JP3146678B2 - Hydrophobic metal oxide powder - Google Patents
Hydrophobic metal oxide powderInfo
- Publication number
- JP3146678B2 JP3146678B2 JP25571292A JP25571292A JP3146678B2 JP 3146678 B2 JP3146678 B2 JP 3146678B2 JP 25571292 A JP25571292 A JP 25571292A JP 25571292 A JP25571292 A JP 25571292A JP 3146678 B2 JP3146678 B2 JP 3146678B2
- Authority
- JP
- Japan
- Prior art keywords
- metal oxide
- oxide powder
- powder
- hydrophobicity
- 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.)
- Expired - Lifetime
Links
Landscapes
- Silicon Compounds (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Developing Agents For Electrophotography (AREA)
- Glanulating (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は粉体流動性改良等の用途
に用いられる疎水性金属酸化物粉体に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a hydrophobic metal oxide powder used for purposes such as improving powder fluidity.
【０００２】[0002]
【従来の技術とその問題点】金属酸化物粉体の表面を有
機物によって疎水化したいわゆる疎水性金属酸化物粉体
は、電子写真、静電記録等において、トナーの流動性、
クリーニング性等の改良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摩擦帯電性が重要な性
質の一つとなっており、種々の処理剤によってその疎水
性と摩擦帯電性が同時に制御されている。この中にあっ
て、負の帯電性を減少させる、あるいは正の帯電性を付
与する方法としては、アミン系の有機化合物によって粉
体の表面を処理する方法が一般的に用いられている。し
かしアミン系の有機化合物として４級アンモニウム塩な
どの低分子化合物を用いた場合、表面との結合性が小さ
いために、得られる帯電量の再現性が低く、また環境特
に湿気の影響を受けやすいなどの問題点が生じやすい。
これに対しアミノ基置換シランカップリング剤、あるい
はアミノ変性ポリシロキサンで処理した場合、これらの
処理剤が化学的あるいは物理的に金属酸化物粉体表面に
強固に固定化されるため効果的に正の帯電性を得ること
ができる。しかしこれらの処理剤は比較的高価であるう
え、市販されている品種が少ないため帯電量を細かく制
御することが困難である。2. Description of the Related Art A so-called hydrophobic metal oxide powder obtained by hydrophobizing the surface of a metal oxide powder with an organic substance is used for electrophotography, electrostatic recording, and the like.
It is widely used as an agent for improving cleaning properties and the like.
In these applications, the triboelectricity of the metal oxide powder itself with respect to iron or iron oxide as a carrier is one of the important properties, and its hydrophobicity and triboelectricity are simultaneously controlled by various treatment agents. ing. Among these, as a method of reducing negative chargeability or imparting positive chargeability, a method of treating the surface of a powder with an amine-based organic compound is generally used. However, when a low molecular weight compound such as a quaternary ammonium salt is used as the amine-based organic compound, the reproducibility of the obtained charge amount is low because of the low binding property to the surface, and the environment is particularly susceptible to moisture. Problems such as are likely to occur.
On the other hand, when treated with an amino group-substituted silane coupling agent or amino-modified polysiloxane, these treatment agents are chemically or physically firmly fixed to the surface of the metal oxide powder, so that the treatment is effectively performed. Can be obtained. However, these treating agents are relatively expensive, and since there are few commercially available varieties, it is difficult to finely control the charge amount.
【０００３】一方、ポリアルキレンイミンは安価でかつ
高分子量を有するアミン系の有機化合物であることから
上記の処理剤の問題点を改良する材料として期待され
る。しかし実際にポリアルキレンイミンのみで金属酸化
物粉体を処理した場合、ポリアルキレンイミンの金属酸
化物表面に対する親和性が低いため均一な表面処理が困
難である上、ポリアルキレンイミン自体は親水性である
ため金属酸化物粉体に疎水性を与えることはできない。
従って、得られた粉体は上記の用途に適さない。On the other hand, polyalkyleneimine is an inexpensive and amine-based organic compound having a high molecular weight, and is therefore expected to be a material for improving the above-mentioned problems of the treating agent. However, when the metal oxide powder is actually treated only with polyalkylenimine, uniform surface treatment is difficult due to the low affinity of the polyalkylenimine to the metal oxide surface, and the polyalkylenimine itself is hydrophilic. Therefore, the metal oxide powder cannot be given hydrophobicity.
