JP3051322B2 - Niobium oxide sol - Google Patents
Niobium oxide solInfo
- Publication number
- JP3051322B2 JP3051322B2 JP7156880A JP15688095A JP3051322B2 JP 3051322 B2 JP3051322 B2 JP 3051322B2 JP 7156880 A JP7156880 A JP 7156880A JP 15688095 A JP15688095 A JP 15688095A JP 3051322 B2 JP3051322 B2 JP 3051322B2
- Authority
- JP
- Japan
- Prior art keywords
- sol
- niobium oxide
- molar ratio
- citric acid
- oxide sol
- 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 - Fee Related
Links
Description
【０００１】[0001]
【産業上の利用分野】本発明はシュウ酸／Ｎｂ2Ｏ5（モ
ル比）＝０．９〜２．０、クエン酸／Ｎｂ2Ｏ5（モル
比）＝０．０１以上の範囲でシュウ酸とクエン酸を含有
してなる酸化ニオブゾルに関し、更に詳しくは酸化ニオ
ブゾルと各種の金属元素とを混合した場合に問題となる
ゾルの安定性を改善したものであって、広範な原料用途
に適応できるゾルを提供することを目的とする。また、
ニオブと他の金属元素を含有したゾルは、例えば触媒、
オプトエレクトロニクス材料、半導体材料等の原料とし
て極めて有用である。The present invention is oxalic acid / Nb 2 O 5 (molar ratio) BACKGROUND OF = 0.9-2.0, citrate / Nb 2 O 5 (molar ratio) = 0.01 oxalic the above range Niobium oxide sol containing acid and citric acid. More specifically, it improves the stability of sol, which is a problem when niobium oxide sol is mixed with various metal elements, and is suitable for a wide range of raw material applications. It is intended to provide a sol that can be used. Also,
Sol containing niobium and other metal elements, for example, a catalyst,
It is extremely useful as a raw material for optoelectronic materials and semiconductor materials.
【０００２】[0002]
【従来の技術】近年、セラミックス原料、電子材料等に
酸化ニオブを使用する需要が高まっており、殊にオプト
エレクトロニクス、触媒等の材料として粒子径が小さ
く、均一な粒度分布を有する酸化ニオブ原料が要求され
ている。2. Description of the Related Art In recent years, there has been an increasing demand for using niobium oxide for ceramic raw materials, electronic materials, and the like. In particular, niobium oxide raw materials having a small particle size and a uniform particle size distribution as materials for optoelectronics, catalysts, and the like have been developed. Has been requested.
【０００３】しかしながら、酸化ニオブ原料は一般に水
酸化ニオブ、酸化ニオブ等の原料粉末を焼成し、これを
粉砕して使用されるため、その粒子は不均一であるだけ
でなく、比較的粒子径の大きなニオブ原料が使用されて
いるのが現状である。[0003] However, niobium oxide raw materials are generally used by baking raw material powders such as niobium hydroxide and niobium oxide and pulverizing the raw materials, so that the particles are not only non-uniform but also have a relatively large particle diameter. At present, large niobium raw materials are used.
【０００４】従って、前述のような均一、微細粒子径の
酸化ニオブ原料の要求が高くなっているのが現状であ
る。Accordingly, at present, there is an increasing demand for a raw material of niobium oxide having a uniform and fine particle diameter as described above.
【０００５】このような現状に於いて、上述の要求に応
じるべく近年各種の元素を微細粒子のゾルで提供する技
術が開発され、ニオブ原料についてもペルオキシニオブ
酸のゾルの技術が開示されている(特開平３−１５３５
２７号)。Under these circumstances, a technique for providing various elements in a sol of fine particles has recently been developed to meet the above-mentioned requirements, and a technique of a peroxyniobic acid sol has been disclosed for a niobium raw material. (Japanese Unexamined Patent Publication No.
No. 27).
