 발명에 따른 고순도 수산화알루미늄 제조방법의 바람직한 일실시예는, 일반수산화알루미늄을 용해한 후 숙성시키는 모액 준비단계와, 상기 모액 준비단계 후, 펄프를 첨가하여 준비된 모액으로부터 불순물을 흡착시키는 정제단계와, 상기 정제단계 후, 모액에 종자를 투입하여 석출시킨 후, 석출된 물질을 여과, 세척 및 건조하는 고순도 수산화알루미늄을 취득하는 취득단계를 포함한다.Preferred embodiment of the high-purity aluminum hydroxide manufacturing method according to the present invention, the mother liquor preparation step of dissolving and aging the general aluminum hydroxide, and after the mother liquor preparation step, a purifying step of adsorbing impurities from the mother liquor prepared by the addition of pulp, After the refining step, after the seed is added to the mother liquor to precipitate, and obtaining a high-purity aluminum hydroxide for filtering, washing and drying the precipitated material.

여기서, 상기 모액 준비단계는, 일반수산화알루미늄과 가성소다(NaOH)를 용해조에 넣어 상기 일반수산화알루미늄을 용해시켜 모액을 만드는 용해공정과, 상기 용해공정을 통해 용해된 모액의 온도를 소정의 숙성시간 동안 천천히 내리면서 불순물을 숙성시키는 숙성공정을 포함할 수 있다.Here, the mother liquor preparation step, the general aluminum hydroxide and caustic soda (NaOH) in the dissolution tank to dissolve the general aluminum hydroxide to form a mother liquor, and the temperature of the mother liquor dissolved through the dissolution step a predetermined aging time It may include a aging process to mature the impurities while slowly lowering.

본 발명에 따른 고순도 수산화알루미늄 제조방법의 다른 실시예는, 가성소다 용액(NaOH)과 일반수산화알루미늄을 용해조에 넣어 일반수산화알루미늄을 용해시켜 모액을 만드는 용해공정과, 상기 용해공정 후 소정시간에 거쳐 모액의 온도를 천천히 내려 불순물을 숙성시키는 숙성공정과, 상기 숙성공정을 거쳐 숙성된 모액에 펄프 재질의 흡착제를 첨가 분산시켜 모액 중의 불순물을 상기 흡착제에 흡착시키는 정제공정과, 상기 정제공정이 완료된 후 불순물을 흡착시킨 상기 펄프를 분리함과 아울러, 모액을 여과한 후 석출조로 보내는 제1여과공정과, 상기 제1여과공정 후 상기 석출조의 모액에 수산화알루미늄 종자를 투여하여 수산화알루미늄을 석출하는 석출공정과, 상기 석출공정 후 입자크기가 작은 석출물과 입자크기가 큰 석출물을 분리하는 분극공정과, 상기 분극공정에서 입자가 큰 석출물을 함유한 모액을 여과하여 여액은 상기 가성소다 용액으로 재순환시키는 제2여과공정과, 상기 제2여과공정을 통해 여과된 석출물을 세척 후 수분을 제거하는 건조공정을 포함한다.Another embodiment of the high-purity aluminum hydroxide manufacturing method according to the present invention, by adding a sodium hydroxide solution (NaOH) and a general aluminum hydroxide in a dissolution tank to dissolve the general aluminum hydroxide to form a mother liquor, and after a predetermined time after the dissolution step Aging process of slowly lowering the temperature of the mother liquor to mature the impurities, purifying the adsorbent of pulp material to the mother liquor aged through the aging process to disperse the impurities in the mother liquor to the adsorbent, and after the purification process is completed The first filtration step of separating the pulp adsorbed with impurities, filtering the mother liquor and sending it to the precipitation tank, and the precipitation step of depositing aluminum hydroxide by administering aluminum hydroxide seed to the mother liquor of the precipitation tank after the first filtration step. And, after the precipitation step to separate the precipitate having a small particle size and the precipitate having a large particle size A second filtration step of filtering the mother liquor containing precipitates having large particles in the polarization step and the polarization step, and recycling the filtrate to the caustic soda solution; and washing the precipitates filtered through the second filtration step to remove water. It includes a drying step.

여기서, 상기 용해공정은, 용해된 모액의 수산화나트륨에 대한 산화알루미늄의 중량비(

Figure 112010024216808-pat00001
)가 0.68∼0.72이다.Here, the dissolution step is a weight ratio of aluminum oxide to sodium hydroxide of the dissolved mother liquid (
Figure 112010024216808-pat00001
) Is 0.68 to 0.72.

또한, 상기 용해공정에서 상기 가성소다(NaOH)의 농도는 탄산나트륨(

Figure 112010049513940-pat00002
)을 기준으로 270g/l 이상이다.In addition, the concentration of caustic soda (NaOH) in the dissolution step is sodium carbonate (
Figure 112010049513940-pat00002
) Is greater than or equal to 270 g / l.

또한, 상기 숙성공정에서 모액의 숙성온도는 130℃ ∼ 90℃로 소정시간 이상 유지할 수 있다.In addition, the maturing temperature of the mother liquid in the aging step can be maintained at 130 ℃ to 90 ℃ or more for a predetermined time.

또한, 상기 숙성공정에서 불순물을 숙성시키는 숙성시간은 1시간 이상일 수 있다.In addition, the aging time for aging the impurities in the aging process may be 1 hour or more.

또한, 상기 석출공정은 초기온도가 85℃ 이상에서 수행될 수 있다.In addition, the precipitation process may be performed at an initial temperature of 85 ℃ or more.

