JP3224298B2 - Method for producing acicular alkali titanate - Google Patents
Method for producing acicular alkali titanateInfo
- Publication number
- JP3224298B2 JP3224298B2 JP35704692A JP35704692A JP3224298B2 JP 3224298 B2 JP3224298 B2 JP 3224298B2 JP 35704692 A JP35704692 A JP 35704692A JP 35704692 A JP35704692 A JP 35704692A JP 3224298 B2 JP3224298 B2 JP 3224298B2
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- JP
- Japan
- Prior art keywords
- acicular
- alkali
- titanyl sulfate
- needle
- crystal particles
- 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.)
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- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、耐熱性、断熱性、化学
的安定性に優れ、プラスチツク、金属等の構造材料の補
強材あるいは摩擦材料等として有用な針状チタン酸アル
カリの製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing acicular alkali titanate which is excellent in heat resistance, heat insulation and chemical stability and is useful as a reinforcing material or a friction material for structural materials such as plastics and metals. .
【０００２】[0002]
【従来の技術】針状（繊維状）チタン酸アルカリは一般
式Ｍ2Ｏ・ｎＴiＯ2（Ｍはアルカリ金属、ｎは８以下の
正数）で示される人工物質であり、アルカリ金属に応じ
様々なｎの値をとるものが合成されている。その中でも
特にｎ＝６となる針状六チタン酸アルカリはその耐熱
性、断熱性、耐摩耗性、高強度、高弾性等からプラスチ
ツク、金属、セラミツクス等の補強材の他、耐火断熱
材、濾過材、摩擦材として広く用いられている材料であ
る。 2. Description of the Related Art Acicular (fibrous) alkali titanate is an artificial substance represented by the general formula M 2 O.nTiO 2 (M is an alkali metal and n is a positive number of 8 or less). Those that take the value of n are synthesized. Among them, the needle-shaped alkali hexatitanate having n = 6 is particularly preferable because of its heat resistance, heat insulation, abrasion resistance, high strength, high elasticity, etc., as well as reinforcing materials such as plastics, metals, ceramics, etc. It is a material widely used as a material and friction material.
【０００３】針状六チタン酸アルカリの製造方法は従来
から種々提案されており、焼成法、メルト法、水熱法、
フラツクス法等に分類できる。しかしながら、工業的に
有用な長繊維は水熱法によれば直接得られるものの、合
成条件が複雑で危険性も伴う上高価であり、他の方法で
は何れも初生相として二チタン酸アルカリあるいは四チ
タン酸アルカリを経由させる必要があり、必然的に焼成
が２回となるなど工程数が増え煩雑となりコスト的にも
不利である。[0003] Various methods for producing acicular alkali hexatitanate have been proposed in the past, including a firing method, a melt method, a hydrothermal method,
It can be classified into the flux method, etc. However, industrially useful long fibers can be obtained directly by the hydrothermal method, but the synthesis conditions are complicated, dangerous and expensive, and in any other method, alkali dititanate or quaternary is used as a primary phase. It is necessary to pass through an alkali titanate, and the number of steps is increased, such as inevitably two firings, which is complicated and disadvantageous in cost.
【０００４】[0004]
【発明が解決しようとする課題】本発明の目的は上記し
た技術の実情に鑑み、補強材あるいは摩擦材などとして
優れた針状六チタン酸アルカリを簡単な工程により経済
的に製造する全く新規な方法を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a completely novel needle-like alkali hexatitanate which is excellent as a reinforcing material or a friction material in a simple process economically in view of the above-mentioned technical situation. It is to provide a method.
【０００５】[0005]
【課題を解決するための手段】本発明は硫酸チタニルの
針状結晶粒子をアルカリ水溶液と接触させることにより
アルカリ金属イオン含有針状含水酸化チタンを生成し、
洗浄により可溶性塩類を除去した後、乾燥、焼成するこ
とを特徴とする針状チタン酸アルカリの製造方法に係
る。According to the present invention, acicular hydrous titanium oxide containing alkali metal ions is produced by contacting acicular crystal particles of titanyl sulfate with an aqueous alkali solution.
