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JP2014018745A - Kneading emulsification dispersion method for kneading target material, and kneading machine for kneading target material - Google Patents

Kneading emulsification dispersion method for kneading target material, and kneading machine for kneading target material Download PDF

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JP2014018745A
JP2014018745A JP2012160415A JP2012160415A JP2014018745A JP 2014018745 A JP2014018745 A JP 2014018745A JP 2012160415 A JP2012160415 A JP 2012160415A JP 2012160415 A JP2012160415 A JP 2012160415A JP 2014018745 A JP2014018745 A JP 2014018745A
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kneading
kneaded
binder resin
target material
resin
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Kazuya Mori
一也 森
Takahiro Yamashita
敬弘 山下
Takashi Hara
敬 原
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Fujifilm Business Innovation Corp
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Fuji Xerox Co Ltd
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Abstract

PROBLEM TO BE SOLVED: To provide a kneading emulsification dispersion method for a kneading target material and a kneading machine for a kneading target material, with which particles in the kneading target material after kneading process have a smaller particle size than particles in the kneading target material before the kneading process.SOLUTION: A kneading emulsification dispersion method for a kneading target material includes a kneading process step of charging the kneading target material containing binding resin into a kneading machine, and kneading the kneading target material while heating it in the kneading machine. The kneading process step includes charging a dispersing medium into the kneading machine.

Description

本発明は、被混練物の混練乳化分散方法及び被混練物の混練機に関する。   The present invention relates to a kneading and emulsifying dispersion method for a material to be kneaded and a kneading machine for the material to be kneaded.

電子写真法など静電荷像を経て画像情報を可視化する方法は、現在様々な分野で利用されている。電子写真法においては、帯電、露光工程により像保持体上に静電潜像を形成し(潜像形成工程)、静電荷像現像用トナー(以下、単に「トナー」と呼ぶ場合がある。)を含む静電荷像現像用現像剤(以下、単に「現像剤」と呼ぶ場合がある。)で静電潜像を現像し(現像工程)、転写工程、定着工程を経て可視化される。   A method of visualizing image information through an electrostatic charge image such as electrophotography is currently used in various fields. In electrophotography, an electrostatic latent image is formed on an image carrier by a charging and exposure process (latent image forming process), and an electrostatic charge image developing toner (hereinafter sometimes simply referred to as “toner”). The electrostatic latent image is developed with a developer for developing an electrostatic charge image (hereinafter sometimes referred to simply as “developer”) (development process), and visualized through a transfer process and a fixing process.

静電荷像現像用トナーは、例えば、以下のような製造方法により得られる。   The electrostatic image developing toner can be obtained, for example, by the following manufacturing method.

例えば、特許文献1には、結着樹脂、着色剤を含有するトナー材料混合物(被混練物)を混練機に投入し、混練機内で加熱加圧しながら溶融混練する工程、混練されたトナー材料混合物に、乳化剤を添加し、混練機内で加熱加圧しながら混練して、トナー材料混合物を乳化分散することにより、トナー材料混合物の粒子を形成する工程を備える静電荷像現像用トナーの製造方法が記載されている。   For example, Patent Document 1 discloses a process in which a toner material mixture (a material to be kneaded) containing a binder resin and a colorant is charged into a kneader and melt-kneaded while being heated and pressurized in the kneader, and the kneaded toner material mixture. A method for producing a toner for developing an electrostatic charge image comprising the steps of adding an emulsifier, kneading while heating and pressing in a kneader, and emulsifying and dispersing the toner material mixture to form particles of the toner material mixture is described. Has been.

特開2010−122687号公報JP 2010-122687 A

本発明の目的は、混練処理前の被混練物である結着樹脂及びその中に含まれる着色剤粒子等を混練処理により小粒径化し、且つ粒度分布を単峰性とする被混練物の混練乳化分散方法及び被混練物の混練機を提供することにある。   The object of the present invention is to reduce the particle size of the binder resin, which is the material to be kneaded before the kneading treatment, and the colorant particles contained therein by kneading treatment, and to make the particle size distribution unimodal. An object of the present invention is to provide a kneading and emulsifying dispersion method and a kneading machine for a material to be kneaded.

請求項1に係る発明は、結着樹脂を含む被混練物を混練機に投入し、前記混練機内で加熱しながら前記被混練物を混練する混練処理工程を含み、前記混練処理工程では、前記混練機に分散媒体を投入する被混練物の混練乳化分散方法である。   The invention according to claim 1 includes a kneading treatment step in which a material to be kneaded containing a binder resin is charged into a kneader and the material to be kneaded is kneaded while being heated in the kneader. This is a method for kneading, emulsifying and dispersing a material to be kneaded, in which a dispersion medium is put into a kneader.

請求項2に係る発明は、前記分散媒体の軟化点が、前記結着樹脂の融点より高いものである請求項1記載の被混練物の混練乳化分散方法である。   The invention according to claim 2 is the method for kneading, emulsifying and dispersing the material to be kneaded according to claim 1, wherein the softening point of the dispersion medium is higher than the melting point of the binder resin.

請求項3に係る発明は、分散媒体と、結着樹脂を含む被混練物及び前記分散媒体が投入される混練容器と、前記混練容器内に設けられた攪拌部材と、前記被混練物を加熱する加熱手段と、を備える被混練物の混練機である。   According to a third aspect of the present invention, there is provided a dispersion medium, a material to be kneaded containing a binder resin, a kneading container into which the dispersion medium is charged, a stirring member provided in the kneading container, and heating the material to be kneaded. A kneading machine for an object to be kneaded, comprising heating means for performing the above.

請求項1に係る発明によると、本構成を有さない場合と比べて、混練処理前の被混練物である結着樹脂及びその中に含まれる着色剤粒子等を混練処理により小粒径化し、且つ粒度分布を単峰性とする被混練物の混練乳化分散方法が提供される。   According to the first aspect of the present invention, compared to the case without this configuration, the binder resin that is the material to be kneaded before the kneading process and the colorant particles contained therein are reduced in size by the kneading process. In addition, a method for kneading, emulsifying and dispersing a material to be kneaded having a unimodal particle size distribution is provided.

請求項2に係る発明によると、本構成を有さない場合と比べて、混練処理前の被混練物である結着樹脂及びその中に含まれる着色剤粒子等を混練処理により小粒径化し、且つ粒度分布を単峰性とし、更に粒度分布の拡がりを抑制する被混練物の混練乳化分散方法が提供される。   According to the second aspect of the present invention, the binder resin, which is the material to be kneaded before the kneading process, and the colorant particles contained therein are reduced in size by the kneading process as compared with the case without this configuration. In addition, there is provided a method for kneading, emulsifying and dispersing a material to be kneaded, which makes the particle size distribution unimodal and further suppresses the spread of the particle size distribution.

