JPH08152737A - Highly dispersible hydrophobic metal oxide powder and production of the same - Google Patents
Highly dispersible hydrophobic metal oxide powder and production of the sameInfo
- Publication number
- JPH08152737A JPH08152737A JP6317778A JP31777894A JPH08152737A JP H08152737 A JPH08152737 A JP H08152737A JP 6317778 A JP6317778 A JP 6317778A JP 31777894 A JP31777894 A JP 31777894A JP H08152737 A JPH08152737 A JP H08152737A
- Authority
- JP
- Japan
- Prior art keywords
- amino
- metal oxide
- oxide powder
- highly dispersible
- modified organopolysiloxane
- 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.)
- Granted
Links
Landscapes
- Developing Agents For Electrophotography (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Silicon Compounds (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Silicon Polymers (AREA)
Abstract
Description
【０００１】本発明はトナー外添削として用いる高分散
性疎水性金属酸化物粉体及びその製造方法に関し、更に
詳しくは電荷調製された高分散性疎水性金属酸化物粉体
及びその製造方法に関する。The present invention relates to a highly dispersible hydrophobic metal oxide powder used as an external additive for toner, and a method for producing the same, and more particularly to a highly dispersed hydrophobic metal oxide powder having a charge adjusted and a method for producing the same.
【０００２】微細な金属酸化物粉体の表面を有機物で被
覆し疎水化した疎水性金属酸化物粉体（以下、単に金属
酸化物とも呼ぶ）は、複写機、レーザープリンタ、普通
紙ファクシミリなどを含む電子写真において、トナーの
流動性改善剤として広く用いられている。これらの用途
においては、キャリアである鉄あるいは酸化鉄に対する
金属酸化物粉体自体の疎水性と流動性が重要な性質の一
つとなっており、種々の処理剤によってその疎水性と流
動性が同時に制御されている。この中にあって、キャリ
アである鉄あるいは酸化鉄に対する良好な摩擦帯電性を
有することも必要で、従来疎水性及び流動性を有する金
属酸化物粉体の鉄に対する摩擦帯電性を付与する場合、
その摩擦帯電量は、それに用いられている処理剤の種類
によって正または負の値を示すので、疎水性金属酸化物
に付与する摩擦帯電量の制御は、使用するトナーの種類
に合わせてアミノ置換シラン化合物やアミノ変性オルガ
ノポリシロキサン等の処理剤を加え、加えた処理剤の種
類と添加量で調製するのが通例である。A hydrophobic metal oxide powder (hereinafter also simply referred to as a metal oxide) obtained by coating the surface of a fine metal oxide powder with an organic substance to make it hydrophobic is used in copying machines, laser printers, plain paper facsimiles, and the like. It is widely used as a toner fluidity improving agent in electrophotography including the above. In these applications, the hydrophobicity and fluidity of the metal oxide powder itself with respect to iron or iron oxide as a carrier are one of the important properties. Controlled. Among these, it is also necessary to have good triboelectric chargeability to iron or iron oxide as a carrier, and in the case of imparting triboelectric chargeability to iron of a metal oxide powder having conventional hydrophobicity and fluidity,
The triboelectrification amount shows a positive or negative value depending on the type of treatment agent used, so that the triboelectrification amount given to the hydrophobic metal oxide can be controlled by amino substitution according to the type of toner used. It is customary to add a treating agent such as a silane compound or an amino-modified organopolysiloxane, and prepare the treating agent according to the type and the amount of the treating agent added.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、疎水性
金属酸化物に付与する摩擦帯電量の制御を、使用するト
ナーの種類に合わせてアミノ置換シラン化合物やアミノ
変性オルガノポリシロキサン等の処理剤を加え、加えた
処理剤の種類と添加量で調製することは、十分な疎水化
を行いかつ電荷を任意に調製することが非常に困難であ
るばかりでなく、操作が複雑の上、試行錯誤で行うの
で、調整効率が悪いという問題があった。そこで、本発
明者等は、十分な疎水化と任意の電荷調製を行うために
鋭意検討を重ねた結果、アミノ基を有する処理剤に少量
の酸性化合物を加えて反応させることにより、正帯電性
を示すアミノ基の量を減らすことができるので、アミノ
基を有する処理剤で処理された疎水性金属酸化物の電荷
を酸性化合物の量で任意に調製できると共に、更に得ら
れた疎水性金属酸化物は粉体の分散性が向上し、トナー
に添加した際のトナーの流動性も大きく向上することを
見出し、この知見に基づいて本発明はなされたものであ
る。したがって本発明が解決しようとする第１の課題
は、電荷の調整され、かつ優れた流動性を有する高分散
性疎水性金属酸化物粉体を提供することにある。本発明
が解決しようとする第２の課題は、電荷の調整され、か
つ優れた流動性を有する高分散性疎水性金属酸化物粉体