Therefore, the obtained powder is not suitable for the above uses.
【０００４】[0004]
【発明の課題】本発明の目的は安価な材料であるポリア
ルキレンイミンを用いて帯電量が制御されかつ十分な疎
水性を持った金属酸化物粉体を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a metal oxide powder whose charge amount is controlled and which has sufficient hydrophobicity using polyalkylenimine which is an inexpensive material.
【０００５】[0005]
【課題解決の手段・発明の構成】発明者らは上記の問題
点を解決し、目的とする疎水性金属酸化物粉体を得るべ
く、鋭意研究を行った結果、オルガノポリシロキサンを
ポリアルキレンイミンと同時に用いて金属酸化物粉体を
表面処理することによって、帯電量が制御されかつ十分
な疎水性を有する金属酸化物粉体が得られることを見出
し、本発明の目的を達成するに至った。すなわち、オル
ガノポリシロキサンが金属酸化物粉体に高い疎水性を与
えると同時に、物理的な付着性が高いオルガノポリシロ
キサンを介してポリアルキレンイミンが金属酸化物粉体
表面に強固に結合して効果的に正の帯電性を与えると同
時に、オルガノポリシロキサンによって金属酸化物粉体
表面が疎水化され、上記の結果が得られた。The inventors of the present invention have conducted intensive studies in order to solve the above-mentioned problems and obtain a desired hydrophobic metal oxide powder. As a result, the organopolysiloxane was converted to a polyalkyleneimine. Simultaneously, the surface treatment of the metal oxide powder was used to control the charge amount, and found that a metal oxide powder having sufficient hydrophobicity was obtained, thereby achieving the object of the present invention. . That is, at the same time that the organopolysiloxane imparts high hydrophobicity to the metal oxide powder, the polyalkyleneimine is firmly bonded to the surface of the metal oxide powder via the highly adherent organopolysiloxane. At the same time, the surface of the metal oxide powder was hydrophobized by the organopolysiloxane, and the above result was obtained.
【０００６】本発明の特徴は、オルガノポリシロキサン
とポリアルキレンイミンによって処理された金属酸化物
粉体を提供することにある。また、本発明の好ましい態
様にては、上記化合物によって処理され、透過率法によ
って測定された疎水化率が６０％以上の値を示す金属酸
化物粉体、特に金属酸化物がシリカ、アルミナまたはチ
タニアである前記の金属酸化物粉体が提供される。以下
に本発明をより具体的に説明する。A feature of the present invention is to provide a metal oxide powder treated with an organopolysiloxane and a polyalkyleneimine. Further, in a preferred embodiment of the present invention, the metal oxide powder treated with the above compound and having a hydrophobicity measured by a transmittance method of 60% or more, in particular, the metal oxide is silica, alumina or The above-mentioned metal oxide powder which is titania is provided. Hereinafter, the present invention will be described more specifically.
