JP4581093B2 - Production method of titanium oxide - Google Patents
Production method of titanium oxide Download PDFInfo
- Publication number
- JP4581093B2 JP4581093B2 JP2006249441A JP2006249441A JP4581093B2 JP 4581093 B2 JP4581093 B2 JP 4581093B2 JP 2006249441 A JP2006249441 A JP 2006249441A JP 2006249441 A JP2006249441 A JP 2006249441A JP 4581093 B2 JP4581093 B2 JP 4581093B2
- Authority
- JP
- Japan
- Prior art keywords
- titanium oxide
- dryness
- nitric acid
- production method
- tio
- 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.)
- Active
Links
Images
Description
本発明は、酸化チタンの製造法に関する。 The present invention relates to a method for producing titanium oxide.
酸化チタンは、光、温度変化に対して非常に安定であり、人体に対しても無害であること、また、着色性や紫外線遮断能力に優れることから、白色塗料や顔料の原材料、チタン酸バリウムなどの電子部品用誘電体の原材料、あるいは、光触媒として活用され、工学的に重要である。 Titanium oxide is very stable against changes in light and temperature, is harmless to the human body, and has excellent colorability and UV blocking ability. It is used as a raw material for dielectrics for electronic parts, etc., or as a photocatalyst, and is important for engineering.
従来の酸化チタンの工業的製造法としては、硫酸チタンを加水分解して焼成する硫酸法と、四塩化チタンを高温で酸化する塩素法がある。しかし、硫酸法では、廃硫酸の処理が必要である、反応に１０００℃以上の高温が必要である、未反応のＴｉＯＳＯ４が残存する、亜硫酸ガスの処理が必要である、という問題があった。また、塩素法では、中間生成物となるＴｉＣｌ４の取り扱いが困難である、反応に１０００℃以上の高温が必要である、ＣａやＭｇなどの不純物が混入する、塩化水素ガスの処理が必要である、という問題があった。このように、従来の製造法は、危険性が高く、環境負荷が大きいという問題を有していた。 Conventional industrial production methods of titanium oxide include a sulfuric acid method in which titanium sulfate is hydrolyzed and fired, and a chlorine method in which titanium tetrachloride is oxidized at a high temperature. However, in the sulfuric acid method, there is a problem that waste sulfuric acid treatment is necessary, the reaction requires a high temperature of 1000 ° C. or more, unreacted TiOSO 4 remains, and treatment with sulfurous acid gas is necessary. . In addition, in the chlorine method, it is difficult to handle TiCl 4 as an intermediate product, the reaction requires a high temperature of 1000 ° C. or more, impurities such as Ca and Mg are mixed, and treatment of hydrogen chloride gas is necessary. There was a problem that there was. Thus, the conventional manufacturing method has a problem that it is highly dangerous and has a large environmental load.
これらの問題を解決する製造法としては、前駆体であるＮａＬｎＴｉＯ４（Ｌｎ＝希土類）を硝酸に溶解して蒸発乾固することにより、１００℃以下の低温で結晶性の酸化チタンを析出させる方法が開示されている（特許文献１）。
しかし、この方法は、原料に高価な希土類酸化物を用いるため、製造コストが高くなってしまうという問題があった。 However, this method has a problem that the manufacturing cost is high because an expensive rare earth oxide is used as a raw material.
そこで、本発明は上記問題点に鑑み、反応条件が穏和であって、環境負荷が小さく、さらに原料が安価であって低コストで酸化チタンを製造することのできる、酸化チタンの製造法を提供することをその目的とする。 Therefore, in view of the above problems, the present invention provides a method for producing titanium oxide, in which the reaction conditions are mild, the environmental load is small, the raw material is inexpensive, and titanium oxide can be produced at low cost. The purpose is to do.