The present invention relates to a method for producing needle-like alkali titanate, which comprises removing soluble salts by washing, drying and baking.
【０００６】本発明者らは、先に硫酸チタニル水溶液を
加熱することにより晶出する硫酸チタニルの針状結晶粒
子をアルカリ水溶液と接触させることによる針状含水酸
化チタンの製造方法を出願（特願平３−２３３９０３
号）しているが、本発明はそれを応用展開した技術であ
る。[0006] The present inventors filed an application for a method for producing acicular titanium oxide hydroxide by bringing acicular crystal particles of titanyl sulfate crystallized by heating an aqueous solution of titanyl sulfate into contact with an alkaline aqueous solution. Hei 3-233903
No.), but the present invention is a technology developed by applying it.
【０００７】即ち、本発明は硫酸チタニルの針状結晶粒
子とアルカリ水溶液とを接触させる際のpＨを調整する
ことにより六チタン酸アルカリ組成比のアルカリ金属イ
オン含有針状含水酸化チタンを生成させ、洗浄により可
溶性塩類を除去した後、乾燥、焼成することを特徴とす
る針状六チタン酸アルカリの製造方法である。That is, according to the present invention, needle-like hydrous titanium oxide containing alkali metal ions having an alkali hexatitanate composition ratio is produced by adjusting the pH when the needle-like crystal particles of titanyl sulfate are brought into contact with an aqueous alkali solution. This is a method for producing acicular alkali hexatitanate, comprising removing soluble salts by washing, drying and calcining.
【０００８】本発明で用いる硫酸チタニルの針状結晶粒
子は、ＴiＯ2濃度が５〜270g／l、硫酸濃度が300g／l以
上、好ましくは300〜1400g／l、特に好ましくは500〜10
00g／lである硫酸チタニル水溶液を加熱することによつ
て得られる。この際、撹拌の有無は問わないが均一な粒
度を得ようとするならば施すほうが好ましい。The needle-like crystal particles of titanyl sulfate used in the present invention have a TiO 2 concentration of 5 to 270 g / l and a sulfuric acid concentration of 300 g / l or more, preferably 300 to 1400 g / l, particularly preferably 500 to 10 g / l.
It is obtained by heating an aqueous solution of titanyl sulfate of 00 g / l. At this time, it does not matter whether or not stirring is performed, but it is preferable to perform the stirring if a uniform particle size is to be obtained.
【０００９】ＴiＯ2濃度が５g／lより低くなると収量が
少なくかつＴiＯ2に対し多量の硫酸を必要とすることか
ら不経済であり、270g／lを超えると晶出する結晶濃度
が高くなり過ぎ、撹拌操作が困難となり結果として結晶
成長が不均一となつてしまう。If the concentration of TiO 2 is lower than 5 g / l, the yield is small and a large amount of sulfuric acid is required for TiO 2 , which is uneconomical. If the concentration exceeds 270 g / l, the concentration of crystals to be crystallized becomes too high. In addition, the stirring operation becomes difficult, and as a result, the crystal growth becomes uneven.
【００１０】硫酸濃度は300g／lより低くなると晶出速
度が著しく低下し、1400g／lを超えた場合も晶出率が低
下したり、生成する結晶粒子も針状から塊状になつてし
まう。When the sulfuric acid concentration is lower than 300 g / l, the crystallization rate is remarkably reduced. When the sulfuric acid concentration is higher than 1400 g / l, the crystallization rate is reduced, and the crystal grains to be formed are changed from needles to lumps.
【００１１】加熱温度は、ＴiＯ2濃度、硫酸濃度にもよ
るが、70℃以上が好ましい。70℃より低くなると反応速
度の低下を招く。また、反応は沸点以上、オートクレー
ブ中、水熱条件下でもかまわない。The heating temperature depends on the TiO 2 concentration and the sulfuric acid concentration, but is preferably 70 ° C. or higher. If the temperature is lower than 70 ° C., the reaction rate decreases. The reaction may be carried out at a temperature higher than the boiling point, in an autoclave, or under hydrothermal conditions.