【０００６】しかしながら、このペルオキシニオブ酸ゾ
ル（Ｈ+[ＮｂＯ2（Ｏ）2]-）は、水酸化ニオブ等の原料
を強酸と過酸化水素水を用いてペルオキシニオブ酸の水
溶液とし、これを5〜50℃の温度に保持してゾルを得る
ものであって、得られたゾルには過酸化物が常に存在し
ていることから、その成分構成において自ずと用途が限
定される。即ち、触媒、オプトエレクトロニクス原料等
への過酸化物の存在は、他の原料との反応性などの問題
で致命的であるが、この過酸化水素の存在なしではこの
ようなゾルは使用できないのが現状である。However, this peroxyniobate sol (H + [NbO 2 (O) 2 ] − ) is prepared by converting a raw material such as niobium hydroxide into an aqueous solution of peroxyniobate using a strong acid and a hydrogen peroxide solution. The sol is obtained by maintaining the temperature at 5 to 50 ° C., and since the obtained sol always contains a peroxide, its use is naturally limited in the composition of its components. That is, the presence of peroxides in catalysts, optoelectronic materials, etc. is fatal due to problems such as reactivity with other materials, but such sols cannot be used without the presence of hydrogen peroxide. Is the current situation.
【０００７】従って、酸化ニオブ原料として成分組成に
よって用途が制限されることがない、均一微細な酸化ニ
オブ原料の出現が要望されているのが現状である。Therefore, at present, there is a demand for the appearance of a uniform and fine niobium oxide raw material whose use is not limited by the composition of the niobium oxide raw material.
【０００８】[0008]
【発明が解決しようとする課題】本発明者らは上述のよ
うな現状に於いて、各種の目的用途に適用できる酸化ニ
オブ材料を得るべく酸化ニオブのゾルについて鋭意検討
を重ね、その結果シュウ酸とニオブ酸化物が（ＣＨＣＯ
Ｏ）2／Ｎｂ2Ｏ5（モル比）が０．２〜０．８の範囲で
構成される粒子径100オングストローム以下の酸化ニオ
ブゾル並びにその製造方法を完成し、先に出願を行った
(特願平５−１３９３７０号)。Under the circumstances described above, the present inventors have intensively studied a sol of niobium oxide in order to obtain a niobium oxide material applicable to various purposes, and as a result, as a result, And niobium oxide (CHCO
O) 2 / Nb 2 O 5 (molar ratio) in the range of 0.2 to 0.8 Niobium oxide sol having a particle diameter of 100 Å or less and a method for producing the same were completed, and an application was filed earlier
(Japanese Patent Application No. 5-139370).
【０００９】しかし、その後この酸化ニオブゾルについ
て更に検討を進めた結果、この酸化ニオブゾルの用途に
於いて、他の金属元素と併用するとゾルの安定性が低下
し、ゲル化によってゾル溶液が不均一化するために使用
できないことが明らかとなった。このような問題は、こ
の酸化ニオブゾルを他の金属元素を含有する原料と併用
する時、あるいは酸化ニオブゾル自体に金属元素を含有
させておく場合に生じるものである。However, as a result of further study on the niobium oxide sol, when the niobium oxide sol is used in combination with other metal elements, the stability of the sol is lowered, and the sol solution becomes non-uniform due to gelation. It turned out that it could not be used to. Such a problem occurs when the niobium oxide sol is used in combination with a raw material containing another metal element, or when the metal element is contained in the niobium oxide sol itself.
【００１０】従って、この酸化ニオブゾルは、微細粒子
径を有する酸化ニオブゾルとして優れた特性を有するに
も拘らず、ニオブ以外の他の金属元素との併用が困難で
あることから、その使用・用途面で制約されている。Therefore, although this niobium oxide sol has excellent properties as a niobium oxide sol having a fine particle diameter, it is difficult to use it in combination with a metal element other than niobium. Is constrained.
【００１１】[0011]
【課題を解決するための手段】係る課題について本発明
者らは更に検討を重ねた結果、上述のシュウ酸によって
安定化された酸化ニオブゾルに、予めクエン酸を含有さ
せておくことにより得られるゾルが、ニオブ以外の他の
金属元素との併用時にゲル化等によって不安定化せず、
安定な酸化ニオブゾルとして使用できることが可能とな
ることを見い出し、先に出願を行った（特願平６−３０
９５８２号）。Means for Solving the Problems As a result of further studies by the inventors of the present invention, the sol obtained by previously containing citric acid in the above-mentioned niobium oxide sol stabilized by oxalic acid was obtained. However, when used in combination with other metal elements other than niobium, it does not become unstable due to gelation, etc.
It has been found that it can be used as a stable niobium oxide sol, and it has been filed earlier (Japanese Patent Application No. 6-30).
No. 9582).
