JP2004279871A - Apparatus for evaluating fluidity of powder and electrostatic charge image developing toner - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To stably produce toner with which high image quality can be obtained with good dot reproducibility by using an evaluation apparatus which is high in the accuracy of a fluidity and does not cause individual differences. <P>SOLUTION: The apparatus for measuring the flow property of powder is used for evaluating the fluidity of the toner by allowing a conical rotor to invade the interior of a powder layer compacted by a consolidation means and measuring the torque or load generated when the conical motor moves in the powder layer. The apparatus comprises at least the conical rotor invading the interior of the toner layer while rotating, a meter for detecting the torque acting on the rotating conical rotor, a load cell for detecting the load applied on a container by rotation of the conical rotor and a lifter for vertically moving the conical rotor or the container. The apparatus is equipped with a means for measuring the height of the powder phase prior to the consolidation. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
得られたトナーを潜像担持体がＯＰＣドラム感光体でクリーニング方式がブレードクリーニングである複写機にセットし、画像評価実験を行なった。
その結果、画像のドット再現性は５段階評価でランク４であった。
【００６４】
実施例２
実施例１と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
また、実施例１と同様に、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク４であった。
【００６５】
実施例３
実施例１と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
また、実施例１と同様に、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク５であった。
【００６６】
実施例４
実施例１と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
また、実施例１と同様に、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク５であった。
【００６７】
実施例５
実施例１と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
また、実施例１と同様に、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク５であった。
【００６８】
比較例１
実施例１と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
さらに、実施例１と同様に、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク３であった。
【００６９】
実施例６
＜トナーバインダーの合成＞
冷却管、攪拌機および窒素導入管の付いた反応槽中に、ビスフェノールＡエチレンオキサイド２モル付加物７２４部、イソフタル酸２７６部およびジブチルチンオキサイド２部を入れ、常圧，２３０℃で８時間反応し、さらに１０〜１５ｍｍＨｇの減圧で５時間反応した後、１６０℃まで冷却して、これに３２部の無水フタル酸を加えて２時間反応した。
次いで、８０℃まで冷却し、酢酸エチル中にてイソフォロンジイソシアネート１８８部と２時間反応を行い、イソシアネート含有プレポリマーＩを得た。次いでプレポリマーＩ２６７部とイソホロンジアミン１４部を５０℃で２時間反応させ、重量平均分子量６４０００のウレア変性ポリエステルＩを得た。
上記と同様にビスフェノールＡエチレンオキサイド２モル付加物７２４部、テレフタル酸２７６部を常圧下、２３０℃で８時間重縮合し、次いで１０〜１５ｍｍＨｇの減圧で５時間反応して、ピーク分子量５０００の変性されていないポリエステルＡを得た。
ウレア変性ポリエステルＩ２００部と変性されていないポリエステルＡ８００部を酢酸エチル／ＭＥＫ（１／１）混合溶剤２０００部に溶解、混合し、トナーバインダーＩの酢酸エチル／ＭＥＫ溶液を得た。一部減圧乾燥し、トナーバインダーＩを単離した。分析の結果Ｔｇは６２℃であった。
【００７０】
＜トナーの作製＞
トナーバインダーＩの酢酸エチル／ＭＥＫ溶液 ２４０部
ペンタエリスリトールテトラベヘネート
（溶融粘度２５ｃｐｓ） ２０部
銅フタロシアニンブルー顔料
（Ｃ．Ｉ．ピグメントブルー１５：３） ４部
上記原材料をビーカー内で、６０℃にてＴＫ式ホモミキサーで１２０００ｒｐｍで攪拌し、均一に溶解、分散させてトナー材料溶液を作製した。
イオン交換水 ７０６部
ハイドロキシアパタイト１０％懸濁液
（日本化学工業（株）製スーパタイト１０） ２９４部
ドデシルベンゼンスルホン酸ナトリウム ０．２部
ビーカー内に上記原材料を入れ均一に溶解した。その後６０℃に昇温し、ＴＫ式ホモミキサーで１２０００ｒｐｍに攪拌しながら、上記トナー材料溶液を投入し１０分間攪拌した。ついでこの混合液を攪拌棒および温度計付のフラスコに移し、３０℃まで昇温して減圧下で溶剤を除去し、濾別、洗浄、乾燥した後、風力分級し、トナー粒子を得た。体積平均粒径は６．５μｍであった。このトナー粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを得た。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
上記作製法で得られたトナーとキャリアをキャリア９７．５部に対し、２．５部の割合で混合し、二成分現像剤を作製した。
得られた現像剤を潜像担持体がＯＰＣドラム感光体でクリーニング方式がブレードクリーニングである複写機にセットし、画像評価実験を行なった。
その結果、画像のドット再現性は５段階評価でランク４であった。
【００７１】
実施例７
実施例６と同様の原材料、作製方法で粉体の作製、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
さらに、実施例６と同様に二成分現像剤を作製し、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク５であった。
【００７２】
実施例８
実施例６と同様の原材料、作製方法で粉体の作製、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
さらに、実施例６と同様に二成分現像剤を作製し、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク５であった。
【００７３】
比較例２
実施例６と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
さらに、実施例６と同様に二成分現像剤を作製し、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク３であった。
【００７４】
実施例９
樹脂：ポリエステル樹脂 １００部
顔料：カーボンブラック １０部
帯電制御剤：サルチル酸亜鉛塩 ２部
離型剤：ライスワックス ５部
添加剤：スチレンアクリル樹脂 ３部
上記原材料をミキサーで充分に混合した後、２軸押出し機によりバレル温度１００℃回転数１１０ｒｐｍで溶融混練した。混練物を圧延冷却後カッターミルで粗粉砕し、ジェット気流を用いた微粉砕機で粉砕後、旋回式風力分級装置を用いて、平均粒径が６μｍの粒度分布に分級した。さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
さらに、上記作製法で得られたトナーとキャリアをキャリア９７．５部に対し、２．５部の割合で混合し、二成分現像剤を作製した。
得られた現像剤を潜像担持体がＯＰＣドラム感光体でクリーニング方式がブレードクリーニングである複写機にセットし、画像評価実験を行なった。
その結果、画像のドット再現性は５段階評価でランク４であった。
【００７５】
実施例１０
実施例９と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
さらに、実施例９と同様に二成分現像剤を作製し、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク５であった。
【００７６】
実施例１１
実施例９と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
さらに、実施例９と同様に二成分現像剤を作製し、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク５であった。
【００７７】
比較例３
実施例９と同様の原材料、作製方法で混練、粉砕、分級を行ない、平均粒径が６．５μｍの粒度分布に分級した。
さらに、母体着色粒子１００部に対して、以下の混合条件にて添加剤を混合し、トナーを作製した。

トナーを作製した後、第一の評価装置により圧密前トナー高さを測定後、圧密し、圧密状態（空間率）および流動性を測定した結果、表１のようになった。
また、第二の評価装置によりトナーを圧密し、圧密状態（不具合点、空間率）および流動性を測定した結果、表２のようになった。
さらに、実施例９と同様に二成分現像剤を作製し、画像評価実験を行なった。その結果、画像のドット再現性は５段階評価でランク３であった。
【００７８】
【表１】

【００７９】
【表２】

【００８０】
表１および表２に示される結果から分かるように、トナー粉体相の本評価装置による流動性評価値とドット再現性との間には強い相関関係が存在し、本評価法によりドット再現性を評価できることが分かる。
また、図９のトルクとドット再現性との関係を表わすグラフ、および図１０の荷重とドット再現性との関係を表わすグラフから分かるように、ドット再現性の良い高画質を得るために必要な、流動性の良いトナーを得るためには、以下の条件を満足することが必要である。また、以下の条件のとき、表１から分かるように２万枚のランニングをしたとき、現像部でのブロッキング等のトナー搬送性の不具合点は生じなかった。
▲１▼円錐ロータ侵入時のトルクの値が０．１〜８．３ｍＮｍである。
▲２▼円錐ロータ侵入時の荷重の値が０．０１〜１．１４Ｎである。
円錐ロータ侵入時のトルク値が０．１ｍＮｍ未満では、トナーの流動性以外の帯電特性が悪くなり画質低下が生じ、８．３ｍＮｍより大きくなれば流動性が低下し、ドット再現性が悪くなる。円錐ロータ侵入時の荷重値が０．０１Ｎ未満では、トナーの帯電特性が悪くなり画質低下が生じ、１．１４Ｎより大きくなるとトナーの流動性が低下しドット再現性が悪くなる。
【００８１】
【発明の効果】
粉体の流動性を、本評価装置を用いて圧密前トナー高さを計測して最適な圧密条件で圧密し、圧密状態を評価した後、粉体相中に円錐ロータを回転させながら侵入させ、円錐ロータが粉体相中を移動するときに発生するトルクまたは荷重を測定することにより、粉体の流動性が精度良く、個人差の無い評価ができるようになり、高画質の得られるトナーの条件を精度良く規定し、高画質の得られるトナーを安定して生産できるようにした。
【図面の簡単な説明】
【図１】本発明の第一の粉体流動性評価装置の構成例の概念図である。
【図２】本発明の第一の粉体流動性評価装置における圧密前高さ計測部の構成例を示す図である。
【図３】円錐ロータの形の一例を示す図である。
【図４】他の円錐ロータの形の例（円錐ロータの断面形状の変化、円錐頂角の変化）を示す図である。
【図５】本発明の第二の粉体流動性評価装置の構成例の概念図である。。
【図６】本発明の第二の粉体流動性評価装置における圧密前高さ計測部の構成例を示す図である。
【図７】本評価装置を用いたトナー製造装置の例を示す概略図である。
【図８】本評価装置を用いて作製したトナーを使った現像装置の例を示す。
【図９】実施例１〜１１、比較例１〜３の円錐ロータ侵入時のトルクとドット再現性との関係を示す図である。
【図１０】実施例１〜１１、比較例１〜３の円錐ロータ侵入時の荷重とドット再現性との関係を示す図である。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an apparatus for evaluating the fluidity of a toner for electrostatic charge development used for one-component development or two-component development in electrophotography and the toner for electrostatic charge development.