の製造方法を提供することにある。However, in order to control the triboelectric charge amount imparted to the hydrophobic metal oxide, a treating agent such as an amino-substituted silane compound or an amino-modified organopolysiloxane is added according to the type of toner used. , It is not only very difficult to sufficiently hydrophobize and to arbitrarily adjust the electric charge by preparing with the kind and the addition amount of the treating agent added, but the operation is complicated, and it is carried out by trial and error. Therefore, there was a problem that the adjustment efficiency was poor. Therefore, the inventors of the present invention have conducted extensive studies in order to perform sufficient hydrophobization and arbitrary charge adjustment, and as a result, by adding a small amount of an acidic compound to a treating agent having an amino group to cause a reaction, a positive charging property is obtained. It is possible to reduce the amount of the amino group exhibiting the above, so that the charge of the hydrophobic metal oxide treated with the treating agent having an amino group can be arbitrarily adjusted by the amount of the acidic compound, and further the obtained hydrophobic metal oxide can be obtained. The present invention has been made on the basis of this finding and found that the dispersibility of powder improves and the fluidity of the toner when added to the toner also greatly improves. Therefore, the first problem to be solved by the present invention is to provide a highly dispersible hydrophobic metal oxide powder having an adjusted charge and excellent fluidity. A second problem to be solved by the present invention is to provide a method for producing a highly dispersible hydrophobic metal oxide powder having an adjusted charge and excellent fluidity.
【０００４】[0004]
【課題を解決するための手段】したがって、本発明が解
決しようとする各課題は、以下の各発明によってそれぞ
れ達成される。 （１）アミノ変性オルガノポリシロキサンあるいはアミ
ノ置換シラン化合物から選択された少なくとも１つを有
する高分散性疎水性金属酸化物粉体であって、前記アミ
ノ基の少なくとも一部がアミン塩からなることを特徴と
する高分散性疎水性金属酸化物粉体。 （２）アミン塩を形成する酸性化合物が無機酸又は有機
酸から選択された少なくとも１つであることを特徴とす
る前記第１項に記載の高分散性疎水性金属酸化物粉体。 （３）アミノ変性オルガノポリシロキサンとアミノ置換
シラン化合物との混合比が０：１〜１：０であることを
特徴とする前記第１項又は第２項に記載の高分散性疎水
性金属酸化物粉体。 （４）浮遊状態にある金属酸化物粉体にアミノ置換シラ
ン化合物および／またはアミノ変性オルガノポリシロキ
サンと酸性化合物との混合物を接触させ、得られた接触
物を加熱することを特徴とする高分散性疎水性金属酸化
物粉体の製造方法。 （５）浮遊状態にある金属酸化物粉体にアミノ置換シラ
ン化合物および／またはアミノ変性オルガノポリシロキ
サンと酸性化合物を接触させる際、これらのいずれかを
先に接触させることを特徴とする前記第４項に記載の高
分散性疎水性金属酸化物粉体の製造方法。Therefore, the respective problems to be solved by the present invention are achieved by the following respective inventions. (1) A highly dispersible hydrophobic metal oxide powder having at least one selected from amino-modified organopolysiloxanes and amino-substituted silane compounds, wherein at least a part of the amino groups comprises an amine salt. Characteristically highly dispersible hydrophobic metal oxide powder. (2) The highly dispersible hydrophobic metal oxide powder according to the above item 1, wherein the acidic compound forming the amine salt is at least one selected from an inorganic acid and an organic acid. (3) The highly dispersible hydrophobic metal oxide as described in the above item 1 or 2, wherein the mixing ratio of the amino-modified organopolysiloxane and the amino-substituted silane compound is 0: 1 to 1: 0. Material powder. (4) Highly dispersed, characterized in that a metal oxide powder in a floating state is contacted with a mixture of an amino-substituted silane compound and / or an amino-modified organopolysiloxane and an acidic compound, and the resulting contact product is heated. Of producing hydrophobic hydrophobic metal oxide powder. (5) When the amino-substituted silane compound and / or the amino-modified organopolysiloxane and the acidic compound are brought into contact with the metal oxide powder in a floating state, any one of them is first brought into contact with the powder. Item 5. A method for producing a highly dispersible hydrophobic metal oxide powder according to Item.