【００１２】しかしながら、このクエン酸を含有したシ
ュウ酸安定化酸化ニオブゾルは、そのその組成が（ＨＣ
ＯＯ）2／Ｎｂ2Ｏ5（モル比）が０．２〜０．８であ
る。However, this oxalic acid-stabilized niobium oxide sol containing citric acid has a composition of (HC
OO) 2 / Nb 2 O 5 ( molar ratio) is 0.2 to 0.8.
【００１３】本発明者らはこのようなシュウ酸安定化酸
化ニオブゾルについて更に研究を進めた結果、クエン酸
が共存している場合、（ＨＣＯＯ）2／Ｎｂ2Ｏ5（モル
比）が０．９以上であっても、ニオブ以外の他の金属元
素との併用時にゲル化等によって不安定化せず、安定な
酸化ニオブゾルとして使用可能なること、更にまた、例
えば活性な水酸化ニオブをシュウ酸とクエン酸とを併用
して解膠しても安定なることを見い出し、係る知見にも
とづき本発明を完成したものである。The present inventors have further studied such an oxalic acid-stabilized niobium oxide sol. As a result, when citric acid coexists, the (HCOO) 2 / Nb 2 O 5 (molar ratio) is 0.1%. Even if it is 9 or more, it does not become unstable due to gelation when used in combination with other metal elements other than niobium and can be used as a stable niobium oxide sol. The present invention has been found to be stable even when deflocculation is carried out in combination with and citric acid, and the present invention has been completed based on such findings.
【００１４】即ち、本発明はシュウ酸／Ｎｂ2Ｏ5（モル
比）＝０．９〜２．０、クエン酸／Ｎｂ2Ｏ5（モル比）
＝０．０１以上の範囲でシュウ酸とクエン酸を含有して
なる酸化ニオブゾルに関する。更に本発明は上記酸化ニ
オブゾルにアンモニウムが含まれた酸化ニオブゾルに関
し、更にまた本発明は、前記酸化ニオブゾルに金属塩と
アンモニウムが含まれた酸化ニオブゾルに関する。That is, in the present invention, oxalic acid / Nb 2 O 5 (molar ratio) = 0.9-2.0, citric acid / Nb 2 O 5 (molar ratio)
= 0.01 or more and relates to a niobium oxide sol containing oxalic acid and citric acid. Further, the present invention relates to a niobium oxide sol in which the above-mentioned niobium oxide sol contains ammonium, and further, the present invention relates to a niobium oxide sol in which the above-mentioned niobium oxide sol contains a metal salt and ammonium.
【００１５】本発明の酸化ニオブゾルの製造方法に関し
て言えば、例えば活性な水酸化ニオブに（ＨＣＯＯ）2
／Ｎｂ2Ｏ5（モル比）＝０．９〜２．５、クエン酸／Ｎ
ｂ2Ｏ5（モル比）＝０．０１以上の範囲となるようにシ
ュウ酸及びクエン酸を加え、温度90℃以上で４時間以上
の加熱反応を行うことにより本発明の酸化ニオブゾルを
得ることができる。（ＨＣＯＯ）2／Ｎｂ2Ｏ5（モル
比）＝２．０以上のシュウ酸を加えた場合に於いては限
外濾過装置等を使用して、シュウ酸を除去し本発明範囲
内即ち、（ＨＣＯＯ）2／Ｎｂ2Ｏ5（モル比）＝０．９
〜２．０の範囲とする。（ＨＣＯＯ）2／Ｎｂ2Ｏ5（モ
ル比）＝２．０以上の場合、ゾル自体が不安定となり望
ましくない。With regard to the method for producing a niobium oxide sol according to the present invention, for example, (HCOO) 2
/ Nb 2 O 5 (molar ratio) = 0.9-2.5, citric acid / N
The niobium oxide sol of the present invention is obtained by adding oxalic acid and citric acid so that b 2 O 5 (molar ratio) = 0.01 or more, and performing a heating reaction at a temperature of 90 ° C. or more for 4 hours or more. Can be. When (HCOO) 2 / Nb 2 O 5 (molar ratio) = 2.0 or more oxalic acid is added, the oxalic acid is removed using an ultrafiltration device or the like, and the oxalic acid is removed within the scope of the present invention. (HCOO) 2 / Nb 2 O 5 ( molar ratio) = 0.9
To 2.0. When (HCOO) 2 / Nb 2 O 5 (molar ratio) = 2.0 or more, the sol itself becomes unstable, which is not desirable.
