JP4779763B2 - Method for producing toner for electrophotography - Google Patents

Method for producing toner for electrophotography Download PDF

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JP4779763B2
JP4779763B2 JP2006094671A JP2006094671A JP4779763B2 JP 4779763 B2 JP4779763 B2 JP 4779763B2 JP 2006094671 A JP2006094671 A JP 2006094671A JP 2006094671 A JP2006094671 A JP 2006094671A JP 4779763 B2 JP4779763 B2 JP 4779763B2
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toner
fine powder
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正博 前田
忠洋 椿
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Casio Computer Co Ltd
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本発明は、電子写真用トナーの製造方法に係り、特に、カブリ特性、画質、及び耐久性の良好な電子写真用トナーの製造方法及びそれにより製造されたトナーに関する。   The present invention relates to a method for producing an electrophotographic toner, and more particularly, to a method for producing an electrophotographic toner having good fog characteristics, image quality, and durability, and a toner produced thereby.

電子写真方式による画像形成は、一般に、帯電させたトナーにより静電荷像を現像して可視化し、現像により得られたトナー像を用紙に転写し、定着することにより行われる。このような画像形成に用いられるトナーの製造方法としては、粉砕法、重合法等があるが、一般には粉砕法が主流を占めている。   In general, image formation by electrophotography is performed by developing and visualizing an electrostatic image with charged toner, and transferring and fixing the toner image obtained by development onto a sheet. As a method for producing such a toner used for image formation, there are a pulverization method, a polymerization method, and the like. In general, the pulverization method dominates.

粉砕法の一般的な製造方法は、結着樹脂、着色剤、離型剤、及び帯電制御剤等の原料を乾式で混合した後、2軸押出機などで溶融混練し、冷却固化した後に粗粉砕を行い、混練粗砕物を得る。その後、ジェットミルなどで微粉砕を行い、適切な粒度分布になるように分級機で粒度調整を行う。更にシリカなどと一緒に混合機で混合することで表面処理を行い、トナーを得るものである。   A general production method of the pulverization method is to mix raw materials such as a binder resin, a colorant, a release agent, and a charge control agent in a dry manner, then melt and knead with a twin-screw extruder or the like, and after cooling and solidifying, Crushing is performed to obtain a kneaded crushed material. Thereafter, fine pulverization is performed with a jet mill or the like, and the particle size is adjusted with a classifier so as to obtain an appropriate particle size distribution. Further, the toner is obtained by performing surface treatment by mixing with silica etc. in a mixer.

このような粉砕トナーの製造工程では、粉砕分級時に規定粒度以下の微粉が発生するが、このような微紛は破棄されていた。そこで、材料の歩留まり向上及び廃棄物低減のため、微粉を再利用することが従来から行われている。この場合、規定粒度以下の微粉の割合は、全体の10〜40質量%程度であり、再利用する目的からしても、発生した微粉は全て製造工程に戻すことが好ましい。しかし、微粉はいわば粒度の小さな未外添トナーであるため、その粉体特性は、嵩密度が低く、流動性が悪く、また、比表面積が大きいため、帯電性及び付着力が高い。   In such a pulverized toner manufacturing process, fine powder having a prescribed particle size or less is generated during pulverization classification, but such fine powder has been discarded. Thus, in order to improve the yield of materials and reduce waste, it has been conventionally practiced to reuse fine powder. In this case, the ratio of fine powder having a specified particle size or less is about 10 to 40% by mass of the whole, and it is preferable to return all generated fine powder to the manufacturing process even for the purpose of reuse. However, since the fine powder is an additive-free toner with a small particle size, its powder characteristics are low in bulk density, poor fluidity, and large in specific surface area, so that it has high chargeability and adhesion.

また、粉砕時に、離型剤や帯電制御剤が粉砕界面になる場合が多く、微粉の組成は、それら離型剤や帯電制御剤が多く含まれることとなり、微粉を再利用する場合は、原料混合時に均一に分散することが好ましい。   In addition, during pulverization, the release agent and charge control agent often become the pulverization interface, and the composition of the fine powder contains a lot of the release agent and charge control agent. It is preferable to disperse uniformly during mixing.

しかし、これまでのように、微粉をそのまま原料混合に戻したのでは、微粉の流動性が悪いために原料混合の際、撹拌の強度が得られなかったり、帯電性及び付着性の高い帯電制御剤や離型剤と選択的に凝集を起こすなど、均一な原料混合が困難であった。   However, as in the past, if the fine powder is returned to the raw material mixture as it is, the flowability of the fine powder is poor, so the mixing strength of the raw material cannot be obtained, or the charge control with high chargeability and adhesion It was difficult to mix the raw materials uniformly, such as causing selective aggregation with the agent and mold release agent.

また、近年のトナーへの要求として、トナーの小粒径化があり、発生する微粉の粒径は小さくなり、発生量も増える傾向にある。微粉の粒径が小さくなることで、嵩密度はより低くなり、帯電性及び付着力は高くなり、不具合は顕著となる。更に、微粉の戻し量が増えることも、均一な原料混合を妨げることとなる。   Further, as a recent demand for toner, there is a reduction in the particle size of the toner, and the particle size of the generated fine powder tends to be small and the amount of generation tends to increase. By reducing the particle size of the fine powder, the bulk density becomes lower, the chargeability and the adhesive force become higher, and the problem becomes remarkable. Furthermore, an increase in the amount of fine powder returned also hinders uniform raw material mixing.

