JP2567480B2 - Batch-type wet dispersion device and method for dispersing electrophotographic photoreceptor coating liquid using the same - Google Patents
Batch-type wet dispersion device and method for dispersing electrophotographic photoreceptor coating liquid using the sameInfo
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- JP2567480B2 JP2567480B2 JP1277168A JP27716889A JP2567480B2 JP 2567480 B2 JP2567480 B2 JP 2567480B2 JP 1277168 A JP1277168 A JP 1277168A JP 27716889 A JP27716889 A JP 27716889A JP 2567480 B2 JP2567480 B2 JP 2567480B2
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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はバッチ式湿式分散装置、詳しくは円筒状ベッ
セル内でデイスクまたはドラムなどの回転分散手段を回
転させることにより被分散液を湿式で分散するタテ型の
バッチ式湿式分散装置及びその装置を用いた電子写真感
光体塗工液の分散方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention relates to a batch type wet dispersion device, more specifically, a liquid to be dispersed is wet-dispersed by rotating a rotary dispersion means such as a disk or a drum in a cylindrical vessel. The present invention relates to a vertical type batch type wet dispersion device and a method for dispersing an electrophotographic photoreceptor coating liquid using the device.
これまで、顔料、染料等の固体を分散する分散装置と
してロールミル、ボールミル、振動ボールミル、アトラ
イター、コロイドミルなど各種いろいろな形状のものが
考えられている。Heretofore, various types of devices such as roll mills, ball mills, vibrating ball mills, attritors and colloid mills have been considered as dispersing devices for dispersing solids such as pigments and dyes.
しかしながら、近年微細化の要求が一段と高く求めら
れるようになり、それに対応して分散装置の改良がなさ
れてきている。However, in recent years, the demand for miniaturization has become much higher, and the dispersion apparatus has been improved accordingly.
顔料、染料等を微細化する有効な手段としてはベッセ
ル内部にガラスビーズ等のメジウムを入れ、回転分散手
段であるデイスクまたはドラムを回転させて微分散する
いわゆるサンドミル分散装置を用いる方法がある。サン
ドミルを用いて顔料等を分散する場合、被分散液を循環
する機構を有する連続式分散方法と、この機構をもたな
いバッチ式分散方法とがある。連続式分散方法の場合、
ベッセル内総てに分散液が充填されるため、分散効率が
良くなるという長所をもつが、循環を行うため、ポンプ
部、配管部、又装置によっては液だめ部が必要となり、
被分散液の総量が多量に必要な上、実際に分散される時
間、すなわちベッセル内に滞留する時間が短いという欠
点がある。また粘性があがるような被分散液の場合、ベ
ッセル内でバイパス現象（被分散液をベッセル内の下か
ら上へ循環している際に、被分散液の粘度の低い部分に
圧力が集中して、不十分な分散のままで被分散液が上へ
抜ける現象）が生じ、分散する所と分散しない所ができ
る可能性が高く、均一な分散は難しい。An effective means for making pigments, dyes, etc. finer is to use a so-called sand mill dispersing device in which a medium such as glass beads is put in a vessel and finely dispersed by rotating a disc or a drum as a rotating dispersing means. When a pigment or the like is dispersed using a sand mill, there are a continuous dispersion method having a mechanism for circulating a liquid to be dispersed and a batch dispersion method having no mechanism. In case of continuous dispersion method,
Since all of the vessel is filled with the dispersion liquid, it has the advantage of improving the dispersion efficiency, but since it circulates, it requires a pump section, a piping section, and depending on the device, a liquid sump section,
There is a drawback that the total amount of the liquid to be dispersed is required to be large and the time for actual dispersion, that is, the time for staying in the vessel is short. Also, in the case of a liquid to be dispersed that increases in viscosity, a bypass phenomenon in the vessel (when the liquid to be dispersed is circulated from the bottom to the top of the vessel, the pressure concentrates on the low viscosity part of the liquid to be dispersed. However, there is a high possibility that the liquid to be dispersed will escape upwards with insufficient dispersion), and there will be a place where the liquid is dispersed and a place where the liquid is not dispersed, and uniform dispersion is difficult.