[0002]
[Prior art]
The image quality of copiers, printers, and the like has been increasing, and recently, the reproducibility of fine dots has become very important. The dot reproducibility is greatly affected by the fluidity in addition to the charge amount of the toner and the developer, and it is necessary to stably supply a uniform toner layer or a developer layer to a fine latent image portion. Are coming.
Further, as the image quality is improved, the particle size and the function of the toner used for the toner are advanced. For this reason, the structure of the toner has become more complicated, and it is necessary to perform finer control at the time of production than before. In particular, since the fluidity of the toner affects various image qualities in addition to the dot reproducibility, a highly accurate evaluation method that does not differ between individuals in terms of evaluation is required.
Also, when the method of producing the toner changes from a pulverization method to another method such as a polymerization method, the change in the flow characteristics with respect to the production conditions is large, and compared with the case of the pulverization method, finer control during production and Evaluation is required.
[0003]
As a method of evaluating the fluidity of the electrostatic charge developing toner in electrophotography, a method of measuring a time required for the toner to fall through a narrow portion of a funnel to which a magnetic field is applied (for example, see Patent Document 1). ), A method in which toner is placed on a tiltable plate, the plate is gradually tilted, and angles at which the flow starts and ends are measured (for example, see Patent Document 2). The toner is put on the crab, and the horizontal and vertical vibrations are applied to the sieve portion, and the amount of toner remaining in each sieve portion after a certain time is multiplied by a preset coefficient to calculate the amount. (For example, see Patent Document 3).
However, these methods have a large variation in data, and there are differences among the measurers, and it was not possible to evaluate a fine difference in fluidity between toners.
Various studies have been made on such a technique academically (for example, see Non-Patent Documents 1 and 2).
[0004]
In order to solve such a problem, the present inventors have made the fluidity of the powder, particularly the toner, to enter the toner powder layer while rotating the conical rotor, and when the conical rotor moves in the toner powder layer. A new evaluation method capable of accurately evaluating the difference in fluidity between fine toners by evaluating the generated torque or load and measuring the generated torque or load has been previously proposed and filed (Japanese Patent Application No. 2002-346881, Application 2002-346831).
According to the new evaluation method, the toner layer can be quantitatively, accurately and accurately evaluated without any individual difference, and the toner layer can be measured as it is in a short time and can be introduced into a production line. And has the advantage of stably producing a toner that provides high image quality.
[0005]
[Patent Document 1]
Japanese Patent Application Laid-Open No. Hei 1-203941 [Patent Document 2]
Japanese Patent Application Laid-Open No. 4-116449 [Patent Document 3]
Japanese Patent Application Laid-Open No. 2000-292967 [Non-Patent Document 1]
Satoh M. : J. , Soc. Powder Technology. , Japan, 31, 783-788 (1994).
[Non-patent document 2]
Munetake Sato et al., "Chemical Engineering Transactions," Vol. 22, no. 6, pp. 1435-1441 (1996)
[0006]
[Problems to be solved by the invention]
An object of the present invention is to produce a toner capable of obtaining high image quality with good dot reproducibility by using an evaluation device having high fluidity accuracy and no individual difference, and to stably produce the toner. .
[0007]
[Means for Solving the Problems]
The present invention is to measure the torque or load generated when the conical rotor moves through the powder phase by rotating the conical rotor into the powder phase that has been compacted in advance, and then moving the conical rotor into the powder phase. TECHNICAL FIELD The present invention relates to an evaluation device for evaluation and a toner for electrostatic charge development capable of obtaining high quality images with good dot reproducibility evaluated using the evaluation device.
[0008]
The powder fluidity evaluation device of the present invention, after consolidating the powder phase in advance, while rotating the conical rotor into the condensed powder phase, intrude (down) or pull out (up), At that time, the torque and load applied to the container containing the conical rotor and the powder phase are measured, and the fluidity of the powder is evaluated based on the values of the torque and the load. The proposed content is improved to solve the above problem.
[0009]
A first invention, which is an improved technique, is a conical rotor that enters a toner layer while rotating, a torque meter that detects a torque applied to the rotating conical rotor, a load cell that detects a load applied to a container by rotation of the conical rotor, and a cone. An apparatus for evaluating the fluidity of a powder, which comprises at least a lift for moving a rotor or a container up and down, further comprising means for measuring the height of the powder phase before compaction, wherein the height of the powder phase before compaction is increased. After measuring the height and controlling the consolidation conditions based on the height information and consolidating the conical rotor, the conical rotor penetrates into the powder phase to measure the torque and load.
[0010]
A second invention, which is an improved technique, includes a conical rotor that rotates and enters a toner layer, a torque meter that detects a torque applied to the rotating conical rotor, a load cell that detects a load applied to a container by rotation of the conical rotor, and a cone. The powder fluidity evaluation device having at least a rotor or a lift for vertically moving the container is further provided with positioning means for preventing the container from moving at the time of compaction. After consolidating the phases and controlling the consolidation state to consolidate, the conical rotor is made to penetrate into the powder phase, and the torque and load are measured.
[0011]
The shape of the conical rotor in these first and second inventions is not particularly limited, but a conical rotor having an apex angle of 20 to 150 ° is suitable.
If the apex angle of the cone is less than 20 °, the resistance to the powder phase is small, so the torque and load are small, and a fine difference in fluidity cannot be evaluated. On the other hand, when the apex angle is larger than 150 °, the force in the direction of pressing the powder phase becomes large, and the powder particles are easily deformed, which is not suitable for evaluating the fluidity of the powder.
The length of the conical rotor must be long enough so that the conical rotor surface is continuously present in the powder phase.
Further, it is preferable that a groove is formed on the surface of the conical rotor. Rather than measuring the friction component between the material surface of the conical rotor and the powder particles, it is better to measure the friction component between the powder particles and the powder particles. For that purpose, when the conical rotor rotates and penetrates into the powder phase, the powder particles enter into the grooves cut on the surface of the conical rotor, and the entered powder particles and the surrounding It is more suitable to measure the state of friction with the powder particles.
Although the shape of the groove is not limited, it is necessary to devise such a way that the contact between the material surface of the conical rotor and the powder particles is reduced. An example is shown in FIG. In this method, a groove is cut straight from the vertex of the cone to the bottom side, and the cross section of the groove has a saw-tooth shape composed of triangular irregularities.
In this case, the contact between the material surface of the conical rotor and the powder particles is only at the tip of the peak of the triangular groove. Most of the contact is between the powder particles that have entered the groove and the powder particles in the vicinity thereof.
[0012]
Any material may be used for the conical rotor, but a material that is easy to process, has a hard surface, and does not deteriorate is preferable. In addition, a material that does not take chargeability is suitable. Examples of this include SUS, Al, Cu, Au, Ag, and brass.
[0013]
The torque and the load of the powder change depending on the rotation speed of the conical rotor and the penetration speed of the conical rotor. In this measurement, in order to improve the accuracy of the measurement, the rotation speed and the penetration speed of the conical rotor were reduced so that the fine contact state between the powder particles could be measured. Was confirmed to be preferable.
・ Number of rotations of conical rotor: 0.1 to 100 rpm
-Penetration speed of conical rotor: 0.5 to 150 mm / min
If the rotation speed of the conical rotor is smaller than 0.1 rpm, the powder phase is susceptible to the delicate state of the powder phase, which causes a problem of variation in torque measurement, which is not suitable for measurement. If it is more than 100 rpm, the powder may be scattered or the like, and the measurement cannot be performed stably.
On the other hand, when the penetration speed of the conical rotor is lower than 0.5 mm / min, it is apt to be affected by the delicate state of the powder phase, which causes a problem of measurement variation, and is not suitable for measurement. If the speed is higher than 150 mm / min, the powder phase is likely to be in a compacted state, and the influence of the deformation of the powder particles appears, so that it is not suitable for fluidity evaluation.
[0014]
As shown in FIG. 1, the apparatus of the first invention comprises a height measurement zone before consolidation, a consolidation zone, and a measurement zone.
The pre-consolidation height measurement zone includes a container for storing powder, an elevating stage for raising and lowering the container, a height measuring unit using a laser, a vibrator, and the like. Note that this configuration is an example and does not limit the present invention.