上記課題を達成するため種々検討した結果、前駆体Ｎａ１６Ｔｉ１０Ｏ２８を硝酸に溶解し、蒸発乾固することでルチル型酸化チタンを製造することができることを見出し、本発明を完成させた。 As a result of various studies to achieve the above-mentioned problems, the present inventors have found that a rutile type titanium oxide can be produced by dissolving the precursor Na 16 Ti 10 O 28 in nitric acid and evaporating to dryness, thereby completing the present invention. .
すなわち、本発明の酸化チタンの製造法は、Ｎａ１６Ｔｉ１０Ｏ２８を硝酸に溶解し、１００℃以下で蒸発乾固することを特徴とする。 That is, the titanium oxide production method of the present invention is characterized in that Na 16 Ti 10 O 28 is dissolved in nitric acid and evaporated to dryness at 100 ° C. or lower.
また、Ｎａ１６Ｔｉ１０Ｏ２８はＮａ２ＣＯ３とＴｉＯ２をＮａ ２ ＣＯ ３ ：ＴｉＯ ２ ＝４：５のモル比で湿式混合し、焼成することで得られたものであることを特徴とする。 Further, Na 16 Ti 10 O 28 is obtained by wet-mixing Na 2 CO 3 and TiO 2 at a molar ratio of Na 2 CO 3 : TiO 2 = 4: 5 and firing. To do.
本発明の硝酸含有水溶液からの酸化チタンの製造法によれば、穏和な環境負荷が小さい反応条件で、かつ、低コストで、結晶性の酸化チタンを製造することができる。 According to the method for producing titanium oxide from the nitric acid-containing aqueous solution of the present invention, crystalline titanium oxide can be produced under reaction conditions with a mild environmental load and at low cost.
本発明の酸化チタンの製造法は、前駆体のＮａ１６Ｔｉ１０Ｏ２８を硝酸に溶解し、１００℃以下で蒸発乾固するものである。この製造法によれば、結晶性のルチル型酸化チタンを製造することができる。酸化チタン成分の原料としては、高純度のアナターゼ相およびルチル相の試薬だけでなく、ルチル鉱石や不純物を含む低純度の原料も用いることができる。さらに、Ｎａ１６Ｔｉ１０Ｏ２８を硝酸に溶解した後に不溶物を濾過などにより除去し、蒸発乾固後に水洗を繰り返し、乾燥をすることで、得られる酸化チタンの純度を向上させることができる。蒸発乾固の温度は、製造効率を考慮して短時間で蒸発乾固させるために、７０℃以上とするのが好ましい。 In the method for producing titanium oxide according to the present invention, the precursor Na 16 Ti 10 O 28 is dissolved in nitric acid and evaporated to dryness at 100 ° C. or lower. According to this production method, crystalline rutile type titanium oxide can be produced. As a raw material for the titanium oxide component, not only high purity anatase phase and rutile phase reagents, but also low purity raw materials containing rutile ore and impurities can be used. Furthermore, after dissolving Na 16 Ti 10 O 28 in nitric acid, insoluble matters are removed by filtration and the like, and after evaporation to dryness, washing with water is repeated and drying is performed, whereby the purity of the obtained titanium oxide can be improved. The temperature for evaporation to dryness is preferably 70 ° C. or higher in order to evaporate to dryness in a short time in consideration of production efficiency.
ここで、前駆体となるＮａ１６Ｔｉ１０Ｏ２８は、Ｎａ２ＣＯ３とＴｉＯ２をアセトンなどで湿式混合し、焼成することで得られる。Ｎａ２ＣＯ３：ＴｉＯ２＝４：５のモル比で混合することで、Ｎａ１６Ｔｉ１０Ｏ２８が得られる。焼成温度は900℃以上、焼成時間は１時間以上とするのが好ましい。 Here, Na 16 Ti 10 O 28 serving as a precursor can be obtained by wet-mixing Na 2 CO 3 and TiO 2 with acetone or the like and baking. By mixing at a molar ratio of Na 2 CO 3 : TiO 2 = 4: 5, Na 16 Ti 10 O 28 is obtained. The firing temperature is preferably 900 ° C. or higher, and the firing time is preferably 1 hour or longer.