このような不具合を解消するため、微粉を戻さない状態で先ず混合し、その後、微粉を戻し、再度混合する方法が提案されている(例えば、特許文献1参照)。しかしながら、この方法では、微粉をそのまま添加するため、微粉の粒径が小さく、戻し量が多い場合、十分な効果が発揮できない。   In order to eliminate such problems, a method has been proposed in which the fine powder is first mixed in a state where the fine powder is not returned, and then the fine powder is returned and mixed again (for example, see Patent Document 1). However, in this method, since the fine powder is added as it is, when the particle diameter of the fine powder is small and the return amount is large, a sufficient effect cannot be exhibited.

原料混合が不均一な場合、トナー粒子の帯電性にばらつきが生じ、白紙印字部の感光体ドラム上にトナーが移ってしまい、白紙かぶりが悪化する。また、白紙印字が続いた場合、トナーを印字していないにも関わらず、カブリトナーによりトナー残量が減ってしまうという不具合が発生する。更に、離型剤が不均一に分散した場合、特にドクターブレードと現像ロールとの摩擦でトナーに帯電を付与する非磁性一成分では、ブレードにトナーが融着し、現像ロール上にトナー薄層を形成できなくなり、結果として白スジの画像を発生させてしまう。   If the mixing of the raw materials is not uniform, the charging property of the toner particles varies, and the toner moves onto the photosensitive drum of the blank paper printing portion, resulting in a worse white paper fog. In addition, when blank paper printing continues, there is a problem that the toner remaining amount is reduced by fog toner even though toner is not printed. Furthermore, when the release agent is dispersed non-uniformly, particularly in the case of a non-magnetic one component that imparts charge to the toner by friction between the doctor blade and the developing roll, the toner is fused to the blade, and a thin toner layer is formed on the developing roll As a result, a white streak image is generated.

微粉を再利用する際の別の問題として、原料混合後の混合粉体の嵩密度が低くなり、混練供給工程でフィードネック現象を起こすことが挙げられる。フィードネック現象とは、嵩密度の低い多くの空気を抱え込んだ原料粉末は、樹脂の溶融過程において、空気が絞り出されて供給側へ戻るが、その分量が多いため、供給しようとする原料を押し戻す作用をすることである。そのため、スクリューへの原料の噛み込みが悪化し、混練機で混練できる量が低下してしまう。   Another problem when reusing fine powder is that the bulk density of the mixed powder after mixing the raw materials becomes low, causing a feed neck phenomenon in the kneading and supplying step. The feed neck phenomenon is a raw material powder that contains a lot of air with a low bulk density.In the resin melting process, the air is squeezed out and returns to the supply side. It acts to push back. Therefore, the biting of the raw material into the screw is deteriorated, and the amount that can be kneaded by the kneader is reduced.

生産量を上げようとしてスクリュー回転数を上げても、十分な効果は得られない上、樹脂の分子切断が顕著になり、ホットオフセットが発生するなどの不具合が生じる。混練温度を上げるなどの対策では、樹脂の粘度が低下し、材料の分散性が悪化してしまう。   Even if the screw rotation speed is increased in order to increase the production amount, a sufficient effect cannot be obtained, and the molecular cutting of the resin becomes remarkable, causing problems such as occurrence of hot offset. By taking measures such as increasing the kneading temperature, the viscosity of the resin decreases and the dispersibility of the material deteriorates.

このような問題を解決するため、微粉を造粒したのち原料混合工程に戻す方法が提案されている(例えば、特許文献2,3)。この方法によれば、微粉は圧縮造粒されることで、嵩密度が高くなり、混練工程での供給量の低下がなく、画像劣化が生ずることなく、微粉を再利用することができる。   In order to solve such problems, methods have been proposed in which fine powder is granulated and then returned to the raw material mixing step (for example, Patent Documents 2 and 3). According to this method, the fine powder is compressed and granulated, so that the bulk density is increased, the supply amount in the kneading process is not reduced, and the fine powder can be reused without causing image deterioration.

しかし、上記のような方法では、造粒機の設備導入が必要であり、製造工程が増えるという問題がある。   However, the method as described above requires the introduction of a granulator facility, which increases the number of manufacturing steps.

一方、顔料マスターバッチを製造する際に、水を添加して混練することが提案されている(例えば、特許文献4参照)。しかし、この提案は、分級工程で発生した微粉を混合工程に戻した場合に生ずる問題を何ら解決するものではない。
特開平5−34976号公報 特開平6−266157号公報 特開平6−266158号公報 特開2004−191787号公報
On the other hand, when manufacturing a pigment masterbatch, adding water and kneading | mixing is proposed (for example, refer patent document 4). However, this proposal does not solve the problem that occurs when the fine powder generated in the classification process is returned to the mixing process.
Japanese Patent Laid-Open No. 5-34976 JP-A-6-266157 JP-A-6-266158 JP 2004-191787 A

本発明は、以上のような事情の下になされ、より簡便な方法で、微粉を再利用するとともに、材料の分散性を向上させ、それによってカブリ特性、画質、及び耐久性の良好な電子写真用トナーを製造する方法及びそれにより製造されたトナーを提供することを目的とする。   The present invention has been made under the circumstances as described above, and reuses fine powder in a simpler method and improves the dispersibility of the material, thereby improving electrophotographic characteristics of fog characteristics, image quality, and durability. It is an object of the present invention to provide a method for producing a toner and a toner produced thereby.