또한, 상기 석출공정은, 수산화알루미늄을 석출하는 석출시간이 72시간 이상 수행될 수 있다.In addition, in the precipitation process, the precipitation time for depositing aluminum hydroxide may be performed for 72 hours or more.

또한, 상기 석출공정에서 최종적으로 얻어지는 수산화나트륨에 대한 산화알루미늄의 중량비(

Figure 112010024216808-pat00003
)는 0.36 이하일 수 있다.
In addition, the weight ratio of aluminum oxide to sodium hydroxide finally obtained in the precipitation step (
Figure 112010024216808-pat00003
) May be less than or equal to 0.36.

본 발명에 따른 고순도 수산화알루미늄 제조방법은, 펄프와 같은 흡착제를 이용하여 불순물을 흡착시킴으로써 친환경적으로 고순도 수산화알루미늄을 제조할 수 있는 효과를 가진다.The method for producing high purity aluminum hydroxide according to the present invention has an effect of producing environmentally friendly high purity aluminum hydroxide by adsorbing impurities using an adsorbent such as pulp.

또한, 본 발명에 따른 고순도 수산화알루미늄 제조방법은, 정제공정 외에 다양한 공정에 수반되는 중요한 석출조건을 제시함은 물론, 공침공정과 같은 조작이 어렵고 비용이 많은 공정을 삭제함으로써, 순도가 높은 수산화알루미늄을 저비용으로도 생산할 수 있는 효과가 있다.
In addition, the high-purity aluminum hydroxide manufacturing method according to the present invention not only suggests important precipitation conditions accompanying various processes in addition to the refining process, but also eliminates difficult and expensive processes such as coprecipitation process, and thus high purity aluminum hydroxide. It can be produced at low cost.

도 1은 본 발명에 따른 고순도 수산화알루미늄 제조방법의 순차적 제조 공정을 나타낸 블록도이다.1 is a block diagram showing a sequential manufacturing process of a high-purity aluminum hydroxide manufacturing method according to the present invention.

이하, 본 발명에 따른 고순도 수산화알루미늄 제조방법의 바람직한 일실시예를 첨부된 도면을 참조하여 상세하게 설명하기로 한다.
Hereinafter, with reference to the accompanying drawings a preferred embodiment of a high-purity aluminum hydroxide manufacturing method according to the present invention will be described in detail.

도 1은 본 발명에 따른 고순도 수산화알루미늄 제조방법의 순차적 제조 공정을 나타낸 블록도이다.1 is a block diagram showing a sequential manufacturing process of a high-purity aluminum hydroxide manufacturing method according to the present invention.

일반적으로, 수산화알루미늄을 제조하기 위해서는, 보오크싸이트(Bauxite)를 가열·가압 상태에서 고농도의 가성소다(NaOH) 용액에 녹여 소듐 알루미네이트(Sodium aluminate,

Figure 112010024216808-pat00004
) 과포화 용액을 만든다.In general, in order to manufacture aluminum hydroxide, bauxite is dissolved in a high concentration of caustic soda (NaOH) solution in a heated and pressurized state, and sodium aluminate,
Figure 112010024216808-pat00004
) Make a supersaturated solution.

이와 같이 만들어진 상기 소듐 알루미네이트를 방치 및 여과공정을 거쳐서 용해되지 않은 불순물을 제거하는 정제공정(S210)을 거친 다음, 정제된 상기 소듐 알루미네이트 용액은 고온에서 석출을 시작하도록 장시간에 걸쳐 온도를 천천히 하강시키는 방법으로 석출공정을 거쳐 최종적으로 원하는 수산화알루미늄을 제조하게 된다. 여기서, 순도가 높은 고순도 수산화알루미늄을 제조하기 위해서는, 상기 공정 중 불순물을 제거하는 정제공정(S210)이 매우 중요하고, 최근 관련 업계의 연구 또한 순도를 높이는 공정인 정제공정(S210)에 초점이 맞춰져 있는 실태다.After the sodium aluminate thus made is left to pass through a filtration step to remove undissolved impurities (S210), the purified sodium aluminate solution is slowly cooled down for a long time to start precipitation at a high temperature. As a method of descending, the precipitation process is performed to finally produce the desired aluminum hydroxide. Here, in order to manufacture high purity aluminum hydroxide with high purity, a purification process (S210) for removing impurities in the process is very important, and recent research in the related industry also focuses on the purification process (S210), which is a process for increasing purity. It is a fact.

본 발명에 따른 고순도 수산화알루미늄 제조방법의 바람직한 일실시예는, 도 1에 참조된 바와 같이, 최종적으로 취득되는 수산화알루미늄의 순도를 높이기 위한 다양하고도 실험적인 공정을 제공한다.One preferred embodiment of the high purity aluminum hydroxide manufacturing method according to the present invention, as shown in Figure 1, provides a variety of experimental processes for increasing the purity of the finally obtained aluminum hydroxide.

