JP2000313620A - Production of granular potassium octatitanate - Google Patents
Production of granular potassium octatitanateInfo
- Publication number
- JP2000313620A JP2000313620A JP11122750A JP12275099A JP2000313620A JP 2000313620 A JP2000313620 A JP 2000313620A JP 11122750 A JP11122750 A JP 11122750A JP 12275099 A JP12275099 A JP 12275099A JP 2000313620 A JP2000313620 A JP 2000313620A
- Authority
- JP
- Japan
- Prior art keywords
- potassium
- granular
- titanate
- dititanate
- firing
- 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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Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Braking Arrangements (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、粒状８チタン酸カ
リウム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 granular potassium octitanate.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】８チタ
ン酸カリウムは、通常、微細な繊維状単結晶として工業
的に生産されており、樹脂強化剤、触媒担体、ブレーキ
用摩擦剤等として広く用いられている。BACKGROUND OF THE INVENTION Potassium 8-titanate is usually industrially produced as a fine fibrous single crystal and widely used as a resin reinforcing agent, a catalyst carrier, a friction agent for brakes, and the like. Used.
【０００３】これらの用途のうち例えばブレーキ用摩擦
剤用途は、耐熱性に優れ、フェード現象の防止や摩擦特
性の熱安定性向上に有効であるというチタン酸カリウム
の有する優れた特徴を活かした用途であるが、該用途に
おいてはチタン酸カリウムが繊維状であることは、必要
とされないか、むしろ好ましくない特性とされていた。[0003] Among these uses, for example, the use of friction agents for brakes is a use of the excellent characteristics of potassium titanate, which is excellent in heat resistance, is effective in preventing a fade phenomenon and improving thermal stability of friction characteristics. However, in this application, the fact that the potassium titanate is in a fibrous state has not been required or has been regarded as an undesirable property.
【０００４】すなわち、チタン酸カリウム繊維は繊維形
状を有しているため嵩高く、流動性に劣り、製造時にお
いて供給路の壁に付着して、これを閉塞させるといった
問題点を有している。また、繊維状であるため粉塵を発
生し易く、作業環境を悪化させるという問題点を有して
いる。That is, the potassium titanate fiber has a problem that it is bulky and inferior in flowability due to its fiber shape, adheres to the wall of the supply passage during production, and blocks it. . In addition, since it is fibrous, there is a problem that dust is easily generated and the working environment is deteriorated.
【０００５】さらに、一般にブレーキ等の摩擦材のマト
リックスとしては、フェノール樹脂等の熱硬化性樹脂が
用いられているが、繊維状のチタン酸カリウムを配合し
た場合、製造工程中で繊維が破損するとその破損断面か
らカリウムイオンが溶出し、樹脂粘度やその硬化特性を
変化させ、物性にばらつきを生じる原因となるという問
題点を有していた。Further, a thermosetting resin such as a phenol resin is generally used as a matrix of a friction material such as a brake. However, when fibrous potassium titanate is blended, the fiber may be damaged during the manufacturing process. Potassium ions are eluted from the damaged cross section, changing the resin viscosity and its curing characteristics, and causing a variation in physical properties.
【０００６】かかる問題点を背景に、近年、粒状のチタ
ン酸カリウムが要望されるようになっているが、チタン
酸カリウムの中でもブレーキ用摩擦材として特に好まし
い８チタン酸カリウムは、その結晶特性から製造の過程
で繊維状に結晶成長し易いという性質を有しており、か
かる性質のため、これまで粒状単結晶を製造することは
困難とされていた。[0006] In view of such a problem, granular potassium titanate has recently been demanded. Among potassium titanates, potassium octa titanate, which is particularly preferable as a friction material for brakes, is used because of its crystal characteristics. It has the property that crystals grow easily in the form of fibers during the production process, and it has been difficult to produce granular single crystals until now because of such properties.
【０００７】一方、８チタン酸カリウムの製造方法とし
て、カリウム源、チタン源から２チタン酸カリウムを合
成し、４チタン酸カリウム、８チタン酸カリウムと順次
組成転換して合成する方法は知られている（例えば、特
公平４−７３２１８号公報等）。しかしながら、この方
法を応用して粒状の８チタン酸カリウムを製造する方法
はこれまで知られていない。On the other hand, as a method for producing potassium octitanate, there has been known a method of synthesizing potassium dititanate from a potassium source and a titanium source, and then sequentially performing compositional conversion to potassium tetratitanate and potassium octitanate. (For example, Japanese Patent Publication No. 4-73218). However, there is no known method for producing granular potassium octa titanate by applying this method.