なお、Ｎａ１６Ｔｉ１０Ｏ２８を除く、ほかの組成のナトリウムチタン酸塩は、硝酸に溶解しないため、前駆体として用いることができない。 Incidentally, except for Na 16 Ti 10 O 28, sodium titanate other composition because it does not dissolve in nitric acid, it can not be used as a precursor.
本発明の酸化チタンの製造法によれば、１００℃以下の穏和な条件で酸化チタンを製造することができ、さらに、希土類酸化物のような高価な原料を用いないので、従来法よりも低コストで酸化チタンを製造することができる。 According to the method for producing titanium oxide of the present invention, titanium oxide can be produced under mild conditions of 100 ° C. or lower, and furthermore, since expensive materials such as rare earth oxides are not used, it is lower than the conventional method. Titanium oxide can be produced at a low cost.
さらに、Ｎａ１６Ｔｉ１０Ｏ２８を溶解する硝酸に適量の塩酸を添加し、蒸発乾固することにより、アナターゼ型酸化チタンを得ることができる。したがって、必要に応じてルチル型とアナターゼ型の酸化チタンを作り分けることができる。 Furthermore, an anatase-type titanium oxide can be obtained by adding an appropriate amount of hydrochloric acid to nitric acid that dissolves Na 16 Ti 10 O 28 and evaporating to dryness. Therefore, rutile type and anatase type titanium oxides can be made as required.
なお、本発明は上記実施形態に限定されるものではなく、本発明の思想を逸脱しない範囲で種々の変形実施が可能である。以下、具体例に基づき、より詳細に説明する。 The present invention is not limited to the above embodiment, and various modifications can be made without departing from the spirit of the present invention. Hereinafter, it demonstrates in detail based on a specific example.
はじめに、前駆体となるＮａ１６Ｔｉ１０Ｏ２８を合成した。原料にＮａ２ＣＯ３（メルク社製）、ＴｉＯ２を用いて、これら原料をＮａ２ＣＯ３：ＴｉＯ２＝４：５のモル比で秤量してアセトンで湿式混合し、1000℃で１時間の焼成を行った。得られた試料のＸＲＤパターンは図１に示すとおりであり、Ｎａ１６Ｔｉ１０Ｏ２８が単一相で合成されたことが確認された。 First, Na 16 Ti 10 O 28 as a precursor was synthesized. Using Na 2 CO 3 (manufactured by Merck) and TiO 2 as raw materials, these raw materials were weighed at a molar ratio of Na 2 CO 3 : TiO 2 = 4: 5, wet-mixed with acetone, and 1000 ° C. for 1 hour. Was fired. The XRD pattern of the obtained sample is as shown in FIG. 1, and it was confirmed that Na 16 Ti 10 O 28 was synthesized in a single phase.
つぎに、上記で得た前駆体１ｇに対して１０Ｍの硝酸100mlを加えて１日撹拌し、濾過した。その後、７０〜９０℃で蒸発乾固させ、水洗を繰り返し行い、自然乾燥させた。 Next, 100 ml of 10M nitric acid was added to 1 g of the precursor obtained above, and the mixture was stirred for 1 day and filtered. Thereafter, it was evaporated to dryness at 70 to 90 ° C., washed repeatedly with water, and naturally dried.