이를 보다 상세하게 설명하면, 본 발명에 따른 고순도 수산화알루미늄 제조방법은, 상기 소듐 알루미네이트 과포화 용액을 숙성시킨 후, 불순물을 흡착시키는 흡착제를 사용하여 상기 소듐 알루미네이트 용액을 정제하고, 불순물이 흡착된 소량의 펄프는 제거함과 아울러, 정제된 상기 소듐 알루미네이트 용액은 고온에서 석출을 시작하도록 장시간에 걸쳐 온도를 천천히 하강시켜 저온에서 석출이 완료됨으로써 순도가 높은 수산화알루미늄을 제조하게 된다.In more detail, in the method for producing high purity aluminum hydroxide according to the present invention, after the aging of the sodium aluminate supersaturated solution, the sodium aluminate solution is purified using an adsorbent adsorbing impurities, and impurities are adsorbed. In addition to removing a small amount of pulp, the purified sodium aluminate solution is slowly lowered the temperature over a long time to start precipitation at a high temperature to complete the precipitation at a low temperature to produce a high purity aluminum hydroxide.

보다 일반적으로, 본 발명에 따른 고순도 수산화알루미늄 제조방법을 설명하면, 도 1에 참조된 바와 같이, 본 발명은, 일반수산화알루미늄을 용해한 후 숙성시키는 모액 준비단계(S100)와, 상기 모액 준비단계(S100) 후, 펄프를 첨가하여 준비된 모액으로부터 불순물을 흡착시키는 정제단계(S200)와, 상기 정제단계(S200) 후, 모액에 종자를 투입하여 석출시킨 후, 석출된 물질을 여과, 세척 및 건조하는 고순도 수산화알루미늄을 취득하는 취득단계(S300)를 포함한다.More generally, when describing a high-purity aluminum hydroxide manufacturing method according to the present invention, as shown in Figure 1, the present invention, the mother liquor preparation step (S100) and the mother liquor preparation step (S100) for aging after dissolving the general aluminum hydroxide ( S100), after purifying the adsorbed impurities from the mother liquor prepared by adding the pulp (S200), and after the purification step (S200), after the seed is added to the mother liquor to precipitate, the precipitated material is filtered, washed and dried An acquisition step (S300) of acquiring high purity aluminum hydroxide is included.

특히, 상기 정제단계(S200)는, 종래 모액속의 불순물을 수산화알루미늄 종자와 함께 공침시키는 공침방법 대신 펄프와 같은 흡착제를 이용하여 불순물을 흡착시킨다는 점에서 특이할 만하다.In particular, the purification step (S200) is unique in that it adsorbs impurities using an adsorbent such as pulp instead of the coprecipitation method of coprecipitation of impurities in the mother liquor with conventional aluminum hydroxide seeds.

여기서, 상기 모액 준비단계(S100)는, 일반수산화알루미늄과 가성소다(NaOH)를 용해조에 넣어 상기 일반수산화알루미늄을 용해시켜 모액을 만드는 용해공정(S110)과, 상기 용해공정(S110)을 통해 용해된 모액의 온도를 소정의 숙성시간 동안 천천히 내리면서 불순물을 숙성시키는 숙성공정(S120)을 포함한다.Here, the mother liquor preparation step (S100), by dissolving the general aluminum hydroxide and sodium hydroxide (NaOH) in the dissolution tank to dissolve the general aluminum hydroxide to make a mother liquor, and dissolution through the dissolution step (S110) Aging process (S120) for aging the impurities while slowly lowering the temperature of the prepared mother liquor for a predetermined aging time.

본 발명에 따른 고순도 수산화알루미늄 제조방법에 있어서, 상기 정제단계(S200) 외에도 그 제조 공정에서 중요한 조건들을 제시하고 있는 바, 상술한 바와 같은 실시예에 의하여 본 발명의 권리범위가 한정되는 것은 아님에 주의하여야 한다.In the method of manufacturing high purity aluminum hydroxide according to the present invention, in addition to the refining step (S200), important conditions are suggested in the manufacturing process, and thus the scope of the present invention is not limited by the embodiments as described above. Be careful.

예를 들면, 본 발명에 따른 고순도 수산화알루미늄 제조방법의 다른 실시예는, 보다 정밀한 조건들 하에서 상술한 실시예보다 상세하게 세분화된 공정을 거쳐 최종적인 수산화알루미늄을 취득할 수 있게 된다. For example, another embodiment of the high-purity aluminum hydroxide manufacturing method according to the present invention, under more precise conditions, can be obtained in a more detailed process than the above-described embodiment to obtain the final aluminum hydroxide.