請求項3に係る発明によると、本構成を有さない場合と比べて、混練処理前の被混練物である結着樹脂及びその中に含まれる着色剤粒子等を混練処理により小粒径化し、且つ粒度分布を単峰性とする被混練物の混練機が提供される。   According to the invention of claim 3, compared to the case without this configuration, the binder resin that is the material to be kneaded before the kneading process and the colorant particles contained therein are reduced in size by the kneading process. In addition, a kneading machine for a material to be kneaded having a unimodal particle size distribution is provided.

本発明の実施形態に係る混練機の一例を示す概略構成図である。It is a schematic structure figure showing an example of a kneading machine concerning an embodiment of the present invention. 図1の混練機の上面模式図である。FIG. 2 is a schematic top view of the kneader in FIG. 1.

本発明の実施の形態について以下説明する。本実施形態は本発明を実施する一例であって、本発明は本実施形態に限定されるものではない。   Embodiments of the present invention will be described below. This embodiment is an example for carrying out the present invention, and the present invention is not limited to this embodiment.

本実施形態は、結着樹脂を含む被混練物を下記に説明する混練機に投入し、前記混練機内で加熱しながら前記被混練物を混練する混練処理工程を含み、混練処理工程では、前記混練機内に下記に説明する分散媒体(以下、メディアと呼ぶ場合がある)を投入する。すなわち、混練処理工程では、混練機内で被混練物とメディアとが混合される。   The present embodiment includes a kneading treatment step in which a material to be kneaded including a binder resin is charged into a kneader described below and kneaded with the material to be kneaded while being heated in the kneader. A dispersion medium described below (hereinafter sometimes referred to as a medium) is put into the kneader. That is, in the kneading process, the material to be kneaded and the medium are mixed in the kneader.

図1は、本発明の実施形態に係る混練機の一例を示す概略構成図であり、図2は、図1の混練機の上面模式図である。図1及び図2に示すように、本実施形態の被混練物の混練機1は、結着樹脂を含む被混練物及びメディアが投入される混練容器10と、混練容器10内に設けられた攪拌部材22を備える攪拌手段としての攪拌機12と、被混練物を加熱する加熱手段としての加熱用ジャケット14と、を備える。混練容器10の上部には、投入口16が設けられている。本実施形態の攪拌機12は、駆動手段としてのモータ18、回転軸20、回転軸20に設置された攪拌部材22から構成され、モータ18により回転軸20を中心に攪拌部材22が回転される。本実施形態の攪拌部材22は、スクリュー状の撹拌羽根を2つ備え、2つの撹拌羽根が対向して配置されている。攪拌部材22の形状はスクリュー状に限定されるものではなく、例えばブレード状等の撹拌羽根等であってもよい。また、撹拌羽根の本数は特に制限されるものではない。加熱用ジャケット14は、混練容器10の外周側面の少なくとも一部に設置されればよいが、混練容器10の外周側面全体に設置されることが好ましい。加熱用ジャケット14は、その内部に加熱媒体が通過する空間が形成されており、その内部空間に加熱媒体が通過することにより、混練容器10を介して混練容器10内の被混練物が加熱される。   FIG. 1 is a schematic configuration diagram illustrating an example of a kneader according to an embodiment of the present invention, and FIG. 2 is a schematic top view of the kneader of FIG. As shown in FIGS. 1 and 2, a kneading machine 1 for a material to be kneaded according to this embodiment is provided in a kneading container 10 into which a material to be kneaded including a binder resin and a medium are charged, and the kneading container 10. A stirrer 12 as a stirring means including the stirring member 22 and a heating jacket 14 as a heating means for heating the material to be kneaded are provided. At the top of the kneading vessel 10, a charging port 16 is provided. The stirrer 12 of this embodiment includes a motor 18 as a driving unit, a rotating shaft 20, and a stirring member 22 installed on the rotating shaft 20, and the stirring member 22 is rotated around the rotating shaft 20 by the motor 18. The stirring member 22 of the present embodiment includes two screw-shaped stirring blades, and the two stirring blades are arranged to face each other. The shape of the stirring member 22 is not limited to a screw shape, and may be a stirring blade such as a blade shape. Further, the number of stirring blades is not particularly limited. The heating jacket 14 may be installed on at least a part of the outer peripheral side surface of the kneading container 10, but is preferably installed on the entire outer peripheral side surface of the kneading container 10. The heating jacket 14 has a space through which the heating medium passes, and the material to be kneaded in the kneading container 10 is heated via the kneading container 10 when the heating medium passes through the inner space. The

図1に示す被混練物の混練機1は、混練処理する際に被混練物を混練容器10に投入し、加熱しながら混練処理し、混練処理後に混練容器10から混練物を取り出す加熱式のバッチ型ニーダである。そして、本実施形態の被混練物の混練乳化分散方法に用いる混練機としては、メディアの回収、再利用等の点から、図1に示すようなバッチ型ニーダを用いることが好ましいが、これに制限されるものではなく、例えば、1軸押出機、2軸押出機、加圧式ニーダ、双腕式ニーダ、バンバリーミキサー、ブラベンダーミキサ等でもよい。   A kneading machine 1 for a material to be kneaded shown in FIG. 1 is a heating type in which a material to be kneaded is put into a kneading container 10 when kneading, and is kneaded while being heated. It is a batch type kneader. And as a kneading machine used for the kneading emulsification dispersion method of the material to be kneaded of this embodiment, it is preferable to use a batch type kneader as shown in FIG. For example, a single screw extruder, a twin screw extruder, a pressure kneader, a double-arm kneader, a Banbury mixer, a Brabender mixer, or the like may be used.

図1の被混練物の混練機1を用いて、本実施形態に係る被混練物の混練乳化分散方法について説明する。   The kneading and emulsifying and dispersing method for a material to be kneaded according to the present embodiment will be described using the kneading machine 1 for the material to be kneaded in FIG.

結着樹脂を含む被混練物及びメディアを投入口16から混練容器10内に投入する。また、加熱用ジャケット14により混練容器10を介して被混練物を加熱し、攪拌部材22により被混練物及びメディアを攪拌して、被混練物の混練処理を実施する(混練処理工程)。被混練物の加熱温度は、結着樹脂の融点より高い温度であることが好ましい。   The material to be kneaded and the medium containing the binder resin are charged into the kneading container 10 from the charging port 16. In addition, the material to be kneaded is heated via the kneading vessel 10 by the heating jacket 14, and the material to be kneaded and the medium are stirred by the stirring member 22 to perform the kneading process of the material to be kneaded (kneading process step). The heating temperature of the material to be kneaded is preferably higher than the melting point of the binder resin.

