JPH08325011A - Aluminum hydroxide and its production - Google Patents
Aluminum hydroxide and its productionInfo
- Publication number
- JPH08325011A JPH08325011A JP7128468A JP12846895A JPH08325011A JP H08325011 A JPH08325011 A JP H08325011A JP 7128468 A JP7128468 A JP 7128468A JP 12846895 A JP12846895 A JP 12846895A JP H08325011 A JPH08325011 A JP H08325011A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum hydroxide
- sodium
- soln
- sulfuric acid
- residue
- 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.)
- Pending
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は水酸化アルミニウムに関
し、従来にない特性を具備したもので、特に水処理剤用
原料に適した水酸化アルミニウムに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to aluminum hydroxide, and more particularly to aluminum hydroxide having characteristics which have not been hitherto available and which is particularly suitable as a raw material for water treatment agents.
【０００２】[0002]
【従来の技術】水酸化アルミニウムの工業的製法として
は、バイヤー法が主要な方法で、ボーキサイトを水酸化
ナトリウム溶液で加熱処理してアルミン酸ナトリウム溶
液とし、これに以前は炭酸ガスを吹き込むことにより水
酸化アルミニウムを析出させていたが、近年は、炭酸ガ
スを吹き込むことをせず水酸化アルミニウムを種子とし
て加えて撹拌することにより水酸化アルミニウムを析出
させ、水酸化アルミニウムを製造している。BACKGROUND OF THE INVENTION As an industrial method for producing aluminum hydroxide, the Bayer method is the main method, in which bauxite is heat-treated with sodium hydroxide solution to form a sodium aluminate solution, which was previously blown with carbon dioxide gas. Although aluminum hydroxide was deposited, in recent years, aluminum hydroxide is deposited by adding aluminum hydroxide as seeds without stirring carbon dioxide gas and stirring the mixture to produce aluminum hydroxide.
【０００３】[0003]
【発明が解決しようとする課題】水酸化アルミニウムは
仮焼してアルミナにし、それを種々の用途に使われてい
るが、水酸化アルミニウムの化合物としての用途で最大
のものは硫酸アルミニウムまたはポリ塩化アルミ等の無
機の水処理剤の原料である。当該原料としての水酸化ア
ルミニウムとしては鉱酸への溶解性という特性が重要な
要件となる。即ち、反応収率からして未溶解残渣が少な
い方がよく、残渣があると反応後除去する工程が必要と
なり、また溶解反応速度は余り早過ぎると突沸反応し危
険であるので、細か過ぎない粒子であって溶解反応速度
が早いものが望まれる特性である。更に、水酸化アルミ
ニウム中の不純物を低減させる必要もあり、不純物のう
ちで最大の不純物であるＮａを極力少なくしたものが望
まれている。しかし、従来世の中にある水酸化アルミニ
ウムは溶解性と低不純物という両特性を同時に満足する
ものはなかった。Aluminum hydroxide is calcined to form alumina, which is used for various purposes. The largest use as a compound of aluminum hydroxide is aluminum sulfate or polychlorinated material. It is a raw material for inorganic water treatment agents such as aluminum. The property of solubility in mineral acid is an important requirement for aluminum hydroxide as the raw material. That is, it is preferable that the amount of undissolved residue is small in view of the reaction yield, and if there is a residue, a step of removing it after the reaction is required. Particles having a high dissolution reaction rate are desirable characteristics. Further, it is necessary to reduce impurities in aluminum hydroxide, and it is desired to reduce Na, which is the largest impurity among the impurities, as much as possible. However, none of the conventional aluminum hydroxides in the world satisfy both properties of solubility and low impurities at the same time.
【０００４】そこで、本発明は酸に対する未溶解残渣が
少なく、かつＮａ不純物の少ないという従来法では一般
的には相反する特性を具備した水酸化アルミニウムを提
供することを目的とする。Therefore, an object of the present invention is to provide an aluminum hydroxide having properties which are generally contradictory to the conventional method in that there are few undissolved residues with respect to an acid and a small amount of Na impurities.