これに対し、バッチ式分散方法では、パイパス現象が
起きるようなことはなく、またベッセル内の滞留時間が
短くなるということもない。しかしながら、バッチ式の
場合には、ベッセル内での被分散液の上下循環が行われ
にくく、又、ベッセル内部でのガラスビーズ等のメジウ
ムの運動エネルギー及び方向がベッセルの上部と下部と
では異なっていることと相まって被分散液全体を均一に
分散することは難しい。とりわけ電子写真感光体塗工液
を分散する場合には、所望の電子写真特性を得るために
は顔料等の粒径、結晶型の制御が重要であり、被分散液
全体を均一に分散することが強く望まれている。On the other hand, in the batch type dispersion method, the bypass phenomenon does not occur, and the residence time in the vessel does not become short. However, in the case of the batch type, it is difficult to vertically circulate the liquid to be dispersed in the vessel, and the kinetic energy and direction of the medium such as glass beads inside the vessel are different between the upper portion and the lower portion of the vessel. It is difficult to uniformly disperse the whole liquid to be dispersed in combination with the above. In particular, when the electrophotographic photoreceptor coating liquid is dispersed, it is important to control the particle size and crystal form of the pigment in order to obtain desired electrophotographic characteristics. Is strongly desired.
本発明の目的は、上述のような欠点と除去したバッチ
式湿式分散装置であって、均一で安定した微細粒子にま
で短時間で効率良く分散することができる分散装置を提
供することである。It is an object of the present invention to provide a batch type wet dispersion device which eliminates the above-mentioned drawbacks and which can efficiently disperse into uniform and stable fine particles in a short time.
また、本発明の目的は、塗膜欠陥をもたらさず、粒径
の小さい分散液を形成することができるバッチ式湿式分
散装置を提供することである。It is also an object of the present invention to provide a batch type wet dispersion device which does not cause coating film defects and can form a dispersion having a small particle size.
また、本発明の目的は、画像欠陥の生じない感光層を
形成することができる電子写真感光体塗工液のバッチ式
湿式分散方法を提供することである。It is another object of the present invention to provide a batch type wet dispersion method of an electrophotographic photoreceptor coating liquid capable of forming a photosensitive layer without image defects.
本発明のバッチ式湿式分散装置は、円筒状ベッセル内
に回転分散手段を有するバッチ式湿式分散装置におい
て、該ベッセルの内壁側面に沿ってらせん状の溝が設け
られていることを特徴とし、好ましくは、前記のらせん
状の溝が、該溝に沿ってベッセルの下方から上方に進む
際の回転方向と前記の回転分散手段の回転方向とが同一
になるように前記のベッセルの内壁側面に沿って設けら
れていることを特徴とする。The batch type wet dispersion device of the present invention is a batch type wet dispersion device having a rotation dispersion means in a cylindrical vessel, characterized in that a spiral groove is provided along the inner wall side surface of the vessel, and preferably Along the inner wall side surface of the vessel so that the spiral groove has the same rotation direction as the spiral dispersion groove advances from the lower side to the upper side of the vessel along the groove. It is characterized by being provided.
また、本発明の電子写真感光体塗工液の分散方法は、
円筒状ベッセル内で回転分散手段を回転させて、顔料又
は染料を含有する電子写真感光体塗工液を分散させる方
法において、該円筒状ベッセルとして該ベッセルの内壁
側面に沿ってらせん状の溝が設けられているベッセルを
用い、該回転分散手段を回転させて該ベッセル内の電子
写真感光体塗工液を分散させることを特徴とし、好まし
くは、前記の回転分散手段の回転方向を、前記の溝に沿
ってベッセルの下方から上方に進む際の回転方向と同一
にすることを特徴とする。Further, the dispersion method of the electrophotographic photoreceptor coating liquid of the present invention,
By rotating the rotating dispersion means in the cylindrical vessel to disperse the electrophotographic photoreceptor coating liquid containing the pigment or dye, a spiral groove is formed along the inner wall side surface of the vessel as the cylindrical vessel. Using the vessel provided, characterized in that the rotation dispersion means is rotated to disperse the electrophotographic photoreceptor coating liquid in the vessel, preferably, the rotation direction of the rotation dispersion means, It is characterized in that the direction of rotation is the same as when traveling upward from below the vessel along the groove.
以下、図面を参照しながら本発明を説明する。 Hereinafter, the present invention will be described with reference to the drawings.