上記課題を解決するため、本発明の第1の態様は、結着樹脂、着色剤、離型剤、及び帯電制御剤を含む原料を混合する工程、原料混合物を溶融混練する工程、混練物を冷却固化した後、粉砕する工程、及び粉砕物を分級する工程を具備する電子写真用トナーの製造方法において、前記分級工程で発生した規定粒度以下の微粉を再利用すべく、前記原料100質量部に対し5〜35質量部となるよう前記混合工程に戻すとともに、この混合工程において、前記微粉量の10〜50質量%の水を添加して混合することを特徴とする電子写真用トナーの製造方法を提供する。 In order to solve the above problems, a first aspect of the present invention includes a step of mixing raw materials including a binder resin, a colorant, a release agent, and a charge control agent, a step of melt-kneading the raw material mixture, and a kneaded product. In a method for producing an electrophotographic toner comprising a step of pulverizing and solidifying after cooling and a step of classifying a pulverized product, 100 parts by mass of the raw material is used to reuse fine powder having a particle size of not more than a specified particle size generated in the classification step. to together be returned to the mixing step so as to be 5 to 35 parts by weight, in the mixing step, the electrophotographic toner, which comprises mixing with the addition of 10 to 50 mass% of water in the amount of fine powder A manufacturing method is provided.

このような電子写真用トナーの製造方法において、離型剤としてカルナバワックスを用いることができる。   In such a method for producing an electrophotographic toner, carnauba wax can be used as a release agent.

以上の方法により製造された電子写真用トナーは、5〜7μmの粒径を有することが望ましい。   The electrophotographic toner produced by the above method desirably has a particle size of 5 to 7 μm.

本発明の第2の態様は、以上の方法により製造された電子写真用トナーを提供する The second aspect of the present invention provides an electrophotographic toner produced by the above method .

本発明によると、微粉を原料混合に戻し再利用する際に、水を添加することで、微粉と内添剤の選択的な凝集を防止し、内添剤の分散性を向上させることができ、それによってカブリ特性、画質、及び耐久性の良好な電子写真用トナーを得ることができる。   According to the present invention, when the fine powder is returned to the raw material mixture and reused, by adding water, selective aggregation of the fine powder and the internal additive can be prevented and the dispersibility of the internal additive can be improved. As a result, an electrophotographic toner having good fog characteristics, image quality, and durability can be obtained.

以下、発明を実施するための最良の形態について説明する。   The best mode for carrying out the invention will be described below.

本発明の一実施形態に係る電子写真用トナーの製造方法は、分級工程で発生した規定粒度以下の微粉を混合工程に戻し、混合工程において原料を混合するに際し、水を添加することを特徴とする。   The method for producing an electrophotographic toner according to an embodiment of the present invention is characterized in that fine powder having a particle size equal to or smaller than a specified particle size generated in the classification step is returned to the mixing step, and water is added when mixing the raw materials in the mixing step. To do.

このように、分級工程で発生した規定粒度以下の微粉を混合工程に戻して原料を混合するに際し、水を添加することにより、次のような作用が生ずるものと考えられる。   Thus, it is considered that when the fine powder having a particle size of not more than the specified particle size generated in the classification step is returned to the mixing step and the raw materials are mixed, the following effects are produced by adding water.

即ち、原料粉体全体の静電気が中和され、微粉と帯電制御剤などとの選択的な凝集が緩和されることにより、従来よりも均一な混合が生じる。また、混練工程で樹脂が溶融する際、原料に含まれた水分の蒸発による吸熱が起こり、樹脂温度を下げる働きにより、帯電制御剤等の内添剤の分散性が向上する。さらに、水を添加することで得られる静電気の中和により、材料同士の静電反発が減少し、また粉体の粘性が上昇し、スクリューへの噛み込みが向上し、混練工程への原料の供給性能が向上する。   That is, the static electricity of the whole raw material powder is neutralized, and the selective aggregation between the fine powder and the charge control agent is alleviated, so that more uniform mixing than in the past occurs. In addition, when the resin is melted in the kneading step, heat absorption occurs due to evaporation of water contained in the raw material, and the dispersibility of the internal additive such as the charge control agent is improved by the function of lowering the resin temperature. Furthermore, neutralization of static electricity obtained by adding water reduces electrostatic repulsion between materials, increases the viscosity of the powder, improves biting into the screw, and improves the raw material to the kneading process. Supply performance is improved.

以上の作用により、戻された微粉を含む原料の混合の際に水を添加することにより、カブリ特性、画質、及び耐久性の良好な電子写真用トナーを得ることができる。   As a result of the above action, an electrophotographic toner having good fog characteristics, image quality, and durability can be obtained by adding water during mixing of the raw material containing the returned fine powder.

本発明の一実施形態に係る電子写真用トナーの製造方法において、分級工程で発生し、混合工程に戻される規定粒度以下の微粉の量は、原料100質量部に対し5〜35質量部でなければならない。微粉の量が5質量部未満では、耐久性が低下し、35質量部を超えると、カブリ特性及び耐久性が低下する。   In the method for producing an electrophotographic toner according to an embodiment of the present invention, the amount of fine powder having a specified particle size or less generated in the classification step and returned to the mixing step should be 5 to 35 parts by mass with respect to 100 parts by mass of the raw material. I must. When the amount of the fine powder is less than 5 parts by mass, the durability is lowered, and when it exceeds 35 parts by mass, the fog characteristic and the durability are lowered.

また、添加される水の量は、微粉量の10〜50質量%でなければならない。水の量が10質量%未満では、カブリ特性及び耐久性が低下し、50質量%を超えると、カブリ特性、画質、及び耐久性のすべてが低下する。   Moreover, the quantity of the water added must be 10-50 mass% of the amount of fine powder. If the amount of water is less than 10% by mass, the fog characteristics and durability deteriorate, and if it exceeds 50% by mass, all of fog characteristics, image quality, and durability decrease.