즉, 본 발명에 따른 고순도 수산화알루미늄 제조방법의 다른 실시예는, 도 1에 참조된 바와 같이, 소듐 알루미네이트 과포화 용액을 제조하기 위하여 상기 가성소다 용액(NaOH)과 일반수산화알루미늄을 용해조에 넣어 일반수산화알루미늄을 용해시켜 모액을 만드는 용해공정(S110)과, 상기 용해공정(S110) 후 소정시간에 거쳐 모액의 온도를 천천히 내려 불순물을 숙성시키는 숙성공정(S120)과, 상기 숙성공정(S120)을 거쳐 숙성된 모액에 펄프 재질의 흡착제를 첨가 분산시켜 모액 중의 불순물을 상기 흡착제에 흡착시키는 정제공정(S210)과, 상기 정제공정(S210)이 완료된 후 불순물을 흡착시킨 상기 펄프를 분리함과 아울러, 모액을 여과한 후 석출조로 보내는 제1여과공정(S310)과, 상기 제1여과공정(S310) 후 상기 석출조의 모액에 수산화알루미늄 종자를 투여하여 수산화알루미늄을 석출하는 석출공정과, 상기 석출공정 후 성장이 덜 된, 즉 입자크기가 작은 석출물과 완전히 성장한, 즉 입자크기가 큰 석출물을 분리하여 입자가 작은 석출물은 상기 석출공정의 수산화알루미늄 종자로 사용하는 분극공정(S330)과, 상기 분극공정(S330)에서 입자가 큰 석출물을 함유한 모액을 여과하여 여액은 상기 가성소다 용액으로 재순환시키는 제2여과공정(S340)과, 상기 제2여과공정(S340)을 통해 여과된 석출물을 세척 후 수분을 제거하는 건조공정(S340)을 포함한다.That is, another embodiment of the high-purity aluminum hydroxide manufacturing method according to the present invention, as shown in Figure 1, in order to prepare a sodium aluminate supersaturated solution, the caustic soda solution (NaOH) and a general aluminum hydroxide in a dissolution tank general Melting step (S110) of dissolving aluminum hydroxide to form a mother liquor, aging step (S120) of slowly lowering the temperature of the mother liquor over a predetermined time after the dissolving step (S110) to mature impurities, and the aging step (S120) By separating and dispersing the adsorbent of the pulp material in the mother liquor through the refining step (S210) for adsorbing the impurities in the mother liquor to the adsorbent, and separating the pulp to adsorb the impurities after the refining step (S210) is completed, After filtering the mother liquor, the first filtration step (S310) sent to the precipitation tank, and after the first filtration step (S310) by administering aluminum hydroxide seed to the mother liquor of the precipitation tank The precipitation step of precipitation of aluminum oxide, and the precipitates which are less grown after the precipitation process, i.e., the precipitates which are completely grown, that is, the precipitates which are grown completely, that is, the particles having large particle size are separated, are used as the aluminum hydroxide seeds of the precipitation process. A second filtration step (S340) and a second filtration step of filtering the mother liquor containing the precipitate having a large particle in the polarization step (S330) and the polarization step (S330) and recycling the filtrate to the caustic soda solution. It includes a drying step (S340) for removing the water after washing the precipitate filtered through (S340).

상기와 같이 구성되는 본 발명에 따른 고순도 수산화알루미늄 제조방법에 대하여 보다 상세하게 설명하면 다음과 같다.Referring to the high-purity aluminum hydroxide manufacturing method according to the present invention configured as described above in more detail.

먼저, 온도를 올릴 수 있는 스테인리스 스틸(Sus 316L) 재질로 만든 용해조에 소듐 알루미네이트(Sodium Aluminate) 공정모액을 제조하기 위해 가성소다(NaOH) 용액을 탄산나트륨(

Figure 112010049513940-pat00005
)을 기준으로 210∼280g/l 로 만들어 넣고, 수분이 함유된 일반수산화알루미늄을
Figure 112010049513940-pat00006
의 중량비(A/C : weight ratio)가 0.60∼0.72가 되도록 일반수산화알루미늄을 첨가한 후, 수산화알루미늄을 분산시키기 위하여 교반속도를 30RPM으로 교반하면서 온도를 120∼130℃로 상승시킨 후, 10분 정도 유지(용해공정(S110)시킨 결과, 표 1 및 표 2에서 알 수 있는 바와 같이
Figure 112010049513940-pat00020
의 중량비(A/C)가 0.68 내지 0.72이고, 가성소다(NaOH) 용액을 탄산나트륨(
Figure 112010049513940-pat00021
)를 기준으로 270g/l 및 280g/l, 즉 270g/l이상으로 한 경우 불순물이 최소화 되었다.First, a solution of caustic soda (NaOH) was added to a sodium carbonate solution to prepare a sodium aluminate process mother liquor in a melting tank made of stainless steel (Sus 316L) that can raise the temperature.
Figure 112010049513940-pat00005
) Of 210-280 g / l based on the standard, and the water containing ordinary aluminum hydroxide
Figure 112010049513940-pat00006
Aluminum hydroxide was added so as to have a weight ratio of 0.60 to 0.72, and then the temperature was raised to 120 to 130 DEG C with stirring at a stirring speed of 30 RPM to disperse the aluminum hydroxide, (The dissolution step (S110), as shown in Tables 1 and 2,
Figure 112010049513940-pat00020
(A / C) of 0.68 to 0.72, and the caustic soda (NaOH) solution is added to a solution of sodium carbonate
Figure 112010049513940-pat00021
) Was 270 g / l and 280 g / l, that is, 270 g / l or more, the impurities were minimized.

출원인은 상술한 대략의 조건 중, 공정모액의

Figure 112010049513940-pat00007
의 중량비(A/C)를 아래의 표 1에 기재된 중량비인 0.68과 0.70의 중간수치인 0.69인 상태에서 상기 수산화알루미늄을 완전히 용해시킨 공정모액을 만들기 위하여, 상기 가성소다 농도는
Figure 112010049513940-pat00008
를 기준으로 270g/l 이 되도록 하여 용해조에 넣고 온도를 125℃까지 승온시킨 후 그 상태에서 10분간 유지하였다.Applicant, among the above rough conditions,
Figure 112010049513940-pat00007
(A / C) was completely dissolved in the state of 0.69, which is an intermediate value between 0.68 and 0.70, shown in Table 1 below, and the caustic soda concentration was
Figure 112010049513940-pat00008
To 270g / l based on the temperature was put in the dissolution tank and the temperature was raised to 125 ℃ and maintained for 10 minutes in that state.