第１図及び第２図は本発明のバッチ式湿式分散装置の
それぞれ異なる具体例を示す断面図である。装置の基本
構成は円筒状ベッセル１とディスク３と該ベッセル１の
内壁側面に沿って設けられたらせん状の溝７より構成さ
れている。具体的には、ジャケット２で囲われた円筒状
ベッセル１内に、ディスク３を有するシャフト５が配置
されており、駆動装置４からの回転駆動はシャフト５を
介してディスク３に伝わり、このディスク３の回転運動
により、被分散液が攪拌され、この際に該らせん状の溝
の存在により一層良好に分散される。尚、円筒状ベッセ
ル１の上部には上ブタ６が設けられている。1 and 2 are cross-sectional views showing different specific examples of the batch type wet dispersion device of the present invention. The basic structure of the apparatus is composed of a cylindrical vessel 1, a disk 3, and a spiral groove 7 provided along the inner wall side surface of the vessel 1. Specifically, a shaft 5 having a disk 3 is arranged in a cylindrical vessel 1 surrounded by a jacket 2, and rotational drive from a drive device 4 is transmitted to the disk 3 via the shaft 5, By the rotary motion of 3, the liquid to be dispersed is stirred, and at this time, it is better dispersed due to the presence of the spiral groove. An upper lid 6 is provided on top of the cylindrical vessel 1.
本発明においては、円筒状ベッセル１の内壁側面にら
せん状の溝７が設けられている。該らせん状の溝７は第
１図に示すように円筒状ベッセル１の内壁を加工して設
けてあっても、又、第２図に示すように円筒状ベッセル
内にらせん状部材８を挿入することによって設けてもよ
い。In the present invention, the spiral groove 7 is provided on the side surface of the inner wall of the cylindrical vessel 1. The spiral groove 7 may be provided by processing the inner wall of the cylindrical vessel 1 as shown in FIG. 1, or the spiral member 8 may be inserted into the cylindrical vessel as shown in FIG. You may provide by doing.
又、円筒状ベッセル内に設けるらせん状の溝を、該溝
に沿ってベッセルの下方から上方に進む際の回転方向と
前記の回転分散手段の回転方向とが同一になるように該
ベッセルの内壁側面に沿って設けると、被分散液の上下
循環も生じることにより被分散液の攪拌、分散が一層効
果的となる。Further, the spiral groove provided in the cylindrical vessel is provided with an inner wall of the vessel so that the rotation direction when going upward from the bottom of the vessel along the groove is the same as the rotation direction of the rotation dispersion means. When it is provided along the side surface, the liquid to be dispersed is vertically circulated, so that the stirring and dispersion of the liquid to be dispersed becomes more effective.
回転分散手段の回転平面と、円筒状ベッセル内壁に設
けられたらせん状の溝とのなす角度は、回転分散手段の
回転数、被分散液の粘度、回転分散手段の径、円筒状ベ
ッセルの内径等により適宜選択されるが、好ましくは５
゜〜45゜、より好ましくは10゜〜30゜、最適には10゜〜
15゜に設定することが望ましい。５゜未満では上下循環
の効果が充分ではなく、また45゜を越えるとらせん状の
溝が抵抗板として働き始めるため、被分散液の電子写真
特性の制御が難しくなる。The angle formed by the rotation plane of the rotation dispersion means and the spiral groove provided on the inner wall of the cylindrical vessel is the number of rotations of the rotation dispersion means, the viscosity of the liquid to be dispersed, the diameter of the rotation dispersion means, the inner diameter of the cylindrical vessel. Etc., but it is preferably 5
° ~ 45 °, more preferably 10 ° ~ 30 °, optimally 10 ° ~
It is desirable to set it at 15 °. If it is less than 5 °, the effect of vertical circulation is not sufficient, and if it exceeds 45 °, the spiral groove begins to function as a resistance plate, so that it becomes difficult to control the electrophotographic characteristics of the liquid to be dispersed.
回転分散手段としては、第１図及び第２図に示したよ
うなデイスクだけでなく、ドラムを用いることも可能で
あり、ドラム、デイスクまたはベッセル内部にピンを設
けてもよい。As the rotation dispersion means, not only the disk as shown in FIGS. 1 and 2 but also a drum can be used, and pins may be provided inside the drum, the disk or the vessel.
この様な分散装置を用いて顔料、染料等を分散するこ
とによって顔料、染料を短時間で均一な分散液とするこ
とが可能である。特に微細な分散粒径が要求される電子
写真感光体塗工液に含有される顔料、染料などの電荷発
生物質の分散に対して有効な手段となる。By dispersing the pigment, the dye, etc. using such a dispersing device, it is possible to make the pigment, the dye into a uniform dispersion liquid in a short time. In particular, it is an effective means for dispersing charge generating substances such as pigments and dyes contained in the electrophotographic photoreceptor coating liquid, which requires a fine dispersed particle size.