なお、混合工程に戻される微紛の規定粒度は、通常5μm以下である。   The specified particle size of the fine powder returned to the mixing step is usually 5 μm or less.

本発明の一実施形態に係るトナーの製造方法は、次のようにして行われる。   The toner manufacturing method according to an embodiment of the present invention is performed as follows.

まず、結着樹脂、着色剤、離型剤、及び帯電制御剤等の材料の計量を行う。このとき、後述する分級工程から戻される微粉量を原料100質量部に対し5〜35質量部の範囲内で決定する。   First, materials such as a binder resin, a colorant, a release agent, and a charge control agent are measured. At this time, the fine powder amount returned from the classification step described later is determined within a range of 5 to 35 parts by mass with respect to 100 parts by mass of the raw material.

次に、計量された材料及び所定量の微紛を混合機により混合する。混合機としては、ヘンシェルミキサー、スーパーミキサー、V型ブレンダー、ナウターミキサー等、任意のものを用いることが出来る。
混合の際には、微粉量の10〜50質量%の水を添加する。水の添加は、例えば、図1に示すようなヘンシェルミキサー1を用いて行うことができる。即ち、ヘンシェルミキサー1の上部蓋の材料添加口にゴム栓3を介して分液ロート2が取り付けられており、この分液ロート2内には所定量の蒸留水が収容されている。ヘンシェルミキサー1内の原料を混合する際に、分液ロート2のコックを開けて、水の添加を行う。混合終了後、原料混合物は、排出口4から排出される。
Next, the weighed material and a predetermined amount of fine powder are mixed by a mixer. As a mixing machine, arbitrary things, such as a Henschel mixer, a super mixer, a V-type blender, and a Nauta mixer, can be used.
At the time of mixing, 10-50 mass% of water of the amount of fine powder is added. The addition of water can be performed using, for example, a Henschel mixer 1 as shown in FIG. That is, a separating funnel 2 is attached to the material addition port of the upper lid of the Henschel mixer 1 via the rubber plug 3, and a predetermined amount of distilled water is accommodated in the separating funnel 2. When mixing the raw materials in the Henschel mixer 1, the cock of the separatory funnel 2 is opened and water is added. After mixing, the raw material mixture is discharged from the discharge port 4.

その後、原料混合物を溶融混練する。混練機としては、特に限定されないが、例えば、2軸混練機、オープンロール型混練機等を用いることができる。オープンロール型混練機としては、連続式2本ロールミル、連続式3本ロールミル、及びバッチ式ロールミル等、任意の型のものを用いることができる。このような溶融混練に際しては、混練機に供給される原料混合物に偏析が少ないため、各成分が均一かつ微細に分散される。   Thereafter, the raw material mixture is melt-kneaded. Although it does not specifically limit as a kneader, For example, a biaxial kneader, an open roll type kneader, etc. can be used. As an open roll type kneader, an arbitrary type such as a continuous two-roll mill, a continuous three-roll mill, and a batch-type roll mill can be used. In such melt-kneading, since the raw material mixture supplied to the kneader has little segregation, each component is uniformly and finely dispersed.

混練機で混練され、排出された溶融混練物は、通常、トナーの製造に用いられる方法に従って、冷却され、粉砕され、所定の粒度に分級されて、トナー粒子母体が得られる。冷却手段、粉砕手段及び分級手段は、特に限定されず、通常トナーの製造に用いられるものを採用することが出来る。例えば、冷却には、圧延や空気流の吹き付けによる冷却手段を用いることができ、粉砕には、衝突板式粉砕機等の気流粉砕機を用いることができ、分級には、様々な気流分級機を用いることができる。   The melt-kneaded material kneaded and discharged by a kneader is usually cooled, pulverized, and classified into a predetermined particle size according to a method used for producing a toner to obtain a toner particle matrix. The cooling means, the pulverizing means, and the classification means are not particularly limited, and those usually used for toner production can be employed. For example, a cooling means by rolling or blowing an air flow can be used for cooling, and an airflow pulverizer such as a collision plate pulverizer can be used for pulverization, and various airflow classifiers can be used for classification. Can be used.

このようにして得たトナー粒子母体に、シリカ等の外添剤を加え、混合・攪拌することにより、電子写真用トナーが得られる。   An electrophotographic toner can be obtained by adding an external additive such as silica to the toner particle matrix thus obtained, followed by mixing and stirring.

以上のように、本発明の一実施形態に係る電子写真用トナーの製造方法により得られたトナーは、分級工程から戻された微紛を原料とともに混合する際に、水を添加したため、混合が均一に行われ、また混練の際には水の蒸発による吸熱作用により樹脂温度を下げて、添加剤の分散性が向上したことにより、カブリ特性、画質、耐久性の良好なトナーを得ることができる。   As described above, since the toner obtained by the method for producing an electrophotographic toner according to the embodiment of the present invention is mixed with the raw material when the fine powder returned from the classification step is mixed with water, mixing is performed. It is performed uniformly, and when kneading, the resin temperature is lowered by the endothermic action of water evaporation, and the dispersibility of the additive is improved, so that a toner having good fog characteristics, image quality, and durability can be obtained. it can.

図2は、以上説明した本発明の電子写真用トナーを用いて画像形成をするための画像形成装置を示す。   FIG. 2 shows an image forming apparatus for forming an image using the electrophotographic toner of the present invention described above.

