JPH0557202B2 - - Google Patents
Info
- Publication number
- JPH0557202B2 JPH0557202B2 JP23329484A JP23329484A JPH0557202B2 JP H0557202 B2 JPH0557202 B2 JP H0557202B2 JP 23329484 A JP23329484 A JP 23329484A JP 23329484 A JP23329484 A JP 23329484A JP H0557202 B2 JPH0557202 B2 JP H0557202B2
- Authority
- JP
- Japan
- Prior art keywords
- bayerite
- aluminum hydroxide
- amorphous aluminum
- purity
- silicon content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 23
- 229910001680 bayerite Inorganic materials 0.000 claims description 23
- 229910052710 silicon Inorganic materials 0.000 claims description 16
- 239000010703 silicon Substances 0.000 claims description 16
- 230000032683 aging Effects 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 15
- 238000000034 method Methods 0.000 description 8
- 230000005070 ripening Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- -1 distilled water Chemical compound 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、高純度バイヤライトの製造方法に関
するものである。さらに詳しくは、不純物として
ケイ素分を含有する非晶質水酸化アルミニウムを
水溶液中で熟成し、結晶化することによりケイ素
分の含有量の極めて少ない高純度バイヤライトを
製造する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing high-purity bayerite. More specifically, the present invention relates to a method for producing high-purity bayerite with an extremely low silicon content by aging amorphous aluminum hydroxide containing silicon as an impurity in an aqueous solution and crystallizing it.
（従来の技術）
結晶性水酸化アルミニウムの一種であるバイヤ
ライトは、吸着剤、触媒あるいは担体等の幅広い
用途に使用され、またその焼成により得られるη
−アルミナは触媒として著しく活性の高い物質で
あり、さらに高温で焼成して得られる高純度α−
アルミナは焼結性に優れており、電子材料用セラ
ミツクス原料、透光焼結性セラミツクス原料など
として多くの用途がある。これら用途において、
不純物の存在は本来の性能を低下させる場合が多
いので、高純度の製品が望まれている。ところ
が、一般的なバイヤライトの製造方法であるアル
ミン酸アルカリ溶液と酸を反応させる、いわゆる
中和法により製造されるバイヤライトには、ナト
リウム、ケイ素、鉄などの多くの不純物を含んで
おり、高純度のバイヤライトを得ることはできな
かつた。(Prior art) Bayerite, a type of crystalline aluminum hydroxide, is used in a wide range of applications such as adsorbents, catalysts, and supports.
-Alumina is a material with extremely high activity as a catalyst, and can be obtained by firing at a high temperature to achieve high purity α-
Alumina has excellent sinterability and has many uses, including as a ceramic raw material for electronic materials and a transparent sinterable ceramic raw material. In these applications,
Since the presence of impurities often reduces the original performance, products with high purity are desired. However, bayerite, which is produced by the so-called neutralization method in which an alkaline aluminate solution and acid are reacted, which is a common method for producing bayerite, contains many impurities such as sodium, silicon, and iron. It was not possible to obtain high purity bayerite.
不純物の少ないバイヤライトを製造する方法に
は、バイヤライトの酸による洗浄、バイヤライト
を含むスラリーの水熱処理等が提案されている
が、これはナトリウム分を対象としたものであ
り、ケイ素分を除去することはできなかつた。 Methods for producing bayerite with few impurities have been proposed, such as washing bayerite with acid and hydrothermal treatment of slurry containing bayerite, but these methods target the sodium content and do not remove the silicon content. It was not possible to remove it.
（発明が解決しようとする問題点）
以上の点から、結晶性水酸化アルミニウム、バ
イヤライトは優れた特性を持ちながら純度の面で
その性能が制限されてきた。高純度バイヤライト
を容易にかつ低コストで製造する方法は現在のと
ころ知られていない。本発明はこれらの点を解決
しようとするものである。(Problems to be Solved by the Invention) From the above points, although crystalline aluminum hydroxide and bayerite have excellent properties, their performance has been limited in terms of purity. There is currently no known method for producing high-purity bayerite easily and at low cost. The present invention seeks to solve these problems.