【００１２】以上の条件によつて得られる硫酸チタニル
の結晶は短軸径0.1〜５μm、長軸径２〜500μmの針状粒
子であり、その粒度はＴiＯ2濃度、硫酸濃度及び加熱温
度により自由に調整できる。The crystals of titanyl sulfate obtained under the above conditions are acicular particles having a minor axis diameter of 0.1 to 5 μm and a major axis diameter of 2 to 500 μm, and the particle size can be freely determined depending on the TiO 2 concentration, sulfuric acid concentration and heating temperature. Can be adjusted.
【００１３】本発明においては上述した硫酸チタニルの
針状結晶粒子をアルカリ水溶液と接触させることにより
アルカリ金属イオン含有針状含水酸化チタンを生成させ
る。ここでいうアルカリ水溶液とは、アルカリ金属の化
合物で水酸化物、炭酸塩、リン酸塩等水溶液としてアル
カリ性を示すものの水溶液をいう。また、その際のpＨ
は7.0以上、好ましくは8.0〜13.0となるように調整す
る。pＨが7.0より低い場合には六チタン酸アルカリ組成
比に足るアルカリ金属イオンが吸着せず、13.0を超える
場合は逆に六チタン酸アルカリ組成比以上のアルカリ金
属イオンが吸着し、次の焼成工程で焼結を引き起こし、
針状形状が崩れてしまう。以上のような条件により六チ
タン酸アルカリ組成比のアルカリ金属イオン含有針状含
水酸化チタンが硫酸チタニルの針状結晶粒子の形骸を保
持したまま生成する。In the present invention, the acicular hydrous titanium oxide containing alkali metal ions is produced by bringing the acicular crystal particles of titanyl sulfate into contact with an aqueous alkali solution. The term “alkali aqueous solution” as used herein refers to an aqueous solution of an alkali metal compound which exhibits alkalinity as an aqueous solution such as a hydroxide, a carbonate, or a phosphate. The pH at that time
Is adjusted to be 7.0 or more, preferably 8.0 to 13.0. When the pH is lower than 7.0, the alkali metal ions sufficient for the alkali hexatitanate composition ratio are not adsorbed. When the pH is higher than 13.0, the alkali metal ions having the alkali hexatitanate composition ratio or higher are conversely adsorbed. Causes sintering,
Needle-like shape collapses. Under the above conditions, the alkali metal ion-containing acicular hydrous titanium oxide having an alkali hexatitanate composition ratio is generated while maintaining the shape of acicular crystal particles of titanyl sulfate.
【００１４】このようにして得られたアルカリ金属イオ
ン含有針状含水酸化チタンは洗浄により可溶性塩類を除
去した後、乾燥、焼成することにより針状六チタン酸ア
ルカリに形骸を保持したまま変換する。この時の焼成温
度は600〜1000℃、好ましくは700〜900℃である。[0014] The alkali metal ion-containing needle-like hydrous titanium oxide thus obtained is subjected to washing to remove soluble salts, and then dried and calcined to be converted into acicular alkali hexatitanate while retaining its form. The firing temperature at this time is 600 to 1000 ° C, preferably 700 to 900 ° C.
【００１５】[0015]
【実施例】以下に本発明の実施例を挙げて説明するが、
本発明はこれに限定されるものではない。The present invention will be described below with reference to examples of the present invention.
The present invention is not limited to this.