【０００８】本発明の目的は、このような粒状８チタン
酸カリウムの製造方法を提供することにある。It is an object of the present invention to provide a method for producing such granular potassium octitanate.
【０００９】[0009]
【課題を解決するための手段】本発明者等は、粒状８チ
タン酸カリウムの製造方法を見出すべく鋭意検討した結
果、比較的粒状物として得られることが容易な２チタン
酸カリウムをまず粒状物として合成し、このものを組成
変換することにより粒状の８チタン酸カリウムを製造す
る方法を見出した。Means for Solving the Problems The inventors of the present invention have conducted intensive studies to find a method for producing granular potassium octa titanate. As a result, potassium dititanate, which is relatively easy to obtain as a granular substance, is first converted to a granular substance. The present inventors have found a method for producing granular potassium octa titanate by subjecting the composition to composition conversion.
【００１０】すなわち、本発明は、加熱により酸化チタ
ンとなるチタン化合物及び加熱により酸化カリウムとな
るカリウム化合物を酸化物換算モル比でＴｉＯ2 ／Ｋ2
Ｏ＝０．８５〜２．０の割合で混合し７００〜９４０℃
で焼成して２チタン酸カリウムを得る第一の工程、第一
の工程で得られた２チタン酸カリウムを水処理した後、
６５０〜９４０℃で焼成する第二の工程、第二の工程で
得られた焼成物を水分散させ分散液のｐＨが６〜８とな
るように酸を加えて中和した後、２００〜８００℃で焼
成する第三の工程とを備えることを特徴とする粒状８チ
タン酸カリウムの製造方法である。That is, according to the present invention, a titanium compound which becomes titanium oxide by heating and a potassium compound which becomes potassium oxide by heating are expressed as TiO 2 / K 2 in terms of oxide equivalent molar ratio.
O = 0.85-2.0 mixed at 700-940 ° C
In the first step of obtaining potassium dititanate by baking in, the potassium dititanate obtained in the first step is treated with water,
The second step of firing at 650 to 940 ° C., and the fired product obtained in the second step is dispersed in water to neutralize the dispersion by adding an acid so that the pH of the dispersion is 6 to 8; And a third step of baking at ℃.
【００１１】[0011]
【発明の実施の形態】本発明の第一の工程において、原
料として用いる加熱により酸化チタンとなるチタン化合
物としては、例えば、アナターゼサンド、ルチルサン
ド、チタンスラグ、ブルッカイト、合成ルチル、合成ア
ナターゼ、合成単斜晶系酸化チタン等、結晶系及び性状
を問わず任意のものを使用できる。BEST MODE FOR CARRYING OUT THE INVENTION In the first step of the present invention, examples of the titanium compound used as a raw material, which becomes titanium oxide by heating, include anatase sand, rutile sand, titanium slag, brookite, synthetic rutile, synthetic anatase, synthetic anatase, and the like. Any material such as monoclinic titanium oxide can be used irrespective of crystal system and properties.
【００１２】また、加熱により酸化カリウムとなるカリ
ウム化合物としては、炭酸カリウム、水酸化カリウム、
硝酸カリウム等を例示でき、特に炭酸カリウムが好まし
い。カリウム化合物とチタン化合物の混合割合は、酸化
物換算モル比でＴｉＯ2 ／Ｋ2 Ｏ＝０．８５〜２．０の
割合とするのが好ましく、より好ましくは１．３〜１．
９５とするのがよい。混合割合を示すモル比が０．８５
未満となると、収率が低下するため好ましくない。また
２．０を超えると、４チタン酸カリウム等の組成が混在
し、最終的に繊維状になりやすいため好ましくない。The potassium compound which becomes potassium oxide upon heating includes potassium carbonate, potassium hydroxide,
Examples thereof include potassium nitrate, and potassium carbonate is particularly preferred. The mixing ratio of the potassium compound and the titanium compound is preferably TiO 2 / K 2 O = 0.85 to 2.0 in terms of the molar ratio in terms of oxide, and more preferably 1.3 to 1.