【０００５】[0005]
【課題を解決するための手段】本発明者は上記目的を達
成すべく鋭意努力し、検討した結果、本発明を見出し
た。即ち、固定ナトリウム（Ｆｉｘ−Ｎａ2 Ｏ）含有量
が０．２２ｗｔ％以下で、下記に規定する硫酸溶解率測
定法による硫酸未溶解残渣量が０．１２ｗｔ％以下であ
ることを特徴とする水酸化アルミニウム並びにその製造
方法としてボーキサイト、カルシウム化合物、ナトリウ
ム化合物および石炭を混合し、粉砕後焼結し、その後、
水、水酸化ナトリウムまたはアルミン酸ナトリウムのう
ち少なくとも１種の水または溶液を加え、焼結物の可溶
分を抽出し、残渣を分離し、更に脱珪処理後、アルミン
酸ナトリウム溶液を造り、その溶液に微細な水酸化アル
ミニウムを種子として添加し炭酸ガスを吹き込んで水酸
化アルミニウムを析出させることを特徴とする水酸化ア
ルミニウムの製造方法を見出した。The present inventor has found the present invention as a result of earnest efforts and studies to achieve the above object. That is, water characterized in that the fixed sodium (Fix-Na 2 O) content is 0.22 wt% or less and the sulfuric acid undissolved residue amount by the sulfuric acid dissolution rate measurement method specified below is 0.12 wt% or less. Aluminum oxide and bauxite as its production method, calcium compound, sodium compound and coal are mixed, crushed and sintered, then,
At least one kind of water or a solution of water, sodium hydroxide or sodium aluminate is added to extract a soluble component of the sinter, the residue is separated, and a silica aluminate solution is prepared after desiliconization treatment. We have found a method for producing aluminum hydroxide, characterized in that fine aluminum hydroxide is added as seeds to the solution and carbon dioxide gas is blown into the solution to precipitate aluminum hydroxide.
【０００６】なお、上記の硫酸溶解率測定法とは１１０
℃で２時間乾燥した水酸化アルミニウム１９５ｇを蒸留
水２５０ｇと濃硫酸３７５ｇとに混合し、撹拌（回転数
２４０rpm ）しながら１０５〜１０７℃にて６０分間溶
解する。その後、溶解液を１リットルの熱湯で希釈し、
Ｃ型定性ロ紙でロ過し、更に１リットルの熱湯で洗浄す
る。ロ紙ごと残渣を１００℃、３０分間乾燥し、ロ紙ご
と秤量し、ロ過前に測定しておいた乾燥ロ紙重量を差し
引いて、残渣重量Ｘｇを求める方法であって、（Ｘ／１
９５）×１００にて硫酸未溶解残渣量（ｗｔ％）とす
る。The above-mentioned method for measuring the solubility of sulfuric acid is 110
195 g of aluminum hydroxide dried at 2 ° C. for 2 hours is mixed with 250 g of distilled water and 375 g of concentrated sulfuric acid, and dissolved at 105 to 107 ° C. for 60 minutes while stirring (rotation speed 240 rpm). Then, dilute the solution with 1 liter of boiling water,
Filter with Type C qualitative paper and wash with 1 liter of boiling water. This is a method of determining the residue weight Xg by drying the residue of the paper together with the paper for 30 minutes at 100 ° C., weighing the paper together and subtracting the weight of the dry paper measured before the filtration.
95) × 100, which is the residual amount of undissolved sulfuric acid (wt%).
【０００７】また、上記の固定ナトリウム（Ｆｉｘ−Ｎ
ａ2 Ｏ）含有量とは水酸化アルミニウム中に含有される
不純物のうちＮａの全量をＮａ2 Ｏとして換算した値、
即ち全ナトリウム（Ｔ−Ｎａ2 Ｏ）より、下記の条件に
て水酸化アルミニウムより溶出した可溶性Ｎａ量をＮａ
2 Ｏとして換算した値、即ち可溶性ナトリウム（Ｗ−Ｎ
ａ2 Ｏ）を差し引いて求めたＮａ2 Ｏ量である。即ち
（Ｆｉｘ−Ｎａ2 Ｏ）＝（Ｔ−Ｎａ2 Ｏ）−（Ｗ−Ｎａ
2 Ｏ）の式より求めるものである。In addition, the above-mentioned fixed sodium (Fix-N
a 2 O) content is a value obtained by converting the total amount of Na among impurities contained in aluminum hydroxide as Na 2 O,
That is, from the total sodium (T-Na 2 O), the amount of soluble Na eluted from aluminum hydroxide was calculated as Na
Value converted as 2 O, that is, soluble sodium (W-N
a 2 O) is subtracted from the amount of Na 2 O. That is, (Fix-Na 2 O) = (T-Na 2 O)-(W-Na