本実施形態では、結着樹脂を含む被混練物が混練される際、混練容器10内で、結着樹脂を含む被混練物と共にメディアも流動するため、メディアを投入しない場合に比べて、結着樹脂を含む被混練物を分散させるエネルギーは高くなると考えられる。また、本実施形態では、結着樹脂を含む被混練物が混練される際に、被混練物である結着樹脂及びその中に含まれる着色剤粒子等は、攪拌部材22により攪拌(或いは粉砕)されるだけでなく、混練容器10内を流動するメディアによっても撹拌、粉砕されると考えられる。これらにより、本実施形態の混練処理後の混練物は、混練処理により小粒径化し、また、例えば、メディアを投入しないで攪拌部材22による攪拌だけで混練処理した混練物より小粒径化し易くなる。また、粒度分布を単峰性としやすくなる。本実施形態の混練処理後の体積平均粒径は、例えば、0.05μm以上0.5μm以下の範囲であることが好ましく、0.1μm以上0.3μm以下の範囲であることがより好ましい。   In the present embodiment, when the material to be kneaded containing the binder resin is kneaded, the medium also flows in the kneading container 10 together with the material to be kneaded containing the binder resin. It is considered that the energy for dispersing the material to be kneaded including the resin is increased. In the present embodiment, when the material to be kneaded containing the binder resin is kneaded, the binder resin that is the material to be kneaded and the colorant particles contained therein are stirred (or pulverized) by the stirring member 22. It is considered that the agitation and pulverization are also performed by the medium flowing in the kneading vessel 10. As a result, the kneaded material after the kneading process of the present embodiment is reduced in particle size by the kneading process, and for example, it is easier to reduce the particle size than the kneaded product kneaded only by stirring with the stirring member 22 without introducing the media. Become. Moreover, it becomes easy to make the particle size distribution unimodal. The volume average particle size after the kneading treatment of the present embodiment is preferably in the range of 0.05 μm to 0.5 μm, for example, and more preferably in the range of 0.1 μm to 0.3 μm.

本実施形態の混練乳化分散処理方法を用いて結着樹脂乳化分散液を調製する場合、例えば、被混練物としての結着樹脂及びメディアを投入口16から混練容器10内に投入し、混合容器内で加熱しながら被混練物を混練処理する。そして、混練処理中、又は混練処理後に、例えば界面活性剤、純水、水酸化ナトリウム等の塩基性物質(pH調整剤)等を添加して、結着樹脂分乳化散液を得てもよい。   When preparing a binder resin emulsified dispersion using the kneading emulsification dispersion processing method of the present embodiment, for example, a binder resin and media as a material to be kneaded are charged into the kneading container 10 from the inlet 16 and mixed. The material to be kneaded is kneaded while being heated inside. Then, during or after the kneading treatment, for example, a basic substance (pH adjuster) such as a surfactant, pure water, sodium hydroxide or the like may be added to obtain a binder resin fraction emulsified dispersion. .

また、本実施形態の混練乳化分散処理方法を用いて静電荷像現像用トナーを調製する場合、例えば、結着樹脂、必要に応じて添加される着色剤、離型剤等のその他の成分等を含む被混練物及びメディアを投入口16から混練容器10内に投入し、混合容器内で加熱しながら被混練物を混練処理する。混練処理後に、例えば、界面活性剤、純水、水酸化ナトリウム等の塩基性物質(pH調整剤)等を添加しトナー分散液とし、前記トナー分散液中において凝集粒子を形成する公知の凝集工程、及び前記凝集粒子を融合する公知の融合工程を経て、静電荷像現像用トナーを得てもよい。   Further, when an electrostatic charge image developing toner is prepared using the kneading and emulsifying dispersion processing method of the present embodiment, for example, a binder resin, a colorant added as necessary, other components such as a release agent, etc. The material to be kneaded and the medium containing the above are introduced into the kneading container 10 from the charging port 16, and the material to be kneaded is kneaded while being heated in the mixing container. After kneading treatment, for example, a known agglomeration step in which a basic substance (pH adjuster) such as surfactant, pure water, sodium hydroxide or the like is added to form a toner dispersion, and agglomerated particles are formed in the toner dispersion. The toner for developing an electrostatic image may be obtained through a known fusing process for fusing the agglomerated particles.

静電荷像現像用トナーの調製において、混練処理後に行われる凝集工程等での凝集粒子の粒径制御や内部構造制御等は、小粒径の粒子から構成される混練物を用いることが好ましい。したがって、前述したように、本実施形態の混練処理方法により得られる混練物中の粒子の体積平均粒径は、混練処理前の被混練物中の粒子の体積平均粒径より小粒径化し、更にはメディアを投入しないで攪拌部材22による攪拌だけで混練処理した混練物中の粒子の体積平均粒径より小粒径化し易いため、本実施形態の混練処理方法により得られる混練物を用いて、混練処理後に行われる凝集工程等での凝集粒子の粒径制御や内部構造制御等を行うことが好ましい。   In the preparation of the toner for developing an electrostatic image, it is preferable to use a kneaded product composed of particles having a small particle diameter in order to control the particle diameter of the aggregated particles and the internal structure in the aggregation process performed after the kneading process. Therefore, as described above, the volume average particle size of the particles in the kneaded product obtained by the kneading treatment method of the present embodiment is smaller than the volume average particle size of the particles in the material to be kneaded before the kneading process, Furthermore, since it is easy to make the particle diameter smaller than the volume average particle diameter of the kneaded material kneaded by only stirring by the stirring member 22 without introducing the medium, the kneaded material obtained by the kneading treatment method of the present embodiment is used. It is preferable to control the particle size of the agglomerated particles, control the internal structure, etc. in the agglomeration step performed after the kneading process.

本実施形態で用いられる分散媒体(メディア)は、被混練物である結着樹脂及びその中に含まれる着色剤粒子等を分散させる固形物であればよいが、結着樹脂を含む被混練物と物理的又は化学的に干渉しない材料から構成されることが好ましい。結着樹脂を含む被混練物と物理的に干渉するとは、例えば、混練処理の際の加熱によって、メディアが溶融、均一化する場合等をいう。また、結着樹脂を含む被混練物と化学的に干渉するとは、例えば、結着樹脂を含む被混練物と化学反応する場合等をいう。   The dispersion medium (media) used in the present embodiment may be a solid material in which the binder resin as the material to be kneaded and the colorant particles contained therein are dispersed, but the material to be kneaded containing the binder resin. Preferably, it is made of a material that does not physically or chemically interfere with the material. The physical interference with the material to be kneaded including the binder resin means, for example, a case where the medium is melted and uniformed by heating during the kneading process. In addition, the chemical interference with the material to be kneaded containing the binder resin means, for example, a case of chemically reacting with the material to be kneaded containing the binder resin.