In this configuration, the sample container containing the powder is raised, the surface of the powder is irradiated with laser, and the amount of change from the reference height is measured based on the reflected light information. This height information is taken into a personal computer as shown in FIG. 2 and reflected in the consolidation conditions in the consolidation step in the next step to perform consolidation with high accuracy. The height of the powder phase before consolidation may be measured by using a vibrator provided at the lower part of the sample container to homogenize the powder phase before measuring the height of the powder phase before consolidation.
The consolidation zone includes a container for storing the powder, an elevating stage for raising and lowering the container, a piston for consolidation, a weight for applying a load to the piston, and the like. Note that this configuration is an example and does not limit the present invention. In this configuration, the sample container containing the powder is raised, brought into contact with the consolidation piston, and further raised so that the weight is floated from the support plate so that all the weight load is applied to the piston, Leave for a certain period of time.
Thereafter, the lifting stage on which the container containing the powder is placed is lowered, and the piston is separated from the powder surface. In order to mitigate the impact when the piston approaches the powder phase surface and makes contact with it, use the pre-consolidated powder phase height information before compaction to reduce the ascending speed of the container before making contact (powder powder To reduce the velocity of impact on the phase surface).
It is better to reduce the speed within a range of 1 to 10 mm before the piston contacts the powder phase surface. If the distance between the piston and the powder phase surface is less than 1 mm, powder leakage from the powder surface occurs, the dispersion of the compaction state increases, and if the distance between the piston and the powder phase surface exceeds 10 mm, the compaction time increases. Becomes longer and measurement in a short time cannot be performed.
[0015]
As shown in FIG. 1, the measurement zone includes a container for storing powder, an elevating stage for raising and lowering the container, a load cell for measuring a load, a torque meter for measuring torque of the powder, and the like. Note that this configuration is an example and does not limit the present invention.
The conical rotor is attached to the tip of the shaft, and the shaft itself is fixed (for vertical movement). The sample container stage containing the powder can be moved up and down by an elevator, and the container containing the powder is placed at the center of the stage. By raising the container, the conical rotor enters the center of the container while rotating. To make it come.
The torque applied to the conical rotor is detected by a torque meter provided above, and the load applied to the container containing the powder is detected by a load cell provided below the container. The amount of movement of the conical rotor is determined by a position detector. This configuration is an example, and other configurations such as raising and lowering the shaft itself by an elevator may be used.
[0016]
The shape of the conical rotor preferably has an apex angle of 20 to 150 ° as shown in FIG.
The length of the conical rotor needs to be long enough so that the conical rotor portion can enter the inside of the powder phase sufficiently. The shape of the groove may be any shape, but care must be taken so that torque and load values are not reproduced due to replacement of the conical rotor. For this purpose, as shown in FIG. 4, the groove shape of the conical rotor is simple, and it is better that the rotor having the same shape can be made many times.
The material of the container is not limited, but a conductive material is suitable so as not to be affected by charging with the powder.
In addition, since the measurement is performed while replacing the powder, it is preferable that the surface is close to a mirror surface to reduce dirt. The size of the container is important, and it is necessary to select a larger (diameter) size relative to the diameter of the conical rotor so that the walls of the container are not affected when the conical rotor enters while rotating.
[0017]
A high-sensitivity type torque meter is preferable, and a non-contact type torque meter is suitable. Load cells with a wide load range and high resolution are suitable. The position detector includes a linear scale, a displacement sensor using light, and the like, and a specification of 0.1 mm or less is suitable for accuracy. It is preferable that the elevator can be driven with high accuracy using a servomotor or a stepping motor.
[0018]
As the torque meter, a high-sensitivity type is preferable, and a non-contact type is suitable. Load cells with a wide load range and high resolution are suitable. The position detector includes a linear scale, a displacement sensor using light, and the like, and a specification of 0.1 mm or less is suitable for accuracy. It is preferable that the elevator can be driven with high accuracy using a servomotor or a stepping motor.
[0019]
In the measurement performed using the apparatus of the first invention, a certain amount of powder is charged into a container and set in the present apparatus.
Thereafter, the lifting stage is raised in the height measurement zone before consolidation, and the surface of the powder is irradiated with a laser to measure the height of the powder phase. There are various methods for measuring the height of the powder phase, and for example, there is a method using triangulation.
In this method, the powder surface is irradiated with a laser, and the position of the diffuse reflected light from the powder surface is detected to determine the amount of displacement.The position of the diffuse reflected light changes as the height position of the laser irradiation surface changes. The change is made using a CCD or the like which can detect a detailed position change in the light receiving unit. As the height detection accuracy, an accuracy of 0.1 mm or less is required.
Further, before measuring the height of the powder phase before consolidation, the height of the powder phase before consolidation may be measured by homogenizing the powder phase with a vibrator below the container. After measurement, lower the container and return to the original position. The powder phase height information before consolidation is taken into a personal computer and reflected in the consolidation conditions in the consolidation process in the next step.
Thereafter, a container containing the powder whose powder height has been measured before compaction is placed on the elevating stage in the compaction zone. In this operation, the elevation stage may be rotated to move from the pre-consolidation height measurement zone to the consolidation zone. Thereafter, the elevating stage is raised in the consolidation zone under the condition controlled by the powder height before consolidation, and the powder surface is pressed by a piston with a constant load to create a consolidated powder phase state.
After consolidating for a certain period of time, lower the container and return it to its original position. At this time, the compacted state is evaluated from the height of the compacted powder phase and the weight of the powder phase. Thereafter, the container containing the powder whose consolidation state has been measured is placed on the elevating stage in the measurement zone, and is made to penetrate into the powder phase in the sample container while rotating the conical rotor. When the torque or load measurement is started, the measurement is performed at the determined number of revolutions and penetration speed.
The direction of rotation of the conical rotor is arbitrary. When the penetration distance of the conical rotor is shallow, the values of torque and load are small, which causes a problem in data reproducibility and the like. Therefore, it is better to make the conical rotor penetrate deeply into a region where data can be reproduced. According to our experimental results, almost stable measurement was possible if the penetration was 5 mm or more.
[0020]
The measurement mode can be set under any conditions. For example, the following measurement modes are available.
(1) Fill the container with powder.
(2) Measure the height of the powder phase before compaction.
(3) Consolidation is performed, and the consolidation state is evaluated.
{Circle around (4)} The conical rotor is caused to enter while rotating, and the torque and load at that time are measured.
(5) When the conical rotor has penetrated from the toner surface layer to a predetermined depth, the penetrating operation is stopped.
(6) The operation of pulling out the conical rotor is started.
{Circle around (7)} When the tip of the conical rotor comes out of the powder phase surface and becomes completely free (the first home position), the drawing operation of the conical rotor is stopped, and the rotation is stopped.
By repeating the above operations (1) to (7), measurement is performed. It may be performed continuously.
[0021]
As another method, there is a method in which a conical rotor is caused to penetrate into a powder phase in which a compacted state is evaluated, and a depth until a predetermined torque value is obtained.
As a method of evaluating the consolidation state, there is a method of calculating a porosity. In this measurement method, the porosity of the powder phase becomes important, and our experiments showed that stable measurement was possible when the porosity was 0.4 or more. If it is less than 0.4, a delicate difference in the consolidation condition affects the torque and load, and stable measurement is difficult. The range of the porosity of the powder phase was 0.4 to 0.7 including various measurement methods. If it is larger than 0.7, the powder is scattered, which is not suitable for measurement.
However, the measurement system, measurement conditions, and the like are not limited to this.
[0022]
Next, the device of the second invention will be described.
As shown in FIG. 5, the device of the second invention comprises a consolidation zone and a measurement zone, but this configuration is an example and does not limit the present invention.
The consolidation zone includes a container for storing the powder, an elevating stage for raising and lowering the container, a piston for consolidation, a weight for applying a load to the piston, and the like. Note that this configuration is an example and does not limit the present invention.
In this configuration, the sample container containing the powder is raised, brought into contact with the consolidation piston, and further raised so that the weight is floated from the support plate so that all the weight load is applied to the piston, Leave for a certain period of time. Thereafter, the lifting stage on which the container containing the powder is placed is lowered, and the piston is separated from the powder surface. Means for positioning the container in advance so that the piston moves smoothly without contacting the side of the container when the piston enters the container, approaches the surface of the powder phase, and contacts and compacts the powder phase. Was provided.
FIG. 6 shows an example of this, in which a convex portion is provided on a part of the elevating stage, and a concave portion is provided on a bottom portion of the container corresponding to the convex portion. The concavo-convex portions may be reversed (the lifting stage is a concave portion, and the bottom portion of the container is a convex portion). Naturally, it is necessary to provide each concave and convex portion at a position where the container and the piston can move smoothly without colliding simply by aligning and fixing the concave portion of the container with the convex portion of the lifting stage.
In FIG. 6, a concave portion is provided at the center of the bottom of the container, and a convex portion is provided at a corresponding portion of the elevating stage. Further, in order to prevent powder leakage or the like at the time of compacting, when the compacting was performed using the present container positioning means, the distance between the piston to be compacted and the side of the vessel was set to be in the range of 1 to 1000 μm.