It is good to be 95. The molar ratio indicating the mixing ratio is 0.85
If it is less than this, the yield is undesirably reduced. On the other hand, if it exceeds 2.0, a composition such as potassium tetratitanate is mixed, and it is liable to eventually become fibrous.
【００１３】チタン化合物とカリウム化合物の混合は、
任意の方法により行うことができ、例えば各種のミキサ
ー、タンブラー、ブレンダー等の混合装置を用いて混合
する方法を例示できる。また、湿式混合した後、スプレ
ードライ法により混合物を造粒する方法等を採用するこ
ともできる。The mixing of the titanium compound and the potassium compound is as follows:
It can be performed by any method, for example, a method of mixing using a mixer such as various mixers, tumblers, blenders and the like. Further, a method of granulating the mixture by a spray drying method after the wet mixing may be employed.
【００１４】第一の工程では、混合原料に塩化カリウム
をフラックスとして添加してもよく、該フラックスの添
加により、最終組成中の繊維生成を抑制することができ
る。塩化カリウムの配合量としては、チタン化合物とカ
リウム化合物の合計量１００重量部に対して１重量部以
上を例示でき、上限は特に制限はないが、多量に配合し
ても効果に差はないので、経済的観点からは通常１〜１
００重量部とするのが好ましく、より好ましくは１〜１
５重量部とするのがよい。In the first step, potassium chloride may be added as a flux to the mixed raw material, and the addition of the flux can suppress the generation of fibers in the final composition. The amount of potassium chloride may be, for example, 1 part by weight or more based on 100 parts by weight of the total amount of the titanium compound and the potassium compound, and the upper limit is not particularly limited. , Usually from economical point of view
00 parts by weight, more preferably 1-1.
It is preferable to use 5 parts by weight.
【００１５】第一の工程における焼成は、焼成温度７０
０〜９４０℃、好ましくは８３０〜９３０℃で行い、通
常３０分〜２４時間行う。焼成温度が９４０℃を超える
と２チタン酸カリウムが繊維状に結晶成長した状態とな
り、ひいては最終目的物たる８チタン酸カリウムが繊維
状となってしまうため好ましくない。The firing in the first step is performed at a firing temperature of 70.
The reaction is carried out at 0 to 940 ° C, preferably 830 to 930 ° C, usually for 30 minutes to 24 hours. If the sintering temperature exceeds 940 ° C., potassium dititanate is in a state of crystal growth in a fibrous form, and eventually, potassium octa titanate, which is the final target, becomes fibrous, which is not preferable.
【００１６】焼成は、電気炉、ロータリーキルン、ロー
タリングキルン、管状炉、流動焼成炉、トンネルキルン
等各種の焼成手段により行うことができる。焼成手段と
してトンネルキルンや電気炉を用いる場合、粒状２チタ
ン酸カリウムは凝集体として得られるので、これを粗
砕、解砕して第二の工程に供するのがよい。The firing can be performed by various firing means such as an electric furnace, a rotary kiln, a rotary kiln, a tubular furnace, a fluidized kiln, and a tunnel kiln. When a tunnel kiln or an electric furnace is used as the firing means, granular potassium dititanate is obtained as an agglomerate, which is preferably crushed and pulverized before the second step.
【００１７】第二の工程においては、第一の工程で得ら
れた粒状２チタン酸カリウムを水処理してカリウムイオ
ンを溶出させる。ここで水処理の方法としては、粒状２
チタン酸カリウムを水中に添加しスラリーとして撹拌す
る方法を例示できる。水処理に際して低濃度の酸（第三
の工程で使用する酸等）を添加してカリウム溶出を促進
させることもできるが、組成調整がやや困難となるた
め、通常は水を使用するのがよい。スラリー濃度として
は、例えば１〜３０重量％、好ましくは３〜１０重量％
が例示でき、処理時間としては１５分〜２４時間、通常
１〜５時間程度を例示できる。処理時間が短すぎると効
率よく４チタン酸カリウムが得られないため好ましくな
いが、水処理により溶出可能なカリウム量は限られてい
るため、処理時間を長くとるのは差し支えない。In the second step, the granular potassium dititanate obtained in the first step is treated with water to elute potassium ions. Here, as a method of water treatment, granular 2
A method in which potassium titanate is added to water and stirred as a slurry can be exemplified. In the water treatment, a low-concentration acid (such as the acid used in the third step) can be added to promote the elution of potassium, but it is slightly difficult to adjust the composition, so that it is usually preferable to use water. . The slurry concentration is, for example, 1 to 30% by weight, preferably 3 to 10% by weight.