【００１６】実施例１ 硫酸法による酸化チタン製造工程から得られる含水酸化
チタンを出発原料とし、該含水酸化チタンに含まれるＴ
iＯ2に対し、2.8倍の濃硫酸を加えて加熱、撹拌して溶
解した。該溶液に水及び硫酸を加えてＴiＯ2濃度14g／
l、硫酸濃度700g／lとし、100〜120℃の温度にて加熱、
撹拌したところ、短軸径0.1〜２μm、長軸径10〜40μm
の硫酸チタニルの針状結晶粒子が晶出した。該針状結晶
粒子を水酸化ナトリウム水溶液と接触させ、pＨが一定
になるまで放置した。このときのpＨは9.5であつた。そ
の後、水で洗浄し250℃にて乾燥したもののＴiＯ2／Ｎa
2Ｏ（モル比）を化学分析にて求めたところ5.81であつ
た。該乾燥品をさらに800℃にて３時間焼成し、Ｘ線回
折にて同定したところ六チタン酸ナトリウムの単一相と
なつていた。この間、結晶粒子は硫酸チタニルの結晶晶
出時の形骸を殆ど保持していた。得られた針状六チタン
酸ナトリウムの電子顕微鏡写真を図１に示した。Example 1 A hydrous titanium oxide obtained from a titanium oxide production process by a sulfuric acid method was used as a starting material, and T contained in the hydrous titanium oxide was used.
to iO 2, heated by adding 2.8 times of concentrated sulfuric acid and stirred to dissolve. Water and sulfuric acid were added to the solution to obtain a TiO 2 concentration of 14 g /
l, sulfuric acid concentration 700 g / l, heated at a temperature of 100 ~ 120 ℃,
When stirred, short axis diameter 0.1-2μm, long axis diameter 10-40μm
Needle crystal particles of titanyl sulfate crystallized out. The needle-like crystal particles were brought into contact with an aqueous solution of sodium hydroxide and allowed to stand until the pH became constant. The pH at this time was 9.5. After that, it was washed with water and dried at 250 ° C., but TiO 2 / Na
2 O (molar ratio) was 5.81 as determined by chemical analysis. The dried product was further calcined at 800 ° C. for 3 hours, and identified by X-ray diffraction to be a single phase of sodium hexatitanate. During this time, the crystal particles almost retained the form of the titanyl sulfate at the time of crystallization. An electron micrograph of the obtained needle-like sodium hexatitanate is shown in FIG.
【００１７】実施例２ 実施例１と同様にして得られた硫酸チタニルの針状結晶
粒子を水酸化カリウム水溶液と接触させ、pＨが一定に
なるまで放置した。このときのpＨは9.4であつた。その
後、水で洗浄し250℃にて乾燥したもののＴiＯ2／Ｋ2Ｏ
（モル比）を化学分析にて求めたところ6.28であつた。
該乾燥品をさらに800℃にて３時間焼成し、Ｘ線回折に
て同定したところ六チタン酸カリウムの単一相となつて
いた。この間、結晶粒子は硫酸チタニルの結晶晶出時の
形骸を殆ど保持していた。得られた針状六チタン酸カリ
ウムの電子顕微鏡写真を図２に示した。Example 2 Needle-like crystal particles of titanyl sulfate obtained in the same manner as in Example 1 were brought into contact with an aqueous solution of potassium hydroxide and allowed to stand until the pH became constant. The pH at this time was 9.4. After that, it was washed with water and dried at 250 ° C., but TiO 2 / K 2 O
(Molar ratio) determined by chemical analysis was 6.28.
The dried product was further calcined at 800 ° C. for 3 hours and identified by X-ray diffraction to be a single phase of potassium hexatitanate. During this time, the crystal particles almost retained the form of the crystal of titanyl sulfate at the time of crystallization. An electron micrograph of the obtained acicular potassium hexatitanate is shown in FIG.
【００１８】実施例３ 実施例１と同様にして得られた硫酸チタニルの針状結晶
粒子を炭酸カリウム水溶液と接触させ、pＨが一定にな
るまで放置した。このときのpＨは10.2であつた。その
後、水で洗浄し250℃にて乾燥したもののＴiＯ2／Ｋ2Ｏ
（モル比）を化学分析にて求めたところ5.79であつた。
該乾燥品をさらに800℃にて３時間焼成し、Ｘ線回折に
て同定したところ六チタン酸カリウムの単一相となつて
いた。この間、結晶粒子は実施例２と同様、硫酸チタニ
ルの結晶晶出時の形骸を殆ど保持していた。Example 3 The needle-like crystal particles of titanyl sulfate obtained in the same manner as in Example 1 were brought into contact with an aqueous solution of potassium carbonate and allowed to stand until the pH became constant. The pH at this time was 10.2. After that, it was washed with water and dried at 250 ° C., but TiO 2 / K 2 O
(Molar ratio) determined by chemical analysis was 5.79.