本実施形態で用いられるメディアは、結着樹脂を含む被混練物と物理的な干渉を避ける点、混練処理後の混練物中の粒子の粒度分布の拡がりを抑制する点等から、結着樹脂の融解温度より高い軟化点を有することが好ましい。結着樹脂の融解温度は、示差走査熱量計(セイコー電子工業社製:DSC−20)を用い、室温(25℃)から150℃まで昇温速度10℃/分の条件下で測定することにより求められる。また、メディアの軟化点は、フローテスター(島津社製: CFT−500C)により測定され、予熱:80℃/300sec,プランジャー圧力:0.980665MPa,ダイサイズ:1mmφ×1mm,昇温速度:3.0℃/minの条件下における溶融開始温度と溶融終了温度との中間温度を指す。また、メディアは、結着樹脂の融解温度より高い軟化点を有し、かつ融解温度を有さないことが好ましい。   The media used in the present embodiment is a binder resin from the viewpoint of avoiding physical interference with the material to be kneaded containing the binder resin, the point of suppressing the expansion of the particle size distribution of the particles in the kneaded material after the kneading process, and the like. It preferably has a softening point higher than the melting temperature. The melting temperature of the binder resin is measured using a differential scanning calorimeter (Seiko Denshi Kogyo Co., Ltd .: DSC-20) by measuring from room temperature (25 ° C.) to 150 ° C. under a temperature rising rate of 10 ° C./min. Desired. The softening point of the media was measured with a flow tester (manufactured by Shimadzu Corp .: CFT-500C), preheating: 80 ° C./300 sec, plunger pressure: 0.980665 MPa, die size: 1 mmφ × 1 mm, heating rate: 3 The intermediate temperature between the melting start temperature and the melting end temperature under the condition of 0.0 ° C./min. The medium preferably has a softening point higher than the melting temperature of the binder resin and does not have a melting temperature.

本実施形態で用いられるメディアは、メディアの損傷を抑制する点等から、攪拌部材または混練容器の内面の材料よりも軟らかいことが好ましい。一般的に攪拌部材22と混練容器10の内面とが衝突しないように、例えば混練容器10の内面と攪拌部材22との間には隙間が設けられる場合がある。そして、メディアの平均粒子直径が混練容器10の内面と攪拌部材22との間の隙間より大きいと、メディアは攪拌部材22により混練容器10の内面に押し付けられ、損傷する場合がある。しかし、攪拌部材または混練容器の内面の材料よりも軟らかいメディアを用いた場合、攪拌部材22により混練容器10の内面に押し付けられる圧力等が緩和されると考えられ、メディアの損傷が抑制される。   The medium used in the present embodiment is preferably softer than the material on the inner surface of the stirring member or the kneading container from the viewpoint of suppressing damage to the medium. In general, for example, a gap may be provided between the inner surface of the kneading vessel 10 and the stirring member 22 so that the stirring member 22 and the inner surface of the kneading vessel 10 do not collide. If the average particle diameter of the media is larger than the gap between the inner surface of the kneading vessel 10 and the stirring member 22, the media may be pressed against the inner surface of the kneading vessel 10 by the stirring member 22 and may be damaged. However, when a medium softer than the material of the stirring member or the inner surface of the kneading container is used, it is considered that the pressure or the like pressed against the inner surface of the kneading container 10 by the stirring member 22 is alleviated, and damage to the medium is suppressed.

また、本実施形態で用いられるメディアは、混練容器10の内面と攪拌部材22との間の隙間より小さい平均粒子直径を有することが好ましい。混練容器10の内面と攪拌部材22との間に設けられる隙間より小さい平均粒子直径を有するメディアを用いた場合、攪拌部材22により混練容器10の内面に押し付けられる圧力等が緩和されると考えられ、混練容器10の内面と攪拌部材22との間に設けられる隙間より大きい平均粒子直径を有するメディアを用いる場合より、メディアの損傷が抑制される。   Moreover, it is preferable that the media used in this embodiment have an average particle diameter smaller than the gap between the inner surface of the kneading vessel 10 and the stirring member 22. When a medium having an average particle diameter smaller than the gap provided between the inner surface of the kneading vessel 10 and the stirring member 22 is used, it is considered that the pressure or the like pressed against the inner surface of the kneading vessel 10 by the stirring member 22 is relieved. Further, damage to the media is suppressed as compared with the case where media having an average particle diameter larger than the gap provided between the inner surface of the kneading container 10 and the stirring member 22 is used.

本実施形態で用いられるメディアを構成する材料は、結着樹脂を含む被混練物と化学的な干渉を避ける等の点で、ガラス、セラミック、ジルコニアやアルミナ等の金属酸化物、ステンレス等の金属、スチレン、アクリロニトリル、ブタジエン等の樹脂等が挙げられる。結着樹脂の融点より高い軟化点を有し、ガラス、セラミック、金属酸化物、金属等より高い弾性率を有する点で樹脂であることが好ましく、例えば、アクリロニトリルスチレン共重合体などのスチレン系樹脂変性体等が挙げられる。   The material constituting the media used in this embodiment is made of glass, ceramic, metal oxides such as zirconia and alumina, and metals such as stainless steel in terms of avoiding chemical interference with the material to be kneaded including the binder resin. , Resins such as styrene, acrylonitrile, and butadiene. The resin is preferably a resin having a softening point higher than the melting point of the binder resin and a higher elastic modulus than that of glass, ceramic, metal oxide, metal, etc., for example, a styrene resin such as acrylonitrile styrene copolymer Examples include modified products.

本実施形態で用いられるメディアの形状は、円柱状、角柱状等いずれの形状であってもよい。   The shape of the media used in the present embodiment may be any shape such as a columnar shape or a prismatic shape.

本実施形態の混練乳化分散処理方法を用いて調製される静電荷像現像用トナーは、結着樹脂を含むものであり、必要に応じて、着色剤、離型剤、帯電制御剤、無機粒子等のその他の成分を含むものである。   The electrostatic image developing toner prepared by using the kneading emulsification dispersion processing method of the present embodiment contains a binder resin, and if necessary, a colorant, a release agent, a charge control agent, inorganic particles. And other components.