And the processing time is, for example, about 15 minutes to 24 hours, usually about 1 to 5 hours. If the treatment time is too short, potassium tetratitanate cannot be efficiently obtained, which is not preferable. However, since the amount of potassium that can be eluted by the water treatment is limited, a longer treatment time may be used.
【００１８】第二の工程における焼成は、６５０〜９４
０℃、好ましくは７７０〜９３０℃で行うのがよい。焼
成温度が９４０℃を上回ると繊維成長が生じるため好ま
しくない。また焼成温度が６５０℃を下回ると、４チタ
ン酸カリウムへの組成変換が十分に起こらないため好ま
しくない。なお、焼成温度が７７０℃を下回ると、焼成
後も２チタン酸カリウムが組成中に残存することがある
が、このものを第三の工程に供しても最終的に目的の粒
状８チタン酸カリウムを得ることができるため、差し支
えない。The firing in the second step is performed at 650 to 94
It is good to carry out at 0 ° C., preferably at 770-930 ° C. If the firing temperature exceeds 940 ° C., fiber growth occurs, which is not preferable. On the other hand, if the firing temperature is lower than 650 ° C., the composition conversion into potassium tetratitanate does not sufficiently occur, which is not preferable. If the firing temperature is lower than 770 ° C., potassium dititanate may remain in the composition even after firing. However, even if this is subjected to the third step, the target granular potassium octa titanate is finally obtained. Can be obtained.
【００１９】第二の工程における焼成時間及び焼成手段
は、第一の焼成工程に準じて行うことができる。第二の
工程により粒状４チタン酸カリウムまたは粒状４チタン
酸カリウムと粒状２チタン酸カリウムの混合物を得るこ
とができ、このものは、焼成手段によっては凝集物とし
て得られるので必要に応じて粗砕、解砕して第三の工程
に供することができる。The firing time and firing means in the second step can be performed according to the first firing step. In the second step, granular potassium tetratitanate or a mixture of granular potassium tetratitanate and granular potassium dititanate can be obtained, which can be obtained as an agglomerate depending on the sintering means. Can be crushed and provided to the third step.
【００２０】第三の工程においては、まず第二の工程で
得られた粒状４チタン酸カリウムまたは粒状４チタン酸
カリウムと粒状２チタン酸カリウムの混合物を酸処理し
て、さらにカリウムイオンを溶出させる。In the third step, first, the granular potassium tetratitanate or a mixture of the granular potassium tetratitanate and the granular potassium dititanate obtained in the second step is subjected to an acid treatment to further elute potassium ions. .
【００２１】該酸処理は、まず第二の工程で得られた粒
状４チタン酸カリウムまたは粒状４チタン酸カリウムと
粒状２チタン酸カリウムの混合物を１〜３０重量％、好
ましくは３〜１０重量％のスラリーとした後、該スラリ
ーのｐＨが６〜８、好ましくは６．５〜７．５になるよ
う、適宜酸を添加して中和しながら撹拌することにより
行われる。ここで用いられる酸としては特に制限はな
く、塩酸、硫酸、硝酸等の鉱酸、酢酸等を例示できる。
酸処理は通常３０分〜５時間程度で完了する。酸処理
後、２００〜８００℃、好ましくは５００〜７００℃で
焼成し、必要に応じて粗砕、解砕、分級して粒状８チタ
ン酸カリウムを得ることができる。In the acid treatment, first, the granular potassium tetratitanate or a mixture of the granular potassium tetratitanate and the granular potassium dititanate obtained in the second step is 1 to 30% by weight, preferably 3 to 10% by weight. After the slurry is prepared, the slurry is stirred while neutralizing by adding an appropriate acid so that the pH of the slurry becomes 6 to 8, preferably 6.5 to 7.5. The acid used here is not particularly limited, and examples thereof include mineral acids such as hydrochloric acid, sulfuric acid, and nitric acid, and acetic acid.