When the distance between the piston performing the consolidation and the side of the container is smaller than 1 μm, the friction component between the piston and the container increases, the consolidation is not performed smoothly, and the piston performs the consolidation during the consolidation and the side of the container. If the distance is larger than 1000 μm, powder leaks from between the piston and the container, and uniform consolidation cannot be performed.
[0023]
The measurement zone of the second invention shown in FIG. 5 is the same as that of the above-described first invention, and the description is omitted.
[0024]
The conditions of the conical rotor and the torque meter used in the second invention are the same as those used in the first invention.
Further, the container used in the second invention is slightly different from that used in the first invention, and the material is not limited, but a material that is easy to process is suitable.
The hardness of the container material is related to the friction with the piston, and it is preferable that the hardness of the container material be larger than the hardness of the piston material. This is to prevent scratches from being generated inside the container due to friction with the piston and the powder, so that stable consolidation cannot be performed. The container is preferably made of a light material so that the powder is put in the container and moved in the vertical direction or the like.
From these relations, it is suitable that Al is used as the material of the container and the surface of the container is subjected to alumite treatment. As the material of the piston, Al, Cu, brass or the like is suitable. In addition, since the measurement is performed while replacing the powder, it is preferable that the surface is close to a mirror surface to reduce dirt.
[0025]
Further, the amplitude of the surface roughness inside the container is preferably in the range of 0.01 to 100 μm from the viewpoint of the slidability with the piston during compaction. If the amplitude of the surface roughness inside the container is smaller than 0.01 μm, it tends to adhere to the piston and it takes time to consolidate. If the amplitude of the surface roughness inside the container is larger than 100 μm, Leakage of the body is likely to occur, which is a problem. The size of the container is important, and it is necessary to select a larger (diameter) size relative to the diameter of the conical rotor so that the walls of the container are not affected when the conical rotor enters while rotating.
[0026]
The measurement performed using the apparatus of the second invention is performed by charging a certain amount of powder into the container and setting the container in the present apparatus using the positioning means of the elevating stage in the consolidation zone.
Thereafter, the elevating stage is raised under controlled conditions in the consolidation zone, and the surface of the powder is pressed with a piston under a constant load to create a compacted powder phase state. After consolidating for a certain period of time, lower the container and return it to its original position. At this time, the compacted state is evaluated from the height of the compacted powder phase and the weight of the powder phase. Thereafter, the container containing the powder whose consolidation state has been measured is placed on the elevating stage in the measurement zone.
This operation may be moved from the consolidation zone to the measurement zone by rotating the lifting stage. Thereafter, the conical rotor is caused to penetrate into the powder phase in the compacted sample container while rotating. When the torque or load measurement is started, the measurement is performed at the determined number of revolutions and penetration speed.
The direction of rotation of the conical rotor is arbitrary. When the penetration distance of the conical rotor is shallow, the values of torque and load are small, which causes a problem in data reproducibility and the like. Therefore, it is better to make the conical rotor penetrate deeply into a region where data can be reproduced. According to our experimental results, almost stable measurement was possible if the penetration was 5 mm or more.
[0027]
The measurement mode can be set under any conditions. For example, the following measurement modes are available.
(1) Fill the container with powder.
{Circle around (2)} The container containing the powder is set in the apparatus using the positioning means.
(3) Consolidation is performed, and the consolidation state is evaluated.
{Circle around (4)} The conical rotor is caused to enter while rotating, and the torque and load at that time are measured.
(5) When the conical rotor has penetrated from the toner surface layer to a predetermined depth, the penetrating operation is stopped.
(6) The operation of pulling out the conical rotor is started.
{Circle around (7)} When the tip of the conical rotor comes out of the powder phase surface and becomes completely free (the first home position), the drawing operation of the conical rotor is stopped, and the rotation is stopped.
By repeating the above operations (1) to (7), measurement is performed. It may be performed continuously.
[0028]
As another measurement method, as shown in FIG. 5, the powder phase is stabilized by applying a vibration with a vibrator before consolidation, and a piston is pressed against the stabilized powder phase to consolidate. Create a state.
Rotate the conical rotor into the condensed powder phase while rotating, measure the torque or load generated when the conical rotor moves through the powder phase, and stop the intrusion operation when it reaches the preset depth. Then, the conical rotor is raised to the initial position (home position). This measurement may be performed once, but it is also effective to repeat this operation to obtain an average torque and load. As another method, there is a method in which a conical rotor is caused to penetrate into a powder phase in which a compacted state is evaluated, and a depth until a predetermined torque value is obtained.
[0029]
As a method of evaluating the consolidation state, there is a method of calculating a porosity. In this measurement method, the porosity of the powder phase becomes important, and our experiments showed that stable measurement was possible when the porosity was 0.4 or more. If it is less than 0.4, a delicate difference in the consolidation condition affects the torque and load, and stable measurement is difficult. The range of the porosity of the powder phase was 0.4 to 0.7 including various measurement methods. If it is larger than 0.7, the powder is scattered, which is not suitable for measurement.
However, the measurement system, measurement conditions, and the like are not limited to this.
[0030]
The toner used in each of the evaluation devices of the first and second inventions preferably has a weight average particle diameter of 4 to 10 μm, more preferably 5 to 7 μm, in order to realize a high quality image. It is.
If the weight average particle diameter is less than 4 μm, problems such as contamination in the apparatus due to toner scattering during long-term use, a decrease in image density in a low humidity environment, poor photoconductor cleaning, and the like are likely to occur, and there is a concern about the effect on the human body. When the weight average particle diameter exceeds 10 μm, the resolution of the fine spots of 100 μm or less is not sufficient, and the fine spots tend to scatter to non-image areas, resulting in poor image quality.
[0031]
When the toner of the present invention is used as a developer in combination with a carrier, the carrier needs to have an average particle diameter of 20 to 100 μm in order to realize a high quality image. When the average particle size of the carrier is in the range of 20 to 100 μm, the charge amount of the toner can be made more uniform when the toner concentration in the developing device is in the range of 2 to 10% by weight.
If it is less than 20 μm, the carrier particles are likely to adhere to the photoreceptor, and the stirring efficiency with the toner is deteriorated, so that it is difficult to obtain a uniform charge amount of the toner. Conversely, when the average particle size of the carrier exceeds 100 μm, fine image reproducibility deteriorates, and high image quality cannot be obtained.
[0032]
Details of the toner and the developer are shown below.
Examples of the resin include polystyrene resin, epoxy resin, polyester resin, polyamide resin, styrene acrylic resin, styrene methacrylate resin, polyurethane resin, vinyl resin, polyolefin resin, styrene butadiene resin, phenol resin, polyethylene resin, silicone resin, butyral resin, and terpene. Resins and polyol resins.
[0033]
As the vinyl resin, homopolymers of styrene such as polystyrene, poly-p-chlorostyrene and polyvinyltoluene and their substituted products: styrene-p-chlorostyrene copolymer, styrene-propylene copolymer, styrene-vinyltoluene copolymer Polymer, styrene-vinylnaphthalene copolymer, styrene-methyl acrylate copolymer, styrene-ethyl acrylate copolymer, styrene-butyl acrylate copolymer, styrene-octyl acrylate copolymer, styrene-methacryl Methyl acrylate copolymer, styrene-ethyl methacrylate copolymer, styrene-butyl methacrylate copolymer, styrene-α-chloromethyl methacrylate copolymer, styrene-acrylonitrile copolymer, styrene-vinyl methyl ether copolymer Coalescence, styrene-vinyl ethyl acetate Copolymer, styrene-vinyl methyl ketone copolymer, styrene-butadiene copolymer, styrene-isoprene copolymer, styrene-acrylonitrile-indene copolymer, styrene-maleic acid copolymer, styrene-maleic acid ester Styrene-based copolymers such as copolymers: polymethyl methacrylate, polybutyl methacrylate, polyvinyl chloride, polyvinyl acetate and the like.
[0034]
The polyester resin is composed of a dihydric alcohol as shown in Group A below and a dibasic acid salt as shown in Group B, and a trivalent or higher alcohol as shown in Group C or A carboxylic acid may be added as a third component.
Group A: ethylene glycol, triethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,4 butanediol, neopentyl glycol, 1,4 butenediol, 1,4-bis (hydroxymethyl) cyclohexane , Bisphenol A, hydrogenated bisphenol A, polyoxyethylenated bisphenol A, polyoxypropylene (2,2) -2,2'-bis (4-hydroxyphenyl) propane, polyoxypropylene (3,3) -2, 2-bis (4-hydroxyphenyl) propane, polyoxyethylene (2,0) -2,2-bis (4-hydroxyphenyl) propane, polyoxypropylene (2,0) -2,2′-bis (4 -Hydroxyphenyl) propane and the like.
Group B: maleic acid, fumaric acid, mesaconic acid, citraconic acid, itaconic acid, glutaconic acid, phthalic acid, isophthalic acid, terephthalic acid, cyclohexanedicarboxylic acid, succinic acid, adipic acid, sebacic acid, malonic acid, linoleic acid, or Esters of these acid anhydrides or lower alcohols.
Group C: trihydric or higher alcohol such as glycerin, trimethylolpropane, pentaerythritol and the like, and trivalent or higher carboxylic acid such as trimellitic acid and pyromellitic acid.