【０００７】本発明に用いられるオルガノポリシロキサ
ンは、金属酸化物表面に十分な疎水性を与えること以外
は特に限定されないが、実用上は置換基としてメチル
基、フェニル基あるいはヒドロ基を有するものが好まし
く、さらに処理操作の面からは１０ｃｓから１０,００
０cｓ程度の粘度のものを用いることが好ましい。現在
市販の材料としては信越シリコーン社製 ＫＦ−９６、
ＫＦ−９９、ＫＦ−５６；東レ・ダウコーニング・シリ
コーン社製 ＳＨ２００、ＳＨ５１０、ＳＨ１１０７等
が例示される。本発明に用いられるポリアルキレンイミ
ンは、ポリエチレンイミン、ポリプロピレンイミン等で
工業用に一般的に用いられている（平均分子量：数百〜
十万程度である）ものでよく、実用上は３０％程度の濃
度のポリエチレンイミン水溶液を用いることが最も好ま
しい。本発明に用いられる金属酸化物粉体は、用途に応
じて選択することが可能であるが、特にシリカ、アルミ
ナまたはチタニアが流動性改良等の用途には好ましい。
粒径も用途に応じて選択することが可能であるが、特に
比表面積が５０ｍ2/ｇ以上のものが上記用途には好まし
い。なお金属酸化物は複合酸化物、混合物であってもよ
い。[0007] The organopolysiloxane used in the present invention is not particularly limited, except that it imparts sufficient hydrophobicity to the surface of the metal oxide. However, in practice, those having a methyl group, a phenyl group or a hydro group as a substituent are preferred. Preferably, from the viewpoint of processing operation, 10 cs to 10,000
It is preferable to use one having a viscosity of about 0 cs. Currently commercially available materials include KF-96 manufactured by Shin-Etsu Silicone Co., Ltd.
KF-99, KF-56; SH200, SH510, SH1107 manufactured by Dow Corning Toray Silicone Co., Ltd. are exemplified. The polyalkyleneimine used in the present invention is generally used for industrial purposes such as polyethyleneimine and polypropyleneimine (average molecular weight: several hundred to
(About 100,000), and practically, it is most preferable to use an aqueous solution of polyethyleneimine having a concentration of about 30%. The metal oxide powder used in the present invention can be selected according to the application, but silica, alumina or titania is particularly preferred for applications such as improvement in fluidity.
The particle size can be selected according to the application, but those having a specific surface area of 50 m 2 / g or more are particularly preferable for the above application. The metal oxide may be a composite oxide or a mixture.
【０００８】本発明の目的とする疎水性金属酸化物粉体
を得るために適当な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特に規定
されない。しかしポリアルキレンイミンを過剰量用いる
ことは疎水性低下の原因となるため、通常被処理金属酸
化物粉体の重量に対してポリアルキレンイミンは水を含
まない重量で２０％以下、特に好ましくは１２％以下の
量を用いることが望ましい。またオルガノポリシロキサ
ンの使用量はポリアルキレンイミンを固定化する目的か
らはポリアルキレンイミンの水を含まない重量に対して
５〜１５０％、特に好ましくは５０〜１００％の量を用
いることが望ましい。The amount of the treating agent suitable for obtaining the hydrophobic metal oxide powder intended in the present invention depends on the kind of the metal oxide powder to be treated, the specific surface area and the kind of the treating agent, and is particularly specified. Not done. However, since the use of an excessive amount of polyalkylenimine causes a decrease in hydrophobicity, the polyalkylenimine is usually 20% or less, particularly preferably 12% by weight, not containing water, based on the weight of the metal oxide powder to be treated. % Is desirably used. For the purpose of immobilizing the polyalkylenimine, it is desirable to use the organopolysiloxane in an amount of 5 to 150%, particularly preferably 50 to 100%, based on the weight of the polyalkylenimine not containing water.