静電荷像現像用トナーを構成する結着樹脂は、例えば、スチレン、パラクロロスチレン、α−メチルスチレン等のスチレン類、アクリル酸メチル、アクリル酸エチル、アクリル酸n−プロピル、アクリル酸n−ブチル、アクリル酸ラウリル、アクリル酸2−エチルヘキシル、メタクリル酸メチル、メタクリル酸エチル、メタクリル酸n−プロピル、メタクリル酸ラウリル、メタクリル酸2−エチルヘキシル等の(メタ)アクリル酸エステル類、アクリロニトリル、メタクリロニトリル等のエチレン性不飽和ニトリル類、ビニルメチルエーテル、ビニルイソブチルエーテル等のビニルエーテル類、ビニルメチルケトン、ビニルエチルケトン、ビニルイソプロペニルケトン等のビニルケトン類、エチレン、プロピレン、ブタジエンなどのポリオレフィン類等の単量体などの重合体、若しくはこれらを2種以上組み合わせた共重合体、又はこれらの混合物等が挙げられる。また、結着樹脂として、例えば、エポキシ樹脂、ポリエステル樹脂、ポリウレタン樹脂、ポリアミド樹脂、セルロース樹脂、ポリエーテル樹脂等、非ビニル縮合系樹脂、これらと前記ビニル系樹脂との混合物、これらの共存下でビニル系単量体を重合して得られるグラフト重合体等が挙げられる。これらの樹脂は、1種類単独で用いてもよいし、2種以上を併用してもよい。   Examples of the binder resin constituting the electrostatic image developing toner include styrenes such as styrene, parachlorostyrene, and α-methylstyrene, methyl acrylate, ethyl acrylate, n-propyl acrylate, and n-butyl acrylate. (Meth) acrylic esters such as lauryl acrylate, 2-ethylhexyl acrylate, methyl methacrylate, ethyl methacrylate, n-propyl methacrylate, lauryl methacrylate, 2-ethylhexyl methacrylate, acrylonitrile, methacrylonitrile, etc. Ethylenically unsaturated nitriles, vinyl ethers such as vinyl methyl ether and vinyl isobutyl ether, vinyl ketones such as vinyl methyl ketone, vinyl ethyl ketone and vinyl isopropenyl ketone, and polyolefins such as ethylene, propylene and butadiene. Polymers such as monomers such as fin acids, or a copolymer of a combination of two or more of these, or mixtures thereof. In addition, as the binder resin, for example, epoxy resin, polyester resin, polyurethane resin, polyamide resin, cellulose resin, polyether resin, etc., non-vinyl condensation resin, a mixture of these with the vinyl resin, and coexistence thereof Examples include graft polymers obtained by polymerizing vinyl monomers. These resins may be used alone or in combination of two or more.

また、結着樹脂は、結晶性樹脂でもよく、非晶性樹脂でもよく、結晶性樹脂と非晶性樹脂とを併用してもよい。   The binder resin may be a crystalline resin, an amorphous resin, or a combination of a crystalline resin and an amorphous resin.

本実施形態において、「結晶性樹脂」の「結晶性」とは、樹脂またはトナーの示差走査熱量測定(DSC)において、階段状の吸熱量変化ではなく、明確な吸熱ピークを有することを指す。具体的には、自動接線処理システムを備えた島津製作所社製の示差走査熱量計(装置名:DSC−60型)を用いた示差走査熱量測定(DSC)において、10℃/minの昇温速度で昇温したときのオンセット点から吸熱ピークのピークトップまでの温度が10℃以内であるときに「明確な」吸熱ピークであるとする。DSC曲線におけるベースラインの平坦部の点及びベースラインからの立ち下がり部の平坦部の点を指定し、その両点間の平坦部の接線の交点が「オンセット点」として自動接線処理システムにより求められる。また、吸熱ピークは、トナーとしたときに、40℃以上50℃以下の幅を有するピークを示す場合がある。   In the present embodiment, “crystallinity” of “crystalline resin” refers to having a clear endothermic peak rather than a stepwise endothermic amount change in differential scanning calorimetry (DSC) of the resin or toner. Specifically, in differential scanning calorimetry (DSC) using a differential scanning calorimeter (equipment name: DSC-60 type) manufactured by Shimadzu Corporation equipped with an automatic tangential processing system, a rate of temperature increase of 10 ° C./min. A “clear” endothermic peak is assumed when the temperature from the onset point to the top of the endothermic peak when the temperature is raised at 10 ° C. is within 10 ° C. The point of the flat part of the baseline in the DSC curve and the point of the flat part of the falling part from the base line are specified, and the intersection of the tangents of the flat part between the two points is set as an “onset point” by the automatic tangent processing system. Desired. Further, the endothermic peak may show a peak having a width of 40 ° C. or more and 50 ° C. or less when the toner is used.

また、「非晶性樹脂」とは、樹脂またはトナーの示差走査熱量測定(DSC)において、オンセット点から吸熱ピークのピークトップまでの温度が10℃を超えるとき、又は明確な吸熱ピークが認められない樹脂であることを指す。具体的には、自動接線処理システムを備えた島津製作所社製の示差走査熱量計(装置名:DSC−60型)を用いた示差走査熱量測定(DSC)において、10℃/minの昇温速度で昇温したときのオンセット点から吸熱ピークのピークトップまでの温度が10℃を超えるとき、又は明確な吸熱ピークが認められないときに「非晶性」であるとする。また、前記オンセット点から吸熱ピークのピークトップまでの温度は、12℃を超えることが好ましく、明確な吸熱ピークが認められないことがより好ましい。DSC曲線における「オンセット点」の求め方は上記「結晶性樹脂」の場合と同様である。   The term “amorphous resin” means that when the temperature from the onset point to the peak top of the endothermic peak exceeds 10 ° C. or a clear endothermic peak is observed in differential scanning calorimetry (DSC) of the resin or toner. It refers to a resin that cannot be used. Specifically, in differential scanning calorimetry (DSC) using a differential scanning calorimeter (equipment name: DSC-60 type) manufactured by Shimadzu Corporation equipped with an automatic tangential processing system, a rate of temperature increase of 10 ° C./min. When the temperature from the onset point to the peak top of the endothermic peak exceeds 10 ° C. or when no clear endothermic peak is observed, it is assumed to be “amorphous”. Further, the temperature from the onset point to the peak top of the endothermic peak preferably exceeds 12 ° C., and more preferably no clear endothermic peak is observed. The method for obtaining the “onset point” in the DSC curve is the same as in the case of the “crystalline resin”.

結晶性樹脂としては、結晶性を持つ樹脂であれば特に制限はなく、具体的には、結晶性ポリエステル樹脂、結晶性ビニル系樹脂が挙げられる。結晶性ビニル系樹脂としては、例えば、(メタ)アクリル酸アミル、(メタ)アクリル酸ヘキシル、(メタ)アクリル酸ヘプチル、(メタ)アクリル酸オクチル、(メタ)アクリル酸ノニル、(メタ)アクリル酸デシル、(メタ)アクリル酸ウンデシル、(メタ)アクリル酸トリデシル、(メタ)アクリル酸ミリスチル、(メタ)アクリル酸セチル、(メタ)アクリル酸ステアリル、(メタ)アクリル酸オレイル、(メタ)アクリル酸ベヘニル等の長鎖アルキル、アルケニルの(メタ)アクリル酸エステルを用いたビニル系樹脂が挙げられる。   The crystalline resin is not particularly limited as long as it is a resin having crystallinity, and specific examples include crystalline polyester resins and crystalline vinyl resins. Examples of the crystalline vinyl resin include amyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, octyl (meth) acrylate, nonyl (meth) acrylate, and (meth) acrylic acid. Decyl, undecyl (meth) acrylate, tridecyl (meth) acrylate, myristyl (meth) acrylate, cetyl (meth) acrylate, stearyl (meth) acrylate, oleyl (meth) acrylate, behenyl (meth) acrylate And vinyl resins using long-chain alkyl and alkenyl (meth) acrylic acid esters.