[0035]
As the polyol resin, an epoxy resin and an alkylene oxide adduct of a dihydric phenol, or a compound having one active hydrogen in the molecule that reacts with the glycidyl ether and the epoxy group, and an active hydrogen that reacts with the epoxy resin in the molecule. There are compounds obtained by reacting two or more compounds.
[0036]
The following are used as the pigment used in the present invention.
Examples of black pigments include azine dyes such as carbon black, oil furnace black, channel black, lamp black, acetylene black, and aniline black, metal salt azo dyes, metal oxides, and composite metal oxides.
Examples of the yellow pigment include cadmium yellow, mineral fast yellow, nickel titanium yellow, navels yellow, naphthol yellow S, Hanza yellow G, Hanza yellow 10G, benzidine yellow GR, quinoline yellow lake, permanent yellow NCG, and tartrazine lake. .
Examples of orange pigments include molybdenum orange, permanent orange GTR, pyrazolone orange, vulcan orange, indanthrene brilliant orange RK, benzidine orange G, and indanthrene brilliant orange GK.
Examples of the red pigment include bengara, cadmium red, permanent red 4R, lithol red, pyrazolone red, watching red calcium salt, lake red D, brilliant carmine 6B, eosin lake, rhodamine lake B, alizarin lake, and brilliant carmine 3B.
Examples of purple pigments include Fast Violet B and Methyl Violet Lake.
Examples of the blue pigment include cobalt blue, alkali blue, Victoria Blue Lake, phthalocyanine blue, metal-free phthalocyanine blue, partially chlorinated phthalocyanine blue, fast sky blue, and indanthrene blue BC.
Green pigments include chrome green, chromium oxide, pigment green B, malachite green lake, and the like.
One or more of these can be used.
[0037]
Particularly in the case of color toners, it is essential to disperse good pigments uniformly.Instead of directly charging pigments into a large amount of resin, a masterbatch in which pigments are once dispersed at a high concentration is prepared and diluted. Is used. In this case, a solvent is generally used to help dispersibility, but there are environmental problems and the like, and in the present invention, water is used to disperse. When water is used, temperature control is important so that residual moisture in the masterbatch does not matter.
[0038]
In the toner of the present invention, a charge control agent is blended (internally added) inside the toner particles. However, they may be mixed (externally added) with the toner particles. The charge control agent makes it possible to control the charge amount optimally according to the development system. In particular, in the present invention, the balance between the particle size distribution and the charge amount can be further stabilized.
Nigrosine and quaternary ammonium salts, triphenylmethane dyes, imidazole metal complexes and salts can be used alone or in combination of two or more to control the toner to have a positive charge. Further, a metal salicylate complex, salts, organic boron salts, calixarene-based compounds, and the like are used to control the toner to have a negative charge.
[0039]
Further, a release agent can be internally added to the toner of the present invention in order to prevent offset during fixing.
Release agents include natural waxes such as candelilla wax, carnauba wax, and rice wax, montan wax and its derivatives, paraffin wax and its derivatives, polyolefin wax and its derivatives, sasol wax, low molecular weight polyethylene, and low molecular weight polypropylene. And alkyl phosphate esters. The melting point of these release agents is preferably from 65 to 90 ° C. If the temperature is lower than this range, blocking during storage of the toner tends to occur. If the temperature is higher than this range, offset may easily occur in a region where the temperature of the fixing roller is low.
[0040]
An additive may be added for the purpose of improving the dispersibility of the release agent and the like. As additives, styrene acrylic resin, polyethylene resin, polystyrene resin, epoxy resin, polyester resin, polyamide resin, styrene methacrylate resin, polyurethane resin, vinyl resin, polyolefin resin, styrene butadiene resin, phenol resin, butyral resin, terpene resin, There are polyol resins and the like, and a mixture of two or more of each resin may be used.
[0041]
As the resin, a crystalline polyester may be used. It is an aliphatic polyester having crystallinity, a sharp molecular weight distribution, and an absolute amount of the low molecular weight as much as possible. This resin undergoes crystal transition at the glass transition temperature (Tg), and at the same time, its melt viscosity sharply drops from the solid state, and exhibits a fixing function to paper.
By using the crystalline polyester resin, low-temperature fixing can be achieved without excessively lowering the Tg or molecular weight of the resin. Therefore, there is no decrease in preservability due to a decrease in Tg. Also, there is no deterioration in gloss and offset resistance that are too high due to the reduction in molecular weight. Therefore, the introduction of the crystalline polyester resin is very effective in improving the low-temperature fixability of the toner.
[0042]
In the toner of the present invention, in order to exhibit low-temperature fixability and ensure hot offset resistance, the content of the crystalline polyester is 1 to 50 with respect to the total amount of the resin and the release agent in the toner. % By weight, and the content of the release agent is preferably 2 to 15% by weight. When the content of the crystalline polyester is less than 1% by weight, there is no effect on the low-temperature fixability, and when it exceeds 50% by weight, the hot offset property deteriorates. When the content of the release agent is less than 2% by weight, there may be no effect on the anti-offset property, and when it exceeds 15% by weight, the fluidity of the toner decreases.
[0043]
Examples of a method for producing the toner according to the present invention include a pulverization method and a polymerization method (suspension polymerization, emulsion polymerization / dispersion polymerization, emulsion aggregation, emulsion association, and the like), but are not limited thereto.
[0044]
As an example of the pulverization method, first, the above-described resin, a pigment or dye as a colorant, a charge control agent, a release agent, other additives, and the like are sufficiently mixed by a mixer such as a Henschel mixer, and then a batch method is performed. The components are kneaded well using a hot roll kneader such as a two-roll mill, a Banbury mixer, a continuous twin screw extruder, or a continuous single screw kneader, followed by rolling, cooling and cutting.
After cutting, the kneaded toner is crushed, coarsely crushed using a hammer mill or the like, further crushed finely using a fine crusher using a jet stream or a mechanical crusher, and a classifier using a swirling stream and a Coanda effect. Is classified to a predetermined particle size by a classifier using Thereafter, an additive composed of inorganic particles or the like is attached or fixed to the particle surface by a mixer. The fluidity of the toner particles after the mixing step is evaluated using the present evaluation device.
In this case, in the sampling inspection, the sample is placed in a sample container, the sample container is directly placed on the sample stage of the evaluation device shown in FIG. 1, and the height of the toner powder phase before compaction is measured. And then measure torque and load. The rotation speed of the conical rotor was 0.1 to 100 rpm, and the penetration speed of the conical rotor was 0.5 to 100 mm / min. The measurement is performed by rotating the conical rotor, and then stopping the penetration after a predetermined penetration distance of 5 mm or more. After that, the conical rotor is pulled out and returned to the original initial position. The torque and the load when the conical rotor enters the toner powder phase are measured to evaluate the fluidity of the toner.
[0045]
When the toner fluidity is evaluated by the present evaluation device, the measured value (torque, load) and the toner fluidity have the following relationship.
When the torque is small, the fluidity is good.
If the torque is large, the fluidity is poor.
When the load is small, the fluidity is good.
When the load is large, the fluidity is poor.
[0046]
The characteristics of the present evaluation device using a conical rotor are as follows, and a sample can be measured quickly and easily as it is, so that highly accurate measurement without individual differences can be performed.
(1) Non-destructive inspection.
(2) The sample can be measured as it is.
(3) Measurement can be performed in a short time.
(4) Anyone can easily measure.
Therefore, measurement on a production line is also possible, and it can be installed between each process in a production process, and quality evaluation can be performed in the middle of the process. For example, after the mixing step, a sample extraction / measurement zone is provided in the course of transporting the powder sample to the next step, and a shutter is opened and closed at a certain timing to transport a fixed amount of the sample to the measurement unit. The tip of the measuring unit is a container made of SUS or the like, and the measurement is directly performed by the present evaluation device. Alternatively, the container is brought to the present evaluation device in another nearby place, and is placed on a sample stage and measured by the present evaluation device. The measured toner is returned to the original sample. As a result of the evaluation, if the numerical value is out of the predetermined setting range, the sample is not sent to the filling process but is sent to the toner reprocessing process. These mechanisms can be applied to inspection after the pulverizing / classifying step, which is a step before the mixing step, inspection after the air sieving step after the mixing step, inspection before filling, and the like. (See FIG. 7)
Further, the toner evaluation device having these functions can be used alone as an evaluation device in the development stage.
[0047]
In the case of toner, as described above, the measured values of the torque and load in this evaluation device indicate fluidity, and quantitative evaluation is possible. In the conventional evaluation method up to now, the difference between toners can be evaluated, but there is a problem that if the type of toner is different, it cannot be evaluated in the same playing field. However, the values measured by this evaluation device are torque values and load values as powder characteristics, and can be evaluated on the same ring even if the type of toner changes or the particle size changes. Evaluation value. In addition, since the difference in fluidity after evaluating the consolidation state can be evaluated, multifaceted evaluation is possible.