【００１６】また別法として、一度上記の如くして製造
したシュウ酸含有酸化ニオブゾルに、クエン酸を加えて
も本発明の酸化ニオブゾルを得ることができる。Alternatively, the niobium oxide sol of the present invention can be obtained by adding citric acid to the oxalic acid-containing niobium oxide sol once produced as described above.
【００１７】クエン酸の含有量に関して言えば、酸化ニ
オブゾルに対してクエン酸／Ｎｂ2Ｏ5（モル比）が０．
０１以上である。クエン酸の含有量は、併用する他の金
属塩の使用量とも関連し、金属塩の使用量が多くなる
程、クエン酸の使用量も多くなる。一般的にクエン酸／
Ｎｂ2Ｏ5（モル比）は３以下である。またクエン酸の添
加により活性な水酸化ニオブの解膠も容易となる。With respect to the content of citric acid, citric acid / Nb 2 O 5 (molar ratio) is 0.1% with respect to niobium oxide sol.
01 or more. The content of citric acid is also related to the amount of other metal salts used in combination, and as the amount of metal salt used increases, the amount of citric acid used also increases. Generally citric acid /
Nb 2 O 5 (molar ratio) is 3 or less. The addition of citric acid also facilitates peptization of active niobium hydroxide.
【００１８】また、アンモニウム含有量に関しては、添
加するクエン酸に対して、ＮＨ3／クエン酸（モル比）
で概ね３〜１５の範囲である。アンモニウムを含有させ
る方法としてはアンモニア水溶液を添加する方法が最適
であるがこれに限定されるものではない。アンモニウム
を含有させる理由は金属元素を含有せしめる場合更に安
定化させることにある。As for the ammonium content, NH 3 / citric acid (molar ratio) is added to citric acid to be added.
The range is approximately 3 to 15. As a method for containing ammonium, a method of adding an aqueous ammonia solution is optimal, but is not limited thereto. The reason for containing ammonium is to further stabilize the case where a metal element is contained.
【００１９】次に、本発明の酸化ニオブゾルは、このゾ
ルに予め金属元素を含有させて使用することもできる。
このような金属元素として、例えばニッケル、アルミニ
ウム、銅、コバルト等の金属元素である。Next, the niobium oxide sol of the present invention can be used by adding a metal element to the sol in advance.
Examples of such a metal element include metal elements such as nickel, aluminum, copper, and cobalt.
【００２０】本発明のゾルに予め金属元素を添加する方
法は、シュウ酸及びクエン酸を含有してなるゾルに、水
溶性金属塩とアンモニウム水溶液を添加する方法であ
る。The method of adding a metal element to the sol of the present invention in advance is a method of adding a water-soluble metal salt and an aqueous ammonium solution to a sol containing oxalic acid and citric acid.
【００２１】このような金属塩の種類としては、本発明
のゾルの使用目的によって異なり、特段限定できない
が、塩化ニッケル、塩化アルミニウム、塩化第二銅、シ
ュウ酸コバルト等水溶性金属塩が使用できる。また、金
属塩の使用量に関してもゾルの使用目的によって異な
り、特に限定できないが、酸化ニオブゾルに対して金属
塩／Ｎｂ2Ｏ5（モル比）で０．０１〜１．５の範囲であ
る。The kind of such a metal salt varies depending on the purpose of use of the sol of the present invention and is not particularly limited. However, water-soluble metal salts such as nickel chloride, aluminum chloride, cupric chloride, and cobalt oxalate can be used. . The amount of the metal salt used also varies depending on the purpose of use of the sol, and is not particularly limited. However, the metal salt / Nb 2 O 5 (molar ratio) is in the range of 0.01 to 1.5 with respect to the niobium oxide sol.
【００２２】金属元素を含ませる場合のアンモニア含有
量は前述の含有量と同じである。金属塩とアンモニアを
含ませる方法としては前記の他金属塩とアンモニア水溶
液とを予め別に混合し、金属元素のアンモニウム錯体を
形成させた後、これをシュウ酸及びクエン酸を含有して
なるゾルに添加混合してもよい。The content of ammonia when the metal element is contained is the same as the content described above. As a method of including a metal salt and ammonia, the other metal salt and an aqueous ammonia solution are separately mixed in advance to form an ammonium complex of a metal element, and then this is converted into a sol containing oxalic acid and citric acid. You may add and mix.