이와 같이, 공정모액의 A/C가 0.69가 되도록 상기 수산화알루미늄이 완전히 용해된 상태에서, 상기 공정모액을 숙성시키기 위해 교반기를 3RPM 정도의 속도로 천천히 가동시켜 교반하고, 1시간 이상에 걸쳐 모액 온도를 100℃로 천천히 낮추어 숙성시켰다. 여기서, 공정모액을 숙성시키는 이유는 앞서 설명한 바와 같이, 공정모액에 함유되어 있는 불순물을 제거하기 용이하도록 불순물의 입자 크기를 크게 하기 위함이다.(숙성공정(S120)) In this way, in the state where the aluminum hydroxide is completely dissolved so that the A / C of the process mother liquor is 0.69, the stirrer is slowly operated at a speed of about 3 RPM to stir the process mother liquor, and the mother liquor temperature is maintained for 1 hour or more. Aged slowly by lowering to 100 ℃. Here, the reason for aging the process mother liquor is to increase the particle size of the impurities so as to easily remove the impurities contained in the process mother liquor as described above. (Maturation process (S120))

A/C
제품성분
A / C
Ingredient
0.600.60 0.620.62 0.640.64 0.660.66 0.680.68 0.700.70 0.720.72 비고Remarks
Fe(ppm)Fe (ppm) 1515 1111 88 66 55 55 55 Ca(ppm)Ca (ppm) 1010 77 55 44 44 44 44

공정모액의_의 중량비에 따른 제품의 영향
Effect of product on weight ratio of process mother liquor

Figure 112010024216808-pat00009
g/l
제품성분
Figure 112010024216808-pat00009
g / l
Ingredient 210210 220220 230230 240240 250250 260260 270270 280280 Fe(ppm)Fe (ppm) 1515 1313 1212 1010 88 55 44 44 Ca(ppm)Ca (ppm) 77 77 66 55 44 44 44 44 Na(%)Na (%) 0.110.11 0.080.08 0.060.06 0.040.04 0.030.03 0.020.02 0.020.02 0.020.02

공정모액의 가성소다(NaOH) 농도에 따른 제품의 영향
Effect of Products on Caustic Soda Concentration

한편, 출원인은 상기 숙성공정(S120) 중 숙성시간에 따른 불순물의 함량관계를 표 3을 참조하여 살펴보면 알 수 있듯이, 상기 공정모액의 A/C는 0.69, 상기 가성소다의 농도를 탄산나트륨 기준으로 270g/l이라는 조건에서 가장 적당한 숙성시간은 1시간 이상 지속되어야 함을 알게 되었다. 특히, Fe의 함량이 5ppm 이하인 경우에만 최근 집중적으로 이목을 받고 있는 LED 제품에 이용할 수 있는 고순도 수산화알루미늄을 제조할 수 있는 이점이 있는 바, 역시 공정모액의 숙성시간은 1시간 이상 유지되어야 함이 바람직하다.Meanwhile, as shown in Table 3, the applicant found that the A / C of the mother liquor of the process was 0.69, the concentration of the caustic soda was 270 g (based on sodium carbonate) / l, we found that the most suitable aging time should last more than one hour. In particular, there is an advantage in manufacturing a high-purity aluminum hydroxide that can be used in LED products that are recently attracting attention only if the content of Fe is less than 5ppm, the maturing time of the process mother liquor should be maintained for at least 1 hour. desirable.

숙성시간(분)
성분
Aging time (minutes)
ingredient
3030 6060 120120 180180 240240 300300
Fe(ppm)Fe (ppm) 1515 44 44 44 44 44 Ca(ppm)Ca (ppm) 66 44 44 44 44 44

공정모액의 숙성시간에 따른 고순도 제품의 불순물 함량관계
Impurity Contents of High Purity Products According to Aging Time of Process Mother Solution

다음으로, 상기 공정모액에 함유된 불순물을 제거하기 위해 잘 숙성된 상기 공정모액에 표 4 및 표 5에 나타난 바와 같이, 리터당 제품 생산량이 가장 많으면서 불순물 제거율이 가장 높은 조건인 리터당 1g에 해당하는 펄프를 투입하고, 교반기 속도를 표 6에 나타난 바와 같이 5RPM 속도로 올려 상기 펄프를 모액에 분산시켜 10분간 불순물을 흡착시킨다.(정제공정(S210))
Next, as shown in Table 4 and Table 5 in the process mother liquor well aged to remove impurities contained in the process mother liquor, which corresponds to 1 g per liter, which is the condition that the highest production rate of impurities and the highest impurities removal rate are shown. The pulp was added, and the stirrer speed was raised to 5 RPM as shown in Table 6 to disperse the pulp in the mother liquor for 10 minutes to adsorb impurities (purification step (S210)).

펄프사용량g/l 여과 후
공정모액 성분
Pulp consumption g / l after filtration
Process mother liquor component
00 0.20.2 0.40.4 0.60.6 0.80.8 1.01.0 1.51.5 22 33

Figure 112010024216808-pat00010
Figure 112010024216808-pat00010
0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 Fe(ppm)Fe (ppm) 1111 88 55 44 33 22 22 22 22 Ca(ppm)Ca (ppm) 55 1One 1One 1One 1One 1One 1One 1One 1One

공정모액 속의 불순물 제거를 위한 흡착제 펄프량에 따른 공정모액의 영향(모액온도 100℃, 교반속도 5RPM. 교반시간 10분)
Effect of process mother liquor on the amount of adsorbent pulp to remove impurities in process mother liquor (preparation mother liquor temperature 100 ℃, stirring speed 5RPM. Stirring time 10 minutes)