結晶性ポリエステル樹脂は、カルボン酸(ジカルボン酸)成分とアルコール(ジオール)成分とから合成されるものであり、本実施形態において、「カルボン酸成分」とは、ポリエステル樹脂の合成前には酸成分であった構成部位を指し、「アルコール成分」とは、ポリエステル樹脂の合成前にはアルコール成分であった構成部位を指す。また、結晶性ポリエステル主鎖に対して他成分を共重合したポリマの場合、他成分が50質量%以下の場合、この共重合体も結晶性ポリエステル樹脂と呼ぶ。   The crystalline polyester resin is synthesized from a carboxylic acid (dicarboxylic acid) component and an alcohol (diol) component, and in this embodiment, the “carboxylic acid component” is an acid component before the synthesis of the polyester resin. The “alcohol component” refers to a component site that was an alcohol component before the synthesis of the polyester resin. In the case of a polymer obtained by copolymerizing other components with respect to the crystalline polyester main chain, when the other components are 50% by mass or less, this copolymer is also called a crystalline polyester resin.

静電荷像現像用トナーを構成する着色剤は、染料であっても顔料であってもよいが、耐光性や耐水性の観点から、顔料であることが好ましい。着色剤としては、例えば、カーボンブラック、アニリンブラック、アニリンブルー、カルコイルブルー、クロムイエロー、ウルトラマリンブルー、デュポンオイルレッド、キノリンイエロー、メチレンブルークロライド、フタロシアンブルー、マラカイトグリーンオキサート、ランプブラック、ローズベンガル、キナクリドン、ベンジジンイエロー、C.I.ピグメント・レッド48:1、C.I.ピグメント・レッド57:1、185、C.I.ピグメント・レッド122、C.I.ピグメント・レッド185、C.I.ピグメント・レッド238、C.I.ピグメント・イエロー12、C.I.ピグメント・イエロー17、C.I.ピグメント・イエロー180、C.I.ピグメント・イエロー97、C.I.ピグメント・イエロー74、C.I.ピグメント・ブルー15:1、C.I.ピグメント・ブルー15:3等の公知の顔料が使用される。その形態は、製品として乾燥された粉末状でも、製造途中の水分を含んだケーキ状でもよい。   The colorant constituting the toner for developing an electrostatic image may be a dye or a pigment, but is preferably a pigment from the viewpoint of light resistance and water resistance. Examples of colorants include carbon black, aniline black, aniline blue, calcoil blue, chrome yellow, ultramarine blue, dupont oil red, quinoline yellow, methylene blue chloride, phthalocyanine blue, malachite green oxalate, lamp black, and rose. Bengal, Quinacridone, Benzidine Yellow, C.I. I. Pigment red 48: 1, C.I. I. Pigment red 57: 1, 185, C.I. I. Pigment red 122, C.I. I. Pigment red 185, C.I. I. Pigment red 238, C.I. I. Pigment yellow 12, C.I. I. Pigment yellow 17, C.I. I. Pigment yellow 180, C.I. I. Pigment yellow 97, C.I. I. Pigment yellow 74, C.I. I. Pigment blue 15: 1, C.I. I. A known pigment such as CI Pigment Blue 15: 3 is used. The form may be in the form of a powder dried as a product or in the form of a cake containing moisture during production.

静電荷像現像用トナーを構成する離型剤は、例えば、ポリエチレン、ポリプロピレン、ポリブテン等の低分子量ポリオレフィン類、加熱により軟化点を有するシリコーン類、オレイン酸アミド、エルカ酸アミド、リシノール酸アミド、ステアリン酸アミド等のような脂肪酸アミド類やカルナウバワックス、ライスワックス、キャンデリラワックス、木ロウ、ホホバ油等のような植物系ワックス、ミツロウのごとき動物系ワックス、モンタンワックス、オゾケライト、セレシン、パラフィンワックス、マイクロクリスタリンワックス、フィッシャトロプシュワックス等のような鉱物、石油系ワックス、およびそれらの変性物等が挙げられる。   The release agent constituting the electrostatic image developing toner includes, for example, low molecular weight polyolefins such as polyethylene, polypropylene and polybutene, silicones having a softening point by heating, oleic acid amide, erucic acid amide, ricinoleic acid amide, stearin Fatty acid amides such as acid amides, plant waxes such as carnauba wax, rice wax, candelilla wax, tree wax, jojoba oil, animal waxes such as beeswax, montan wax, ozokerite, ceresin, paraffin wax And minerals such as microcrystalline wax and Fischer-Tropsch wax, petroleum wax, and modified products thereof.

これらの離型剤は単独で使用可能な他、2種類以上組み合わせて使用してもよい。これら離型剤の含有量としては結着樹脂100質量部に対して、1質量部以上10質量部以下が好ましく、5質量部以上9質量部以下がより好ましい。   These mold release agents can be used alone or in combination of two or more. The content of these release agents is preferably 1 part by mass or more and 10 parts by mass or less, and more preferably 5 parts by mass or more and 9 parts by mass or less with respect to 100 parts by mass of the binder resin.

静電荷像現像用トナーを構成する帯電制御剤は、例えば、アゾ系金属錯体、サルチル酸もしくはアルキルサルチル酸の金属錯体もしくは金属塩等が挙げられる。   Examples of the charge control agent constituting the toner for developing an electrostatic image include azo metal complexes, metal complexes or metal salts of salicylic acid or alkylsalicylic acid.

静電荷像現像用トナーを構成する無機粒子は、例えば、シリカ粒子、酸化チタン粒子、アルミナ粒子、酸化セリウム粒子、あるいはこれらの表面を疎水化処理したもの等公知の無機粒子を単独または二種以上を組み合わせて使用すればよいが、発色性やオーバヘッドプロジェクタ(OHP)透過性等の透明性を損なわないという観点から屈折率が結着樹脂よりも小さいシリカ粒子が好ましい。またシリカ粒子は種々の表面処理が施されてもよく、例えばシラン系カップリング剤、チタン系カップリング剤、シリコーンオイル等で表面処理したものが好ましい。   The inorganic particles constituting the electrostatic image developing toner are, for example, silica particles, titanium oxide particles, alumina particles, cerium oxide particles, or known inorganic particles such as those obtained by hydrophobizing the surface thereof, alone or in combination. However, silica particles having a refractive index smaller than that of the binder resin are preferable from the viewpoint of not impairing transparency such as color developability and overhead projector (OHP) transparency. Further, the silica particles may be subjected to various surface treatments, and for example, those subjected to surface treatment with a silane coupling agent, a titanium coupling agent, silicone oil or the like are preferable.

以下、実施例及び比較例を挙げ、本発明をより具体的に詳細に説明するが、本発明は、以下の実施例に限定されるものではない。   Hereinafter, although an example and a comparative example are given and the present invention is explained more concretely in detail, the present invention is not limited to the following examples.