【０００５】以下、本発明を更に詳しく説明すると、本
発明で用いられる金属酸化物粉体は、ケイ素、アルミニ
ウム、チタンなどの金属の酸化物でその粒径は用途に適
したものであれば良く、特に比表面積５０ｍ2 ／ｇ以上
のものが好ましい。また本発明に用いられるアミノ置換
シラン化合物としては、代表的な化合物として以下のも
のが挙げられる。The present invention will be described in more detail below. The metal oxide powder used in the present invention may be an oxide of a metal such as silicon, aluminum or titanium, as long as its particle size is suitable for the intended use. Particularly, those having a specific surface area of 50 m 2 / g or more are preferable. Further, as the amino-substituted silane compound used in the present invention, the following compounds can be mentioned as typical compounds.
【０００６】[0006]
【化１】 Embedded image
【０００７】本発明で用いられるアミノ変性オルガノポ
リシロキサンとしては、側鎖または末端にアミノ基を含
むアルキル基を有するオルガノポリシロキサンであれ
ば、特に限定されず、このような化合物は、例えばＸ−
２２−１６１Ａ、ＫＦ８５７、ＫＦ３９３等の商品名で
信越化学（株）から市販されている。本発明を構成する
金属酸化物粉体を得るために使用されるアミノ置換シラ
ン化合物および／またはアミノ変性オルガノポリシロキ
サン等の処理剤の使用量は、被処理金属酸化物粉体の種
類、比表面積や処理剤の種類に依存しており、粉末表面
に均一に被覆されなおかつ透過率法で８０％以上の疎水
性が得られる量であればよく特に規定されないが、好ま
しくは前記処理剤の使用量は、被処理金属酸化物粉体に
対して、５〜４０重量％であり、特に好ましくは１０〜
３０重量％を用いることが好ましい。The amino-modified organopolysiloxane used in the present invention is not particularly limited as long as it is an organopolysiloxane having an alkyl group containing an amino group at its side chain or terminal, and such a compound is, for example, X-.
22-161A, KF857, KF393, etc. are commercially available from Shin-Etsu Chemical Co., Ltd. The amount of the treating agent such as amino-substituted silane compound and / or amino-modified organopolysiloxane used to obtain the metal oxide powder constituting the present invention depends on the type of the metal oxide powder to be treated and the specific surface area. It depends on the type of the treatment agent and the treating agent, and is not particularly limited as long as the powder surface is uniformly coated and a hydrophobicity of 80% or more by the transmittance method is obtained, but the amount of the treating agent used is preferable. Is 5 to 40% by weight based on the metal oxide powder to be treated, and particularly preferably 10 to
It is preferable to use 30% by weight.
【０００８】本発明に用いられる酸性化合物は、無機酸
又は有機酸があり、具体的な例としては、無機酸は、硫
酸、塩酸、硝酸、燐酸、フッ酸、臭酸、フルオロスルホ
ン酸、過塩素酸およびこれらの混合酸等が挙げられる。
また有機酸としては、ギ酸、酢酸、ブタン酸、サリチル
酸、メタンスルホン酸、ベンゼンスルホン酸、パラトル
エンスルホン酸、トリフルオロ酢酸、トリフルオロスル
ホン酸、ペルフルオロブチルスルホン酸、ペルフルオロ
オクチルスルホン酸、ペルフルオロブチルカルボン酸等
が挙げられる。これらの酸性化合物は、有機酸と無機酸
の混合液を用いることもできる。これらの酸性化合物の
添加量は、所望の電荷量に合わせてアミノ基の割合を減
らすのに必要なモル数を考慮して適宜決定されるもの
で、使用に際し試験により決定しうる事項である。The acidic compound used in the present invention is an inorganic acid or an organic acid. Specific examples of the inorganic acid include sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, hydrofluoric acid, bromic acid, fluorosulfonic acid, and peroxy acid. Examples include chloric acid and mixed acids thereof.