【０００９】鉄に対する摩擦帯電量の測定方法は、文
献、例えば「色材」55[9]630-636.1982などに規定され
ている。透過率法は処理された金属酸化物粉体の疎水化
率を実験的に求める方法で、以下の手順からなる。処理
された金属酸化物粉体１.０ｇと水１００ｍlを抽出用分
別漏斗に入れ、５分間はげしく振盪攪拌する。その後１
分間静置し、分別漏斗の底から少量の懸濁液を抜き出
す。この液の５５０ｎｍの光に対する透過率を、純水の
透過率を１００％として表した値をその金属酸化物の疎
水化率とする。このようにして測定された疎水化率の値
が高いほど、その金属酸化物粉体の吸湿性が減少して湿
度によるトナーの帯電量の変化を小さくし、かつ凝集を
防ぐ効果が高まり、利用価値は高いが、実用上は６０％
以上、好ましくは７０％以上の値をもつことが望まし
い。A method for measuring the triboelectric charge amount with respect to iron is specified in a literature, for example, “Coloring Material” 55 [9] 630-636.1982. The transmittance method is a method of experimentally determining the hydrophobicity of the treated metal oxide powder, and comprises the following procedure. 1.0 g of the treated metal oxide powder and 100 ml of water are put into a separating funnel for extraction, and vigorously shaken and stirred for 5 minutes. Then one
Let stand for a minute and withdraw a small amount of suspension from the bottom of the separatory funnel. The value obtained by expressing the transmittance of this liquid at 550 nm light with the transmittance of pure water as 100% is defined as the hydrophobicity of the metal oxide. The higher the value of the hydrophobization ratio measured in this way, the less the hygroscopicity of the metal oxide powder, the smaller the change in the charge amount of the toner due to humidity, and the more effective it is to prevent agglomeration. High value, but practically 60%
More preferably, it is desirable to have a value of 70% or more.
【００１０】本発明に用いられる金属酸化物粉体の処理
には、従来公知の方法が適応される。すなわち、被処理
金属酸化物粉体を機械的に十分攪拌をしながら、これに
オルガノポリシロキサン、ポリアルキレンイミンを滴下
あるいは噴霧して加える。また用いるポリアルキレンイ
ミンおよびオルガノポリシロキサンの粘度に応じて、ア
ルコール、ケトンあるいは炭化水素等の溶剤を希釈剤と
して用いることも可能である。処理剤添加後、窒素気流
下で１００〜２５０℃の範囲の温度、特に好ましくは１
３０〜１７０℃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。また金属酸化物粉体の種
類によって、上記のような乾式の処理が困難な場合には
溶剤を相当量用いた湿式条件で処理することも可能であ
る。For the treatment of the metal oxide powder used in the present invention, a conventionally known method is applied. That is, an organopolysiloxane and a polyalkyleneimine are added dropwise or sprayed to the metal oxide powder to be treated while mechanically sufficiently stirring the metal oxide powder. Further, depending on the viscosity of the polyalkylenimine and the organopolysiloxane to be used, it is also possible to use a solvent such as alcohol, ketone or hydrocarbon as a diluent. After the addition of the treating agent, a temperature in the range of 100 to 250 ° C., particularly preferably 1
The reaction is completed by heating at a temperature in the range of 30 to 170 ° C., and the solvent is removed. If the above-mentioned dry treatment is difficult depending on the type of the metal oxide powder, the treatment can be carried out under wet conditions using a considerable amount of a solvent.
【００１１】[0011]
【発明の効果】本発明によって構成される疎水性金属酸
化物粉体は、オルガノポリシロキサンをポリアルキレン
イミンと併用することによって、ポリアルキレンイミン
がより強固に金属酸化物粉体表面に固定された結果、以
下の特徴を持つ。オルガノポリシロキサンを用いない場
合に比べてより高い正の帯電性が得られ、その再現性も
高い。また湿気等に対する安定性も向上した。さらに、
本発明によって得られる疎水性金属酸化物粉体は、処理
剤の使用量を変化させることによって、帯電量の制御が
可能であり、広い用途への適応が期待される。According to the hydrophobic metal oxide powder constituted by the present invention, the polyalkyleneimine is more firmly fixed on the surface of the metal oxide powder by using the organopolysiloxane in combination with the polyalkyleneimine. As a result, it has the following features. A higher positive chargeability is obtained as compared with the case where no organopolysiloxane is used, and the reproducibility is high. In addition, the stability against moisture and the like was improved. further,
The hydrophobic metal oxide powder obtained by the present invention can control the charge amount by changing the amount of the treating agent used, and is expected to be applicable to a wide range of applications.
