JPS629533B2 - - Google Patents
Info
- Publication number
- JPS629533B2 JPS629533B2 JP24460783A JP24460783A JPS629533B2 JP S629533 B2 JPS629533 B2 JP S629533B2 JP 24460783 A JP24460783 A JP 24460783A JP 24460783 A JP24460783 A JP 24460783A JP S629533 B2 JPS629533 B2 JP S629533B2
- Authority
- JP
- Japan
- Prior art keywords
- precipitate
- titania
- solution
- hydrochloric acid
- hydroxide
- 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
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000003957 anion exchange resin Substances 0.000 claims description 6
- 150000004679 hydroxides Chemical class 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- -1 and after cooling Chemical compound 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Description
本発明は、市販酸化チタンより不純物を除去し
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。
チタニアは工業的に重要な原料であるが、種々
の不純物を含んでおり、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い
る。市販品の不純物を示すと第１表のとおりであ
る。
The present invention relates to a method for efficiently obtaining high purity titania by removing impurities from commercially available titanium oxide. Although titania is an industrially important raw material, it contains various impurities, and when used in electronic materials such as titania porcelain and barium titanate, high purity is required. Conventionally, in order to obtain high-purity titania, metallic titanium has been oxidized. Table 1 shows impurities in commercially available products.
【表】【table】
【表】
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発すべ
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、チタンのみを分離させる方法を
見出し、本発明を完成するに至つたのである。す
なわち、本発明は、酸化チタンを炭酸ナトリウム
と溶融し、酸を加え溶解して得られる溶液に過酸
化水素を添加し、これをアンモニア水で中和して
過し、液を加熱沸騰させて生成する白色沈殿
を取した後、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で
ある。
本発明を詳細に説明すると、まず、市販チタニ
アを炭酸ナトリウムと溶融し、冷後、塩酸または
〓〓〓〓
硫酸を加えて加熱溶解させた溶液に過酸化水素水
を添加する。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
ン酸の色であつて、同時にFe2+はFe3+に、Mnも
原子価の高い状態になる。これをアンモニア水を
用いて中和を行なうと、PH3.5くらいからFe3+、
AlおよびMnの水酸化物が生じてくるが、PH７を
超さなければ、Tiの水酸化物は生じてこない。
この状態で紙を用いて過を行なうと、紙上
にFe3+、AlおよびMnの水酸化物が残り、Ca、
Mg、Na、Ｋ、Ti等は液に移る。この液を加
熱沸騰させると、溶液は白く濁り、Tiの水酸化
物の沈殿を生ずる。
上記沈殿の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
の沈殿を塩酸に溶解し、微量に含まれている
Fe3+を除去するためにCl型陰イオン交換樹脂
（ダウエツクス１×８）に通す。この際、塩酸濃
度が0.2N以下にならなければ、Fe3+は完全に樹
脂に吸着される。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
（OH）4が沈殿してくる。この沈殿を過し、沈殿
を1200〜1800℃に仮焼すると、高純度チタニアが
得られる。
本発明において用いられる陰イオン交換樹脂と
しては、ダウエツクス１×８（商品名、ダウケミ
カル社製）、アンバライトIRA―400（商品名、米
国ロームアンドハース社製）などが挙げられる。
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。
次に、本発明を実施例により、さらに具体的に
説明する。
市販酸化チタン0.2ｇ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）10mlを加え、加熱
溶解する。この溶液に30％過酸化水素水５mlを添
加し、アンモニア水（１：１）を加えて中和し、
PH７に調整する。5B紙を用いて沈殿を過
し、液を加熱沸騰させること、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
5B紙で過し、沈殿を2N塩酸10mlに溶解す
る。
別に陰イオン交換樹脂柱として、クロマトグラ
フ管にダウエツクス１×８ 10mlを充填し、2N
塩酸50mlを流したものを用意する。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
を流し終つてから、さらに2N塩酸20mlを流し、
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（OH）4の沈殿を生ず
る。この沈殿を5B紙を用いて過し、沈殿物
を電気炉で1200〜1800℃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％、収率は99％であつた。
不純物の分析結果は第２表に示すとおりであ
る。[Table] As a result of intensive research to develop a method to efficiently remove impurities from commercially available titania and produce high-purity titania, the present invention was developed as a method to separate only titanium by utilizing the properties of peroxytitanic acid. They discovered this and completed the present invention. That is, in the present invention, hydrogen peroxide is added to the solution obtained by melting titanium oxide with sodium carbonate, adding acid and dissolving it, neutralizing this with aqueous ammonia and filtering it, and heating the liquid to boiling. After removing the white precipitate that is produced, 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. This is a method for producing high-purity titania. To explain the present invention in detail, first, commercially available titania is melted with sodium carbonate, and after cooling, hydrochloric acid or
Hydrogen peroxide solution is added to the solution in which sulfuric acid is added and dissolved by heating. 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, Fe 2+ becomes Fe 3+ and Mn also becomes highly valent. When this is neutralized using ammonia water, Fe 3+ ,
Al and Mn hydroxides are produced, but Ti hydroxides are not produced unless the pH exceeds 7.