교반속도
성분
Stirring speed
ingredient
0rpm0 rpm 2rpm2 rpm 4rpm4 rpm 6rpm6 rpm 8rpm8 rpm 10rpm10 rpm 12rpm12 rpm
모액의 A/CA / C of mother liquor 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 펄프 투여 후 공정모액의 Fe(ppm) 함량Fe (ppm) content of process mother liquor after pulp administration 1111 66 22 22 22 22 22

10분 반응시간 중 교반기 속도(RPM)에 따른 공정모액의 변화
Change of process mother liquor according to stirrer speed (RPM) during 10 min reaction time

반응시간(분)
성분
Response time (minutes)
ingredient
00 55 1010 1515 2020 2525
여과 후 모액 A/CMother liquor A / C after filtration 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 0.690.69 Fe(ppm)Fe (ppm) 1111 22 22 22 22 22 Ca(ppm)Ca (ppm) 55 1One 1One 1One 1One 1One

흡착시간에 따른 공정모액의 변화(온도 95℃, 펄프사용량 1g/l, 교반속도 5RPM)
Change of process mother liquor according to adsorption time (temperature 95 ℃, pulp consumption 1g / l, stirring speed 5RPM)

한편, 상기 공정모액으로부터 불순물을 흡착시킨 상기 펄프는 그 다음 공정인 제1여과공정(S310)에서 제거되는데, 여기서 상기 펄프를 제거하기 위해 모액 1

Figure 112010024216808-pat00011
당 가로 및 세로 25cm×25cm 여과 면적의 폴리에틸렌(Poly ethylene) 재질의 여포를 부착한 필터 여과기(Filter press)를 이용하여 2기압 압력으로 여과하여 불순물이 제거된 깨끗한 공정모액은 그 다음 공정인 석출공정을 위해 석출조로 보내고, 불순물을 흡착시킨 상기 펄프는 세척 후 재활용 폐기물로 처리한다.(제1여과공정(S310))On the other hand, the pulp adsorbed impurities from the process mother liquor is removed in the next step of the first filtration process (S310), where the mother liquor 1 to remove the pulp
Figure 112010024216808-pat00011
The clean process mother liquor was removed by filtration at 2 atmospheres using a filter press with a polyfoam of 25 cm x 25 cm filtration area. The pulp is sent to the precipitation tank for adsorption, and the pulp adsorbed with impurities is treated as recycled waste after washing (first filtration step S310).

이처럼, 불순물을 제거한 정제된 공정모액은 다음으로 석출공정을 거치게 된다. 이때, 상기 공정모액은

Figure 112010024216808-pat00012
의 중량비가 0.69이고, 온도는 90℃로 유지된 상태다. 상기 석출공정은 석출물과 종자가 부상될 수 있도록 교반기의 속도를 15RPM으로 증가시키고, 석출을 돕기 위해 수산화알루미늄 종자(평균입도 30um)를 모액 1L당 40g을 넣어 표 7에 나타나 있는 바와 같이 90℃ 이상에서 석출을 시작하고, 표 8에 나타난 바와 같이 그 석출시간은 72시간 이상으로 유지시킨다.(석출공정)
As such, the purified process mother liquor from which impurities are removed is subjected to a precipitation process next. At this time, the process mother liquor
Figure 112010024216808-pat00012
The weight ratio of is 0.69, and the temperature is maintained at 90 ° C. The precipitation process is to increase the speed of the stirrer to 15RPM so that the precipitates and seeds can be floated, and 40g per 1L of the mother hydroxide seed (average particle size 30um) to aid precipitation, as shown in Table 7 above 90 ℃ Precipitation is started at, and the precipitation time is maintained at 72 hours or more as shown in Table 8.

초기석출물
온도℃
성분
Initial precipitate
Temperature
ingredient
90℃90 ° C 85℃85 ℃ 80℃80 ℃ 75℃75 ℃ 70℃70 ℃ 65℃65 ℃
석출물에 함유된 Na 중량%Na wt% in the precipitate 0.020.02 0.020.02 0.040.04 0.080.08 0.150.15 0.300.30

초기 석출온도에 따른 석출물의 Na% 함량관계(석출시간 72시간)
Na% content of precipitate according to initial precipitation temperature (precipitation time 72 hours)

시간 (hr)
성분
Hour (hr)
ingredient
4848 6060 7272 8484 9696 108108 120120 132132
최종 공정액 중량비Final process weight ratio 0.380.38 0.360.36 0.340.34 0.340.34 0.330.33 0.330.33 0.330.33 0.320.32 석출물에 함유된 Na%Na% in precipitate 0.210.21 0.100.10 0.020.02 0.020.02 0.020.02 0.020.02 0.020.02 0.020.02

석출시간에 따른 석출물의 Na함량 및 석출 후 공정액의 최종

Figure 112010024216808-pat00013
중량비(최종 석출온도 40℃, 초기 석출온도 90℃, 종자 65g/l, 평균입도 40um)
Na content of precipitate according to precipitation time and final process solution after precipitation
Figure 112010024216808-pat00013
Weight ratio (final precipitation temperature 40 ℃, initial precipitation temperature 90 ℃, seed 65g / l, average particle size 40um)

상기 석출공정을 통해 석출된 석출물은 상기 가성소다(NaOH)의 함량이 최소화되면 될수록 불순물 함량비가 작은 고순도 수산화알루미늄이 된다. 이와 같이 상기 가성소다의 함량이 최소화될 수 있도록 하는 석출조건으로서, 출원인은 표 7 및 8에 참조된 바와 같이, 초기 석출온도 90℃, 최종 석출온도 40℃, 그 석출시간은 72시간 이상으로 하였을 경우, 최종 석출액의