（問題点を解決するための手段）
本発明者らは、高純度バイヤライトの製造方法
を種々検討した結果、ケイ素分を不純物として含
有する非晶質水酸化アルミニウムを、40℃以下の
アンモニアアルカリ性水溶液中で熟成し、結晶化
することによつて、非晶質水酸化アルミニウム中
のケイ素分が溶液中へ放出され、高純度のバイヤ
ライトが生成するという新しい事実を見い出し
た。(Means for Solving the Problems) As a result of studying various methods for producing high-purity bayerite, the present inventors discovered that amorphous aluminum hydroxide, which contains silicon as an impurity, was A new fact was discovered that by aging and crystallizing in an aqueous solution, the silicon content in amorphous aluminum hydroxide is released into the solution, producing highly pure bayerite.
すなわち、本発明は、ケイ素分を不純物として
含有する非晶質水酸化アルミニウムを、40℃以下
のアンモニアアルカリ性水溶液中で熟成し、結晶
化することにより、この中に含まれているケイ素
分を効率よく除去し、高純度のバイヤライトを製
造することにある。 That is, the present invention efficiently removes the silicon content by aging amorphous aluminum hydroxide containing silicon as an impurity in an ammonia alkaline aqueous solution at 40°C or less and crystallizing it. The purpose is to remove well and produce high-purity bayerite.
本発明において原料として用いる非晶質水酸化
アルミニウムは通常、湿式法、特にアルミン酸ナ
トリウム溶液と酸を反応により調製される。この
非晶質水酸化アルミニウムの表面にはナトリウム
塩類が多く付着しているため、予め水洗しナトリ
ウム分を除去しておかなければならない。この非
晶質水酸化アルミニウムを特定条件下で熟成す
る。 Amorphous aluminum hydroxide used as a raw material in the present invention is usually prepared by a wet method, particularly by reacting a sodium aluminate solution with an acid. Since many sodium salts adhere to the surface of this amorphous aluminum hydroxide, it is necessary to remove the sodium content by washing with water in advance. This amorphous aluminum hydroxide is aged under specific conditions.
熟成時の温度は40℃以下、好ましくは30℃以下
である。熟成温度が40℃以上では、バイヤライト
と擬ペーマイトが共存し、熟成温度の上昇に伴な
い擬ペーマイト生成量が増加する。 The temperature during ripening is 40°C or lower, preferably 30°C or lower. When the ripening temperature is 40°C or higher, bayerite and pseudopeumite coexist, and the amount of pseudopeumite produced increases as the ripening temperature rises.
熟成に使用する溶液としては、アンモニア水溶
液などの金属イオンを含まないPHの高い水溶液で
ある。苛性ソーダ水溶液で熟成した場合、バイヤ
ライト中にナトリウム分が混入する恐れがある。 The solution used for ripening is an aqueous solution with a high pH that does not contain metal ions, such as an aqueous ammonia solution. When aged in a caustic soda aqueous solution, there is a risk that sodium content may be mixed into bayerite.
溶液のPHは７以上、通常12以上、好ましくは13
以上がよい。PHが７以下ではバイヤライト化が起
こりにくい。 The pH of the solution is 7 or higher, usually 12 or higher, preferably 13
The above is good. Bayerite conversion is difficult to occur when the pH is below 7.
熟成時間は、要するに非晶質水酸化アルミニウ
ムがバイヤライトに結晶転移すればよく、温度、
PHなどの熟成条件により若干変化するが、通常１
時間以上行なう。ここで非晶質水酸化アルミニウ
ムからバイヤライトへの結晶転移はいわゆる不可
逆変化であり、一度バイヤライト化すると、再び
非晶質水酸化アルミニウムには戻らない。 In short, the ripening time is sufficient as long as the amorphous aluminum hydroxide undergoes a crystal transition to bayerite, and the aging time depends on the temperature, temperature,
It varies slightly depending on the aging conditions such as pH, but usually 1
Do it for more than an hour. Here, the crystal transition from amorphous aluminum hydroxide to bayerite is a so-called irreversible change, and once it becomes bayerite, it does not return to amorphous aluminum hydroxide again.
熟成終了後、水酸化アルミニウムを過などの
方法により母液から分離し、蒸留水などの精製し
た水で洗浄した後乾燥する。以上の方法により高
純度のバイヤライトが得られる。 After aging, aluminum hydroxide is separated from the mother liquor by a method such as filtration, washed with purified water such as distilled water, and then dried. High purity bayerite can be obtained by the above method.