The dried product was further calcined at 800 ° C. for 3 hours and identified by X-ray diffraction to be a single phase of potassium hexatitanate. During this period, the crystal grains almost retained the form of the crystal of titanyl sulfate at the time of crystallization, as in Example 2.
【００１９】実施例４ 硫酸法による酸化チタン製造工程から得られる含水酸化
チタンを出発原料とし、該含水酸化チタンに含まれるＴ
iＯ2に対し、2.8倍の濃硫酸を加えて加熱、撹拌して溶
解した。該溶液に水及び硫酸を加えてＴiＯ2濃度200g／
l、硫酸濃度1000g／lとし、70〜90℃の温度にて加熱、
撹拌したところ、短軸径１〜３μm、長軸径３〜12μmの
硫酸チタニルの針状結晶粒子が晶出した。該針状結晶粒
子を水酸化カリウム水溶液と接触させ、pＨが一定にな
るまで放置した。このときのpＨは12.5であつた。その
後、水で洗浄し250℃にて乾燥したもののＴiＯ2／Ｋ2Ｏ
（モル比）を化学分析にて求めたところ6.31であつた。
該乾燥品をさらに650℃にて３時間焼成し、Ｘ線回折に
て同定したところ六チタン酸カリウムの単一相となつて
いた。この間、結晶粒子は硫酸チタニルの結晶晶出時の
形骸を殆ど保持していた。得られた針状六チタン酸カリ
ウムの電子顕微鏡写真を図３に示した。Example 4 Titanium hydroxide obtained from the titanium oxide production process by the sulfuric acid method was used as a starting material, and T contained in the titanium oxide was used.
to iO 2, heated by adding 2.8 times of concentrated sulfuric acid and stirred to dissolve. Water and sulfuric acid were added to the solution to obtain a TiO 2 concentration of 200 g /
l, sulfuric acid concentration 1000g / l, heating at 70-90 ° C,
Upon stirring, needle-like crystal particles of titanyl sulfate having a short axis diameter of 1 to 3 μm and a long axis diameter of 3 to 12 μm were crystallized. The needle-shaped crystal particles were brought into contact with an aqueous solution of potassium hydroxide and allowed to stand until the pH became constant. The pH at this time was 12.5. After that, it was washed with water and dried at 250 ° C., but TiO 2 / K 2 O
(Molar ratio) determined by chemical analysis was 6.31.
The dried product was further calcined at 650 ° C. for 3 hours and identified as a single phase of potassium hexatitanate by X-ray diffraction. During this time, the crystal particles almost retained the form of the crystal of titanyl sulfate at the time of crystallization. An electron micrograph of the obtained acicular potassium hexatitanate is shown in FIG.
【００２０】実施例５ 硫酸法による酸化チタン製造工程から得られる含水酸化
チタンを出発原料とし、該含水酸化チタンに含まれるＴ
iＯ2に対し、2.8倍の濃硫酸を加えて加熱、撹拌して溶
解した。該溶液に水及び硫酸を加えてＴiＯ2濃度120g／
l、硫酸濃度400g／lとし、100〜120℃の温度にて加熱、
撹拌したところ、短軸径0.5〜２μm、長軸径５〜20μm
の硫酸チタニルの針状結晶粒子が晶出した。該針状結晶
粒子を炭酸カリウム水溶液と接触させ、pＨが一定にな
るまで放置した。このときのpＨは8.1であつた。その
後、水で洗浄し250℃にて乾燥したもののＴiＯ2／Ｋ2Ｏ
（モル比）を化学分析にて求めたところ5.75であつた。
該乾燥品をさらに950℃にて３時間焼成し、Ｘ線回折に
て同定したところ六チタン酸カリウムの単一相となつて
いた。この間、結晶粒子は硫酸チタニルの結晶晶出時の
形骸を殆ど保持していた。得られた針状六チタン酸カリ
ウムの電子顕微鏡写真を図４に示した。Example 5 Titanium oxide hydroxide obtained from a titanium oxide production step by a sulfuric acid method was used as a starting material, and T contained in the titanium oxide hydroxide was used.