The acid treatment is usually completed in about 30 minutes to 5 hours. After the acid treatment, the mixture is calcined at 200 to 800 ° C., preferably 500 to 700 ° C., and if necessary, crushed, crushed, and classified to obtain granular potassium octitanate.
【００２２】本発明により得られる粒状８チタン酸カリ
ウムとしては、平均長径１０〜２００μｍ、平均短径５
〜１５０μｍ、平均アスペクト比５未満、好ましくは３
未満のものが例示される。このような粒状８チタン酸カ
リウムの形状は、走査型電子顕微鏡（ＳＥＭ）により観
察し測定することができる。通常、５００個程度を測定
しその平均値として算出する。また、本発明によれば単
結晶の粒状８チタン酸カリウムを得ることができる。The granular potassium octitanate obtained by the present invention has an average major axis of 10 to 200 μm and an average minor axis of 5 μm.
１５０150 μm, average aspect ratio less than 5, preferably 3
Less than are exemplified. The shape of such granular potassium octa titanate can be observed and measured with a scanning electron microscope (SEM). Usually, about 500 pieces are measured and calculated as an average value. Further, according to the present invention, single-crystal granular potassium octitanate can be obtained.
【００２３】また、本発明により得られる粒状８チタン
酸カリウムのメジアン径としては、３０〜１００μｍが
例示される。このようなメジアン径は、レーザー回折式
粒度分布測定装置等により測定することができる。本発
明によれば、従来製造の困難だった粒状８チタン酸カリ
ウムが提供され、このものはブレーキ用摩擦剤を始め、
各種の用途に好適に使用できる。The median diameter of the granular potassium octitanate obtained by the present invention is, for example, 30 to 100 μm. Such a median diameter can be measured by a laser diffraction type particle size distribution measuring device or the like. According to the present invention, there is provided granular potassium 8-titanate which has been conventionally difficult to manufacture, including a friction agent for brakes,
It can be suitably used for various applications.
【００２４】[0024]
【実施例】以下に実施例及び比較例を挙げ、本発明をさ
らに詳細に説明する。 （実施例１）酸化チタン１０ｇと炭酸カリウム９ｇ（Ｔ
ｉＯ2 ／Ｋ2 Ｏ＝１．９２）及び塩化カリウム１ｇを乳
鉢にてよく混合し、マッフル炉中、９００℃にて４時間
焼成した。生成物は解砕してＳＥＭ観察、Ｘ線回折した
結果、粒状２チタン酸カリウムであった。The present invention will be described in more detail with reference to the following Examples and Comparative Examples. (Example 1) 10 g of titanium oxide and 9 g of potassium carbonate (T
(iO 2 / K 2 O = 1.92) and potassium chloride (1 g) were well mixed in a mortar and fired in a muffle furnace at 900 ° C. for 4 hours. The product was disintegrated and observed by SEM and X-ray diffraction, and as a result, it was found to be granular potassium dititanate.
【００２５】得られた粒状２チタン酸カリウムを４％ス
ラリーとして３時間撹拌し、濾別、乾燥した後、マッフ
ル炉中、９００℃で１時間焼成した。生成物は解砕して
ＳＥＭ観察、Ｘ線回折した結果、粒状４チタン酸カリウ
ムであった。The obtained granular potassium dititanate was stirred as a 4% slurry for 3 hours, filtered, dried, and then calcined in a muffle furnace at 900 ° C. for 1 hour. The product was disintegrated and observed by SEM and X-ray diffraction. As a result, it was found to be granular potassium tetratitanate.
【００２６】得られた粒状４チタン酸カリウムを４％ス
ラリーとし、７０％Ｈ2 ＳＯ4 を適宜添加して、ｐＨが
７に保たれるよう維持しながら３時間撹拌した後、濾
別、乾燥し、マッフル炉中、６００℃で１時間焼成し
た。The obtained granular potassium tetratitanate was made into a 4% slurry, and 70% H 2 SO 4 was appropriately added thereto, followed by stirring for 3 hours while maintaining the pH at 7, followed by filtration and drying. Then, it was baked at 600 ° C. for 1 hour in a muffle furnace.