（効果）
本発明は、非晶質水酸化アルミニウムを生成し
た後にケイ素分を除去するため、操作が容易であ
り、かつ、経済的な方法である。また、製造され
た結晶性水酸化アルミニウムは、ケイ素分の含有
量が極めて少いために、焼成によつて得られる焼
結体の表面あるいは内部にケイ素分とアルミナと
の反応による白濁点を生成したり、焼結性を低下
させることもない。その結果、焼結体の透光性、
表面平滑性、強度などの特性の著しく好いものが
得られる。(Effects) The present invention is an easy-to-operate and economical method because the silicon content is removed after producing amorphous aluminum hydroxide. In addition, since the produced crystalline aluminum hydroxide has an extremely low silicon content, a cloudy point is generated on the surface or inside of the sintered body obtained by firing due to the reaction between the silicon content and alumina. Nor does it reduce sinterability. As a result, the translucency of the sintered body,
Extremely good properties such as surface smoothness and strength can be obtained.
（実施例） 以下、実施例により本発明を詳細に説明する。(Example) Hereinafter, the present invention will be explained in detail with reference to Examples.
なお、ケイ素分の定量は吸光光度法により、水
酸化アルミニウム中のケイ素分を二酸化ケイ素換
算値で示した。 The silicon content was determined by spectrophotometry, and the silicon content in aluminum hydroxide was expressed as a silicon dioxide equivalent value.
実施例 １
アルミン酸ナトリウム溶液に炭酸ガスを反応さ
せて調整した非晶質水酸化アルミニウム45ｇに蒸
留水900mlを加え撹拌した後、これを過した。
得られた非晶質水酸化アルミニウムケータを再び
蒸留水900mlに分散し、同様の洗浄操作を５回行
なつた。その結果、得られた非晶質水酸化アルミ
ニウム中のケイ素分含有量は64ppmであつた。次
にこの非晶質水酸化アルミニウムを乾燥せずに、
アンモニア溶液（１：１）、1000mlに浸漬し、10
℃に保持し、560rpmで４時間撹拌し、熟成を行
なつた。熟成終了後、スラリーを過し、得られ
た水酸化アルミニウムを蒸留水900mlで洗浄し、
再び過した後、80℃で乾燥した。かくして得ら
れた水酸化アルミニウムは粉末Ｘ線回折の結果鋭
いピークを有するバイヤライトであり、ケイ素含
有量は8ppmであつた。Example 1 900 ml of distilled water was added to 45 g of amorphous aluminum hydroxide prepared by reacting a sodium aluminate solution with carbon dioxide gas, stirred, and filtered.
The obtained amorphous aluminum hydroxide cage was again dispersed in 900 ml of distilled water, and the same washing operation was performed five times. As a result, the silicon content in the obtained amorphous aluminum hydroxide was 64 ppm. Next, without drying this amorphous aluminum hydroxide,
Soaked in 1000ml of ammonia solution (1:1), 10
The mixture was maintained at ℃ and stirred at 560 rpm for 4 hours for ripening. After aging, filter the slurry and wash the resulting aluminum hydroxide with 900ml of distilled water.
After filtering again, it was dried at 80°C. As a result of powder X-ray diffraction, the aluminum hydroxide thus obtained was found to be bayerite with a sharp peak, and the silicon content was 8 ppm.
Claims (1)
化アルミニウムを、40℃以下のアンモニアアルカ
リ性水溶液中で熟成し、結晶化することを特徴と
する高純度バイヤライトの製造方法。1. A method for producing high-purity bayerite, which comprises aging and crystallizing amorphous aluminum hydroxide containing silicon as an impurity in an ammonia alkaline aqueous solution at 40° C. or lower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23329484A JPS61111915A (en) | 1984-11-07 | 1984-11-07 | Production of high-purity bayerite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23329484A JPS61111915A (en) | 1984-11-07 | 1984-11-07 | Production of high-purity bayerite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61111915A JPS61111915A (en) | 1986-05-30 |
| JPH0557202B2 true JPH0557202B2 (en) | 1993-08-23 |
Family
ID=16952845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23329484A Granted JPS61111915A (en) | 1984-11-07 | 1984-11-07 | Production of high-purity bayerite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61111915A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ297741B6 (en) * | 2004-04-15 | 2007-03-21 | Výzkumný ústav anorganické chemie, a. s. | Process for preparing aluminium hydroxide with bayerite crystalline structure |
| CN108264074A (en) * | 2018-02-01 | 2018-07-10 | 西安建筑科技大学 | A kind of preparation method of bayerite |
-
1984
- 1984-11-07 JP JP23329484A patent/JPS61111915A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61111915A (en) | 1986-05-30 |
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