Figure 112010024216808-pat00014
의 중량비(A/C)가 0.34 이하로 됨을 알 수 있었다. 이처럼, 최종 석출액의 중량비(A/C)가 0.34 이하일 경우에는 품질과 경쟁성을 갖추는 조건이 된다.The precipitate precipitated through the precipitation process becomes high purity aluminum hydroxide having a smaller impurity content ratio as the content of the caustic soda (NaOH) is minimized. As the precipitation conditions such that the content of the caustic soda can be minimized, Applicants, as shown in Tables 7 and 8, the initial precipitation temperature 90 ℃, the final precipitation temperature 40 ℃, the precipitation time was 72 hours or more Case, the final precipitate
Figure 112010024216808-pat00014
It was found that the weight ratio (A / C) of became 0.34 or less. As such, when the weight ratio (A / C) of the final precipitate is 0.34 or less, it is a condition of having quality and competitiveness.

다음으로, 상기 석출공정이 끝나면, 분극공정(S330)을 시작한다. 상기 분극공정(S330)은 성장이 덜된 석출물을 사이클론(Cyclone) 분극기를 이용하여 평균입도가 30um 이하인 석출물을 별도로 분리하여 상기 석출공정 시 투여되는 수산화알루미늄 종자로 사용하고, 입자가 잘 성장한 석출물(평균입도 60um)은 이어지는 제2여과공정(S340)을 거치도록 한다.(분극공정(S330))Next, when the precipitation process is completed, the polarization process (S330) is started. In the polarization step (S330), precipitates having less growth are separated as precipitates having an average particle size of 30 μm or less using a cyclone polarizer, and are used as aluminum hydroxide seeds administered during the precipitation process, and particles having a well-grown precipitate (average) Particle size 60um) is subjected to the second filtration process (S340) to be continued. (Polarization process (S330))

상기 분극공정(S330) 후, 평균입도 60um인 잘 성장한 석출물은 필터를 이용하여 고형물과 여액으로 분리한 후 여액은 다시 상기 용해공정(S110)에 필요한 가성소다 용액의 용도로 보내어 재순환시키고, 고순도 수산화알루미늄인 석출물은 80℃ 이상의 깨끗한 물로 세척 후 오염을 최소화할 수 있는 플루이디징 블로워(Fluidizing blower) 타입의 건조기로 상전이를 일으키지 않고 수분을 제거하기 위해 130℃에서 60분 이내로 건조시킨다.(제2여과공정(S340) 및 건조공정(S340))After the polarization step (S330), the well-grown precipitate having an average particle size of 60um is separated into a solid and a filtrate by using a filter, and the filtrate is recycled to the use of caustic soda solution required for the dissolution step (S110) and recycled, and high purity hydroxide. The precipitate, which is aluminum, is a fluidizing blower type dryer that can minimize contamination after washing with clean water of 80 ° C. or higher and dried within 130 minutes at 130 ° C. to remove moisture without causing a phase transition. Filtration process (S340) and drying process (S340))

이와 같이 건조되어 얻게되는 상기 고순도 수산화알루미늄은 최종적으로 포장공정(S360)을 통해 포장되어 완성되게 된다.(포장공정(S360))
The high purity aluminum hydroxide obtained by drying in this way is finally packaged through the packaging process (S360) is completed (packaging process (S360)).

종류
성분
Kinds
ingredient
본 발명에 의해 제조된 고순도 수산화알루미늄High Purity Aluminum Hydroxide Prepared By The Invention 종래의 고순도 수산화알루미늄Conventional High Purity Aluminum Hydroxide 종래 일반화알루미늄Conventional Generalized Aluminum

Figure 112010024216808-pat00015
Figure 112010024216808-pat00015
% >99.9> 99.9 >99.9> 99.9 >99.7> 99.7 Na%Na% 0.020.02 0.040.04 0.150.15 Fe ppmFe ppm <3<3 <5<5 100100 Si ppmSi ppm <2<2 <5<5 6565 Ti ppmTi ppm <3<3 <3<3 4040 Mg ppmMg ppm <1<1 <1<1 3030 Ca ppmCa ppm <1<1 <1<1 77

본 발명에 따른 제조방법으로 제조한 고순도 수산화알루미늄과 종래 수산화알루미늄과의 비교
Comparison between high purity aluminum hydroxide prepared by the production method according to the present invention and conventional aluminum hydroxide

이상, 본 발명에 따른 고순도 수산화알루미늄 제조방법의 바람직한 일실시예 및 다른 실시예를 첨부된 도면을 참조하여 상세하게 설명하였다. 그러나, 본 발명의 실시예가 반드시 이에 한정되는 것은 아니며, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에 의하여 본 발명과 균등한 범위에 속하는 다양한 변형 또는 다른 실시예의 구현이 가능함은 당연하다. 따라서, 본 발명의 진정한 권리범위는 후술하는 특허청구범위에 의하여 정해져야 할 것이다.Or more, with reference to the accompanying drawings, a preferred embodiment and another embodiment of a high-purity aluminum hydroxide manufacturing method according to the present invention has been described in detail. However, embodiments of the present invention are not necessarily limited thereto, and it is obvious that various modifications or other embodiments falling within the scope equivalent to the present invention may be implemented by those skilled in the art. Therefore, the true scope of the present invention will be defined by the claims below.