Further, as the organic acid, formic acid, acetic acid, butanoic acid, salicylic acid, methanesulfonic acid, benzenesulfonic acid, paratoluenesulfonic acid, trifluoroacetic acid, trifluorosulfonic acid, perfluorobutylsulfonic acid, perfluorooctylsulfonic acid, perfluorobutylcarboxylic acid. Acid etc. are mentioned. As these acidic compounds, a mixed solution of an organic acid and an inorganic acid can also be used. The amount of these acidic compounds added is appropriately determined in consideration of the number of moles necessary to reduce the proportion of amino groups in accordance with the desired charge amount, and is a matter that can be determined by a test before use.
【０００９】〔透過率法〕本発明に用いられる透過率法
とは、処理された金属酸化物粉体の疎水率を実験的に求
める方法であり、これは以下の手順によって測定され
る。処理された金属酸化物粉体１．０ｇと蒸留水１００
ｍｌを抽出用フラスコに入れ、１０分間激しく振とう攪
拌する。その後１０分間静置し、フラスコのそこから少
量の懸濁液を抜き出す。この液の５５０ｍｍの光に対す
る透過率を、蒸留水の透過率を１００％として表した値
をその金属酸化物粉体の疎水率とする。このようにして
測定された疎水率の値が高いほど、その金属酸化物粉体
の吸湿性が減少して湿度に対して安定であり利用価値が
高くなる。[Transmittance Method] The transmittance method used in the present invention is a method for experimentally determining the hydrophobicity of the treated metal oxide powder, which is measured by the following procedure. 1.0 g of treated metal oxide powder and 100 distilled water
Place ml in extraction flask and shake vigorously for 10 minutes. Then, it is left to stand for 10 minutes, and a small amount of the suspension is extracted from the flask. The value of the transmittance of this liquid for light of 550 mm, where the transmittance of distilled water is 100%, is the hydrophobicity of the metal oxide powder. The higher the value of the hydrophobicity measured in this manner, the less the hygroscopicity of the metal oxide powder, the more stable it is to humidity, and the higher the utility value.
【００１０】〔篩振とう法〕本発明に用いられる篩振と
う法とは、金属酸化物粉体を含むトナーの流動性を測定
するもので、以下の手順によって測定される。処理され
た金属酸化物粉体０．０５ｇを、スチレン−アクリル樹
脂中にカーボン１８％を分散、粉砕後、平均粒径７±３
μｍに分級して得られた樹脂粉１０ｇに加え、機械的に
３０秒間混合しトナーを調製する。このようにして得ら
れたトナーを電磁式篩振とう器で１分間振とうし、１０
０メッシュ（目の開き１５０μｍ）を通過した粉体重量
を、最初に仕込んだ粉体重量５ｇを１００％として表し
た値をその金属酸化物粉体を含むトナーの流動性とす
る。このようにして測定された流動性が高いほど、金属
酸化物粉体の分散性が良好であることを示し、したがっ
て、現像した際に、カブリの発生や画像濃度の低下が起
こりにくい。[Sieving Shaking Method] The sieving shaking method used in the present invention measures the fluidity of a toner containing a metal oxide powder and is measured by the following procedure. An average particle size of 7 ± 3 after dispersing 18% of carbon in styrene-acrylic resin with 0.05 g of the treated metal oxide powder
Toner is prepared by mechanically mixing for 30 seconds in addition to 10 g of the resin powder obtained by classifying to μm. The toner thus obtained was shaken for 1 minute on an electromagnetic sieve shaker,
The weight of the powder that has passed through 0 mesh (opening size of 150 μm) is defined as the fluidity of the toner containing the metal oxide powder, with the value of the weight of the initially charged powder of 5 g expressed as 100%. The higher the fluidity measured in this way, the better the dispersibility of the metal oxide powder is, and therefore, the occurrence of fogging and the decrease in image density are less likely to occur during development.
【００１１】〔摩擦帯電量〕本発明では、調製された電
荷は鉄に対する摩擦帯電量として表される。鉄に対する
摩擦帯電量の測定方法は、文献、例えば「色材」「５
５、９、６３０−６３６、１９８２）等によって規定さ
れている。[Triboelectric Charge Amount] In the present invention, the prepared charge is expressed as a triboelectric charge amount with respect to iron. The method of measuring the triboelectric charge amount with respect to iron is described in the literature, for example, “coloring material” “5
5, 9, 630-636, 1982) and the like.