図2に示す画像形成装置は、現像装置11と感光体ドラム12とを備えている。現像装置11は、内部にトナーを収容するトナーホッパー13、トナーを供給する供給ロール14、供給ロール14から供給されたトナーを感光体ドラム12に付与し、感光体ドラム12の表面の静電潜像を現像する弾性体からなる現像ロール15、この現像ロール15に摺接して、現像ロール15表面のトナー層の厚さを規制するドクターブレード16を具備している。感光体ドラム12の周囲には、感光体ドラム12の表面を一様に帯電する帯電ロール17、帯電した感光体ドラム12の表面に原稿像を露光して、静電潜像を形成するLED18が配置されている。   The image forming apparatus shown in FIG. 2 includes a developing device 11 and a photosensitive drum 12. The developing device 11 applies a toner hopper 13 that contains toner therein, a supply roll 14 that supplies toner, and toner supplied from the supply roll 14 to the photosensitive drum 12, and electrostatic latent on the surface of the photosensitive drum 12. A developing roll 15 made of an elastic body for developing an image, and a doctor blade 16 that is in sliding contact with the developing roll 15 and regulates the thickness of the toner layer on the surface of the developing roll 15 are provided. Around the photosensitive drum 12, there are a charging roll 17 for uniformly charging the surface of the photosensitive drum 12, and an LED 18 for exposing a document image to the charged surface of the photosensitive drum 12 to form an electrostatic latent image. Has been placed.

感光体ドラム12の下部には、転写ベルト19が感光体ドラム12の回転とともに走行しており、転写シート20により感光体ドラム12と接触して、現像されたトナー像は、用紙21に転写される。なお、転写後も感光体ドラム12の表面に残留する、転写されなかったトナーは、クリーニングブレード22により除去される。   A transfer belt 19 runs along with the rotation of the photoconductive drum 12 below the photoconductive drum 12. The developed toner image is transferred onto the paper 21 by contacting the photoconductive drum 12 by the transfer sheet 20. The The toner that has not been transferred and remains on the surface of the photosensitive drum 12 even after the transfer is removed by the cleaning blade 22.

以上のように構成される画像形成装置に上述した本実施形態に係るトナーを実装し、弾性現像ロールの搬送速度を100mm/秒以上の高速で動作させても、外添剤の凝集による生ずるカブリ特性、画質、耐久性は良好であり、ドクターブレード上の融着は生じない。   Even if the toner according to the present embodiment described above is mounted on the image forming apparatus configured as described above and the elastic developing roll is transported at a high speed of 100 mm / second or more, fog caused by aggregation of external additives occurs. Properties, image quality, and durability are good, and no fusion on the doctor blade occurs.

また、画像形成装置の定着器がオイルの供給機構を持たないものであっても、定着は支障なく行うことができる。   Even if the fixing device of the image forming apparatus does not have an oil supply mechanism, fixing can be performed without any problem.

以下、本発明の参考例、実施例、及び比較例を示し、本発明について更に具体的に説明する。   Hereinafter, the present invention will be described in more detail with reference to reference examples, examples, and comparative examples.

最初に、以下の実施例及び比較例における原料混合条件、水の添加条件、外添剤混合条件、混練条件、軟化点、ガラス転移点及び粒径の測定方法について説明する。   First, raw material mixing conditions, water addition conditions, external additive mixing conditions, kneading conditions, softening points, glass transition points, and particle diameter measuring methods in the following Examples and Comparative Examples will be described.

1.原料混合条件
原料の混合は、図1に示すようなヘンシェルミキサー1を用いて行い、投入量はヘンシェルミキサー1の容積に対し、70〜80%の範囲になるように調整する。撹拌羽としては、標準の羽を装着し、周速20m/secで回転させる。
1. Raw material mixing conditions The raw materials are mixed using a Henschel mixer 1 as shown in FIG. 1, and the input amount is adjusted to be in the range of 70 to 80% with respect to the volume of the Henschel mixer 1. As a stirring blade, a standard blade is attached and rotated at a peripheral speed of 20 m / sec.

2.水の添加条件
図1に示すヘンシェルミキサー1の上部蓋の材料添加口にゴム栓3を介して取り付けられた分液ロート2内に予め蒸留水を計量しておく。ヘンシェルミキサー1内に収容された原料の撹拌開始10秒後に、分液ロート2のコックを開けて、水の添加をスタートさせ、30秒間の間に必要量の添加を終了させる。
2. Water Addition Conditions Distilled water is weighed in advance into a separating funnel 2 attached via a rubber stopper 3 to the material addition port of the upper lid of the Henschel mixer 1 shown in FIG. 10 seconds after the start of stirring of the raw material stored in the Henschel mixer 1, the cock of the separatory funnel 2 is opened to start the addition of water, and the addition of the necessary amount is completed within 30 seconds.

3.外添剤混合条件
外添剤の混合は、ヘンシェルミキサーを用いて行う。投入量はヘンシェルミキサーの容積に対し、70〜80%の範囲になるように調整する。撹拌羽は強撹拌羽を装着し、周速40m/secで回転させる。
3. External additive mixing conditions The external additive is mixed using a Henschel mixer. The input amount is adjusted to be in the range of 70 to 80% with respect to the volume of the Henschel mixer. The stirring blade is equipped with a strong stirring blade and is rotated at a peripheral speed of 40 m / sec.

4.混練条件
2軸押出機(スクリュウー径43mm、L/D=34)を使用する。混練温度の設定は、スクリュー長さ方向に8分割されたゾーンのうち供給側4ゾーンは70℃、排出側4ゾーンは100℃に設定する。供給量は25kg/hで行う。
4). Kneading conditions A twin screw extruder (screw diameter 43 mm, L / D = 34) is used. The kneading temperature is set to 70 ° C. for the 4 zones on the supply side and 100 ° C. for the 4 zones on the discharge side among the 8 zones divided in the screw length direction. The supply rate is 25 kg / h.