<実施例1>
(結着樹脂分散液の調製)
図1に示す混練機(混練容器の内面と攪拌部材との間の隙間が3.0mm)を用いて、樹脂粒子分散液を調整した。まず、混練容器に、結着樹脂としてのポリエステル樹脂(融点(Tm)105℃以上109℃以下)300質量部、メディア(粒子直径2.5mm、高さ約3mmの円柱状のスチレン系樹脂変性体(旭化成ケミカルズ株式会社製)であって、130℃以上で軟化するが融点を持たないもの)50質量部、界面活性剤25質量部を添加し、攪拌部材の回転数50rpm、ジャケット温度110℃として、60分間加熱撹拌し、ポリエステル樹脂を軟化させた(溶融混練工程)。なお、メディアは、軟化している樹脂中に分散していた。次に、塩基性物質としての水酸化ナトリウム水溶液6質量部を添加した。次いで、混練容器内の温度を95℃以上に維持しながら、純水600質量部を徐々に添加した。添加完了により乳化分散し、結着樹脂水分散体を得た。得られた樹脂水分散液の体積平均粒径は115nmであり、粒度分布は単峰性であった。これらの結果を表1にまとめた。
<Example 1>
(Preparation of binder resin dispersion)
The resin particle dispersion was prepared using the kneader shown in FIG. 1 (the gap between the inner surface of the kneading container and the stirring member was 3.0 mm). First, in a kneading container, 300 parts by mass of a polyester resin (melting point (Tm) of 105 ° C. or more and 109 ° C. or less) as a binder resin, a medium (particle diameter 2.5 mm, height 3 mm height) (Made by Asahi Kasei Chemicals Co., Ltd., which softens at 130 ° C. or higher but does not have a melting point) 50 parts by weight, 25 parts by weight of a surfactant are added, and the rotation speed of the stirring member is 50 rpm and the jacket temperature is 110 ° C. The mixture was heated and stirred for 60 minutes to soften the polyester resin (melt kneading step). The media was dispersed in the softened resin. Next, 6 parts by mass of an aqueous sodium hydroxide solution as a basic substance was added. Next, 600 parts by mass of pure water was gradually added while maintaining the temperature in the kneading vessel at 95 ° C. or higher. When the addition was completed, the mixture was emulsified and dispersed to obtain a binder resin aqueous dispersion. The obtained resin water dispersion had a volume average particle size of 115 nm and a particle size distribution that was unimodal. These results are summarized in Table 1.

体積平均粒径は、ナノトラックUPA(日機装株式会社製)を用いて測定することにより求めた。具体的には、ナノトラックUPA(日機装株式会社製)で測定される樹脂水分散液の粒度分布を基にして分割された粒度範囲(チャネル)に対して体積を小径側から累積分布を描いて、累積16%となる粒径を体積D16v、累積50%となる粒径を体積D50v、累積84%となる粒径を体積D84vと定義し、D50vを体積平均粒径として求めた。   The volume average particle diameter was determined by measuring using Nanotrac UPA (Nikkiso Co., Ltd.). Specifically, the cumulative distribution is drawn from the small diameter side to the particle size range (channel) divided based on the particle size distribution of the resin water dispersion measured by Nanotrack UPA (manufactured by Nikkiso Co., Ltd.). In addition, the particle diameter of cumulative 16% was defined as volume D16v, the particle diameter of cumulative 50% was defined as volume D50v, the particle diameter of cumulative 84% was defined as volume D84v, and D50v was determined as the volume average particle diameter.

<実施例2>
(結着樹脂着色分散液の調整)
まず、混練容器に、結着樹脂としてのポリエステル樹脂(融点(Tm)105℃以上109℃以下)270質量部、着色剤としてのマゼンタ顔料15質量部、離型剤15質量部、メディア(平均粒子直径2.5mm、高さ約3mmの円柱状のスチレン系樹脂変性体(旭化成ケミカルズ株式会社製)であって、130℃以上で軟化するが融点を持たないもの)100質量部を添加し、攪拌部材の回転数50rpm、ジャケット温度110℃として、30分間加熱撹拌し、混合物を軟化させた(溶融混練工程)。なお、メディアは軟化している混合物中に分散していた。次に、界面活性剤25質量部と、塩基性物質としての水酸化カリウム水溶液7.5質量部を添加した。次いで、混練容器内の温度を95℃以上に維持しながら、純水600質量部を徐々に添加した。添加完了により、赤色着色分散液を得た。得られた着色分散液の体積平均粒径は164nmであり、粒度分布は単峰性であった。これらの結果を表1にまとめた。
<Example 2>
(Adjustment of binder resin coloring dispersion)
First, in a kneading container, 270 parts by mass of a polyester resin as a binder resin (melting point (Tm) 105 ° C. or higher and 109 ° C. or lower), 15 parts by mass of a magenta pigment as a colorant, 15 parts by mass of a release agent, media (average particles) A columnar styrene-based resin modified product (made by Asahi Kasei Chemicals Corporation) having a diameter of 2.5 mm and a height of about 3 mm, which is softened at 130 ° C. or higher but does not have a melting point) is added 100 parts by mass and stirred. The mixture was heated and stirred for 30 minutes at a member rotation speed of 50 rpm and a jacket temperature of 110 ° C. to soften the mixture (melt kneading step). The media was dispersed in the softened mixture. Next, 25 parts by mass of a surfactant and 7.5 parts by mass of an aqueous potassium hydroxide solution as a basic substance were added. Next, 600 parts by mass of pure water was gradually added while maintaining the temperature in the kneading vessel at 95 ° C. or higher. Upon completion of the addition, a red colored dispersion was obtained. The obtained color dispersion had a volume average particle size of 164 nm and a unimodal particle size distribution. These results are summarized in Table 1.

<実施例3>
(結着樹脂着色分散液の調整)
まず、混練容器に、結着樹脂としてのポリエステル樹脂(融点(Tm)105℃以上109℃以下)240質量部、着色剤としてのイエロー顔料60質量部、メディア(平均粒子直径2.5mm、高さ約3mmの円柱状のスチレン系樹脂変性体(旭化成ケミカルズ株式会社製)であって、130℃以上で軟化するが融点を持たないもの)100質量部を添加し、攪拌部材の回転数50rpm、ジャケット温度110℃として、30分間加熱撹拌し、混合物を軟化させた(溶融混練工程)。なお、メディアは軟化している混合物中に分散していた。次に、界面活性剤25質量部と、塩基性物質としての水酸化カリウム水溶液6.5質量部を添加した。次いで、混練容器内の温度を95℃以上に維持しながら、純水600質量部を徐々に添加した。添加完了により黄色着色分散液を得た。得られた着色分散液の体積平均粒径は140nmであり、粒度分布は単峰性であった。これらの結果を表1にまとめた。
<Example 3>
(Adjustment of binder resin coloring dispersion)
First, in a kneading container, 240 parts by mass of a polyester resin (melting point (Tm) 105 ° C. to 109 ° C.) as a binder resin, 60 parts by mass of a yellow pigment as a colorant, media (average particle diameter 2.5 mm, height) About 3 mm cylindrical modified styrenic resin (made by Asahi Kasei Chemicals Co., Ltd., which softens at 130 ° C. or higher but does not have a melting point), 100 parts by mass, stirring member rotation speed 50 rpm, jacket The mixture was heated and stirred at a temperature of 110 ° C. for 30 minutes to soften the mixture (melt kneading step). The media was dispersed in the softened mixture. Next, 25 parts by mass of a surfactant and 6.5 parts by mass of an aqueous potassium hydroxide solution as a basic substance were added. Next, 600 parts by mass of pure water was gradually added while maintaining the temperature in the kneading vessel at 95 ° C. or higher. A yellow colored dispersion was obtained upon completion of the addition. The obtained color dispersion had a volume average particle size of 140 nm and a unimodal particle size distribution. These results are summarized in Table 1.