【００１２】本発明で電荷調製された高分散性疎水性金
属酸化物粉体を製造する方法は、浮遊状態にある金属酸
化物粉体にアミノ置換シラン化合物および／またはアミ
ノ変性オルガノポリシロキサン等の処理剤を接触させ、
ついで無機酸および／または有機酸と接触させるか、浮
遊状態にある金属酸化物粉体に無機酸および／または有
機酸を接触させ、ついでアミノ置換シラン化合物および
／またはアミノ変性オルガノポリシロキサン等の処理剤
を接触させるか、または浮遊状態にある金属酸化物粉体
にアミノ置換シラン化合物および／またはアミノ変性オ
ルガノポリシロキサンと無機酸および／または有機酸と
の混合物と接触させるかのいずれかの方法で製造するこ
とができる。具体的には被処理金属酸化物を機械的に十
分攪拌しながら、これに上記処理剤を連続的にまたはそ
の混合物を滴下あるいは噴霧して加える。この時用いる
処理剤の粘度に応じて、アルコール、ケトンあるいは炭
化水素などの溶剤を希釈剤として用いることも可能であ
る。処理剤添加後、窒素雰囲気で１００〜３００℃の範
囲の温度で加熱して反応を完結させるとともに溶剤を除
去する。このようにして得られた電荷調製された高分散
性疎水性金属酸化物粉体は、複写機、レーザープリン
タ、普通紙ファクシミリなどを含む電子写真において、
トナーの流動性改善剤として広く用いられる。The method for producing a highly dispersed hydrophobic metal oxide powder having a charge adjusted according to the present invention is a method in which an amino-substituted silane compound and / or an amino-modified organopolysiloxane or the like is added to a metal oxide powder in a floating state. Contact the treatment agent,
Next, contact with an inorganic acid and / or an organic acid, or contact with a metal oxide powder in a floating state with an inorganic acid and / or an organic acid, and then treatment with an amino-substituted silane compound and / or an amino-modified organopolysiloxane, etc. Either by contacting the agent or by contacting the metal oxide powder in the floating state with a mixture of an amino-substituted silane compound and / or an amino-modified organopolysiloxane and an inorganic acid and / or an organic acid. It can be manufactured. Specifically, while the metal oxide to be treated is mechanically sufficiently stirred, the above treatment agent is added thereto continuously or by dropping or spraying a mixture thereof. It is also possible to use a solvent such as alcohol, ketone or hydrocarbon as a diluent depending on the viscosity of the treating agent used at this time. After the treating agent is added, the reaction is completed by heating at a temperature in the range of 100 to 300 ° C. in a nitrogen atmosphere to remove the solvent. The charge-adjusted highly dispersible hydrophobic metal oxide powder thus obtained is used in electrophotography including copiers, laser printers, plain paper facsimiles, etc.
Widely used as a fluidity improver for toner.
【００１３】[0013]
【作用】本発明では、アミノ変性オルガノポリシロキサ
ンあるいはアミノ置換シラン化合物のアミノ基が酸によ
りアミン塩を形成することにより、電荷量を調整するこ
とができるので、分散性が向上する。したがって優れた
流動性が得られ、同時に疎水性となる。また浮遊状態下
で金属酸化物粉体にアミノ置換シラン化合物および／ま
たはアミノ変性オルガノポリシロキサンと酸性化合物と
を接触させるので、金属酸化物粉体にアミノ置換シラン
化合物および／またはアミノ変性オルガノポリシロキサ
ンと酸性化合物を短時間で均一に存在させることがで
き、分散性を向上させることができる。In the present invention, since the amino group of the amino-modified organopolysiloxane or amino-substituted silane compound forms an amine salt with an acid, the amount of charge can be adjusted, so that the dispersibility is improved. Therefore, excellent fluidity is obtained, and at the same time, it is hydrophobic. Further, since the metal oxide powder is brought into contact with the amino-substituted silane compound and / or amino-modified organopolysiloxane and the acidic compound in a floating state, the metal oxide powder is subjected to the amino-substituted silane compound and / or amino-modified organopolysiloxane. The acidic compound can be uniformly present in a short time, and the dispersibility can be improved.