5.軟化点の測定
装置:フローテスター(CFT−500D:島津製作所製)
試料:1g
昇温速度:6℃/分
荷重:20kg
ノズル:直径1mm、長さ1mm
1/2法:試料の半分が流出した温度を軟化点とする。
5. Measurement of softening point Apparatus: Flow tester (CFT-500D: manufactured by Shimadzu Corporation)
Sample: 1g
Temperature increase rate: 6 ° C / min Load: 20kg
Nozzle: 1mm diameter, 1mm length
1/2 method: The temperature at which half of the sample flows out is taken as the softening point.

6.ガラス転移点(Tg)の測定
装置:示差走査熱量計(DSC−60:島津製作所社製)
試料:8mg
昇温条件:10℃/分で160℃まで昇温し、降温速度10℃/分で35℃まで冷却した後、再度10℃/分で160℃まで昇温する。
6). Measurement of glass transition point (Tg) Device: differential scanning calorimeter (DSC-60: manufactured by Shimadzu Corporation)
Sample: 8mg
Temperature raising conditions: The temperature is raised to 160 ° C. at 10 ° C./min, cooled to 35 ° C. at a temperature lowering rate of 10 ° C./min, and then raised again to 160 ° C. at 10 ° C./min.

2回目の昇温時において、転移により得られる曲線部分の2つの接線の交点をガラス転移点とする。   At the time of the second temperature increase, the intersection of two tangents of the curve portion obtained by the transition is defined as the glass transition point.

7.粒径の測定
装置:マルチサイザーII(コールター社製)
試料:ビーカーに試料少量と精製水、界面活性剤を入れ、超音波洗浄器にて分散する。
7). Particle size measurement device: Multisizer II (Coulter)
Sample: Place a small amount of sample, purified water, and surfactant in a beaker and disperse with an ultrasonic cleaner.

測定:アパーチャーは100μmで行い、カウントは50,000個で行い、体積平均粒径を得る。   Measurement: The aperture is 100 μm, the count is 50,000, and the volume average particle diameter is obtained.

参考例(微粉再利用なし)
結着樹脂として、ポリエステル樹脂(軟化点120℃、Tg67℃)を90質量部、着色剤として、C.I.ピグメントレッド122を5質量部、離型剤として、カルナバワックス1号粉末(加藤洋行)を4質量部、帯電制御剤として、E−84(オリエント化学株式会社)を1質量部をヘンシェルミキサー(三井鉱山社製、標準羽装着)に投入し、3分間撹拌混合した。
Reference example (no fine powder reuse)
As a binder resin, 90 parts by mass of a polyester resin (softening point: 120 ° C., Tg: 67 ° C.) and a colorant: I. 5 parts by weight of Pigment Red 122, 4 parts by weight of Carnauba Wax No. 1 powder (Yoyuki Kato) as a release agent, 1 part by weight of E-84 (Orient Chemical Co., Ltd.) as a charge control agent, Henschel mixer (Mitsui (Mine Co., Ltd., equipped with standard wings) and mixed with stirring for 3 minutes.

得られた混合粉体を2軸押出機で溶融混練し、延伸、冷却し、ロートプレックス(ホソカワミクロン社製、2mmスクリーン)で粗粉砕した後、衝突式粉砕機・風力分級機にて、トナー平均粒径が6.0μmになるように粉砕分級を行い、微粒子を得た。得られた微粒子100重量部に外添剤として、「RY200」(疎水性シリカ:日本アエロジル社製)を2重量部添加し、ヘンシェルミキサー(三井鉱山社製、撹拌強化羽装着)で3分間撹拌混合し、トナーを得た。なお、分級工程で規定粒度以下の微粉を得た。得られた微粉の平均粒径は3.5μmであった。  The obtained mixed powder is melt-kneaded with a twin screw extruder, stretched, cooled, coarsely pulverized with a Rotoplex (manufactured by Hosokawa Micron Co., Ltd., 2 mm screen), and then averaged with a collision pulverizer / air classifier. The fine particles were obtained by pulverization and classification so that the particle diameter was 6.0 μm. As an external additive, 2 parts by weight of “RY200” (hydrophobic silica: manufactured by Nippon Aerosil Co., Ltd.) is added to 100 parts by weight of the obtained fine particles, and the mixture is stirred for 3 minutes with a Henschel mixer (manufactured by Mitsui Mining Co., Ltd., equipped with stirring reinforcing blades). The toner was obtained by mixing. In addition, the fine powder below a regulation particle size was obtained at the classification process. The average particle size of the obtained fine powder was 3.5 μm.

実施例1
結着樹脂、着色剤、離型剤、及び帯電制御剤に対し、参考例で得られた微粉25質量部を加え、原料混合の際、混合機上部から水を5重量部添加したことを除いて、参考例1と同様にしてトナーを得た。
Example 1
25 parts by weight of the fine powder obtained in the reference example was added to the binder resin, colorant, release agent, and charge control agent, and 5 parts by weight of water was added from the top of the mixer when mixing the raw materials. Thus, a toner was obtained in the same manner as in Reference Example 1.

比較例1
原料混合の際、水を添加しないことを除いて、実施例1と同様にしてトナーを得た。
Comparative Example 1
A toner was obtained in the same manner as in Example 1 except that water was not added when mixing the raw materials.

比較例2
参考例1で得られた微粉を乾式ロールコンパクタ(フロイント産業社製、TF−208)で造粒し、造粒微粉を得た。
Comparative Example 2
The fine powder obtained in Reference Example 1 was granulated with a dry roll compactor (Freund Sangyo Co., Ltd., TF-208) to obtain granulated fine powder.