【００２３】このようにして得ることができる金属元素
を含有する本発明のゾルは、ゾル溶液の安定性に優れた
ものとなる。The sol of the present invention containing a metal element obtained in this manner has excellent sol solution stability.
【００２４】[0024]
【実施例】以下に本発明の実施例を掲げ更に説明を行う
が、本発明はこれらに限定されるものではない。また、
％は特に断らない限り全て重量％を示す。The present invention will be further described below with reference to examples of the present invention, but the present invention is not limited to these examples. Also,
All percentages are by weight unless otherwise specified.
【００２５】（実施例１）酸化ニオブ(スタルク社製)40
0gを、フッ化水素酸(ＨＦ10％)4.2Lに溶解した。この溶
液をアンモニウム水(ＮＨ315％)2.8Lに60分間かけて添
加した後、フィルタープレスでろ過、洗浄し水酸化ニオ
ブを得た。この活性な水酸化ニオブの組成分析を行った
結果、Ｎｂ2Ｏ5含有量は25.0％であった。(Example 1) Niobium oxide (manufactured by Starck) 40
0 g was dissolved in 4.2 L of hydrofluoric acid (HF 10%). The solution was added to 2.8 L of aqueous ammonium (NH 3 15%) over 60 minutes, and then filtered and washed with a filter press to obtain niobium hydroxide. As a result of a composition analysis of this active niobium hydroxide, the Nb 2 O 5 content was 25.0%.
【００２６】この水酸化ニオブを用いて、表１に示す組
成のニオブゾルを調整した。Using this niobium hydroxide, a niobium sol having a composition shown in Table 1 was prepared.
【００２７】水酸化ニオブ400gに表１に示した量のシュ
ウ酸二水和物を添加し、次いでＮｂ2Ｏ5濃度が10％とな
るように水を添加した。この溶液を攪拌しながら環流条
件下95℃で反応を行った。反応の進行に伴い、液は次第
に青色を帯び、均一なゾル状態を呈した。この時点をも
って反応を終了した。Oxalic acid dihydrate was added to 400 g of niobium hydroxide in the amount shown in Table 1, and then water was added so that the Nb 2 O 5 concentration became 10%. The solution was reacted at 95 ° C. under reflux while stirring. As the reaction proceeded, the solution gradually became blue and exhibited a uniform sol state. The reaction was completed at this point.
【００２８】このシュウ酸含有酸化ニオブゾル1kgに表
１に示した量のクエン酸一水和物とＮｂ2Ｏ5濃度が5％
となるように水を添加し、20分間攪拌を行うことにより
本発明の酸化ニオブゾルを得た。The citric acid monohydrate and the Nb 2 O 5 concentration of 5% shown in Table 1 were added to 1 kg of the oxalic acid-containing niobium oxide sol.
Was added thereto, and the mixture was stirred for 20 minutes to obtain a niobium oxide sol of the present invention.
【００２９】別に、コバルトをＣｏとして4％を含有す
る触媒原料用塩酸塩溶液を調整し、表１に示したＣｏ含
有量となるように上記本発明の酸化ニオブゾル100gと混
合した（本発明例１〜８）。Separately, a hydrochloride solution for a catalyst raw material containing 4% of cobalt as Co was prepared and mixed with 100 g of the above-mentioned niobium oxide sol of the present invention so as to have a Co content shown in Table 1 (Examples of the present invention). 1-8).
【００３０】また、本発明例と同様な方法により比較例
として表１に示した組成の混合液も合わせて調整した
（比較例１〜４）。Further, mixed liquids having the compositions shown in Table 1 as comparative examples were also prepared by the same method as in the present invention (Comparative Examples 1 to 4).
【００３１】これらの混合液の1時間、3日、1ケ月及び3ケ
月保存後の液の状態を観察した。結果を表１に示した。The state of the liquid mixture after storage for 1 hour, 3 days, 1 month and 3 months was observed. The results are shown in Table 1.