本発明で分散できる顔料、染料は無機物、有機物のい
ずれでも良く、例えば、アゾ顔料、フタロシアニン系顔
料、アントアントロン顔料、ジベンズピレンキノン顔
料、ピラントロン顔料、インジゴ顔料、キナクリドン系
顔料、非対称キノシアニン、キノシアニン・ピリリウム
系染料、金属酸化物等が挙げられる。以下にその一例を
示す。本発明は以下の物質以外のものを分散する場合で
も極めて有効であり、以下の物質によって本発明に用い
る被分散物質が制限されるものではない。Pigments and dyes that can be dispersed in the present invention may be any of inorganic and organic substances, for example, azo pigments, phthalocyanine pigments, anthanthrone pigments, dibenzpyrenequinone pigments, pyranthrone pigments, indigo pigments, quinacridone pigments, asymmetric quinocyanines, quinocyanines. -Pyrylium dyes, metal oxides and the like can be mentioned. An example is shown below. The present invention is extremely effective even when dispersing substances other than the following substances, and the substances to be dispersed used in the present invention are not limited by the following substances.
（１）酸化亜鉛 （２）酸化チタン （３）酸化スズ （４）硫化カドミウム （27）スクエアリック酸メチン染料 （28）インジゴ染料（C.I.No.78000） （29）β−型銅フタロシアニン （41）ｔ型メタルフリーフタロシアニン （42）チタニルフタロシアニン これらの顔料、染料を適当な有機溶剤、例えばテトラ
ヒドロフラン、シクロヘキサノン、メチルエチルケト
ン、酢酸エチル、メタノール、メチルセロソルブ、アセ
トン、ジオキオサン、N,N−ジメチルホルムアミドなど
を分散媒として被分散液に調製する。この時に結着剤と
して高分子物質を一緒に加えても良いし、顔料等と分散
媒だけであらかじめ分散した後、結着剤を加えても良
い。結着剤としては広範な絶縁性樹脂から選択でき、ま
たポリ−Ｎ−ビニルカルバゾール、ポリビニルアントラ
センやポリビニルピレンなどの有機光導電性ポリマーか
らも選択できる。好ましくは、ポリビニルブチラール、
ポリアリレート（ビスフエノールＡとフタル酸の縮重合
体など）、ポリカーボネート、ポリエステル、フエノキ
シ樹脂、ポリ酢酸ビニル、アクリル樹脂、ポリアクリル
アミド樹脂、ポリアミド、ポリビニルピリジン、セルロ
ース系樹脂、ウレタン樹脂、エポキシ樹脂、カゼイン、
ポリビニルアルコール、ポリビニルピロリドンなどの絶
縁性樹脂を挙げることができる。(1) Zinc oxide (2) Titanium oxide (3) Tin oxide (4) Cadmium sulfide (27) Squaric acid methine dye (28) Indigo dye (CINo.78000) (29) β-type copper phthalocyanine (41) t-type metal-free phthalocyanine (42) titanyl phthalocyanine These pigments and dyes can be mixed with suitable organic solvents such as tetrahydrofuran, cyclohexanone, methyl ethyl ketone, ethyl acetate, methanol, methyl cellosolve, acetone, dioxoane, N, N-dimethylformamide, etc. Is used as a dispersion medium to prepare a liquid to be dispersed. At this time, a polymer substance may be added together as a binder, or the binder may be added after previously dispersing only with a pigment or the like and a dispersion medium. The binder can be selected from a wide range of insulating resins, and can also be selected from organic photoconductive polymers such as poly-N-vinylcarbazole, polyvinylanthracene and polyvinylpyrene. Preferably, polyvinyl butyral,
Polyarylate (condensation polymer of bisphenol A and phthalic acid, etc.), polycarbonate, polyester, phenoxy resin, polyvinyl acetate, acrylic resin, polyacrylamide resin, polyamide, polyvinyl pyridine, cellulose resin, urethane resin, epoxy resin, casein ,
Insulating resins such as polyvinyl alcohol and polyvinyl pyrrolidone can be used.
分散媒に対する顔料または染料および結着剤を含めた
固型分の割合は重量％で0.5〜80％程度であれば良い。
特に電子写真感光体の電荷発生物質を分散する時は３〜
15％が好ましい。結着剤の量はその分散する顔料等によ
って適当量選ぶことができる。The ratio of the solid component including the pigment or dye and the binder to the dispersion medium may be about 0.5 to 80% by weight.
Especially when the charge generating substance of the electrophotographic photosensitive member is dispersed,
15% is preferred. The amount of the binder can be selected in an appropriate amount depending on the dispersed pigment and the like.