<実施例4>
軟化点が80℃であるメディア(旭化成ケミカルズ株式会社製社製、円柱状のスチレン系樹脂変性体)を用いたこと以外は、実施例1と同様に結着樹脂分散液を調整した。その結果、結着樹脂分散液の体積平均粒子径は285nmであり、粒度分布は単峰性であった。これらの結果を表1にまとめた。
<Example 4>
A binder resin dispersion was prepared in the same manner as in Example 1 except that a medium having a softening point of 80 ° C. (made by Asahi Kasei Chemicals Co., Ltd., a cylindrical styrenic resin modified product) was used. As a result, the volume average particle size of the binder resin dispersion was 285 nm, and the particle size distribution was unimodal. These results are summarized in Table 1.

<比較例>
メディアを添加しないこと以外は、実施例1と同様に結着樹脂分散液を調整した。その結果、結着樹脂分散液は得られるものの、結着樹脂分散液の体積平均粒子径は825nmであり、粒度分布は多峰性で、各実施例より広がっていた。これらの結果を表1にまとめた。
<Comparative example>
A binder resin dispersion was prepared in the same manner as in Example 1 except that no media was added. As a result, although a binder resin dispersion was obtained, the volume average particle diameter of the binder resin dispersion was 825 nm, the particle size distribution was multimodal, and was wider than in each example. These results are summarized in Table 1.

Figure 2014018745
Figure 2014018745

混練処理の際にメディアを投入した実施例1〜4では、混練処理後の粒子(結着樹脂の粒子)の体積平均粒径は、混練処理の際にメディアを投入していない比較例における混練処理後の粒子(結着樹脂の粒子)の体積平均粒径より小粒径化した。混練処理の際にメディアを投入した実施例1〜4の混練処理後の粒子の粒度分布は、いずれも単峰性であったが、特に、結着樹脂の融解温度より高い軟化点を有するメディアを用いた実施例1〜3は、結着樹脂の融解温度より低い軟化点を有するメディアを用いた実施例4より、粒度分布の拡がりが抑制された。また、結着樹脂の融点より高い軟化点を有するメディアを用いた実施例1〜3において、混練処理後のメディアを目視により観察した結果、メディアの変形は観察されなかった。   In Examples 1 to 4 in which the media was added during the kneading process, the volume average particle diameter of the particles after the kneading process (binder resin particles) was the same as in the comparative example in which no media was input during the kneading process. The particle size was made smaller than the volume average particle size of the treated particles (binder resin particles). The particle size distribution of the particles after the kneading treatment in Examples 1 to 4 in which the media was added during the kneading treatment was unimodal, but in particular, the media having a softening point higher than the melting temperature of the binder resin. In Examples 1 to 3 using the above, the spread of the particle size distribution was suppressed more than in Example 4 using a medium having a softening point lower than the melting temperature of the binder resin. Further, in Examples 1 to 3 using media having a softening point higher than the melting point of the binder resin, the media after the kneading treatment were visually observed. As a result, no deformation of the media was observed.

1 被混練物の混練機、10 混練容器、12 攪拌機、14 加熱用ジャケット、16 投入口、18 モータ、20 回転軸、22 攪拌部材。   DESCRIPTION OF SYMBOLS 1 Kneading machine of to-be-kneaded material, 10 Kneading container, 12 Stirrer, 14 Jacket for heating, 16 Inlet, 18 Motor, 20 Rotating shaft, 22 Stirring member.

Claims (3)

結着樹脂を含む被混練物を混練機に投入し、前記混練機内で加熱しながら前記被混練物を混練する混練工程を含み、
前記溶融混練工程では、前記混練機に分散媒体を投入することを特徴とする被混練物の混練乳化分散方法。
A kneading step of charging a kneaded material containing a binder resin into a kneader and kneading the kneaded material while heating in the kneader;
In the melt-kneading step, a dispersion medium is introduced into the kneader.
前記分散媒体の軟化点が、前記結着樹脂の融点より高いことを特徴とする請求項1記載の被混練物の混練乳化分散方法。   The method for kneading and emulsifying and dispersing a material to be kneaded according to claim 1, wherein the softening point of the dispersion medium is higher than the melting point of the binder resin. 分散媒体と、
結着樹脂を含む被混練物及び前記分散媒体が投入される混練容器と、
前記混練容器内に設けられた攪拌部材と、
前記被混練物を加熱する加熱手段と、を備えることを特徴とする被混練物の混練機。
A dispersion medium;
A kneaded container containing a binder to be kneaded and the dispersion medium;
A stirring member provided in the kneading vessel;
And a heating means for heating the material to be kneaded.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6159455A (en) * 1984-08-31 1986-03-26 Canon Inc Toner
JPS62201462A (en) * 1986-02-28 1987-09-05 Canon Inc Production of toner or capsuled toner for developing electrostatic charge image
JPS62209466A (en) * 1986-03-10 1987-09-14 Canon Inc Resin composition for toner and toner for developing electrostatic charge image
JPS62223764A (en) * 1986-03-25 1987-10-01 Canon Inc Capsuled toner
JPH05123558A (en) * 1991-11-07 1993-05-21 Mitsui Miike Kakoki Kk Media stirring type kneader
JP2011126089A (en) * 2009-12-16 2011-06-30 Ricoh Co Ltd Kneading apparatus and toner manufacturing method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6159455A (en) * 1984-08-31 1986-03-26 Canon Inc Toner
JPS62201462A (en) * 1986-02-28 1987-09-05 Canon Inc Production of toner or capsuled toner for developing electrostatic charge image
JPS62209466A (en) * 1986-03-10 1987-09-14 Canon Inc Resin composition for toner and toner for developing electrostatic charge image
JPS62223764A (en) * 1986-03-25 1987-10-01 Canon Inc Capsuled toner
JPH05123558A (en) * 1991-11-07 1993-05-21 Mitsui Miike Kakoki Kk Media stirring type kneader
JP2011126089A (en) * 2009-12-16 2011-06-30 Ricoh Co Ltd Kneading apparatus and toner manufacturing method

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