【００２７】生成物を解砕し目的物を得た。このもの
は、ＳＥＭ観察、Ｘ線回折の結果平均長径１０８μｍ、
平均短径４６μｍ、平均アスペクト比２．７の粒状８チ
タン酸カリウムであった。またメジアン径は７３μｍで
あった。The desired product was obtained by crushing the product. This was obtained by SEM observation and X-ray diffraction.
It was granular potassium octa titanate having an average minor axis of 46 μm and an average aspect ratio of 2.7. The median diameter was 73 μm.
【００２８】（実施例２〜７及び比較例１〜４）原料混
合比及び焼成温度を表１に示す条件に変更した他は実施
例１と同様にして８チタン酸カリウムを合成した。中間
生成物及び最終生成物の形状及び組成を併せて表１に示
す。なお、表１における組成の「２」は２チタン酸カリ
ウムを、「４」は４チタン酸カリウムを、「８」は８チ
タン酸カリウムを示す。「４＞２」は４チタン酸カリウ
ムが２チタン酸カリウムよりも相対的に多く含まれてい
ることを意味しており、「４＝２」は４チタン酸カリウ
ムと２チタン酸カリウムがほぼ同量含まれていることを
意味している。また、形状における短径及び長径並びに
メジアン径の単位はμｍである。Examples 2 to 7 and Comparative Examples 1 to 4 Potassium 8-titanate was synthesized in the same manner as in Example 1 except that the raw material mixing ratio and the firing temperature were changed to the conditions shown in Table 1. Table 1 also shows the shapes and compositions of the intermediate product and the final product. In Table 1, “2” indicates potassium dititanate, “4” indicates potassium tetratitanate, and “8” indicates potassium octa titanate. “4> 2” means that potassium tetratitanate is contained relatively more than potassium dititanate, and “4 = 2” means that potassium tetratitanate and potassium dititanate are almost the same. It means that the amount is included. The unit of the minor axis, major axis, and median diameter in the shape is μm.
【００２９】[0029]
【表１】 [Table 1]
【００３０】また、実施例１、比較例１及び比較例２で
得られた８チタン酸カリウムのＳＥＭ写真を図１〜図３
に示す。表１から明らかなように、本発明に従い製造さ
れた実施例１〜７の８チタン酸カリウムは、いずれもア
スペクト比が３未満であり、粒状であることがわかる。
これに対し、比較例１〜４で得られた８チタン酸カリウ
ムは、アスペクト比が７以上であり、繊維形状を有して
いることがわかる。また、図１〜図３からも明らかなよ
うに、実施例１で得られた８チタン酸カリウムは粒状で
あるのに対し、比較例１及び２で得られた８チタン酸カ
リウムは繊維形状を有している。FIGS. 1 to 3 show SEM photographs of the potassium octitanate obtained in Example 1, Comparative Example 1 and Comparative Example 2.
Shown in As is clear from Table 1, the potassium octitanates of Examples 1 to 7 produced according to the present invention have an aspect ratio of less than 3 and are all granular.
On the other hand, potassium octitanate obtained in Comparative Examples 1 to 4 has an aspect ratio of 7 or more and has a fiber shape. In addition, as is clear from FIGS. 1 to 3, potassium octitanate obtained in Example 1 is granular, whereas potassium octitanate obtained in Comparative Examples 1 and 2 has a fiber shape. Have.
【００３１】[0031]
【発明の効果】本発明によれば、粒状８チタン酸カリウ
ムを安定して製造することができる。本発明により製造
される粒状８チタン酸カリウムは、ブレーキ用摩擦剤等
の各種の用途に好適に使用することができる。According to the present invention, granular potassium octitanate can be produced stably. The granular potassium octitanate produced according to the present invention can be suitably used for various applications such as a friction agent for a brake.
【図１】本発明の実施例１により製造された粒状８チタ
ン酸カリウムの粒子形状を示す電子顕微鏡写真。FIG. 1 is an electron micrograph showing the particle shape of granular potassium octa titanate produced according to Example 1 of the present invention.
【図２】比較例１で製造された８チタン酸カリウムの粒
子形状を示す電子顕微鏡写真。FIG. 2 is an electron micrograph showing the particle shape of potassium octa titanate produced in Comparative Example 1.