実施例１〜10 第１図に示した分散装置を用いて、10種類の顔料を分
散した。それぞれの分散条件を第１表に示す。第１表中
の顔料No.は前記した顔料番号である。なお、結着剤は
分散開始時より投入した。Examples 1 to 10 Ten kinds of pigments were dispersed using the dispersing device shown in FIG. Table 1 shows the respective dispersion conditions. Pigment No. in Table 1 is the above-mentioned pigment number. The binder was added from the start of dispersion.
この分散装置の円筒状ベッセルは内径78mmの円筒状容
器の内壁側面に幅6mm,深さ6mmの溝を、該溝に沿ってベ
ッセルの下方から上方に進む際の回転方向とディスクの
回転方向とが同一になるように、且つらせん状の溝とデ
ィスクの回転平面とのなす角度が15゜となるようにらせ
ん状に設けたものであった。また、デイスクの枚数は４
枚であり、デイスクの下側には高さ10mm、直径8mmのピ
ンを４本取り付けた。分散時にメジウムとしてガラスビ
ーズ（東芝バロテイーニ社製GB−201M）を用い、ビーズ
と被分散液との容積比を1:1とした。The cylindrical vessel of this dispersion device has a groove having a width of 6 mm and a depth of 6 mm on the side surface of the inner wall of a cylindrical container having an inner diameter of 78 mm, and the rotation direction and the rotation direction of the disk when advancing upward from below the vessel along the groove. And the spiral groove and the plane of rotation of the disk make an angle of 15 °. The number of disks is 4
Four pins with a height of 10 mm and a diameter of 8 mm were attached to the lower side of the disk. At the time of dispersion, glass beads (GB-201M manufactured by Toshiba Balottini Co., Ltd.) were used as a medium, and the volume ratio of the beads to the liquid to be dispersed was set to 1: 1.
実施例１〜10における分散上がりの粒径及び標準偏差
は第２表に示す通りであった。 The particle size and standard deviation after dispersion in Examples 1 to 10 are as shown in Table 2.
なお、粒径の測定は液相沈降法を基本原理とした堀場
製作所遠心式粒度分布測定装置（CAPA700）を使用して
平均粒径の値を用いた。The particle size was measured by using a centrifugal particle size distribution analyzer (CAPA700) manufactured by Horiba Ltd., which uses the liquid phase sedimentation method as a basic principle, and the average particle size was used.
比較例１〜10 比較例としてらせん状の溝のないベッセルを用い、第
１表と同じ条件で分散を行った。比較例１〜10の分散上
がりの平均粒径及び標準偏差は第３表に示す通りであっ
た。 Comparative Examples 1 to 10 As a comparative example, a vessel without a spiral groove was used, and dispersion was performed under the same conditions as in Table 1. The average particle size and standard deviation after dispersion in Comparative Examples 1 to 10 are as shown in Table 3.
実施例１〜10及び比較例１〜10の結果からも明らかな
ように、らせん状の溝を設けたベッセルを用いた場合に
は、被分散液中の顔料が細かく分散されており、粒径の
分布巾もせまく、均一性が高い。 As is clear from the results of Examples 1 to 10 and Comparative Examples 1 to 10, when the vessel provided with the spiral groove was used, the pigment in the liquid to be dispersed was finely dispersed, and the particle size was The distribution width is narrow and the uniformity is high.
一方、らせん状の溝のないベッセルを用いた比較例１
〜10ではらせん状の溝を設けたベッセルを使用したもの
に比べて、いずれも分散上がりの平均粒径が大きく、実
施例と同じ分散時間では分散が不十分であった。また、
粒径の分布巾も広く、分散が不均一であることが判る。On the other hand, Comparative Example 1 using a vessel without spiral grooves
In each of Examples 10 to 10, the average particle size after dispersion was large as compared with the case where the vessel provided with the spiral groove was used, and the dispersion was insufficient at the same dispersion time as in the examples. Also,
It can be seen that the particle size distribution is wide and the dispersion is not uniform.
更に、実施例１〜10であげた被分散液のうち、実施例
２のものをシクロヘキサノン／メチルエチルケトン＝1/
1（重量比）の混合溶媒を用いて２重量％の液に希釈調
製し、ワイヤーバーを用いて50μｍ厚のアルミシートに
塗布した。また、同様にして実施例3,4,6,7及び８のも
のをテトラヒドロフラン溶媒で、実施例９のものを酢酸
ブチルで、実施例10のものをメチルエチルケトンで、各
々２重量％の液に調製し、50μｍ厚のアルミシートに塗
布した。これらの塗膜を観察したところ、ブツ，ポチの
ないきれいな塗膜が得られた。Furthermore, among the liquids to be dispersed listed in Examples 1 to 10, cyclohexanone / methyl ethyl ketone = 1 /
A 1% (weight ratio) mixed solvent was used to dilute and prepare a 2% by weight liquid, which was applied to a 50 μm thick aluminum sheet using a wire bar. Similarly, the solutions of Examples 3, 4, 6, 7 and 8 were prepared with a tetrahydrofuran solvent, the composition of Example 9 with butyl acetate, and the composition of Example 10 with methyl ethyl ketone to prepare 2% by weight liquids. And applied to a 50 μm thick aluminum sheet. When these coating films were observed, a clean coating film free of spots and spots was obtained.