[0048]
The torque and load characteristics during the movement of the conical rotor in the toner powder phase are closely related to the fluidity of the powder. It is easy to move because of its small adhesive force, and even if the conical rotor is moved in the powder phase, the torque is small and the load change is small. On the contrary, when the fluidity of the powder is poor, it is difficult to move due to the large adhesive force between the individual powder particles, and when the conical rotor is moved within the powder phase, the conical rotor is moved. And the force (load) acting in the downward direction also increases.
Therefore, according to the evaluation method of the present invention, the fluidity can be evaluated based on the following relationship.
When fluidity is good → The torque and load when moving in the powder phase are small.
When the fluidity is poor → The torque and load when moving in the powder phase are large.
The fluidity of the toner is largely determined by the mixing step in the toner production step. That is, the fluidity of the toner particles greatly changes depending on the state in which the additive composed of the inorganic particles or the like is attached or fixed to the surface of the toner particles.
The mixing state of the toner varies depending on the mixing conditions (feed amount, rotation speed, mixing time, etc.) in the mixing step. Therefore, the mixing conditions play an important role in the fluidity, and the evaluation of the fluidity after the mixing step is important.
[0049]
In a printer or a copying machine, in order to realize high image quality, it is necessary to enhance the reproducibility of very minute dots. To achieve this, toner development that is faithful to very small latent images is required. To enable this faithful development, it is necessary to supply a uniform toner brush to the development area. For this purpose, it is necessary that the toner charge amount is in an appropriate condition, but the ease of movement of the toner and the ease of transport so that a stable and uniform toner brush can be supplied to the development area are extremely high. It becomes important. That is, in order to increase the reproducibility of minute dots, it is necessary to increase the fluidity of the toner.
Therefore, the fluidity of the toner was evaluated with this device using a conical rotor, and the relationship with the dot reproducibility was examined.As a result, there was a very strong correlation, and the dot reproducibility improved when the torque and load were small. Was.
[0050]
From the results, it was found that the toner having good dot reproducibility exhibited the following torque and load characteristics.
{Circle around (1)} The value of the torque when the conical rotor enters (at the time of entry of 20 mm) is 0.1 to 8.3 mNm.
{Circle around (2)} The value of the load when the conical rotor enters (at the time of entry of 20 mm) is 0.01 to 1.14 N.
[0051]
Note that other methods can be used for the evaluation mode without any problem. The evaluation item may be an intrusion distance to a certain load, an intrusion distance to a certain torque, or the like other than the torque and the load, or an integrated value of the torque and the load. Further, other evaluation items may be used.
After the mixing step, the mixture is passed through a sieve of 250 mesh or more to remove coarse particles and aggregated particles to obtain the toner of the present invention.
[0052]
A method other than the pulverization method is considered as a method for producing the toner according to the present invention. As an example of the polymerization method, a monomer composition obtained by adding a colorant and a charge control agent to a monomer is suspended in an aqueous medium. The toner particles are obtained by turbidity and polymerization. The granulation method is not particularly limited.
For example, the toner of the present invention is obtained by dissolving at least an isocyanate group-containing polyester prepolymer in an organic solvent, dispersing a pigment colorant, and dissolving or dispersing a release agent in an aqueous medium. Urea-modified polyester resin having a urea group by dispersing the prepolymer in the dispersion in the presence of inorganic fine particles and / or polymer fine particles and reacting the prepolymer with a polyamine and / or a monoamine having an active hydrogen-containing group in the dispersion. Is formed, and the liquid medium contained therein is removed from the dispersion containing the urea-modified polyester resin.
The urea-modified polyester resin has a Tg of 40 to 65 ° C, preferably 45 to 60 ° C. Its number average molecular weight Mn is 2,500 to 50,000, preferably 2,500 to 30,000. Its weight average molecular weight Mw is 10,000 to 500,000, preferably 30,000 to 100,000.
[0053]
This toner contains, as a binder resin, a urea-modified polyester-based resin having a urea bond and having a high molecular weight by a reaction between the prepolymer and the amine. The coloring agent is highly dispersed in the binder resin.
The obtained dried toner powder is subjected to air classification, and an additive composed of inorganic fine particles or the like is attached or fixed to the particle surface by a mixer under the above-described optimum mixing conditions. Alternatively, the charge control agent may be injected into the surface of the dried toner powder and fixedly injected. After that, an additive such as inorganic fine particles may be attached or fixed to the particle surface. By driving the charge control agent onto the surface, the charge amount of the toner can be easily controlled.
[0054]
Specific means for mixing and sticking and pouring are methods of applying impact force to the powder mixture by high-speed rotating blades, throwing the powder mixture into a high-speed air stream, accelerating it, and combining particles or There is a method in which the particles are made to collide with an appropriate collision plate. As the equipment, Angular mill (manufactured by Hosokawa Micron), I-type mill (manufactured by Nippon Pneumatic) was modified to reduce the pulverized air pressure, hybridization system (manufactured by Nara Machinery Co., Ltd.), Kryptron System (manufactured by Kawasaki Heavy Industries, Ltd.), automatic mortar and the like.
[0055]
After this mixing step, evaluation is performed using the present evaluation apparatus to evaluate whether or not a predetermined fluidity is obtained.
In the case of these methods also, inspection after granulation, inspection after treatment of charge control agent, inspection after mixing process of additives, inspection after air sieving process after mixing process, inspection before filling etc. Applicable.
Although the fluidity is affected by the shape of the toner, a very spherical toner having an average circularity of 0.9 to 0.99 has excellent fluidity and high dot reproducibility. Image quality can be improved.
Further, when used as a two-component developer, a two-component developer is obtained by mixing with a magnetic carrier described later at a predetermined mixing ratio.
[0056]
The present toner is used as a one-component developer used in a contact or non-contact developing system. Various known contact or non-contact development systems are used. For example, there are a contact developing method using an aluminum sleeve, a contact developing method using a conductive rubber belt, and a non-contact developing method using a developing sleeve in which a conductive resin layer containing carbon black or the like is formed on the surface of an aluminum tube. .
In addition, when the toner is developed using an AC bias voltage component during development, the toner has excellent fluidity, so that the toner vibrates faithfully in accordance with an electric field, and can faithfully develop a fine latent image. Good development becomes possible.
[0057]
Further, in the one-component developing method, the present toner is used in a developing method in which a roller-shaped blade for uniforming a toner layer is provided at an outlet of a toner supply unit. Further, a developing method using a supply roller as shown in FIG. 8 may be employed. In the case of such a method, not only filming on the photosensitive member but also filming on the doctor roller and the supply roller occurs. For this reason, not only can the toner layer not be formed uniformly, but also the toner charging becomes non-uniform, and the toner charge becomes small. For this reason, defective development occurs. However, when the toner of the present invention is used, filming does not occur on the doctor roller and the supply roller, stable development is performed, and a system having excellent durability characteristics is obtained.
Since the present toner has excellent fluidity, it can be sufficiently stored in a cartridge container, and is also suitable for an apparatus configured to transport toner from the cartridge container to the developing unit.
[0058]
When a magnetic toner is used, fine particles of a magnetic substance may be internally added to the toner particles. As the magnetic material, a ferromagnetic material such as ferrite, magnetite, iron, nickel, cobalt, or an alloy thereof can be considered. The average particle size of the magnetic material is preferably 0.1 to 1 μm. The content of the magnetic substance is preferably from 10 to 70 parts by weight based on 100 parts by weight of the toner.
[0059]
As the carrier used for the two-component developer, known carriers can be used. For example, magnetic particles such as iron powder, ferrite powder, nickel powder, and magnetite powder, or the surface of these magnetic particles is coated with a fluororesin or vinyl resin. And those treated with a silicone resin or the like, or magnetic particle-dispersed resin particles in which magnetic particles are dispersed in a resin. The average particle size of these magnetic carriers is preferably 20 to 100 μm. Preferably, it is 20 to 70 μm.
[0060]
As described above, the two-component developer of the present invention can be used by adding an inorganic fine powder to a toner as a fluidity improver.
Examples of the inorganic fine powder of the present invention include Si, Ti, Al, Mg, Ca, Sr, Ba, In, Ga, Ni, Mn, W, Fe, Co, Zn, Cr, Mo, Cu, Ag, V, and Zr. Oxides and composite oxides. Among them, fine particles of silicon dioxide (silica), titanium dioxide (titania), and alumina are preferably used. Further, it is effective to perform a surface modification treatment with a hydrophobizing agent or the like. The following are typical examples of the hydrophobizing agent.
Dimethyldichlorosilane, trimethylchlorosilane, methyltrichlorosilane, allyldimethyldichlorosilane, allylphenyldichlorosilane, benzyldimethylchlorosilane, bromomethyldimethylchlorosilane, α-chloroethyltrichlorosilane, p-chloroethyltrichlorosilane, Chloromethyldimethylchlorosilane, chloromethyltrichlorosilane, hexaphenyldisilazane, hexatolyldisilazane and the like.
The inorganic fine powder is preferably used in an amount of 0.1 to 2% by weight based on the toner. If it is less than 0.1% by weight, the effect of improving toner aggregation is poor. If it exceeds 2% by weight, problems such as scattering of toner between fine lines, contamination inside the machine, scratches and abrasion of the photoreceptor tend to occur. is there.
