JPS60137825A - Production of titania of high purity - Google Patents
Production of titania of high purityInfo
- Publication number
- JPS60137825A JPS60137825A JP24460783A JP24460783A JPS60137825A JP S60137825 A JPS60137825 A JP S60137825A JP 24460783 A JP24460783 A JP 24460783A JP 24460783 A JP24460783 A JP 24460783A JP S60137825 A JPS60137825 A JP S60137825A
- Authority
- JP
- Japan
- Prior art keywords
- titania
- added
- solution
- acid
- titanium oxide
- 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.)
- Granted
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、市販酸化チタンよシネ純物を除去して、効率
よく高純度チタニアを得る方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for efficiently obtaining high purity titania by removing commercially available titanium oxide and cine pure substances.
チタニアは工業的に重要な原料であるが、桓々の不純物
を含んでおシ、チタニア磁器、チタン酸バリウム等の電
子材料関係に用いる場合には、高純度のものが要求され
る。従来、高純度チタニアを得るためには、金属チタン
を酸化して用いてｈる。市販品の不純物を示すと第１表
のとおりである。Although titania is an industrially important raw material, it contains many impurities and requires high purity when used in electronic materials such as titania porcelain and barium titanate. Conventionally, in order to obtain high-purity titania, metallic titanium is oxidized and used. Table 1 shows impurities in commercially available products.
第１表 市販チタニアの不純物組成 （イ）本発明は、
市販チタニアより不純物を効率よく除き、高純度チタニ
アを製造する方法を開光すべく鋭意研究を重ねた結果、
ペルオキシチタン酸の性質を利用して、チタンのみ全分
離させる方法を見出し、本発明を完成するに至ったので
ある。すなわち、本発明は、酸化チタン全炭酸ナトリウ
ムと浴融し、今後、酸を加え溶解してイ↓チられる溶液
に過ｌ！Ｒ（ヒ水素金添加し、こｎ２アンモニア水で中
オロして濾過し、Ｐ液を加熱那ｊ１４−させて生成する
白色沈殿をＰ取した後、この沈殿全塩酸に溶解した溶液
を陰イオン交換樹脂で処；ｌ−！Ｉｉ Ｌ 、処理溶液
にアンモニア水を加えて水酸化物とし、この水酸化物を
焼成することを特徴とする。Ｈ４５純度チタニアの製造
法である。Table 1 Impurity composition of commercially available titania (a) The present invention:
As a result of intensive research to discover a method to efficiently remove impurities from commercially available titania and produce high-purity titania,
By utilizing the properties of peroxytitanic acid, they discovered a method for completely separating only titanium, and completed the present invention. That is, in the present invention, titanium oxide is melted in a bath with all sodium carbonate, and then an acid is added and dissolved to form a solution that can be melted. R (add gold arsenide, rinse with n2 aqueous ammonia, filter, heat the P solution and collect the white precipitate produced, then dissolve the entire precipitate in hydrochloric acid and anion. Treatment with an exchange resin; l-!Ii L The process is characterized by adding ammonia water to the treatment solution to form a hydroxide, and firing the hydroxide.This is a method for producing H45 purity titania.
本発明の詳細な説明すると、捷ず、市販チタニア全炭酸
ナトリウムと溶融し、今後、塩酸または硫酸を加えて加
熱溶解させた溶故に、Ｉａ酸化水素水全添加ｒる。この
過酸化水素水の添加により、溶液は黄褐色に変化するが
、これはペルオキシチタン酸の色であって、同時にＦｅ
”Ｆ）：ｌ： Ｆｅ”＋に、馳も原子価の商い状態にな
る。これ全アンモニア水を用いて中和を行なうと、’
ｐＨ３，５（らいからＦｅｓ＋、Ａ７およびＭｎの水酸
化９勿が生じてくるが、−ｐ、Ｈ７を超さなければ、Ｔ
ｉの水酸化物は生じてこない。この状態でＦ紙金用いて
濾過を行なうと、沖紙上にｐｅ！＋、ＡｔおよびＭｎの
水酸化物が残り、Ｃａ 、 Ｍｇ、Ｎａ、に、Ｔｉ等は
Ｐ液に移る。このＦ液を加熱沸騰きせると、溶液は白く
濁り、Ｔ ｉの水酸１し物の沈殿を生ずる。To explain the present invention in detail, without stirring, commercially available titania is melted with all sodium carbonate, and then hydrochloric acid or sulfuric acid is added and dissolved by heating, and all Ia hydrogen oxide water is added thereto. By adding this hydrogen peroxide solution, the solution changes to a yellowish brown color, which is the color of peroxytitanic acid, and at the same time, it turns into a yellowish brown color.