また、比較例3,4,6,7,8,9および10を前記と同様にし
て２重量％の液に希釈調製してアルミシートに塗布した
ところ、比較例3,6,7,8,9および10は目視において、塗
膜上に凝集物よりなるポチが観察された。Further, Comparative Examples 3, 4, 6, 7, 8, 9, and 10 were diluted and prepared in the same manner as described above in a 2% by weight liquid and applied to an aluminum sheet. In Nos. 9 and 10, spots consisting of aggregates were visually observed on the coating film.
以上のようにらせん状の溝を設けたベッセルを使用し
た分散装置を用いて分散することにより短時間で均一で
小さな粒径の被分散液を得ることができる。As described above, by dispersing using a dispersing device using a vessel provided with a spiral groove, a liquid to be dispersed having a uniform and small particle size can be obtained in a short time.
比較例11 分散時間を44時間とした以外は比較例１と同様にして
分散を行った。Comparative Example 11 Dispersion was performed in the same manner as Comparative Example 1 except that the dispersion time was 44 hours.
比較例12 分散時間を85時間とした以外は比較例８と同様にして
分散を行った。Comparative Example 12 Dispersion was performed in the same manner as Comparative Example 8 except that the dispersion time was 85 hours.
以上の比較例11及び12の分散上がりの平均粒径及び標
準偏差は第４表に示す通りであった。The average particle size and standard deviation of the dispersions of Comparative Examples 11 and 12 are as shown in Table 4.
実施例１及び８並びに比較例11及び12の結果から明ら
かなように、らせん状の溝を設けたベッセルを使用して
分散を行った方が平均粒径が同じ程度であっても、粒度
分布がせまく、均一な分散液を得ることができる。 As is clear from the results of Examples 1 and 8 and Comparative Examples 11 and 12, even if the average particle size is about the same when the dispersion is performed using a vessel provided with a spiral groove, the particle size distribution As a result, a uniform dispersion can be obtained.
比較例13 らせん状の溝が該溝に沿ってベッセルの下方から上方
に進む際の回転方向とディスクの回転方向とが逆方向と
なるように設けられている以外は実施例１〜10で用いた
分散装置と同様のベッセルを用い、それ以外は実施例１
と同様にして分散を行った。Comparative Example 13 Used in Examples 1 to 10 except that the spiral groove is provided so that the rotation direction when traveling upward from the bottom of the vessel along the groove and the rotation direction of the disk are opposite directions. The same vessel as that used for the dispersing device was used, and other than that, Example 1
Dispersion was performed in the same manner as in.
比較例14 らせん状の溝が該溝に沿ってベッセルの下方から上方
に進む際の回転方向とディスクの回転方向とが逆方向と
なるように設けられている以外は実施例１〜10で用いた
分散装置と同様のベッセルを用い、それ以外は実施例８
と同様にして分散を行った。Comparative Example 14 Used in Examples 1 to 10 except that the spiral groove is provided so that the rotation direction when traveling upward from the bottom of the vessel along the groove and the rotation direction of the disk are opposite directions. A vessel similar to that used for the dispersing device was used, and otherwise, Example 8 was used.
Dispersion was performed in the same manner as in.
以上の比較例14および15の分散上がりの平均粒径及び
標準偏差は第５表に示す通りであった。The average particle size and standard deviation after dispersion in Comparative Examples 14 and 15 are shown in Table 5.
実施例１及び８並びに比較例13及び14の結果から明ら
かなように、らせん状の溝が該溝に沿ってベッセルの下
方から上方に進む際の回転方向と回転分散手段の回転方
向が同一となるように設けられているベッセルを使用し
て分散を行った方が、平均粒径が同じ程度であっても、
粒度分布がせまく、均一な分散液を得ることができる。 As is clear from the results of Examples 1 and 8 and Comparative Examples 13 and 14, the direction of rotation of the spiral groove when traveling from the lower side of the vessel to the upper side along the groove is the same as that of the rotation dispersion means. It is better to disperse using a vessel provided so that even if the average particle size is about the same,
The particle size distribution is narrow and a uniform dispersion can be obtained.