【図３】比較例２で製造された８チタン酸カリウムの粒
子形状を示す電子顕微鏡写真。FIG. 3 is an electron micrograph showing the particle shape of potassium octa titanate produced in Comparative Example 2.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 稲田 幸輔 徳島県徳島市川内町加賀須野463 大塚化 学株式会社徳島工場内 Ｆターム(参考） 3J058 BA61 EA31 EA37 GA26 GA62 GA68 GA82 GA92 4G047 CA06 CB04 CC03 CD03 ────────────────────────────────────────────────── ─── Continuing from the front page (72) Inventor Kosuke Inada 463 Kagasuno, Kawauchi-cho, Tokushima City, Tokushima Prefecture F-term (reference) 3J058 BA61 EA31 EA37 GA26 GA62 GA68 GA82 GA92 4G047 CA06 CB04 CC03 CD03
Claims (5)
物及び加熱により酸化カリウムとなるカリウム化合物を
酸化物換算モル比でＴｉＯ2 ／Ｋ2 Ｏ＝０．８５〜２．
０の割合で混合し７００〜９４０℃で焼成して２チタン
酸カリウムを得る第一の工程、第一の工程で得られた２
チタン酸カリウムを水処理した後、６５０〜９４０℃で
焼成する第二の工程、第二の工程で得られた焼成物を水
分散させ分散液のｐＨが６〜８となるよう酸を加えて中
和した後、２００〜８００℃で焼成する第三の工程から
なる粒状８チタン酸カリウムの製造方法。1. A titanium compound which becomes titanium oxide when heated and a potassium compound which becomes potassium oxide when heated are expressed as TiO 2 / K 2 O = 0.85-2.
A first step of mixing at a ratio of 0 and firing at 700 to 940 ° C. to obtain potassium dititanate;
After the potassium titanate is treated with water, the second step of firing at 650 to 940 ° C., the fired product obtained in the second step is dispersed in water, and an acid is added so that the pH of the dispersion becomes 6 to 8. A method for producing granular potassium octa titanate comprising a third step of baking at 200 to 800 ° C. after neutralization.
塩化カリウムを混合原料に添加する請求項１に記載の粒
状８チタン酸カリウムの製造方法。2. The method according to claim 1, wherein potassium chloride is added as a flux to the mixed raw material in the first step.
量１００重量部に対して塩化カリウムを１重量部以上添
加する請求項２に記載の粒状８チタン酸カリウムの製造
方法。3. The method according to claim 2, wherein 1 part by weight or more of potassium chloride is added to 100 parts by weight of the total amount of the titanium compound and the potassium compound.
れる平均アスペクト比５未満の粒状８チタン酸カリウ
ム。4. A granular potassium octa titanate having an average aspect ratio of less than 5, which is obtained by the production method according to claim 1.
求項４に記載の粒状８チタン酸カリウム。5. The granular potassium octitanate according to claim 4, wherein the median diameter is 30 to 100 μm.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12275099A JP4319285B2 (en) | 1999-04-28 | 1999-04-28 | Method for producing granular potassium potassium titanate |
| AU38413/00A AU3841300A (en) | 1999-04-28 | 2000-04-20 | Method for preparing potassium octatitanate in particulate form |
| PCT/JP2000/002610 WO2000066497A1 (en) | 1999-04-28 | 2000-04-20 | Method for preparing potassium octatitanate in particulate form |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12275099A JP4319285B2 (en) | 1999-04-28 | 1999-04-28 | Method for producing granular potassium potassium titanate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000313620A true JP2000313620A (en) | 2000-11-14 |
| JP4319285B2 JP4319285B2 (en) | 2009-08-26 |
Family
ID=14843685
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12275099A Expired - Fee Related JP4319285B2 (en) | 1999-04-28 | 1999-04-28 | Method for producing granular potassium potassium titanate |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP4319285B2 (en) |
| AU (1) | AU3841300A (en) |
| WO (1) | WO2000066497A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008123046A1 (en) * | 2007-04-04 | 2008-10-16 | Otsuka Chemical Co., Ltd. | Potassium titanate, process for production of the same, friction materials, and resin compositions |
| WO2013099380A1 (en) * | 2011-12-28 | 2013-07-04 | 株式会社クボタ | Titanium oxide compound, production method therefor, lithium ion secondary battery using same, potassium tetratitanate, and hydrous tetratitinate compound |