ロール径200mm、ロール幅80mm、ロール圧力20MPa、ロール回転数20rpm、供給量が120kg/hになるようにスクリューフィーダー回転数を調整した。整粒器では、スクリーンに2mmの目開きを使用した。造粒前の微粉の嵩密度は0.25g/cm3 、造粒後の微粉の嵩密度は0.53g/cm3 であった。微粉を上記造粒微粉に変えたことを除いて、比較例1と同様にしてトナーを得た。 The screw feeder rotation speed was adjusted so that the roll diameter was 200 mm, the roll width was 80 mm, the roll pressure was 20 MPa, the roll rotation speed was 20 rpm, and the supply amount was 120 kg / h. In the granulator, a 2 mm opening was used for the screen. The bulk density of the fine powder before granulation was 0.25 g / cm 3 , and the bulk density of the fine powder after granulation was 0.53 g / cm 3 . A toner was obtained in the same manner as in Comparative Example 1 except that the fine powder was changed to the granulated fine powder.

実施例2
微粉量を5質量部、水を1質量部としたことを除いて、実施例1と同様にしてトナーを得た。
Example 2
A toner was obtained in the same manner as in Example 1 except that the amount of fine powder was 5 parts by mass and water was 1 part by mass.

実施例3
微粉量を35質量部、水を7質量部としたことを除いて、実施例1と同様にしてトナーを得た。
Example 3
A toner was obtained in the same manner as in Example 1 except that the amount of fine powder was 35 parts by mass and water was 7 parts by mass.

比較例3
微粉量を2質量部としたことを除いて、実施例1と同様にしてトナーを得た。
Comparative Example 3
A toner was obtained in the same manner as in Example 1 except that the amount of fine powder was 2 parts by mass.

比較例4
微粉量を40質量部、水を8質量部としたことを除いて、実施例1と同様にしてトナーを得た。
Comparative Example 4
A toner was obtained in the same manner as in Example 1 except that the amount of fine powder was 40 parts by mass and water was 8 parts by mass.

比較例5
微粉量を25質量部、水を15質量部としたことを除いて、実施例1と同様にしてトナーを得た。
Comparative Example 5
A toner was obtained in the same manner as in Example 1 except that the amount of fine powder was 25 parts by mass and water was 15 parts by mass.

比較例6
微粉量を25質量部、水を2質量部としたことを除いて、実施例1と同様にしてトナーを得た。
Comparative Example 6
A toner was obtained in the same manner as in Example 1 except that the amount of fine powder was 25 parts by mass and water was 2 parts by mass.

以上の参考例、実施例、及び比較例で得たトナー試料について、下記の試験を行い、特性を評価した。   The toner samples obtained in the above Reference Examples, Examples and Comparative Examples were subjected to the following tests and evaluated for characteristics.

試験1−かぶり
非磁性一成分現像装置「カシオページプレストN−5」(カシオ計算機社製:カラープリンタ毎分29枚(A4横)機、プロセススピード129mm/sec)にトナーを実装し、通常環境(25℃、50%RH)において、普通紙(XEROX−P紙A4サイズ)を用いて5%印字画像を10,000枚連続印字したあと、白紙印字を行い、印字している途中でフロント扉を開けることにより、印字を強制終了させ、その時のOPCドラム上のカブリトナーをメンディングテープに写しとり、目視にて比較し、下記の基準で評価した。
Test 1-fogging Non-magnetic one-component developing device "Casio Page Presto N-5" (Casio Computer Co., Ltd .: color printer 29 sheets per minute (A4 horizontal) machine, process speed 129 mm / sec) mounted with toner in normal environment At 25 ° C and 50% RH, after printing 10,000 sheets of 5% print images continuously using plain paper (XEROX-P paper A4 size), white paper is printed and the front door is being printed. Then, the printing was forcibly terminated, the fog toner on the OPC drum at that time was copied onto a mending tape, visually compared, and evaluated according to the following criteria.

◎:参考例よりカブリが少ない
○:参考例と同等
×:参考例よりもカブリが多い
試験2−高画質
試験1で使用した装置を用い、通常環境(25℃、50%RH)において、普通紙(XEROX−P紙A4サイズ)を用いて5%印字画像を10,000枚連続印字したあと、ハーフトーン画像及びベタ画像を印字し、下記の基準で画像の均一性を評価した。
◎: Less fog than the reference example ○: Equivalent to the reference example ×: Test with more fog than the reference example 2-High image quality Normal in normal environment (25 ° C, 50% RH) using the equipment used in test 1 After continuous printing of 10,000 5% print images using paper (XEROX-P paper A4 size), halftone images and solid images were printed, and the uniformity of the images was evaluated according to the following criteria.

◎:参考例より良好
○:参考例と同等
×:参考例よりも均一でない
試験3−耐久性
試験1と同様の装置を用い、通常環境(25℃、50%RH)において、5%印字画像を14,000枚連続印字した。途中、2,000枚おきにベタ画像、ハーフトーン画像を印字しブレード融着による白スジの発生枚数を評価した。
◎: Better than the reference example ○: Equivalent to the reference example ×: Test less uniform than the reference example 3—Durability 5% printed image in the normal environment (25 ° C., 50% RH) using the same equipment as test 1. 14,000 sheets were continuously printed. In the middle, solid images and halftone images were printed every 2,000 sheets, and the number of white lines generated by blade fusion was evaluated.