to iO 2, heated by adding 2.8 times of concentrated sulfuric acid and stirred to dissolve. Water and sulfuric acid were added to the solution to obtain a TiO 2 concentration of 120 g /
l, sulfuric acid concentration 400 g / l, heated at a temperature of 100 ~ 120 ℃,
After stirring, short axis diameter 0.5-2μm, long axis diameter 5-20μm
Needle crystal particles of titanyl sulfate crystallized out. The needle-shaped crystal particles were brought into contact with an aqueous solution of potassium carbonate and allowed to stand until the pH became constant. The pH at this time was 8.1. After that, it was washed with water and dried at 250 ° C., but TiO 2 / K 2 O
(Molar ratio) determined by chemical analysis was 5.75.
The dried product was further calcined at 950 ° C. for 3 hours and identified as a single phase of potassium hexatitanate by X-ray diffraction. During this time, the crystal particles almost retained the form of the titanyl sulfate at the time of crystallization. An electron micrograph of the obtained acicular potassium hexatitanate is shown in FIG.
【００２１】比較例１ 実施例１と同様にして得られた硫酸チタニルの針状結晶
粒子を水酸化ナトリウム水溶液と接触させ、pＨが一定
になるまで放置した。このときのpＨは5.0であつた。そ
の後、水で洗浄し250℃にて乾燥したもののＴiＯ2／Ｎa
2Ｏ（モル比）を化学分析にて求めたところ24.61であつ
た。該乾燥品をさらに800℃にて３時間焼成し、Ｘ線回
折にて同定したところ酸化チタン（ルチル形）の単一相
となつていた。Comparative Example 1 The needle-like crystal particles of titanyl sulfate obtained in the same manner as in Example 1 were brought into contact with an aqueous solution of sodium hydroxide and allowed to stand until the pH became constant. The pH at this time was 5.0. After that, it was washed with water and dried at 250 ° C., but TiO 2 / Na
2 O (molar ratio) was determined by chemical analysis to be 24.61. The dried product was further calcined at 800 ° C. for 3 hours, and identified by X-ray diffraction to be a single phase of titanium oxide (rutile type).
【００２２】比較例２ 実施例１と同様にして得られた硫酸チタニルの針状結晶
粒子を水酸化ナトリウム水溶液と接触させ、pＨが一定
になるまで放置した。このときのpＨは13.8であつた。
その後、水で洗浄し250℃にて乾燥したもののＴiＯ2／
Ｎa2Ｏ（モル比）を化学分析にて求めたところ4.41であ
つた。該乾燥品をさらに800℃にて３時間焼成し、Ｘ線
回折にて同定したところ六チタン酸ナトリウムの単一相
となつていたが、その形状は一部は粉状化し、また折れ
たものがほとんどであつた。Comparative Example 2 The needle-like crystal particles of titanyl sulfate obtained in the same manner as in Example 1 were brought into contact with an aqueous solution of sodium hydroxide and allowed to stand until the pH became constant. The pH at this time was 13.8.
Thereafter, TiO though and dried washed with water 250 ° C. 2 /
When Na 2 O (molar ratio) was determined by chemical analysis, it was 4.41. The dried product was further baked at 800 ° C. for 3 hours, and identified by X-ray diffraction. As a result, it was found to be a single phase of sodium hexatitanate. Was the most.