2 O).
【０００８】全ナトリウム（Ｔ−Ｎａ2 Ｏ）量は以下の
方法で求める。即ち、試料水酸化アルミニウム１．００
０ｇを１００ｍｌのビーカーに正確に秤量する。そのビ
ーカーに試薬特級硫酸を（１：１）に蒸留水にて調製し
た希硫酸溶液を１０ｍｌを添加する。加えたビーカーを
硫酸白煙がでない程度の温度（２５０℃位）で１５分間
加熱する。その後、乾固試料を蒸留水にて２５０ｍｌの
メスフラスコに移し２０℃に水冷する。水冷後、Ｌｉと
して０．２ｍｇ／ｍｌのＬｉ内部標準溶液を正確に２５
ｍｌ加え、更に蒸留水を加え、全量２５０ｍｌの定容と
する。その後、ＪＩＳ Ｈ１９０１−１９７７に則っと
った方法で炎光光度計でＮａ量を測定し、Ｎａ2 Ｏ換算
しＴ−Ｎａ2 Ｏとする。The amount of total sodium (T-Na 2 O) is determined by the following method. That is, sample aluminum hydroxide 1.00
Accurately weigh 0 g into a 100 ml beaker. To the beaker, 10 ml of a dilute sulfuric acid solution prepared by adding distilled water to a reagent grade sulfuric acid (1: 1) is added. The added beaker is heated for 15 minutes at a temperature (about 250 ° C) at which sulfuric acid white smoke is not generated. Then, the dried solid sample is transferred to a 250 ml volumetric flask with distilled water and water-cooled to 20 ° C. After cooling with water, exactly 25 mg of 0.2 mg / ml Li internal standard solution was added as Li.
ml, and then distilled water to make a total volume of 250 ml. Then, the amount of Na is measured with a flame photometer by a method according to JIS H1901-1977, and converted into Na 2 O to obtain T-Na 2 O.
【０００９】次に可溶性ナトリウム（Ｗ−Ｎａ2 Ｏ）の
定量法について述べる。１００ｍｌのビーカーに水酸化
アルミニウム５ｇを１ｍｇの単位まで秤り取る。５０〜
６０℃の温湯５０ｍｌを加え、８０〜９０℃にて２時間
保持する。その後、その内容物を５Ｂのロ紙を用いてロ
過し温湯で４回洗浄する。そのロ液を２０℃に冷却し、
Ｌｉとして０．２ｍｇ／ｍｌのＬｉ内部標準溶液を１０
ｍｌ加え、更に蒸留水で全量１００ｍｌにし、ＪＩＳ
Ｈ１９０１−１９７７に則っとり炎光光度計でＮａ量を
測定し、Ｎａ2 Ｏ換算しＷ−Ｎａ2 Ｏとする。Next, a method for quantifying soluble sodium (W-Na 2 O) will be described. 5 g of aluminum hydroxide is weighed to the unit of 1 mg in a 100 ml beaker. 50-
Add 50 ml of hot water at 60 ° C and hold at 80-90 ° C for 2 hours. Then, the contents are filtered with 5B paper and washed 4 times with warm water. Cool the filtrate to 20 ° C,
0.2 mg / ml Li internal standard solution was added as Li.
ml, and then add distilled water to bring the total volume to 100 ml.
According to H1901-1977, the amount of Na is measured with a flame photometer and converted into Na 2 O to obtain W-Na 2 O.
【００１０】本発明の水酸化アルミニウムはギブサイト
Ａｌ（ＯＨ）3 （Ａｌ2 Ｏ3 ・３Ｈ2 Ｏ）である。本発
明の水酸化アルミニウムの特徴となる特性について述べ
る。まず、Ｆｉｘ−Ｎａ2 Ｏの値は０．２２ｗｔ％以下
で、安定して造れる下限値は０．０３ｗｔ％程度であ
る。次に硫酸未溶解残渣量は０．１２ｗｔ％以下で下限
値は０ｗｔ％に近いものまで造ることができる。The aluminum hydroxide of the present invention is gibbsite Al (OH) 3 (Al 2 O 3 .3H 2 O). The characteristic features of the aluminum hydroxide of the present invention will be described. First, the value of Fix-Na 2 O is 0.22 wt% or less, and the lower limit value for stable production is about 0.03 wt%. Next, the sulfuric acid undissolved residue amount is 0.12 wt% or less, and the lower limit value can be made close to 0 wt%.