[0061]
The developer of the present invention may further contain other additives within a range that does not substantially adversely affect the lubricant, for example, lubricant powders such as polytetrafluoroethylene-based fluororesin powder, zinc stearate powder, and polyvinylidene fluoride powder; Alternatively, an abrasive such as cerium oxide powder, silicon carbide powder, or strontium titanate powder; or a small amount of a conductivity-imparting agent such as carbon black powder, zinc oxide powder, or tin oxide powder can be used as a developing property improver.
In addition, this evaluation method can be used for toners and capsule toners produced by a polymerization method or a spray drying method produced without using a kneading step or a pulverizing step.
[0062]
【Example】
Hereinafter, Examples will be described, but they do not limit the present invention in any way. All parts in the following formulations are parts by weight.
In this case, a toner was prepared in which the toner composition, the toner preparation method, and the mixing conditions were changed, the toner fluidity was evaluated using the present evaluation method, and the dot reproducibility was evaluated in five steps as a rough feeling of the image (rank 1). : Bad → rank 5: good).
In addition, a running durability test of 20,000 sheets was performed using a copying machine using OPC, and defects in toner transportability such as blocking in a developing section were evaluated. The case where there was no defect was evaluated as ○, and the case where there was a defect was evaluated as x.
The fluidity of the toner was evaluated using this evaluation device, and the torque and load values when the conical rotor penetrated 20 mm from the surface of the toner powder phase were measured.
In the case of using the first apparatus, the height of the toner phase before consolidation of the toner is measured in advance, and the data is obtained below (the distance between the piston and the height of the toner phase before consolidation is 5 mm; After the porosity was measured and the porosity was measured, the torque and the load were evaluated. In the case where the second device was used, the toner was preliminarily confined in the consolidation zone using the container positioning means. After measuring the porosity, the torque and load were evaluated.
The evaluation conditions for the conical rotor were as follows. In addition, the torque and load when the space ratio was 0.53 were adopted for the evaluation.
・ Vertical angle of conical rotor: 50 °
・ Number of rotations of the conical rotor: 2 rpm
-Penetration speed of conical rotor: 5 mm / min
[0063]
Example 1
Resin: polyester resin 100 parts Pigment: magenta pigment (CI Pigment Red 57) 4 parts Charge control agent: zinc salicylate 5 parts After sufficiently mixing the above raw materials with a mixer, a barrel temperature of 100 was obtained by a twin screw extruder. The mixture was melt-kneaded at 110 ° C. kneader rotation speed of 110 rpm. The kneaded product was rolled and cooled, coarsely pulverized by a cutter mill, pulverized by a fine pulverizer using a jet stream, and then classified into a particle size distribution having an average particle size of 6.5 μm by using a revolving air classifier. Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
The obtained toner was set in a copying machine in which the latent image carrier was an OPC drum photosensitive member and the cleaning method was blade cleaning, and an image evaluation experiment was performed.
As a result, the dot reproducibility of the image was ranked 4 on a 5-point scale.
[0064]
Example 2
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 1, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
An image evaluation experiment was performed in the same manner as in Example 1. As a result, the dot reproducibility of the image was ranked 4 on a 5-point scale.
[0065]
Example 3
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 1, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
An image evaluation experiment was performed in the same manner as in Example 1. As a result, the dot reproducibility of the image was ranked 5 on a five-point scale.
[0066]
Example 4
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 1, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
An image evaluation experiment was performed in the same manner as in Example 1. As a result, the dot reproducibility of the image was ranked 5 on a five-point scale.
[0067]
Example 5
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 1, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
An image evaluation experiment was performed in the same manner as in Example 1. As a result, the dot reproducibility of the image was ranked 5 on a five-point scale.
[0068]
Comparative Example 1
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 1, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
Further, an image evaluation experiment was performed in the same manner as in Example 1. As a result, the dot reproducibility of the image was ranked 3 on a five-point scale.
[0069]
Example 6
<Synthesis of toner binder>
724 parts of bisphenol A ethylene oxide 2 mol adduct, 276 parts of isophthalic acid and 2 parts of dibutyltin oxide were placed in a reaction vessel equipped with a cooling pipe, a stirrer and a nitrogen introduction pipe, and reacted at 230 ° C. for 8 hours under normal pressure. After further reacting at a reduced pressure of 10 to 15 mmHg for 5 hours, the mixture was cooled to 160 ° C., and 32 parts of phthalic anhydride was added thereto and reacted for 2 hours.
Next, the mixture was cooled to 80 ° C. and reacted with 188 parts of isophorone diisocyanate in ethyl acetate for 2 hours to obtain an isocyanate-containing prepolymer I. Next, 267 parts of Prepolymer I and 14 parts of isophoronediamine were reacted at 50 ° C. for 2 hours to obtain a urea-modified polyester I having a weight average molecular weight of 64000.
In the same manner as described above, 724 parts of bisphenol A ethylene oxide 2 mol adduct and 276 parts of terephthalic acid are polycondensed at 230 ° C. for 8 hours under normal pressure, and then reacted at a reduced pressure of 10 to 15 mmHg for 5 hours to modify the peak molecular weight to 5,000. Untreated polyester A was obtained.
200 parts of urea-modified polyester I and 800 parts of unmodified polyester A were dissolved and mixed in 2000 parts of a mixed solvent of ethyl acetate / MEK (1/1) to obtain a solution of toner binder I in ethyl acetate / MEK. A part of the mixture was dried under reduced pressure to isolate the toner binder I. As a result of analysis, Tg was 62 ° C.
[0070]
<Preparation of toner>
Ethyl acetate / MEK solution of toner binder I 240 parts Pentaerythritol tetrabehenate (melt viscosity 25 cps) 20 parts Copper phthalocyanine blue pigment (CI pigment blue 15: 3) 4 parts The above raw materials are placed in a beaker at 60 ° C. The mixture was stirred at 12,000 rpm with a TK homomixer to uniformly dissolve and disperse to prepare a toner material solution.
Ion-exchanged water 706 parts Hydroxyapatite 10% suspension (Supatite 10 manufactured by Nippon Chemical Industry Co., Ltd.) 294 parts Sodium dodecylbenzenesulfonate 0.2 part The above-mentioned raw materials were put in a beaker and uniformly dissolved. Thereafter, the temperature was raised to 60 ° C., and the above-mentioned toner material solution was charged and stirred for 10 minutes while stirring at 12,000 rpm with a TK homomixer. Then, the mixture was transferred to a flask equipped with a stir bar and a thermometer, heated to 30 ° C. to remove the solvent under reduced pressure, separated by filtration, washed and dried, and then subjected to air classification to obtain toner particles. The volume average particle size was 6.5 μm. An additive was mixed with 100 parts of the toner particles under the following mixing conditions to obtain a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
The toner and carrier obtained by the above method were mixed in a ratio of 2.5 parts to 97.5 parts of the carrier to prepare a two-component developer.
The obtained developer was set in a copying machine in which the latent image carrier was an OPC drum photosensitive member and the cleaning method was blade cleaning, and an image evaluation experiment was performed.
As a result, the dot reproducibility of the image was ranked 4 on a 5-point scale.
[0071]
Example 7
Powder was prepared and classified using the same raw materials and preparation method as in Example 6, and classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
Further, a two-component developer was prepared in the same manner as in Example 6, and an image evaluation experiment was performed. As a result, the dot reproducibility of the image was ranked 5 on a five-point scale.
[0072]
Example 8
Powder was prepared and classified using the same raw materials and preparation method as in Example 6, and classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
Further, a two-component developer was prepared in the same manner as in Example 6, and an image evaluation experiment was performed. As a result, the dot reproducibility of the image was ranked 5 on a five-point scale.
[0073]
Comparative Example 2
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 6, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
Further, a two-component developer was prepared in the same manner as in Example 6, and an image evaluation experiment was performed. As a result, the dot reproducibility of the image was ranked 3 on a five-point scale.
[0074]
Example 9
Resin: 100 parts of polyester resin Pigment: 10 parts of carbon black Charge control agent: 2 parts of zinc salicylate Release agent: 5 parts of rice wax Additive: 3 parts of styrene acrylic resin After thoroughly mixing the above raw materials with a mixer, 2 parts Melt kneading was performed at a barrel temperature of 100 ° C. and a rotation speed of 110 rpm by a shaft extruder. The kneaded product was rolled and cooled, coarsely pulverized by a cutter mill, pulverized by a fine pulverizer using a jet stream, and then classified into a particle size distribution having an average particle size of 6 μm using a revolving air classifier. Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
Further, the toner and the carrier obtained by the above-mentioned production method were mixed at a ratio of 2.5 parts to 97.5 parts of the carrier to prepare a two-component developer.
The obtained developer was set in a copying machine in which the latent image carrier was an OPC drum photosensitive member and the cleaning method was blade cleaning, and an image evaluation experiment was performed.
As a result, the dot reproducibility of the image was ranked 4 on a 5-point scale.
[0075]
Example 10
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 9, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
Further, a two-component developer was prepared in the same manner as in Example 9, and an image evaluation experiment was performed. As a result, the dot reproducibility of the image was ranked 5 on a five-point scale.