実施例11 １μｍ厚の６−ナイロン下引き処理をした80φ×360m
mのアルミシリンダー上に、電子写真感光体用塗工液と
して実施例２で形成した分散液を浸漬法にて塗布し、10
0℃で10分間乾燥して0.9μｍ厚の電荷発生層を形成し
た。Example 11 1- [mu] m-thick 6-nylon 80 [deg.] X 360 m under-treated
The dispersion liquid formed in Example 2 was applied as a coating liquid for an electrophotographic photosensitive member onto an aluminum cylinder of m by a dipping method,
It was dried at 0 ° C. for 10 minutes to form a 0.9 μm thick charge generation layer.
次に構造式 のヒドラゾン化合物10部及びスチレン−アクリン樹脂
（MS−200,新日鉄化学製）10部をモノクロルベンゼン80
部に溶解し、この溶液を電荷発生層の上に浸漬法によっ
て塗布し、100℃で熱風乾燥させて19μｍ厚の電荷輸送
層を形成して電子写真感光体を製造した。Next is the structural formula 10 parts of hydrazone compound and 10 parts of styrene-acrine resin (MS-200, manufactured by Nippon Steel Chemical Co., Ltd.) with monochlorobenzene 80
Part, and this solution was applied onto the charge generation layer by a dipping method and dried with hot air at 100 ° C. to form a 19 μm-thick charge transport layer to produce an electrophotographic photoreceptor.
比較例15 比較例２で形成された分散液を電子写真感光体用塗工
液として用いる以外は実施例11と同様にして電子写真感
光体を製造した。ただし、この場合電荷発生層形成時
に、目視により塗布ムラが認められた。また塗膜端部に
は粒子凝集によるダレが認められた。Comparative Example 15 An electrophotographic photosensitive member was produced in the same manner as in Example 11 except that the dispersion liquid formed in Comparative Example 2 was used as a coating liquid for electrophotographic photosensitive member. However, in this case, coating unevenness was visually observed when the charge generation layer was formed. Also, dripping due to particle aggregation was observed at the end of the coating film.
このようにして製造した実施例11及び比較例15の電子
写真感光体を、−5.6kVコロナ帯電、画像露光、トナー
現象、普通紙へのトナー転写、ウレタンゴムブレードに
よるクリーニング工程を有する電子写真複写機に取り付
けてコピーを行った。The electrophotographic photoconductors of Example 11 and Comparative Example 15 produced in this manner were subjected to electrophotographic copying including a step of -5.6 kV corona charging, image exposure, toner phenomenon, toner transfer to plain paper, and cleaning step with urethane rubber blade. I attached it to the machine and made a copy.
本発明による分散装置及び分散方法を用いて得た塗工
液を用いた実施例11の電子写真感光体では、画像欠陥の
ない良好な画像が得られた。With the electrophotographic photosensitive member of Example 11 using the coating liquid obtained by using the dispersing device and the dispersing method according to the present invention, good images without image defects were obtained.
一方、従来の分散装置を用いて得た塗工液を用いた比
較例15の電子写真感光体では、白ポチ，カブリなどの画
像欠陥が発生した。On the other hand, in the electrophotographic photosensitive member of Comparative Example 15 using the coating liquid obtained by using the conventional dispersing device, image defects such as white spots and fog occurred.
このように、本発明によって分散を行えば、短時間で
微細粒子まで均一に分散することができ、塗膜面もムラ
がないので画像欠陥のない良好な画像が得られる。As described above, when the dispersion is performed according to the present invention, even fine particles can be uniformly dispersed in a short time, and the coating film surface is not uneven, so that a good image without image defects can be obtained.
［発明の効果］ 以上説明したように、本発明によるベッセルを有する
分散装置を用いて分散を行うことにより、短時間で効率
良く微分散することができ、しかも均一で安定した微細
粒子に分散することができる。また、本発明の電子写真
感光体塗工液の分散方法によれば、画像欠陥の起きない
感光層を形成することができる。[Effects of the Invention] As described above, by performing dispersion using the dispersion device having a vessel according to the present invention, fine dispersion can be efficiently performed in a short time, and further, it is dispersed into uniform and stable fine particles. be able to. Further, according to the dispersion method of the electrophotographic photosensitive member coating liquid of the present invention, it is possible to form a photosensitive layer free from image defects.