【００１１】更に本発明の水酸化アルミニウムの大きな
特徴となる特性は１次粒子および２次粒子が揃っている
ことである。アンドレアゼンピペット法による２次粒子
径ｄ50は１８〜１１０μｍであって、ＲＲＳ粒度線図に
プロットした場合、均等数ｎ値は４〜９となり、本発明
の水酸化アルミニウムの２次粒子は粒度が揃っているも
のである。Further, the characteristic feature of the aluminum hydroxide of the present invention is that primary particles and secondary particles are uniform. The secondary particle diameter d 50 by the Andreasen pipette method is 18 to 110 μm, and when plotted on the RRS particle size diagram, the uniform number n value is 4 to 9, and the secondary particles of the aluminum hydroxide of the present invention have a particle size of Are available.
【００１２】次に本発明の製造方法について述べる。原
料としてはボーキサイト、カルシウム化合物、ナトリウ
ム化合物および石炭を使用する。カルシウム化合物とし
てはカルシウムの酸化物、水酸化物、炭酸塩等をいい、
ナトリウム化合物とはナトリウムの水酸化物、炭酸塩を
いう。それぞれを石灰石および炭酸ナトリウムとした場
合、原料としてボーキサイト、石灰石、炭酸ソーダおよ
び石炭を重量比で１．５〜１．８：２：０．１：０．２
の割合で混合し、それを１〜５ｍｍ程度に粉砕し、ロー
タリーキルン等により１２００〜１３００℃にて１〜２
時間焼結し、その後、水、水酸化ナトリウムまたはアル
ミン酸ナトリウムのうち少なくとも１種の水または溶液
を加え、焼結物の可溶分を９０〜１００℃にて抽出し、
残渣を分離し、更に１５０〜２００℃で３０分〜１時間
で処理し珪素分をアルミノ珪酸ナトリウムとして析出し
脱珪処理をし、アルミン酸ナトリウム溶液を造る。Next, the manufacturing method of the present invention will be described. Bauxite, calcium compounds, sodium compounds and coal are used as raw materials. The calcium compound refers to calcium oxide, hydroxide, carbonate, etc.,
The sodium compound refers to sodium hydroxide or carbonate. When each is limestone and sodium carbonate, bauxite, limestone, sodium carbonate and coal are used as raw materials in a weight ratio of 1.5 to 1.8: 2: 0.1: 0.2.
In a ratio of 1 to 5 mm and crushed to a size of 1 to 5 mm, and a rotary kiln or the like at 1200 to 1300 ° C. for 1 to 2
Sintering for a period of time, then adding water or a solution of at least one of water, sodium hydroxide or sodium aluminate, extracting the soluble matter of the sintered product at 90 to 100 ° C.,
The residue is separated and further treated at 150 to 200 ° C. for 30 minutes to 1 hour to deposit a silicon content as sodium aluminosilicate and desiliconize to prepare a sodium aluminate solution.
【００１３】このアルミン酸ナトリウム溶液に水酸化ア
ルミニウムの種子を添加するが、その趣旨について述べ
る。種子として用いる水酸化アルミニウムの好ましい平
均粒子径は３μｍ以下で、３μｍを超えると種子の添加
量を多くする必要がでるとともに、析出する水酸化アル
ミニウムの硫酸未溶解残渣量も多くなるので好ましくな
い。Aluminum hydroxide seeds are added to this sodium aluminate solution, the purpose of which will be described. The preferred average particle size of aluminum hydroxide used as seeds is 3 μm or less, and if it exceeds 3 μm, it is necessary to increase the addition amount of seeds and the amount of the undissolved sulfuric acid residue of the precipitated aluminum hydroxide also increases, which is not preferable.
【００１４】種子の添加量を次式、即ちThe amount of seeds added is calculated by the following formula:
【数１】 で定義する種子率で表示すると、０．１５〜１５％が好
ましい。種子率が０．１５％未満では低Ｆｉｘ−Ｎａ2
Ｏかつ低硫酸未溶解残渣の水酸化アルミニウムは安定し
て造ることができず、また種子率が１５％を超えるとそ
れ以上添加してもその効果はそれ程向上しないため経済
的でないので好ましくない。[Equation 1] When expressed by the seed rate defined in, 0.15 to 15% is preferable. When the seed rate is less than 0.15%, low Fix-Na 2
O and a low-sulfuric acid undissolved residue of aluminum hydroxide cannot be stably produced. Further, if the seed rate exceeds 15%, the effect is not improved so much even if it is added more, which is not economically preferable.