【００１２】[0012]
【発明の具体的開示】本発明に対する理解を助ける目的
で以下に実施例および比較例を示すが、これらは本発明
をなんら限定するものではない。Specific disclosure of the present invention Examples and comparative examples are shown below for the purpose of assisting the understanding of the present invention, but they do not limit the present invention in any way.
【００１３】［実施例１］加熱乾燥したシリカ粉体（日
本アエロジル社製「アエロジル＃１３０」比表面積１３
０ｍ2/ｇ）１０ｇをステンレス鋼製の容器に仕込み、室
温で窒素雰囲気下で攪拌しながら、下記の組成の処理剤
を噴霧した。 処理剤 ポリエチレンイミン（３０％水溶液） ２.００ｇ ジメチルポリシロキサン（信越化学社製「KF-96」(50cs)） １.００ｇ ｎ−プロパノ−ル ５.０ｍl 噴霧終了後、さらに室温で５分攪拌した後、窒素気流下
で外部加熱を行った。４０分かけて１５０℃まで昇温さ
せ、この温度で６０分保持したのち、室温まで放冷し
た。同様の操作を繰り返して計５ロットの疎水性シリカ
粉体を得た。これらの粉体の透過率法による疎水化率お
よび鉄に対する摩擦帯電量の最大値と最小値は、それぞ
れ９４％、８６％と１０９μＣ／ｇ、９８μＣ／ｇであ
った。Example 1 Heat-dried silica powder ("Aerosil # 130" manufactured by Nippon Aerosil Co., Ltd., specific surface area 13
(0 m 2 / g) 10 g was charged into a stainless steel container, and a treating agent having the following composition was sprayed while stirring at room temperature under a nitrogen atmosphere. Treatment agent Polyethyleneimine (30% aqueous solution) 2.00 g Dimethylpolysiloxane ("KF-96" (50cs) manufactured by Shin-Etsu Chemical Co., Ltd.) 1.00 g n-propanol 5.0 ml After spraying, stirring is continued at room temperature for 5 minutes. After that, external heating was performed under a nitrogen stream. The temperature was raised to 150 ° C. over 40 minutes, maintained at this temperature for 60 minutes, and allowed to cool to room temperature. The same operation was repeated to obtain a total of 5 lots of hydrophobic silica powder. The maximum value and the minimum value of the hydrophobicity of these powders by the transmittance method and the triboelectric charge amount with respect to iron were 94%, 86%, 109 μC / g and 98 μC / g, respectively.
【００１４】［実施例２〜９］実施例１において、処理
剤の組成または種類を変化させた場合の結果を表１にま
とめて示す。疎水化率と摩擦帯電量は実施例１の場合と
同様に５ロット中の最大値と最小値を示した。[Examples 2 to 9] Table 1 shows the results obtained in Example 1 when the composition or type of the treating agent was changed. The hydrophobicity and the triboelectric charge showed the maximum value and the minimum value in 5 lots as in the case of Example 1.