【００２３】[0023]
【発明の効果】本発明によれば、硫酸チタニルの針状結
晶粒子をアルカリ水溶液と接触させ、アルカリ金属イオ
ン含有針状含水酸化チタンを生成し、その後焼成すると
いう極めて簡単な工程により針状六チタン酸アルカリを
製造できる。また本発明では硫酸チタニルの針状結晶粒
子とアルカリ水溶液との接触により針状含水酸化チタン
が生成した際に六チタン酸アルカリ組成比に相当するア
ルカリ金属イオンを吸着するため、次の焼成段階でのチ
タン酸塩への反応が均一かつ速やかに進み、焼成温度も
1000℃以下に押さえることができる。According to the present invention, acicular crystal particles of titanyl sulfate are brought into contact with an aqueous alkali solution to produce acicular hydrous titanium oxide containing alkali metal ions, and then calcined. Can produce alkali titanate. Further, in the present invention, when needle-like hydrous titanium oxide is generated by contact of needle-like crystal particles of titanyl sulfate with an aqueous alkali solution, an alkali metal ion corresponding to an alkali hexatitanate composition ratio is adsorbed. The reaction to the titanate proceeds uniformly and quickly, and the firing temperature
It can be kept below 1000 ° C.
【図１】本発明の実施例１により得られた針状六チタン
酸ナトリウムの粒子構造を示す電子顕微鏡写真である。FIG. 1 is an electron micrograph showing the particle structure of acicular sodium hexatitanate obtained according to Example 1 of the present invention.
【図２】本発明の実施例２により得られた針状六チタン
酸カリウムの粒子構造を示す電子顕微鏡写真である。FIG. 2 is an electron micrograph showing the particle structure of acicular potassium hexatitanate obtained according to Example 2 of the present invention.
【図３】本発明の実施例４により得られた針状六チタン
酸カリウムの粒子構造を示す電子顕微鏡写真である。FIG. 3 is an electron micrograph showing the particle structure of acicular potassium hexatitanate obtained according to Example 4 of the present invention.
【図４】本発明の実施例５により得られた針状六チタン
酸カリウムの粒子構造を示す電子顕微鏡写真である。FIG. 4 is an electron micrograph showing the particle structure of acicular potassium hexatitanate obtained according to Example 5 of the present invention.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平５−139747（ＪＰ，Ａ) 特開 平５−155697（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C30B 1/00 - 35/00 C01G 23/00 ＣＡ（ＳＴＮ) ＪＩＣＳＴファイル（ＪＯＩＳ) ＷＰＩ（ＤＩＡＬＯＧ)────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-5-139747 (JP, A) JP-A-5-155697 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C30B 1/00-35/00 C01G 23/00 CA (STN) JICST file (JOIS) WPI (DIALOG)
Claims (2)
水溶液と接触させることによりアルカリ金属イオン含有
針状含水酸化チタンを生成し、洗浄により可溶性塩類を
除去した後、乾燥、焼成することを特徴とする針状チタ
ン酸アルカリの製造方法。1. An acicular titanium oxide hydroxide containing alkali metal ions is produced by contacting acicular crystal particles of titanyl sulfate with an aqueous alkali solution, and after removing soluble salts by washing, drying and calcining. For producing acicular alkali titanate.
00g／l以上である硫酸チタニル水溶液を加熱することに
より晶出する硫酸チタニルの針状結晶粒子を用いる請求
項１の針状チタン酸アルカリの製造方法。2. A TiO 2 concentration of 5 to 270 g / l and a sulfuric acid concentration of 3
2. The method for producing needle-like alkali titanate according to claim 1, wherein needle-like crystal particles of titanyl sulfate crystallized by heating an aqueous solution of titanyl sulfate of not less than 00 g / l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35704692A JP3224298B2 (en) | 1992-12-21 | 1992-12-21 | Method for producing acicular alkali titanate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35704692A JP3224298B2 (en) | 1992-12-21 | 1992-12-21 | Method for producing acicular alkali titanate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06183898A JPH06183898A (en) | 1994-07-05 |
| JP3224298B2 true JP3224298B2 (en) | 2001-10-29 |
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| Application Number | Title | Priority Date | Filing Date |
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