【００１５】上記の種子を添加後、下記のような条件で
炭酸ガスを吹き込み分解させ水酸化アルミニウムを析出
させる。吹き込む溶液のアルミン酸ナトリウム溶液はＡ
ｌ2Ｏ3 換算量として７０〜９０ｇ／ｌ、ＮａＯＨで９
０〜１１０ｇ／ｌの濃度が好ましく、炭酸ガス分解時の
好ましい液温度は５０〜９５℃で、より好ましくは６０
〜９０℃である。Ｆｉｘ−Ｎａ2 Ｏ量は温度が高い方が
少なくなる傾向があるのに対し、硫酸未溶解残渣は温度
が低い方が少ない傾向がある。After the above seeds have been added, carbon dioxide is blown under the following conditions to decompose and precipitate aluminum hydroxide. Sodium aluminate solution of the blowing solution is A
70 to 90 g / l as l 2 O 3 conversion amount, 9 with NaOH
A concentration of 0 to 110 g / l is preferable, and a preferable liquid temperature at the time of carbon dioxide decomposition is 50 to 95 ° C., more preferably 60.
~ 90 ° C. The amount of Fix-Na 2 O tends to decrease as the temperature rises, whereas the sulfuric acid undissolved residue tends to decrease as the temperature lowers.
【００１６】炭酸ガスは空気等で希釈しＣＯ2 ガス濃度
として２０〜４０％にて、上記アルミン酸ナトリウム溶
液１リットル当り上記ガスを０．３〜３Ｎｌ／ｍｉｎの
好ましい投入量で吹き込む。０．３Ｎｌ／ｍｉｎ未満で
は高い析出率を得るのに時間がかかるようになり、３Ｎ
ｌ／ｍｉｎを超えると安定操業に支障を来たし好ましく
ない。炭酸ガス投入時間は一般的に１〜５時間程度が好
ましい。The carbon dioxide gas is diluted with air or the like, and the CO 2 gas concentration is 20 to 40%, and the above gas is blown in at a preferable amount of 0.3 to 3 Nl / min per liter of the sodium aluminate solution. If it is less than 0.3 Nl / min, it takes time to obtain a high deposition rate, and 3N
If it exceeds 1 / min, stable operation is hindered, which is not preferable. Generally, the carbon dioxide charging time is preferably about 1 to 5 hours.
【００１７】本発明の製造方法を種子添加バイヤー法と
比較すると、本発明は反応時間が短く、かつ析出率が７
０〜９０ｗｔ％と高いため、反応槽容積当りの水酸化ア
ルミニウムの生産性が高い。なお、種子を入れ循環させ
る現在主流のバイヤー法の析出率は４０〜６０ｗｔ％で
ある。Comparing the production method of the present invention with the seed addition Bayer method, the present invention shows that the reaction time is short and the precipitation rate is 7%.
Since it is as high as 0 to 90 wt%, the productivity of aluminum hydroxide per reaction tank volume is high. Incidentally, the precipitation rate of the currently mainstream Bayer method in which seeds are put and circulated is 40 to 60 wt%.
【００１８】次に本発明の水酸化アルミニウムを造るた
めの上記の製造方法における条件について述べる。種子
率は高い方が好ましく、例えばｄ50＝２μｍの種子の種
子率が０．５ｗｔ％のとき、析出反応温度が８０℃以下
ではＦｉｘ−Ｎａ2 Ｏが０．２ｗｔ％以上となってしま
う。ただ種子の粒径が細かくなると種子率の下限値が下
がってもよい傾向は見られる。Next, the conditions in the above manufacturing method for producing the aluminum hydroxide of the present invention will be described. It is preferable that the seed rate is high. For example, when the seed rate of d 50 = 2 μm seeds is 0.5 wt%, Fix-Na 2 O becomes 0.2 wt% or more at a precipitation reaction temperature of 80 ° C. or lower. However, there is a tendency that the lower limit of the seed rate may be lowered as the grain size of the seed becomes smaller.