【００１５】[0015]
【表１】 実施例１〜９ 処理剤使用量 測定値 実施例 ポリエチレ オルガノポリ 疎水化率 帯電量 ンイミン*a シロキサン （％） (μC/g） (ｇ) (ｇ) (最大値/最小値) (最大値/最小値) １ 20 10*b 94 / 86 109 / 79 ２ 10 10*b 96 / 92 71 / 54 ３ 5 10*b 96 / 91 43 / 12 ４ 2 5*b 98 / 92 -74 /-120 ５ 2 10*b 91 / 84 -194 /-250 ６ 10 10*c 96 / 92 83 / 43 ７ 20 10*c 84 / 78 138 / 95 ８ 10 5*d 81 / 70 99 / 63 ９ 20 10*d 82 / 69 94 / 77 * a ：ポリエチレンイミン３０％水溶液の重量* b ：信越シリコーン社製 ＫＦ-９６ (５０ｃｓ)* c ：信越シリコーン社製 ＫＦ-９９* d ：信越シリコーン社製 ＫＦ-５６[Table 1] Examples 1 to 9 Measured values of amount of treating agent used Example Polyethylene Organopoly Hydrophobization rate Charge amount imine * a siloxane (%) (μC / g) (g) (g) (maximum / minimum value) ( (Maximum / minimum) 1 20 10 * b 94/86 109/79 2 10 10 * b 96/92 71/54 35 10 * b 96/91 43/12 42 5 * b 98/92 -74 / -120 5 2 10 * b 91/84 -194 / -250 6 10 10 * c 96/92 83/43 7 20 10 * c 84/78 138/95 8 10 5 * d 81/70 99/63 9 20 10 * d 82/69 94/77 * a: Weight of a 30% aqueous solution of polyethyleneimine * b: KF-96 (50 cs) manufactured by Shin-Etsu Silicone * c: KF-99 manufactured by Shin-Etsu Silicone * d: KF manufactured by Shin-Etsu Silicone -56
【００１６】［比較例１］加熱乾燥したシリカ粉体（日
本アエロジル社製「アエロジル＃１３０」比表面積１３
０ｍ2/ｇ）１０ｇをステンレス鋼製の容器に仕込み、室
温で窒素雰囲気下で攪拌しながら、下記の組成の処理剤
を噴霧した。 処理剤 ポリエチレンイミン（３０％水溶液） ２.００ｇ ｎ−プロパノ−ル ５.０ｍl 噴霧終了後、さらに室温で５分攪拌した後、窒素気流下
で外部加熱を行った。４０分かけて１５０℃まで昇温さ
せ、この温度で６０分保持したのち、室温まで放冷し
た。この粉体は親水性で、鉄に対する摩擦帯電量は、２
３μＣ／ｇであった。Comparative Example 1 Heat-dried silica powder ("Aerosil # 130" manufactured by Nippon Aerosil Co., Ltd., specific surface area 13
(0 m 2 / g) 10 g was charged into a stainless steel container, and a treating agent having the following composition was sprayed while stirring at room temperature under a nitrogen atmosphere. Treatment agent Polyethyleneimine (30% aqueous solution) 2.00 g n-propanol 5.0 ml After spraying was completed, the mixture was further stirred at room temperature for 5 minutes, and then externally heated under a nitrogen stream. The temperature was raised to 150 ° C. over 40 minutes, maintained at this temperature for 60 minutes, and allowed to cool to room temperature. This powder is hydrophilic and has a triboelectric charge of 2
It was 3 μC / g.
【００１７】［実施例１０］加熱乾燥したアルミナ粉体
（日本アエロジル社製「アルミニウム・オキサイドＣ」
比表面積９０ｍ2/ｇ）１０ｇをステンレス鋼製の容器に
仕込み、室温で窒素雰囲気下で攪拌しながら、下記の組
成の処理剤を噴霧した。 処理剤 ポリエチレンイミン（３０％水溶液） ２.００ｇ ジメチルポリシロキサン（信越化学社製「KF-96」(50cs)） １.００ｇ ｎ−プロパノ−ル ５.０ｍl 噴霧終了後、さらに室温で５分攪拌した後、窒素気流下
で外部加熱を行った。４０分かけて１５０℃まで昇温さ
せ、この温度で６０分保持したのち、室温まで放冷し
た。同様の操作を繰り返して計５ロットの疎水性アルミ
ナ粉体を得た。これらの粉体の透過率法による疎水化率
および鉄に対する摩擦帯電量の最大値と最小値は、それ
ぞれ８２％、６３％と９９μＣ／ｇ、４２μＣ／ｇであ
った。Example 10 Heat-dried alumina powder ("Aluminum oxide C" manufactured by Nippon Aerosil Co., Ltd.)