【００１４】[0014]
【実施例】以下、本発明を更に詳しく説明するが、本発
明はこの例にのみ限定されるものではない。The present invention will be described in more detail below, but the present invention is not limited to this example.
【００１５】実施例１〜６及び比較例１〜６ 加熱乾燥した金属酸化物粉体２０ｇをステンレス製の容
器に仕込み、窒素雰囲気下、攪拌しながら浮遊状態を形
成し、ついで処理剤を室温で浮遊状態下の金属酸化物粉
体に噴霧した。噴霧終了後、さらに室温で３０分間攪拌
した後窒素気流下で外部加熱を行い３０分かけて２５０
℃まで昇温させ、この温度で３時間保持した後、室温ま
で放冷した。実施例１〜６、比較例１〜６により得られ
た粉体の透過率法による疎水化率、鉄に対する摩擦帯電
量および得られた粉体を添加したトナーの流動性を表１
に示す。Examples 1 to 6 and Comparative Examples 1 to 6 20 g of the heat-dried metal oxide powder was charged into a stainless steel container, and a floating state was formed under nitrogen atmosphere with stirring. It was sprayed on the metal oxide powder in a floating state. After the spraying is completed, the mixture is further stirred at room temperature for 30 minutes and then externally heated under a nitrogen stream for 250 minutes.
The temperature was raised to 0 ° C., the temperature was maintained for 3 hours, and then the mixture was allowed to cool to room temperature. Table 1 shows the hydrophobicity of the powders obtained in Examples 1 to 6 and Comparative Examples 1 to 6 by the transmittance method, the amount of triboelectricity with respect to iron, and the fluidity of the toner to which the powders are added.
Shown in
【００１６】[0016]
【表１】 [Table 1]
【００１７】表１から明らかなように、本発明の実施例
１〜６には、疎水化率及び摩擦帯電量に遜色なく流動性
が６８％〜８９％と優れていることがわかる。これに対
して比較例１〜６では、流動性が４１％以下という結果
が得られ、流動性がないか又は不十分であるこがわか
る。As is clear from Table 1, Examples 1 to 6 of the present invention have excellent fluidity of 68% to 89%, comparable to the hydrophobicity and the triboelectric charge amount. On the other hand, in Comparative Examples 1 to 6, the result that the fluidity is 41% or less is obtained, and it can be seen that the fluidity is absent or insufficient.
【００１８】[0018]
【発明の効果】本発明は、アミノ変性オルガノポリシロ
キサンあるいはアミノ置換シラン化合物のアミノ基をア
ミン塩としたことにより、金属酸化物粉体の疎水性はも
ちろんのこと、摩擦帯電量を調整することができと共に
優れた流動性がえられ、したがってトナーの流動性を著
しく改善することができるという格別顕著な効果を奏す
るものである。INDUSTRIAL APPLICABILITY According to the present invention, the amino group of the amino-modified organopolysiloxane or amino-substituted silane compound is changed to an amine salt to adjust not only the hydrophobicity of the metal oxide powder but also the triboelectric charge amount. In addition to the above, excellent fluidity can be obtained, and therefore, the fluidity of the toner can be remarkably improved, which is a remarkable effect.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成７年２月１７日[Submission date] February 17, 1995
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１３[Correction target item name] 0013
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００１３】[0013]
【作用】 本発明では、アミノ変性オルガノポリシロキ
サンあるいはアミノ置換シラン化合物のアミノ基が酸に
よりアミン塩を形成することにより、電荷量を調整する
ことができ、なおかつ粉体の分散性も向上する。したが
って優れた流動性が得られ、同時に疎水性となる。また
浮遊状態下で金属酸化物粉体にアミノ置換シラン化合物
および／またはアミノ変性オルガノポリシロキサンと酸
性化合物とを接触させるので、金属酸化物粉体にアミノ
置換シラン化合物および／またはアミノ変性オルガノポ
リシロキサンと酸性化合物を短時間で均一に存在させる
ことができ、分散性を向上させることができる。According to the present invention, by an amino group of amino-modified organopolysiloxane or amino-substituted silane compound to form an amine salt with an acid, Ki out to adjust the amount of charge is yet improved dispersibility of the powder . Therefore, excellent fluidity is obtained, and at the same time, it is hydrophobic. Further, since the metal oxide powder is brought into contact with the amino-substituted silane compound and / or amino-modified organopolysiloxane and the acidic compound in a floating state, the metal oxide powder is subjected to the amino-substituted silane compound and / or amino-modified organopolysiloxane. The acidic compound can be uniformly present in a short time, and the dispersibility can be improved.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 桜井 英章 埼玉県大宮市北袋町一丁目297番地 三菱 マテリアル株式会社中央研究所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hideaki Sakurai 1-297, Kitabukuro-cho, Omiya City, Saitama Prefecture Central Research Laboratory, Mitsubishi Materials Corporation
Claims (5)
いはアミノ置換シラン化合物から選択された少なくとも
１つを有する高分散性疎水性金属酸化物粉体であって、
前記アミノ基の少なくとも一部がアミン塩からなること
を特徴とする高分散性疎水性金属酸化物粉体。1. A highly dispersible hydrophobic metal oxide powder having at least one selected from amino-modified organopolysiloxane and amino-substituted silane compound,
Highly dispersible hydrophobic metal oxide powder characterized in that at least a part of the amino group comprises an amine salt.