【００１９】更に分解反応温度が８０℃の場合、ｄ50＝
３．０μｍの種子では種子率が８ｗｔ％以上でないと好
ましくない。またｄ50＝０．５μｍの種子では、種子率
が０．２ｗｔ％以上なら、Ｆｉｘ−Ｎａ2 Ｏが０．２２
ｗｔ％以下であってかつ硫酸未溶解残渣が０．１２ｗｔ
％以下の水酸化アルミニウムを造ることができる。Further, when the decomposition reaction temperature is 80 ° C., d 50 =
For seeds of 3.0 μm, it is not preferable unless the seed rate is 8 wt% or more. For seeds with d 50 = 0.5 μm, Fix-Na 2 O is 0.22% if the seed rate is 0.2 wt% or more.
% or less and 0.12 wt.% of undissolved sulfuric acid residue
% Aluminum hydroxide can be produced.
【００２０】[0020]
【実施例】以下に実施例および比較例により詳説する。 実施例１〜１３ 中国産ボーキサイト、石灰石、炭酸ソーダおよび石炭
（歴青炭）を１．５：２：０．１：０．２の重量比で混
合し、２ｍｍ程度に粉砕し、ロータリーキルンにて１２
５０℃、１時間焼結する。この焼結物に対し以下の組成
のアルミン酸ナトリウム溶液になるように水を加え、９
５℃にて１時間溶解し、残渣を分離し、１５０℃、４０
分間脱珪処理しアルミノ珪酸ナトリウム等の固形物を除
去し、アルミン酸ナトリウム溶液を得た。[Examples] Examples and comparative examples will be described in detail below. Examples 1 to 13 Bauxite, limestone, sodium carbonate and coal (bituminous coal) produced in China were mixed in a weight ratio of 1.5: 2: 0.1: 0.2, pulverized to about 2 mm, and then rotary kiln was used. 12
Sinter at 50 ° C. for 1 hour. Water was added to this sintered product so that a sodium aluminate solution having the following composition was obtained.
Dissolve at 5 ° C for 1 hour, separate the residue, 150 ° C, 40
Demineralization treatment was performed for minutes to remove solid substances such as sodium aluminosilicate to obtain a sodium aluminate solution.
【００２１】このアルミン酸ナトリウム溶液の組成は Ｆｒｅｅ−ＮａＯＨ １１０ｇ／ｌ Ａｌ2 Ｏ3 （換算） ９０ 〃 Ｎａ2 ＣＯ3! ３０ 〃 Ｋ2 Ｏ ８ 〃 ＳｉＯ2 ０．３ 〃 であった。The composition of this sodium aluminate solution was Free-NaOH 110 g / l Al 2 O 3 (converted) 90 〃 Na 2 CO 3! 30 〃 K 2 O 8 〃 SiO 2 0.3 〃.
【００２２】このアルミン酸ナトリウム溶液に対し、表
１に示す条件、即ち種子粒径ｄ50、種子率、析出温度
で、１０リットルの反応容器にて恒温槽にて２４０rpm
の撹拌機を取付け、空気で希釈しＣＯ2 濃度４０％のガ
スを１０リットルの上記アルミン酸ナトリウム溶液に対
し５．５Ｎｌ／ｍｉｎの速度で吹き込み３時間分解し水
酸化アルミニウムを析出させた。For this sodium aluminate solution, under the conditions shown in Table 1, ie, seed particle size d 50 , seed rate and precipitation temperature, 240 rpm in a thermostat in a 10 liter reaction vessel.
Was installed, and a gas having a CO 2 concentration of 40% was blown into 10 liters of the above sodium aluminate solution at a rate of 5.5 Nl / min to decompose for 3 hours to precipitate aluminum hydroxide.
【００２３】得られた水酸化アルミニウムの特性を表１
に示す。なお上記の種子として使用した水酸化アルミニ
ウムは下記の特性のものであった。The characteristics of the obtained aluminum hydroxide are shown in Table 1.
Shown in The aluminum hydroxide used as the seed had the following characteristics.