◎:14,000枚まで発生しない
○:12,000枚以降に発生
×:12,000枚未満で発生
試験4−混練供給性能
混練工程にて、原料供給量を、25kg/hから45kg/hまで5kg/h刻みに徐々に上げていき、フィードネック現象の発生の有無を観察した。
◎: Not generated up to 14,000 sheets ○: Generated after 12,000 sheets ×: Generated with less than 12,000 sheets Test 4-kneading supply performance In the kneading process, the raw material supply amount was changed from 25 kg / h to 45 kg / h. The feed rate was gradually increased to 5 kg / h until the feed neck phenomenon was observed.

◎:40kg/h以上の供給量があれば良好であり、○30kg/h以上であれば許容できる。×25kg/h以下の場合、生産性として十分でない。   A: Good if there is a supply amount of 40 kg / h or more, and ○ 30 kg / h or more is acceptable. When it is 25 kg / h or less, the productivity is not sufficient.

以上の試験結果を下記表に示す。

Figure 0004779763
The above test results are shown in the following table.
Figure 0004779763

上記表から、次のことがわかる。即ち、実施例1〜3では、原料混合時に、分級工程から戻された所定量の微粉と所定量の水を添加することで、十分な混練供給性能を保ったまま、混練することができ、カブリ、高画質、耐久性の良好なトナーを得ることができた。   From the above table, the following can be understood. That is, in Examples 1 to 3, by adding a predetermined amount of fine powder returned from the classification step and a predetermined amount of water during raw material mixing, kneading can be performed while maintaining sufficient kneading supply performance, A toner with good fog, high image quality, and durability could be obtained.

これに対し、水を添加しない比較例1では、カブリ、耐久性、混練供給性能が劣っており、水を添加する代わりに微粉を造粒した比較例2では、耐久性が劣っていた。また、混合する微粉量が少ない比較例3では、耐久性が劣っており、多すぎる比較例4では、カブリ、耐久性、混練供給性能が劣っていた。更に、水の量が多すぎる比較例5では、カブリ、画質、耐久性が劣っており、水の量が少ない比較例6では、カブリ、耐久性が劣っており、混練供給性能が劣っていた。   On the other hand, in Comparative Example 1 in which water was not added, fogging, durability, and kneading supply performance were inferior, and in Comparative Example 2 in which fine powder was granulated instead of adding water, durability was inferior. Moreover, in Comparative Example 3 with a small amount of fine powder to be mixed, durability was inferior, and in Comparative Example 4 in which there was too much, fogging, durability, and kneading supply performance were inferior. Furthermore, in Comparative Example 5 in which the amount of water is too large, fog, image quality, and durability are inferior. In Comparative Example 6, in which the amount of water is small, fog and durability are inferior, and the kneading supply performance is inferior. .

本発明の一実施形態に用いる、水を添加する分液ロートを備えたヘンシェルミキサーを示す図。The figure which shows the Henschel mixer provided with the separating funnel which adds water used for one Embodiment of this invention. 本発明の一実施形態に係るトナーを用いる画像形成装置の概略を示す図。1 is a diagram schematically illustrating an image forming apparatus using toner according to an embodiment of the present invention.

符号の説明Explanation of symbols

1…ヘンシェルミキサー、2…分液ロート、3…ゴム栓、4…排出口、11…現像装置、12…感光体ドラム、13…トナーホッパー、14…供給ロール、15…現像ロール、16…ドクターブレード、17…帯電ロール、18…LED、19…転写ベルト、20…転写シート、21…用紙、22…クリーニングブレード。   DESCRIPTION OF SYMBOLS 1 ... Henschel mixer, 2 ... Separation funnel, 3 ... Rubber stopper, 4 ... Discharge port, 11 ... Developing device, 12 ... Photoconductor drum, 13 ... Toner hopper, 14 ... Supply roll, 15 ... Developing roll, 16 ... Doctor Blade 17, charging roll 18 LED 19 transfer belt 20 transfer sheet 21 paper 22 cleaning blade

Claims (4)

結着樹脂、着色剤、離型剤、及び帯電制御剤を含む原料を混合する工程、
原料混合物を溶融混練する工程、
混練物を冷却固化した後、粉砕する工程、及び
粉砕物を分級する工程
を具備する電子写真用トナーの製造方法において、
前記分級工程で発生した規定粒度以下の微粉を再利用すべく、前記原料100質量部に対し5〜35質量部となるよう前記混合工程に戻すとともに、この混合工程において、前記微粉量の10〜50質量%の水を添加して混合することを特徴とする電子写真用トナーの製造方法。
Mixing raw materials including a binder resin, a colorant, a release agent, and a charge control agent;
A step of melt-kneading the raw material mixture,
In the method for producing an electrophotographic toner comprising the steps of cooling and solidifying the kneaded product and then pulverizing, and classifying the pulverized product,
In order to reuse the fines following provisions particle size generated in the classifying step, the to return to the mixing step so as to be 5 to 35 parts by mass with respect to the raw material 100 parts by weight, 10 in the mixing step, the amount of fine powder A method for producing an electrophotographic toner, comprising adding and mixing ˜50 mass% water.
前記離型剤がカルナバワックスであることを特徴とする請求項1に記載のトナーの製造方法。   The toner production method according to claim 1, wherein the release agent is carnauba wax. 5〜7μmの粒径を有することを特徴とする請求項1又は2に記載のトナーの製造方法。   The toner production method according to claim 1, wherein the toner has a particle size of 5 to 7 μm. 請求項1〜3のいずれかに記載のトナーの製造方法により製造されたことを特徴とする電子写真用トナー。   An electrophotographic toner produced by the toner production method according to claim 1.
JP2006094671A 2006-03-30 2006-03-30 Method for producing toner for electrophotography Expired - Fee Related JP4779763B2 (en)

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