又は有機酸から選択された少なくとも１つであることを
特徴とする請求項１に記載の高分散性疎水性金属酸化物
粉体。2. The highly dispersible hydrophobic metal oxide powder according to claim 1, wherein the acidic compound forming an amine salt is at least one selected from an inorganic acid and an organic acid.
ミノ置換シラン化合物との混合比が０：１〜１：０であ
ることを特徴とする請求項１又は請求項２に記載の高分
散性疎水性金属酸化物粉体。3. The highly dispersible hydrophobic metal according to claim 1, wherein the mixing ratio of the amino-modified organopolysiloxane and the amino-substituted silane compound is 0: 1 to 1: 0. Oxide powder.
置換シラン化合物および／またはアミノ変性オルガノポ
リシロキサンと酸性化合物との混合物を接触させ、得ら
れた接触物を加熱することを特徴とする高分散性疎水性
金属酸化物粉体の製造方法。4. A metal oxide powder in a floating state is contacted with a mixture of an amino-substituted silane compound and / or an amino-modified organopolysiloxane and an acidic compound, and the resulting contact product is heated. A method for producing a highly dispersible hydrophobic metal oxide powder.
置換シラン化合物および／またはアミノ変性オルガノポ
リシロキサンと酸性化合物を接触させる際、これらのい
ずれかを先に接触させることを特徴とする請求項４に記
載の高分散性疎水性金属酸化物粉体の製造方法。5. When the metal oxide powder in a floating state is contacted with the amino-substituted silane compound and / or the amino-modified organopolysiloxane and the acidic compound, one of them is first contacted. Item 5. A method for producing a highly dispersible hydrophobic metal oxide powder according to Item 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31777894A JP3261903B2 (en) | 1994-11-29 | 1994-11-29 | Highly dispersible hydrophobic metal oxide powder and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31777894A JP3261903B2 (en) | 1994-11-29 | 1994-11-29 | Highly dispersible hydrophobic metal oxide powder and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08152737A true JPH08152737A (en) | 1996-06-11 |
| JP3261903B2 JP3261903B2 (en) | 2002-03-04 |
Family
ID=18091953
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31777894A Expired - Lifetime JP3261903B2 (en) | 1994-11-29 | 1994-11-29 | Highly dispersible hydrophobic metal oxide powder and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3261903B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000327948A (en) * | 1999-05-18 | 2000-11-28 | Toda Kogyo Corp | Hydrophobilized powdery particles of metal compound and production thereof |
| JP2006001832A (en) * | 2004-06-16 | 2006-01-05 | Degussa Ag | Surface modified silica gel |
| JP2007176747A (en) * | 2005-12-28 | 2007-07-12 | Tokuyama Corp | Surface-coated silica and production method thereof |
-
1994
- 1994-11-29 JP JP31777894A patent/JP3261903B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000327948A (en) * | 1999-05-18 | 2000-11-28 | Toda Kogyo Corp | Hydrophobilized powdery particles of metal compound and production thereof |
| JP2006001832A (en) * | 2004-06-16 | 2006-01-05 | Degussa Ag | Surface modified silica gel |
| JP2007176747A (en) * | 2005-12-28 | 2007-07-12 | Tokuyama Corp | Surface-coated silica and production method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3261903B2 (en) | 2002-03-04 |
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