``F):l: Fe''+ also causes valence to change. When this is neutralized using total ammonia water, '
pH 3.5 (from leprosy, hydroxylation of Fes+, A7 and Mn will occur, but unless it exceeds -p, H7, T
The hydroxide of i is not produced. When filtration is performed using F paper gold in this state, pe! +, At and Mn hydroxides remain, and Ca, Mg, Na, Ti, etc. are transferred to the P solution. When this solution F is heated to boiling, the solution becomes cloudy and a precipitate of Ti hydroxyl alone is produced.
上記沈殿の濾過を行なうことにより、Ｃａ 、 Ｍｇ、
Ｎａ、ＫからＴｉを分離することができる。この沈殿全
塩酸に溶解し、微：ｆｊｔに含まｆしているＦｅ３“全
除去するためにＣ４型陰イオン交換樹脂（ダウエックス
１×８）に通す。この際、塩酸製置が０．２ Ｎ以下に
ならなければ、 Ｆｅ３＋は完全にイＩ７３脂に挟着ち
□れる。この溶出液に希アンモニア水（１：１）ｉ加え
てアルカリ性にすると、’Ｉ’１（ＯＩＪ）、が沈殿し
てくる。この沈殿を濾過し、沈殿を１，２００〜１．８
００ ’Ｃに仮焼すると、高純度チタニアが４４４られ
る。By filtering the above precipitate, Ca, Mg,
Ti can be separated from Na and K. The entire precipitate was dissolved in hydrochloric acid and passed through a C4 type anion exchange resin (Dowex 1x8) to completely remove the Fe3 contained in the fine amount of fjt. If the concentration does not fall below N, Fe3+ will be completely sandwiched between I73 fats. When dilute ammonia water (1:1) is added to this eluate to make it alkaline, 'I'1 (OIJ) will precipitate. This precipitate is filtered and the precipitate has a concentration of 1,200 to 1.8
When calcined to 00'C, 444% of high purity titania is produced.
本究明において用いられる陰イオン交換樹脂としては、
ダウエックス１ｘ ８ （部品名、ダウケミカル社製）
、アンバライ）ＩＲＡ−４００（商品名。The anion exchange resin used in this study is
DOWEX 1x 8 (Part name, manufactured by Dow Chemical Company)
, Anbarai) IRA-400 (product name.
米国ロームアンドハース社製）などが卒げら７″Ｌる。(manufactured by Rohm and Haas, USA) etc. are 7"L.
本発明によれば、市販チタニアより不純物の極端に少な
い高純度チタニアを製造することができ、経済的で、工
業的製法として好適である。According to the present invention, it is possible to produce highly pure titania with extremely less impurities than commercially available titania, and it is economical and suitable as an industrial production method.
次に、本発明を実施例により、さらに具体的に説明する
。Next, the present invention will be explained in more detail with reference to Examples.
市販酸化チタン０．２７を白金ルツボに秤取し、１０倍
量の炭酸ナトリウムを加え溶融する。これが冷却した後
、希塩酸（１：１）１０−を加え、加熱溶解する。この
溶液に３０％過酸化水素水５ｍｅ ｆ添加し、アンモニ
ア水（１：１）を加えて中和し、ｐｍ ７に調整する。Weigh out 0.27 g of commercially available titanium oxide into a platinum crucible, add 10 times the amount of sodium carbonate, and melt. After this is cooled, 10-10% of dilute hydrochloric acid (1:1) is added and dissolved by heating. Add 5 mef of 30% hydrogen peroxide solution to this solution, neutralize by adding aqueous ammonia (1:1), and adjust the pH to 7.