10 g of a specific surface area (90 m 2 / g) was charged into a stainless steel container, and a treating agent having the following composition was sprayed while stirring at room temperature under a nitrogen atmosphere. Treatment agent Polyethyleneimine (30% aqueous solution) 2.00 g Dimethylpolysiloxane ("KF-96" (50cs) manufactured by Shin-Etsu Chemical Co., Ltd.) 1.00 g n-propanol 5.0 ml After spraying, stirring is continued at room temperature for 5 minutes. After that, external heating was performed under a nitrogen stream. The temperature was raised to 150 ° C. over 40 minutes, maintained at this temperature for 60 minutes, and allowed to cool to room temperature. The same operation was repeated to obtain a total of 5 lots of hydrophobic alumina powder. The maximum value and the minimum value of the hydrophobicity of these powders by the transmittance method and the triboelectric charge amount with respect to iron were 82%, 63%, 99 μC / g and 42 μC / g, respectively.
【００１８】［実施例１２］加熱乾燥したチタニア粉体
（日本アエロジル社製「チタニウム・オキサイドＰ２
５」比表面積８０ｍ2/ｇ）１０ｇをステンレス鋼製の容
器に仕込み、室温で窒素雰囲気下で攪拌しながら、下記
の組成の処理剤を噴霧した。 処理剤 ポリエチレンイミン（３０％水溶液） ２.００ｇ ジメチルポリシロキサン（信越化学社製「KF-96」(50cs)） １.００ｇ アセトン ５.０ｍl 噴霧終了後、さらに室温で５分攪拌した後、窒素気流下
で外部加熱を行った。４０分かけて１５０℃まで昇温さ
せ、この温度で６０分保持したのち、室温まで放冷し
た。同様の操作を繰り返して計５ロットの疎水性チタニ
ア粉体を得た。これらの粉体の透過率法による疎水化率
および鉄に対する摩擦帯電量の最大値と最小値は、それ
ぞれ７０％、６３％と５４μＣ／ｇ、２３μＣ／ｇであ
った。Example 12 Heat-dried titania powder ("Titanium oxide P2" manufactured by Nippon Aerosil Co., Ltd.)
5 "10 g of a specific surface area of 80 m 2 / g) was charged into a stainless steel container, and a treating agent having the following composition was sprayed while stirring at room temperature under a nitrogen atmosphere. Treatment agent Polyethyleneimine (30% aqueous solution) 2.00 g Dimethylpolysiloxane ("KF-96" (50cs) manufactured by Shin-Etsu Chemical Co., Ltd.) 1.00 g Acetone 5.0 ml External heating was performed under air flow. The temperature was raised to 150 ° C. over 40 minutes, maintained at this temperature for 60 minutes, and allowed to cool to room temperature. The same operation was repeated to obtain a total of 5 lots of hydrophobic titania powder. The maximum value and the minimum value of the hydrophobicity of these powders by the transmittance method and the triboelectric charge amount with respect to iron were 70%, 63%, 54 μC / g and 23 μC / g, respectively.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ Ｃ０９Ｃ 3/10 Ｃ０９Ｃ 3/10 Ｇ０３Ｇ 9/08 ３７４ Ｇ０３Ｇ 9/08 ３７４ (56)参考文献 特開 昭54−101795（ＪＰ，Ａ) 特開 平３−126601（ＪＰ，Ａ) 特開 平３−163172（ＪＰ，Ａ) 特開 平６−80406（ＪＰ，Ａ) 特開 平２−308173（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C01B 13/14 C01B 33/18 C01F 7/02 C01G 23/04 G03G 9/08 374 B01J 2/00 C09C 3/10 ＣＡ（ＳＴＮ)──────────────────────────────────────────────────の Continuation of the front page (51) Int.Cl. 7 Identification symbol FI C09C 3/10 C09C 3/10 G03G 9/08 374 G03G 9/08 374 (56) References JP-A-54-101795 (JP, A) JP-A-3-126601 (JP, A) JP-A-3-163172 (JP, A) JP-A-6-80406 (JP, A) JP-A-2-308173 (JP, A) (58) Survey Field (Int.Cl. 7 , DB name) C01B 13/14 C01B 33/18 C01F 7/02 C01G 23/04 G03G 9/08 374 B01J 2/00 C09C 3/10 CA (STN)
Claims (3)
ンイミンの被覆を有する金属酸化物粉体。1. A metal oxide powder having a coating of an organopolysiloxane and a polyalkylenimine.