[0076]
Example 11
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 9, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
Further, a two-component developer was prepared in the same manner as in Example 9, and an image evaluation experiment was performed. As a result, the dot reproducibility of the image was ranked 5 on a five-point scale.
[0077]
Comparative Example 3
Kneading, pulverization, and classification were performed using the same raw materials and production method as in Example 9, and the particles were classified into a particle size distribution having an average particle size of 6.5 μm.
Further, an additive was mixed with 100 parts of the base colored particles under the following mixing conditions to prepare a toner.

After the toner was produced, the height of the toner before compaction was measured by the first evaluation device, and then compacted. The compacted state (space ratio) and fluidity were measured, and the results are as shown in Table 1.
In addition, the toner was compacted by the second evaluation device, and the compacted state (point of failure, void ratio) and fluidity were measured.
Further, a two-component developer was prepared in the same manner as in Example 9, and an image evaluation experiment was performed. As a result, the dot reproducibility of the image was ranked 3 on a five-point scale.
[0078]
[Table 1]

[0079]
[Table 2]

[0080]
As can be seen from the results shown in Tables 1 and 2, there is a strong correlation between the fluidity evaluation value of the toner powder phase by the present evaluation device and the dot reproducibility. It can be seen that can be evaluated.
Further, as can be seen from the graph of FIG. 9 showing the relationship between the torque and the dot reproducibility, and the graph of FIG. 10 showing the relationship between the load and the dot reproducibility, it is necessary to obtain high image quality with good dot reproducibility. In order to obtain a toner having good fluidity, the following conditions must be satisfied. Further, under the following conditions, as can be seen from Table 1, when 20,000 sheets were run, there were no problems in toner transportability such as blocking in the developing section.
{Circle around (1)} The value of the torque when the conical rotor enters is 0.1 to 8.3 mNm.
{Circle around (2)} The value of the load when the conical rotor enters is 0.01 to 1.14 N.
If the torque value at the time of penetration of the conical rotor is less than 0.1 mNm, the charging characteristics other than the fluidity of the toner will be deteriorated and the image quality will be deteriorated. If it is larger than 8.3 mNm, the fluidity will be reduced and the dot reproducibility will be deteriorated. If the load value at the time of entering the conical rotor is less than 0.01 N, the charging characteristics of the toner will deteriorate and the image quality will deteriorate. If the load value exceeds 1.14 N, the fluidity of the toner will decrease and the dot reproducibility will deteriorate.
[0081]
【The invention's effect】
The fluidity of the powder is measured by measuring the height of the toner before consolidation using this evaluation device, consolidating under optimal consolidation conditions, evaluating the consolidation state, and then allowing the conical rotor to enter the powder phase while rotating. By measuring the torque or load generated when the conical rotor moves through the powder phase, the fluidity of the powder can be evaluated with high precision and without individual differences, and a toner with high image quality can be obtained. The conditions (1) and (2) are precisely defined so that a toner with high image quality can be stably produced.
[Brief description of the drawings]
FIG. 1 is a conceptual diagram of a configuration example of a first powder fluidity evaluation device of the present invention.
FIG. 2 is a diagram showing a configuration example of a height measuring unit before consolidation in the first powder fluidity evaluation device of the present invention.
FIG. 3 is a diagram showing an example of the shape of a conical rotor.
FIG. 4 is a diagram showing another example of the shape of the conical rotor (change in the cross-sectional shape of the conical rotor, change in the cone apex angle).
FIG. 5 is a conceptual diagram of a configuration example of a second powder fluidity evaluation device of the present invention. .
FIG. 6 is a diagram showing a configuration example of a height measuring unit before consolidation in a second powder fluidity evaluation device of the present invention.
FIG. 7 is a schematic diagram illustrating an example of a toner manufacturing apparatus using the present evaluation device.
FIG. 8 shows an example of a developing device using a toner produced using the present evaluation device.
FIG. 9 is a diagram showing a relationship between torque and dot reproducibility when a conical rotor enters in Examples 1 to 11 and Comparative Examples 1 to 3.
FIG. 10 is a diagram showing the relationship between the load and the dot reproducibility when the conical rotor enters in Examples 1 to 11 and Comparative Examples 1 to 3.

Claims (29)

It is necessary to measure the torque or load generated when the conical rotor moves through the powder layer by rotating the conical rotor into the powder layer compacted by the consolidation means and evaluate the fluidity of the toner. A conical rotor that is used to enter the toner layer while rotating, a torque meter that detects torque applied to the rotating conical rotor, a load cell that detects a load applied to the container by rotation of the conical rotor, and moves the conical rotor or the container up and down. What is claimed is: 1. A powder fluidity evaluation device comprising at least an elevator, comprising: means for measuring the height of a powder phase before compaction. 2. The powder phase according to claim 1, wherein after measuring the height of the powder phase by a powder phase height measuring means before compaction in advance, the compaction condition is controlled by the height information to compact the powder phase. Powder fluidity evaluation device. Using the height of the powder phase before consolidation measured by the powder phase height measuring means before consolidation, the distance between the piston and the powder phase during consolidation is in the range of 1 to 10 mm to the powder phase surface of the piston. The powder fluidity evaluation device according to claim 1 or 2, wherein the collision speed of the powder is reduced. Before measuring the height of the powder phase before consolidation, the state of the powder phase is stabilized by a vibrator provided below the container, and then the powder phase before consolidation is measured by the powder phase height measuring means before consolidation. The powder fluidity evaluation device according to any one of claims 1 to 3, wherein a height of the powder fluidity is measured. The powder fluidity evaluation device according to any one of claims 1 to 4, wherein the porosity of the powder phase after compaction is set to 0.4 to 0.7. The conical rotor is caused to penetrate into the powder layer compacted by the compacting means while rotating, and the torque or load generated when the conical rotor moves through the powder layer is measured to evaluate the fluidity of the powder. A cone rotor that enters the powder layer while rotating, a torque meter that detects the torque applied to the rotating cone rotor, a load cell that detects the load applied to the container by the rotation of the cone rotor, and raises and lowers the cone rotor or the container. What is claimed is: 1. A powder fluidity evaluation device comprising at least an elevator for moving, wherein a positioning means is provided to prevent the container from moving during compaction. 7. The powder fluidity evaluation device according to claim 6, wherein the positioning means uses the uneven shape of the bottom surface of the container. The powder fluidity evaluation device according to claim 6 or 7, wherein a distance between a piston for performing the consolidation and a side surface of the container is in a range of 1 to 1000 µm. The powder fluidity evaluation device according to any one of claims 6 to 8, wherein the amplitude of the surface roughness inside the container is in the range of 0.01 to 100 µm. The powder fluidity evaluation device according to any one of claims 6 to 9, wherein the hardness of the container material is greater than the hardness of the piston material. The powder fluidity evaluation device according to any one of claims 6 to 10, wherein Al is used as a material of the container. 12. A vibrator under the container, wherein the powder phase is stabilized by the vibrator before consolidation, and then consolidation is performed. Powder fluidity evaluation device. 13. The powder fluidity evaluation device according to claim 1, wherein the apex angle of the conical rotor is 20 to 150 [deg.]. 14. The powder fluidity evaluation device according to claim 1, wherein a groove is formed in a surface of the conical rotor. The powder fluidity evaluation device according to any one of claims 1 to 14, wherein the number of revolutions of the conical rotor is 0.1 to 100 rpm. The powder fluidity evaluation device according to any one of claims 1 to 15, wherein a penetration speed of the conical rotor is 0.5 to 150 mm / min. The torque value when the conical rotor 20 mm penetrates into the conical rotor 20 mm while rotating the toner after the mixing step of mixing the additive, using the powder fluidity evaluation device according to any one of claims 1 to 16. 0.3 mNm. The load value when the conical rotor 20 mm enters while rotating the toner after the mixing step of mixing the additive is 0.01 to 1 using the powder fluidity evaluation device according to any one of claims 1 to 16. 14. An electrostatic charge developing toner, characterized in that it has a pressure of 14 N. 19. The electrostatic charge developing toner according to claim 17, wherein a charge control agent and / or a release agent is included in at least a toner composed of a resin and a pigment. The electrostatic charge developing toner according to any one of claims 17 to 19, wherein an additive is attached or fixed to the surface of the toner powder. 21. The electrostatic charge developing toner according to claim 17, wherein the toner has an average particle diameter of 4 to 10 [mu] m. 22. The toner according to claim 17, wherein the toner is manufactured by a polymerization method or a spray drying method. 23. The toner according to claim 17, wherein the toner has an average circularity of 0.9 to 0.99. 24. A one-component developing method comprising performing contact or non-contact development using the electrostatic charge developing toner according to claim 17. The one-component developing method according to claim 24, wherein a doctor roller is used. 24. A two-component developing method, wherein the developing is performed using the developer for electrostatic charge development according to claim 17 and a developer comprising a carrier having a particle size of 20 to 100 [mu] m. 27. The developing method according to claim 24, wherein the developing is performed by applying an AC bias voltage component. 17. A method for producing an electrostatic charge developing toner, comprising: performing an evaluation in a toner production process using the powder fluidity evaluation apparatus according to claim 1; and producing the toner based on the evaluation. Method. A toner cartridge containing the toner according to any one of claims 17 to 23.

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