| JP2013241329A (en) * | 2013-05-07 | 2013-12-05 | Kubota Corp | Titanium oxide compound |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11352265B2 (en) | 2016-12-13 | 2022-06-07 | Otsuka Chemical Co., Ltd. | Potassium titanate powder, method for producing same, friction modifier, resin composition, friction material, and friction member |
| CN114671459A (en) * | 2022-03-16 | 2022-06-28 | 张家港大塚化学有限公司 | Preparation method of non-fibrous potassium octatitanate |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02129030A (en) * | 1988-11-04 | 1990-05-17 | Natl Inst For Res In Inorg Mater | Production of octotitanic acid salt |
| JP2678810B2 (en) * | 1990-07-06 | 1997-11-19 | 株式会社クボタ | Method for producing potassium octatitanate polycrystalline fiber |
| JPH05194973A (en) * | 1992-01-22 | 1993-08-03 | Toyohisa Fujita | Electric-field-responsive fluid |
| JP3031650B2 (en) * | 1993-05-24 | 2000-04-10 | 株式会社クボタ | Fluororesin composition for sliding members |
| JP3028207B2 (en) * | 1996-11-11 | 2000-04-04 | 大塚化学株式会社 | Method for producing granular potassium hexatitanate |
| JP4090530B2 (en) * | 1997-02-28 | 2008-05-28 | Ｊｆｅミネラル株式会社 | Method for producing non-fibrous potassium titanate |
| JPH10279924A (en) * | 1997-04-09 | 1998-10-20 | Kubota Corp | Friction material for non-asbestos brake |
-
1999
- 1999-04-28 JP JP12275099A patent/JP4319285B2/en not_active Expired - Fee Related
-
2000
- 2000-04-20 WO PCT/JP2000/002610 patent/WO2000066497A1/en active Application Filing
- 2000-04-20 AU AU38413/00A patent/AU3841300A/en not_active Abandoned
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008123046A1 (en) * | 2007-04-04 | 2008-10-16 | Otsuka Chemical Co., Ltd. | Potassium titanate, process for production of the same, friction materials, and resin compositions |
| EP2130798A1 (en) | 2007-04-04 | 2009-12-09 | Otsuka Chemical Holdings Co., Ltd. | Potassium titanate, process for production of the same, friction materials, and resin compositions |
| US7901659B2 (en) | 2007-04-04 | 2011-03-08 | Otsuka Chemical Co., Ltd. | Potassium titanate, method for manufacturing the same, friction material and resin composition |
| US20110158898A1 (en) * | 2007-04-04 | 2011-06-30 | Nobuki Itoi | Method for manufacturing potassium titanate |
| US8241595B2 (en) | 2007-04-04 | 2012-08-14 | Otsuka Chemical, Co., Ltd. | Method for manufacturing potassium titanate |
| JP5531613B2 (en) * | 2007-04-04 | 2014-06-25 | 大塚化学株式会社 | Potassium titanate, method for producing the same, friction material and resin composition |
| KR101428833B1 (en) | 2007-04-04 | 2014-08-08 | 오츠카 가가쿠 가부시키가이샤 | Potassium titanate, process for production of the same, friction materials, and resin compositions |
| WO2013099380A1 (en) * | 2011-12-28 | 2013-07-04 | 株式会社クボタ | Titanium oxide compound, production method therefor, lithium ion secondary battery using same, potassium tetratitanate, and hydrous tetratitinate compound |
| JP2013136491A (en) * | 2011-12-28 | 2013-07-11 | Kubota Corp | Production method of titanium oxide compound, negative electrode, lithium ion secondary battery |
| US9174854B2 (en) | 2011-12-28 | 2015-11-03 | Kubota Corporation | Bronze-type titanium oxide compound containing potassium, method of manufacturing the same, and lithium-ion secondary battery using the same |
| JP2013241329A (en) * | 2013-05-07 | 2013-12-05 | Kubota Corp | Titanium oxide compound |
Also Published As
| Publication number | Publication date |
|---|---|
| AU3841300A (en) | 2000-11-17 |
| WO2000066497A1 (en) | 2000-11-09 |
| JP4319285B2 (en) | 2009-08-26 |
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