６０％以上の値を示す請求項１に記載の金属酸化物粉
体。2. The metal oxide powder according to claim 1, which has a hydrophobicity measured by a transmittance method of 60% or more.
タニアである請求項１に記載の金属酸化物粉体。3. The metal oxide powder according to claim 1, wherein the metal oxide is silica, alumina or titania.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25571292A JP3146678B2 (en) | 1992-08-31 | 1992-08-31 | Hydrophobic metal oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25571292A JP3146678B2 (en) | 1992-08-31 | 1992-08-31 | Hydrophobic metal oxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0680405A JPH0680405A (en) | 1994-03-22 |
| JP3146678B2 true JP3146678B2 (en) | 2001-03-19 |
Family
ID=17282598
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25571292A Expired - Lifetime JP3146678B2 (en) | 1992-08-31 | 1992-08-31 | Hydrophobic metal oxide powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3146678B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101384679B (en) * | 2006-02-14 | 2011-11-02 | 宝洁公司 | Responsive coated particles |
| CN103003156B (en) | 2010-05-18 | 2015-09-16 | 洲际大品牌有限责任公司 | The flexible package of Reclosable and manufacture method thereof |
-
1992
- 1992-08-31 JP JP25571292A patent/JP3146678B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0680405A (en) | 1994-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5843525A (en) | Surface-modified metal oxide fine particles and process for producing the same | |
| US4902570A (en) | Process for preparing highly dispersed metal oxides whose surfaces are modified by an ammonium-functional organopolysiloxane as a positive chargeable controlling agent for toners | |
| JP4118637B2 (en) | Silica with low silanol group content | |
| JPH0131442B2 (en) | ||
| JPH06227810A (en) | Hydrophobic silica powder, its production and electrophotographic developer | |
| EP0949302B1 (en) | Fine powder of hydrophobic titanium oxide, and method for producing it | |
| JP2006096641A (en) | Modified hydrophobized silica and method of manufacturing the same | |
| EP0799791B1 (en) | Hydrophobic metal oxide powder and use thereof | |
| JP4743845B2 (en) | Hydrophobic positively charged silica fine powder, method for producing the same, and toner for developing electrostatic latent image to which it is added as an external additive | |
| JP2016006547A (en) | Toner composition and method of preparing the same | |
| JP3146679B2 (en) | Hydrophobic metal oxide powder | |
| JP3146678B2 (en) | Hydrophobic metal oxide powder | |
| JP4304661B2 (en) | Method for producing fluorine-containing surface-modified alumina powder and use thereof | |
| JP2014162681A (en) | Surface-treated silica powder and method for manufacturing the same | |
| JP3344204B2 (en) | Hydrophobic metal oxide powder and its use | |
| JP3344133B2 (en) | Hydrophobic metal oxide powder and electrophotographic developer containing the same | |
| JPH0132161B2 (en) | ||
| JPS63101855A (en) | Electrostatic charge image developer | |
| JP4186254B2 (en) | Method for producing surface-modified metal oxide fine powder and method for producing electrophotographic toner composition | |
| JP2946896B2 (en) | Hydrophobic alumina | |
| JPH0683099A (en) | Electrophotographic developer | |
| JPH0683098A (en) | Electrophotographic developer | |
| JP3965496B2 (en) | Electrophotographic developer | |
| JP4122566B2 (en) | Hydrophobic metal oxide fine powder, production method thereof, and toner composition for electrophotography | |
| JPH0431312A (en) | Hydrophobic alumina |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20001205 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080112 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090112 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090112 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100112 Year of fee payment: 9 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100112 Year of fee payment: 9 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100112 Year of fee payment: 9 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110112 Year of fee payment: 10 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120112 Year of fee payment: 11 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130112 Year of fee payment: 12 |
|
| EXPY | Cancellation because of completion of term | ||
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130112 Year of fee payment: 12 |