【００２４】 [0024]
【００２５】[0025]
【表１】 [Table 1]
【００２６】実施例１４〜１９ 本発明の製造方法としては実施例であるが水酸化アルミ
ニウムのものとしては比較例のものについて記す。実施
例１〜１３で分解に使用したアルミン酸ナトリウム溶液
に対し、表２に示す種子粒径、種子率、分解温度で炭酸
ガスを吹き込み水酸化アルミニウムを析出させた。得ら
れた水酸化アルミニウムの特性を表２に示す。表２に示
した製造条件以外は実施例１〜１３と同一条件、同一操
作をした。Examples 14 to 19 The production method of the present invention is an example, but the aluminum hydroxide is a comparative example. Carbon dioxide was blown into the sodium aluminate solutions used for decomposition in Examples 1 to 13 at the seed particle size, seed rate and decomposition temperature shown in Table 2 to precipitate aluminum hydroxide. The properties of the obtained aluminum hydroxide are shown in Table 2. Except for the manufacturing conditions shown in Table 2, the same conditions and operations as in Examples 1 to 13 were performed.
【００２７】[0027]
【表２】 [Table 2]
【００２８】比較例１〜３ 実施例１〜１３に対し、水酸化アルミニウムの種子を添
加することなく炭酸ガス分解を表３に示す条件で行い表
３に示す特性の水酸化アルミニウムを得た。Comparative Examples 1 to 3 In contrast to Examples 1 to 13, carbon dioxide gas decomposition was carried out under the conditions shown in Table 3 without adding aluminum hydroxide seeds to obtain aluminum hydroxide having the characteristics shown in Table 3.
【００２９】[0029]
【表３】 [Table 3]
【００３０】参考例１〜１０ 種子添加バイヤー法により析出された市販品の水酸化ア
ルミニウム製品の特性を表４に示す。Reference Examples 1 to 10 Table 4 shows the characteristics of commercial aluminum hydroxide products deposited by the seed addition Bayer method.
【００３１】[0031]
【表４】 [Table 4]
【００３２】[0032]
【発明の効果】本発明により、酸に対する未溶解残渣量
が少なく、かつＮａ不純物、特に固定ナトリウム含有量
が少ない特性を持つ水酸化アルミニウムが初めて得られ
た。本発明のものは１次粒子および２次粒子の粒径が揃
っている特徴も具備している。本発明の水酸化アルミニ
ウムは高品位の無機の水処理剤の原料として有用であ
る。Industrial Applicability According to the present invention, aluminum hydroxide having a characteristic of having a small amount of undissolved residue with respect to an acid and a small content of Na impurities, especially fixed sodium, was obtained for the first time. The present invention also has a feature that the particle diameters of the primary particles and the secondary particles are uniform. The aluminum hydroxide of the present invention is useful as a raw material for a high-quality inorganic water treatment agent.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 川合 康夫 神奈川県横浜市神奈川区恵比須町８番地 昭和電工株式会社横浜工場内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Yasuo Kawai 8 Ebisu-cho, Kanagawa-ku, Yokohama, Kanagawa Prefecture Showa Denko KK Yokohama factory
Claims (2)
有量が０．２２ｗｔ％以下で、下記に規定する硫酸溶解
率測定法による硫酸未溶解残渣量が０．１２ｗｔ％以下
であることを特徴とする水酸化アルミニウム。硫酸溶解
率測定法：１１０℃で２時間乾燥した水酸化アルミニウ
ム１９５ｇを蒸留水２５０ｇと濃硫酸３７５ｇとに混合
し、撹拌（回転数２４０rpm ）しながら１０５〜１０７
℃にて６０分間溶解する。その後、溶解液を１リットル
の熱湯で希釈し、Ｃ型定性ロ紙でロ過し、更に１リット
ルの熱湯で洗浄する。ロ紙ごと残渣を１００℃、３０分
間乾燥し、ロ紙ごと秤量し、ロ過前に測定しておいた乾
燥ロ紙重量を差し引いて、残渣重量Ｘｇを求め、（Ｘ／
１９５）×１００にて硫酸未溶解残渣量（ｗｔ％）とす
る。1. The content of fixed sodium (Fix-Na 2 O) is 0.22 wt% or less, and the amount of sulfuric acid undissolved residue measured by the sulfuric acid dissolution rate measurement method specified below is 0.12 wt% or less. Aluminum hydroxide. Sulfuric acid dissolution rate measurement method: 195 g of aluminum hydroxide dried at 110 ° C. for 2 hours was mixed with 250 g of distilled water and 375 g of concentrated sulfuric acid, and the mixture was stirred at a rotational speed of 240 rpm for 105-107.