５Ｂ濾紙を用いて沈殿を濾過し、Ｐ液を加熱沸騰させる
こと、Ｐ液は白濁を生じ、水酸化チタンの沈殿が生成す
る。この沈殿を５ＢＰ紙で濾過し、沈＄を２Ｎ塩酸１０
−に溶解する。The precipitate is filtered using 5B filter paper, and the P solution is heated to boiling. The P solution becomes cloudy and a titanium hydroxide precipitate is formed. This precipitate was filtered through 5BP paper, and the precipitate was dissolved in 2N hydrochloric acid 10
- dissolves in
別に陰イオン交換樹脂柱として、クロマトグラフ管にダ
ウエックスＩ Ｘ ８ １０ ｍｅを充填し、２Ｎ塩酸
５〇−金泥したもの全用意する。上記２Ｎ塩酸試料溶液
を陰イオン交換樹脂柱に流し、試料溶液を流し終ってか
ら、ぜらに２Ｎ塩酸２０ｒｎｌ！ヲ流し、この溶出液に
希アンモニア水（１：１）を加えてアルカリ性にすると
、Ｔｉ（ＯＲ入の沈殿を生ずる。この沈殿を５ＢＦ紙を
用いて濾過し、沈殿物を電気炉で１，２００〜１．８０
Ｄ Ｃで仮焼すると、純粋なチタニアが得られる。得
られたチタニアの純度は９９．７俤、収率は９９チであ
った。Separately, as an anion exchange resin column, a chromatography tube filled with DOWEX IX810 me and mixed with 2N hydrochloric acid 50-gold solution was prepared. Pour the above 2N hydrochloric acid sample solution onto the anion exchange resin column, and after the sample solution has finished flowing, pour 20rnl of 2N hydrochloric acid into the bathtub. When the eluate is made alkaline by adding dilute ammonia water (1:1), a precipitate containing Ti (OR) is generated. This precipitate is filtered using 5BF paper, and the precipitate is heated in an electric furnace for 1. 200-1.80
Calcining at DC yields pure titania. The purity of the obtained titania was 99.7 yen, and the yield was 99 yen.
不純物の分析結果は第２表に示すとおりである。The analysis results of impurities are shown in Table 2.
第２表Table 2
Claims (1)
溶解して得られる溶液に過酸化水素水を′添加し、これ
をアンモニア水で中和してν過し、Ｐ液を加熱沸騰させ
て生成する白色沈殿を戸数した後、この沈殿を塩酸に溶
解した溶液を陰イオン交換樹脂で処理し、処理溶液にア
ンモニア水を加えて水酸化物とし、この水酸化物を焼成
することを特徴とする高純度チタニアの製造法。Titanium oxide is melted with sodium carbonate, then acid is added and dissolved, hydrogen peroxide is added to the resulting solution, this is neutralized with aqueous ammonia and filtered, and the P solution is heated to boiling. After removing the white precipitate that forms, a solution of this precipitate dissolved in hydrochloric acid is treated with an anion exchange resin, aqueous ammonia is added to the treated solution to form a hydroxide, and this hydroxide is calcined. A method for producing high-purity titania.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24460783A JPS60137825A (en) | 1983-12-27 | 1983-12-27 | Production of titania of high purity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24460783A JPS60137825A (en) | 1983-12-27 | 1983-12-27 | Production of titania of high purity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60137825A true JPS60137825A (en) | 1985-07-22 |
| JPS629533B2 JPS629533B2 (en) | 1987-02-28 |
Family
ID=17121245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24460783A Granted JPS60137825A (en) | 1983-12-27 | 1983-12-27 | Production of titania of high purity |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60137825A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0280378A2 (en) * | 1987-02-26 | 1988-08-31 | Mita Industrial Co. Ltd. | White toner |
| KR20020063532A (en) * | 2002-06-07 | 2002-08-03 | 이종국 | Preparation of Titania Whiskers by Exudation of Na ions in Sodium Titanate Whiskers |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01180822U (en) * | 1988-06-01 | 1989-12-26 |
-
1983
- 1983-12-27 JP JP24460783A patent/JPS60137825A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0280378A2 (en) * | 1987-02-26 | 1988-08-31 | Mita Industrial Co. Ltd. | White toner |
| KR20020063532A (en) * | 2002-06-07 | 2002-08-03 | 이종국 | Preparation of Titania Whiskers by Exudation of Na ions in Sodium Titanate Whiskers |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS629533B2 (en) | 1987-02-28 |
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