【００３２】[0032]
【表１】 [Table 1]
【００３３】（実施例２）実施例１と同様にして製造し
た活性な水酸化ニオブ400gにシュウ酸／Ｎｂ2Ｏ5（モル
比）＝１．７、クエン酸／Ｎｂ2Ｏ5（モル比）＝２．５
になるようにシュウ酸二水和物、クエン酸一水和物及び
Ｎｂ2Ｏ5濃度が8％となるように水を加え、この溶液を
攪拌しながら環流条件下95℃で7.5時間の反応を行っ
た。反応の進行に伴い、液は次第に青色を帯び、均一な
ゾル状態を呈した（本発明例９）。Example 2 Oxalic acid / Nb 2 O 5 (molar ratio) = 1.7, citric acid / Nb 2 O 5 (molar ratio) were added to 400 g of active niobium hydroxide produced in the same manner as in Example 1. ) = 2.5
Oxalic acid dihydrate, citric acid monohydrate and water were added so that the concentration of Nb 2 O 5 became 8%, and the solution was stirred at 95 ° C. for 7.5 hours under reflux under stirring. Was done. As the reaction proceeded, the liquid gradually became blue and exhibited a uniform sol state (Example 9 of the present invention).
【００３４】更にこれにpHが概ね10となるように29％ア
ンモニア水を添加し、水を加え10分間攪拌を行うことに
より、Ｎｂ2Ｏ5濃度8％のゾルを得た（本発明例１
０）。Further, 29% ammonia water was added so that the pH became approximately 10, water was added, and the mixture was stirred for 10 minutes to obtain a sol having a Nb 2 O 5 concentration of 8% (Example 1 of the present invention).
0).
【００３５】別に、Ｃｏ2.8％、Ｎｉ1.3％、Ａｌ1.5％
を含有する塩酸塩溶液を調整し、上記ゾル100gにこの溶
液12gを加えよく混合し、この溶液を室温で保存し、液
の状態を観察した。その結果を表２に示した。Separately, Co 2.8%, Ni 1.3%, Al 1.5%
Was prepared, 12 g of this solution was added to 100 g of the sol, and the mixture was mixed well. The solution was stored at room temperature, and the state of the solution was observed. The results are shown in Table 2.
【００３６】[0036]
【表２】 [Table 2]
【００３７】（実施例３）実施例１と同様にして製造し
た活性な水酸化ニオブにシュウ酸／Ｎｂ2Ｏ5（モル比）
２．５になるようにシュウ酸二水和物及びＮｂ2Ｏ5濃度
が12％となるように水を加え、この溶液を攪拌しながら
環流条件下95℃で6時間の反応を行った。反応の終結に
伴い、液は次第に青色を帯び、均一なゾル状態を呈し
た。Example 3 Oxalic acid / Nb 2 O 5 (molar ratio) was added to active niobium hydroxide produced in the same manner as in Example 1.
Oxalic acid dihydrate and water were added so that the concentration of Nb 2 O 5 became 12% to 2.5, and the reaction was carried out at 95 ° C. for 6 hours under reflux while stirring the solution. With the end of the reaction, the liquid gradually turned blue and exhibited a uniform sol state.
【００３８】次いで、反応後に得られたゾルを限外濾過
モジュール（旭化成工業製SLP-1053型）を使用し、シュ
ウ酸／Ｎｂ2Ｏ5（モル比）１．６に調整した。このゾル
の組成分析を行った結果、Ｎｂ2Ｏ5の濃度10％、pH3、
また、動的散乱光による粒度分布測定装置(PACIFIC SCI
ENTIFIC社製NICOMP Model-370型)により測定した粒子径
は60オングストロームであった。Next, the sol obtained after the reaction was adjusted to oxalic acid / Nb 2 O 5 (molar ratio) 1.6 using an ultrafiltration module (SLP-1053 manufactured by Asahi Kasei Corporation). As a result of composition analysis of this sol, the concentration of Nb 2 O 5 was 10%,
In addition, a particle size distribution analyzer (PACIFIC SCI
The particle diameter measured by ENTIFIC (NICOMP Model-370 type) was 60 angstroms.
【００３９】このゾルにクエン酸／Ｎｂ2Ｏ5（モル比）
が１．４、Ｎｂ2Ｏ5の濃度が8％になるようにクエン酸
一水和物及び水を加え、5分間攪拌を行うことにより本
発明の酸化ニオブゾルを得た。このゾルは4ヶ月間室温
で放置するも極めて安定であった。To this sol, citric acid / Nb 2 O 5 (molar ratio)
Was added and citric acid monohydrate and water were added so that the concentration of Nb 2 O 5 became 8%, and the mixture was stirred for 5 minutes to obtain a niobium oxide sol of the present invention. This sol was extremely stable when left at room temperature for 4 months.