S100: 모액 준비단계 S110: 용해공정
S120: 숙성공정 S200: 정제단계
S210: 정제공정 S300: 취득단계
S310: 제1여과공정 S320: 석출공정
S330: 분극공정 S340: 제2여과공정
S350: 건조공정 S360: 포장공정
S100: mother liquor preparation step S110: dissolution process
S120: aging process S200: purification step
S210: Refining Process S300: Acquisition Step
S310: first filtration process S320: precipitation process
S330: polarization step S340: second filtration step
S350: drying process S360: packaging process

Claims (7)

가성소다 용액(NaOH)과 일반수산화알루미늄을 용해조에 넣어 일반수산화알루미늄을 용해된 모액의 수산화나트륨에 대한 산화알루미늄의 중량비(
Figure 112010049513940-pat00022
)가 0.68∼0.72가 되도록 용해시켜 모액을 만드는 용해공정과;
상기 용해공정 후 소정시간에 거쳐 모액의 온도를 천천히 내려 불순물을 숙성시키는 숙성공정과;
상기 숙성공정을 거쳐 숙성된 모액에 펄프 재질의 흡착제를 첨가 분산시켜 모액 중의 불순물을 상기 흡착제에 흡착시키는 정제공정과;
상기 정제공정이 완료된 후 불순물을 흡착시킨 상기 펄프를 분리함과 아울러, 모액을 여과한 후 석출조로 보내는 제1여과공정과;
상기 제1여과공정 후 상기 석출조의 모액에 수산화알루미늄 종자를 투여하여 수산화알루미늄을 석출하는 석출공정과;
상기 석출공정 후 입자크기가 작은 석출물과 입자크기가 큰 석출물을 분리하는 분극공정과;
상기 분극공정에서 입자가 큰 석출물을 함유한 모액을 여과하여 여액은 상기 가성소다 용액으로 재순환시키는 제2여과공정과;
상기 제2여과공정을 통해 여과된 석출물을 세척 후 수분을 제거하는 건조공정을 포함하고,
상기 용해공정에서 상기 가성소다(NaOH)의 농도는 탄산나트륨(
Figure 112010049513940-pat00017
)을 기준으로 270g/l 이상인 고순도 수산화알루미늄 제조방법.
The weight ratio of aluminum oxide to sodium hydroxide in the mother liquor in which caustic soda solution (NaOH) and aluminum hydroxide were added to a dissolution tank was dissolved.
Figure 112010049513940-pat00022
) Is in the range of 0.68 to 0.72, thereby producing a mother liquor;
A aging step of slowly lowering the temperature of the mother liquor over a predetermined time after the dissolution step to mature impurities;
A purifying step of adding and dispersing an adsorbent made of pulp material to the mother liquor aged through the aging step to adsorb impurities in the mother liquor to the adsorbent;
A first filtration step of separating the pulp to which the impurities are adsorbed after the purification step is completed, and filtering the mother liquor and then sending it to a precipitation tank;
A precipitation step of depositing aluminum hydroxide by administering aluminum hydroxide seed to the mother liquor of the precipitation tank after the first filtration step;
A polarization step of separating the precipitate having a small particle size and the precipitate having a large particle size after the precipitation process;
A second filtration step of filtering the mother liquor containing the large precipitate in the polarization step and recycling the filtrate to the caustic soda solution;
It includes a drying step of removing water after washing the precipitate filtered through the second filtration process,
The concentration of caustic soda (NaOH) in the dissolution step is sodium carbonate (
Figure 112010049513940-pat00017
) Of not less than 270 g / l.
삭제delete 청구항 1에 있어서,
상기 숙성공정에서 모액의 숙성온도는 130℃ ∼ 90℃로 소정시간 이상 유지하는 고순도 수산화알루미늄 제조방법.
The method according to claim 1,
Method of producing a high purity aluminum hydroxide to maintain the aging temperature of the mother liquor in the aging step at 130 ℃ to 90 ℃ over a predetermined time.
청구항 3에 있어서,
상기 숙성공정에서 불순물을 숙성시키는 숙성시간은 1시간 이상인 고순도 수산화알루미늄 제조방법.
The method according to claim 3,
The aging time for the maturation of impurities in the aging step is 1 hour or more.
청구항 1에 있어서,
상기 석출공정은 초기온도가 85℃ 이상에서 수행되는 고순도 수산화알루미늄 제조방법.
The method according to claim 1,
The precipitation process is a high purity aluminum hydroxide manufacturing method is carried out at an initial temperature of 85 ℃ or more.
청구항 1에 있어서,
상기 석출공정은, 수산화알루미늄을 석출하는 석출시간이 72시간 이상 수행되는 고순도 수산화알루미늄 제조방법.
The method according to claim 1,
The precipitation step is a high-purity aluminum hydroxide manufacturing method in which the precipitation time for depositing aluminum hydroxide is performed for 72 hours or more.
청구항 1에 있어서,
상기 석출공정에서 최종적으로 얻어지는 수산화나트륨에 대한 산화알루미늄의 중량비(
Figure 112010024216808-pat00018
)는 0.36 이하 인 고순도 수산화알루미늄 제조방법.

The method according to claim 1,
The weight ratio of aluminum oxide to sodium hydroxide finally obtained in the precipitation step (
Figure 112010024216808-pat00018
) Is a method of producing high purity aluminum hydroxide less than 0.36.

KR1020100035063A 2010-04-16 2010-04-16 Method for manufacturing high purity aluminium trihydroxide Expired - Fee Related KR100996472B1 (en)

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