When filtration is carried out using paper in this state, hydroxides of Fe 3+ , Al and Mn remain on the paper, and Ca,
Mg, Na, K, Ti, etc. move into the liquid. When this solution is heated to boiling, it becomes cloudy and a Ti hydroxide precipitates. By carrying out the above precipitation, Ca,
Ti can be separated from Mg, Na, and K. This precipitate is dissolved in hydrochloric acid, and a trace amount of
Pass through a Cl type anion exchange resin (Dowex 1×8) to remove Fe 3+ . At this time, unless the hydrochloric acid concentration becomes 0.2N or less, Fe 3+ is completely adsorbed by the resin. When this eluate is made alkaline by adding dilute ammonia water (1:1), Ti
(OH) 4 will precipitate. High purity titania is obtained by passing through this precipitation and calcining the precipitate at 1200 to 1800°C. Examples of the anion exchange resin used in the present invention include DOWEX 1×8 (trade name, manufactured by Dow Chemical Company), Amberlite IRA-400 (trade name, manufactured by Rohm and Haas Company, USA), and the like. 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. Next, the present invention will be explained in more detail with reference to Examples. Weighed 0.2g of commercially available titanium oxide into a platinum crucible,
Add 10 times the amount of sodium carbonate and melt. After this has cooled, add 10 ml of dilute hydrochloric acid (1:1) and dissolve by heating. Add 5 ml of 30% hydrogen peroxide to this solution, neutralize by adding ammonia water (1:1),
Adjust to PH7. Filter the precipitate using 5B paper and heat the liquid to boiling. The liquid becomes cloudy and a titanium hydroxide precipitate is formed. This precipitation
Pass through 5B paper and dissolve the precipitate in 10 ml of 2N hydrochloric acid. Separately, fill a chromatography tube with 10ml of Dowex 1x8 as an anion exchange resin column, and
Prepare a container in which 50ml of hydrochloric acid has been poured. Pour the above 2N hydrochloric acid sample solution onto the anion exchange resin column, and after the sample solution has finished flowing, add 20ml of 2N hydrochloric acid,
When this eluate is made alkaline by adding dilute ammonia water (1:1), Ti(OH) 4 precipitates. This precipitate is filtered through 5B paper and the precipitate is calcined in an electric furnace at 1200-1800°C to obtain pure titania. The purity of the titania obtained is
The yield was 99.7%. The analysis results of impurities are shown in Table 2.
【表】
〓〓〓〓
[Table] 〓〓〓〓
Claims (1)
後、酸を加え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過
し、液を加熱沸騰させて生成する白色沈殿を
取した後、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。1 Melt titanium oxide with sodium carbonate, cool it, add acid to dissolve it, add hydrogen peroxide to the resulting solution, neutralize it with aqueous ammonia, filter it, and heat the liquid to boiling. After removing the white precipitate, this precipitate is dissolved in hydrochloric acid and treated with an anion exchange resin, aqueous ammonia is added to the treated solution to form a hydroxide, and this hydroxide is calcined. Production method of 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 JPS60137825A (en) | 1985-07-22 |
| JPS629533B2 true 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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01180822U (en) * | 1988-06-01 | 1989-12-26 |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4855204A (en) * | 1987-02-26 | 1989-08-08 | Mita Industrial Co., Ltd. | White toner containing a high purity titanium dioxide pigment |
| KR20020063532A (en) * | 2002-06-07 | 2002-08-03 | 이종국 | Preparation of Titania Whiskers by Exudation of Na ions in Sodium Titanate Whiskers |
-
1983
- 1983-12-27 JP JP24460783A patent/JPS60137825A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01180822U (en) * | 1988-06-01 | 1989-12-26 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60137825A (en) | 1985-07-22 |
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