【００４０】また、4ヶ月間放置後のこのゾルに23％ア
ンモニア水溶液をＮＨ3／クエン酸（モル比）６．８に
なるように加えた。ゾルを3ヶ月間室温で放置したが製
造時と変わることなく沈殿を見ない安定なものであっ
た。Further, a 23% aqueous ammonia solution was added to the sol after standing for 4 months so as to have a NH 3 / citric acid (molar ratio) of 6.8. The sol was allowed to stand at room temperature for 3 months, but it was stable without any precipitation as it was at the time of production.
【００４１】[0041]
【発明の効果】本発明の酸化ニオブゾルは、酸化ニオブ
ゾルと各種の金属元素とを混合した場合に問題となるゾ
ルの安定性を改善したものであって、広範な原料用途に
適応できるゾルである。また、ニオブと他の金属元素を
含有したゾルは、例えば触媒、オプトエレクトロニクス
材料、半導体材料等の原料として極めて有用である。The niobium oxide sol of the present invention has improved stability of the sol which becomes a problem when the niobium oxide sol is mixed with various metal elements, and is a sol which can be applied to a wide range of raw material applications. . A sol containing niobium and another metal element is extremely useful as a raw material for, for example, a catalyst, an optoelectronic material, a semiconductor material, and the like.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) C01G 33/00 ＣＡ（ＳＴＮ)──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int. Cl. 7 , DB name) C01G 33/00 CA (STN)
Claims (3)
〜２．０、クエン酸／Ｎｂ2Ｏ5（モル比）＝０．０１以
上の範囲でシュウ酸及びクエン酸を含有してなる酸化ニ
オブゾル。1. Oxalic acid / Nb 2 O 5 (molar ratio) = 0.9
2.0, citric acid / Nb 2 O 5 (molar ratio) = 0.01 containing oxalic acid and citric acid in the above range comprising niobium oxide sol.
〜２．０、クエン酸／Ｎｂ2Ｏ5（モル比）＝０．０１以
上の範囲でシュウ酸とクエン酸及びアンモニウムを含有
してなる酸化ニオブゾル。2. Oxalic acid / Nb 2 O 5 (molar ratio) = 0.9
2.0, citric acid / Nb 2 O 5 (molar ratio) = 0.01 comprising of oxalic acid and citric acid and ammonium in the above range niobium oxide sol.
〜２．０、クエン酸／Ｎｂ2Ｏ5（モル比）＝０．０１以
上の範囲でシュウ酸とクエン酸及び金属塩とアンモニウ
ムを含有してなる酸化ニオブゾル。3. Oxalic acid / Nb 2 O 5 (molar ratio) = 0.9
2.0, citric acid / Nb 2 O 5 (molar ratio) = 0.01 or more ranges comprising oxalic acid and citric acid and metal salts and ammonium niobium oxide sol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7156880A JP3051322B2 (en) | 1995-05-30 | 1995-05-30 | Niobium oxide sol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7156880A JP3051322B2 (en) | 1995-05-30 | 1995-05-30 | Niobium oxide sol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08325018A JPH08325018A (en) | 1996-12-10 |
| JP3051322B2 true JP3051322B2 (en) | 2000-06-12 |
Family
ID=15637416
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7156880A Expired - Fee Related JP3051322B2 (en) | 1995-05-30 | 1995-05-30 | Niobium oxide sol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3051322B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4651000B2 (en) * | 2004-01-13 | 2011-03-16 | 多木化学株式会社 | Method for producing niobium oxide sol |
| WO2007144950A1 (en) | 2006-06-15 | 2007-12-21 | Nippon Paint Co., Ltd. | Coated steel sheet |
| BRPI0621828B1 (en) | 2006-06-15 | 2018-01-02 | Nippon Steel & Sumitomo Metal Corporation | COATED STEEL SHEET |
| JP6156876B2 (en) * | 2013-10-24 | 2017-07-05 | 多木化学株式会社 | Method for producing niobate sol |
-
1995
- 1995-05-30 JP JP7156880A patent/JP3051322B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08325018A (en) | 1996-12-10 |
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