第１図及び第２図は本発明の分散装置のそれぞれ異なる
具体例を示す断面図である。 １……円筒状ベッセル ２……ジャケット ３……ディスク ４……駆動装置 ５……シャフト ６……上ブタ ７……らせん状の溝 ８……らせん状部材1 and 2 are cross-sectional views showing different specific examples of the dispersion apparatus of the present invention. 1 ... Cylindrical vessel 2 ... Jacket 3 ... Disk 4 ... Drive device 5 ... Shaft 6 ... Upper lid 7 ... Helical groove 8 ... Helical member
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭63−301953（ＪＰ，Ａ) 実開 平２−95539（ＪＰ，Ｕ) 実開 昭59−178055（ＪＰ，Ｕ) 実開 昭51−17266（ＪＰ，Ｕ) 特公 昭45−31575（ＪＰ，Ｂ１) 特公 昭58−18612（ＪＰ，Ｂ２) 実公 昭51−45010（ＪＰ，Ｙ２) ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-63-301953 (JP, A) Actually open 2-95539 (JP, U) Actually open 59-178055 (JP, U) Actually open 51- 17266 (JP, U) JP 45-31575 (JP, B1) JP 58-18612 (JP, B2) JP 51-45010 (JP, Y2)
Claims (4)
バッチ式湿式分散装置において、該ベッセルの内壁側面
に沿ってらせん状の溝が設けられていることを特徴とす
るバッチ式湿式分散装置。1. A batch type wet dispersion apparatus having a cylindrical dispersion vessel having a rotation dispersion means, wherein a spiral groove is provided along a side surface of an inner wall of the vessel.
セルの下方から上方に進む際の回転方向と前記の回転分
散手段の回転方向とが同一になるように前記のベッセル
の内壁側面に沿って設けられていることを特徴とする請
求項１記載のバッチ式湿式分散装置。2. The inner wall of the vessel so that the spiral groove has the same rotation direction when traveling from the lower side to the upper side of the vessel along the groove and the rotation direction of the rotation dispersion means. The batch type wet dispersion apparatus according to claim 1, wherein the batch type wet dispersion apparatus is provided along a side surface.
せて、顔料又は染料を含有する電子写真感光体塗工液を
分散させる方法において、該円筒状ベッセルとして該ベ
ッセルの内壁側面に沿ってらせん状の溝が設けられてい
るベッセルを用い、該回転分散手段を回転させて該ベッ
セル内の電子写真感光体塗工液を分散させることを特徴
とする電子写真感光体塗工液の分散方法。3. A method for dispersing an electrophotographic photoreceptor coating liquid containing a pigment or a dye by rotating a rotation dispersion means in a cylindrical vessel, wherein the cylindrical vessel is provided along the inner wall side surface of the vessel. A method for dispersing an electrophotographic photoreceptor coating solution, comprising using a vessel provided with a spiral groove, and rotating the rotational dispersion means to disperse the electrophotographic photoreceptor coating solution in the vessel. .
溝に沿ってベッセルの下方から上方に進む際の回転方向
と同一にすることを特徴とする請求項３記載の電子写真
感光体塗工液の分散方法。4. The electrophotographic photosensitive member according to claim 3, wherein the rotation direction of the rotation dispersion means is the same as the rotation direction when going upward from below the vessel along the groove. Dispersion method of coating liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1277168A JP2567480B2 (en) | 1989-10-26 | 1989-10-26 | Batch-type wet dispersion device and method for dispersing electrophotographic photoreceptor coating liquid using the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1277168A JP2567480B2 (en) | 1989-10-26 | 1989-10-26 | Batch-type wet dispersion device and method for dispersing electrophotographic photoreceptor coating liquid using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03143537A JPH03143537A (en) | 1991-06-19 |
| JP2567480B2 true JP2567480B2 (en) | 1996-12-25 |
Family
ID=17579753
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1277168A Expired - Fee Related JP2567480B2 (en) | 1989-10-26 | 1989-10-26 | Batch-type wet dispersion device and method for dispersing electrophotographic photoreceptor coating liquid using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2567480B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004041956A (en) * | 2002-07-12 | 2004-02-12 | Co-Op Chem Co Ltd | Fluid mixing apparatus and homogeneous dispersion liquid obtained by using the same |
| CA2517014C (en) * | 2003-03-06 | 2012-07-17 | Dentsply International Inc. | Dispensing and mixing tip |
| CN100544810C (en) * | 2004-09-15 | 2009-09-30 | 株式会社吴羽 | solid-liquid contact device and method |
| JP6835487B2 (en) * | 2016-06-10 | 2021-02-24 | デンカ株式会社 | Stirrer |
-
1989
- 1989-10-26 JP JP1277168A patent/JP2567480B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03143537A (en) | 1991-06-19 |
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