Dissolve at 60 ° C for 60 minutes. Then, the solution is diluted with 1 liter of hot water, filtered with a C-type qualitative filter paper, and further washed with 1 liter of hot water. The residue with the paper is dried at 100 ° C. for 30 minutes, the paper is weighed, and the weight of the dry paper measured before the filtration is subtracted to obtain the residue weight Xg.
195) × 100, which is the residual amount of undissolved sulfuric acid (wt%).
リウム化合物および石炭を混合し、粉砕後焼結し、その
後、水、水酸化ナトリウムまたはアルミン酸ナトリウム
のうち少なくとも１種の水または溶液を加え、焼結物の
可溶分を抽出し、残渣を分離し、更に脱珪処理後、アル
ミン酸ナトリウム溶液を造り、その溶液に微細な水酸化
アルミニウムを種子として添加し炭酸ガスを吹き込んで
水酸化アルミニウムを析出させることを特徴とする水酸
化アルミニウムの製造方法。2. A sintered product obtained by mixing bauxite, a calcium compound, a sodium compound, and coal, pulverizing and sintering, and then adding at least one water or solution of water, sodium hydroxide or sodium aluminate to the sintered product. Soluble content is extracted, the residue is separated, and after desiliconization, a sodium aluminate solution is made, and fine aluminum hydroxide is added as seeds to the solution and carbon dioxide gas is blown into it to precipitate aluminum hydroxide. A method for producing aluminum hydroxide, comprising:
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7128468A JPH08325011A (en) | 1995-05-26 | 1995-05-26 | Aluminum hydroxide and its production |
| CN95109122A CN1075043C (en) | 1995-05-26 | 1995-06-27 | Aluminium hydroxide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7128468A JPH08325011A (en) | 1995-05-26 | 1995-05-26 | Aluminum hydroxide and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08325011A true JPH08325011A (en) | 1996-12-10 |
Family
ID=14985481
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7128468A Pending JPH08325011A (en) | 1995-05-26 | 1995-05-26 | Aluminum hydroxide and its production |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JPH08325011A (en) |
| CN (1) | CN1075043C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008019158A (en) * | 2006-06-14 | 2008-01-31 | Hiroko Ishikuri | Method for producing high purity aluminum hydroxide and high purity aluminum hydroxide obtained by the method |
| CN100378000C (en) * | 2006-08-25 | 2008-04-02 | 中国铝业股份有限公司 | Method for producing micropowder aluminium hydroxide by neutralization method |
| WO2009066308A3 (en) * | 2007-07-09 | 2009-07-16 | Aditya Birla Science & Technol | Extraction of alumina |
| CN114130382A (en) * | 2021-12-14 | 2022-03-04 | 河南能源化工集团研究总院有限公司 | Aluminum hydroxide powder and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102476A (en) * | 1985-04-01 | 1987-01-17 | 山东铝厂 | A kind of production of aluminum hydroxide method as weighting agent and fire retardant |
| CN1031689A (en) * | 1987-09-02 | 1989-03-15 | 山东铝厂 | Producing sandy alumina through continuous stirring and decomposition of seed technology |
| CN1032650A (en) * | 1987-10-17 | 1989-05-03 | 全苏铝镁电极工业科学研究设计院 | The preparation method of aluminium hydroxide |
-
1995
- 1995-05-26 JP JP7128468A patent/JPH08325011A/en active Pending
- 1995-06-27 CN CN95109122A patent/CN1075043C/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008019158A (en) * | 2006-06-14 | 2008-01-31 | Hiroko Ishikuri | Method for producing high purity aluminum hydroxide and high purity aluminum hydroxide obtained by the method |
| CN100378000C (en) * | 2006-08-25 | 2008-04-02 | 中国铝业股份有限公司 | Method for producing micropowder aluminium hydroxide by neutralization method |
| WO2009066308A3 (en) * | 2007-07-09 | 2009-07-16 | Aditya Birla Science & Technol | Extraction of alumina |
| CN114130382A (en) * | 2021-12-14 | 2022-03-04 | 河南能源化工集团研究总院有限公司 | Aluminum hydroxide powder and preparation method thereof |
| CN114130382B (en) * | 2021-12-14 | 2023-11-21 | 河南能源化工集团研究总院有限公司 | Aluminum hydroxide powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1129194A (en) | 1996-08-21 |
| CN1075043C (en) | 2001-11-21 |
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