蒸発乾固させた後のＸＲＤパターンを図２に示す。結晶性の単一相のルチル型酸化チタンが低温で合成されたことが確認された。 The XRD pattern after evaporating to dryness is shown in FIG. It was confirmed that crystalline single-phase rutile-type titanium oxide was synthesized at low temperature.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006249441A JP4581093B2 (en) | 2006-09-14 | 2006-09-14 | Production method of titanium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006249441A JP4581093B2 (en) | 2006-09-14 | 2006-09-14 | Production method of titanium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2008069039A JP2008069039A (en) | 2008-03-27 |
| JP4581093B2 true JP4581093B2 (en) | 2010-11-17 |
Family
ID=39290973
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006249441A Active JP4581093B2 (en) | 2006-09-14 | 2006-09-14 | Production method of titanium oxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4581093B2 (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02167822A (en) * | 1988-12-20 | 1990-06-28 | Otsuka Chem Co Ltd | Production of fibrous sodium titanate |
| JP2003112922A (en) * | 2001-10-03 | 2003-04-18 | Nippon Steel & Sumikin Welding Co Ltd | Method for producing sodium titanate |
| WO2005019348A1 (en) * | 2003-07-21 | 2005-03-03 | Merck Patent Gmbh | Silicon dioxide-coated nanoparticulate uv protectant |
-
2006
- 2006-09-14 JP JP2006249441A patent/JP4581093B2/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02167822A (en) * | 1988-12-20 | 1990-06-28 | Otsuka Chem Co Ltd | Production of fibrous sodium titanate |
| JP2003112922A (en) * | 2001-10-03 | 2003-04-18 | Nippon Steel & Sumikin Welding Co Ltd | Method for producing sodium titanate |
| WO2005019348A1 (en) * | 2003-07-21 | 2005-03-03 | Merck Patent Gmbh | Silicon dioxide-coated nanoparticulate uv protectant |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2008069039A (en) | 2008-03-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101456583B (en) | Synthetic method for preparing rutile type nano titanic oxide sol or powder at low temperature | |
| KR20000067090A (en) | manufacturing method of titanium dioxide powder for photocatalyst | |
| CN100391852C (en) | Method for preparing hano-level titanium dioxide by controlling crystal form | |
| BRPI0608611A2 (en) | sulphate process for the production of titania from a titanium material | |
| JP4436910B2 (en) | Photocatalyst containing titanium oxide, its production method and use | |
| US11203527B2 (en) | Acid recovery from acid-rich solutions | |
| CN102167400A (en) | Method for preparing vanadium pentoxide from vanadium-containing solution | |
| Grzmil et al. | Influence of Phosphate, Potassium, Lithium, and Aluminium on the Anatase− Rutile Phase Transformation | |
| BRPI0309330B1 (en) | process for the production of uncle 2 product from the liquid phase of the sulfuric acid leaching process of a pretreated titaniferous ore. | |
| BRPI0609680A2 (en) | sulphate process for the production of titania from a titanium material | |
| JP4581093B2 (en) | Production method of titanium oxide | |
| CN109399712A (en) | A method of with hydrogen peroxide clean manufacturing high purity vanadic anhydride | |
| CA2712116C (en) | The production of titanium trifluoride | |
| KR20140092483A (en) | Conversion method of crystal shape to control titanium dioxide | |
| KR100420275B1 (en) | Preparation of TiO2 fine powder from titanium tetrachloride with inorganic acid | |
| CN105056874B (en) | A kind of preparation method and its usage of eight potassium titanate crystal whiskers | |
| JP4565160B2 (en) | New titanium dioxide and method for producing the same | |
| CA2539830A1 (en) | Method for processing iron-laden spent sulfuric acid | |
| CN107774284B (en) | Preparation method of aqueous nano antibacterial photocatalytic titanium oxide composite sol | |
| CN101918318A (en) | A process for the production of titanium salts | |
| WO2005040436A1 (en) | Method for processing heavy metal chloride residues | |
| JP2008156158A (en) | Method for producing spherical peroxotitanium hydrate and spherical titanium oxide | |
| JP2006103999A (en) | Method of manufacturing titanium oxide fine particle | |
| CN1442368A (en) | Method of controlling nano titanium dioxide crystal form and obtained nano titanium dioxide using said method | |
| PL208989B1 (en) | Method for the manufacture of visible radiation active photo-catalyst used for discolouring coloured liquid wastes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20080331 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20100225 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20100301 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20100524 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20100706 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20100802 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |